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Sample records for cations potentiometric titration

  1. A potentiometric titration study of the interaction of heparin with metal cations.

    PubMed Central

    Grant, D; Long, W F; Williamson, F B

    1992-01-01

    Potentiometric titrations, at ionic strengths (I) ranging from 0.0057 to 0.336, suggest that Ca2+, Cu2+, Li+ and Na+ bind to heparin in a manner that depends on cation identity. These interactions were less affected by the value of I than those of heparin with Mg2+, which binds weakly below I0.050 and with K+, which binds weakly at I0.0057. Of the interactions studied, that of heparin with Cu2+ was the least readily reversible. PMID:1637338

  2. 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.

  3. 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.

  4. Potentiometric titrations of rutile suspensions to 250 C

    SciTech Connect

    Machesky, M.L.; Wesolowski, D.J.; Palmer, D.A.; Ichiro-Hayashi, Ken

    1998-04-15

    A stirred hydrogen electrode concentration cell was used to conduct potentiometric titrations of rutile suspensions from 25 to 250 C in NaCl and tetramethylammonium chloride media (0.03 to 1.1 m). Hydrothermal pretreatment of the rutile improved titration reproducibility, decreased titration hysteresis, and facilitated determination of the point of zero net proton charge (pHznpc). These pHznpc values are 5.4, 5.1, 4.7, 4.4, 4.3 ({+-} 0.2 pH units), and 4.2 ({+-} 0.3 pH units) at 25, 50, 100, 150, 200, and 250 C, respectively. The difference between these pHznpc values and 1/2 pK{sub w} (the neutral pH of water) is rather constant between 25 and 250 C ({minus} 1.45 {+-} 0.2). This constancy is useful for predictive purposes and, more fundamentally, may reflect similarities between the hydration behavior of surface hydroxyl groups and water. A three-layer, 1pKa surface complexation model with three adjustable parameters (two capacitance values and one counterion binding constant) adequately described all titration data. The most apparent trend in these data for pH values greater than the pHznpc was the increase in proton release (negative surface charge) with increasing temperature. This reflects more efficient screening by Na{sup +} relative to Cl{sup {minus}}. Replacing Na{sup +} with the larger tetramethylammonium cation for some conditions resulted in decreased proton release due to the less efficient screening of negative surface charge by this larger cation.

  5. 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.

  6. Monte Carlo studies on potentiometric titration of (carboxymethyl)cellulose.

    PubMed

    Nishio, T

    1996-01-01

    Monte Carlo simulations of the potentiometric titration are carried out for (carboxymethyl)cellulose in aqueous salt solutions by a previously developed method. A nearly elliptic cylinder with spherical ionizable groups is assumed as model of (carboxymethyl)cellulose molecule. The spherical charges with a hard core potential are adopted as mobile hydrated ions. A fairly satisfactory agreement of the titration curves with the experimental data is achieved by using reasonable molecular dimensions. Dependence of the calculated titration profiles on the molecular model and the characteristics of the system are discussed. PMID:17023342

  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. Potentiometric titration of gold, platinum, and some other precious metals

    SciTech Connect

    Selig, W.S.

    1991-02-04

    Gold, platinum, and several other platinum metals can be determined by titration with cetylpyridinium chloride (CPC). CPC forms a precipitate with AuCl{sub 4}{sup {minus}} and PtCl{sub 6}{sup 2{minus}}. Differentiation of AuCl{sub 4{minus}} and PtCl{sub 6}{sup 2{minus}} with this titrant is not possible; however, their sum can be determined. Titration with tetraphenylarsonium chloride at pH 1 is selective for tetrachloroaurate, which thus can be determined in the presence of hexachloroplatinate. Hexachloroosmate(IV), tetrachloroplatinite(II), tetrachloropalladate(II), hexachloropalladate(IV), and hexachloroiridate(IV) can also be determined potentiometrically vs. CPC. The indicating electrode is prepared by coating a spectroscopic graphite rod with a solution of poly(vinyl chloride) (PVC) and dioctylphthalate (DOP) in tetrahydrofuran (THF). Gold in gold cyanide plating baths and in potassium aurocyanide can be determined by potentiometric titration vs standard silver nitrate, using a silver ion-selective indicating electrode. The monovalent gold need not be converted to the trivalent state with aqua regia, resulting in a considerable saving of time and effort. Free cyanide and aurocyanide can be titrated sequentially by this method. Chloride does not interfere and can, in fact, also be sequentially determined. 17 refs., 2 figs., 3 tabs.

  10. 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. PMID:26320956

  11. 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 probably part of a single macromolecular scaffold. Fresh Ulva tissue appears to contain the same three functional groups but at lower concentrations, based on wet weight. The titration in natural seawater was largely dominated by the non-carbonate alkalinity of the solution and could not be robustly modeled. Results of fits with ionic strengths fixed at their experimental values indicate that the pKas of all three groups display prominent Debije-Hückel-type behavior, hence that these acid dissociation reactions involve a different mechanism than metal-proton exchange reactions on mineral surfaces, whose distribution coefficients (i.e., equilibrium constants) generally show a weak ionic strength dependence.

  12. 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.

  13. Simple home-made sensors for potentiometric titrations. [Nitroform CH(NO/sub 2/)/sub 3/

    SciTech Connect

    Selig, W.

    1982-04-01

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

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

    NASA Astrophysics Data System (ADS)

    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 KIO3 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.

  15. 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.

  16. 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. PMID:12207255

  17. Stabilization of the initial electrochemical potential for a metal-based potentiometric titration study of a biosorption process.

    PubMed

    Naja, Ghinwa; Mustin, Christian; Volesky, Bohumil; Berthelin, Jacques

    2006-01-01

    An interactive metal-based potentiometric titration method has been developed using an ion selective electrode for studying the sorption of metal cations. The accuracy of this technique was verified by analyzing the metal sorption mechanism for the biomass of Rhizopus arrhizus fungus and diatomite, two dissimilar materials (organic and mineral, strong sorbent and weak sorbent) of a different order of cation exchange capacity. The problem of the initial electrochemical potential was addressed identifying the usefulness of a Na-sulfonic resin as a strong chelating agent applied before the beginning of sorption titration experiments so that the titration curves and the sorption uptake could be quantitatively compared. The resin stabilized the initial electrochemical potential to -405+/-5 mV corresponding to 2 micro gl(-1) of lead concentration in solution. The amounts of lead sorbed by R. arrhizus biomass and diatomite were 0.9 mmol g(-1) (C(e)=5.16 x 10(-2)mM) and 0.052 mmol g(-1) (C(e)=5.97 x 10(-2) mM), respectively. Lead sorption by the fungal biomass was pinpointed to at least two types of chemical active sites. The first type was distinguished by high reactivity and a low number of sites whereas the other was characterized by their higher number and lower reactivity. PMID:16325652

  18. Zn(2+)-heparin interaction studied by potentiometric titration.

    PubMed Central

    Grant, D; Long, W F; Williamson, F B

    1992-01-01

    Measurement of the decrease in pH that accompanies the addition of Zn2+ to heparin in solution provided an indirect method of examining cation-polyanion interaction. Construction of plots analogous to isothermal saturation binding plots revealed the existence, for defined conditions of interaction, of a [heparin]-independent direct proportionality between the fraction of the maximal pH change occurring and the [Zn2+]/[heparin disaccharide] ratio. This accords with results from polarimetric examination of Ca(2+)- and Cu(2+)-heparin interactions. It suggests that, under the conditions used, cation-heparin interaction may result in the formation of a complex that exists in a colloid-like phase, between which and the aqueous phase, exchange of cations does not follow simple solution-phase reversible equilibrium thermodynamic behaviour. The results suggest that the putative Zn(2+)-containing complex is less stable in the presence of NaCl than is the corresponding Ca(2+)-containing complex. Addition of Zn2+ to low concentrations of heparins is accompanied by the usual decrease in pH, followed by a removal of H+ from solution as the [Zn2+]/[heparin disaccharide] ratio increases, suggesting dissolution of the putative complex. This reversal of the initial pH change was not seen for most other cation-heparin interactions under the conditions studied. PMID:1445244

  19. 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. PMID:15984215

  20. Potentiometric Titration of Industrial Samples—End-point Detection by Means of Wavelets

    NASA Astrophysics Data System (ADS)

    Jakubowska, M.; Baś, B.; Niewiara, E.; Reczyński, W.; Kubiak, W. W.

    2009-08-01

    A continuous wavelet transform with a specially defined dedicated mother wavelet is applied for data treatment as a signal-processing tool in a potentiometric titration. The inflection points of the titration curve are localized in one step of the calculations. The imperfection of signal, random noise, or spikes has no influence on the operation of the procedure. The proposed algorithm does not require any prior information about the nature or the type of analyte and/or the shape of the titration curve. Although the optimization of transformation parameters should be done, they may be chosen from a wide interval. The accuracy and precision of the proposed end-point estimation is examined on several simulated curves and instrumental potentiometric titrations. Under normal working conditions, analyte concentrations with variation coefficients between 1% and 5% have been determined. The procedure based on the wavelets provides an objective criterion for the determination of the end point. It can be reproduced and fully automated, thus contributing to a more versatile titration analysis.

  1. Determination of the pKa values of beta-blockers by automated potentiometric titrations.

    PubMed

    Martínez, V; Maguregui, M I; Jiménez, R M; Alonso, R M

    2000-08-15

    The acid-base equilibrium constants of the beta-blockers atenolol, oxprenolol, timolol and labetalol were determined by automated potentiometric titrations. The pKa values were obtained in water-rich or water methanol medium (20% MeOH) to obviate the solubility problems associated with the compounds. The initial estimates of pKa values were obtained from Gran's method and then, were refined by the NYTIT and ZETA versions of the LETAGROP computer program. The resultant values were 9.4 (I = 0.1 M KCl, 20% methanol) for atenolol, 9.6 (I = 0.1 M KCl) for oxprenolol, 9.4 (I = 0.1 M KCl, 20% methanol) for timolol and 7.4 and 9.4 (I = 0.1 M KCl) for labetalol. The potentiometric method was found to be accurate and easily applicable. The operational criteria for applying the methodology are indicated. PMID:10933539

  2. 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.

  3. Comparison of HPLC, UV spectrophotometry and potentiometric titration methods for the determination of lumefantrine in pharmaceutical products.

    PubMed

    da Costa César, Isabela; Nogueira, Fernando Henrique Andrade; Pianetti, Gérson Antônio

    2008-09-10

    This paper describes the development and evaluation of a HPLC, UV spectrophotometry and potentiometric titration methods to quantify lumefantrine in raw materials and tablets. HPLC analyses were carried out using a Symmetry C(18) column and a mobile phase composed of methanol and 0.05% trifluoroacetic acid (80:20), with a flow rate of 1.0ml/min and UV detection at 335nm. For the spectrophotometric analyses, methanol was used as solvent and the wavelength of 335nm was selected for the detection. Non-aqueous titration of lumefantrine was carried out using perchloric acid as titrant and glacial acetic acid/acetic anhydride as solvent. The end point was potentiometrically determined. The three evaluated methods showed to be adequate to quantify lumefantrine in raw materials, while HPLC and UV methods presented the most reliable results for the analyses of tablets. PMID:18571353

  4. Uncertainty evaluation in the chloroquine phosphate potentiometric titration: application of three different approaches.

    PubMed

    Rodomonte, Andrea Luca; Montinaro, Annalisa; Bartolomei, Monica

    2006-09-11

    A measurement result cannot be properly interpreted if not accompanied by its uncertainty. Several methods to estimate uncertainty have been developed. From those methods three in particular were chosen in this work to estimate the uncertainty of the Eu. Ph. chloroquine phosphate assay, a potentiometric titration commonly used in medicinal control laboratories. The famous error-budget approach (also called bottom-up or step-by-step) described by the ISO Guide to the expression of Uncertainty in Measurement (GUM) was the first method chosen. It is based on the combination of uncertainty contributions that have to be directly derived from the measurement process. The second method employed was the Analytical Method Committee top-down which estimates uncertainty through reproducibility obtained during inter-laboratory studies. Data for its application were collected in a proficiency testing study carried out by over 50 laboratories throughout Europe. The last method chosen was the one proposed by Barwick and Ellison. It uses a combination of precision, trueness and ruggedness data to estimate uncertainty. These data were collected from a validation process specifically designed for uncertainty estimation. All the three approaches presented a distinctive set of advantages and drawbacks in their implementation. An expanded uncertainty of about 1% was assessed for the assay investigated. PMID:16870384

  5. 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.

  6. 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-Lovri?, 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. PMID:18267138

  7. 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.

  8. Effect of water content in perchloric acid on the non-aqueous potentiometric titration of nitrogen-containing compounds.

    PubMed

    Qi, X S; Miller, R B; Namiki, Y; Zhang, J; Jacobus, R

    1997-11-01

    In the United States Pharmacopeia (USP), 0.1 N perchloric acid in acetic acid volumetric solution (hereafter HClO4 VS) used for non-aqueous titration has specified a water content between 0.02 and 0.05%. Preparing this titrant with such a narrow range of water content is very time consuming, precludes the use of commercially available titrants, and, consequently, prompted an investigation to try and expand the range up to 0.5%. In this study, the titrimetric results obtained using HClO4 VS containing more water were very close to those obtained using the USP specified titrants. A maximum assay difference of 0.7% in the titrations of three selected nitrogen-containing compounds, clonidine hydrochloride, dipyridamole, and adenosine were observed. The titrimetric results obtained using these titrants were also precise with RSDs of not more than 0.4%. Therefore, a wider range of water content in HClO4 VS between 0.02 and 0.5% is suggested for the USP potentiometric titration of nitrogen-containing compounds. PMID:9589398

  9. Automated Potentiometric Titrations in KCl/Water-Saturated Octanol: Method for Quantifying Factors Influencing Ion-Pair Partitioning

    PubMed Central

    2009-01-01

    The knowledge base of factors influencing ion pair partitioning is very sparse, primarily because of the difficulty in determining accurate log PI 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 PI 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 PN − I)). Simple model compounds can be used. The titration procedure is described in detail, along with a program for calculating pKa′′ 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 PI and log D. In contrast to the common assumption that diff (log PN − 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 PI 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 PI. 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 DN and log DI. This work also brings attention to the fascinating world of nature’s highly stabilized ion pairs. PMID:19265385

  10. 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.; Barczy?ski, 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 ?-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.

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

    PubMed

    Meloun, Milan; Ne?asová, Veronika; Jav?rek, 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 (?pK>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

  12. 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 ?-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 these studies are restricted to goethite, those studies in which titrations with excess acid and base have been used for the determination of proton active site concentrations of sorbents should be reconsidered.

  13. Potentiometric titrations of Bacillus subtilis cells to low pH and a comparison of modeling approaches

    NASA Astrophysics Data System (ADS)

    Fein, Jeremy B.; Boily, Jean-François; Yee, Nathan; Gorman-Lewis, Drew; Turner, Benjamin F.

    2005-03-01

    To provide constraints on the speciation of bacterial surface functional groups, we have conducted potentiometric titrations using the gram-positive aerobic species Bacillus subtilis, covering the pH range 2.1 to 9.8. Titration experiments were conducted using an auto-titrator assembly, with the bacteria suspended in fixed ionic strength (0.01 to 0.3 M) NaClO 4 solutions. We observed significant adsorption of protons over the entire pH range of this study, including to the lowest pH values examined, indicating that proton saturation of the cell wall did not occur under any of the conditions of the experiments. Ionic strength, over the range studied here, did not have a significant effect on the observed buffering behavior relative to experimental uncertainty. Electrophoretic mobility measurements indicate that the cell wall is negatively charged, even under the lowest pH conditions studied. These experimental results necessitate a definition of the zero proton condition such that the total proton concentration at the pH of suspension is offset to account for the negative bacterial surface charge that tends towards neutrality at pH <2. The buffering intensity of the bacterial suspensions reveals a wide spread of apparent pKa values. This spread was modeled using three significantly different approaches: a Non-Electrostatic Model, a Constant Capacitance Model, and a Langmuir-Freundlich Model. The approaches differ in the manner in which they treat the surface electric field effects, and in whether they treat the proton-active sites as discrete functional groups or as continuous distributions of related sites. Each type of model tested, however, provides an excellent fit to the experimental data, indicating that titration data alone are insufficient for characterizing the molecular-scale reactions that occur on the bacterial surface. Spectroscopic data on the molecular-scale properties of the bacterial surface are required to differentiate between the underlying mechanisms of proton adsorption inherent in these models. The applicability and underlying conceptual foundation of each model is discussed in the context of our current knowledge of the structure of bacterial cell walls.

  14. Electrohydrodynamic properties of succinoglycan as probed by fluorescence correlation spectroscopy, potentiometric titration and capillary electrophoresis.

    PubMed

    Duval, Jérôme F L; Slaveykova, Vera I; Hosse, Monika; Buffle, Jacques; Wilkinson, Kevin J

    2006-10-01

    The electrostatic, hydrodynamic and conformational properties of aqueous solutions of succinoglycan have been analyzed by fluorescence correlation spectroscopy (FCS), proton titration, and capillary electrophoresis (CE) over a large range of pH values and electrolyte (NaCl) concentrations. Using the theoretical formalism developed previously for the electrokinetic properties of soft, permeable particles, a quantitative analysis for the electro-hydrodynamics of succinoglycan is performed by taking into account, in a self-consistent manner, the measured values of the diffusion coefficients, electric charge densities, and electrophoretic mobilities. For that purpose, two limiting conformations for the polysaccharide in solution are tested, i.e. succinoglycan behaves as (i) a spherical, random coil polymer or (ii) a rodlike particle with charged lateral chains. The results show that satisfactory modeling of the titration data for ionic strengths larger than 50 mM can be accomplished using both geometries over the entire range of pH values. Electrophoretic mobilities measured for sufficiently large pH values (pH > 5-6) are in line with predictions based on either model. The best manner to discriminate between these two conceptual models is briefly discussed. For low pH values (pH < 5), both models indicate aggregation, resulting in an increase of the hydrodynamic permeability and a decrease of the diffusion coefficient. PMID:17025358

  15. Predicting proton titration in cationic micelle and bilayer environments.

    PubMed

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

    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 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

  16. 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.

  17. 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.

  18. 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. PMID:21543082

  19. Effect of fluoride, chloride, bromide, and thiocynate on potentiometric titrations of iron(II)-tin(II) mixtures with cerium(IV)

    SciTech Connect

    Kwok, Y.M.

    1980-07-31

    A two-step curve is expected in the potentiometric titration of Fe(II)-Sn(II) mixtures with Ce(IV) in H/sub 2/SO/sub 4/. Each end point should indicate the respective oxidation of Sn(II) and Fe(II). However, experimentally only one end point was found; it corresponded to the total oxidation of Sn(II) and Fe(II). When this oxidation-reduction reaction was carried out in the presence of Cl/sup -/, the theoretical behavior was observed. The present study was done to ascertain if monovalent anions other than Cl/sup -/ have a similar effect on this oxidation-reduction system. The monovalent species F/sup -/, Br/sup -/, and SCN/sup -/ were selected for this study, and the results indicate that each affects the rate of reaction relative to the ease of oxidation of the individual ions.

  20. 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. PMID:18969846

  1. 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 at 50 mmol L -1 KCl the extra negative charge due to the interaction between polyDADMAC and PAHA is just compensated by K + incorporation in the complex. Therefore, a pseudo 1-1 stoichiometry exists at about 50 mmol L -1 1-1 electrolyte concentration and only at this salt concentration polyDADMAC titrations and conventional proton titrations give identical results. Most likely this is also true for other HA samples and other pH values. For FA further study is required to reveal the conditions for which polyDADMAC and proton titrations give identical results.

  2. 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. PMID:25365626

  3. The Determination of the pKaof Multiprotic, Weak Acids by Analyzing Potentiometric Acid Base Titration Data with Difference Plots

    NASA Astrophysics Data System (ADS)

    Kraft, Arno

    2003-05-01

    This paper discusses the pKa determination of mono-, di-, and triprotic weak acids with the help of difference (Bjerrum) plots, and the effect of strong acid base concentration errors, ligand weight errors, and nonlinear electrode response. Experimental examples are given for the titration of an acidic heterocycle, as well as glycine, ethylenediamine, and tris(2-aminoethyl)amine (the last two after addition of excess HCl to ensure complete protonation) with standarized NaOH. The analysis procedure makes use of Microsoft Excel spreadsheets and nonlinear least squares curve fitting of the experimental data to the theoretical Bjerrum function. In addition to providing pKa values for mono- and multiprotic acids, this approach has been found suitable for detecting small errors in parameters, such as strong acid and ligand concentration, and corrections can often become necessary to achieve the best fit. Difference plots allow the pKa values of monoprotic and multiprotic weak acids to be determined rapidly and with good precision.

  4. Mixtures of hydrogenated and fluorinated lactobionamide surfactants with cationic surfactants: study of hydrogenated and fluorinated chains miscibility through potentiometric techniques.

    PubMed

    Peyre, Véronique; Patil, Sandeep; Durand, Grégory; Pucci, Bernard

    2007-11-01

    The work reported herein deals with the aqueous behavior of hydrocarbon and/or fluorocarbon ionic and nonionic surfactants mixtures. These mixtures were studied using potentiometric techniques in NaBr (0.1 mol L-1) aqueous solution as well as in pure water. Mixed micelles were formed from a cationic surfactant (dodecyl or tetradecyltrimethylammonium bromide respectively called DTABr or TTABr) and neutral lactobionamide surfactants bearing a hydrogenated dodecyl chain (H12Lac) or a fluorinated chain (CF3-(CF2)5-(CH2)2- or CF3-(CF2)7-(CH2)2-). We showed that concentrations of ionic and nonionic surfactants in the monomeric form as well as the composition of the mixed micelles can be specified thanks to a potentiometric technique. The complete characterization does not request any model of micellization a priori. The activities of the micellar phase constituents, as well as the free enthalpies of mixing, were calculated. The subsequent interpretation only relies on the experimental characterization. Comparison of the behaviors of the various systems with a model derived from the regular solution theory reveals the predominant part of electrostatic interactions in the micellization phenomenon. It also appears that the energy of interaction between hydrogenated and fluorinated chains is unfavorable to mixing and is of much lower magnitude than the electric charges interactions. PMID:17935362

  5. Determination of pKa values of new phenacyl-piperidine derivatives by potentiometric titration method in aqueous medium at room temperature (25±0.5oC).

    PubMed

    Zafar, Shaista; Akhtar, Shamim; Tariq, Talat; Mushtaq, Noushin; Akram, Arfa; Ahmed, Ahsaan; Arif, Muhammad; Naeem, Sabahat; Anwar, Sana

    2014-07-01

    Dissociation constant (pKa) of ten novel phenacyl derivatives of piperidine were determined by potentiometric titration method in aqueous medium at room temperature (25 ±0.5°C). The sample solutions were prepared in deionized water with ionic strength 0.01M and titrated with 0.1M NaOH solution. In addition, ?G values were also calculated. Different prediction software programs were used to calculate pKa values too and compared to the experimentally observed pKa values. The experimental and theoretical values were found in close agreement. The results obtained in this research would help to predict the good absorption of the studied compounds and can be selected as lead molecules for the synthesis of CNS active agents because of their lipophilic nature especially compound VII. PMID:25015461

  6. 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

  7. The effects of O-substituents of hexahomotrioxacalix[3]arene on potentiometric discrimination between dopamine and biological organic/inorganic cations.

    PubMed

    Saijo, Ryosuke; Murakami, Hiroyuki; Tsunekawa, Saori; Imanishi, Souhei; Shirai, Naohiro; Ikeda, Shin-Ichi; Odashima, Kazunori

    2007-03-01

    As an interesting type of molecular recognition at a membrane surface, the tri-O-acetic acid ester (host 2) of hexahomotrioxacalix[3]arene, when incorporated into poly(vinyl chloride) (PVC) liquid membranes, displays a high potentiometric selectivity for dopamine over, not only other catecholamines (noradrenaline, adrenaline), but also quaternary ammonium guests (tetramethylammonium, choline, and acetylcholine) and inorganic cations (Na+, K+, NH4+). Interestingly, changes in membrane potential based on the host-guest complexation of host 2 that were observed dopamine/inorganic cation selectivity were not displayed by the related hosts 3 and 4, which contain amide substituents. This paper describes our efforts to separately estimate the two factors contributing to the dopamine selectivities, i.e., the guest lipophilicity factor and the host-guest complexation factor, in an attempt to understand the effects of the O-substituents of these hosts. The potentiometric experiments showed that, although the guests had roughly equal lipophilicity, the electromotive force (EMF) response for dopamine by host 2 was excellent. Furthermore, host 2 displayed ca. a 20-fold stronger complexation for dopamine, compared to noradrenaline, adrenaline, K+, and NH4+ cations. These results indicate that the high potentiometric selectivity of the ion-selective electrode for dopamine mainly reflect, not the guest lipophilicity factor but the host-guest complexation factor. On the other hand, host 3 displayed ca. a 3000-fold stronger binding to Na+ than dopamine, thus explaining the reasons for the lower dopamine-selectivities of host 3 compared to host 2. It is interesting to note that the high potentiometric selectivities for dopamine were displayed by not only host 2 but also host 5, regardless of the simple structure of the O-substituents. PMID:17329883

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

    PubMed

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

    2006-12-19

    We perform differential potentiometric titration measurements for the binding of Ca2+ ions to micelles composed of the carboxylic acid end-standing Pluronic P85 block copolymer (i.e., CAE-85 (COOH-(EO)26-(PO)39-(EO)26-COOH)). Two different ion-selective electrodes (ISEs) are used to detect the free calcium concentration; the first ISE is an indicator electrode, and the second is a reference electrode. The titration is done by adding the block copolymers to a known solution of Ca2+ at neutral pH and high enough temperature (above the critical micellization temperature CMT) and various amount of added monovalent salt. By measuring the difference in the electromotive force between the two ISEs, the amount of Ca2+ that is bound by the micelles is calculated. This is then used to determine the binding constant of Ca2+ with the micelles, which is a missing parameter needed to perform molecular realistic self-consistent-field (SCF) calculations. It turns out that the micelles from block copolymer CAE-85 bind Ca2+ ions both electrostatically and specifically. The specific binding between Ca2+ and carboxylic groups in the corona of the micelles is modeled through the reaction equilibrium -COOCa+ <==> -COO- + Ca2+ with pKCa = 1.7 +/- 0.06. PMID:17154568

  9. 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

  10. 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

  11. A potentiometric study of the adsorption of a cationic surfactant onto laponite in water-methanol and water-dimethylsulfoxide mixtures.

    PubMed

    Turmine, M; Mayaffre, A; Letellier, P

    2003-08-01

    We studied the adsorption of a cationic surfactant, dodecyltrimethylammonium bromide (DTABr), onto laponite in water-methanol and water-DMSO mixtures at 298 K. Adsorption isotherms were determined by potentiometric methods using DTA(+) and Br(-)-selective electrodes. All of the isotherm shapes in the mixture were classical. Activity coefficients were determined for the transfer between water and hydroorganic mixtures. Comparison of the adsorption isotherms obtained for different surfactant chemical potentials showed that at higher concentrations of free surfactant, the aggregation state does not depend on the nature of the surrounding media. A study of the influence of the ionic strength showed that there is a common intersection point in each hydroorganic mixture. This point corresponds to the charge compensation point and depends on the nature of the surrounding medium. PMID:12885513

  12. A comparison of cationic polymerization and esterification for end-point detection in the catalytic thermometric titration of organic bases.

    PubMed

    J Greenhow, E; Viñas, P

    1984-08-01

    A systematic comparison has been made of two indicator systems for the non-aqueous catalytic thermometric titration of strong and weak organic bases. The indicator reagents, alpha-methylstyrene and mixtures of acetic anhydride and hydroxy compounds, are shown to give results (for 14 representative bases) which do not diner significantly in coefficient of variation or titration error. Calibration graphs for all the samples, in the range 0.01-0.1 meq, are linear, with correlation coefficients of 0.995 or better. Aniline, benzylamine, n-butylamine, morpholine, pyrrole, l-dopa, alpha-methyl-l-dopa, dl-alpha-alanine, dl-leucine and l-cysteine cannot be determined when acetic anhydride is present in the sample solution, but some primary and second amines can. This is explained in terms of rates of acetylation of the amino groups. PMID:18963660

  13. 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)

  14. Precipitation titration of perchlorate using new titrants

    SciTech Connect

    Selig, W.

    1980-05-01

    We have evaluated the following new titrants for the potentiometric precipitation titration of perchlorate: cetyltrimethylammonium chloride (CETAC), cetyltrimethylammonium bromide (CETAB), cetylpyridinium chloride (CPC), and benzyldimethyltetradecylammonium chloride (BDTAC). Titrations were monitored with a fluoroborate ion-selective electrode (ISE) and a double-junction reference electrode. The titration system was controlled by a Tektronix 4051 graphics system. The perchlorate, nitrate, and calcium ISE may also be used to monitor emf's. 7 tables, 2 figures.

  15. Structure of the S. aureus PI-specific phospholipase C reveals modulation of active site access by a titratable ?-cation latched loop.

    PubMed

    Goldstein, Rebecca; Cheng, Jiongjia; Stec, Boguslaw; Roberts, Mary F

    2012-03-27

    Staphylococcus aureus secretes a phosphatidylinositol-specific phospholipase C (PI-PLC) as a virulence factor that is unusual in exhibiting higher activity at acidic pH values than other enzymes in this class. We have determined the crystal structure of this enzyme at pH 4.6 and pH 7.5. Under slightly basic conditions, the S. aureus PI-PLC structure closely follows the conformation of other bacterial PI-PLCs. However, when crystallized under acidic conditions, a large section of mobile loop at the ??-barrel rim in the vicinity of the active site shows ~10 Å shift. This loop displacement at acidic pH is the result of a titratable intramolecular ?-cation interaction between His258 and Phe249. This was verified by a structure of the mutant protein H258Y crystallized at pH 4.6, which does not exhibit the large loop shift. The intramolecular ?-cation interaction for S. aureus PI-PLC provides an explanation for the activity of the enzyme at acid pH and also suggests how phosphatidylcholine, as a competitor for Phe249, may kinetically activate this enzyme. PMID:22390775

  16. 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. © 2015 Wiley Periodicals, Inc. Biopolymers 105: 199-211, 2016. PMID:26574155

  17. Titration Techniques

    NASA Astrophysics Data System (ADS)

    Jacobsen, Jerrold J.; Houston Jetzer, Kelly; Patani, Néha; Zimmerman, John; Zweerink, Gerald

    1995-07-01

    Significant attention is paid to the proper technique for reading a meniscus. Video shows meniscus-viewing techniques for colorless and dark liquids and the consequences of not reading a meniscus at eye level. Lessons are provided on approaching the end point, focusing on end point colors produced via different commonly used indicators. The concept of a titration curve is illustrated by means of a pH meter. Carefully recorded images of the entire range of meniscus values in a buret, pipet, and graduated cylinder are included so that you can show your students, in lecture or pre-lab discussion, any meniscus and discuss how to read the buret properly. These buret meniscus values are very carefully recorded at the rate of one video frame per hundredth of a milliliter, so that an image showing any given meniscus value can be obtained. These images can be easily incorporated into a computer-based multimedia environment for testing or meniscus-reading exercises. Two of the authors have used this technique and found the exercise to be very well received by their students. Video on side two shows nearly 100 "bloopers", demonstrating both the right way and wrong ways to do tasks associated with titration. This material can be used in a variety of situations: to show students the correct way to do something; to test students by asking them "What is this person doing wrong?"; or to develop multimedia, computer-based lessons. The contents of Titration Techniques are listed below: Side 1 Titration: what it is. A simple titration; Acid-base titration animation; A brief redox titration; Redox titration animation; A complete acid-base titration. Titration techniques. Hand technique variations; Stopcock; Using a buret to measure liquid volumes; Wait before reading meniscus; Dirty and clean burets; Read meniscus at eye level (see Fig. 1); Meniscus viewing techniques--light colored liquids; Meniscus viewing techniques--dark liquids; Using a magnetic stirrer; Rough titration; Significant figures; Approaching the end point; End point colors; Titration with a pH meter; Titration curves; Colors of indicators. Meniscus values. Buret meniscus values; Pipet meniscus values; Graduated cylinder meniscus values. Side 2"Bloopers". Introducing the people; Titration animation; Inspecting the buret; Rinsing the buret with water; Preparing a solid sample; Obtaining a liquid sample; Delivering a liquid sample with a Mohr pipet; Pipetting a liquid sample with a Mohr pipet; Rinsing the Mohr pipet with sample; Using the Mohr pipet to transfer sample; Delivering a liquid sample with a volumetric pipet; Pipetting a liquid sample with a volumetric pipet; Rinsing the volumetric pipet with sample; Using the volumetric pipet to transfer sample; Obtaining the titrant; Rinsing the buret with titrant; Filling the buret with titrant; Adding the indicator; The initial reading; Beginning the titration; Delivering titrant; The final reading. Figure 3. Near the end point a single drop of titrant can cause a lasting color change.

  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 (?4f), nephelauxetic effect (?), bonding (b1/2) and percent covalency (?) parameters have been calculated to explain the nature of complexation. The intensity parameters like oscillator strength (P) and Judd-Ofelt parameters (T?, ? = 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 (?G, ?H and ?S) of complexes were also calculated and the negative values of ?G and ?H show that the complex reactions are spontaneous and exothermic. The positive values of ?S indicate high stability of complex reactions which are enthalpy-driven.

  19. 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)

  20. 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

  1. PVC Membrane Sensors for Potentiometric Determination of Acebutolol

    PubMed Central

    Mostafa, Gamal Abdel-Hafiz; Hefnawy, Mohamed Mahmoud; Al-Majed, Abdulrahman

    2007-01-01

    The construction and general performance characteristics of two novel potentiometric membrane sensors responsive to the acebutolol are described. The sensors are based on the use of ion-association complexes of acebutolol (AC) with tetraphenylborate(TPB) (I) and phosphomolybdate(PM) (II) as exchange sites in a PVC matrix. The sensors show a fast, stable and near- Nernstian for the mono charge cation of AC over the concentration range 1×10-3 - ?10-6 M at 25 °C over the pH range 2.0 - 6.0 with cationic slope of 51.5 ± 0.5 and 53.0 ± 0.5 per concentration decade for AC-I and AC-II sensors respectively. The lower detection limit is 6×10-6 M and 4×0-6 M with the response time 20-30 s in the same order of both sensors. Selectivity coefficients of AC related to a number of interfering cation and some organic compounds were investigated. There are negligible interferences are caused by most of the investigated species. The direct determination of 3 - 370 ?g/ml of AC shows an average recovery of 99.4 and 99.5% and a mean relative standard deviation of 1.5% at 100.0 ?g/ml for sensor I and II respectively. The results obtained by determination of AC in tablets using the proposed sensors which comparable favorably with those obtained by the British pharmacopoeia method. In the present investigation the electrodes have been utilized as end point indicator for some precipitation titration reactions.

  2. 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.

  3. Modern Directions for Potentiometric Sensors.

    PubMed

    Bakker, Eric; Chumbimuni-Torres, Karin

    2008-01-01

    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

  4. 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.

  5. 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??g/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??g/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

  6. 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 ?g/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 ?g/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.

  7. 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.

  8. All-solid-state potentiometric sensors with a multiwalled carbon nanotube inner transducing layer for anion detection in environmental samples.

    PubMed

    Yuan, Dajing; Anthis, Alexandre H C; Ghahraman Afshar, Majid; Pankratova, Nadezda; Cuartero, Maria; Crespo, Gastón A; Bakker, Eric

    2015-09-01

    While ion to electron transducing layers for the fabrication of potentiometric membrane electrodes for the detection of cations have been well established, similar progress for the sensing of anions has not yet been realized. We report for this reason on a novel approach for the development of all-solid-state anion selective electrodes using lipophilic multiwalled carbon nanotubes (f-MWCNTs) as the inner ion to electron transducing layer. This material can be solvent cast, as it conveniently dissolves in tetrahydrofuran (THF), an important advantage to develop uniform films without the need for using surfactants that might deteriorate the performance of the electrode. Solid contact sensors for carbonate, nitrate, nitrite, and dihydrogen phosphate are fabricated and characterized, and all exhibit comparable analytical characteristics to the inner liquid electrodes. For example, the carbonate sensor exhibits a Nernstian slope of 27.2 ± 0.8 mV·dec(-1), a LOD = 2.3 ?M, a response time of 1 s, a linear range of four logarithmic units, and a medium-term stability of 0.04 mV·h(-1) is obtained in a pH 8.6 buffered solution. Water layer test, reversibility, and selectivity for chloride, nitrate, and hydroxide are also reported. The excellent properties of f-MWCNTs as a transducer are contrasted to the deficient performance of poly(3-octyl-thiophene) (POT) for carbonate detection. This is evidenced both with a significant drift in the potentiometric measures as well as a pronounced sensitivity to light (either sunlight or artificial light). This latter aspect may compromise its potential for environmental in situ measurements (night/day cycles). The concentration of carbonate is determined in a river sample (Arve river, Geneva) and compared to a reference method (automatic titrator with potentiometric pH detection). The results suggest that nanostructured materials such as f-MWCNTs are an attractive platform as a general ion-to-electron transducer for anion-selective electrodes. PMID:26272001

  9. 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.

  10. 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.

  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. Micromechanical potentiometric sensors

    DOEpatents

    Thundat, Thomas G. (Knoxville, TN)

    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.

  13. 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.

  14. 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. PMID:21286616

  15. 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 sorption data for which complementary titration data were not available. The two-site model accounts for variability in the titration data and most metal sorption data are fit well using the pKa2 and ?? values reported above. A linear free energy relationship (LFER) appears to exist for some of the metals; however, redox and cation exchange reactions may limit the prediction of surface complexation constants for additional metals using the LFER. ?? 2003 Elsevier Ltd. All rights reserved.

  16. Potentiometric pH sensors based on chemically modified electrodes with electropolymerized metal-tetraaminophthalocyanine.

    PubMed

    Kang, T F; Xie, Z Y; Tang, H; Shen, G L; Yu, R Q

    1997-12-19

    Potentiometric pH sensors based on polymer film were prepared by electropolymerization of the monomer nickel(II)-4,4',4'',4'''-tetraaminophthalocyanine (NiTAPc) or copper(II)-4,4',4'',4'''-tetraaminophthalocyanine (CuTAPc) on glassy carbon (GC) electrodes. The polymer of metal tetraaminophthalocyanine (p-MTAPc) film coated electrodes show a slope of 55 +/- 1 mV/pH (at 20 degrees C) and nearly Nernstain potentiometric response to pH over the range of pH 1-13. The electrodes possess good potential reproducibility and high selectivity, and are useful sensing devices in pH determination and end-point indication of acid-base potentiometric titration. PMID:18967005

  17. 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)

  18. Characterization and determination of titratable groups of proteins by linearization of titration curves. II. Application to lysozyme

    SciTech Connect

    Godinho, O.E.S.; Aleixo, L.M.; Alves, J.P.H.

    1982-07-01

    The potentiometric acid-base titration curves of fully protonated lysozyme at ionic strenghts of 0.10 and 1.0 M has been performed. The stoichiometry and the pK/sub a/ values of each titratable group have been determined through the linearization of titration curves. Two types of carboxylic groups with pK/sub a/ values of 3.76 and 5.02, the imidazole group with pK/sub a/ 7.37 and the amino group with pK/sub a/ 9.63, have been identified at an ionic strength of 0.10 M at 25.0/sup 0/C. The number of titratable groups found per mole of protein has been 5.12 and 5.60 for the two types of carboxylic groups, 1.13 for the imidazole group, and 3.19 for the amino groups. The endpoint of the titration of the protein obtained by this method accords quite well with the endpoint obtained by the use of Gran function applied to the excess of strong base.

  19. A Ho(III) potentiometric polymeric membrane sensor based on a new four dentate neutral ion carrier.

    PubMed

    Zamani, Hassan Ali; Zanganeh-Asadabadi, Abbas; Rohani, Mitra; Zabihi, Mohammad Saleh; Fadaee, Javad; Ganjali, Mohammad Reza; Faridbod, Farnoush; Meghdadi, Soraia

    2013-03-01

    In this research, we report a new Ho(3+)-PVC membrane electrode based on N-(4,5-dimethyl-2-(picolinamido)phenyl)picolinamide (H(2)Me(2)bpb) as a suitable ion carrier. Poly vinylchloride (PVC)-based membrane composed of H(2)Me(2)bpb with oleic acid (OA) as anionic additives, and o-nitrophenyloctyl ether (NPOE) as plasticized solvent mediator. The sensor exhibits a Nernstian slope of 20.1 ± 0.2 mV decade(-1) over the concentration range of 1.0 × 10(-6) to 1.0 × 1(-2) mol L(-1), and a detection limit of 5.0 × 10(-7) mol L(-1) of Ho(3+) ions. The potentiometric response of the sensor is independent of the solution pH in the range of 3.5-9.4. It has a very short response time, in the whole concentration range (<10s), and can be used for at least eight weeks. The proposed electrode shows a good selectivity towards Ho(3+) ions over a wide variety of cations, including alkali, alkaline earth, transition and heavy metal ions. To assess its analytical applicability the proposed Ho(3+) sensor was successfully applied as an indicator electrode in the titration of Ho(3+) ion solutions in certified reference materials, alloy samples and for the determination of the fluoride ion in two mouthwash preparations. PMID:25427515

  20. 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…

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

    PubMed

    Bezáková, Zelmíra; Stankovi?ová, 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). PMID:24393115

  2. 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, ?-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 ?-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 of certain proteins from the HC. This approach thus has an immediate analytical value as well as potential applications in HC engineering. PMID:25350777

  3. 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 ?L desalinated sample plug is passed to a potentiometric flow cell of 13 ?L 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

  4. Peptide-lanthanide cation equilibria in aqueous phase. I. Bound shifts for L-carnosine-praseodymium complexes

    NASA Astrophysics Data System (ADS)

    Mossoyan, J.; Asso, M.; Benlian, D.

    L-Carnosine complexes of Pr 3+ were characterized in aqueous solution by 1H NMR and potentiometric titration. A rigorous treatment of chemical shifts and pH variation data with lanthanide concentration is presented. Two different forms of the peptide ligand, forming simultaneously two complexes, were taken into account. At low pH values the cation is only coordinated at the carboxylate site of the ligand in a weak complex ( β2 = 6) whereas in neutral solution a stronger complex ( β1 = 37) is present as a consequence of the deprotonation of the imidazole ring. The computation of induced bound shifts † 2 and Δ1 for resonating nuclei of the peptide in both forms yields consistent figures. These provide the experimental basis for a conformational model which is usually not obtainable for labile complexes with low stability constants.

  5. 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. PMID:19682817

  6. 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.

  7. APAP and Alternative Titration Methods

    PubMed Central

    Ahmed, Omer; Parthasarathy, Sairam

    2010-01-01

    Purpose of review Positive airway pressure therapy (PAP) is commonly prescribed treatment for obstructive sleep apnea (OSA). Traditionally, the determination of the optimal pressure for treatment of sleep-disordered breathing was made by manual titration of the device by a sleep technician in attendance during polysomnography. However, the advent of alternative methods for determination of optimal PAP – such as auto-titrating PAP (APAP) – has seen tremendous growth over the past decade. The purpose of this review is to improve our understanding of the currently available alternative methods for titration of PAP in patients with sleep-disordered breathing (SDB) with special emphasis on obstructive sleep apnea. Recent Findings Recent prospective-randomized studies of alternative methods of titration suggest that pressure determinations made by such devices are comparable to traditional manual titrations made in the sleep laboratory. Obstacles to the adoption of such alternative modes of titration into day-to-day practice may be attributable to issues surrounding appropriate patient selection, differences between devices, re-imbursement policies of third party payors, consensus amongst sleep experts, and individual physicians’ practice patterns and volumes. While newer generations and types of auto-titrating PAP devices are entering the sleep field constantly, providers’ knowledge and time availability remain limiting factors. Summary There is tremendous growth in the technology and scientific evidence in support of alternative modes of PAP titration for sleep-disordered breathing, but barriers to implementation remain. PMID:20806054

  8. Standard Solutions and Titratable Acidity

    NASA Astrophysics Data System (ADS)

    Nielsen, S. Suzanne

    Many types of chemical analyses are made using a method in which a constituent is titrated with a solution of known strength to an indicator endpoint. Such a solution is referred to as a standard solution. From the volume and concentration of standard solution used in the titration, and the sample size, the concentration of the constituent in the sample can be calculated.

  9. 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. PMID:26201018

  10. 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

  11. 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. PMID:25687018

  12. 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)

  13. Coacervation of cationic gemini surfactant with N-benzoylglutamic acid in aqueous solution.

    PubMed

    Wang, Meina; Fan, Yaxun; Han, Yuchun; Nie, Zongxiu; Wang, Yilin

    2013-12-01

    Coacervation of cationic gemini surfactant hexamethylene-1,6-bis(dodecyldimethylammonium bromide) (12-6-12) with pH-sensitive N-benzoylglutamic acid (H2Bzglu) has been investigated by potentiometric pH-titration, turbidity titration, dynamic light scattering (DLS), isothermal titration calorimetry (ITC), TEM, (1)H NMR, and light microscopy. Phase boundaries of the 12-6-12/H2Bzglu mixture were obtained over the pH range from 2 to 9 and in the H2Bzglu concentration range from 30.0 to 50.0 mM at pH 4.5. When the H2Bzglu concentration is beyond 30.0 mM, the 12-6-12/H2Bzglu mixed solution undergoes the phase transitions from soluble aggregate, to precipitate, coacervate, and soluble aggregate again as pH increases. The results indicate that coacervation occurs at extremely low 12-6-12 concentration and lasts over a wide surfactant range, and can be enhanced or suppressed by changing pH, 12-6-12/H2Bzglu molar ratio and H2Bzglu concentration. The coacervates present a disorderly connected lay structure. Coacervation only takes place at pH 4-5, where the aggregates are nearly charge neutralized, and a minimum H2Bzglu concentration of 30.0 mM is required for coacervation. In this pH range, H2Bzglu mainly exist as HBzglu(-). The investigations on intermolecular interactions indicate that the aggregation of 12-6-12 is greatly promoted by the strong electrostatic and hydrophobic interactions with the HBzglu(-) molecules, and the interaction also promotes the formation of dimers, trimers, and tetramers of HBzglu(-) through hydrogen bonds. The double chains of 12-6-12 and the HBzglu(-) oligomers can play the bridging roles connecting aggregates. These factors endow the mixed system with a very high efficiency in generating coacervation. PMID:24205784

  14. Potentiometric assessment of iron release during ferritin reduction by exogenous agents.

    PubMed

    Vladimirova, Lilia S; Kochev, Valery K

    2010-09-01

    This work studied the possibilities for quantitative determination of iron mobilization in connection with ferritin reduction by ascorbic acid (vitamin C) and sodium dithionite in vitro. The iron storage protein was incubated with an excess of reductant in aerobic conditions in the absence of complexing agents in the medium. The release of Fe(2+) was let to go to completion, and the overall content of Fe(2+) in the solution was evaluated with the aid of potentiometric titration using Ce(4+) as an oxidizing titrant. Results suggest a moderate iron efflux under the influence of the chosen reducing agents. Although such a reduction of the protein mineral core by dihydroxyfumarate contributes greatly to the iron mobilization, ferritin behavior with vitamin C and dithionite seems to be different. Although redox properties of dihydroxyfumarate are determined by hydroxyl groups similar to those of ascorbic acid, the two compounds differ significantly in structure, and this could be the basis for an explanation of the specificities in their interaction with ferritin. As revealed by the study, potentiometric titration promises to be a reliable tool for evaluation of the amount of Fe(2+) present in the solution as a result of the reduction of the ferritin's mineral core. PMID:20434425

  15. 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…

  16. High-sensitivity titration microcalorimeter

    NASA Astrophysics Data System (ADS)

    Velikov, A. A.; Grigoryev, S. V.; Chuikin, A. V.

    2015-02-01

    A differential titration microcalorimeter for studying intermolecular interactions in solutions has been designed. To increase the speed of the instrument, the dynamic correction method has been used. It has been shown that electrical calibration of the microcalorimeter is consistent with its chemical calibration. The use of the instrument for measuring the integral heats of dilution of 1-propanol has been demonstrated.

  17. 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…

  18. 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.

  19. Spectroscopic and potentiometric studies on derivatized natural humic acid.

    PubMed

    Andjelkovic, Tatjana; Perovic, Jelica; Purenovic, Milovan; Blagojevic, Srdjan; Nikolic, Ruzica; Andjelkovic, Darko; Bojic, Aleksandar

    2006-12-01

    Isolated soil humic acid (HA) and commercial Aldrich HA were derivatized by esterification with methanol-thionyl and acetylation with acetic anhidride, in order to obtain derivatives with selectively blocked carboxyl and phenol groups, respectively. Results obtained by FT-IR spectroscopy and potentiometry show that the methanol-thionyl procedure is a selective, specific and efficient route for blocking carboxyl groups. The good correlation between results obtained by direct potentiometry after HA esterification and by classical calcium-acetate and baryta exchange methods suggests that esterification followed by direct acid-base potentiometric titration can be used as a method for the estimation of carboxyl and phenol group contents. Phenol groups can not be specifically identified by the acetylation method, due to the low selectivity of the acetylation method. The average values of apparent and intrinsic pK of underivatized and derivatized HAs confirm decrease in ionizable groups content due to derivatization and their values are related to the different chemical structures of the acids. PMID:17159314

  20. Cobaltihexamine as an index cation for measuring the cation exchange capacity of humic acids

    NASA Astrophysics Data System (ADS)

    Maes, André; van Elewijck, Francis; Vancluysen, Jacqueline; Tits, Jan; Cremers, Adrien

    Cobaltihexamine (CoHM) is proposed as an index cation for measuring the cation exchange capacities (CEC) of "intact" and dissolved soil humic substances. Samples containing 2 to 5 mg humic substances were sufficient for each CoHM-CEC measurement. CoHM cation exchange capacity versus pH curves were better resolved than acid base titration curves in 0.1 M NaClO4 and were slightly displaced towards lower pH values. Three adsorption maxima were obtained in the pH range 3 to 10, and these corresponded to functional group entities observed in pH/ml curves from acid-base titration.

  1. Endosomal escape and siRNA delivery with cationic shell crosslinked knedel-like nanoparticles with tunable buffering capacities

    PubMed Central

    Shrestha, Ritu; Elsabahy, Mahmoud; Florez-Malaver, Stephanie; Samarajeewa, Sandani; Wooley, Karen L.

    2012-01-01

    Cationic shell crosslinked knedel-like nanoparticles (cSCKs) have emerged as a highly efficient transfection agent for nucleic acids delivery. In this study, a new class of cSCKs with tunable buffering capacities has been developed by altering the amounts of histamines and primary amines incorporated into their crosslinked shell regions. The effect of histamine content of these nanoparticles with a hydrodynamic diameter of ca. 20 nm, on the siRNA-binding affinity, cytotoxicity, immunogenicity, and transfection efficiency was investigated. The modification of cSCKs with histamine was found to reduce the siRNA-binding affinity and cellular binding. On the other hand, it significantly reduced the toxicity and immunogenicity of the nanoparticles with subsequent increase in the transfection efficiency. In addition, escape from endosomes was facilitated by having two species of low and high pKas (i.e. histamine and primary amine groups, respectively), as demonstrated by the potentiometric titration experiments and the effect of bafilomycin A1, an inhibitor of the endosomal acidification, on the transfection efficiency of cSCKs. Histamine modification of 15 mol% was a threshold, above which cSCKs with higher histamine content completely lost the ability to bind siRNA and to transfect cells. This study highlights the potential of histamine incorporation to augment the gene silencing activity of cationic nanoparticles, reduce their toxicity, and increase their biocompatibility, which is of particular importance in the design of nucleic acids delivery vectors. PMID:22901966

  2. Potentiometric sensors for trace-level analysis

    PubMed Central

    Bakker, Eric; Pretsch, Ernö

    2005-01-01

    This review summarizes recent progress in the development and application of potentiometric sensors with limits of detection (LODs) in the range 10?8–10?11 M. These LODs relate to total sample concentrations and are defined according to a definition unique to potentiometric sensors. LODs calculated according to traditional protocols (three times the standard deviation of the noise) yield values that are two orders of magnitude lower. We are targeting this article at analytical chemists who are non-specialists in the development of such sensors so that this technology may be adopted by a growing number of research groups to solve real-world analytical problems. We discuss the unique response features of potentiometric sensors and compare them to other analytical techniques, emphasizing that the choice of the method must depend on the problem of interest. We discuss recent directions in sensor design and development and present a list of 23 sensors with low LODs, with references. We give recent examples where potentiometric sensors have been used to solve trace-level analytical problems, including the speciation of lead and copper ions in drinking water, the measurement of free copper in sea water, and the uptake of cadmium ions by plant roots as a function of their speciation. PMID:16642205

  3. 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…

  4. 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…

  5. 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)

  6. Solid titration of octacalcium phosphate.

    PubMed

    Pan, H-B; Darvell, B W

    2009-01-01

    Octacalcium phosphate (OCP) is of considerable importance as a precursor in the formation of dental enamel and an intermediate phase in the precipitation of hydroxyapatite (HAp) in bone. However, agreement is poor on the solubility product (pK(sp)), possibly due to the formation of the more stable phase HAp. The system was investigated using solid titration, which has shown reliability in work on HAp and related fluoride minerals, with OCP in 100 mM KCl at 37.0 +/- 0.1 degrees C. The constitution of the end point precipitate was determined by X-ray diffraction and selected-electron area diffraction; the particle morphology and elements present were examined by high-resolution field emission scanning, transmission electron microscopy and energy-dispersive X-ray analysis. The titration curve for OCP was found for pH approximately 3.4-7.4. The precipitate was HAp at pH 3.6 and 4.5; no residual OCP or other phase was detected. Dicalcium phosphate dihydrate (DCPD) was then found to form at pH 3.6 on further addition of OCP titrant after equilibrium had been achieved, possibly due to easier nucleation at lower pH. However, markedly crystalline HAp was formed in equilibrium for OCP titration with HAp seeding, verifying HAp as the more stable phase. A solubility isotherm for OCP was not obtained as HAp appears to be less soluble in the pH range studied. This adds weight to the view that HAp may be the most stable phase of all calcium phosphates, with further doubt being cast on DCPD being the most stable phase below pH 4.2. However, metastable DCPD may form in an Ostwald succession, depending on supersaturation and nucleation conditions. PMID:19556792

  7. Fluorapatite surface composition in aqueous solution deduced from potentiometric, electrokinetic, and solubility measurements, and spectroscopic observations

    NASA Astrophysics Data System (ADS)

    Chaïrat, Claire; Oelkers, Eric H.; Schott, Jacques; Lartigue, Jean-Eric

    2007-12-01

    The surface chemistry of fluorapatite in aqueous solution was investigated using electrokinetic techniques, potentiometric titrations, solubility measurements, and attenuated total reflection infrared spectroscopy. All methods indicate the formation of Ca/F depleted, P enriched altered layer via exchange reactions between H + and Ca 2+, and OH - and F - at the fluorapatite (FAP) surface. Observations suggest that this leached layer has a di-calcium phosphate (CaHPO 4) composition and that it controls the apparent solubility of FAP. Electrokinetic measurements yield an iso-electric point value of 1 ± 0.5 consistent with a negatively charged FAP surface at pH > 1. In contrast, surface titrations give an apparent pH of point of zero charge of ˜7.7, consistent with a positively charged surface at pH < 7.7. These differences are shown to stem from proton consumption by both proton exchange and dissolution reactions at the FAP surface. After taking account for these effects, FAP surface charge is shown to be negative to at least pH 4 by surface titration analysis.

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

    PubMed

    Bra?i?, Matej; Hansson, Per; Pérez, Lourdes; Zemlji?, 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(?)-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. PMID:26474215

  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. 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.

  11. Measurement of pork freshness using potentiometric sensor.

    PubMed

    Kaneki, N; Miura, T; Shimada, K; Tanaka, H; Ito, S; Hotori, K; Akasaka, C; Ohkubo, S; Asano, Y

    2004-01-01

    This study evaluated pork freshness using potentiometric solid-state electrodes in order to detect chemical indices such as reduced compounds, organic compounds and sulfides, which are produced during the initial stage of putrefaction in meat. Pt, CuS and Ag(2)S electrodes selected as solid-state electrodes have, respectively, been used to detect the organic compounds (regarded as chemical indices of deterioration in meat freshness). The outputs of these electrodes have been analyzed by principal component analysis (PCA) and multiple regression analysis (MRA) in order to find the correlation with the results of viable bacterial counts. By using the potentiometric sensor, the pork freshness was evaluated and the PCA and MRA corresponded to the degree of bacterial increases more simply and rapidly than other methods such as viable bacterial counts or a biosensor. PMID:18969283

  12. Amperometric titration of Cd(II), Hg(II) and Zn(II) in molten alkali thiocyanates with electrolytically generated sulphide ions.

    PubMed

    Cescon, P; Pucciarelli, F; Fiorani, M

    1970-07-01

    The feasibility of the titration of some cations in molten sodium thiocyanate-potassium thiocyanate mixture with electrolytically generated sulphide ions has been tested at 443 K. Quantitative data are given for the titration of cadmium, mercury and zinc ions. PMID:18960785

  13. A disposable voltammetric cell for determining the titratable acidity in vinegar.

    PubMed

    Kotani, Akira; Miyaguchi, Yuji; Harada, Dai; Kusu, Fumiyo

    2003-11-01

    A disposable voltammetric cell using three pencil leads as working, reference, and counter electrodes was developed for determining the titratable acidity, i.e. the acid content in vinegar. The materials of the pencil leads were graphite-reinforcement carbons (GRCs). A voltammetric determination of acid was made by measuring the reduction prepeak current of 3,5-di-t-butyl-1,2-benzoquinone (DBBQ) due to the presence of acids in unbuffered solution. The potential stability of the pseudo-reference electrode of GRC was examined. The prepeak current was found to be proportional to the acetic acid concentration from 0.05 to 2.7 mM with a correlation coefficient of 0.999. The cell-to-cell reproducibility for 1 mM acetic acid was evaluated with ten individual disposable cells. The RSD of the prepeak current and the SD of the prepeak potential were 2.56% and 0.008, respectively. The titratable acidity in five vinegar samples was determined by voltammetry using disposable cells and compared with that of the titratable acidity determined by the conventional potentiometric titration method. We then observed the results by both methods, and found a correlation coefficient of 0.972. As such, the voltammetry using disposable-cell required only one thousandth the volume of a vinegar sample for the titration method. The disposable cell was superior to the conventional electrochemical cell, in terms of facility, environment-friendly, and economy, and thus a sensor using the present cell would be useful for routine work in the quality control of vinegar. PMID:14640441

  14. Electrooxidation of iodide in the presence of 4-hydroxycoumarin: application to a simple coulometric titration of 4-hydroxycoumarin.

    PubMed

    Nematollahi, Davood; Hamzehloei, Ali; Hesari, Mehdi; Rahimi, Javad

    2003-06-01

    The electrochemical oxidation of iodide ion in the presence of 4-hydroxycoumarin (1) was studied using cyclic voltammetry and controlled-potential coulometry. The result indicates that the resulting iodine takes part in a halogenation reaction and reacts with 4-hydroxycoumarin (1). According to the obtained results, a new and simple coulometric titration method with potentiometric end-point detection for the determination of 4-hydroxycoumarin (1) is presented. In the presented method, 2-200 micromol of 4-hydroxycoumarin (1) was successfully determined. PMID:12834239

  15. 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…

  16. 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…

  17. Dissolved oxygen: method comparison with potentiometric stripping analysis

    SciTech Connect

    Fayyad, M.; Tutunji, M.; Ramakrishna, R.S.; Taha, Z.

    1987-04-01

    Three methods for determination of dissolved oxygen in samples of natural water are compared; potentiometric stripping analysis, PSA compares well with oxygen selective electrodes. Although potentiometric stripping analysis and oxygen selective electrode methods are found to be simple, rapid and of higher reproducibility than the usual Winkler procedure, the use of oxygen selective electrodes has many disadvantages.

  18. Development of a novel MWCNTs-triazene-modified carbon paste electrode for potentiometric assessment of Hg(II) in the aquatic environments.

    PubMed

    Mashhadizadeh, Mohammad Hossein; Ramezani, Soleyman; Rofouei, Mohammad Kazem

    2015-02-01

    In this approach, a new chemically modified carbon paste electrode was assembled for potentiometric assay of mercury(II) ion in the aqueous environments. Hereby, MWCNTs were used in the carbon paste composition to meliorate the electrical conductivity and sensitivity of the carbon paste owing to its exceptional physicochemical characteristics. Likewise, participation of the BEPT as a super-selective ionophore in the carbon paste composition boosted significantly the selectivity of the modified electrode towards Hg(II) ions over a wide concentration range of 4.0 × 10(-9)-2.2 × 10(-3) mol L(-1) with a lower detection limit of 3.1 × 10(-9) mol L(-1). Besides, Nernstian slope of the proposed sensor was 28.9(± 0.4)mV/decade over a pH range of 3.0-5.2 with potentiometric short response time of 10s. In the interim, by storing in the dark and cool dry place during non-usage period, the electrode can be used for at least 30 days without any momentous divergence of the potentiometric response. Eventually, to judge about its practical efficiency, the arranged sensor was utilized successfully as an indicator electrode for potentiometric titration of mercury(II) with standard solution of EDTA. As well, the quantitative analysis of mercury(II) ions in some aqueous samples with sensible accuracy and precision was satisfactorily performed. PMID:25492198

  19. 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.

  20. Kinetics, thermodynamics and surface heterogeneity assessment of uranium(VI) adsorption onto cation exchange resin derived from a lignocellulosic residue

    NASA Astrophysics Data System (ADS)

    Anirudhan, T. S.; Radhakrishnan, P. G.

    2009-02-01

    A new cation exchange resin (PGTFS-COOH) having a carboxylate functional group at the chain end was prepared by grafting poly(hydroxyethylmethacrylate) onto tamarind fruit shell, TFS (a lignocellulosic residue) using potassium peroxydisulphate-sodium thiosulphate redox initiator, and in the presence of N,N'-methylenebisacrylamide (MBA) as a crosslinking agent, followed by functionalisation. The adsorbent was characterized with the help of FTIR, XRD, scanning electron micrographs (SEM), and potentiometric titrations. The kinetic and isotherm data, obtained at optimum pH value 6.0 at different temperatures could be fitted with pseudo-second-order equation and Sips isotherm model, respectively. An increase in temperature induces positive effect on the adsorption process. The calculated activation energy of adsorption ( Ea, 18.67 kJ/mol) indicates that U(VI) adsorption was largely due to diffusion-controlled process. The values of adsorption enthalpy, Gibbs free energy, and entropy were calculated using thermodynamic function relationships. The decrease in adsorption enthalpy with increasing U(VI) uploading on the adsorbent, reflects the surface energetic heterogeneity of the adsorbent. The isosteric heat of adsorption was quantitatively correlated with the fractional loading for the U(VI) ions adsorption onto PGTFS-COOH. The results showed that the PGTFS-COOH possessed heterogeneous surface with sorption sites having different activities.

  1. Potentiometric sensing array for monitoring aquatic systems.

    PubMed

    Pankratova, Nadezda; Crespo, Gastón A; Afshar, Majid Ghahraman; Crespi, Miquel Coll; Jeanneret, Stéphane; Cherubini, Thomas; Tercier-Waeber, Mary-Lou; Pomati, Francesco; Bakker, Eric

    2015-05-01

    Since aquatic environments are highly heterogeneous and dynamic, there is the need in aquatic ecosystem monitoring to replace traditional approaches based on periodical sampling followed by laboratory analysis with new automated techniques that allow one to obtain monitoring data with high spatial and temporal resolution. We report here on a potentiometric sensing array based on polymeric membrane materials for the continuous monitoring of nutrients and chemical species relevant for the carbon cycle in freshwater ecosystems. The proposed setup operates autonomously, with measurement, calibration, fluidic control and acquisition triggers all integrated into a self-contained instrument. Experimental validation was performed on an automated monitoring platform on lake Greifensee (Switzerland) using potentiometric sensors selective for hydrogen ions, carbonate, calcium, nitrate and ammonium. Results from the field tests were compared with those obtained by traditional laboratory analysis. A linear correlation between calcium and nitrate activities measured with ISEs and relevant concentrations measured in the laboratory was found, with the slopes corresponding to apparent single ion activity coefficients ?(*)(Ca(2+)) = 0.55(SD = 0.1mM) and ?(*)(NO(3)(-)) = 0.75(SD = 4.7?m). Good correlation between pH values measured with ISE and CTD probes (SD = 0.2 pH) suggests adequate reliability of the methodology. PMID:25850652

  2. Competitive sorption of protons and metal cations onto kaolinite: experiments and modeling.

    PubMed

    Heidmann, Ilona; Christl, Iso; Leu, Christian; Kretzschmar, Ruben

    2005-02-15

    Competitive sorption of protons, Cu, and Pb onto kaolinite (KGa-2) was investigated over wide concentration ranges and quantitatively described using three different models based on surface complexation and cation exchange reactions. In all models, two types of binding sites were assumed for kaolinite: edge sites (SOH0.5-) with pH-dependent charge and face sites (X-) with permanent negative charge. In a first step, proton sorption was measured by potentiometric acid-base titrations of kaolinite dispersed in 0.01, 0.03, and 0.1 M NaNO3 electrolyte solutions. The acid-base titration data were fitted to obtain site densities and protonation constants for the edge and face sites, respectively. In a second step, the sorption of Cu and Pb onto kaolinite was investigated at fixed pH values by metal titration using ion-selective electrodes for Cu2+ and Pb2+, respectively, and by independent batch sorption experiments. Our metal sorption data cover a range of pH 4-8 for Cu and pH 4-6 for Pb, three different ionic strengths (0.01, 0.03, and 0.1 M NaNO3), and up to eight orders of magnitude in free metal ion activity. An additional experiment was conducted to explore the sorption competition between Cu and Pb. In all three models, sorption of protons and metal cations to the edge sites of kaolinite was described with a 1-pK basic Stern (BS) approach. The three models differed only in the description of cation sorption to the face sites. In the first model (BS/GT), we used a Gaines-Thomas (GT) cation exchange equation for the face sites. This model yielded a satisfactory description of Cu sorption, but failed to describe Pb sorption isotherms at pH 4, 5, and 6. In the second model (BS/BS), we replaced the Gaines-Thomas equation by a basic Stern surface complexation formulation, thereby introducing electrostatic terms for sorption to face sites and allowing for free binding sites X-. This did not improve the fits of Cu or Pb sorption to kaolinite, however. In the third model (BS/BS(ext)), we extended the BS/BS-model by introducing additional monodentate sorption complexes at face sites (XCu+ and XPbNO3). This model described both Cu and Pb sorption very well over the entire range in metal concentrations and pH. It also correctly predicted the competitive effect of Pb on sorption of Cu. Model calculations with all three models suggested that Cu and Pb were sorbed mainly to face sites at low pH, while sorption to edge sites dominated at high pH values. PMID:15589531

  3. 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)

  4. DNA Nanostructure-Based Magnetic Beads for Potentiometric Aptasensing.

    PubMed

    Ding, Jiawang; Gu, Yue; Li, Fei; Zhang, Hongxia; Qin, Wei

    2015-07-01

    In this work, a simple, general, and sensitive potentiometric platform is presented, which allows potentiometric sensing to be applied to any class of molecule irrespective of the analyte charge. DNA nanostructures are self-assembled on magnetic beads via the incorporation of an aptamer into a hybridization chain reaction. The aptamer-target binding event leads to the disassembly of the DNA nanostructures, which results in a dramatic change in the surface charge of the magnetic beads. Such a surface charge change can be sensitively detected by a polycation-sensitive membrane electrode using protamine as an indicator. With an endocrine disruptor bisphenol A as a model, the proposed potentiometric method shows a wide linear range from 0.1 to 100 nM with a low detection limit of 80 pM (3?). The proposed sensing strategy will lay a foundation for the development of potentiometric sensors for highly sensitive and selective detection of various targets. PMID:26044085

  5. New potentiometric transducer based on a Mn(II) [2-formylquinoline thiosemicarbazone] complex for static and hydrodynamic assessment of azides.

    PubMed

    Kamel, Ayman H

    2015-11-01

    A new potentiometric transducer for selective recognition of azide is characterized and developed. The PVC plasticized based sensor incorporates Mn(II) [2-formylquinoline thiosemicarbazone] complex in the presence of tri dodecyl methyl ammonium chloride (TDMAC) as a lipophilic cationic additive. The sensor displayed a near-Nernstian response for azide over 1.0×10(-2)-1.0×10(-5) mol L(-1), with an anionic slope of -55.8±0.6 mV decade(-1) and lower limit of detection 0.34 µg mL(-1). The sensor was pH independent in the range 5.5-9 and presented good selectivity features towards several inorganic anions, and it is easily used in a flow injection system and compared with a tubular detector. The intrinsic characteristics of the detector in a low dispersion manifold were determined and compared with data obtained under a hydrodynamic mode of operation. This simple and inexpensive automation, with a good potentiometric detector, enabled the analysis of ~33 samples h(-1) without requiring pre-treatment procedures. The proposed method is also applied to the analysis of trace levels of azide in primer mixtures. Significantly improved accuracy, precision, response time, stability and selectivity were offered by these simple and cost-effective potentiometric sensor compared with other standard techniques. The method has the requisite accuracy, sensitivity and precision to determine azide ions. PMID:26452931

  6. 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

  7. A selective potentiometric copper (II) ion sensor based on the functionalized ZnO nanorods.

    PubMed

    Khun, K; Ibupoto, Z H; Liu, X; Nur, O; Willander, M; Danielsson, B

    2014-09-01

    In this work, ZnO nanorods were hydrothermally grown on the gold-coated glass substrate and characterized by field emission scanning electron microscopy (FESEM) and X-ray diffraction (XRD) techniques. The ZnO nanorods were functionalized by two different approaches and performance of the sensor electrode was monitored. Fourier transform infrared spectroscopy (FTIR) was carried out for the confirmation of interaction between the ionophore molecules and ZnO nanorods. In addition to this, the surface of the electrode was characterized by X-ray photoelectron spectroscopy (XPS) showing the chemical and electronic state of the ionophore and ZnO nanorod components. The ionophore solution was prepared in the stabilizer, poly vinyl chloride (PVC) and additives, and then functionalized on the ZnO nanorods that have shown the Nernstian response with the slope of 31 mV/decade. However, the Cu2+ ion sensor was fabricated only by immobilizing the selective copper ion ionophore membrane without the use of PVC, plasticizers, additives and stabilizers and the sensor electrode showed a linear potentiometric response with a slope of 56.4 mV/decade within a large dynamic concentration range (from 1.0 x 10(-6) to 1.0 x 10(-1) M) of copper (II) nitrate solutions. The sensor showed excellent repeatability and reproducibility with response time of less than 10 s. The negligible response to potentially interfering metal ions such as calcium (Ca2+), magnesium (Mg2+), potassium (K+), iron (Fe3+), zinc (Zn2+), and sodium (Na+) allows this sensor to be used in biological studies. It may also be used as an indicator electrode in the potentiometric titration. PMID:25924323

  8. 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. PMID:22841067

  9. 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

  10. 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+.

  11. 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. PMID:21482256

  12. The potentiometric determination of stability constants for zinc acetate complexes in aqueous solutions to 295°C

    NASA Astrophysics Data System (ADS)

    Glordano, Thomas H.; Drummond, S. E.

    1991-09-01

    A potentiometric method was used to determine the formation quotients of zinc acetate complexes in aqueous solutions from 50 to 295°C at ionic strengths of 0.03,0.3, and 1.0 m. The potentiometric titrations were carried out in an externally heated, Teflon-lined concentration cell fitted with hydrogen electrodes. Formal sodium acetate concentrations of the experimental solutions ranged from 0.001 to 0. 1 m with acetic acid to sodium acetate ratios ranging from 30 to 300. Sodium trifluoromethanesulfonate (F3CSO3Na) was used as a supporting electrolyte. Stoichiometries and formation quotients for the complexes ZnCH3COO+, Zn(CH3COO)2, and Zn(CH3COO)-3 were derived from the titration data by regression analysis. Stability constants at infinite dilution (Kn) and other relevant thermodynamic quantities were calculated for these three complexes. Logarithms for the formation constants of the general reaction Zn2+ + nCH3COO- = Zn(CH3COO)n2-n are n = 1-(1.9 ± 0.2, 50°C), (2.3 ± 0.1, 100°C), (2.8 ± 0.1, 150°C), (3.5 ± 0.1, 200°C), (4.3 ± 0.2, 250°C), (5.3 ± 0.3, 300°C); n = 2-(3.4 ± 0.1, 50°C), (4.0 ± 0.1, 100°C), (4.83 ± 0.09, 150°C), (5.9 ± 0.1, 200°C), (7.1 ± 0.1, 250°C), (8.7 ± 0.2, 300°C); n = 3-(4.1 ± 0.3, 50°C), (4.7 ± 0.3, 100°C), (5.5 ± 0.3, 150°C), (6.6 ± 0.3, 200°C), (7.9 ± 0.3, 250°C), (9.4 ± 0.3, 300°C). Calculations of zinc speciation in acetate-chloride solutions show that zinc acetate complexes should have an importance similar to zinc chloride complexes in high acetate waters where chloride to acetate molal ratios are less than about 10.

  13. Analysis of mathematical modelling on potentiometric biosensors.

    PubMed

    Mehala, N; Rajendran, L

    2014-01-01

    A mathematical model of potentiometric enzyme electrodes for a nonsteady condition has been developed. The model is based on the system of two coupled nonlinear time-dependent reaction diffusion equations for Michaelis-Menten formalism that describes the concentrations of substrate and product within the enzymatic layer. Analytical expressions for the concentration of substrate and product and the corresponding flux response have been derived for all values of parameters using the new homotopy perturbation method. Furthermore, the complex inversion formula is employed in this work to solve the boundary value problem. The analytical solutions obtained allow a full description of the response curves for only two kinetic parameters (unsaturation/saturation parameter and reaction/diffusion parameter). Theoretical descriptions are given for the two limiting cases (zero and first order kinetics) and relatively simple approaches for general cases are presented. All the analytical results are compared with simulation results using Scilab/Matlab program. The numerical results agree with the appropriate theories. PMID:25969765

  14. Structural characterization of hexadecyltrimethylammonium-smectite composites and their potentiometric electrode applications

    NASA Astrophysics Data System (ADS)

    Cubuk, Osman; Caglar, Bulent; Topcu, Cihan; Coldur, Fatih; Sarp, Gokhan; Tabak, Ahmet; Sahin, Erdal

    2015-05-01

    Organosmectites were prepared by the intercalation of hexadecyltrimethylammonium cations at various ratios into interlayer of Unye smectite. Structural, thermal, morphological and textural properties of the synthesized organosmectites were characterized. Afterwards, a novel potentiometric PVC-membrane thiocyanate selective electrode was prepared based on the obtained hexadecyltrimethylammonium modified smectites as electroactive material. The basal spacing values of organosmectites were observed in the range of 15.61 and 35.50 Å. Powder X-ray diffraction data show that the surfactant cations penetrated into the smectite layers with different molecular arrangements. Modification of smectite with hexadecyltrimethylammonium led to appreciable decreases in the intensities of the FTIR bands at 3402 and 1635 cm-1 and the new characteristic vibrational bands at 2927, 2850, 1472 and 722 cm-1 originating from the surfactant molecules appeared. The thermal analysis data showed that the decomposition of surfactant species occurred in the temperature range of 170-720 °C and the amount of dehydrated water gradually decreased with the increase in surfactant amount. The intercalation of surfactant species within the gallery spacing led gradually to smaller surface areas. In addition, the electrophoretic mobility values indicate that excess surfactant loadings also generate positive charges on the organosmectite surfaces. The most convenient membrane composition resulting in the best potentiometric performance was investigated. The optimum membrane composition was determined to have 20.0% (w/w) 2.5CEC.HDTMA-smectite, 26.0% (w/w) PVC, 54.0% (w/w) DBP The fabricated electrode exhibited a linear response over the thiocyanate concentration range of 1.0 × 10-4-1.0 × 10-1 M (R2 = 0.9996) with a slope of -48.6 mV/decade. The detection limit, response time and pH working range were determined as 4.3 × 10-5 M, ∼10 s and 4-8, respectively. The proposed electrode exhibited selective potentiometric response to thiocyanate comparable to most of the common anions.

  15. 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…

  16. Virtual Titrator: A Student-Oriented Instrument.

    ERIC Educational Resources Information Center

    Ritter, David; Johnson, Michael

    1997-01-01

    Describes a titrator system, constructed from a computer-interfaced pH-meter, that was designed to increase student involvement in the process. Combines automatic data collection with real-time graphical display and interactive controls to focus attention on the process rather than on bits of data. Improves understanding of concepts and…

  17. 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)

  18. 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…

  19. 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,…

  20. 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,…

  1. 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 equivalence point. Although applied to acid-base titrations in this paper, the approach should be generally applicable to other types of titrations. PMID:16536416

  2. A potentiometric tattoo sensor for monitoring ammonium in sweat.

    PubMed

    Guinovart, Tomàs; Bandodkar, Amay J; Windmiller, Joshua R; Andrade, Francisco J; Wang, Joseph

    2013-11-21

    The development and analytical characterization of a novel ion-selective potentiometric cell in a temporary-transfer tattoo platform for monitoring ammonium levels in sweat is presented. The fabrication of this skin-worn sensor, which is based on a screen-printed design, incorporates all-solid-state potentiometric sensor technology for both the working and reference electrodes, in connection to ammonium-selective polymeric membrane based on the nonactin ionophore. The resulting tattooed potentiometric sensor exhibits a working range between 10(-4) M to 0.1 M, well within the physiological levels of ammonium in sweat. Testing under stringent mechanical stress expected on the epidermis shows that the analytical performance is not affected by factors such as stretching or bending. Since the levels of ammonium are related to the breakdown of proteins, the new wearable potentiometric tattoo sensor offers considerable promise for monitoring sport performance or detecting metabolic disorders in healthcare. Such combination of the epidermal integration, screen-printed technology and potentiometric sensing represents an attractive path towards non-invasive monitoring of a variety of electrolytes in human perspiration. PMID:24098883

  3. Potentiometric surface of the middle Potomac Aquifer in Virginia 1993

    USGS Publications Warehouse

    Hammond, E.C.; McFarland, E.R.; Focazio, M.J.

    1994-01-01

    Ground-water level measurements from 50 wells in the middle Potomac aquifer in the Coastal Plain Physiographic Province of Virginia in 1993 were used to prepare a map of the potentiometric surface of the aquifer. The map shows the potentiometric surface of the middle Potomac aquifer sharply declining eastward from nearly 100 feet above sear level near the western boundary of the aquifer to 20 feet below sea level, and continues declining gradually toward the Chesapeake Bay and Atlantic Ocean. A cone of depression is apparent around well fields in Franklin, Virginia. The potentiometric surface also appears to be affected by pumping in the area of Henrico County and Hanover County, Virginia. The highest ground-water-level measurement was 89 feet above sea level in Chesterfield County near Richmond, and the lowest ground-water-level measurement was 179 feet below sea level in southeastern Isle of Wight County, Virginia.

  4. Potentiometric surface of the lower Potomac Aquifer in Virginia 1993

    USGS Publications Warehouse

    Hammond, E.C.; McFarland, E.R.; Focazio, M.J.

    1994-01-01

    Ground-water level measurements from 17 wells in the lower Potomac aquifer in the Coastal Plain Physiographic Province of Virginia in 1993 were used to prepare a map of the potentiometric surface of the aquifer. The map shows the potentiometric surface of the lower Potomac aquifer indicating a regional trend toward the Chesapeake Bay and Atlantic Ocean. The potentiometric-surface data indicate that there are two cones of depression, one around well fields in Henrico County and the other around large well fields in Isle of Wight County and Franklin, Virginia. The highest ground-water-level measurement was 47 feet above sea level in southeast Southampton County, and the lowest ground-water-level measurement was 161 feet below sea level in the southeast area of Isle of Wight County near Franklin, Virginia.

  5. 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. PMID:22868165

  6. S-perindopril assay using a potentiometric, enantioselective membrane electrode.

    PubMed

    Stefan, R I; Van Staden, J K; Aboul-Enein, H Y

    1999-01-01

    A potentiometric, enantioselective membrane electrode based on graphite paste (graphite powder and paraffin oil) has been constructed. The graphite paste is impregnated with a 10(-3) mol/L 2-hydroxy-3-trimethylammoniopropyl-beta-cyclodextrin (as chloride salt) solution. The potentiometric, enantioselective membrane electrode can be used reliably for enantiopurity tests of S-perindopril using a chronopotentiometric (zero current) technique, in the 10(-5)-10(-2) mol/L concentration range (detection limit 5 x 10(-6) mol/L), with an average recovery of 99.58% (RSD = 0.33%). The enantioselectivity was determined over R-perindopril and D-proline. The response characteristics of the enantioselective, potentiometric membrane electrode were also determined for R-perindopril. It was shown that L-proline is the main interfering compound. The surface of the electrode can be regenerated simply by polishing, obtaining a fresh surface ready to be used in a new assay. PMID:10467314

  7. 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.

  8. 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)

  9. Potentiometric determination of chlorides with an "Air-Gap" cyanide sensor.

    PubMed

    Baranowski, R; Kubik, T

    1993-09-01

    A new electroanalytical method for determining chloride ions with an Air-Gap cyanide sensor system is described. The method is based on the reaction of chloride with mercury(II) cyanide in dilute sulphuric acid. This reaction leads to hydrogen cyanide which can be determined with an Air-Gap cyanide sensor. Optimum concentrations of mercury(II) cyanide and sulphuric acid were established and an analytical curve was prepared for 1 x 10(-1)-1 x 10(-5)M Cl(-). The slope of the calibration curve was equal to 62.8 mV/log C. The correlation coefficient (R) was equal to 0.9992. The method can determine chloride with good results in high saline solutions and in the presence of surfactants, which is in contrast to direct potentiometry with a chloride electrode. The method was applied for chloride determination in fuses used for initiating explosions. The chlorides were determined both in the raw materials used to prepare the fuse braids and in the other fuse components. Chloride was also determined in drinking water and river water. In dependence of source, chloride amount analyzed in drinking water was in the range 2.18-182.6 mg/l. and 25.8 mg/l. in river water. A comparative analysis was carried out. In the first case, chloride was determined by a turbidimetric method, whereas in the second one by potentiometric titration against a chloride-ISE. PMID:18965807

  10. Coulometric titration of urea with electrogenerated hypobromite.

    PubMed

    Kato, Jun; Koseki, Takuma; Aoki, Yukie; Yamada, Ayako; Tanaka, Tatsuhiko

    2013-01-01

    A definitive method is described for the indirect assay of several tens of milligrams of urea by coulometric titration. Urea was decomposed in concentrated sulfuric acid using a Kjeldahl flask. Subsequently, the formed ammonium ion was titrated with electrogenerated hypobromite ion in a sodium bromide-sodium tetraborate medium of pH 8.6, with amperometric end-point detection. Parameters affecting the pretreatment procedure were evaluated. The optimized conditions included the heating of 2 g of urea at around 300°C for 2 h with 10 cm(3) of sulfuric acid. Under the proposed conditions, the assay value with expanded uncertainty (k = 2), 99.870 ± 0.026%, agreed well with the certified value of NIST SRM 912a urea, 99.9 ± 0.1%. PMID:23842420

  11. Spectrophotometric titration of zirconium in siliceous materials.

    PubMed

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

    An accurate and selective complexometric titration procedure based upon a spectrophotometrically detected end-point has been developed for the determination of zirconium in glasses, glass-ceramics and refractories. A p-bromomandelic acid separation step for zirconium imparts excellent selectivity to the procedure. The method is particularly important for the 1-5% concentration range where a simple, accurate and selective method for the determination of zirconium has been lacking. PMID:18962344

  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. PMID:19071280

  14. 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…

  15. 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.

  16. 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…

  17. 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. PMID:26002212

  18. A mechanistic description of Ni and Zn sorption on Na-montmorillonite Part I: Titration and sorption measurements

    NASA Astrophysics Data System (ADS)

    Baeyens, Bart; Bradbury, Michael H.

    1997-09-01

    In this paper experimental investigations into the acid/base titration characteristics of Na-montmorillonite and the sorption behaviour of Ni and Zn under a wide variety of conditions are presented. From these measurements the dominant sorption mechanisms could be deduced. In the following paper (Bradbury and Baeyens, 1997) the titration and sorption data are analysed to determine the parameters in cation exchange and surface complexation based models which together provide a quantitative description of the titration and sorption data. A conditioning procedure was applied to the SWy-1 Na-montmorillonite starting material in order to remove background metal impurities, soluble salts and sparingly soluble minerals which could influence titration and sorption measurements. The purified clay, in the homo-ionic Na form, was thoroughly physico-chemically characterised before carrying out batch titration measurements on suspensions in 0.1 and 0.5 M NaClO 4. The influence of background impurities, not removed by the conditioning, and cation exchange processes on the form of the titration curves is discussed. Titration data can be analysed to yield site capacities and protonation/deprotonation constants for the amphoteric surface hydroxyl groups (?SOH). The acid endpoint in the titration data was used to estimate an ?SOH site capacity of 0.08 mol kg -1. The sorption of Ni and Zn on conditioned Na-montmorillonite was studied at trace concentrations as a function of pH over a range from ˜ 3 to ˜ 10 to produce so-called "sorption edges". In the case of Ni, such measurements were carried out as a function of the NaClO 4 background electrolyte concentration. In addition, sorption isotherms were determined for both nuclides at several fixed pH values in 0.1 M NaClO 4. From the form of the "edges" it was deduced that two main sorption mechanisms were controlling the uptake of Ni and Zn onto the clay mineral; a pH-independent component, identified as cation exchange on the permanent charge sites, and a pH-dependent one, interpreted as surface complexation on the amphoteric surface hydroxyl groups. The non-linearity of the sorption isotherms indicated that at least two different ?SOH type sites were contributing to the overall sorption on Na-montmorillonite.

  19. Chicken (Gallus gallus) hemolytic complement: optimal conditions for its titration.

    PubMed

    Barta, O; Barta, V

    1975-01-01

    The effect of pH, ionic strength, cation concentration, ethylenediaminetetraacetic acid trisodium salt (Na3EDTA), time and temperature were studied to determine the optimal conditions for titrating the hemolytic complement (C) activity in sera of chicken (Gallus gallus). Swine erythrocytes (E) sensitized with rabbit antibodies were the most sensitive, while chicken serum had a smaller amount of "natural" antibody against them than against red blood cells from other five species tested. The highest titers of chicken C, when tested with swine sensitized E, were detected when isotonic NaCl-barbital buffer was used as diluent, having the ionic strength of 0.15, conductance of 11 millimhos/cm at 20 degrees C. However, maximal chicken C titers detected with sensitized rabbit E were obtained at ionic strength of 0.07 to 0.11 depending on pH. A final concentration of 1 X 10(-3) M of Mg2+ and 3 X 10(-4) M of Ca2+ and pH 8 were optimal in both cases. The temperature of 30 degrees C and time of 60 minutes were appropriate to reveal the maximal titers.. PMID:241720

  20. Liposome/Graphene Oxide Interaction Studied by Isothermal Titration Calorimetry.

    PubMed

    Huang, Po-Jung Jimmy; Wang, Feng; Liu, Juewen

    2016-03-15

    The interaction between graphene oxide (GO) and lipid bilayers is important for fundamental surface science and many applications. In this work, isothermal titration calorimetry (ITC), cryo-TEM, and fluorescence spectroscopy were used to study the adsorption of three types of liposomes. Heat release was observed when GO was mixed with zwitterionic DOPC liposomes, while heat absorption occurred with cationic DOTAP liposomes. For comparison, anionic DOPG liposomes released heat when mixed with DOTAP. DOPC was adsorbed as intact liposomes, but DOTAP ruptured and induced stacking and folding of GO sheets. This study suggests the release of more water molecules from the GO surface when mixed with DOTAP liposomes. This can be rationalized by the full rupture of the DOTAP liposomes interacting with the whole GO surface, including hydrophobic regions, while DOPC liposomes only interact with a small area on GO near the edge, which is likely to be more hydrophilic. This interesting biointerfacial observation has enhanced our fundamental understanding of lipid/GO interactions. PMID:26908113

  1. 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

  2. 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

  3. 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.

  4. Potentiometric sensors using cotton yarns, carbon nanotubes and polymeric membranes.

    PubMed

    Guinovart, Tomàs; Parrilla, Marc; Crespo, Gastón A; Rius, F Xavier; Andrade, Francisco J

    2013-09-21

    A simple and generalized approach to build electrochemical sensors for wearable devices is presented. Commercial cotton yarns are first turned into electrical conductors through a simple dyeing process using a carbon nanotube ink. These conductive yarns are then partially coated with a suitable polymeric membrane to build ion-selective electrodes. Potentiometric measurements using these yarn-potentiometric sensors are demonstrated. Examples of yarns that can sense pH, K(+) and NH4(+) are presented. In all cases, these sensing yarns show limits of detection and linear ranges that are similar to those obtained with lab-made solid-state ion-selective electrodes. Through the immobilization of these sensors in a band-aid, it is shown that this approach could be easily implemented in a wearable device. Factors affecting the performance of the sensors and future potential applications are discussed. PMID:23775189

  5. 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 data illustrates the complementarity of molecular and macro-scale descriptions of the clay reactivity.

  6. 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.

  7. 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.

  8. 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)

  9. 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.

  10. "Footprint" titrations yield valid thermodynamic isotherms.

    PubMed Central

    Brenowitz, M; Senear, D F; Shea, M A; Ackers, G K

    1986-01-01

    A central issue in gene regulation is the mechanism, and biological function, of the cooperative binding of regulatory protein ligands to specific sites on DNA. To elucidate the physical-chemical basis of these interactions we have developed a thermodynamically rigorous method for conducting DNase I "footprint" (protection) titration experiments. The intrinsic binding constants and also those for cooperative interactions between various sites can be resolved from the individual-site binding curves determined by this technique. Experimental studies of cI-repressor-operator binding have demonstrated that the method provides an accurate representation of the fractional saturation of a binding site. We present individual-site binding curves for a lambda operator with two competent sites that demonstrate the presence of cooperative interactions between the sites. These curves set a lower limit to the magnitude of the cooperative free energy without comparison to single-site mutant operators. Images PMID:3464963

  11. 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). PMID:26079704

  12. 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, ?H) 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. PMID:26794356

  13. Crown-Ether Derived Graphene Hybrid Composite for Membrane-Free Potentiometric Sensing of Alkali Metal Ions.

    PubMed

    Olsen, Gunnar; Ulstrup, Jens; Chi, Qijin

    2016-01-13

    We report the design and synthesis of newly functionalized graphene hybrid material that can be used for selective membrane-free potentiometric detection of alkali metal ions, represented by potassium ions. Reduced graphene oxide (RGO) functionalized covalently by 18-crown[6] ether with a dense surface coverage is achieved by the introduction of a flexible linking molecule. The resulting hybrid composite is highly stable and is capable of detecting potassium ions down to micromolar ranges with a selectivity over other cations (including Ca(2+), Li(+), Na(+), NH4(+)) at concentrations up to 25 mM. This material can be combined further with disposable chips, demonstrating its promise as an effective ion-selective sensing component for practical applications. PMID:26703780

  14. 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.

  15. 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.

  16. Manganese(III) Porphyrin-based Potentiometric Sensors for Diclofenac Assay in Pharmaceutical Preparations

    PubMed Central

    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. PMID:22163384

  17. 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.…

  18. 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…

  19. 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.

  20. 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.

  1. A Dating Analogy for Acid-Base Titration Problems

    NASA Astrophysics Data System (ADS)

    Delorenzo, Ronald

    1995-11-01

    Although many students can easily and quickly calculate the answers to titration problems using formulas, they frequently have trouble understanding the consequences of concentrating or diluting unknowns before titrating them. I use a combination of dimensional analysis and dating analogies to alleviate this confusion.

  2. 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…

  3. 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…

  4. 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.…

  5. 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.

  6. 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 (δQV = 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. PMID:26889710

  7. Titration and hysteresis in epigenetic chromatin silencing

    NASA Astrophysics Data System (ADS)

    Dayarian, Adel; Sengupta, Anirvan M.

    2013-06-01

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

  8. 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.

  9. Potentiometric map of the Lower Wilcox Aquifer in Mississippi, fall 1979

    USGS Publications Warehouse

    Wasson, B.E.

    1980-01-01

    The potentiometric map of the lower Wilcox aquifer is one of a series of maps, prepared by the U.S. Geological Survey in cooperation with the Mississippi Department of Natural Resources , delineating the potentiometric surfaces of the major aquifers in Mississippi. In the outcrop area of the lower Wilcox 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 but is strongly affected by pumpage from public and industrial wells in several areas in northwestern Mississippi. This pumpage has caused a large shallow depression in the potentiometric surface in the Marks-Batesville-Charleston-Tunica area. (USGS)

  10. Potentiometric surface of Floridan aquifer May 1975, and change of potentiometric surface 1969 to 1975, Southwest Florida Water Management District and adjacent areas

    USGS Publications Warehouse

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

    1976-01-01

    Maps showing the potentiometric surface of the Floridan aquifer for May 1975, and changes of potentiometric surface from 1964 to 1975 were prepared for areas in southwest Florida. Contours and color codes describe water-level changes. The larger map, scale 1:500,000, reflects the water-level changes from 1969-75. The smaller map shows the changes from January 1964 to May 1969. (Woodard-USGS)

  11. A novel potentiometric method for the determination of real crosslinking ratio of poly(aspartic acid) gels.

    PubMed

    Torma, Viktória; Gyenes, Tamás; Szakács, Zoltán; Zrínyi, Miklós

    2010-03-01

    In order to obtain nontoxic functional polymer gels for biomedical applications, chemically crosslinked poly(aspartic acid) gels have been prepared using 1,4-diaminobutane as crosslinker. The presence of COOH and amino groups on the network chains renders these gels pH sensitive. Due to the specific hydrophobic-hydrophilic balance, these gels show a significant volume transition at a well-defined pH close to the pK value of uncrosslinked poly(aspartic acid). Since the magnitude of volume change critically depends on the degree of crosslinking, it is an important task to determine the topological characteristics of these networks. A novel method based on potentiometric acid-base titration has been developed to assess the crosslinking ratio, excluding physical crosslinks and entanglements. It turned out that only 25% of all crosslinker molecules forms real crosslinks between the poly(aspartic acid) chains; the rest react with one of its functional groups and forms short pendant side chains. At a nominal crosslinking ratio of 0.1, the number average molecular mass between crosslinks is found to be M(c) = 2300. PMID:19761876

  12. 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.

  13. 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.

  14. 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.

  15. 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

  16. 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.

  17. 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)

  18. 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)

  19. 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.

  20. A Variety of Electrochemical Methods in a Coulometric Titration Experiment

    NASA Astrophysics Data System (ADS)

    Lotz, Albert

    1998-06-01

    An experiment for a practical course is described in which the amounts of HCl and KI in a mixture of standardized solutions are determined by three coulometric titrations. The iodide content is titrated with bromine that is generated at the anode from bromide which oxidizes the I- to I2 and further to IBr2-. The titration is followed with a twin-polarizable platinum electrode which essentially records the I2 and (after the endpoint) Br2 levels. Analysis of the chloride content is performed indirectly by titration of the acid through cathodic reduction of H+ to H2. The titration is monitored with a glass electrode. Finally I- and Cl- are determined simultaneously by anodic dissolution of a silver wire with a silver electrode recording the course of the titration. The experiment provides an internal check of the quality of the analysis and presents a variety of electrochemical methods of pedagogical value. Hints for the practical performance of the experiment in laboratory courses are given, and the necessary electronic circuits for self-assembling are described. Laboratory experiences with students' data collection by hand, recorder and computer are dealt with in this experiment. A complete list of earlier papers is provided, which can be found in this Journal, on the subject of coulometric analysis.

  1. Potentiometric-level monitoring program: Mississippi and Louisiana. Annual status report for fiscal year 1984

    SciTech Connect

    Not Available

    1986-07-01

    Potentiometric-level data presented in this report were collected from October 1983 through September 1984 at 79 wells in Mississippi and Louisiana. These wells are located near Richton and Cypress Creek Domes in Mississippi and Vacherie Dome in Louisiana. Fourteen wells were added to the program during this period. Two of these wells were not measurable. Two wells previously unmeasurable were located and measured. One well was destroyed during military maneuvers in the area. Analysis of the data indicated minimal, if any, change in potentiometric levels during the past year in the Citronelle, Hattiesburg, Cockfield, Sparta, and Wilcox Formations in Mississippi. A continuing decline in potentiometric levels, ranging from 0.3 to 0.6 foot per year, occurred in the wells screened in the caprock at Richton and Cypress Creek Domes. The Catahoula Formation experienced a continuing decline in potentiometric levels of about 2 feet per year. Two wells in the Cook Mountain Formation showed a continuing rise in potentiometric levels ranging from 8 to 30 ft during the past fiscal year. Wells screened in the Austin Formation in Louisiana showed a fall in potentiometric levels of 2 to 3 ft over the past fiscal year. Other formations in Louisiana generally showed no change in potentiometric levels over the past year. 26 refs., 2 figs., 3 tabs.

  2. Self-Titrating Anticoagulant Nanocomplexes That Restore Homeostatic Regulation of the Coagulation Cascade

    PubMed Central

    2015-01-01

    Antithrombotic therapy is a critical portion of the treatment regime for a number of life-threatening conditions, including cardiovascular disease, stroke, and cancer; yet, proper clinical management of anticoagulation remains a challenge because existing agents increase the propensity for bleeding in patients. Here, we describe the development of a bioresponsive peptide–polysaccharide nanocomplex that utilizes a negative feedback mechanism to self-titrate the release of anticoagulant in response to varying levels of coagulation activity. This nanoscale self-titrating activatable therapeutic, or nanoSTAT, consists of a cationic thrombin-cleavable peptide and heparin, an anionic polysaccharide and widely used clinical anticoagulant. Under nonthrombotic conditions, nanoSTATs circulate inactively, neither releasing anticoagulant nor significantly prolonging bleeding time. However, in response to life-threatening pulmonary embolism, nanoSTATs locally release their drug payload and prevent thrombosis. This autonomous negative feedback regulator may improve antithrombotic therapy by increasing the therapeutic window and decreasing the bleeding risk of anticoagulants. PMID:25119520

  3. Complexometric Titrations: Competition of Complexing Agents in the Determination of Water Hardness with EDTA

    NASA Astrophysics Data System (ADS)

    Yappert, M. Cecilia; Dupre, Donald B.

    1997-12-01

    The competition of complexing agents for the same metal ion and the formation of colored metal-ion complexes is demonstrated with the use of an overhead projector. This demonstration can be used to emphasize both the relevance of the relative values of formation constants in the complexation of metal cations and the applicability of complexometric titrations in quantitative chemical analysis. The demonstration is based on the traditional determination of water hardness in which EDTA is used as the titrant that complexes Mg2+ and Ca2+ ions. The color change that signals the end of the titration represents the successful removal of the Mg2+ ions from the metallochromic indicator Calmagite. This removal is possible because the value of the formation constant of the [Mg(EDTA)]2- complex is about 3 orders of magnitude greater than that corresponding to the [Mg(Calmagite)]- complex. The color change from wine-red (metal-bound indicator) to blue (unbound indicator) can be seen clearly in a large classroom with the use of overhead projection.

  4. Transport of Divalent Cations

    PubMed Central

    Van de Geijn, Siebe C.; Petit, Charles M.

    1979-01-01

    The cation exchange capacity of the intact xylem vessels in cut shoots of papyrus (Cyperus papyrus spec.) has been determined. The cation exchange capacity is independent of the cation concentration in the transpiration stream, and is equal for Ca and Co. The high value of the cation exchange capacity (0.6 to 1 × 10?7 equivalents per square centimeter vessel wall surface) leads to the hypothesis that the porous structure of the vessel wall, and not only the inner vessel wall surface, acts as a cation exchanger. Differences between anion ([32P]phosphate, [45Ca]EDTA2?, [115Cdm]-EDTA2?), and cation ([45Ca]2+, [115Cdm]2+) movement are explained in terms of transport with the transpiration flux or by exchange reactions. The competition between exchange sites and natural or synthetic ligands for the divalent cations is discussed. Images PMID:16661112

  5. 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.

  6. 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. PMID:25857888

  7. 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.

  8. Potentiometric-spectroscopic evaluation of metal-ion complexes by humic fractions extracted from corn tissue

    NASA Astrophysics Data System (ADS)

    Evangelou, V. P.; Marsi, M.; Chappell, M. A.

    2002-08-01

    Humic fraction (HF) functional group-type and content are expected to depend on molecular size, which in turn, is expected to influence formation of heavy-metal complexes. In this study, corn ( Zea mays L .) stalks and leaves were decomposed for an 8-month period to produce water-soluble humic substances. These substances were separated into three water-soluble fractions, HF1, HF2 and HF3, from highest to lowest relative molecular size. Functional group determination showed that carboxylic, and phenolic OH acidity increased as relative molecular size of humic fractions decreased. We also observed decreasing C/O ratios from larger to smaller corn tissue-derived humic fractions, whereas N/C and H/C ratios remained relatively unaffected. Furthermore, using potentiometric titration and FTIR spectroscopy we studied formation of Ca 2+-, Cd 2+-, and Cu 2+-humic fraction complexes and how they were affected by pH and molecular size. We determined that metal-humic complexes exhibited at least two types of functional group-sites with respect to Ca 2+, Cd 2+, and Cu 2+ complexation. Strength of metal-ion humic complexes followed the order Cu 2+>Cd 2+>Ca 2+ and was affected by pH, especially for low affinity sites. Carboxylic groups were most likely the dominant group-sites involved in complex formation. Magnitude of the metal-humic formation constants in the logarithmic form at the lowest equilibrium metal-ion concentration, under the various pH values tested, varied from 5.39 to 5.90 for Ca 2+, 5.36 to 6.01 for Cd 2+, and 6.93 to 7.71 for Cu 2+. Furthermore, the formation constants appeared to be positively influenced by decreasing molecular size of water-soluble humic fraction, and increasing pH. However, our molecular spectra showed that the p Ka of corn humic fractions increased with decreasing relative molecular size and that Cu 2+ was more covalently bonded by humic fractions than were Ca 2+ and Cd 2+, and the nature of the covalent bond character was independent of pH.

  9. CO2 Selective Potentiometric Sensor in Thick-film Technology

    PubMed Central

    Sahner, Kathy; Schulz, Anne; Kita, Jaroslaw; Merkle, Rotraut; Maier, Joachim; Moos, Ralf

    2008-01-01

    A potentiometric sensor device based on screen-printed Nasicon films was investigated. In order to transfer the promising sensor concept of an open sodium titanate reference to thick film technology, “sodium-rich” and “sodium-poor” formulations were compared. While the “sodium-rich” composition was found to react with the ion conducting Nasicon during thermal treatment, the “sodium-poor” reference mixture was identified as an appropriate reference composition. Screen-printed sensor devices were prepared and tested with respect to CO2 response, reproducibility, and cross-interference of oxygen. Excellent agreement with the theory was observed. With the integration of a screen-printed heater, sensor elements were operated actively heated in a cold gas stream.

  10. The Cation-? Interaction

    PubMed Central

    DOUGHERTY, DENNIS A.

    2014-01-01

    CONSPECTUS The chemistry community now recognizes the cation-? 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-? 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 ? systems. Important gas phase studies established the fundamental nature of the cation-? interaction. The strength of the cation-? interaction – Li+ binds to benzene with 38 kcal/mol of binding energy; NH4+ with 19 kcal/mol– distinguishes it from the weaker polar-? interactions observed in the benzene dimer or water-benzene complexes. In addition to the substantial intrinsic strength of the cation-? interaction in gas phase studies, the cation-? interaction remains energetically significant in aqueous media and under biological conditions. Many studies have shown that cation-? 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-? interaction includes a substantial electrostatic component. The six (four) C??–H?+ bond dipoles of a molecule like benzene (ethylene) combine to produce a region of negative electrostatic potential on the face of the ? 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 is more polarizable than benzene, but a decidedly poorer cation binder. Many studies have documented cation-? interactions in protein structures, where Lys or Arg side chains interact with Phe, Tyr, or Trp. In addition, countless studies have established the importance of cation-? interaction in a range of biological processes. Our work has focused on molecular neurobiology, and we have shown that neurotransmitters generally use a cation-? interaction to bind to their receptors. We have also shown that many drug-receptor interactions involve cation-? interactions. A cation-? interaction plays a critical role in the binding of nicotine to ACh receptors in the brain, an especially significant case. Other researchers have established important cation-? interactions in the recognition of the “histone code,” in terpene biosynthesis, in chemical catalysis, and in many other systems. PMID:23214924

  11. Reliability of home CPAP titration with different automatic CPAP devices

    PubMed Central

    Sériès, Frédéric; Plante, Julie; Lacasse, Yves

    2008-01-01

    Background CPAP titration may be completed by automatic apparatus. However, differences in pressure behaviour could interfere with the reliability of pressure recommendations. Our objective was to compare pressure behaviour and effective pressure recommendations between three Automatic CPAP machines (Autoset Spirit, Remstar Auto, GK 420). Methods Sixteen untreated obstructive sleep apnea patients were randomly allocated to one of the 3 tested machines for a one-week home titration trial in a crossover design with a 10 days washout period between trials. Results The median pressure value was significantly lower with machine GK 420 (5.9 +/- 1.8 cm H2O) than with the other devices both after one night and one week of CPAP titration (7.4 +/- 1.3 and 6.6 +/- 1.9 cm H2O). The maximal pressure obtained over the one-week titration was significantly higher with Remstar Auto (12.6 +/- 2.4 cm H2O, Mean +/- SD) than with the two other ones (10.9 +/- 1.0 and 11.0 +/- 2.4 cm H2O). The variance in pressure recommendation significantly differed between the three machines after one night and between Autoset Spirit and the two other machines after 1 week. Conclusion Pressure behaviour and pressure recommendation significantly differ between Auto CPAP machines both after one night and one week of home titration. PMID:18652688

  12. Galvanostatic Entrapment of Penicillinase into Polytyramine Films and its Utilization for the Potentiometric Determination of Penicillin

    PubMed Central

    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 ?M for penicillin and achieved a minimum detectable concentration of 0.3 ?M. 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. PMID:22319276

  13. 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)

  14. Nano- and microsized zeolites as a perspective material for potentiometric biosensors creation

    NASA Astrophysics Data System (ADS)

    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.

    2015-02-01

    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.

  15. Potentiometric map of the Meridian-Upper Wilcox Aquifer in Mississippi, fall 1979

    USGS Publications Warehouse

    Wasson, B.E.

    1980-01-01

    The potentiometric map of the Meridian-upper Wilcox 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 Meridian-upper Wilcox 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 large groundwater withdrawals in the Greenwood, Indianola, Marks, Grenada, and Memphis areas. Historically, water levels in or near the outcrop of the Meridian-upper Wilcox have shown little or no long-term changes, but during the past 20 years water levels have declined from 1 to 2 feet per year in much of the confined part of the aquifer. (USGS)

  16. Potentiometric map of the Sparta aquifer system in Mississippi, fall, 1980

    USGS Publications Warehouse

    Wasson, B.E.

    1980-01-01

    This potentiometric map of the Sparta aquifer system is the tenth 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 Sparta, the potentiometric surface is strongly affected by recharge from precipitation, by topography, and by drainage of the aquifer into 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, Yazoo City, Cleveland, Clarksdale, and Memphis areas. Historically, water levels in or near the outcrop of the Sparta have shown little or no long-term changes, but during the past 20 years, in much of the confined part of the aquifer, water levels have declined from 1 to 3 feet per year. (USGS)

  17. 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.

  18. Predicting Acid-Base Titration Curves without Calculations

    NASA Astrophysics Data System (ADS)

    Barnum, Dennis W.

    1999-07-01

    A common approach to teaching acid-base chemistry is to have students calculate titration curves. Students often concentrate on setting up the equations or the spreadsheet and either lose sight of or fail to recognize the general principles that the calculations are intended to convey. In this paper a qualitative and systematic method for sketching titration curves is presented. Even the more complex cases such as salts or polyprotic acids and bases are treated just as easily as simple monoprotic acids. Having students predict the shape of titration curves from known equilibrium constants helps to focus attention on the general principles without distraction by the mathematics. Because the method is very fast, students can work through more examples.

  19. Potentiometric-level monitoring program - Mississippi and Louisiana: annual status report for fiscal year 1983

    SciTech Connect

    Not Available

    1984-03-01

    Potentiometric-level data presented in this report were collected from October 1982 to September 1983 at 62 wells in Mississippi and Louisiana near Richton and Vacherie Domes, respectively. Six wells were added to the monitoring program during this period, and one previously measured well was damaged and has been deleted from the monitoring program. Analysis of the data indicates that most of the potentiometric-level changes recorded during fiscal year 1983 were small (less than 2 feet) and attributable to seasonal fluctuations. Of the 62 wells monitored, 18 exhibited potentiometric-level changes in excess of 2 feet. In Mississippi, the data generally indicate that a long-term, potentiometric-level increase is occurring in the Sparta, Kosciusko, Hattiesburg, Wilcox, and Citronelle Formations. Only seasonal fluctuations in potentiometric levels were observed in the caprock, and in the Catahoula and Cockfield Formations. In Louisiana, a long-term, potentiometric-level decline was observed for the Lower Austin Formation while an increase was observed for the Sparta and Upper Austin Formations. Seasonal fluctuations were observed in the Wilcox, Carrizo, and Nacatoch Formations. This work is a continuation of that described in ONWI-478 for fiscal year 1982. 24 references, 2 figures, 3 tables.

  20. Elucidation of ionic interactions in the protic ionic liquid solutions by isothermal titration calorimetry.

    PubMed

    Rai, Gitanjali; Kumar, Anil

    2014-04-17

    The strong hydrogen-bonded network noted in protic ionic liquids (PILs) may lead to stronger interactions of the ionic entities of PILs with solvents (water, methanol, ethylene glycol, dimethylsulfoxide (DMSO), N,N'-dimethylformamide (DMF)) as compared with those of aprotic ionic liquids (APILs). The PILs used in this work are 1-methylimidazolium tetrafluoroborate, 2-methylpyridinium tetrafluoroborate, and N-methylpyrrolodinium tetrafluoroborate in comparison to 1-butyl-3-methylimidazolium tetrafluoroborate, which is classified as an APIL. In this work, the excess partial molar enthalpy, H(E)IL obtained from isothermal calorimetric titrations at 298.15 K is used to probe the nature of interactions of the PIL cations with solvent molecules against those present in APIL-solvent systems. This work also reports interesting flip-flopping in the thermal behavior of these PIL-solvent systems depending upon the structure of the cationic ring of a PIL. In some cases, these flip-flops are the specific fingerprints for specific PILs in a common solvent environment. The excess partial molar enthalpy at infinite dilution, H(E,?)IL, of these PILs bears a critical dependence on the solvent properties. An analysis of relative apparent molar enthalpies, ?L, of the PIL solutions by the ion interaction model of Pitzer yields important information on ionic interactions of these systems. PMID:24650134

  1. 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.

  2. 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 ? 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.

  3. Constant-Current Coulometric Titration of Hydrochloric Acid

    NASA Astrophysics Data System (ADS)

    Swim, James; Earps, Edward; Reed, Laura M.; Paul, David

    1996-07-01

    The titration of a strong acid with a strong base and the electrolysis of water are two classic laboratory exercises that are either performed or demonstrated in secondary school classrooms in order to introduce two important areas of chemsitry: acid-base chemistry and electrochemistry. In this experiment we have combined these two classical experiments into one complete laboratory experience. Here we report how the elctrolysis of an aqueous solution can be used to determine the concentration of hydrochloric acid in a coulometric titration.

  4. 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.

  5. 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.

  6. Titrating-delay matching-to-sample in the pigeon.

    PubMed

    Kangas, Brian D; Vaidya, Manish; Branch, Marc N

    2010-07-01

    The titrating-delay matching-to-sample (TDMTS) procedure offers researchers an additional behavioral task thought to capture some important features of remembering. In this procedure, the delay between sample offset and comparison onset adjusts as a function of the subject's performance. Specifically, correct matches increase the delay and incorrect matches decrease the delay, and steady-state titrated delays serve as the primary dependent measure. The present series of experiments investigated the effects of several procedural variables on performance in TDMTS procedures in an effort to elucidate better its features to allow for more precision in future use. Experiment 1 reports results from a parametric analysis of fixed-ratio response requirements on the sample key that indicated improved remembering in the form of higher daily titrated delay values as the requirement was increased. Experiment 2 investigated the extent to which the initial delay value in each session affected session-wide delay values. Results indicated that regardless of value of the initial delay, the subjects' performances adjusted the delay values in the direction of the known baseline delay-value levels. Experiment 3 manipulated the step size by which delay values were adjusted and the results indicated that larger step sizes increased both session-to-session variability and within-session range of titrated delay values, although the average values remained approximately the same. These results suggest that the TDMTS task serves as a promising procedure to study what many refer to as memory. PMID:21279163

  7. Titrating-Delay Matching-to-Sample in the Pigeon

    ERIC Educational Resources Information Center

    Kangas, Brian D.; Vaidya, Manish; Branch, Marc N.

    2010-01-01

    The titrating-delay matching-to-sample (TDMTS) procedure offers researchers an additional behavioral task thought to capture some important features of remembering. In this procedure, the delay between sample offset and comparison onset adjusts as a function of the subject's performance. Specifically, correct matches increase the delay and…

  8. 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.

  9. 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.

  10. 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.

  11. 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)

  12. 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…

  13. 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…

  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. Potentiometric and Relaxometric Properties of a Gadolinium-based MRI Contrast Agent for Sensing Tissue pH

    PubMed Central

    Kálmán, Ferenc K.; Woods, Mark; Caravan, Peter; Jurek, Paul; Spiller, Marga; Tircsó, Gyula; Király, Róbert; Brücher, Ern?; Sherry, A. Dean

    2008-01-01

    The pH sensitive contrast agent, GdDOTA-4AmP (Gd1) has been successfully used to map tissue pH by MRI. Further studies now demonstrate that two distinct chemical forms of the complex can be prepared depending upon the pH at which Gd3+ is mixed with ligand 1. The desired pH sensitive form of this complex, referred to here as a Type II complex, is obtained as the exclusive product only when the complexation reaction is performed above pH 8. At lower pH values, a second complex is formed that, by analogy with an intermediate formed during preparation of GdDOTA, we tentatively assign this to a Type I complex where the Gd3+ is coordinated only by the appended side-chain arms of 1. The proportion of Type I complex formed is largely determined by the pH of the complexation reaction. The magnitude of pH dependent change in relaxivity of Gd1 was found to be less than earlier reported (S. Zhang, K. Wu, and A. D. Sherry, Angew. Chem., Int. Ed., 1999, 38, 3192), likely due to contamination of the earlier sample by an unknown amount of Type I complex. Examination of the NMRD and relaxivity temperature profiles, coupled with information from potentiometric titrations, shows that the amphoteric character of the phosphonate side-chains enables rapid prototropic exchange between the single bound water of the complex with those of the bulk water thereby giving Gd1 a unique pH dependent relaxivity that is quite useful for pH mapping of tissues by MRI. PMID:17539632

  17. 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.

  18. 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 (<10min), 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

  19. 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

  20. Miniaturized graphite sensors doped with metal-bathophenanthroline complexes for the selective potentiometric determination of uric acid in biological fluids.

    PubMed

    Hassan, S S; Rizk, N M

    1997-08-01

    Miniaturized poly(vinyl chloride) matrix membrane sensors in an all-solid-state graphite support, responsive to urate anion, were developed. The membranes incorporate lipophilic ion-pair complexes of urate anion with ruthenium(III), iron(II), nickel(II) and copper(I) bathophenanthroline (4,7-diphenyl-1,10-phenanthroline) counter cations. The sensors demonstrate a near-Nernstian response to urate over the concentration range 1 x 10(-2)-1 x 10(-5) mol l-1 and have micromolar detection limits and good selectivity properties. The response is virtually unaffected by pH changes in the range 7-10 and the response times are 5-10 s in aqueous solutions and in human serum and urine samples. A flow injection detector incorporating an iron(II) bathophenanthroline-urate graphite sensor was used for continuous monitoring of uric acid. The minimum detectable concentration was approximately 8 micrograms ml-1 and the sample throughput was approximately 120 h-1. Direct potentiometric determination of uric acid in the static and hydrodynamic modes of operation over the range 15 micrograms ml-1-1.5 mg ml-1 showed average recoveries of 98.7 and 97.8% with RSDs of 0.6 and 0.7%, respectively. Application of the method to the determination of uric acid in human serum and urine gave results that compared favourably with those obtained by the standard spectrophotometric method. PMID:9338988

  1. 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)

  2. 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±0.5mVdecade(-1) over the linear range of 5.0×10(-5)-1.0×10(-2)molL(-1) and the detection limit 1.0×10(-5)molL(-1), as well as the response time 10s. It can be used in the pH range 6.2-8.5 for 10months 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

  3. Cyclodextrin-based potentiometric sensors for midazolam and diazepam.

    PubMed

    Amorim, C G; Araújo, A N; Montenegro, M C B S M; Silva, V L

    2008-12-01

    In this work the implementation of benzodiazepine ion-selective electrodes for pharmaceutical formulations control is described. The solid-contact electrodes for midazolam and diazepam are based on polymeric membranes incorporating respectively beta-cyclodextrin and (2-hydroxiproyl)-gamma-cyclodextrin as ionophores, 2-fluorophenyl 2-nitrophenyl ether as plasticizer and potassium tetrakis (p-chlorophenyl) borate as ionic additive. For conventionally shaped midazolam electrode a slope of 61.9+/-1.3 mVdec(-1), a LLLR of 5.7+/-2.7 x 10(-4)gL(-1) and pH range of 2.6-5.4 was obtained, while the corresponding values for diazepam electrodes were of 67.6+/-3.0 mVdec(-1), 4.9+/-1.5 x 10(-2)gL(-1) and 1.9-2.7 pH units, respectively. Membrane optimization was based on the molar ratio between the ionophore and additive for midazolam and on inclusion cavity of cyclodextrin for diazepam. The miniaturization of the above-described electrodes gave rise to potentiometric detectors for sequential-injection lab-on-valve system with similar characteristics albeit the useful lifetime shortened from 1 year to approximately 15 days under continuous operation. The optimized flow conditions were achieved for sample injection volumes of 20 microL propelled towards the detection cell at the flow rate of 16 microLs(-1) during 80s. Real sample analysis revealed statistical accuracy and between-days precision comparable to the general used chromatographic-based procedure. PMID:18835673

  4. Difference between the potentiometric surfaces of the Magothy Aquifer in Fall of 1975 and Fall of 1986 in southern Maryland

    USGS Publications Warehouse

    Mack, F.K.; Andreasen, D.C.; Curtin, S.E.; Wheeler, J.C.

    1987-01-01

    The potentiometric map is highlighted with indications concerning: (1) outcrop areas of the Magothy aquifer; (2) the approximate location of the line of equal difference between the potentiometric surface in fall 1975 and fall 1986; (3) observation and/or supply wells yielding < 10,000 gallons/day (gpd); and (4) other supply wells with yields > 10,000 gpd. (Lantz-PTT)

  5. Difference between the potentiometric surface of the Aquia Aquifer in Spring of 1979 and Fall of 1986 in southern Maryland

    USGS Publications Warehouse

    Mack, F.K.; Andreasen, D.C.; Curtin, S.E.; Wheeler, J.C.

    1987-01-01

    The potentiometric map is highlighted with indications concerning: (1) outcrop areas of the Aquia aquifer; (2) the approximate line of equal distance between the potentiometric surfaces of spring 1979 and fall 1986; (3) observation and/or supply wells yielding < 10,000 gallons/day (gpd); and (4) other supply wells with yields > 10,000 gpd. (Lantz-PTT)

  6. Characterization of molecular interactions using isothermal titration calorimetry.

    PubMed

    Krell, Tino; Lacal, Jesús; García-Fontana, Cristina; Silva-Jiménez, Hortencia; Rico-Jiménez, Miriam; Lugo, Andrés Corral; Darias, José Antonio Reyes; Ramos, Juan-Luis

    2014-01-01

    Isothermal titration calorimetry (ITC) is based on a simple titration of one ligand with another and the small heat changes caused by the molecular interaction are detected. From one ITC experiment the complete set of thermodynamic parameters of binding including association and dissociation constants as well as changes in enthalpy, entropy, and free energy can be derived. Using this technique almost any type of molecular interaction can be analyzed. Both ligands are in solution, and there is no need for their chemical derivatization. There are no limits as to the choice of the analysis buffer, and the analysis temperature can be set between 4 and 80 °C. This technique has been primarily applied to study the interaction between various proteins of Pseudomonas with small molecule ligands. In addition, ITC has been used to study the binding of Pseudomonas proteins to target DNA fragments. PMID:24818906

  7. Kids in a Candy Store: An Analogy for Back Titration

    NASA Astrophysics Data System (ADS)

    Last, Arthur M.

    1998-09-01

    A simple analogy for back titration is presented. A child is sent into a candy store with a known amount of money in order to purchase a candy bar and the cost of the bar is subsequently determined by counting the amount of change the child brings back. This is analogous to adding excess acid to a base and determining how much base was present by titrating the unreacted acid. The analogy is extended to illustrate what happens when an acidic or basic impurity is present in the system and is further developed to cover a situation in which the acid and unknown base react in a 2:1 ratio rather than a 1:1 ratio.

  8. Tattoo-based potentiometric ion-selective sensors for epidermal pH monitoring.

    PubMed

    Bandodkar, Amay J; Hung, Vinci W S; Jia, Wenzhao; Valdés-Ramírez, Gabriela; Windmiller, Joshua R; Martinez, Alexandra G; Ramírez, Julian; Chan, Garrett; Kerman, Kagan; Wang, Joseph

    2013-01-01

    This article presents the fabrication and characterization of novel tattoo-based solid-contact ion-selective electrodes (ISEs) for non-invasive potentiometric monitoring of epidermal pH levels. The new fabrication approach combines commercially available temporary transfer tattoo paper with conventional screen printing and solid-contact polymer ISE methodologies. The resulting tattoo-based potentiometric sensors exhibit rapid and sensitive response to a wide range of pH changes with no carry-over effects. Furthermore, the tattoo ISE sensors endure repetitive mechanical deformation, which is a key requirement of wearable and epidermal sensors. The flexible and conformal nature of the tattoo sensors enable them to be mounted on nearly any exposed skin surface for real-time pH monitoring of the human perspiration, as illustrated from the response during a strenuous physical activity. The resulting tattoo-based ISE sensors offer considerable promise as wearable potentiometric sensors suitable for diverse applications. PMID:23113321

  9. Potentiometric surface of the Peedee Aquifer in the central coastal plain of North Carolina, December 1986

    USGS Publications Warehouse

    Brockman, Allen R.; Lyke, William L.; Winner, M.D., Jr.

    1989-01-01

    Water level measurements were made in 37 wells open to the Peedee aquifer at the end of 1986 to determine the configuration of its potentiometric surface over an area of about 4,100 square miles in the central Coastal Plain of North Carolina. The potentiometric surface of the Peedee slopes southeastward from an altitude of more than 100 ft above sea level along the western limits of the aquifer to less than 20 ft near the coastline. Several cones of depression have formed in response to the effects of groundwater pumpage. The largest cone occurs near the City of Jacksonville in Onslow County where the potentiometric surface is nearly 70 ft below sea level.

  10. Potentiometric surface of the Brightseat-upper Potomac Aquifer in Virginia 1993

    USGS Publications Warehouse

    Hammond, E.C.; McFarland, E.R.; Focazio, M.J.

    1994-01-01

    Ground-water level measurements from 30 wells in the Brightseat-upper Potomac aquifer in the Coastal Plain Physiographic Province of Virginia in 1993 were used to prepare a map of the potentiometric surface of the aquifer. The map shows the potentiometric surface of the Brightseat-upper Potomac aquifer indicating a regional trend toward the Chesapeake Bay and Atlantic Ocean. The potentiometric-surface data indicate that cones of depression are apparent around West Point and in southeastern Isle of Wight County near Franklin, Virginia. The highest ground-water-level measurement was 4 feet above sea level in northern Accomack County, and the lowest ground-water-level measure- ment was 117 feet below sea level in Franklin, Virginia.

  11. Potentiometric Urea Biosensor Based on Carbon Nanotubes and Polyion Complex Film.

    PubMed

    Nguyen, Linh Thi My; Yoon, Hyon Hee

    2015-02-01

    Enzymatic electrode for a potentiometric urea sensor was prepared by sequential coating of carbon nanotube (CNT), urease (Urs) and polyion complex (mixture of poly-L-lysine hydrobromide and poly (sodium 4-styrenesulfonate), PIC) on an ITO glass. The prepared electrode (ITO/CNT/Urs/PIC) was characterized by potentiometric measurements at different urea concentrations in Tris-HCI buffer (pH 7.0). The potentiometric response of the electrode was linear in the range of 1 x 10(-5) to 3 x 10(-3) M with a correlation coefficient of 0.999 and a sensitivity of 59.1 mV/decade. It was found that the addition of CNT caused considerable improvement of the sensitivity of the electrode to urea. The response time was approximately 60-90 s. A half of the initial sensitivity was retained for 15-17 d at room temperature. PMID:26353625

  12. Generalized potentiometric-surface map of the High Plains aquifer in Wyoming, 1981

    USGS Publications Warehouse

    Avery, Charles; Pettijohn, Robert A.

    1984-01-01

    A potentiometric-surface map shows the general configuration of the water surface for the High Plains Aquifer, which is composed of Oligocene age and younger rocks in southeastern Wyoming. The potentiometric contours are shown at 100-foot intervals on a map at a scale of 1:250,000. The High Plains Aquifer in Wyoming underlies an area of 8,190 square miles and geologically consists of the White River Formation of Oligocene age, the Arikaree Formation of early Miocene age, the Ogallala Formation of late Miocene age, and alluvial deposits of Quaternary age. The altitude of the potentiometric surface declines from about 7 ,100 feet in southwestern Laramie County to about 4,100 feet in eastern Goshen County. Typically, the slope is between 20 and 30 feet per mile; the general direction of flow is eastward. (USGS)

  13. 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)

  14. Solubility of dicalcium phosphate dihydrate by solid titration.

    PubMed

    Pan, H-B; Darvell, B W

    2009-01-01

    Solid-titration results for hydroxyapatite (HAp), octacalcium phosphate, beta-tricalcium phosphate and tetracalcium phosphate have shown that the only stable phase in 100 mmol x l(-1) KCl at 37 degrees C is HAp. In particular, dicalcium phosphate dihydrate (DCPD) did not form at pH <4.2 (where it is otherwise believed to be stable) except as a metastable phase under conditions of slight supersaturation. The behaviour of DCPD itself under the same conditions requires checking. Solid titration was used to determine the apparent solubility of DCPD in a 100-mmol x l(-1) KCl solution at 37.0 +/- 0.1 degrees C over the pH range 3.2-11.6. The constitution of the precipitate was determined by X-ray diffraction, particle morphology was observed by scanning and transmission electron microscopy, and the precipitate Ca/P ratio was calculated by energy-dispersive X-ray analysis. The titration curve for DCPD was substantially lower than the position reported elsewhere. DCPD was the only identified phase at equilibrium at pH 3.60 and 4.50, but HAp was formed after seeding with 1 mg HAp at DCPD equilibrium at pH 4.47, 3.60 and 3.30. It is concluded that the titration curve observed for DCPD corresponds to the solubility isotherm for the phase, but that this represents a metastable equilibrium. HAp is more stable than DCPD, particularly below pH 4.2. The implications for calcium phosphate studies are profound as the reverse is generally believed to be true. Thus, solubility results and the nature of the carious lesion need reconsideration. PMID:19439946

  15. 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

  16. Titration of hydrophobic polyelectrolytes using Monte Carlo simulations

    NASA Astrophysics Data System (ADS)

    Ulrich, Serge; Laguecir, Abohachem; Stoll, Serge

    2005-03-01

    The conformation and titration curves of weak (or annealed) hydrophobic polyelectrolytes have been examined using Monte Carlo simulations with screened Coulomb potentials in the grand canonical ensemble. The influence of the ionic concentration pH and presence of hydrophobic interactions has been systematically investigated. A large number of conformations such as extended, pearl-necklace, cigar-shape, and collapsed structures resulting from the subtle balance of short-range hydrophobic attractive interactions and long-range electrostatic repulsive interactions between the monomers have been observed. Titration curves were calculated by adjusting the pH-pK0 values (pK0 represents the intrinsic dissociation constant of an isolated monomer) and then calculating the ionization degree ? of the polyelectrolyte. Important transitions related to cascades of conformational changes were observed in the titration curves, mainly at low ionic concentration and with the presence of strong hydrophobic interactions. We demonstrated that the presence of hydrophobic interactions plays an important role in the acid-base properties of a polyelectrolyte in promoting the formation of compact conformations and hence decreasing the polyelectrolyte degree of ionization for a given pH-pK0 value.

  17. 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)

  18. 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,…

  19. 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…

  20. 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,…

  1. 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…

  2. Differential electrolytic potentiometric determination of some amino acids in dosage forms.

    PubMed

    Al-Ghannam, Sheikha M; Abulkibash, Abdalla; Al-Olyyan, Abeer M

    2004-01-01

    The application of direct-current differential electrolytic potentiometry to the nonaqueous titration of amino acids was investigated. The basic character of amino acids in acetic acid was enhanced to permit their direct titration with perchloric acid. A pair of antimony electrodes was used as an indicating system. The shapes of the titration curves obtained were almost symmetrical with sharp peaks. The optimum current density for those titrations was found to be 1-2 microA/cm2. The procedure was applied successfully to the determination of certain amino acids in drug formulations, and the results were favorably compared statistically with those obtained by official methods. PMID:15287666

  3. 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

  4. 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.

  5. Depression May Reduce Adherence during CPAP Titration Trial

    PubMed Central

    Law, Mandy; Naughton, Matthew; Ho, Sally; Roebuck, Teanau; Dabscheck, Eli

    2014-01-01

    Study Objectives: Depression is a risk factor for medication non-compliance. We aimed to identify if depression is associated with poorer adherence during home-based autotitrating continuous positive airway pressure (autoPAP) titration. Design: Mixed retrospective-observational study. Setting: Academic center. Participants: Two-hundred forty continuous positive airway pressure-naïve obstructive sleep apnea (OSA) patients. Measurements: Patients underwent approximately 1 week of home-based autoPAP titration with adherence data downloaded from the device. Electronic hospital records were reviewed in a consecutive manner for inclusion. Three areas of potential predictors were examined: (i) demographics and clinical factors, (ii) disease severity, and (iii) device-related variables. Depression and anxiety were assessed using the Hospital Anxiety and Depression Scale (HADS). Scores on the subscales were categorized as normal or clinical diagnoses of depression (? 8) and anxiety (? 11). The primary outcome variable was the mean hours of autoPAP used per night. Results: Patients were diagnosed with OSA by either attended polysomnography (n = 73, AHI 25.5[15.1-41.5]) or unattended home oximetry (n = 167, ODI3 34.0[22.4-57.4]) and had home-based autoPAP titration over 6.2 ± 1.2 nights. Mean autoPAP use was 4.5 ± 2.4 hours per night. Multiple linear regression analysis revealed that depression and lower 95th percentile pressures significantly predicted lesser hours of autoPAP use (R2 = 0.19, p < 0.001). Significantly milder OSA in those requiring lower pressures may have confounded the relationship between 95th percentile pressure and autoPAP use. Conclusion: Depression was independently associated with poorer adherence during home-based autoPAP titration. Depression may be a potential target for clinicians and future research aimed at enhancing adherence to autoPAP therapy. Citation: Law M; Naughton M; Ho S; Roebuck T; Dabscheck E. Depression may reduce adherence during CPAP titration trial. J Clin Sleep Med 2014;10(2):163-169. PMID:24532999

  6. Hydroxy-thioxanthones as suitable neutral ionophores for the preparation of PVC-membrane potentiometric sensors for Al(III) ion.

    PubMed

    Shamsipur, Mojtaba; Ershad, Sohrab; Yari, Absollah; Sharghi, Hashem; Salimi, Ali Reza

    2004-02-01

    The complexation of five recently synthesized hydroxy-thioxanthone derivatives with Al3+ ion was studied in a methanol solution spectrophotometrically, and the stepwise formation constants of the resulting 1:1 and 2:1 (ligand-to-metal) complexes were evaluated. The suitability of the thioxanthone derivatives as neutral ionophores for the preparation of a new Al3+ ion-selective PVC-membrane electrode was investigated, and 1-hydroxy-3-methyl-thiocanthone was selected as the best compound for this purpose. The prepared electrode exhibits a Nernstian response for Al3+ ions over a wide concentration range (2.0 x 10(-2) to 2.0 x 10(-6) M), with a limit of detection of 1.0 x 10(-6) M. It has a very fast response time of about 5 s and can be used for at least 3 months without any considerable divergence in the potentials. The proposed membrane sensor revealed very good selectivities for Al3+ over a wide variety of other metal ions, and could be used at a working pH range of 3.4 - 5.0. It was used as an indicator electrode in potentiometric titration of aluminum ions with EDTA, and in the determination of Al3+ in different real samples. PMID:15055955

  7. 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.

  8. 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.

  9. 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.

  10. 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 between particle and crystal size, as obtained from XRD. In the course of establishing these relationships we've gained the knowledge of how to control TiO x structure, which enables the design of new and better catalysts. Understanding the synthesis-structure-function relationships allow for the design of a tandem photo/thermocatalytic reaction system for producing and consuming H2O2. By partially overcoating a TiO 2 photocatalyst with a ˜2 nm silica layer we observe a 56-fold rate improvement compared to bare-TiO2 for H2O2 synthesis from the proton-assisted reduction of O2. Addition of metal-SiO2 thermocatalysts (metal=Ti, Nb, or Ta) with sites needed for H2O2 activation creates a tandem system wherein the H2O2 produced in situ is utilized for alkene epoxidation. Compared to a thermocatalytic-only system, the tandem system accelerates epoxidation for cis-cyclooctene(11x faster), styrene(20x) and 1-octene(30x). This approach demonstrates a means for epoxidation with O2 that avoids H2O2 purification and transport, simplifies the total process, provides new opportunities for control by independent H2O2 production and consumption in the same reactor, and enhances rates relative to thermocatalytic-only epoxidation by intimately coupling H2O2 generation and consumption. Critically, establishment of titanium-silica synthesis-structure-function relationships enables the design of new catalysts and systems that are less energy- and material-intensive, leading towards more sustainable chemistry.

  11. 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

  12. 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.

  13. 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…

  14. 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…

  15. 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

  16. 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…

  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. 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…

  1. 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 ...

  2. 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. PMID:25715032

  3. 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

  4. 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.

  5. 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.

  6. A Dibasic Acid Titration for the Physical Chemistry Laboratory

    NASA Astrophysics Data System (ADS)

    Brabson, G. D.; Clay, J. T.; Walters, E. A.

    1995-07-01

    A physical chemistry laboratory experiment is described in which both pK, and pK2 are determined for weak dibasic acids with closely spaced acid dissociation constants. The method is acid-base titration. Data are acquired by a computer interfaced to a pH meter, however emphasis on experimental technique is retained by requiring students to manipulate a buret, read it, and manually enter the volumes into the computer. The computer is then used to ease the burden of tedious and repetitious calculations which yield the two pKa values.

  7. Simulating titration to goal clinical trials with statins.

    PubMed

    Southworth, Harry

    2004-05-01

    Many countries have local guidelines on the management of subjects' lipid levels with and without pharmaceutical intervention. The statin class of drugs is the preferred class for reducing low density lipoprotein cholesterol (LDL-C). Different statins have different potencies and different dose ranges. It is of interest to simulate clinical trials in which subjects are titrated through the dose ranges of various statins in accordance with local guidelines, in order to estimate the proportion of subjects who reach treatment goal of LDL-C at any particular dose of any particular statin. PMID:15206539

  8. Cation binding to 15-TBA quadruplex DNA is a multiple-pathway cation-dependent process

    PubMed Central

    Reshetnikov, Roman V.; Sponer, Jiri; Rassokhina, Olga I.; Kopylov, Alexei M.; Tsvetkov, Philipp O.; Makarov, Alexander A.; Golovin, Andrey V.

    2011-01-01

    A combination of explicit solvent molecular dynamics simulation (30 simulations reaching 4?µs in total), hybrid quantum mechanics/molecular mechanics approach and isothermal titration calorimetry was used to investigate the atomistic picture of ion binding to 15-mer thrombin-binding quadruplex DNA (G-DNA) aptamer. Binding of ions to G-DNA is complex multiple pathway process, which is strongly affected by the type of the cation. The individual ion-binding events are substantially modulated by the connecting loops of the aptamer, which play several roles. They stabilize the molecule during time periods when the bound ions are not present, they modulate the route of the ion into the stem and they also stabilize the internal ions by closing the gates through which the ions enter the quadruplex. Using our extensive simulations, we for the first time observed full spontaneous exchange of internal cation between quadruplex molecule and bulk solvent at atomistic resolution. The simulation suggests that expulsion of the internally bound ion is correlated with initial binding of the incoming ion. The incoming ion then readily replaces the bound ion while minimizing any destabilization of the solute molecule during the exchange. PMID:21893589

  9. Potentiometric surface of the lower Cape Fear Aquifer in the central coastal plain of North Carolina, December 1986

    USGS Publications Warehouse

    Winner, M.D., Jr.; 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.

  10. Altitude and configuration of the potentiometric surface, Casey Village, Warminster and Upper Southampton townships, Bucks County, Pennsylvania, August 3, 1995

    USGS Publications Warehouse

    Sloto, Ronald A.; Grazul, Kevin E.

    1995-01-01

    A map showing the potentiometric surface in Casey Village, Warminster and Upper Southampton Townships, Bucks County, was constructed from water levels measured on August 3, 1995. The potentiometric surface, measured in 17 wells screened between 18 and 64 feet below land surface, ranged from 321.99 to 344.80 feet above sea level. The potentiometric surface, measured in 12 wells screened between 48 and 108 feet below land surface, ranged from 321.95 to 337.50 feet above sea level.

  11. 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 0.7µL 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

  12. Acetoclastic methanogenic activity measurement by a titration bioassay.

    PubMed

    Rozzi, Alberto; Castellazzi, Luca; Speece, Richard E

    2002-01-01

    A titration bioassay, designed to accurately determine the activity of acetoclastic methanogens, is described that also allows evaluation of inhibition due to potential toxicants on the active biomass. The instrument is made of a pH-stat connected to an anaerobic batch reactor. Acetate is blended and mixed with anaerobic sludge in the reactor where a 1:1 N2 and CO2 mixture is sparged at the beginning of each test. As the acetoclastic methanogens consume acetate, the pH increase, and the titration unit adds acetic acid and keeps the pH constant. The rate of titrant addition is directly proportional to the methanogenic activity. A very useful feature of the system is its potential to operate for long periods (days) at constant pH and substrate (acetate) concentration. The theoretical background and principle of operation are described as well as some of the practical problems encountered with the use of the instrument. Estimation of kinetic constants for an anaerobic culture according to the Michaelis-Menten model is presented. Examples of inhibition by inorganics (NaCl) and chlorinated solvents (chloroform) are also given. PMID:11745170

  13. Cation-selective electropreconcentration.

    PubMed

    Shin, Il Hyung; Kim, Ki-Jung; Kim, Jiman; Kim, Hee Chan; Chun, Honggu

    2014-06-01

    A cation-selective microfluidic sample preconcentration system is described. The cation sample was electropreconcentrated using a reversed-direction electroosmotic flow (EOF) and an anion-permselective filter, where an electric double layer (EDL) overlap condition existed. The anion-permselective filter between microchannels was fabricated by three different methods: 1) extending a positively charged, nanoporous, polymer membrane by photopolymerization of poly(diallyldimethylammonium chloride) (PDADMAC); 2) etching a nanochannel and then coating it with a positively-charged monomer, N-[3-(trimethoxysilyl)propyl]-N'-(4-vinylbenzyl)ethylenediamine hydrochloride (TMSVE); and, 3) etching a nanochannel and then coating it with a positively-charged, pre-formed polymer, polyE-323. The EOF direction in the microchannel was reversed by both TMSVE and polyE-323 coatings. The cation-selective preconcentration was investigated using charged fluorescent dyes and tetramethylrhodamine isothiocyanate (TRITC)-tagged peptides/proteins. The preconcentration in the three different systems was compared with respect to efficiency, dependence on buffer concentration and pH, tolerable flow rate, and sample adsorption. Both TMSVE- and polyE-323-coated nanochannels showed robust preconcentration at high flow rates, whereas the PDADMAC membrane maintained anion-permselectivity at higher buffer concentrations. The TMSVE-coated nanochannels showed a more stable preconcentration process, whereas the polyE-323-coated nanochannels showed a lower peptide sample adsorption and robust efficiency under a wide range of buffer pHs. The system described here can potentially be used for the preconcentration of cationic peptides/proteins on microfluidic devices for subsequent analyses. PMID:24733115

  14. Seasonal and annual variations in the potentiometric surface of the Floridan Aquifer in Duval County, Florida, 1960-77

    USGS Publications Warehouse

    Leve, Gilbert W.

    1980-01-01

    Potentiometric levels of the Floridan aquifer in Duval County, Fla., are constantly changing in response to gains of water to the aquifer, primarily by recharge from rainfall; and losses from the aquifer, primarily by withdrawals from hundreds of wells. Seasonal variations of the potentiometric level in one well at Jacksonville was 4.2 feet during 1976. During the 18 year period from 1960 to 1977 the mean annual decline of potentiometric levels in the county was about 8 feet because of a large increase in withdrawals and to a lesser extent a decline in average annual rainfall in recharge areas. Maps of the potentiometric surface in 1960 and 1977 indicate that the greatest decline was more than 20 feet in the south-central part of the county. The decline was less than 5 feet in the western part of the county. (Kosco-USGS)

  15. Hyperbranched cationic amylopectin derivatives for gene delivery.

    PubMed

    Zhou, Yanfang; Yang, Bin; Ren, Xianyue; Liu, Zhenzhen; Deng, Zheng; Chen, Luming; Deng, Yubin; Zhang, Li-Ming; Yang, Liqun

    2012-06-01

    A series of hyperbranched cationic amylopectin derivatives conjugated with 1,2-ethylenediamine, diethylenetriamine and 3-(dimethylamino)-1-propylamine residues, named as EDA-Amp, DETA-Amp and DMAPA-Amp, were synthesized by the N,N'-carbonyldiimidazole activation method at room temperature. Their structures were characterized by FTIR and (1)H NMR analyses, and their buffering capability was assessed by acid-base titration. The amylopectin derivatives exhibited better blood compatibility and lower cytotoxicity when compared to branched polyethyleneimine (bPEI) in the hemolysis and MTT assays. Atomic force microscopy and optical microscopy confirmed that the amylopectin derivatives exhibited lower damage for erythrocytes than bPEI. The amylopectin derivatives could bind and condense plasmid DNA (pDNA) to form the complexes with the size ranging from 100 to 300 nm. The resultant complexes showed higher transfection efficiency in 293T cells than in A549 cells. The DMAPA-Amp derivative-mediated gene transfection for Forkhead box O1 exhibited higher protein expression than that of the EDA-Amp and DETA-Amp derivatives in 293T cells, which was analyzed by western blot, flow cytometry and Hoechst staining assay. On the basis of these data, amylopectin derivatives exhibit potential as nonviral gene vectors. PMID:22445252

  16. 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

  17. SSB Binding to ssDNA Using Isothermal Titration Calorimetry

    PubMed Central

    Kozlov, Alexander G.; Lohman, Timothy M.

    2015-01-01

    Isothermal titration calorimetry (ITC) is a powerful method for studying protein–DNA interactions in solution. As long as binding is accompanied by an appreciable enthalpy change, ITC studies can yield quantitative information on stoichiometries, binding energetics (affinity, binding enthalpy and entropy) and potential site–site interactions (cooperativity). This can provide a full thermodynamic description of an interacting system which is necessary to understand the stability and specificity of protein–DNA interactions and to correlate the activities or functions of different species. Here we describe procedures to perform and analyze ITC studies using as examples, the E. coli SSB (homotetramer with 4 OB-folds) and D. radiodurans SSB (homodimer with 4 OB-folds). For oligomeric protein systems such as these, we emphasize the need to be aware of the likelihood that solution conditions will influence not only the affinity and enthalpy of binding but also the mode by which the SSB oligomer binds ssDNA. PMID:22976176

  18. Isothermal titration calorimetry study of epicatechin binding to serum albumin.

    PubMed

    Frazier, Richard A; Papadopoulou, Athina; Green, Rebecca J

    2006-08-28

    The interaction of epicatechin with bovine serum albumin (BSA) was studied by isothermal titration calorimetry. The binding constant (K) and associated thermodynamic binding parameters (n, DeltaH) were determined for the interaction at three solution concentrations of BSA using a binding model assuming independent binding sites. These data show weak non-covalent binding of epicatechin to BSA. The interaction energetics varied with BSA concentration in the calorimeter cell, suggesting that the binding of epicatechin induced BSA aggregation. The free energy (DeltaG) remained constant within a range of 2 kJ mol(-1) and negative entropy was observed, indicating an enthalpy driven exothermic interaction. It is concluded that the non-covalent epicatechin-BSA complex is formed by hydrogen bonding. PMID:16522360

  19. Ultrasensitivity by Molecular Titration in Spatially Propagating Enzymatic Reactions

    PubMed Central

    Semenov, Sergey N.; Markvoort, Albert J.; Gevers, Wouter B.L.; Piruska, Aigars; de Greef, Tom F.A.; Huck, Wilhelm T.S.

    2013-01-01

    Delineating design principles of biological systems by reconstitution of purified components offers a platform to gauge the influence of critical physicochemical parameters on minimal biological systems of reduced complexity. Here we unravel the effect of strong reversible inhibitors on the spatiotemporal propagation of enzymatic reactions in a confined environment in vitro. We use micropatterned, enzyme-laden agarose gels which are stamped on polyacrylamide films containing immobilized substrates and reversible inhibitors. Quantitative fluorescence imaging combined with detailed numerical simulations of the reaction-diffusion process reveal that a shallow gradient of enzyme is converted into a steep product gradient by addition of strong inhibitors, consistent with a mathematical model of molecular titration. The results confirm that ultrasensitive and threshold effects at the molecular level can convert a graded input signal to a steep spatial response at macroscopic length scales. PMID:23972857

  20. Sailing on the "C": A Vitamin Titration with a Twist

    NASA Astrophysics Data System (ADS)

    Sowa, S.; Kondo, A. E.

    2003-05-01

    The experiment takes the traditional redox titration of vitamin C using iodine with starch as an indicator, and presents it to the student as a challenge in guided-inquiry format. Two versions, with different levels of difficulty, are provided, to accommodate students with varying levels of problem-solving skills. The "challenge" is both quantitative and qualitative: if you were an eighteenth-century sea captain packing for a voyage to the New World, would you take oranges, lemons, limes, or grapefruits to prevent your crew from getting scurvy? The challenge ties in history, nutrition, and health with chemistry, and provides students an opportunity to work with familiar food products in the laboratory.

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

    PubMed

    Burakowski, Andrzej; Gli?ski, Jacek

    2014-01-01

    Classical acoustic acid-base titration was monitored using sound speed and density measurements. Plots of these parameters, as well as of the adiabatic compressibility coefficient calculated from them, exhibit changes with the volume of added titrant. Compressibility changes can be explained and quantitatively predicted theoretically in terms of Pasynski theory of non-compressible hydrates combined with that of the additivity of the hydration numbers with the amount and type of ions and molecules present in solution. It also seems that this development could be applied in chemical engineering for monitoring the course of chemical processes, since the applied experimental methods can be carried out almost independently on the medium under test (harmful, aggressive, etc.). PMID:25109640

  2. Coulometric Karl Fischer titration simplifies water content testing

    SciTech Connect

    Poynter, W.G. ); Barrios, R.J. )

    1994-04-11

    The well-known Karl Fischer method for analyzing water content of nonaqueous samples has been modified to facilitate field use. The conventional, visual-endpoint filtration has been altered to produce a coulometric, or electrochemical, procedure. The coulometric method has all the advantages of the original karl Fischer laboratory method, but can be packaged in a small, convenient module. The analysis takes little time and can be used in the field as well as the laboratory. The relatively new coulometric method is described in API Manual of Petroleum Measurement Standards (MPMS) Chapter 10.9 and in ASTM D 4928. The titration is gaining increasing acceptance in the petroleum industry, where it is used by production engineers, transporters, and processors. The paper describes this method.

  3. Development and certification of an automated differential titration photocalorimeter

    NASA Astrophysics Data System (ADS)

    Gubarev, Yu. A.; Lebedeva, N. Sh.; V'yugin, A. I.; Golubev, S. N.

    2015-04-01

    An automated differential titration photocalorimeter (ADTPC) has been designed for investigating photoinduced processes. This instrument provides means to record thermal and spectral (absorbance) changes in a calorimetric cell. Metrological characteristics of the described ADTPC are detection limit, 0.001 J with a reproducibility of 0.0002 J or better; short-duration noise level, ±5 rel. units; long-duration noise level, ±29 rel. units. ADTPC has been certified against the heats of mixing of solvents and the heat of neutralization reaction between tris(hydroxymethyl)aminomethane and HCl. The photocalorimetric unit of the device has additionally been certified against the heat of photolysis of K3[Fe(C2O4)3] and the heat of isomerization of azobenzene in heptane. Within the claimed errors, the heats measured with ADTPC are in agreement with the values recommended for the above systems.

  4. Solubility of strontium-substituted apatite by solid titration.

    PubMed

    Pan, H B; Li, Z Y; Lam, W M; Wong, J C; Darvell, B W; Luk, K D K; Lu, W W

    2009-06-01

    Solid titration was used to explore the solubility isotherms of partially (Srx-HAp, x=1, 5, 10, 40, 60 mol.%) and fully substituted strontium hydroxyapatite (Sr-HAp). Solubility increased with increasing strontium content. No phase other than strontium-substituted HAp, corresponding to the original titrant, was detected in the solid present at equilibrium; in particular, dicalcium hydrogen phosphate was not detected at low pH. The increase in solubility with strontium content is interpreted as a destabilization of the crystal structure by the larger strontium ion. Carbonated HAp was formed in simulated body fluid containing carbonate on seeding with Sr10-HAp, but the precipitate was strontium-substituted on seeding with Sr-HAp. Strontium-substituted HAp might be usable as a template for the growth of new bone, since nucleation appears to be facilitated. PMID:19135423

  5. 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. PMID:26227041

  6. Isothermal Titration Calorimetry for Measuring Macromolecule-Ligand Affinity

    PubMed Central

    Duff,, Michael R.; Grubbs, Jordan; Howell, Elizabeth E.

    2011-01-01

    Isothermal titration calorimetry (ITC) is a useful tool for understanding the complete thermodynamic picture of a binding reaction. In biological sciences, macromolecular interactions are essential in understanding the machinery of the cell. Experimental conditions, such as buffer and temperature, can be tailored to the particular binding system being studied. However, careful planning is needed since certain ligand and macromolecule concentration ranges are necessary to obtain useful data. Concentrations of the macromolecule and ligand need to be accurately determined for reliable results. Care also needs to be taken when preparing the samples as impurities can significantly affect the experiment. When ITC experiments, along with controls, are performed properly, useful binding information, such as the stoichiometry, affinity and enthalpy, are obtained. By running additional experiments under different buffer or temperature conditions, more detailed information can be obtained about the system. A protocol for the basic setup of an ITC experiment is given. PMID:21931288

  7. Novel approaches to analysis by flow injection gradient titration.

    PubMed

    Wójtowicz, Marzena; Kozak, Joanna; Ko?cielniak, Pawe?

    2007-09-26

    Two novel procedures for flow injection gradient titration with the use of a single stock standard solution are proposed. In the multi-point single-line (MP-SL) method the calibration graph is constructed on the basis of a set of standard solutions, which are generated in a standard reservoir and subsequently injected into the titrant. According to the single-point multi-line (SP-ML) procedure the standard solution and a sample are injected into the titrant stream from four loops of different capacities, hence four calibration graphs are able to be constructed and the analytical result is calculated on the basis of a generalized slope of these graphs. Both approaches have been tested on the example of spectrophotometric acid-base titration of hydrochloric and acetic acids with using bromothymol blue and phenolphthalein as indicators, respectively, and sodium hydroxide as a titrant. Under optimized experimental conditions the analytical results of precision less than 1.8 and 2.5% (RSD) and of accuracy less than 3.0 and 5.4% (relative error (RE)) were obtained for MP-SL and SP-ML procedures, respectively, in ranges of 0.0031-0.0631 mol L(-1) for samples of hydrochloric acid and of 0.1680-1.7600 mol L(-1) for samples of acetic acid. The feasibility of both methods was illustrated by applying them to the total acidity determination in vinegar samples with precision lower than 0.5 and 2.9% (RSD) for MP-SL and SP-ML procedures, respectively. PMID:17903467

  8. 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.

  9. 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.

  10. 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.

  11. Approximate potentiometric surface of the bedrock aquifer at Great Bay, southeastern New Hampshire, 2001

    USGS Publications Warehouse

    Roseen, Robert M.; Degnan, J.R.; Brannaka, L.K.; Ballestero, T.P.; Mack, T.J.

    2003-01-01

    Ground-water elevations (heads) in 265 wells were used to map the potentiometric-head surface in the fractured-bedrock aquifer adjacent to Great Bay, N.H. Remotely sensed data, spring-water temperatures and specific conductances, land-surface elevations, and simulated heads were also used to guide construction of the potentiometric surface. Heads in the bedrock aquifer locally varied more than 20 ft (feet) between adjacent wells as little as 200 ft apart. The depth to water below land surface was greater on the western and northwestern sides of the bay (about 20 ft) than on the southern and eastern sides (about 8 ft). Topography has a greater effect on heads than does temporal variation or measurement accuracy. Head gradients are steeper at the southern side of Great Bay, where the topographic relief is greatest, than at the northwestern and northeastern sides.

  12. Potentiometric measurements in sequential injection analysis lab-on-valve (SIA-LOV) flow-system.

    PubMed

    Kikas, Timo; Ivaska, Ari

    2007-01-15

    Advantages of using sequential injection analysis lab-on-valve (SIA-LOV) in potentiometric measurements are studied with Ca(2+) sensitive solid-contact ion-selective electrodes (SC-ISE) and pH electrode based on polyaniline (PANI). Experiments show that Ca(2+)-SC-ISE requires a stopped flow mode to be used in order to get longer equilibration time. On the other hand, PANI based pH electrode gives better results under flow conditions. SIA-LOV was found to be a flexible solution handling system for potentiometric measurements. The technique gives a possibility to fine-tune the calibration range or even recondition the electrode before every measurement without losing in linear range of calibration. PMID:19071283

  13. 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.

  14. Detection of high-charge density polyanion contaminants in biomedical heparin preparations using potentiometric polyanion sensors.

    PubMed

    Wang, Lin; Buchanan, Stacey; Meyerhoff, Mark E

    2008-12-15

    A very simple and inexpensive method to detect oversulfated chondroitin sulfate (OSCS) or other high-charge density polyanionic structures as contaminants in heparin products using potentiometric polyanion sensors is described. In the potentiometric measurement, a greater change in the phase boundary equilibrium potential of polymeric membranes formulated with tridodecylmethylammonium (TDMA) anion exchange sites is observed for the contaminated heparin than for the untainted heparin due to the higher charge density of OSCS or other impurities compared to that of porcine heparin. Detection of 0.5 wt % OSCS impurity is readily achieved using only 1 mg/mL of final polyion concentration. Even lower detection limits for OSCS contamination may be possible if higher final concentrations of heparin preparations can be employed in the test procedure. PMID:19007240

  15. 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.

  16. 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. PMID:25852356

  17. 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)

  18. Maltodextrins as new chiral selectors in the design of potentiometric, enantioselective membrane electrodes.

    PubMed

    Stefan, R I; van Staden, J F; Aboul-Enein, H Y

    2001-05-01

    Maltodextrins (dextrose equivalent (DE) 4.0-7.0, 13.0-17.0, and 16.5-19.5) are proposed as novel chiral selectors for the construction of potentiometric, enantioselective membrane electrodes. The potentiometric, enantioselective membrane electrodes can be used reliably for the assay of S-captopril as raw material and in pharmaceutical formulations such as Novocaptopril tablets, by use of direct potentiometry. The best response was obtained when maltodextrin with higher DE was used for construction of the electrode. The best enantioselectivity and time-stability was achieved for the lower DE maltodextrin. L-proline was found to be the main interferent for all the proposed electrodes. The surface of the electrodes can be regenerated by simply polishing; this furnishes a fresh surface ready for use in a new assay. PMID:11393233

  19. The use of isothermal titration calorimetry and molecular dynamics to show variability in DNA transfection performance.

    PubMed

    Samsonova, Olga; Glinca, Serghei; Biela, Adam; Pfeiffer, Christian; Dayyoub, Eyas; Sahin, Damla; Klebe, Gerhard; Kissel, Thomas

    2013-02-01

    The mechanism causing variability in DNA transfection efficacy for low-molecular-weight pDMAEMA (poly(2-(dimethylamino)ethyl methacrylate) and pDMAEMA-b-pHEMA (poly(2-(dimethyl amino)ethylmethacrylate)-block-poly(2-hydroxyl methacrylate)) has so far remained unclear, apart from the evidence of beneficial effects of the pHEMA grafting. This study has explicitly characterized the electrostatically driven self-assembly process of linear polymethacrylate polymers with DNA-generating nanocarriers for efficient gene transfection. Isothermal titration calorimetry (ITC) showed clear differences in binding-heat profiles of homo-polycationic and pHEMA grafted polymers with DNA. Polyethylene imine, a branched polycationic polymer of 25kDa with high transfection potential that has previously been successfully used in transfection experiments, demonstrated a heat flow profile that was partly identical to pDMAEMA-b-pHEMA. Computational molecular dynamics (MD) simulated the folding process of polymer in water from a linear to a coiled state: homo-pDMAEMA and pHEMA grafts reduced their overall positive charge accessibility upon folding, down to 45% and 63%, respectively. The homo-pDMAEMA formed the globular conformation more preferably than pHEMA grafts, thus impeding electrostatic interaction with DNA. These findings substantiate the known disadvantage of low-molecular-weight linear polymers compared to higher-molecular-weight polymers in transfection performance; here we have disclosed the ability of a non-cationic chain elongation to be beneficial for the self-assembly process. The combination of MD and ITC has proved to be a suitable approach for carrier-payload interaction studies and may be used to predict the efficacy of a polymer as a nanocarrier from the flexibility of its structure. PMID:23059414

  20. 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). PMID:4091553

  1. 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.

  2. 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

  3. 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

  4. 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.

  5. Man-tailored biomimetic sensor of molecularly imprinted materials for the potentiometric measurement of oxytetracycline.

    PubMed

    Moreira, Felismina T C; Kamel, Ayman H; Guerreiro, Joana R L; Sales, M Goreti F

    2010-10-15

    A novel biomimetic sensor for the potentiometric transduction of oxytetracycline is presented. The artificial host was imprinted in methacrylic acid and/or acrylamide based polymers. Different amounts of molecularly imprinted and non-imprinted polymers were dispersed in different plasticizing solvents and entrapped in a poly(vinyl chloride) matrix. Only molecularly imprinted based sensors allowed a potentiometric transduction, suggesting the existence of host-guest interactions. These sensors exhibited a near-Nernstian response in steady state evaluations; slopes and detection limits ranged 42-63 mV/decade and 2.5-31.3 μg/mL, respectively. Sensors were independent from the pH of test solutions within 2-5. Good selectivity was observed towards glycine, ciprofloxacin, creatinine, acid nalidixic, sulfadiazine, cysteine, hydroxylamine and lactose. In flowing media, the biomimetic sensors presented good reproducibility (RSD of ±0.7%), fast response, good sensitivity (65 mV/decade), wide linear range (5.0×10(-5) to 1.0×10(-2) mol/L), low detection limit (19.8 μg/mL), and a stable baseline for a 5×10(-3) M citrate buffer (pH 2.5) carrier. The sensors were successfully applied to the analysis of drugs and urine. This work confirms the possibility of using molecularly imprinted polymers as ionophores for organic ion recognition in potentiometric transduction. PMID:20688507

  6. 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. PMID:24333582

  7. 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. PMID:25516367

  8. Surface cationized cellulose nanofibrils for the production of contact active antimicrobial surfaces.

    PubMed

    Saini, Seema; Yücel Falco, Çi?dem; 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

  9. Analysis of chromite by cation-exchange using ethylenediaminetetra-acetic acid.

    PubMed

    Jawaid, M; Ingman, F

    1975-12-01

    A method for the separation and determination of five major elements in chromite ore (and chrome-bearing refractories), based on complexation of the metals with EDTA is described. After removal of silica, the cations are separated into two groups by passing the solution through a cation-exchange resin (Dowex 50W-X8, in Na-form) in the presence of an excess of the complexing agent. The optimum conditions for the separation are discussed on the basis of exchange constants that were either known or determined. The first group contains Cr and Fe, which emerge in the filtrate at pH between 1.5 and 2.1, whereas A1, Mg and Ca, which are adsorbed on the resin, form another group. Complexometric titrations are used for the subsequent determination of the cations in each group. The method is simpler and more rapid and accurate for routine analysis than the current methods. PMID:18961783

  10. Binding of cationic surfactants to a thermo-sensitive copolymer below and above its cloud point.

    PubMed

    Peng, Baoliang; Han, Xia; Liu, Honglai; Tam, Kam C

    2013-12-15

    The binding interactions between cationic surfactants and a statistical thermo-sensitive copolymer based on oligo(ethylene glycol) methacrylates were studied by isothermal titration calorimetry (ITC), surfactant selective electrode (SSE) and dynamic light scattering (DLS). Strong binding interactions were observed between this copolymer and cationic surfactants. The binding is driven by the hydrophobic effect, occurring on the hydrophobic backbone instead of the ethylene-glycol side chains. The surfactant saturation concentration C2 depended on the polymer concentration, but was not affected by temperature. Three types of cationic alkyltrimethylammonium bromide surfactants (RTAB with R equal to C12, C14, and C16), namely, dodecyltrimethylammonium bromide (DoTAB), tetradecyltrimethylammonium bromide (TTAB), and cetyltrimethylammonium bromide (CTAB), were examined, and the results confirmed that the binding affinity followed the sequence: CTAB>TTAB>DoTAB. PMID:24144369

  11. A Laser-Pointer-Based Spectrometer for Endpoint Detection of EDTA Titrations

    ERIC Educational Resources Information Center

    Dahm, Christopher E.; Hall, James W.; Mattioni, Brian E.

    2004-01-01

    A laser spectrometer for the ethylenediaminetetra-acetic acid (EDTA) titration of magnesium or calcium ions that is designed around a handheld laser pointer as the source and a photoresistor as the detector is developed. Findings show that the use of the spectrometer reduces the degree of uncertainty and error in one part of the EDTA titrations,…

  12. Effects of Acute and Chronic Cocaine Administration on Titrating-Delay Matching-to-Sample Performance

    ERIC Educational Resources Information Center

    Kangas, Brian D.; Branch, Marc N.

    2012-01-01

    The effects of cocaine were examined under a titrating-delay matching-to-sample procedure. In this procedure, the delay between sample stimulus offset and comparison stimuli onset adjusts as a function of the subject's performance. Specifically, matches increase the delay and mismatches decrease the delay. Titrated delay values served as the…

  13. A Laser-Pointer-Based Spectrometer for Endpoint Detection of EDTA Titrations

    ERIC Educational Resources Information Center

    Dahm, Christopher E.; Hall, James W.; Mattioni, Brian E.

    2004-01-01

    A laser spectrometer for the ethylenediaminetetra-acetic acid (EDTA) titration of magnesium or calcium ions that is designed around a handheld laser pointer as the source and a photoresistor as the detector is developed. Findings show that the use of the spectrometer reduces the degree of uncertainty and error in one part of the EDTA titrations

  14. Effects of Acute and Chronic Cocaine Administration on Titrating-Delay Matching-to-Sample Performance

    ERIC Educational Resources Information Center

    Kangas, Brian D.; Branch, Marc N.

    2012-01-01

    The effects of cocaine were examined under a titrating-delay matching-to-sample procedure. In this procedure, the delay between sample stimulus offset and comparison stimuli onset adjusts as a function of the subject's performance. Specifically, matches increase the delay and mismatches decrease the delay. Titrated delay values served as the…

  15. Feasibility Study of Rapid Opioid Rotation and Titration

    PubMed Central

    Korkmazsky, Marina; Ghandehari, Javid; Sanchez, Angela; Lin, Hung-Mo; Pappagallo, Marco

    2011-01-01

    Background Opioid guidelines recommend opioid rotation and switching for patients who do not achieve adequate pain relief or who experience intolerable adverse events (AEs) with their current opioid. However, specific recommendations and protocols for opioid rotation are lacking, making the practice time consuming and difficult for primary care physicians to accomplish independently or coordinate with a pain specialist. Objectives To assess the safety and feasibility of using 24-hour intravenous patient-controlled analgesia (IV-PCA) to achieve rapid opioid rotation and titration (RORT). Study design Open-label pilot study. Setting Hospital research center. Methods At admission, patients (aged ? 18 years) with treatment-refractory chronic pain who were taking morphine or oxycodone for ? 3 months and had pain scores ? 4 on a 10-point scale, underwent opioid rotation to oral oxymorphone extended release (ER). They also received IV-PCA oxymorphone for 24 hours as needed. At discharge, the participants were taking oral oxymorphone ER with oxymorphone immediate release (IR) as needed based on their total 24-hour oral plus IV-PCA oxymorphone use. During a 2-week follow-up, their oxymorphone usage was titrated as needed. Main outcome measures were AEs, Patient Global Impression of Change (PGIC), Brief Pain Inventory (0 = no pain/interference, 10 = worst pain/complete interference), treatment satisfaction, and change in oxymorphone dose. Results Twelve patients enrolled and completed the 24-hour IV-PCA; 10 completed the 2-week follow-up post-24-hour IV-PCA. PGIC status improved by 12 hours (odds ratio [OR], 0.19, 95% CI, 0.08–0.44; P < 0.001), and both PGIC status and activity scores improved by 24 hours (OR, 0.23, 95% CI, 0.09–0.55; P = 0.001; OR, 0.49, 95% CI, 0.25–0.96; P = 0.04, respectively) and 2 weeks (OR, 0.14, 95% CI, 0.04–0.46; P = 0.001; OR, 0.21, 95% CI, 0.06–0.72; P = 0.01) versus 6 hours. During the 24-hour IV-PCA time period, 6 of 10 patients accomplished ? 50% of their overall dose titration. At 2 weeks, 8 of 10 participants were Greatly Satisfied or Somewhat Satisfied with the overall RORT procedure. RORT was well tolerated, with no serious AEs. Limitations This was a pilot open-label study in a small number of participants. A larger randomized study with long-term follow-up and comparison to traditional protocols is necessary. Conclusions Preliminary data suggest that RORT can be performed safely and effectively by incorporating IV-PCA during the first 24 hours. Further investigations are needed to determine whether RORT can become an ambulatory treatment intervention in pain practice. PMID:21267044

  16. 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.

  17. 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 year to show the approximate annual low and high water-level conditions, respectively. Most of the water-level data for this map were collected by the U.S. Geological Survey during the period September 15-19, 2008. Supplemental water-level data were collected by other agencies and companies. A corresponding potentiometric-surface map was prepared for areas east and north of the Southwest Florida Water Management District boundary by the U.S. Geological Survey office in Orlando, Florida (Kinnaman and Dixon, 2009). Most water-level measurements were made during a 5-day period; therefore, measurements do not represent a 'snapshot' of conditions at a specific time, nor do they necessarily coincide with the seasonal high water-level condition.

  18. 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 approximate annual low and high water-level conditions, respectively. Most of the water-level data for this map were collected by the U.S. Geological Survey during the period May 18-22, 2009. Supplemental water-level data were collected by other agencies and companies. A corresponding potentiometric-surface map was prepared for areas east and north of the Southwest Florida Water Management District boundary by the U.S. Geological Survey office in Orlando, Florida (Kinnaman and Dixon, 2009). Most water-level measurements were made during a 5-day period; therefore, measurements do not represent a 'snapshot' of conditions at a specific time, nor do they necessarily coincide with the seasonal low water-level condition. The potentiometric contours are generalized to synoptically portray the head in a dynamic hydrologic system, taking due account of the variations in hydrogeologic conditions, such as differing depths of wells, nonsimultaneous measurements of water levels, variable effects of pumping, and changing climatic influence. The potentiometric contours may not conform exactly with the individual measurements of water levels.

  19. Alkaline titrations of poly(dG-dC).poly(dG-dC): microemulsion versus solution behavior.

    PubMed

    Airoldi, Marta; Gennaro, Giuseppe; Giomini, Marcello; Giuliani, Anna Maria; Giustini, Mauro

    2007-06-01

    PolyGC was titrated with a strong base in the presence of increasing concentrations of NaCl (from 0.00 to 0.60M) either in water solution or with the polynucleotide solubilized in the aqueous core of reverse micelles, i.e., the cationic quaternary water-in-oil microemulsion CTAB/n-hexane/n-pentanol/water. The results for matched samples in the two media were compared. CD and UV spectroscopies and, for the solution experiments, pH measurements were used to follow the course of deprotonation. In both media the primary effect of the addition of base was denaturation of the polynucleotide, reversible by back-titration with a strong acid. In solution, the apparent pK(a) of the transition decreases with increasing the salt concentration and a roughly linear dependence of pK(a) on p[NaCl] has been found. A parallel monotonic decay with ionic strength has been found in solution for R(OH), defined as the number of hydroxyl ions required per monomeric unit of polyGC to reach half-transition. By contrast, in microemulsion, R(OH) has been found to be independent of the NaCl concentration (and 10 to 50 times lower than in solution). This result is proposed as an indirect evidence of the independence of pK(a) on the salt concentration in microemulsion, where the pH cannot be measured. A sort of buffering effect of the positive charges on the micellar wall and of their counter-ions on the ionic strength could well explain this discrepancy of behavior in the two media. PMID:17508778

  20. Probing lectin-mucin interactions by isothermal titration microcalorimetry.

    PubMed

    Dam, Tarun K; Brewer, C Fred

    2015-01-01

    Isothermal titration microcalorimetry (ITC) can directly determine the thermodynamic binding parameters of biological molecules including affinity constant, binding stoichiometry, and heat of binding (enthalpy) and indirectly the entropy and free energy of binding. ITC has been extensively used to study the binding of lectins to mono- and oligosaccharides, but limited applications to lectin-glycoprotein interactions. Inherent experimental challenges to ITC include sample precipitation during the experiment and relative high amount of sample required, but careful design of experiments can minimize these problems and allow valuable information to be obtained. For example, the thermodynamics of binding of lectins to multivalent globular and linear glycoproteins (mucins) have been described. The results are consistent with a dynamic binding mechanism in which lectins bind and jump from carbohydrate to carbohydrate epitope in these molecules leading to increased affinity. Importantly, the mechanism of binding of lectins to mucins appears similar to that for a variety of protein ligands binding to DNA. Recent results also show that high affinity lectin-mucin cross-linking interactions are driven by favorable entropy of binding that is associated with the bind and jump mechanism. The results suggest that the binding of ligands to biopolymers, in general, may involve a common mechanism that involves enhanced entropic effects that facilitate binding interactions. PMID:25253134

  1. Hot biological catalysis: isothermal titration calorimetry to characterize enzymatic reactions.

    PubMed

    Mazzei, Luca; Ciurli, Stefano; Zambelli, Barbara

    2014-01-01

    Isothermal titration calorimetry (ITC) is a well-described technique that measures the heat released or absorbed during a chemical reaction, using it as an intrinsic probe to characterize virtually every chemical process. Nowadays, this technique is extensively applied to determine thermodynamic parameters of biomolecular binding equilibria. In addition, ITC has been demonstrated to be able of directly measuring kinetics and thermodynamic parameters (kcat, KM, ?H) of enzymatic reactions, even though this application is still underexploited. As heat changes spontaneously occur during enzymatic catalysis, ITC does not require any modification or labeling of the system under analysis and can be performed in solution. Moreover, the method needs little amount of material. These properties make ITC an invaluable, powerful and unique tool to study enzyme kinetics in several applications, such as, for example, drug discovery. In this work an experimental ITC-based method to quantify kinetics and thermodynamics of enzymatic reactions is thoroughly described. This method is applied to determine kcat and KM of the enzymatic hydrolysis of urea by Canavalia ensiformis (jack bean) urease. Calculation of intrinsic molar enthalpy (?Hint) of the reaction is performed. The values thus obtained are consistent with previous data reported in literature, demonstrating the reliability of the methodology. PMID:24747990

  2. New chemical titration proposed for potassium mud testing

    SciTech Connect

    Zilch, H.E.

    1984-01-01

    An accurate and easy-to-use procedure for measuring the potassium ion concentration in drilling and completion fluids has been developed and successfully used in Union Oil Co. of California's drilling operations. This volumetric analysis is based on the quantitative conversion of soluble sodium tetraphenylboron to the insoluble potassium tetraphenylboron and back titration with a quaternary ammonium salt in the presence of Titan yellow (Clayton yellow) indicator. This gives an easy-to-read color change endpoint from milky white to intense pink. The procedure described here is as fast as flame emission analysis and as accurate as the gravimetric analysis. This method has been used for several years in the fertilizer industry with success, but is new to drilling operations, at least in this revised form. This method, adapted from the potash industry, is easier and more accurate than other methods. Results compare favorably (within 3%) with flame emision or atomic absorption methods. The NaTPB method is proposed as a replacement for the method described in API RP 13B.

  3. Colorimetric nanoplasmonic assay to determine purity and titrate extracellular vesicles.

    PubMed

    Maiolo, Daniele; Paolini, Lucia; Di Noto, Giuseppe; Zendrini, Andrea; Berti, Debora; Bergese, Paolo; Ricotta, Doris

    2015-04-21

    Extracellular Vesicles (EVs) - cell secreted vesicles that carry rich molecular information of the parental cell and constitute an important mode of intercellular communication - are becoming a primary topic in translational medicine. EVs (that comprise exosomes and microvesicles/microparticles) have a size ranging from 40 nm to 1 ?m and share several physicochemical proprieties, including size, density, surface charge, and light interaction, with other nano-objects present in body fluids, such as single and aggregated proteins. This makes separation, titration, and characterization of EVs challenging and time-consuming. Here we present a cost-effective and fast colorimetric assay for probing by eye protein contaminants and determine the concentration of EV preparations, which exploits the synergy between colloidal gold nanoplasmonics, nanoparticle-protein corona, and nanoparticle-membrane interaction. The assay hits a limit of detection of protein contaminants of 5 ng/?L and has a dynamic range of EV concentration ranging from 35 fM to 35 pM, which matches the typical range of EV concentration in body fluids. This work provides the first example of the exploitation of the nanoparticle-protein corona in analytical chemistry. PMID:25674701

  4. Mapping glycoside hydrolase substrate subsites by isothermal titration calorimetry

    PubMed Central

    Zolotnitsky, Gennady; Cogan, Uri; Adir, Noam; Solomon, Vered; Shoham, Gil; Shoham, Yuval

    2004-01-01

    Relating thermodynamic parameters to structural and biochemical data allows a better understanding of substrate binding and its contribution to catalysis. The analysis of the binding of carbohydrates to proteins or enzymes is a special challenge because of the multiple interactions and forces involved. Isothermal titration calorimetry (ITC) provides a direct measure of binding enthalpy (?Ha) and allows the determination of the binding constant (free energy), entropy, and stoichiometry. In this study, we used ITC to elucidate the binding thermodynamics of xylosaccharides for two xylanases of family 10 isolated from Geobacillus stearothermophilus T-6. The change in the heat capacity of binding (?Cp = ?H/?T) for xylosaccharides differing in one sugar unit was determined by using ITC measurements at different temperatures. Because hydrophobic stacking interactions are associated with negative ?Cp, the data allow us to predict the substrate binding preference in the binding subsites based on the crystal structure of the enzyme. The proposed positional binding preference was consistent with mutants lacking aromatic binding residues at different subsites and was also supported by tryptophan fluorescence analysis. PMID:15277671

  5. Isothermal titration calorimetry in nanoliter droplets with subsecond time constants.

    PubMed

    Lubbers, Brad; Baudenbacher, Franz

    2011-10-15

    We reduced the reaction volume in microfabricated suspended-membrane titration calorimeters to nanoliter droplets and improved the sensitivities to below a nanowatt with time constants of around 100 ms. The device performance was characterized using exothermic acid-base neutralizations and a detailed numerical model. The finite element based numerical model allowed us to determine the sensitivities within 1% and the temporal dynamics of the temperature rise in neutralization reactions as a function of droplet size. The model was used to determine the optimum calorimeter design (membrane size and thickness, junction area, and thermopile thickness) and sensitivities for sample volumes of 1 nL for silicon nitride and polymer membranes. We obtained a maximum sensitivity of 153 pW/(Hz)(1/2) for a 1 ?m SiN membrane and 79 pW/(Hz)(1/2) for a 1 ?m polymer membrane. The time constant of the calorimeter system was determined experimentally using a pulsed laser to increase the temperature of nanoliter sample volumes. For a 2.5 nanoliter sample volume, we experimentally determined a noise equivalent power of 500 pW/(Hz)(1/2) and a 1/e time constant of 110 ms for a modified commercially available infrared sensor with a thin-film thermopile. Furthermore, we demonstrated detection of 1.4 nJ reaction energies from injection of 25 pL of 1 mM HCl into a 2.5 nL droplet of 1 mM NaOH. PMID:21913688

  6. On the physical meaning of the isothermal titration calorimetry measurements in calorimeters with full cells.

    PubMed

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

    2009-12-01

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

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

    PubMed Central

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

    2009-01-01

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

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

    SciTech Connect

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

    1991-01-01

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

  9. 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.

  10. Potentiometric surface of the upper Cape Fear Aquifer in the central coastal plain of North Carolina, December 1986

    USGS Publications Warehouse

    Winner, M.D., Jr.; 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.

  11. 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)

  12. Isothermal titration calorimetric analysis on solubilization of an octane oil-in-water emulsion in surfactant micelles and surfactant-anionic polymer complexes.

    PubMed

    Zhang, Hui; Zeeb, Benjamin; Salminen, Hanna; Weiss, Jochen

    2015-01-15

    Polymers may alter the ability of surfactant micelles to solubilize hydrophobic molecules depending on surfactant-polymer interactions. In this study, isothermal titration calorimetry (ITC) was used to investigate the solubilization thermodynamics of an octane oil-in-water emulsion in anionic sodium dodecylsulphate (SDS), nonionic polyoxyethylene sorbitan monooleate (Tween 80), cationic cetyltrimethylammonium bromide (CTAB) surfactant micelles and respective complexes formed by these micelles and an anionic polymer (carboxymethyl cellulose). Results indicated that the oil solubilization in single ionic micelles was endothermic, while in nonionic micelles or mixed ionic/nonionic micelles it was exothermic. The addition of carboxymethyl cellulose did not influence the solubilization behavior in these micelles, but affected the solubilization capacities of these systems. The solubilization capacity of cationic micelles or mixed cationic/nonionic micelles was enhanced while that of nonionic or anionic micelles was decreased. Based on the phase separation model, a molecular pathway mechanism driven by enthalpy was proposed for octane solubilization in surfactant micelles and surfactant-polymer complexes. PMID:25454419

  13. Underground Test Area Subproject Phase I Data Analysis Task. Volume II - Potentiometric Data Document Package

    SciTech Connect

    1996-12-01

    Volume II of the documentation for the Phase I Data Analysis Task performed in support of the current Regional Flow Model, Transport Model, and Risk Assessment for the Nevada Test Site Underground Test Area Subproject contains the potentiometric data. Because of the size and complexity of the model area, a considerable quantity of data was collected and analyzed in support of the modeling efforts. The data analysis task was consequently broken into eight subtasks, and descriptions of each subtask's activities are contained in one of the eight volumes that comprise the Phase I Data Analysis Documentation.

  14. Potentiometric maps of the Sparta Sand, northern Louisiana and southern Arkansas, 1900, 1965, 1975, and 1980

    USGS Publications Warehouse

    Ryals, G.N.

    1980-01-01

    The potentiometric surface of the Sparta Sand in northern Louisiana is shown by contours on four maps. Maps for 1900, 1965 , and spring 1975 are generalized, small-scale maps from previously published reports. The spring 1980 map (1:500,000) is based on measurements in 144 wells and includes the southern tier of counties in southern Arkansas. The map shows regional effects of pumping from the Sparta Sand and effects of local pumping centers at Magnolia and El Dorado, Ark., and at Minden, Ruston, Jonesboro-Hodge, Winnfield, Bastrop, and in the Monroe area of Louisiana. (USGS)

  15. Potentiometric and spectrophotometric equilibrium study on Fe(III) and new catechol-bisphosphonate conjugates.

    PubMed

    Crisponi, Guido; Nurchi, Valeria Marina; Pivetta, Tiziana

    2008-02-01

    The coordination properties of mixed catechol-bisphosphonates towards Fe(III) are presented. From the potentiometric and spectroscopic results it was possible to state that iron coordination takes place only on the bisphosphonate moiety at acidic pH, and involves both catechol and bisphosphonate groups on two different iron(III) ions at higher pH values. Steric constracts keep both groups from chelating the same metal ion. Quantum mechanical calculations confirm this statement and allow to determine the minimum length of the linker for a stable conformation of complexes in which the same iron(III) ion is coordinated by both catechol and bisphosphonate. PMID:17854902

  16. Chemically fashioned ZnO nanowalls and their potential application for potentiometric cholesterol biosensor

    NASA Astrophysics Data System (ADS)

    Israr, M. Q.; Sadaf, J. R.; Nur, O.; Willander, M.; Salman, S.; Danielsson, B.

    2011-06-01

    Chemically fashioned zinc oxide (ZnO) nanowalls on aluminum wire have been characterized and utilized to fabricate a potentiometric cholesterol biosensor by an electrostatic conjugation with cholesterol oxidase. The sensitivity, specificity, reusability, and stability of the conjugated surface of ZnO nanowalls with thickness of ˜80 nm have been investigated over a wide logarithmic concentrations of cholesterol electrolyte solution ranging from 1×10-6-1×10-3 M. The presented biosensor illustrates good linear sensitivity slope curve (˜53 mV/decade) corresponding to cholesterol concentrations along with rapid output response time of ˜5 s.

  17. Potentiometric surface of the upper Floridan aquifer, west-central Florida, May 2011

    USGS Publications Warehouse

    Ortiz, Anita G.

    2011-01-01

    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 May 2011. 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 groundwater levels usually are at an annual low and withdrawals for agricultural use typically are high. The cumulative average rainfall of 45.74 inches for west-central Florida (from June 2010 through May 2011) was 6.85 inches below the historical cumulative average of 52.59 inches (Southwest Florida Water Management District, 2011). 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 from 1975 through 2010. Water-level data are collected in May and September each year to show the approximate annual low and high water-level conditions, respectively. Most of the water-level data for this map were collected by the U.S. Geological Survey during the period May 23-27, 2011. Supplemental water-level data were collected by other agencies and companies. Most water-level measurements were made during a 5-day period; therefore, measurements do not represent a "snapshot" of conditions at a specific time, nor do they necessarily coincide with the seasonal low water-level condition.

  18. Cation-cation contact pairing in water: Guanidinium

    NASA Astrophysics Data System (ADS)

    Shih, Orion; England, Alice H.; Dallinger, Gregory C.; Smith, Jacob W.; Duffey, Kaitlin C.; Cohen, Ronald C.; Prendergast, David; Saykally, Richard J.

    2013-07-01

    The formation of like-charge guanidinium-guanidinium contact ion pairs in water is evidenced and characterized by X-ray absorption spectroscopy and first-principles spectral simulations based on molecular dynamics sampling. Observed concentration-induced nitrogen K-edge resonance shifts result from ?* state mixing and the release of water molecules from each first solvation sphere as two solvated guanidinium ions associate into a stacked pair configuration. Possible biological implications of this counterintuitive cation-cation pairing are discussed.

  19. The Difference Between the Potentiometric Surfaces of the Aquia Aquifer in Southern Maryland, September 1982 and September 2007

    USGS Publications Warehouse

    Curtin, Stephen E.; Andreasen, David C.; Staley, Andrew W.

    2009-01-01

    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 2007. The map, based on water-level measurements in 53 wells, shows that the potentiometric surface during the 25-year period declined from zero in the northernmost part of the study area, which is the outcrop of the aquifer, to 117 feet at Lexington Park. Lexington Park is near the southeasternmost part of the study area and approaches the downdip boundary of the aquifer.

  20. Louisiana Ground-Water Map No.13: Hydrogeology and Potentiometric Surface of the Sparta Aquifer in Northern Louisiana, October 1996

    USGS Publications Warehouse

    Brantly, Jeffrey A.; Seanor, Ronald C.; McCoy, Kaycee L.

    2002-01-01

    This report describes the thickness and areal extent of the Sparta aquifer, identifies sands within the fresh-water extent of the aquifer, and presents data and a map that illustrate the generalized potentiometric surface (water levels) during October 1996. The report includes a detailed geophysical log, structure contour maps, hydrogeologic sections, and hydrographs of water levels in selected wells. The potentiometric surface-map can be used for determining direction of ground-water flow, hydraulic gradients, and the effects of withdrawals on the aquifer.

  1. Louisiana Ground-Water Map No. 13: Hydrogeology and Potentiometric Surface of the Sparta Aquifer in Northern Louisiana, October 1996

    USGS Publications Warehouse

    Brantly, Jeffrey A.; Seanor, Ronald C.; McCoy, Kaycee L.

    2002-01-01

    This report describes the thickness and areal extent of the Sparta aquifer, identifies sands within the fresh-water extent of the aquifer, and presents data and a map that illustrate the generalized potentiometric surface (water levels) during October 1996. The report includes a detailed geophysical log, structure contour maps, hydrogeologic sections, and hydrographs of water levels in selected wells. The potentiometric surface-map can be used for determining direction of ground-water flow, hydraulic gradients, and the effects of withdrawals on the aquifer.

  2. The Difference Between the Potentiometric Surfaces of the Upper Patapsco Aquifer in Southern Maryland, September 1990 and September 2007

    USGS Publications Warehouse

    Curtin, Stephen E.; Andreasen, David C.; Staley, Andrew W.

    2009-01-01

    This report presents a map showing the change in the potentiometric surface of the upper Patapsco aquifer in the Patapsco Formation of Early Cretaceous age in Southern Maryland for September 1990 and September 2007. The map, based on water-level measurements in 33 wells, shows that during the 17-year period, the change in the potentiometric surface ranged from zero at the edge of the outcrop area in northern Anne Arundel County to a decline of 28 feet at Crofton Meadows, 38 feet at Arnold, 36 feet at Waldorf, 35 feet at the Chalk Point power plant, and 40 feet at Lexington Park.

  3. The Difference Between the Potentiometric Surfaces of the Magothy Aquifer in Southern Maryland, September 1975 and September 2007

    USGS Publications Warehouse

    Curtin, Stephen E.; Andreasen, David C.; Staley, Andrew W.

    2009-01-01

    This report presents a map showing the change in the potentiometric surface of the Magothy aquifer in the Magothy Formation of Late Cretaceous age in Southern Maryland for September 1975 and September 2007. The map, based on water-level measurements in 51 wells, shows that during the 32-year period, the potentiometric surface had no change at the outcrop area, which is in the northernmost part of the study area, but declined 90 feet at Waldorf. Waldorf is located near the southwesternmost part of the study area, and approaches the downdip boundary of the aquifer.

  4. A Computer-Based Simulation of an Acid-Base Titration

    ERIC Educational Resources Information Center

    Boblick, John M.

    1971-01-01

    Reviews the advantages of computer simulated environments for experiments, referring in particular to acid-base titrations. Includes pre-lab instructions and a sample computer printout of a student's use of an acid-base simulation. Ten references. (PR)

  5. Going Beyond, Going Further: The Preparation of Acid-Base Titration Curves.

    ERIC Educational Resources Information Center

    McClendon, Michael

    1984-01-01

    Background information, list of materials needed, and procedures used are provided for a simple technique for generating mechanically plotted acid-base titration curves. The method is suitable for second-year high school chemistry students. (JN)

  6. The Softening of Hard Water and Complexometric Titrations. An Undergraduate Experiment

    NASA Astrophysics Data System (ADS)

    Ceretti, Helena; Hughes, Enrique A.; Zalts, Anita

    1999-10-01

    A 2-hour experiment for undergraduates is presented in which (i) water hardness is explained and demonstrated; (ii) ion-exchange resin properties are visually demonstrated and then used for softening water; (iii) complexometric titrations are used for evaluating water hardness before and after softening; and (iv) acid-base titration can be used to show that the Ca/Mg ions removed by the ion exchanger are replaced by H ions.

  7. 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. PMID:25933534

  8. Geochemical Modeling of Reactions and Partitioning of Trace Metals and Radionuclides during Titration of Contaminated Acidic Sediments

    SciTech Connect

    Zhang, Fan; Parker, Jack C.; Luo, Wensui; Spalding, Brian Patrick; Brooks, Scott C; Watson, David B; Jardine, Philip M; Gu, Baohua

    2008-01-01

    Many geochemical reactions that control aqueous metal concentrations are directly affected by solution pH. However, changes in solution pH are strongly buffered by various aqueous phase and solid phase precipitation/dissolution and adsorption/desorption reactions. The ability to predict acid-base behavior of the soil-solution system is thus critical to predict metal transport under variable pH conditions. This study was undertaken to develop a practical generic geochemical modeling approach to predict aqueous and solid phase concentrations of metals and anions during conditions of acid or base additions. The method of Spalding and Spalding was utilized to model soil buffer capacity and pH-dependent cation exchange capacity by treating aquifer solids as a polyprotic acid. To simulate the dynamic and pH-dependent anion exchange capacity, the aquifer solids were simultaneously treated as a polyprotic base controlled by mineral precipitation/dissolution reactions. An equilibrium reaction model that describes aqueous complexation, precipitation, sorption and soil buffering with pH-dependent ion exchange was developed using HydroGeoChem v5.0 (HGC5). Comparison of model results with experimental titration data of pH, Al, Ca, Mg, Sr, Mn, Ni, Co, and SO{sub 4}{sup 2-} for contaminated sediments indicated close agreement, suggesting that the model could potentially be used to predict the acid-base behavior of the sediment-solution system under variable pH conditions.

  9. Titration of strong and weak acids by sequential injection analysis technique.

    PubMed

    Maskula, S; Nyman, J; Ivaska, A

    2000-05-31

    A sequential injection analysis (SIA) titration method has been developed for acid-base titrations. Strong and weak acids in different concentration ranges have been titrated with a strong base. The method is based on sequential aspiration of an acidic sample zone and only one zone of the base into a carrier stream of distilled water. On their way to the detector, the sample and the reagent zones are partially mixed due to the dispersion and thereby the base is partially neutralised by the acid. The base zone contains the indicator. An LED-spectrophotometer is used as detector. It senses the colour of the unneutralised base and the signal is recorded as a typical SIA peak. The peak area of the unreacted base was found to be proportional to the logarithm of the acid concentration. Calibration curves with good linearity were obtained for a strong acid in the concentration ranges of 10(-4)-10(-2) and 0.1-3 M. Automatic sample dilution was implemented when sulphuric acid at concentration of 6-13 M was titrated. For a weak acid, i.e. acetic acid, a linear calibration curve was obtained in the range of 3x10(-4)-8x10(-2) M. By changing the volumes of the injected sample and the reagent, different acids as well as different concentration ranges of the acids can be titrated without any other adjustments in the SIA manifold or the titration protocol. PMID:18967966

  10. Potentiometric Surface of the Lower Patapsco 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 lower Patapsco aquifer in the Patapsco Formation of Early Cretaceous age in Southern Maryland during September 2007. The map is based on water-level measurements in 65 wells. The highest measured water level was 111 feet above sea level near the northwestern boundary and outcrop area of the aquifer in northern Prince George's County. From this area, the potentiometric surface declined towards well fields at Severndale and Arnold. The measured ground-water levels were 87 feet below sea level at Severndale, and 42 feet below sea level at Arnold. There was also a cone of depression covering a large area in Charles County that includes Waldorf, La Plata, Indian Head, and the Morgantown power plant. The ground-water levels measured were as low as 219 feet below sea level at Waldorf, 187 feet below sea level at La Plata, 106 feet below sea level at Indian Head, and 89 feet below sea level at the Morgantown power plant.

  11. Generalized potentiometric surface of the aquifers in the Cockfield Formation, southeastern Arkansas, spring 1980

    USGS Publications Warehouse

    Ackerman, D.J.

    1987-01-01

    This map shows the generalized contours of the altitude of water levels in wells completed in the Cockfield Formation in southeastern Arkansas for 1980. Most water levels used in constructing the map were made in the spring of 1980. However, in parts of the State water levels from the spring of 1980 were unavailable. Where data indicated no long-term changes in nearby water levels, measurements from as early as 1952 and as late as 1983 were used. At a few locations the altitude of the water surface in a stream was used to define the potentiometric surface. Available water level data limited the interpretation of potentiometric surface primarily to the area of occurrence of the aquifers south of the Arkansas River. Water level data from Arkansas and adjacent states used in the construction of this map are from the groundwater file of the U.S. Geological Survey 's National Water Data Storage and Retrieval System. This map was prepared as part of the Gulf Coast Regional Aquifer-System Analysis study. (Lantz-PTT)

  12. Potentiometric Surface of the Lower Patapsco Aquifer in Southern Maryland, September 2009

    USGS Publications Warehouse

    Curtin, Stephen E.; Andreasin, David C.; Staley, Andrew W.

    2010-01-01

    This report presents a map showing the potentiometric surface of the lower Patapsco aquifer in the Patapsco Formation of Early Cretaceous age in Southern Maryland during September 2009. The map is based on water-level measurements in 64 wells. The highest measured water level was 110 feet above sea level near the northwestern boundary and outcrop area of the aquifer in northern Prince George's County. From this area, the potentiometric surface declined towards well fields at Severndale, Broad Creek, and Arnold. The measured groundwater levels were 99 feet below sea level at Severndale, 50 feet below sea level at Broad Creek, and 36 feet below sea level at Arnold. There was also a cone of depression in Charles County that includes Waldorf, La Plata, Indian Head, and the Morgantown power plant. The groundwater levels measured were as low as 215 feet below sea level at Waldorf, 149 feet below sea level at La Plata, 121 feet below sea level at Indian Head, and 96 feet below sea level at the Morgantown power plant. The map also shows well yield in gallons per day for 2008 at wells or well fields.

  13. Catheter-type sensor for potentiometric monitoring of oxygen, pH and carbon dioxide.

    PubMed

    Meruva, R K; Meyerhoff, M E

    1998-02-01

    The fabrication and analytical performance of a catheter-type electrode suitable for potentiometric monitoring of PO2, pH and PCO2 in flowing blood is described. The catheter electrode is based on impregnating a single segment of dual-lumen gas permeable silicone rubber tubing with the proton ionophore tridodecylamine to impart H+ permselectivity to both inner and outer walls of the tubing. One lumen is filled with an unbuffered bicarbonate solution and the other lumen is filled with a strong buffer. By inserting Ag/AgCl reference electrode wires in each lumen and a cobalt electrode in the buffered lumen, simultaneous potentiometric detection of PO2, pH and PCO2 is achieved. The response of cobalt electrode to PO2 arises from a steady-state mixed potential owing to slow oxidation of cobalt and simultaneous reduction of oxygen on the surface of the cobalt electrode. The response towards PCO2 is completely analogous to the response mechanism of a conventional Severinghaus PCO2 sensor (i.e., change in pH of the bicarbonate solution). Continuous measurements of PO2, pH and PCO2 during 4-5 h blood pump studies using the catheter electrodes correlate well with conventional bench-top blood gas analyzer (PO2: r2 = 0.992; pH: r2 = 0.940; PCO2: r2 = 0.993. PMID:9597736

  14. Potentiometric Surface of the Upper Patapsco 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 upper Patapsco aquifer in the Patapsco Formation of Early Cretaceous age in Southern Maryland during September 2007. The map is based on water-level measurements in 50 wells. The highest measured water level was 120 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 south toward a well field in the Annapolis-Arnold area, and from all directions toward four cones of depression. These cones are located in the Waldorf-La Plata area, Chalk Point-Prince Frederick area, Swan Point subdivision in southern Charles County, and the Lexington Park-St. Inigoes area. The lowest measured ground-water level was 44 feet below sea level at Arnold, 106 feet below sea level south of Waldorf, 54 feet below sea level at Swan Point, 59 feet below sea level at Chalk Point, and 58 feet below sea level at Lexington Park.

  15. A biomimetic potentiometric sensor based on molecularly imprinted polymer for the determination of memantine in tablets.

    PubMed

    Arvand, Majid; Samie, Hedyeh Asadi

    2013-06-01

    Memantine hydrochloride is one of the first novel class medications for treatment of Alzheimer's disease. In this work, a biomimetic potentiometric sensor, based on a non-covalent imprinted polymer, was fabricated for the recognition and determination of memantine in pure drug and tablet pharmaceutical form. The molecularly imprinted polymer was synthesized by precipitation polymerization, using memantine hydrochloride as a template molecule, methacrylic acid as a functional monomer, and ethylene glycol dimethacrylate as a cross-linking agent. The sensor was developed by dispersing the memantine imprinted polymer particles in dibutyl sebacate plasticizer and embedding in poly(vinyl chloride) matrix. The wide linear range (10(-5) -10(-1) ?M), with a near Nernstian response of 57.4?mV/decade, a limit of detection 6.0?×?10(-6) ?M, fast response time (~15?s) and a satisfactory long-term stability (4?months) are characterizations of the proposed sensor. The sensor showed a high selectivity and a sensitive response to the template in aqueous system. The standard electrode potentials were determined at different temperatures and used to calculate the isothermal coefficient of the electrode. It was used as indicator electrode in potentiometric determination of memantine in pharmaceutical formulations. PMID:22514137

  16. Potentiometric urea biosensor utilizing nanobiocomposite of chitosan-iron oxide magnetic nanoparticles

    NASA Astrophysics Data System (ADS)

    Ali, A.; AlSalhi, M. S.; Atif, M.; Ansari, Anees A.; Israr, M. Q.; Sadaf, J. R.; Ahmed, E.; Nur, O.; Willander, M.

    2013-02-01

    The iron oxide (Fe3O4) magnetic nanoparticles have been fabricated through a simple, cheap and reproducible approach. Scanning electron microscope, x-rays powder diffraction of the fabricated nanoparticles. Furthermore, the fabrication of potentiometric urea biosensor is carried out through drop casting the initially prepared isopropanol and chitosan solution, containing Fe3O4 nanoparticles, on the glass fiber filter with a diameter of 2 cm and a copper wire (of thickness -500 μm) has been utilized to extract the voltage signal from the functionalized nanoparticles. The functionalization of surface of the Fe3O4 nanoparticles is obtained by the electrostatically immobilization of urease onto the nanobiocomposite of the chitosan- Fe3O4 in order to enhance the sensitivity, specificity, stability and reusability of urea biosensor. Electrochemical detection procedure has been adopted to measure the potentiometric response over the wide logarithmic concentration range of the 0.1 mM to 80 mM. The Fe3O4 nanoparticles based urea biosensor depicts good sensitivity with ~42 mV per decade at room temperature. Durability of the biosensor could be considerably enhanced by applying a thin layer of the nafion. In addition, the reasonably stable output response of the biosensor has been found to be around 12 sec.

  17. New molecularly-imprinted polymer for carnitine and its application as ionophore in potentiometric selective membranes.

    PubMed

    Moret, Joséphine; Moreira, Felismina T C; Almeida, Sofia A A; Sales, M Goreti F

    2014-10-01

    Carnitine (CRT) is a biological metabolite found in urine that contributes in assessingseveral disease conditions, including cancer. Novel quick screening procedures for CRT are therefore fundamental. This work proposes a novel potentiometric device where molecularly imprinted polymers (MIPs) were used as ionophores. The host-tailored sites were imprinted on a polymeric network assembled by radical polymerization of methacrylic acid (MAA) and trimethylpropane trimethacrylate (TRIM). Non-imprinted polymers (NIPs) were produced as control by removing the template from the reaction media. The selective membrane was prepared by dispersing MIP or NIP particles in plasticizer and poly(vinyl chloride), PVC, and casting this mixture over a solid contact support made of graphite. The composition of the selective membrane was investigated with regard to kind/amount of sensory material (MIP or NIP), and the need for a lipophilic additive. Overall, MIP sensors with additive exhibited the best performance, with near-Nernstian response down to ~1×10(-4)mol L(-1), at pH5, and a detection limit of ~8×10(-5)mol L(-1). Suitable selectivity was found for all membranes, assessed by the matched potential method against some of the most common species in urine (urea, sodium, creatinine, sulfate, fructose and hemoglobin). CRT selective membranes including MIP materials were applied successfully to the potentiometric determination of CRT in urine samples. PMID:25175239

  18. Simultaneous determination of fermented milk aroma compounds by a potentiometric sensor array.

    PubMed

    Hruskar, Mirjana; Major, Nikola; Krpan, Marina; Vahci?, Nada

    2010-09-15

    The paper reports on the application of an electronic tongue for simultaneous determination of ethanol, acetaldehyde, diacetyl, lactic acid, acetic acid and citric acid content in probiotic fermented milk. The alphaAstree electronic tongue by Alpha M.O.S. was employed. The sensor array comprised of seven non-specific, cross-sensitive sensors developed especially for food analysis coupled with a reference Ag/AgCl electrode. Samples of plain, strawberry, apple-pear and forest-fruit flavored probiotic fermented milk were analyzed both by standard methods and by the potentiometric sensor array. The results obtained by these methods were used for the development of neural network models for rapid estimation of aroma compounds content in probiotic fermented milk. The highest correlation (0.967) and lowest standard deviation of error for the training (0.585), selection (0.503) and testing (0.571) subset was obtained for the estimation of ethanol content. The lowest correlation (0.669) was obtained for the estimation of acetaldehyde content. The model exhibited poor performance in average error and standard deviations of errors in all subsets which could be explained by low sensitivity of the sensor array to the compound. The obtained results indicate that the potentiometric electronic tongue coupled with artificial neural networks can be applied as a rapid method for the determination of aroma compounds in probiotic fermented milk. PMID:20801331

  19. Potentiometric surface and specific conductance of the Sparta and Memphis aquifers in eastern Arkansas, 1995

    USGS Publications Warehouse

    Stanton, Gregory P.

    1997-01-01

    The Sparta and Memphis aquifers in eastern and south-central Arkansas are a major source of water for industrial, public supply, and agricultural uses. An estimated 240 million gallons per day was withdrawn from the Sparta and Memphis aquifers in 1995, an increase of about 17 million gallons per day from 1990. During the spring and early summer of 1995, the water level in the Sparta and Memphis aquifers was measured in 145 wells, the specific conductance of 101 ground-water samples collected from those aquifers was measured. Maps of areal distribution of potentiometric surface and specific conductance generated from these data reveal spatial trends in these parameters across the eastern and south-central Arkansas study area. The altitude of the potentiometric surface ranged from about 206 feet below sea level in Union County to about 307 feet above sea level in Saline County. The potentiometric surface of the Sparta and Memphis aquifers contains cones of depression descending below sea level in the central and southern portions of the study area, and a potentiometric high along the western study area boundary. Major recharge areas exhibit potentiometric highs greater than 200 feet above sea level and specific conductance values less than 200 microsiemens per centimeter, and generally are located in the outcrop/subcrop areas on the southern one-third of the western boundary and the northern portion of the study area. The regional direction of ground-water flow is from the north and west to the south and east, away from the outcrop and subcrop and northern regions, except near areas affected by intense ground-water withdrawals; such areas are manifested by large cones of depression centered in Columbia, Jefferson, and Union Counties. The cones of depression in adjoining Columbia and Union Counties are coalescing at or near sea level. The lowest water level measured was about 206 feet below sea level in Union County. Increased specific conductance values were measured in the areas of the cones of depression in Columbia and Union Counties. The cones of depression centered in Jefferson County coincides with an elongate area where ground water in the aquifer has low specific conductance. This area extends eastward from the outcrop/subcrop region of recharge. This extension of ground water with low specific conductance possibly indicates increased ground-water movement to the east-southeast from the outcrop/subcrop area induced by ground- water withdrawals in Jefferson County. Specific conductance increases markedly to the northeast and gradually to the south of this area. Long-term hydrographs of eight wells in the study areas, during the period 1970-1995, reveal water-level declines ranging from less than 0.5 foot per year in Phillips County to more than 2.0 feet per year in Union County. Water-level declines of greater than 1.5 feet per year generally are associated with the cones of depression centered in Columbia, Jefferson, and Union Counties.

  20. Enthalpies and constants of dissociation of several neutral and cationic acids in aqueous and methanol/water solutions at various temperatures.

    PubMed

    Shoghi, Elham; Romero, Lilian; Reta, Mario; Ràfols, Clara; Bosch, Elisabeth

    2009-05-01

    The acidic dissociation enthalpies and constants of anilinium, protonated tris(hydroxymethyl)aminomethane (HTris(+)), benzoic and acetic acids, have been determined at several temperatures in pure water and in methanol/water mixtures by potentiometry and by isothermal titration microcalorimetry (ITC). The pK(a) values determined by both techniques are in accordance when the dissociation process involves large amounts of heat. However, for the neutral acids the ITC technique gave slightly lower pK(a) values than those from potentiometry at the highest temperatures studied due to the small amounts of heat involved in the acidic dissociation. The dissociation enthalpies have been determined directly by calorimetry and the obtained values slightly decrease with the increase of temperature. Therefore, only a rough estimation of the dissociation enthalpies can be obtained from potentiometric pK(a) by means of the Van't Hoff approach. PMID:19261425

  1. Cation–cation interactions and cation exchange in a series of isostructural framework uranyl tungstates

    SciTech Connect

    Balboni, Enrica; Burns, Peter C.

    2014-05-01

    The isotypical compounds (UO{sub 2}){sub 3}(WO{sub 6})(H{sub 2}O){sub 5} (1), Ag(UO{sub 2}){sub 3}(WO{sub 6})(OH)(H{sub 2}O){sub 3} (2), K(UO{sub 2}){sub 3}(WO{sub 6})OH(H{sub 2}O){sub 4} (3), Rb(UO{sub 2}){sub 3}(WO{sub 6})(OH)(H{sub 2}O){sub 3.5} (4), and Cs(UO{sub 2}){sub 3}(WO{sub 6})OH(H{sub 2}O){sub 3} (5) were synthesized, characterized, and their structures determined. Each crystallizes in space group Cc. (1): a=12.979 (3), b=10.238 (2), c=11.302 (2), ?=102.044 (2); (2): a=13.148 (2), b=9.520 (1), c=11.083 (2), ?=101.568 (2); (3): a=13.111 (8), b=9.930 (6), c=11.242 (7), ?=101.024 (7); (4): a=12.940 (2), b=10.231 (2), c=11.259(2), ?=102.205 (2); (5): a=12.983 (3), b=10.191 (3), c=11.263 (4), ?=101.661 (4). Compounds 1–5 are a framework of uranyl and tungsten polyhedra containing cation–cation interactions. The framework has three symmetrically distinct U(VI) cations, one tungsten, sixteen to eighteen oxygen atoms, and in 2–5, one monovalent cation. Each atom occupies a general position. Each U(VI) cation is present as a typical (UO{sub 2}){sup 2+} uranyl ion in an overall pentagonal bipyramidal coordination environment. Each pentagonal bipyramid shares two equatorial edges with two other pentagonal bipyramids, forming a trimer. Trimers are connected into chains by edge-sharing with WO{sub 6} octahedra. Chains are linked through cation–cation interactions between two symmetrically independent uranyl ions. This yields a remarkably complex system of intersecting channels that extend along [0 0 1] and [?1 1 0]. The cation exchange properties of 2 and 3 were characterized at room temperature and at 140 °C. - Graphical abstract: Chains of uranium and tungsten polyhedra are connected into a three dimensional framework by cation–cation interactions occurring between two symmetrically independent uranyl pentagonal bipyramids. Monovalent cations present in channels within the structure can be exchanged by room temperature or mild hydrothermal treatments. The framework of these compounds is robust to cation exchange and heat. (yellow polyhedra=uranium pentagonal bipyramids; blue polyhedra=tungsten octahedral, purple balls=K; yellow balls=Na; grey balls=Tl). - Highlights: • Five isostructural uranyl tungstates compounds were synthesized hydrothermally. • The structures consist of a chains of uranium and tungstate polyhedral. • Chains are connected into a framework by cation–cation interactions. • Cation exchange does not alter the structural integrity of the compounds. • Cation exchange was successful at room temperature and mild hydrothermal conditions.

  2. Potentiometric surface of the Wilcox-Carrizo Aquifer; Bienville, Red River, and northern Natchitoches, and southern Webster parishes, Louisiana

    USGS Publications Warehouse

    Ryals, G.N.

    1981-01-01

    The potentiometric surface of the Wilcox-Carrizo aquifer in central northwestern Louisiana is shown by contours using data collected from 1960 to 1980. The aquifer is not affected by regional water-level declines as no large pumping centers have been developed. Seasonal water-level fluctuations in wells are generally less than 10 feet annually. (USGS)

  3. Historical potentiometric surface of the Edwards-Trinity aquifer system and contiguous hydraulically connected units, west-central Texas

    USGS Publications Warehouse

    Bush, Peter W.; Ardis, Ann F.; Wynn, Kirby H.

    1993-01-01

    The historical potentiometric-surface map of the Edwards-Trinity aquifer system and contiguous hydraulically connected units is based on 1,789 water-level (or pressure-head) measurements made in wells between December 1915 and November 1969. The mapped data reflect a wide range of rainfall conditions. On the basis of interpretations of historical climatologic data by the National Oceanic and Atmospheric Administration, near- normal rainfall conditions preceded 55 percent of the measurements. Moderately dry conditions preceded 20 percent of the measurements; moderately wet conditions preceded 22 percent of the measurements; very dry conditions preceded less than 1 percent; and very wet conditions preceded 3 percent. The historical potentiometric-surface map represents general predevelopment conditions because negligible ground-water withdrawals existed in most areas when the water-level measurements used to construct the map were made. However, in Bexar, Reeves, Pecos, Reagan, and Upton Counties, early withdrawals caused declines in water levels that are reflected in water-level features shown on the map. Topographic relief and stream or spring drainage are two major factors affecting the configuration of the historical potentiometric surface. The strong influence of stream or spring drainage on the potentiometric surface shows that the regional direction of ground-water movement is largely dictated by the locations of major discharge feature. a

  4. Cation-cation contact pairing in water: guanidinium.

    PubMed

    Shih, Orion; England, Alice H; Dallinger, Gregory C; Smith, Jacob W; Duffey, Kaitlin C; Cohen, Ronald C; Prendergast, David; Saykally, Richard J

    2013-07-21

    The formation of like-charge guanidinium-guanidinium contact ion pairs in water is evidenced and characterized by X-ray absorption spectroscopy and first-principles spectral simulations based on molecular dynamics sampling. Observed concentration-induced nitrogen K-edge resonance shifts result from ?* state mixing and the release of water molecules from each first solvation sphere as two solvated guanidinium ions associate into a stacked pair configuration. Possible biological implications of this counterintuitive cation-cation pairing are discussed. PMID:23883058

  5. Creating potentiometric surfaces from combined water well and oil well data in the midcontinent of the United States

    USGS Publications Warehouse

    Gianoutsos, Nicholas J.; Nelson, Philip H.

    2013-01-01

    For years, hydrologists have defined potentiometric surfaces using measured hydraulic-head values in water wells from aquifers. Down-dip, the oil and gas industry is also interested in the formation pressures of many of the same geologic formations for the purpose of hydrocarbon recovery. In oil and gas exploration, drillstem tests (DSTs) provide the formation pressure for a given depth interval in a well. These DST measurements can be used to calculate hydraulic-head values in deep hydrocarbon-bearing formations in areas where water wells do not exist. Unlike hydraulic-head measurements in water wells, which have a low number of problematic data points (outliers), only a small subset of the DST data measure true formation pressures. Using 3D imaging capabilities to view and clean the data, we have developed a process to estimate potentiometric surfaces from erratic DST data sets of hydrocarbon-bearing formations in the midcontinent of the U.S. The analysis indicates that the potentiometric surface is more readily defined through human interpretation of the chaotic DST data sets rather than through the application of filtering and geostatistical analysis. The data are viewed as a series of narrow, 400-mile-long swaths and a 2D viewer is used to select a subset of hydraulic-head values that represent the potentiometric surface. The user-selected subsets for each swath are then combined into one data set for each formation. These data are then joined with the hydraulic-head values from water wells to define the 3D potentiometric surfaces. The final product is an interactive, 3D digital display containing: (1) the subsurface structure of the formation, (2) the cluster of DST-derived hydraulic head values, (3) the user-selected subset of hydraulic-head values that define the potentiometric surface, (4) the hydraulic-head measurements from the corresponding shallow aquifer, (5) the resulting potentiometric surface encompassing both oil and gas and water wells, and (6) the land surface elevation of the region. Examples from the midcontinent of the United States, specifically Kansas, Oklahoma, and parts of adjacent states illustrate the process.

  6. Potentiometric map of the Eutaw-McShan Aquifer in northeastern Mississippi, September, October, and November 1978

    USGS Publications Warehouse

    Wasson, B.E.

    1980-01-01

    This potentiometric map of the Eutaw-McShan aquifer in northeastern Mississippi is the third 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. From its outcrop area the Eutaw-McShan aquifer dips about 30 feet per mile to the west and southwest. Thickness of the aquifer commonly is between 200 and 300 feet in most of the area, and commonly about one-half this thickness consists of sand. In the outcrop area the potentiometric surface is strongly affected by recharge from precipitation, topography, and drainage of the aquifer by streams. The potentiometric surface of the aquifer slopes generally to the west away from the area of outcrop and it is strongly affected by large ground-water withdrawals at or near Tupelo, Aberdeen, and West Point. Historically, water levels in or near the outcrop of the Eutaw-McShan aquifer have shown little or no long-term changes. Withdrawals of water by wells 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 declines during recent years in several observation wells in Lee County ranged from 2 to 9 feet per year. One hydrograph in Clay County that is near the center of the depression in the potentiometric surface at West Point shows about 5 feet per year of water-level decline since 1972. (USGS)

  7. Polymeric membrane neutral phenol-sensitive electrodes for potentiometric G-quadruplex/hemin DNAzyme-based biosensing.

    PubMed

    Wang, Xuewei; Ding, Zhaofeng; Ren, Qingwei; Qin, Wei

    2013-02-01

    The first potentiometric transducer for G-quadruplex/hemin DNAzyme-based biosensing has been developed by using potential responses of electrically neutral oligomeric phenols on polymeric membrane electrodes. In the presence of G-quadruplex/hemin DNAzyme and H(2)O(2), monomeric phenols (e.g., phenol, methylphenols, and methoxyphenols) can be condensed into oligomeric phenols. Because both substrates and products are nonionic under optimal pH conditions, these reactions are traditionally not considered in designing potentiometric biosensing schemes. However, in this paper, the electrically neutral oligomeric phenols have been found to induce highly sensitive potential responses on quaternary ammonium salt-doped polymeric membrane electrodes owing to their high lipophilicities. In contrast, the potential responses to monomeric phenolic substrates are rather low. Thus, the G-quadruplex/hemin DNAzyme-catalyzed oxidative coupling of monomeric phenols can induce large potential signals, and the catalytic activities of DNAzymes can be probed. A comparison of potential responses induced by peroxidations of 13 monomeric phenols indicates that p-methoxyphenol is the most efficient substrate for potentiometric detection of G-quadruplex/hemin DNAzymes. Finally, two label-free and separation-free potentiometric DNA assay protocols based on the G-quadruplex/hemin DNAzyme have been developed with sensitivities higher than those of colorimetric and fluorometric methods. Coupled with other features such as reliable instrumentation, low cost, ease of miniaturization, and resistance to color and turbid interferences, the proposed polymeric membrane-based potentiometric sensor promises to be a competitive transducer for peroxidase-mimicking DNAzyme-involved biosensing. PMID:23289675

  8. Electrometric method for the determination of the nitrogen content in metals and ferroalloys

    SciTech Connect

    Agafonov, P.F.; Zueva, V.L.

    1985-11-01

    To determine cationic and nonionogenic surfactants in a mixture, the authors used potentiometric titration of aqueous solutions of the surfactants with 0.01M solution of tetraphenylborate. The indicator electrodes were polyvinyl chloride membrane electrodes with electroactive substances -- the cetylpyridinium salt of dodecylbenzenesulfonic acid, recommended for the determination of ionic surfactants and barium (II), respectively.

  9. Effect of the Fv-1 locus on the titration of murine leukemia viruses.

    PubMed Central

    Jolicoeur, P; Baltimore, D

    1975-01-01

    Titration of N- and B-tropic murine leukemia viruses on sensitive and resistant cell lines has been studied by direct XC plaque assay and infective center assay. The titration of cloned B-tropic virus by infective center assay on BALB/3T3 (Fv-1b/b) and NIH/3T3 (Fv-1n/n) cells gave one-hit patterns, with 100-fold less infected NIH/3T3 cells than BALB/3T3 cells. The titration of B-tropic virus on DBA/2 cells (Fv-1n/n) was also a one-hit. The titration of a one-hit curve, and there were about 100-fold less infected BALB/3T3 cells than NIH/3T3 cells. Comparable results were obtained by titrating the cloned N-tropic virus on congenic SIM (Fv-1n/n) and SIM.R (Fv-1b/b) cells or the Gross N-tropic virus on BALB/3T3 cells. Therefore, our data indicate that the multiple-hit phenomenon described previously may not be an essential part of the Fv-1 gene restriction. PMID:172659

  10. Effect of temperature on the protonation of N-(2-hydroxyethyl)ethylenediamine-N,N',N'-triacetic acid in aqueous solutions: Potentiometric and calorimetric studies

    SciTech Connect

    Li, Xingliang; Zhang, Zhicheng; Endrizzi, Francesco; Martin, Leigh R.; Luo, Shunzhong; Rao, Linfeng

    2015-06-01

    The TALSPEAK process (Trivalent Actinide Lanthanide Separations by Phosphorus-reagent Extraction from Aqueous Komplexes) has been demonstrated in several pilot-scale operations to be effective at separating trivalent actinides (An3+) from trivalent lanthanides (Ln3+). However, fundamental studies have revealed undesired aspects of TALSPEAK, such as the significant partitioning of Na+, lactic acid, and water into the organic phase, thermodynamically unpredictable pH dependence, and the slow extraction kinetics. In the modified TALSPEAK process, the combination of the aqueous holdback complexant HEDTA (N-(2-hydroxyethyl)ethylenediamine-N,N',N'-triacetic acid) with the extractant HEH[EHP] (2-ethyl(hexyl) phosphonic acid mono-2-ethylhexyl ester) in the organic phase has been found to exhibit a nearly flat pH dependence between 2.5 and 4.5 and more rapid phase transfer kinetics for the heavier lanthanides. To help understand the speciation of Ln3+ and An3+ in the modified TALSPEAK, systematic studies are underway on the thermodynamics of major reactions in the HEDTA system under conditions relevant to the process (e.g., higher temperatures). Thermodynamics of the protonation and complexation of HEDTA with Ln3+ were studied at variable temperatures. Equilibrium constants and enthalpies were determined by a combination of techniques including potentiometry and calorimetry. This paper presents the protonation constants of HEDTA at T = (25 to 70) °C. The potentiometric titrations have demonstrated that, stepwise, the first two protonation constants decrease and the third one slightly increases with the increase of temperature. This trend is in good agreement with the enthalpy of protonation directly determined by calorimetry. The results of NMR analysis further confirm that the first two protonation reactions occur on the diamine nitrogen atoms, while the third protonation reaction occurs on the oxygen of a carboxylate group. These data, in conjunction with the thermodynamic parameters of Ln3+/An3+ complexes with HEDTA at different temperatures, will help to predict the speciation and temperature-dependent behavior of Ln3+/An3+ in the modified TALSPEAK process.

  11. Potentiometric Surface of the Aquia 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 Aquia aquifer in the Aquia Formation of Paleocene age in Southern Maryland during September 2007. The map is based on water-level measurements in 85 wells. The highest measured water level was 50 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 just south of this area and in the remainder of the study area. The hydraulic gradient increased southeastward toward an extensive cone of depression around well fields at Lexington Park and Solomons Island. A water level measured west of the Cheasapeake Beach area has declined to 57 feet below sea level due to increased withdrawals. The lowest water level measured was 162 feet below sea level at the center of a cone of depression at Lexington Park.

  12. Potentiometric surfaces in the Cockfield and Wilcox aquifers of southern and northeastern Arkansas, 2003

    USGS Publications Warehouse

    Yeatts, Daniel S.

    2004-01-01

    This report presents the results of water-level measurements made at wells in the Cockfield Formation and Wilcox Group of southern and northeastern Arkansas during 2003, and the water levels are displayed in potentiometric-surface maps and hydrographs. During March and April 2003, the water level was measured at 55 wells completed in the Cockfield aquifer, 13 wells completed in the Wilcox aquifer of southern Arkansas, and 43 wells completed in the Wilcox aquifer of northeastern Arkansas. The Cockfield Formation generally consists of discontinuous sand units interbedded with silt, clay, and lignite in southeastern Arkansas. Sand beds near the base of the Cockfield Formation constitute most of the Cockfield aquifer. Withdrawals from the Cockfield aquifer in the study area during 2000 totaled about 9 million gallons per day. The potentiometric surface of the Cockfield aquifer constructed from the 2003 water levels shows that regional direction of ground-water flow generally is towards the east and southeast, away from the outcrop, except in areas of intense ground-water withdrawals. Some local ground-water flow in the outcrop area is toward rivers that have eroded into the Cockfield Formation and deposited alluvium in south Bradley and Calhoun Counties (Ouachita River), and in north Dallas County (Saline River). An evaluation of 20 wells with water-level data from 1983 to 2003 shows that water levels in 15 wells have declined at a rate of -0.04 to -0.97 feet per year, and water levels in 5 wells have risen at a rate of 0.07 to 0.32 feet per year. An evaluation of the same 20 wells from 2000 to 2003 shows that water levels have declined in only 8 wells, and water levels have risen in 12 wells. The Wilcox Group is distributed throughout most of southern and eastern Arkansas. There are two study areas in southern and northeastern Arkansas. The Wilcox Group of the southern study area consists of interbedded clay, sandy clay, sand, and lignite. Thin discontinuous sand units constitute the Wilcox aquifer in the southern study area. Withdrawals from the aquifer in the southern study area were about 1 million gallons per day during 2000. The potentiometric surface of the Wilcox aquifer in the southern study area shows that regional ground-water flow generally is south and east, except in Clark County where flow is towards the Ouachita River. The Wilcox Group in the northeastern study area consists of thin interbedded lignitic sand and clays. A sand bed of about 200 feet thick in the middle to lower part of the Wilcox Group constitutes the major producing unit of the Wilcox aquifer in the northeastern study area. Withdrawals from the aquifer in the northeastern study area were about 23 million gallons per day during 2000. The potentiometric surface of the Wilcox aquifer in the northeastern study area shows that ground-water flow generally is south and east, except where ground-water withdrawals may have altered the natural direction of flow near the centers of pumping at Paragould and West Memphis. An evaluation of 27 wells with water-level data from 1983 to 2003 in the northeastern study area shows that water levels in all 27 wells have been declining at a rate of -0.17 to -1.73 feet per year. An evaluation of the same 27 wells from 2000 to 2003 shows that water levels in 18 wells have risen and in 9 wells have declined.

  13. Potentiometric Surface of the Aquia 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 Aquia aquifer in the Aquia Formation of Paleocene age in Southern Maryland during September 2009. The map is based on water-level measurements in 82 wells. The highest measured water level was 48 feet above sea level near the northern boundary and in the outcrop area of the aquifer in the central part of Anne Arundel County. Water levels also were above sea level in Kent County and northern Queen Anne's County. Water levels were below sea level south and east of these areas and in the remainder of the study area. The hydraulic gradient increased southeastward toward a cone of depression around well fields at Lexington Park and Solomons Island. The lowest measured water level was 145 feet below sea level at the center of a cone of depression at Lexington Park. The map also shows well yield in gallons per day for 2008 at wells or well fields.

  14. Two Analyte Calibration From The Transient Response Of Potentiometric Sensors Employed With The SIA Technique

    SciTech Connect

    Cartas, Raul; Mimendia, Aitor; Valle, Manel del; Legin, Andrey

    2009-05-23

    Calibration models for multi-analyte electronic tongues have been commonly built using a set of sensors, at least one per analyte under study. Complex signals recorded with these systems are formed by the sensors' responses to the analytes of interest plus interferents, from which a multivariate response model is then developed. This work describes a data treatment method for the simultaneous quantification of two species in solution employing the signal from a single sensor. The approach used here takes advantage of the complex information recorded with one electrode's transient after insertion of sample for building the calibration models for both analytes. The departure information from the electrode was firstly processed by discrete wavelet for transforming the signals to extract useful information and reduce its length, and then by artificial neural networks for fitting a model. Two different potentiometric sensors were used as study case for simultaneously corroborating the effectiveness of the approach.

  15. Potentiometric-scanning ion conductance microscopy for measurement at tight junctions

    PubMed Central

    Zhou, Yi; Chen, Chiao-Chen; Weber, Anna E.; Zhou, Lushan; Baker, Lane A.; Hou, Jianghui

    2013-01-01

    Scanning Ion Conductance Microscopy (SICM) has been developed originally for high-resolution imaging of topographic features. Recently, we have described a hybrid voltage scanning mode of SICM, termed Potentiometric-SICM (P-SICM) for recording transmembrane ionic conductance at specific nanostructures of synthetic and biological interfaces. With this technique, paracellular conductance through tight junctions – a subcellular structure that has been difficult to interrogate previously – has been realized. P-SICM utilizes a dual-barrel pipet to differentiate paracellular from transcellular transport processes with nanoscale spatial resolution. The unique combination of voltage scanning and topographic imaging enables P-SICM to capture paracellular conductance within a nominal radius of several hundred nanometers. This review summarizes recent advances in paracellular conductance recording with an emphasis on the P-SICM based approach, which is applied to detect claudin-2 mediated permeability changes at the tight junction. PMID:24533255

  16. A new buffer system for the potentiometric determination of fluoride ion

    SciTech Connect

    Zhobinskii, E.Y.; Askochenskaya, R.M.; Novikova, L.B; Wl' Figarov, O.S.

    1985-05-01

    This paper attempts to eliminate the lengthy stage of hydrolytic separation of the elements during the potentiometric determination of fluoride ions and also to develop a universal method for the determination of flouride ions. During the development of a procedure for the determination of fluoride ions it is necessary to eliminate the interfering effects of elements which form stable fluoride complexes such as A1 (III), Fe (III), Si (III), Ti (IV), V (IV), Mo (V), and W (V). By the addition of diethylenetriaminepentaacetate to the buffer solution and preliminary extraction of the benzoylphenylhydroxylaminates of the interfering elements with chloroform it was possible to develop a method for the determination of fluoride with a detection limit of 1.10/sup -5/ M.

  17. Potentiometric Electronic Tongue to Resolve Mixtures of Sulfide and Perchlorate Anions

    PubMed Central

    Wilson, Deivy; Abbas, Mohammed N.; Radwan, Abdel Latief A.; del Valle, Manel

    2011-01-01

    This work describes the use of an array of potentiometric sensors and an artificial neural network response model to determine perchlorate and sulfide ions in polluted waters, by what is known as an electronic tongue. Sensors used have been all-solid-state PVC membrane selective electrodes, where their ionophores were different metal-phtalocyanine complexes with specific and anion generic responses. The study case illustrates the potential use of electronic tongues in the quantification of mixtures when interfering effects need to be counterbalanced: relative errors in determination of individual ions can be decreased typically from 25% to less than 5%, if compared to the use of a single proposed ion-selective electrode. PMID:22163795

  18. Selectivity characteristics of potentiometric carbon dioxide sensors with various gas membrane materials

    SciTech Connect

    Kobos, R.K.; Parks, S.J.; Meyerhoff, M.E.

    1982-10-01

    The selectivity characteristics of potentiometric carbon dioxide sensors with regard to various organic and inorganic acid interferences have been systematically examined. When used in conjunction with a standard silicone rubber CO/sub 2/ permeable membrane, the sensor displays surprisingly large response to several organic acids having low volatility, e.g., benzoic, cinnamic, and salicylic acids. If the outer membrane is changed to a microporous Teflon material, the response to these substances is diminished, but poor selectivity over volatile organics and acidic gases results. The use of a new homogeneous Teflon-like membrane meterial is shown to offer dramatic improvement in selectivity for CO/sub 2/ over all of the compounds tested. The mechanistic reasons for this enhanced selectivity are discussed as are alternate methods for reducing organic acid interferences when using more conventional membrane materials. 4 figures, 1 table.

  19. Potentiometric surfaces of the coastal plain aquifers of South Carolina prior to development

    USGS Publications Warehouse

    Aucott, Walter R.; Speiran, Gary K.

    1985-01-01

    Characteristics of the Coastal Plains aquifers of South Carolina are being studied as a part of the Regional Aquifer Systems Analysis program of the U.S. Geological Survey. A framework has been developed to best represent the hydrology of the Coastal Plain aquifers by dividing them into a system of five aquifers. This framework includes a surficial aquifer consisting of coastal terrace deposits, a limestone and stratigraphically equivalent sand aquifer of Eocene age, and three sand aquifers of Cretaceous age. This report presents a general description of the aquifer framework, potentiometric maps for the aquifers of Eocene and Cretaceous age prior to development, and a general description of the flow system prior to development. In the lower Coastal Plain, flow in the aquifer of Eocene age is generally perpendicular to the coast but is almost parallel to the coast in the aquifers of Cretaceous age. (USGS)

  20. Real-time telemetry system for amperometric and potentiometric electrochemical sensors.

    PubMed

    Wang, Wei-Song; Huang, Hong-Yi; Chen, Shu-Chun; Ho, Kuo-Chuan; Lin, Chia-Yu; Chou, Tse-Chuan; Hu, Chih-Hsien; Wang, Wen-Fong; Wu, Cheng-Feng; Luo, Ching-Hsing

    2011-01-01

    A real-time telemetry system, which consists of readout circuits, an analog-to-digital converter (ADC), a microcontroller unit (MCU), a graphical user interface (GUI), and a radio frequency (RF) transceiver, is proposed for amperometric and potentiometric electrochemical sensors. By integrating the proposed system with the electrochemical sensors, analyte detection can be conveniently performed. The data is displayed in real-time on a GUI and optionally uploaded to a database via the Internet, allowing it to be accessed remotely. An MCU was implemented using a field programmable gate array (FPGA) to filter noise, transmit data, and provide control over peripheral devices to reduce power consumption, which in sleep mode is 70 mW lower than in operating mode. The readout circuits, which were implemented in the TSMC 0.18-?m CMOS process, include a potentiostat and an instrumentation amplifier (IA). The measurement results show that the proposed potentiostat has a detectable current range of 1 nA to 100 ?A, and linearity with an R2 value of 0.99998 in each measured current range. The proposed IA has a common-mode rejection ratio (CMRR) greater than 90 dB. The proposed system was integrated with a potentiometric pH sensor and an amperometric nitrite sensor for in vitro experiments. The proposed system has high linearity (an R2 value greater than 0.99 was obtained in each experiment), a small size of 5.6 cm × 8.7 cm, high portability, and high integration. PMID:22164093

  1. Real-Time Telemetry System for Amperometric and Potentiometric Electrochemical Sensors

    PubMed Central

    Wang, Wei-Song; Huang, Hong-Yi; Chen, Shu-Chun; Ho, Kuo-Chuan; Lin, Chia-Yu; Chou, Tse-Chuan; Hu, Chih-Hsien; Wang, Wen-Fong; Wu, Cheng-Feng; Luo, Ching-Hsing

    2011-01-01

    A real-time telemetry system, which consists of readout circuits, an analog-to-digital converter (ADC), a microcontroller unit (MCU), a graphical user interface (GUI), and a radio frequency (RF) transceiver, is proposed for amperometric and potentiometric electrochemical sensors. By integrating the proposed system with the electrochemical sensors, analyte detection can be conveniently performed. The data is displayed in real-time on a GUI and optionally uploaded to a database via the Internet, allowing it to be accessed remotely. An MCU was implemented using a field programmable gate array (FPGA) to filter noise, transmit data, and provide control over peripheral devices to reduce power consumption, which in sleep mode is 70 mW lower than in operating mode. The readout circuits, which were implemented in the TSMC 0.18-?m CMOS process, include a potentiostat and an instrumentation amplifier (IA). The measurement results show that the proposed potentiostat has a detectable current range of 1 nA to 100 ?A, and linearity with an R2 value of 0.99998 in each measured current range. The proposed IA has a common-mode rejection ratio (CMRR) greater than 90 dB. The proposed system was integrated with a potentiometric pH sensor and an amperometric nitrite sensor for in vitro experiments. The proposed system has high linearity (an R2 value greater than 0.99 was obtained in each experiment), a small size of 5.6 cm × 8.7 cm, high portability, and high integration. PMID:22164093

  2. Tuning cation-anion interactions in ionic liquids by changing the conformational flexibility of the cation.

    PubMed

    Blundell, R K; Licence, P

    2014-10-18

    Cation-anion interactions can be tuned via the degree of cation constraint. X-ray Photoelectron Spectroscopy (XPS) experiments reveal that anion-cation based interactions may be enhanced by introducing conformational restriction into the substituent chains of quaternary ammonium cations. A larger degree of charge-transfer was observed for the constrained [C8C1Pyrr](+) cation relative to the [N6,6,6,14](+) cation. PMID:25166921

  3. Introducing Titratable Water to All-Atom Molecular Dynamics at Constant pH

    PubMed Central

    Chen, Wei; Wallace, Jason A.; Yue, Zhi; Shen, Jana K.

    2013-01-01

    Recent development of titratable coions has paved the way for realizing all-atom molecular dynamics at constant pH. To further improve physical realism, here we describe a technique in which proton titration of the solute is directly coupled to the interconversion between water and hydroxide or hydronium. We test the new method in replica-exchange continuous constant pH molecular dynamics simulations of three proteins, HP36, BBL, and HEWL. The calculated pKa values based on 10-ns sampling per replica have the average absolute and root-mean-square errors of 0.7 and 0.9 pH units, respectively. Introducing titratable water in molecular dynamics offers a means to model proton exchange between solute and solvent, thus opening a door to gaining new insights into the intricate details of biological phenomena involving proton translocation. PMID:23972860

  4. Acid-Base Titration of (S)-Aspartic Acid: A Circular Dichroism Spectrophotometry Experiment

    NASA Astrophysics Data System (ADS)

    Cavaleiro, Ana M. V.; Pedrosa de Jesus, Júlio D.

    2000-09-01

    The magnitude of the circular dichroism of (S)-aspartic acid in aqueous solutions at a fixed wavelength varies with the addition of strong base. This laboratory experiment consists of the circular dichroism spectrophotometric acid-base titration of (S)-aspartic acid in dilute aqueous solutions, and the use of the resulting data to determine the ionization constant of the protonated amino group. The work familiarizes students with circular dichroism and illustrates the possibility of performing titrations using a less usual instrumental method of following the course of a reaction. It shows the use of a chiroptical property in the determination of the concentration in solution of an optically active molecule, and exemplifies the use of a spectrophotometric titration in the determination of an ionization constant.

  5. Spectrophotometric titration with cobalt(III) for the determination of accurate absorption coefficients of transferrins.

    PubMed Central

    He, Q Y; Mason, A B; Woodworth, R C

    1996-01-01

    A rapid and sensitive technique, involving difference spectral titration with cobalt(III), to measure the epsilon values of chicken ovotransferrin, human serum transferrin, the N-lobe of human transferrin and several single point mutants is reported. The resulting epsilon values were compared with the values calculated from the equation proposed by Pace, Vajdos, Fee, Grimsley and Gray [(1995) Protein Sci. 4, 2411-2423]. The titrations with cobalt feature sharp break-points and do not destroy the protein samples. The choice of buffer was found to be important, depending on the metal-binding avidity of the proteins. Cobalt titration should prove useful for studying the comparative metal-binding properties of transferrin and mutants of transferrin being generated by recombinant technology. PMID:8761464

  6. Low-coordinate bismuth cations.

    PubMed

    Schwamm, Ryan J; Day, Benjamin M; Coles, Martyn P; Fitchett, Christopher M

    2014-04-01

    Chloride abstraction from the diamido-bismuth compound Bi(Me2Si{NAr}2)Cl (1, Ar = 2,6-i-Pr2C6H3) using MCl3 (M = Al, Ga) is a facile route to cationic species. Stoichiometric reactions afford the tetrachlorometallate salts [Bi(Me2Si{NAr}2)][MCl4] (2a, M = Al; 3a, M = Ga), whereas reaction with 0.5 equiv of the group 13 reagent gives the ?-chlorido bridged cations [{Bi(Me2Si{NAr}2)}2(?-Cl)][MCl4] (2b, M = Al; 3b, M = Ga). The crystal structure of 2a shows a formally two-coordinate bismuth cation, with a Bi···Cl contact to the [AlCl4](-) anion, whereas the structure of 3b shows a total of three Bi···Cl contacts to [GaCl4](-). Both species associate as {1:1}2 dimers in the solid state through additional Bi···Cl interactions. Attempted preparation of cationic complexes using either NaBR4 (R = Ph, Et) or [HNEt3][BPh4] were unsuccessful. Instead of forming the borate salts, the neutral compounds Bi(Me2Si{NAr}2)R (4, R = Et; 5, R = Ph) were isolated as a result of aryl/alkyl transfer from boron to bismuth. PMID:24635124

  7. Clozapine-induced myocarditis may be associated with rapid titration: A case report verified with autopsy.

    PubMed

    Chopra, Nitin; de Leon, Jose

    2016-01-01

    Clozapine-induced myocarditis is a poorly understood, rare, potentially fatal adverse drug reaction with absolute risks ranging from 7 to 34 per 1000 in Australia and 0.07-0.6 per 1000 in other countries. Hypersensitivity reactions have been postulated including some cases probably associated with rapid titrations. This case describes a 50-year-old African-American man with schizoaffective disorder, naïve to clozapine, who probably died from clozapine-induced myocarditis. He was started on 25?mg/day of clozapine and received 1625?mg over 14 days, prior to his death on day 15. The autopsy found predominantly lymphocytic infiltrate of the perivascular soft tissue and myocardium of the ventricles, with occasional eosinophils. Using the Liverpool ADR Causality Assessment Tool, it was deemed probable that the patient's death was secondary to myocarditis. The patient had fulminant death with no obvious changes in vital signs. Neither C-reactive protein nor troponin was measured, but it is unlikely that the results would have arrived in time to prevent the patient's death. Age, rapid titration, and concomitant use of valproate contributed to this case, which was probably an idiosyncratic adverse drug reaction associated with rapid titration. Lamotrigine-induced Stevens-Johnson syndrome also appears to be an idiosyncratic adverse drug reaction associated with rapid titration, but its incidence has been remarkably reduced since the recommended starting lamotrigine dose was reduced and corrected by the effect of inhibitors such as valproate. Similarly, clozapine-induced myocarditis incidence probably can be reduced with the use of slow titrations, including even slower titrations for patients with lower ability to metabolize clozapine, such as those taking valproate. PMID:26681239

  8. Comparison of acid secretion rates measured by gastric aspiration and by in vivo intragastric titration in healthy human subjects.

    PubMed

    Feldman, M

    1979-05-01

    In nine healthy subjects acid secretion rates, measured first by gastric aspiration and then by in vivo intragastric titration to pH 5, were compared. In vivo intragastric titration was initiated by instilling 50, 100, or 700 ml saline (pH 5) into the stomach, followed by a continuous intragastric saline infusion at 3.3 ml/min. Irrespective of the volume of saline used to initiate in vivo intragastric titration, acid secretion rates during titration were two to three times greater than secretion rates during gastric aspiration (P less than 0.005). This difference was not due to transpyloric acid losses during aspiration, since such losses were corrected for by nonabsorbable marker recovery; nor was the difference due to a higher intragastric pH during in vivo titration, since significant differences in acid secretion rates between aspiration and titration persisted when in vivo titration was performed at an acid pH. These findings suggest that in vivo intragastric titration leads to higher measured acid secretory rates than gastric aspiration because the titration method is associated with gastric distention and even small degrees of gastric distention stimulate gastric acid secretion. PMID:437422

  9. Using Isothermal Titration Calorimetry to Determine Thermodynamic Parameters of Protein–Glycosaminoglycan Interactions

    PubMed Central

    Dutta, Amit K.; Rösgen, Jörg; Rajarathnam, Krishna

    2015-01-01

    It has now become increasingly clear that a complete atomic description of how biomacromolecules recognize each other requires knowledge not only of the structures of the complexes but also of how kinetics and thermodynamics drive the binding process. In particular, such knowledge is lacking for protein–glycosaminoglycan (GAG) complexes. Isothermal titration calorimetry (ITC) is the only technique that can provide various thermodynamic parameters—enthalpy, entropy, free energy (binding constant), and stoichiometry—from a single experiment. Here we describe different factors that must be taken into consideration in carrying out ITC titrations to obtain meaningful thermodynamic data of protein–GAG interactions. PMID:25325962

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

    PubMed Central

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

    2009-01-01

    Abstract Isothermal titration calorimetry was used to monitor the energetic landscape of a catalytic RNA, specifically that of the hepatitis delta virus ribozyme. Using mutants that isolated various tertiary interactions, the thermodynamic parameters of several ribozyme-substrate intermediates were determined. The results shed light on the impact of several tertiary interactions on the global structure of the ribozyme. In addition, the data indicate that the formation of the P1.1 pseudoknot is the limiting step of the molecular mechanism. Last, as illustrated here, isothermal titration calorimetry appears to be a method of choice for the elucidation of an RNA's folding pathway. PMID:19134473

  11. Determination of the acidic sites of purified single-walled carbon nanotubes by acid base titration

    NASA Astrophysics Data System (ADS)

    Hu, H.; Bhowmik, P.; Zhao, B.; Hamon, M. A.; Itkis, M. E.; Haddon, R. C.

    2001-09-01

    We report the measurement of the acidic sites in three different samples of commercially available full-length purified single-walled carbon nanotubes (SWNTs) - as obtained from CarboLex (CLI), Carbon Solutions (CSI) and Tubes@Rice (TAR) - by simple acid-base titration methods. Titration of the purified SWNTs with NaOH and NaHCO 3 solutions was used to determine the total percentage of acidic sites and carboxylic acid groups, respectively. The total percentage of acidic sites in full length purified SWNTs from TAR, CLI and CSI are about 1-3%.

  12. Selective two-step titration of thorium by sulfate displacement of the diethylenetriaminepentaacetic acid complex

    SciTech Connect

    Kiefer, P.

    1980-07-01

    Thorium and other metals are complexed with excess diethylenetriaminepentaacetic acid (DTPA) at pH 1.4, the excess DTPA is titrated with Bi(III) to a xylenol orange end point, sulfate is added to complex Th(IV), and the displaced DTPA again is titrated with Bi(III). Of 61 metal ions and nonmetal anions tested, only Ga(III), Sc(III), tungstate, citrate, oxalate, and thiosulfate interfere seriously. Lesser interferences are In(III), Zr(IV), V(IV), and permanganate. The standard deviation is 2 ..mu..g for 56 to 840 ..mu..g Th.

  13. Potentiometric surfaces and water-level trends in the Cockfield (upper Claiborne) aquifer in southern Arkansas and the Wilcox (lower Wilcox) aquifer of northeastern and southern Arkansas, 2012

    USGS Publications Warehouse

    Rodgers, Kirk D.

    2015-01-01

    Two potentiometric-surface maps, one for the southern area and one for the northeastern area, were constructed to show the altitude of the water surface in the Wilcox aquifer. The direction of groundwater flow in the northeastern are

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

    PubMed

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

    2013-01-01

    In this study, Na(+) uptake and acid-base balance in the euryhaline pupfish Cyprinodon variegatus variegatus were characterized when fish were exposed to pH 4.5 freshwater (7mM Na(+)). Similar to the related cyprinodont, Fundulus heteroclitus, Na(+) uptake was significantly inhibited when exposed to low pH water. However, it initially appeared that C. v. variegatus increased apparent net acid excretion at low pH relative to circumneutral pH. This result is opposite to previous observations for F. heteroclitus under similar conditions where fish were observed to switch from apparent net H(+) excretion at circumneutral pH to apparent net H(+) uptake at low pH. Further investigation revealed disparate observations between these studies were the result of using double endpoint titrations to measure titratable alkalinity fluxes in the current study, while the earlier study utilized single endpoint titrations to measure these fluxes (i.e.,. Cyprinodon acid-base transport is qualitatively similar to Fundulus when characterized using single endpoint titrations). This led to a comparative investigation of these two methods. We hypothesized that either the single endpoint methodology was being influenced by a change in the buffer capacity of the water (e.g., mucus being released by the fish) at low pH, or the double endpoint methodology was not properly accounting for ammonia flux by the fish. A series of follow-up experiments indicated that buffer capacity of the water did not change significantly, that excretion of protein (a surrogate for mucus) was actually reduced at low pH, and that the double endpoint methodology does not properly account for NH(3) excretion by fish under low pH conditions. As a result, it overestimates net H(+) excretion during low pH exposure. After applying the maximum possible correction for this error (i.e., assuming that all ammonia is excreted as NH(3)), the double endpoint methodology indicates that net H(+) transport was reduced to effectively zero in both species at pH 4.5. However, significant differences between the double endpoint (no net H(+) transport at low pH) and single endpoint titrations (net H(+) uptake at low pH) remain to be explained. PMID:23000354

  15. Cationic electrodepositable coating composition comprising lignin

    DOEpatents

    Fenn, David; Bowman, Mark P; Zawacky, Steven R; Van Buskirk, Ellor J; Kamarchik, Peter

    2013-07-30

    A cationic electrodepositable coating composition is disclosed. The present invention in directed to a cationic electrodepositable coating composition comprising a lignin-containing cationic salt resin, that comprises (A) the reaction product of: lignin, an amine, and a carbonyl compound; (B) the reaction product of lignin, epichlorohydrin, and an amine; or (C) combinations thereof.

  16. Difference between the potentiometric surfaces of the Lower Patapsco aquifer in southern Maryland, September 1990 and September 2009

    USGS Publications Warehouse

    Curtin, Stephen E.; Andreasen, David C.; Staley, Andrew W.

    2010-01-01

    This report presents a map showing the change in the potentiometric surface of the lower Patapsco aquifer in the Patapsco Formation of Early Cretaceous age in Southern Maryland between September 1990 and September 2009. The map, based on water level differences obtained from 45 wells, shows that the change of the potentiometric surface during the 19-year period ranged from increases of 25 feet at Indian Head and 4 feet near the outcrop area in Glen Burnie, to declines of 35 feet at Arnold, 56 feet at Severndale, 28 feet at Crofton Meadows, 73 feet at Waldorf, 79 feet near La Plata, 35 feet at the Morgantown power plant, and 32 feet at Swan Point. The map also shows well yield in gallons per day for 2008 at wells or well fields.

  17. The Difference Between the Potentiometric Surfaces of the Lower Patapsco Aquifer in Southern Maryland, September 1990 and September 2007

    USGS Publications Warehouse

    Curtin, Stephen E.; Andreasen, David C.; Staley, Andrew W.

    2009-01-01

    This report presents a map showing the change in the potentiometric surface of the lower Patapsco aquifer in the Patapsco Formation of Early Cretaceous age in Southern Maryland for September 1990 and September 2007. The map, based on water-level measurements in 45 wells, shows that the change of the potentiometric surface during the 17-year period ranged from increases of 19 feet at Indian Head and 6 feet near the outcrop area in Glen Burnie, to declines of 41 feet at Arnold, 45 feet at Severndale, 68 feet at Crofton Meadows, 77 feet at Waldorf, 76 feet at La Plata, 28 feet at the Morgantown power plant, and 35 feet at the Swan Point subdivision south of Morgantown.

  18. Potentiometric sensors doped with biomolecules as a new approach to small molecule/biomolecule binding kinetics analysis.

    PubMed

    Daems, D; De Wael, K; Vissenberg, K; Van Camp, G; Nagels, L

    2014-04-15

    The most successful binding kinetics analysis systems at this moment include surface plasmon resonance (SPR), quartz microcrystal balance (QMB) and surface acoustic wave (SAW). Although these are powerful methods, they generally are complex, expensive and require the use of monolayers. Here, we report on potentiometric sensors as an inexpensive and simple alternative to do binding kinetics analysis between small molecules in solution and biomolecules (covalently) attached in a biopolymer sensor coating layer. As an example, dopamine and an anti-dopamine aptamer were used as the small molecule and the biomolecule respectively. Binding between both follows a Langmuir adsorption type model and creates a surface potential. The system operates in Flow Injection Analysis mode (FIA). Besides being an interesting new binding kinetics tool, the approach allows systematic design of potentiometric biosensors (in the present study a dopamine sensor), and gives new insights into the functioning of ion-selective electrodes (ISE's). PMID:24325980

  19. Determination of organic pharmaceuticals with N-bromosuccinimide. Part 4. Some pyrazolone derivatives by back titration

    TOXLINE Toxicology Bibliographic Information

    Amer MM; El-Zeany BA; Taha AM; El-Sawy OA

    IPA COPYRIGHT: ASHP A back titration method is described for the determination of pyrazolone derivatives with N-bromosuccinimide. A reaction mechanism involving quaternization of the N-methyl group at the 2-position, followed by ring cleavage and bromination of the aromatic ring is proposed; this was confirmed by NMR spectral analysis of the brominated phenazone.

  20. The Simulation of an Oxidation-Reduction Titration Curve with Computer Algebra

    ERIC Educational Resources Information Center

    Whiteley, Richard V., Jr.

    2015-01-01

    Although the simulation of an oxidation/reduction titration curve is an important exercise in an undergraduate course in quantitative analysis, that exercise is frequently simplified to accommodate computational limitations. With the use of readily available computer algebra systems, however, such curves for complicated systems can be generated…

  1. Charge Density Quantification of Polyelectrolyte Polysaccharides by Conductometric Titration: An Analytical Chemistry Experiment

    ERIC Educational Resources Information Center

    Farris, Stefano; Mora, Luigi; Capretti, Giorgio; Piergiovanni, Luciano

    2012-01-01

    An easy analytical method for determination of the charge density of polyelectrolytes, including polysaccharides and other biopolymers, is presented. The basic principles of conductometric titration, which is used in the pulp and paper industry as well as in colloid and interface science, were adapted to quantify the charge densities of a…

  2. Coulometric Titration of Ethylenediaminetetraacetate (EDTA) with Spectrophotometric Endpoint Detection: An Experiment for the Instrumental Analysis Laboratory

    ERIC Educational Resources Information Center

    Williams, Kathryn R.; Young, Vaneica Y.; Killian, Benjamin J.

    2011-01-01

    Ethylenediaminetetraacetate (EDTA) is commonly used as an anticoagulant in blood-collection procedures. In this experiment for the instrumental analysis laboratory, students determine the quantity of EDTA in commercial collection tubes by coulometric titration with electrolytically generated Cu[superscript 2+]. The endpoint is detected…

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

    PubMed

    Krainer, Georg; Keller, Sandro

    2015-04-01

    Isothermal titration calorimetry (ITC) is the gold standard for dissecting the thermodynamics of a biomolecular binding process within a single experiment. However, reliable determination of the dissociation constant (KD) from a single titration is typically limited to the range 100 μM>KD>1 nM. Interactions characterized by a lower KD can be assessed indirectly by so-called competition or displacement assays, provided that a suitable competitive ligand is available whose KD falls within the directly accessible window. However, this protocol is limited by the fact that it necessitates at least two titrations to characterize one high-affinity inhibitor, resulting in considerable consumption of both sample material and time. Here, we introduce a fast and efficient ITC displacement assay that allows for the simultaneous characterization of both a high-affinity ligand and a moderate-affinity ligand competing for the same binding site on a receptor within a single experiment. The protocol is based on a titration of the high-affinity ligand into a solution containing the moderate-affinity ligand bound to the receptor present in excess. The resulting biphasic binding isotherm enables accurate and precise determination of KD values and binding enthalpies (ΔH) of both ligands. We discuss the theoretical background underlying the approach, demonstrate its practical application to metal ion chelation, explore its potential and limitations with the aid of simulations and statistical analyses, and elaborate on potential applications to protein-inhibitor interactions. PMID:25461813

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

    ERIC Educational Resources Information Center

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

    2015-01-01

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

  5. Coulometric Titration of Ethylenediaminetetraacetate (EDTA) with Spectrophotometric Endpoint Detection: An Experiment for the Instrumental Analysis Laboratory

    ERIC Educational Resources Information Center

    Williams, Kathryn R.; Young, Vaneica Y.; Killian, Benjamin J.

    2011-01-01

    Ethylenediaminetetraacetate (EDTA) is commonly used as an anticoagulant in blood-collection procedures. In this experiment for the instrumental analysis laboratory, students determine the quantity of EDTA in commercial collection tubes by coulometric titration with electrolytically generated Cu[superscript 2+]. The endpoint is detected…

  6. Titration of Monoprotic Acids with Sodium Hydroxide Contaminated by Sodium Carbonate.

    ERIC Educational Resources Information Center

    Michalowski, Tadeusz

    1988-01-01

    Discusses the effects of using carbon dioxide contaminated sodium hydroxide solution as a titrant for a solution of a weak monoprotic acid and the resulting distortion of the titration curve in comparison to one obtained when an uncontaminated titrant is used. (CW)

  7. Tested Demonstrations: Comparison of Strong Acid and Weak Acid Titration Curves.

    ERIC Educational Resources Information Center

    Gilbert, George L., Ed.

    1979-01-01

    A lecture demonstration is presented for comparing titration curves. A plot of pH vs volume of strong base is produced by connecting the external output of a pH meter to a strip recorder. Thus, pH is recorded as a function of time. (BB)

  8. Charge Density Quantification of Polyelectrolyte Polysaccharides by Conductometric Titration: An Analytical Chemistry Experiment

    ERIC Educational Resources Information Center

    Farris, Stefano; Mora, Luigi; Capretti, Giorgio; Piergiovanni, Luciano

    2012-01-01

    An easy analytical method for determination of the charge density of polyelectrolytes, including polysaccharides and other biopolymers, is presented. The basic principles of conductometric titration, which is used in the pulp and paper industry as well as in colloid and interface science, were adapted to quantify the charge densities of a…

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

    ERIC Educational Resources Information Center

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

    2015-01-01

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

  10. The possibility of determining the activity coefficients of individual ions from acid-base titration data

    NASA Astrophysics Data System (ADS)

    Jano, I.; Hardcastle, J. E.

    1998-07-01

    A method is described for obtaining the activity coefficients of individual ions from experimental titration data. For this purpose, a general polyprotic acid-base-titration-curve equation is derived. The equation allows obtaining the dissociation equilibrium constants of the acid and the ratio of the activity coefficient of each ion to the activity coefficient of the undissociated acid directly from the titration data. Results obtained are compared with coefficients calculated using Debye-Hückel equation. A general equation relating the ionic strength to the pH of the titration medium is also established. Une méthode pour l'obtention des coefficients d'activité des ions individuels à partir des données expérimentales de titrage est établie. À ce but, une équation générale est dérivée pour représenter la courbe de titrage d'un acide avec une base. Cette équation permet d'obtenir les constants d'équilibre de dissociation de l'acide et le rapport de coefficient d'activité de chaque ion au coefficient d'activité de l'acide non-dissocié à partir des données de titrage. Les résultats ainsi obtenus sont comparés avec les coefficients calculés à l'aide de l'équation de Debye-Hückel. Une équation liant la force ionique au pH du milieu est établie aussi.

  11. Avian influenza virus isolation, propagation and titration in embryonated chicken eggs

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Avian influenza (AI) virus is usually isolated, propagated, and titrated in embryonated chickens eggs (ECE). Most any sample type can be accommodated for culture with appropriate processing. Isolation may also be accomplished in cell culture particularly if mammalian lineage isolates are suspected, ...

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

    Technology Transfer Automated Retrieval System (TEKTRAN)

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

  13. The Simulation of an Oxidation-Reduction Titration Curve with Computer Algebra

    ERIC Educational Resources Information Center

    Whiteley, Richard V., Jr.

    2015-01-01

    Although the simulation of an oxidation/reduction titration curve is an important exercise in an undergraduate course in quantitative analysis, that exercise is frequently simplified to accommodate computational limitations. With the use of readily available computer algebra systems, however, such curves for complicated systems can be generated…

  14. Titration of a Solid Acid Monitored by X-Ray Diffraction

    ERIC Educational Resources Information Center

    Dungey, Keenan E.; Epstein, Paul

    2007-01-01

    An experiment is described to introduce students to an important class of solid-state reactions while reinforcing concepts of titration by using a pH meter and a powder X-ray diffractometer. The experiment was successful in teaching students the abstract concepts of solid-state structure and diffraction by applying the diffraction concepts learned…

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

    PubMed

    Coelho, Lúcia H G; Gutz, Ivano G R

    2006-03-15

    A chemometric method for analysis of conductometric titration data was introduced to extend its applicability to lower concentrations and more complex acid-base systems. Auxiliary pH measurements were made during the titration to assist the calculation of the distribution of protonable species on base of known or guessed equilibrium constants. Conductivity values of each ionized or ionizable species possibly present in the sample were introduced in a general equation where the only unknown parameters were the total concentrations of (conjugated) bases and of strong electrolytes not involved in acid-base equilibria. All these concentrations were adjusted by a multiparametric nonlinear regression (NLR) method, based on the Levenberg-Marquardt algorithm. This first conductometric titration method with NLR analysis (CT-NLR) was successfully applied to simulated conductometric titration data and to synthetic samples with multiple components at concentrations as low as those found in rainwater (approximately 10 micromol L(-1)). It was possible to resolve and quantify mixtures containing a strong acid, formic acid, acetic acid, ammonium ion, bicarbonate and inert electrolyte with accuracy of 5% or better. PMID:18970555

  16. Solvatochromic Dyes as pH-Independent Indicators for Ionophore Nanosphere-Based Complexometric Titrations.

    PubMed

    Zhai, Jingying; Xie, Xiaojiang; Bakker, Eric

    2015-12-15

    For half a century, complexometric titrations of metal ions have been performed with water-soluble chelators and indicators that typically require careful pH control. Very recently, ion-selective nanosphere emulsions were introduced that exhibit ion-exchange properties and are doped with lipophilic ionophores originally developed for chemical ion sensors. They may serve as novel, highly selective and pH independent complexometric reagents. While ion optode emulsions have been demonstrated as useful indicators for such titrations, they exhibit a pH cross-response that unfortunately complicates the identification of the end point. Here, we present pH-independent optode nanospheres as indicators for complexometric titrations, with calcium as an initial example. The nanospheres incorporate an ionic solvatochromic dye (SD), ion exchanger and ionophore. The solvatochromic dye will be only expelled from the core of the nanosphere into the aqueous solution at the end point at which point it results in an optical signal change. The titration curves are demonstrated to be pH-independent and with sharper end points than with previously reported chromoionophore-based optical nanospheres as indicator. The calcium concentration in mineral water was successfully determined using this method. PMID:26595520

  17. Beta-blocker titration failure is independent of severity of heart failure.

    PubMed

    Anthonio, R L; van Veldhuisen, D J; Breekland, A; Crijns, H J; van Gilst, W H

    2000-02-15

    In the present study, predictors of complicated initiation of beta blockade in patients with idiopathic dilated cardiomyopathy was studied. We found that generally accepted measures of severity of heart failure are not predictable, whereas low systolic blood pressure (< or =120 mm Hg) was the strongest predictor for problematic (up)titration. PMID:10728963

  18. Titration of a Solid Acid Monitored by X-Ray Diffraction

    ERIC Educational Resources Information Center

    Dungey, Keenan E.; Epstein, Paul

    2007-01-01

    An experiment is described to introduce students to an important class of solid-state reactions while reinforcing concepts of titration by using a pH meter and a powder X-ray diffractometer. The experiment was successful in teaching students the abstract concepts of solid-state structure and diffraction by applying the diffraction concepts learned…

  19. 40 CFR Appendix A to Part 425 - Potassium Ferricyanide Titration Method

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 30 2014-07-01 2014-07-01 false Potassium Ferricyanide Titration Method A Appendix A to Part 425 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) EFFLUENT GUIDELINES AND STANDARDS (CONTINUED) LEATHER TANNING AND FINISHING POINT SOURCE CATEGORY Pt. 425, App. A Appendix A to Part...

  20. Monitoring unfractionated heparin therapy: relationship between eight anti-Xa assays and a protamine titration assay.

    PubMed

    Kitchen, S; Theaker, J; Preston, F E

    2000-03-01

    Several studies have demonstrated that heparin assays, such as anti-activated factor X (anti-Xa) assays, can be successfully substituted for activated partial thromboplastin time for heparin dosage monitoring. A number of different assays are available and the relationship between results with different techniques is largely unknown. The aim of the present study was to assess the relationship between heparin assays by protamine titration and anti-Xa assays. Samples were collected from 43 patients receiving unfractionated heparin (UFH). In each sample, the heparin level was determined using a protamine titration assay and eight commercially available anti-Xa assays. The mean heparin level by protamine titration was 0.31 U/ml. Mean anti-Xa activity results ranged from 0.40 to 0.42 IU/ml for the three clotting-based assays, and from 0.32 to 0.40 IU/ml for five chromogenic assays. Thus mean results of different anti-Xa assays varied by up to 30%. The range of anti-Xa activity equivalent, on average, to 0.2-0.4 U/ml by protamine titration, considered to be the therapeutic range, was approximately 0.25-0.5 IU/ml, depending on the assay. The relationship between results of clotting and chromogenic methods was similar irrespective of whether or not warfarin-induced prolongation of international normalized ratios was present. PMID:10759006

  1. Bacteriological analysis of water by potentiometric measurement of lipoic acid reduction: preliminary assays for selective detection of indicator organisms.

    PubMed

    Charriere, G; Jouenne, T; Lemeland, J F; Selegny, E; Junter, G A

    1984-01-01

    The practical task of adapting an original potentiometric technique to the bacteriological analysis of water is discussed. Various laboratory strains of organisms belonging to the usual aquatic flora were inoculated one by one in a minimal lactose broth supplied with lipoic (thioctic) acid. The time evolution of the redox potential of the cultures was followed during incubation by combined gold versus reference electrodes. When the incubation temperature was regulated at 36 degrees C, most organisms were able to grow and to reduce the coenzyme, generating changes in the redox potential of the culture. However, very few organisms developed significant reductive activity when the temperature was increased to 41 degrees C and when the broth was provided with sodium deoxycholate. Among the fecal coliform organisms, only Escherichia coli and Klebsiella pneumoniae exhibited early but reproducible potential-time responses. Positive potentiometric responses were also recorded with Acinetobacter calcoaceticus. E. coli showed rapid potentiometric signals as compared with K. pneumoniae. The time required for 100-mV shift of potential to be detected was related to the logarithm of the initial concentration of E. coli or K. pneumoniae in the culture broth. Experiments on natural surface water samples showed the the potentiometric method, associated with the selective incubation conditions, mainly detected E. coli among the bacterial flora of the tested environmental water. The calibration curve relating the time required for a 100-mV shift of potential to be detected to the number of fecal coliforms, as determined by control fecal coliform-selective plate counts, was consistent with the composite standard curve of detection times obtained with six different laboratory strains of E. coli.(ABSTRACT TRUNCATED AT 250 WORDS) PMID:6421230

  2. Hydrogen-ion titrations of amino acids and proteins in solutions containing concentrated electrolyte

    SciTech Connect

    Fergg, F.; Kuehner, D.E.; Blanch, H.W.; Prausnitz, J.M.

    1994-12-01

    This report describes a first attempt to quantify the net charge as a function of solution pH for lysozyme and {alpha}-chymotrypsin at 0.1 M, 1.0 M and 3.0 M ionic strength, (IS). The calculations are based on the residue (titratable group) pK{sub a}`s in the amino-acid sequence of the protein. To determine these pK{sub a}`s, a simple theory was used which assumes that the pK{sub a}`s are independent from each other in the protein and are equal to their pK{sub a} values in free amino-acid solution (Independent-Site Theory, IST). Residue pK{sub a}`s were obtained from amino-acid hydrogen-ion titrations at three different KCl concentrations corresponding to 0.1M, 1.0M and 3.0M ionic strength. After construction of a suitable apparatus, the experimental procedure and data reduction were computerized to perform a large number of titrations. Most measured pK{sub a}`s showed high reproducibility (the difference of pK{sub a} values observed between two experiments was less than 0.05). For IS = 0.1M, observed pK{sub a}`s agreed with literature values to within a few hundredths of a pH unit. Furthermore, the ionic-strength dependence of the pK{sub a}`s followed the trends reported in the literature, viz. pK{sub a} values decrease with increasing ionic strength until they reach a minimum at about IS = 0.5M. At still higher IS, pK{sub a}`s increase as the ionic strength rises to 3M. The known pK{sub a}`s of all titratable groups in a protein were used with the IST to give a first approximation of how the protein net charge varies with pH at high ionic strength. A comparison of the titration curves based on the IST with experimental lysozyme and {alpha}-chymotrypsin titration data indicates acceptable agreement at IS = 0.1M. However, comparison of measured and calculated titration curves at IS = 1M and IS = 3M indicates only quantitative agreement.

  3. Divalent cations induce protofibril gelation.

    PubMed

    Marx, G

    1988-02-01

    Soluble fibrin oligomers (protofibrils) undergo phase change merely by adding 1-2 mM Ca2+ or 25-100 microM Zn2+. The cation-induced "protofibrin" clots appear similar to normally formed fibrin gels. Maximal clot turbidity of protofibrin gels increases with cations in a concentration-dependent manner. Magnesium (less than 0.5 mM) is ineffective in inducing protofibril gelation. Turbidity and degree of polymerization (DP) [indirectly expressed as AT (activation time)] appear to be positively correlated, regardless of whether the divalent cation is Ca2+ or Zn2+. Cross sections of Ca2+-induced protofibrin fibers are approximately 6-18-fibrin-monomers-thick. With both Ca2+ and 40 microM Zn2+, fiber cross section increases to 30-50 monomers thick. Negatively stained Zn2+-and Ca2+-induced protofibrin gels exhibit banding periodicity of approximately 240 A, similar to that of normally generated fibrin gels. Regions of lateral merging of individual segments of the protofibrin leads to increased cross section of the fiber and forms a branch required for gelation. These findings indicate that the rate of coagulation and the ultimate thickness of the fibers both relate to lateral associative processes of protofibrils, which are augmented by physiologic concentrations of 2+ and Zn2+. PMID:3341371

  4. Gaseous protein cations are amphoteric

    SciTech Connect

    Stephenson, J.L. Jr.; McLuckey, S.A.

    1997-02-19

    Singly- and multiply-protonated ubiquitin molecules are found to react with iodide anions, and certain other anions, by attachment of the anion, in competition with proton transfer to the anion. The resulting adduct ions are relatively weakly bound and dissociate upon collisional activation by loss of the neutral acid derived from the anion. Adduct ions that behave similarly can also be formed via ion/molecule reactions involving the neutral acid. The ion/molecule reaction phenomenology, however, stands in contrast with that expected based on the reaction site(s) being charged. Reaction rates increase inversely with charge state and the total number of neutral molecules that add to the protein cations increases inversely with cation charge. These observations are inconsistent with the formation of proton-bound clusters but are fully consistent with the formation of ion pairs or dipole/dipole bonding involving the neutral acid and neutral basic sites in the protein. The ion/ion reactions can be interpreted on the basis of conjugate acid/base chemistry in which the anion, which is a strong gaseous base, reacts with a protonated site, which is a strong gaseous acid. Adduct ions can also be formed via ion/molecule reaction which, on the basis of microscopic reversibility, implies that the neutral acid interacts with neutral basic sites on the protein cation. 26 refs., 10 figs., 1 tab.

  5. Potentiometric bioimaging with a large-scale integration (LSI)-based electrochemical device for detection of enzyme activity.

    PubMed

    Kanno, Yusuke; Ino, Kosuke; Sakamoto, Chika; Inoue, Kumi Y; Matsudaira, Masahki; Suda, Atsushi; Kunikata, Ryota; Ishikawa, Tomohiro; Abe, Hiroya; Shiku, Hitoshi; Matsue, Tomokazu

    2016-03-15

    This paper describes potentiometric bioimaging for enzyme activity using a large-scale integration (LSI)-based electrochemical device with 400 sensors. Potentiometric detection is useful for bioimaging because redox species are not consumed or produced during the detection process; therefore, there is no effect on cell activity and the detectable signal is sustained. In this study, the potentiometer mode of the LSI-based device was applied for the detection of glucose oxidase (GOx) and alkaline phosphatase (ALP) activity. The enzyme activities were quantitatively detected within the concentration ranges of 25-250 μg/mL and 0.10-5.0 ng/mL. In addition, GOx activity in hydrogels and the ALP activity of embryoid bodies (EBs) from embryonic stem (ES) cells were successfully imaged based on detection of the open circuit potentials of individual sensors in real time. To the best of our knowledge, this is the first report of potentiometric imaging using LSI-based electrochemical arrays to detect enzyme activity in ES cells. The LSI-based device is thus demonstrated to be a promising tool for bioimaging of enzyme activity. PMID:26499066

  6. A new construction for a potentiometric, enantioselective membrane electrode--its utilization to the S-captopril assay.

    PubMed

    Stefan, R I; van Staden, J K; Aboul-Enein, H Y

    1999-05-01

    A novel potentiometric, enantioselective membrane electrode based on graphite paste (graphite powder and paraffin oil) has been constructed. The graphite paste is impregnated with 2-hydroxy-3-trimethylammoniopropyl-beta-cyclodextrin (as chloride salt) solution, 10(-3) mol l(-1). The potentiometric, enantioselective membrane electrode can be used reliable for S-captopril assay as raw material and from Novocaptopril tablets, using a chronopotentiometry (zero current) technique, in the 10(-6)-10(-2) mol l(-1) concentration range (detection limit 2 x 10(-7) mol l(-1)), with an average recovery of 99.99% (RSD=0.05%). The enantioselectivity was determined over R-captopril and D-proline. The response characteristics of the enantioselective, potentiometric membrane electrode were determined also for R-captopril. It was shown that only L-proline is the main interfering compound. The surface of the electrode can be regenerated by simply polishing, obtaining fresh surface ready to be used in a new assay. PMID:18967558

  7. Potentiometric-surface map of the Wyodak-Anderson Coal Bed, Powder River Structural Basin, Wyoming, 1973-84

    USGS Publications Warehouse

    Daddow, Pamela B.

    1986-01-01

    Previous water level maps of shallow aquifers in the Powder River structural basin in Wyoming were based on water levels from wells completed in different stratigraphic intervals within thick sequences of sedimentary rocks. A potentiometric surface using water levels from a single aquifer had never been mapped throughout the basin. The sandstone aquifers in the Fort Union Formation of Paleocene age and the Wasatch Formation of Eocene age are discontinuous and lenticular, and do not extend even short distances. Coal aquifers are more continuous and the Wyodak-Anderson coal bed, in the Fort Union Formation, has been mapped in much of the Powder River structural basin in Wyoming. Water level altitudes in the Wyodak-Anderson coal bed and other stratigraphically equivalent coal beds were mapped to determine if they represent a continuous potentiometric surface in the Powder River structural basin. The potentiometric surface, except in the vicinity of the Wyodak mine east of Gillette, represents a premining condition as it was based on water level measurements made during 1973-84 that were not significantly affected by mining. The map was prepared in cooperation with the U.S. Bureau of Land Management. (Lantz-PTT)

  8. Altitude of potentiometric surface, fall 1985, and historic water- level changes in the Memphis aquifer in western Tennessee

    USGS Publications Warehouse

    Parks, W.S.; Carmichael, J.K.

    1990-01-01

    Recharge to the Memphis aquifer of Tertiary age is from precipitation on the outcrop, which forms a broad belt across western Tennessee, or by downward infiltration of water from the overlying fluvial deposits of Tertiary and Quaternary age and alluvium of Quaternary age. In the outcrop-recharge belts, where the Memphis aquifer is under water-table conditions, the potentiometric surface is complex and generally resembles the topography. To the west of the outcrop-recharge belt where the Memphis aquifer is confined, the potentiometric surface gently slopes westward, and the water moves slowly in that direction. A major cone of depression in the potentiometric surface in the Memphis area is the result of long-term (1986-present) pumping at municipal and industrial well fields. Water levels in the Memphis aquifer have declined at average rates ranging from less than 0.1 to 1.3 ft/year during the period 1928-85. The largest declines have been in the Memphis area where withdrawals averaged about 191 million gal/day in 1985. Near the center of the major cone of depression in the Memphis area water levels ceased to decline in about 1975, and the center of the cone essentially has stabilized. Away from the center of the cone, water levels are still declining at a low rate, and the cone is still expanding as a result of the long-term effects of pumping. (USGS)

  9. The Quantitative Resolution of a Mixture of Group II Metal Ions by Thermometric Titration with EDTA. An Analytical Chemistry Experiment.

    ERIC Educational Resources Information Center

    Smith, Robert L.; Popham, Ronald E.

    1983-01-01

    Presents an experiment in thermometric titration used in an analytic chemistry-chemical instrumentation course, consisting of two titrations, one a mixture of calcium and magnesium, the other of calcium, magnesium, and barium ions. Provides equipment and solutions list/specifications, graphs, and discussion of results. (JM)

  10. Direct sensing of total acidity by chronopotentiometric flash titrations at polymer membrane ion-selective electrodes.

    PubMed

    Gemene, Kebede L; Bakker, Eric

    2008-05-15

    Polymer membrane ion-selective electrodes containing lipophilic ionophores are traditionally interrogated by zero current potentiometry, which, ideally, gives information on the sample activity of ionic species. It is shown here that a discrete cathodic current pulse across an H (+)-selective polymeric membrane doped with the ionophore ETH 5294 may be used for the chronopotentiometric detection of pH in well-buffered samples. However, a reduction in the buffer capacity leads to large deviations from the expected Nernstian response slope. This is explained by the local depletion of hydrogen ions at the sample-membrane interface as a result of the galvanostatically imposed ion flux in direction of the membrane. This depletion is found to be a function of the total acidity of the sample and can be directly monitored chronopotentiometrically in a flash titration experiment. The subsequent application of a baseline potential pulse reverses the extraction process of the current pulse, allowing one to interrogate the sample with minimal perturbation. In one protocol, total acidity is found to be proportional to the magnitude of applied current at the flash titration end point. More conveniently, the square root of the flash titration end point time observed at a fixed applied current is a linear function of the total acid concentration. This suggests that it is possible to perform rapid localized pH titrations at ion-selective electrodes without the need for volumetric titrimetry. The technique is explored here for acetic acid, MES and citric acid with promising results. Polymeric membrane electrodes based on poly(vinyl chloride) plasticized with o-nitrophenyl octyl ether in a 1:2 mass ratio may be used for the detection of acids of up to ca. 1 mM concentration, with flash titration times on the order of a few seconds. Possible limitations of the technique are discussed, including variations of the acid diffusion coefficients and influence of electrical migration. PMID:18370399

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

    NASA Astrophysics Data System (ADS)

    Turner, Benjamin F.; Fein, Jeremy B.

    2006-11-01

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

  12. Potentiometric surface of the Deadwood Aquifer in the Black Hills area, South Dakota

    USGS Publications Warehouse

    Strobel, Michael L.; Galloway, Joel M.; Hamade, Ghaith R.; Jarrell, Gregory J.

    2000-01-01

    This map is a product of the Black Hills Hydrology Study, which was initiated in 1990 to assess the quantity, quality, and distribution of surface water and ground water in the Black Hills area of South Dakota (Driscoll, 1992). This long-term study is a cooperative effort between the U.S. Geological Survey (USGS), the South Dakota Department of Environment and Natural Resources, and the West Dakota Water Development District, which represents various local and county cooperators. This map is part of a series of 1:100,000-scale maps for the study. The maps include a hydrogeologic map, structure-contour maps (altitudes of the tops of formations) for five formations that contain major aquifers in the study area, and potentiometric maps for these five major aquifers (the Inyan Kara, Minnekahta, Minnelusa, Madison, and Deadwood aquifers).The study area consists of the topographically defined Black Hills and adjacent areas located in western South Dakota. The Black Hills area is an elongated, dome-shaped feature, about 125 miles long and 60 miles wide, which was uplifted during the Laramide orogeny (Feldman and Heimlich, 1980). The oldest geologic units in the study area are Precambrian metamorphic and igneous rocks, which are exposed in the central core of the Black Hills. Surrounding the Precambrian core is a layered series of sedimentary rocks including limestones, sandstones, and shales that are exposed in roughly concentric rings around the uplifted flanks of the Black Hills. The bedrock sedimentary units typically dip away from the uplifted Black Hills at angles that approach or exceed 10 degrees near the outcrops, and decrease with distance from the uplift. Many of the sedimentary units contain aquifers, both within and beyond the study area. Recharge to these aquifers occurs from infiltration of precipitation upon the outcrops and, in some cases, from infiltration of streamflow (Hortness and Driscoll, 1998). Artesian conditions generally exist within these aquifers where an upper confining layer is present. Flowing wells and springs that originate from the confined aquifers are common around the periphery of the Black Hills.The purpose of this map is to show the potentiometric surface of the Deadwood aquifer within the study area. The map provides a tool for evaluating ground-water flow directions and hydraulic gradients in the Deadwood aquifer.

  13. Determination of acetylsalicylic acid by FIA-potentiometric system in drugs after on-line hydrolysis.

    PubMed

    Kubota, L T; Fernandes, J C; Rover, L; Neto, G de O

    1999-10-01

    A potentiometric flow injection (FI) system was developed for the acetylsalicylic acid (ASA) determination in drugs, without previous treatment. The tubular potentiometric electrode for salicylate (SA) was based on tricaprylyl-trimethyl-ammonium-salicylate (aliquat-salicylate) as the ion-exchanger, supported on poly(ethylene-co-vinyl-acetate) (EVA) matrix and applied directly onto a conducting support. The standards and samples were freshly prepared in ethanol solution (0.10 mol l(-1) Tris-SO(4) buffer, pH 8.0, containing 0.25 mol l(-1) Na(2)SO(4) and 8.0% v/v ethanol) to facilitate the dissolution of ASA and were injected directly into the system. The SA formed due to the on-line alkaline hydrolysis of alcoholic ASA solution, with 0.50 mol l(-1) NaOH (coil, 50 cm length), was monitored by the tubular electrode after neutralization with 0.25 mol l(-1) H(2)SO(4). A solution of 0.10 mol l(-1) Tris-SO(4) buffer (pH 8.0), containing 0.25 mol l(-1) Na(2)SO(4) was employed as carrier. In optimized conditions (flow rate of 2.1 ml min(-1) and volume of injection of 150 mul), the tubular electrode showed a linear response to ASA in the concentration range between 4.0x10(-3) and 4.0x10(-2) mol l(-1). A conversion factor of ASA to SA of 85% occurs in these conditions with an increase of about 130% in the signal to the system with on-line hydrolysis (three-channel) in comparison to the system without (one-channel). The response time of the electrode was about 5 s with an analytical frequency of 28 samples per h and a relative standard deviation (R.S.D.) of 2.1% for 30 successive injections. Determinations of ASA in tablet samples by the proposed method exhibited relative differences of 1.0-3.5%, compared to the official method of the British Pharmacopoeia. The useful lifetime of the sensor was greater than 1 month, in continuous use. PMID:18967757

  14. Solid-state potentiometric sensors for nitrogen monoxide, nitrogen dioxide, and carbon monoxide

    NASA Astrophysics Data System (ADS)

    White, Briggs Mckenney

    There is currently a large need for the development of solid-state potentiometric sensors for monitoring the NOX emanating from combustion processes. In an effort to better understand the phenomena behind the sensor response, sensors of the form: La2CuO4|YSZ|Pt were investigated. These sensors showed promising results. The effect of electrode microstructure on sensor response time and sensitivity was investigated. Electrodes that have high surface/bulk ratios respond faster and are more sensitive than electrodes with low surface/bulk ratios. They are also stable at lower operating temperatures where signals are inherently larger. The resistance of La2CuO4, a p-type semiconductor, was measured as a function of various pollutants to verify that the possibility that Fermi level changes are responsible for the potentiometric response of the sensor. The resistance of La2CuO4 and the potential of La2CuO4|YSZ|Pt sensors have similar dependencies on temperature and NOX/CO concentration. This correspondence along with temperature-programmed desorption results suggest that the adsorption/desorption of NOX/CO on/from La2CuO4 shifts the Fermi level and is measured by the electrometer as the electrode potential. The electrochemistry at Pt and La2CuO4 electrodes in NOX environments was investigated with D.C. polarization and electrochemical impedance spectroscopy. The polarization resistance values for both electrodes decreased with increasing concentrations of NO and NO 2. Theoretical considerations and experimental approaches were refined concerning three-electrode polarization measurements in the solid-state. Using an independent reference electrode, the sensor response was shown to be a composite of the individual electrode responses. In the case of O 2, the potentials of both electrodes change significantly; however, they do so in identical fashion and the net sensor signal is insignificant to O2. The sensor responds to NO, NO2, and CO because the Fermi level of the La2CuO4 shifts when they adsorb on it. This contribution to the sensor response is often overlooked; however, in the case of La2CuO4-based sensors it is not only a contributor to the response, it dominants the response. In other words, the sensor response is the net difference between the sums of the electrode potential contributions (heterogeneous catalysis, adsorption/desorption, and electrochemical reactions) or in other words, the "Differential Electrode Equilibria."

  15. Cationic micellar nanoparticles for DNA and doxorubicin co-delivery.

    PubMed

    Lin, Jian-Tao; Zou, Ying; Wang, Chao; Zhong, Yue-Chun; Zhao, Yi; Zhu, Hui-Er; Wang, Guan-Hai; Zhang, Li-Ming; Zheng, Xue-Bao

    2014-11-01

    Cationic micellar nanoparticles for chemotherapeutic drugs and therapeutic gene co-delivery were prepared based on a poly-(N-?-carbobenzyloxy-l-lysine) (PZLL) and dendritic polyamidoamine (PAMAM) block copolymer (PZLL-D3). PZLL-D3 was synthesized by a copper-catalyzed azide alkyne cyclization (click) reaction between ?-alkyne-PZLL and azide focal point PAMAM dendrons. Its structure was characterized by (1)H NMR and FTIR, and its buffering capability was determined by acid-base titration. MTT, agarose gel electrophoresis and flow cytometry studies showed that PZLL-D3 revealed low in vitro cytotoxicity, strong pDNA condensation ability, protection of pDNA against deoxyribonuclease I degradation and high gene transfection efficiency in 293T and HeLa cells. In addition, the micellar nanoparticles delivered pDNA and anticancer drug doxorubicin (DOX) simultaneously and efficiently to tumor cells, and the DOX loaded nanoparticles showed sustained in vitro release at pH=7.4 and 5.8. PMID:25280725

  16. Weak protein-cationic co-ion interactions addressed by X-ray crystallography and mass spectrometry.

    PubMed

    Bénas, Philippe; Auzeil, Nicolas; Legrand, Laurent; Brachet, Franck; Regazzetti, Anne; Riès-Kautt, Madeleine

    2014-08-01

    The adsorption of Rb(+), Cs(+), Mn(2+), Co(2+) and Yb(3+) onto the positively charged hen egg-white lysozyme (HEWL) has been investigated by solving 13 X-ray structures of HEWL crystallized with their chlorides and by applying electrospray ionization mass spectrometry (ESI-MS) first to dissolved protein crystals and then to the protein in buffered salt solutions. The number of bound cations follows the order Cs(+) < Mn(2+) ≃ Co(2+) < Yb(3+) at 293 K. HEWL binds less Rb(+) (qtot = 0.7) than Cs(+) (qtot = 3.9) at 100 K. Crystal flash-cooling drastically increases the binding of Cs(+), but poorly affects that of Yb(3+), suggesting different interactions. The addition of glycerol increases the number of bound Yb(3+) cations, but only slightly increases that of Rb(+). HEWL titrations with the same chlorides, followed by ESI-MS analysis, show that only about 10% of HEWL binds Cs(+) and about 40% binds 1-2 Yb(3+) cations, while the highest binding reaches 60-70% for protein binding 1-3 Mn(2+) or Co(2+) cations. The binding sites identified by X-ray crystallography show that the monovalent Rb(+) and Cs(+) preferentially bind to carbonyl groups, whereas the multivalent Mn(2+), Co(2+) and Yb(3+) interact with carboxylic groups. This work elucidates the basis of the effect of the Hofmeister cation series on protein solubility. PMID:25084340

  17. Computational prediction and experimental selectivity coefficients for hydroxyzine and cetirizine molecularly imprinted polymer based potentiometric sensors.

    PubMed

    Azimi, Abolfazl; Javanbakht, Mehran

    2014-02-17

    In spite of the increasing usages number of molecularly imprinted polymers (MIPs) in many scientific applications, the theoretical aspects of participating intra molecular forces are not fully understood. This work investigates effects of the electrostatic force, the Mulliken charge and the role of cavity's backbone atoms on the selectivity of MIPs. Moreover, charge distribution, which is a computational parameter, was proposed for the prediction of the selectivity coefficients of MIP-based sensors. In the computational approaches and experimental study, methacrylic acid (MAA) was chosen as the functional monomer and ethylene glycol dimethacrylate (EGDMA) as the cross linker for hydroxyzine and cetirizine imprinted polymers. Ab initio, DFT B3LYP method was carried out on molecular optimization. With regard to results obtained from molecules optimization and hydrogen bonding properties, possible configurations of 1:n (n?5) template/monomer complexes were designed and optimized. The binding energy for each complex in gas phase was calculated. Depending on the most stable configuration, hydroxyzine and cetirizine imprinted polymer models were designed. The calculations including the porogen were also investigated. The theoretical charge distributions for the template and some potential interfering molecules were calculated. The results showed a correlation between the selectivity coefficients and the theoretical charge distributions. The results surprisingly show that charge distribution based model was able to predict the selectivity coefficients of MIP based potentiometric sensors. PMID:24491780

  18. A highly selective potentiometric sensor of molybdate based on a mu-oxo-bridged manganeseporphyrin dimer.

    PubMed

    Fang, Zheng-Hui; Han, Zhi-Xiang; Zhang, Xiao-Bing; Shen, Guo-Li; Yu, Ru-Qin

    2006-07-01

    A novel high-selective potentiometric sensor for molybdate was prepared with a PVC membrane combining mu-oxo-bis[5,10,15,20-tetra(p-methylphenyl)porphinatomanganese(III)] [[Mn(p-Me)TPP](2)O] as an electroactive material and 2-nitrophenyl octyl ether (o-NPOE) as a plasticizer in the percentage ratio of 3:65:32, [Mn(p-Me)TPP](2)O:o-NPOE:PVC (w:w). The sensor exhibited a linear response with a Nernstian slope of 30.5 mV per decade within a concentration range of 2.1 x 10(-6) to 1.0 x 10(-1) M MoO4(2-), with a working pH range from 5.0 to 12.5, and a fast response time of less than 15 s. The electrode showed improved selectivity toward molybdate with respect to common coexisting anions compared to monometalloporphyrin counterparts. Several electroactive materials and solvent mediators were compared and the experimental conditions were optimized. The sensor is preliminary applied to the assay of MoO4(2-) in corrosion inhibitor samples with satisfactory results. PMID:16837744

  19. Potentiometric combination ion/carbon dioxide sensors for in vitro and in vivo blood measurements.

    PubMed

    Collison, M E; Aebli, G V; Petty, J; Meyerhoff, M E

    1989-11-01

    The development and analytical performance of a novel potentiometric combination ion/pCO2 sensor design for in vitro and in vivo measurements are reported. The design is based on incorporating an appropriate ionophore within the outer silicone gas permeable membranes of both conventional macro and new catheter-type pCO2 sensors. Simultaneous measurement of the potentials across the ion-selective/gas permeable membrane and the inner glass or polymer pH sensitive membrane provides the basis for continuous monitoring of both ionic and pCO2 levels with the same device. A macro-sized K+/pCO2 embodiment of the sensor is constructed from a commercial Severinghaus CO2 sensor and is used to demonstrate the principles and capabilities of the proposed design. A flexible, miniaturized (outer diameter = 1.2 mm) combination K+/pCO2 catheter sensor is also described. The catheter-type sensor is fabricated by inserting a tubular polymer membrane pH electrode into an outer silicone rubber tube doped with valinomycin. Continuous measurements of K+ and pCO2 during 6-h blood pump studies using both the macro and catheter-type combination sensors correlate well with those of conventional bench-top analyzers. In addition, continuous (4 h) intravascular measurements with the combination catheter sensor in dogs show good agreement with those of commercial blood analyzers (R = 0.984 and 0.962 for pCO2 and K+, respectively. PMID:2510554

  20. Development of novel potentiometric sensors for determination of tartrazine dye concentration in foodstuff products.

    PubMed

    Abu Shawish, Hazem M; Ghalwa, Nasser Abu; Saadeh, Salman M; El Harazeen, Heba

    2013-05-01

    Tartrazine dye Na(3)TZ in foodstuff products was determined by a new modified carbon paste electrode, encoded sensor A, and a coated silver wire electrode, encoded sensor B, based on tartrazine TZ- cetryltrimethyl ammoniumbromide CTAB as a chemical modifier TZ-CTA. The electrodes exhibit the following characteristics listed respectively: a Nernstian slope of 17.9±0.5 and 19.4±0.2 mV/decade for tartrazine ion over a wide concentration range from 4.3×10(-7) to 1.0×10(-2) and 1.1×10(-7) to 1.0×10(-2) M. The lower detection limits: 3.2×10(-7) and 5.5×10(-8) M. Short response time (5-8 s) over the pH range 3.8-7.7 and 4.2-8.1. The proposed sensors display significantly high selectivity for TZ ion over a wide variety of sugars, some anions, common organic, inorganic compounds and additives. The developed electrodes were applied to the potentiometric determination of tartrazine ion in different kinds of foodstuffs: solid jelly (strawberry and custard) powder samples and soft drink (orange) samples with satisfactory results. PMID:23265466

  1. A potentiometric biosensor for the detection of notch 3 using functionalized ZnO nanorods.

    PubMed

    Ibupoto, Z H; Khun, K; Liu, X; Willander, M

    2014-09-01

    The notch signalling plays a vital and radical role for the activity of cellular proliferation, differentiation and apoptosis. In this study, for the first time a particular biosensor is developed for the detection of notch 3. ZnO nanorods were fabricated on the gold coated glass substrate by hydrothermal method and afterwards were decorated with the gold nanoparticles by electrodepositing technique. Scanning electron microscopy (SEM) has shown the perpendicular to the substrate growth pattern of ZnO nanorods. X-ray diffraction (XRD) studies showed the c-axis oriented growth direction with wurtzite crystal structure of ZnO nanorods. X-ray Photoelectron Spectroscopy (XPS) and energy dispersive X-ray (EDX) techniques have shown the presence of Zn, O and Au atoms in the prepared functional material. Furthermore, the anti-notch 3 was physically adsorbed on the gold nanoparticles functionalized ZnO nanorods. The developed potentiometric immunosensor has shown response to the wide range of notch 3 molecules. The detected range included 1.00 x 10(-5)-1.50 x 10(0 ) ?g/mL with a sensitivity of 23.15 ± 0.31 mV/decade. The analytical parameters including reproducibility, stability, and selectivity were also investigated and the observed results indicate the acceptable performance of the notch 3 biosensor. Moreover, the proposed notch 3 biosensor exhibited a fast response time of 10 s. PMID:25924320

  2. Development of potentiometric equipment for the identification of altered dry-cured hams: A preliminary study.

    PubMed

    Girón, Joel; Gil-Sánchez, Luís; García-Breijo, Eduardo; Pagán, M Jesús; Barat, José M; Grau, Raúl

    2015-08-01

    Microbiological contamination in dry-cured ham can occur in the early stages of the process, a large number of microorganisms involved in spoilage can produce alterations in the product. These include non-common odours, which are detected at the end of the process by a procedure called "cala", consisting of a sharp instrument punctured in every ham; this is smelled by an expert taster, who classifies hams as good and altered hams. An electronic device would be suitable for this process given the large amount of hams. The present research aims to develop objective equipment based on the potentiometry technique that identifies altered hams. A probe was developed, containing silver, nickel and copper electrodes, and was employed to classify altered and unaltered hams prior to classification by a tester. The results shown lower Ag and higher Cu potential values for altered hams. The differences in potentiometric response reveal a classification model, although further studies are required to obtain a reliable classification model. PMID:25839997

  3. Technical Note: Maximising accuracy and minimising cost of a potentiometrically regulated ocean acidification simulation system

    NASA Astrophysics Data System (ADS)

    MacLeod, C. D.; Doyle, H. L.; Currie, K. I.

    2015-02-01

    This article describes a potentiometric ocean acidification simulation system which automatically regulates pH through the injection of 100% CO2 gas into temperature-controlled seawater. The system is ideally suited to long-term experimental studies of the effect of acidification on biological processes involving small-bodied (10-20 mm) calcifying or non-calcifying organisms. Using hobbyist-grade equipment, the system was constructed for approximately USD 1200 per treatment unit (tank, pH regulation apparatus, chiller, pump/filter unit). An overall tolerance of ±0.05 pHT units (SD) was achieved over 90 days in two acidified treatments (7.60 and 7.40) at 12 °C using glass electrodes calibrated with synthetic seawater buffers, thereby preventing liquid junction error. The performance of the system was validated through the independent calculation of pHT (12 °C) using dissolved inorganic carbon and total alkalinity data taken from discrete acidified seawater samples. The system was used to compare the shell growth of the marine gastropod Zeacumantus subcarinatus infected with the trematode parasite Maritrema novaezealandensis with that of uninfected snails at pH levels of 7.4, 7.6, and 8.1.

  4. A polyaniline based ultrasensitive potentiometric immunosensor for cardiac troponin complex detection.

    PubMed

    Zhang, Qi; Prabhu, Alok; San, Avdar; Al-Sharab, Jafar F; Levon, Kalle

    2015-10-15

    An ultrasensitive immunosensor based on potentiometric ELISA for the detection of a cardiac biomarker, troponin I-T-C (Tn I-T-C) complex, was developed. The sensor fabrication involves typical sandwich ELISA procedures, while the final signal readout was achieved using open circuit potentiometry (OCP). Glassy carbon (GC) working electrodes were first coated with emulsion-polymerized polyaniline/dinonylnaphthalenesulfonic acid (PANI/DNNSA) and the coated surface was utilized as a transducer layer on which sandwich ELISA incubation steps were performed. An enzymatic reaction between o-phenylenediamine (OPD) and hydrogen peroxide (H2O2) was catalyzed by horseradish peroxidase (HRP) labeled on the secondary antibodies. The polymer transducer charged state was mediated through electron (e(-)) and charge transfers between the transducer and charged species generated by the same enzymatic reaction. Such a change in the polymer transducer led to potential variations against an Ag/AgCl reference electrode as a function of Tn I-T-C complex concentration during incubations. The sequence of OPD and H2O2 additions, electrochemical properties of the PANI/DNNSA layer and non-specific binding prevention were all crucial factors for the assay performance. Under optimized conditions, the assay has a low limit of detection (LOD) (< 5 pg/mL or 56 fM), a wide dynamic range (> 6 orders of magnitude), high repeatability (coefficient of variance < 8% for all concentrations higher than 5 pg/mL) and a short detection time (< 10 min). PMID:25966464

  5. Indirect trace determination of nitrilotriacetic acid in water by potentiometric stripping analysis

    SciTech Connect

    Fayyad, M.

    1987-01-01

    Release of the ligand nitrilotriacetic acid (NTA) into sewage systems and receiving waters resulting from its use in detergents as a phosphate substitute is causing great concern. Certain methods for its determination have been introduced, but the need for development of reliable and efficient techniques is still essential. The spectroscopic methods reported for the determination of NTA in natural waters are rather expensive to carry out, and even then their detection limit is typically above 100 ppb. Obviously they cannot be employed for trace determination of the ligand in water. Polarographic and voltammetric techniques can be used for the indirect determination of NTA by using a metal:NTA complex as a polarographic-active species. Detection limits of 50 ppb were reached without preconcentration. Recently an indirect trace determination of NTA in natural waters, using Bi:NTA complex, by differential pulse anodic stripping voltammetry has been reported. However, this method is affected by the nature of the electrolyte present in solution and its concentration. The authors now report the development of a simple, rapid, and reliable method for indirect trace determination of NTA by potentiometric stripping analysis (PSA).

  6. Synthesis, potentiometric and antimicrobial studies on metal complexes of isoxazole Schiff bases

    NASA Astrophysics Data System (ADS)

    Prashanthi, Y.; Kiranmai, K.; Subhashini, N. J. P.; Shivaraj

    2008-06-01

    The metal complexes of Cu(II), Ni(II) and Co(II) with Schiff bases of 3-(2-hydroxy-3-ethoxybenzylideneamino)-5-methyl isoxazole [HEBMI] and 3-(2-hydroxy-5-nitrobenzylidene amino)-5-methyl isoxazole [HNBMI] which were obtained by the condensation of 3-amino-5-methyl isoxazole with substituted salicylaldehydes have been synthesized. Schiff bases and their complexes have been characterized on the basis of elemental analysis, magnetic moments, molar conductivity, thermal analysis and spectral (IR, UV, NMR and Mass) studies. The spectral data show that these ligands act in a monovalent bidentate fashion, co-ordinating through phenolic oxygen and azomethine nitrogen atoms. Chelates of Co(II), Ni(II) appear to be octahedral and Cu(II) appears to be distorted octahedral. To investigate the relationship between formation constants of binary complexes and antimicrobial activity, the dissociation constants of Schiff bases and stability constants of their binary metal complexes have been determined potentiometrically in aqueous solution at 30 ± 1 °C and at 0.1 M KNO 3 ionic strength and discussed. Antimicrobial activities of the Schiff bases and their complexes were screened. The structure-activity correlation in Schiff bases and their metal(II) complexes are discussed, based on the effect of their stability constants. It is observed that the activity enhances upon complexation and the order of activity is in accordance with stability order of metal ions.

  7. A new potentiometric SO? sensor based on Li?PO? electrolyte film and its response characteristics.

    PubMed

    Wang, H; Liu, Z; Chen, D; Jiang, Z

    2015-07-01

    A potentiometric SO2 gas sensor based on Li3PO4 solid electrolyte has been developed using Au as the reference electrode and Li2SO4/V2O5 as the sensing electrode. The Li3PO4 film was deposited on Al2O3 substrate by resistance heating evaporation. Two Au films with designed patterns were formed on the Li3PO4 film by micro-fabrication technologies. The sensing electrode covers one electrode partly using thick-film technology. The electromotive force values between the sensing electrode and the reference electrode were measured and various characteristics were studied including sensitivity, response characteristics, and stability and selectivity. According to the results, we conclude that an optimal working temperature of the SO2 sensor is 500?°C, the measurement range is 0-100 ppm, the sensitivity is about 32.47 mV/dec, the response and the recovery time is about 5 min and 10 min, respectively. And the stability and the selectivity of the sensor are good, making it have potential in SO2 measurement of living environment. PMID:26233408

  8. Technical Note: Maximising accuracy and minimising cost of a potentiometrically regulated ocean acidification simulation system

    NASA Astrophysics Data System (ADS)

    MacLeod, C. D.; Doyle, H. L.; Currie, K. I.

    2014-05-01

    This article describes a potentiometric ocean acidification simulation system which automatically regulates pH through the injection of 100% CO2 gas into temperature-controlled seawater. The system is ideally suited to long-term experimental studies of the effect of acidification on biological processes involving small-bodied (10-20 mm) calcifying or non-calcifying organisms. Using hobbyist grade equipment, the system was constructed for approximately USD 1200 per treatment unit (tank, pH regulation apparatus, chiller, pump/filter unit). An overall accuracy of ±0.05 pHT units (SD) was achieved over 90 days in two acidified treatments (7.60 and 7.40) at 12 °C using glass electrodes calibrated with salt water buffers, thereby preventing liquid junction error. The accuracy of the system was validated through the independent calculation of pHT (12 °C) using dissolved inorganic carbon (DIC) and total alkalinity (AT) data taken from discrete acidified seawater samples. The system was used to compare the shell growth of the marine gastropod Zeacumantus subcarinatus infected with the trematode parasite Maritrema novaezealandensis with that of uninfected snails, at pH levels of 7.4, 7.6, and 8.1.

  9. Cation disorder in shocked orthopyroxene.

    NASA Technical Reports Server (NTRS)

    Dundon, R. W.; Hafner, S. S.

    1971-01-01

    The study of cation distributions over nonequivalent lattice sites in minerals may reveal information on the history of temperature and pressure in rocks. Chemically homogeneous orthopyroxene specimens were shocked under well-controlled conditions in the laboratory in order to provide a basis for the interpretation of more complex natural materials. As a result of the investigation it is concluded that the distribution of magnesium and iron over the M1 and M2 positions in Bamle enstatite shocked at 1 megabar is highly disordered. It corresponds to an equilibrium distribution of at least 1000 C.

  10. Resorcarene-based receptor: versatile behavior in its interaction with heavy and soft metal cations.

    PubMed

    Danil de Namor, Angela F; Chaaban, Jinane K; Piro, Oscar E; Castellano, Eduardo E

    2006-02-01

    Standard solution Gibbs energies, DeltasG degrees, of the resorcarene-based receptor 5,11,17,23-ethylthiomethylated calix[4]resorcarene, (characterized by 1H NMR and X-ray diffraction studies) in its monomeric state (established through partition experiments) in various solvents are for the first time reported in the area of resorcarene chemistry. Transfer Gibbs energies of from hexane (reference solvent) to other medium are calculated. Agreement between DeltatG degrees (referred to the pure solvents) and standard partition Gibbs energies, DeltapG degrees (solvent mutually saturated) is found. Cation-ligand interactions were investigated through 1H NMR (CD3CN and CD3OD) and conductometric titrations in acetonitrile and methanol. 1H NMR data revealed the sites of interaction of with the metal cation. The composition of the metal-ion complexes (Ag+ and Pb2+ in acetonitrile and Ag+ and Cu2+ in methanol) was established through conductometric titrations. Thus, complexes of 1:1 stoichiometry were formed between and Ag+ and Pb2+ in acetonitrile and Cu2+ in methanol. However, in moving from acetonitrile to methanol, the composition of the silver complex was altered. Thus, two metal cations are hosted by a unit of the ligand. As far as Cu2+ and in acetonitrile is concerned, conductance data suggest that metalates are formed in which up to four units of Cu2+ are taken up per unit of resorcarene. The contrasting behavior of with Cu2+ in acetonitrile relative to methanol is discussed. As far as mercury (II) is concerned, the unusual jump in conductance observed in the titration of Hg2+ with in acetonitrile and methanol after the formation of a multicharged complex (undefined composition) is attributed to the presence of highly charged smaller units (higher mobility) resulting from the departure of pendant arms from the resorcarene backbone. Isolation of these species followed by X-ray diffraction studies corroborated this statement. The thermodynamic characterization of metal-ion complexes of Ag+ and Pb2+ in acetonitrile and Cu2+ and Ag+ in methanol is reported. Final conclusions are given. PMID:16471836

  11. Tetrathiafulvalene-based azine ligands for anion and metal cation coordination

    PubMed Central

    Ayadi, Awatef; El Alamy, Aziz; Alévêque, Olivier; Allain, Magali; Zouari, Nabil; Bouachrine, Mohammed

    2015-01-01

    Summary The synthesis and full characterization of two tetrathiafulvalene-appended azine ligands, namely 2-([2,2’-bi(1,3-dithiolylidene)]-4-yl)-6-((2,4-dinitrophenyl)hydrazono)methyl)pyridine (L1) and 5-([2,2’-bi(1,3-dithiolylidene)]-4-yl)-2-((2,4-dinitrophenyl)hydrazono)methyl)pyridine (L2) are described. The crystal structure of ligand L1 indicates that the ligand is completely planar with the presence of a strong intramolecular N3–H3···O1 hydrogen bonding. Titration experiments with inorganic anions showed that both ligands are suitable candidates for the sensing of fluoride anions. Ligand L2 was reacted with a Re(I) cation to yield the corresponding rhenium tricarbonyl complex 3. In the crystal structure of the newly prepared electroactive rhenium complex the TTF is neutral and the rhenium cation is hexacoordinated. The electrochemical behavior of the three compounds indicates that they are promising for the construction of crystalline radical cation salts. PMID:26425193

  12. Cyclic Group 15 Radical Cations.

    PubMed

    Brückner, Angelika; Hinz, Alexander; Priebe, Jacqueline B; Schulz, Axel; Villinger, Alexander

    2015-06-15

    Singlet cyclo-1,3-dipnicta-2,4-diazane-1,3-diyls of the type [E(?-NTer)2 E] (2, E=P, As, Ter=2,6-dimesitylphenyl) can undergo a one-electron-oxidation utilizing silver salts of weakly coordinating anions such as [AgLn][B(C6F5)4 ] (L=donor solvents) to afford the novel cyclic radical cations, [E(?-NTer)2E](+·) (3(+·)). When smaller and more basic anions were employed in the reaction, the anions were found to form covalent bonds to the radical centers yielding dipnictadiazanes, [FP(?-NTer)2PF] (5) and [(CF3CO2)P(?-NTer)2P(CF3CO2)] (6). A two-electron oxidation process, resulting in the formation of dications of the type [E(?-NTer)2E](2+), could not be observed. Computational and EPR data revealed that the spin density is almost completely localized at the two heavier pnictogen centers E of the former 1,3-dipnictadiazane-1,3-diyls. The bonding situation in the radical cations features a rare example of a transannular one-electron ? bond without having a ? bond. PMID:25960190

  13. Successful management of a difficult cancer pain patient by appropriate adjuvant and morphine titration.

    PubMed

    Rana, Shiv Ps; Ahmed, Arif; Kumar, Vindo; Chaudhary, Prakash K; Khurana, Deepa; Mishra, Seema

    2011-05-01

    Morphine has been used for many years to relieve cancer pain. Oral morphine (in either immediate release or modified release form) remains the analgesic of choice for moderate or severe cancer pain. The dose of oral morphine is titrated up to achieve adequate relief from pain with minimal side effects. Antidepressant and anticonvulsant drugs, when used in addition to conventional analgesics, give excellent relief from cancer pain. Most cancer pain responds to pharmacological measures with oral morphine but some pain like neuropathic and bony pain, pain in children and elderly age group, and advanced malignancy pain are very difficult to treat. Here, we report the management of a similar patient of severe cancer pain and the difficulty that we came across during dose titration of oral morphine and adjuvant analgesic. PMID:21976860

  14. Volumetric determination of uranium titanous sulfate as reductant before oxidimetric titration

    USGS Publications Warehouse

    Wahlberg, J.S.; Skinner, D.L.; Rader, L.F., Jr.

    1957-01-01

    Need for a more rapid volumetric method for the routine determination of uranium in uranium-rich materials has led to the development of a method that uses titanous sulfate as a reductant before oxidimetric titration. Separation of the hydrogen sulfide group is not necessary. Interfering elements precipitated by cupferron are removed by automatic filtrations made simultaneously rather than by the longer chloroform extraction method. Uranium is reduced from VI to IV by addition of an excess of titanous sulfate solution, cupric ion serving as an indicator by forming red metallic copper when reduction is complete. The copper is reoxidized by addition of mercuric perchlorate. The reduced uranium is then determined by addition of excess ferric sulfate and titration with ceric sulfate. The method has proved to be rapid, accurate, and economical.

  15. An automatic system for acidity determination based on sequential injection titration and the monosegmented flow approach.

    PubMed

    Kozak, Joanna; Wójtowicz, Marzena; Gawenda, Nadzieja; Ko?cielniak, Pawe?

    2011-06-15

    An automatic sequential injection system, combining monosegmented flow analysis, sequential injection analysis and sequential injection titration is proposed for acidity determination. The system enables controllable sample dilution and generation of standards of required concentration in a monosegmented sequential injection manner, sequential injection titration of the prepared solutions, data collecting, and handling. It has been tested on spectrophotometric determination of acetic, citric and phosphoric acids with sodium hydroxide used as a titrant and phenolphthalein or thymolphthalein (in the case of phosphoric acid determination) as indicators. Accuracy better than |4.4|% (RE) and repeatability better than 2.9% (RSD) have been obtained. It has been applied to the determination of total acidity in vinegars and various soft drinks. The system provides low sample (less than 0.3 mL) consumption. On average, analysis of a sample takes several minutes. PMID:21641455

  16. Standard test method for aluminum in iron ores by complexometric titration

    SciTech Connect

    Not Available

    1980-01-01

    This method covers the determination of aluminum in iron ores, concentrates, and agglomerates in the concentration range from 0.25 to 5% aluminium. The sample is fused in a zirconium crucible with a mixed flux of sodium carbonate and sodium peroxide. The fused mass is dissolved in dilute hydrochloric acid. The R/sub 2/O/sub 3/ hydroxides are precipitated with ammonia and redissolved in hydrochloric acid. Iron, titanium, etc., are removed with cupferron and chloroform. The aqueous phase is treated with nitric and perchloric acids and evaporated to dryness. After dissolving in dilute hydrochloric acid, the solution is filtered, and the filtrate is treated with an excess of ethylenediaminetetraacetic acid (EDTA). The excess EDTA is titrated with a standard zinc solution using xylenol orange indicator. Ammonium fluoride is added to release the EDTA bound to aluminum. This EDTA is then titrated with standard zinc solution, and the percent aluminum is calculated.

  17. Complexometric titration of total iron with o-mercaptobenzoic acid as indicator.

    PubMed

    Bhandari, L M; Khosla, M M; Rao, S P

    1970-02-01

    The soluble deep blue complex of iron(II) with o-mercaptobenzoic acid in aqueous pyridine medium (pH 6.4-7.4) can be titrated with EDTA at room temperature with a sharp colour change from blue to light yellow. o-Mercaptobenzoic acid forms a 2:1 complex with iron(II), maximum absorption at 600 nm. Its stability constant was found to be log K = 7.7. With iron(III), a transient blue colour is first formed which soon becomes colourless and then on the addition of excess of reagent, the deep blue complex is formed on reduction of the iron(III). Iron can be titrated in the presence of copper, if the latter is masked with sodium thiosulphate. Cobalt and nickel interfere. Common anions such as chloride, tartrate, phosphate, oxalate, citrate and acetate have no interference. PMID:18960715

  18. Determinations of Carbon Dioxide by Titration: New Experiments for General, Physical, and Quantitative Analysis Courses

    NASA Astrophysics Data System (ADS)

    Crossno, S. K.; Kalbus, L. H.; Kalbus, G. E.

    1996-02-01

    The determination of mixtures containing NaOH and Na2CO3 or Na2CO3 and NaHCO3 by titration is a common experiment in a Quantitative Analysis course. This determination can be adapted for the analysis of CO2 within a sample. The CO2 is released and absorbed in a solution containing excess NaOH. Titration with standard HCl leads to the determination of CO2 present in the sample. A number of interesting experiments in Quantitative Analysis, General and/or Physical Chemistry have been developed. Among these are the following determinations: CO2 content in carbonated beverages, carbonate and bicarbonate in various real life samples, and the molecular weight of CO2.

  19. Multicenter trial of automated nitroprusside infusion for postoperative hypertension. Titrator Multicenter Study Group.

    PubMed

    Chitwood, W R; Cosgrove, D M; Lust, R M

    1992-09-01

    Hypertension is common after a cardiac operation and may result in postoperative hemorrhagic and other complications. Most often this problem has been treated using manually controlled doses of intravenous sodium nitroprusside. To evaluate the clinical impact of an automated closed-loop administration system on patients after cardiotomy, a prospective trial was conducted at nine clinical centers. Patients with hypertension were managed by either manual nitroprusside titration (n = 532) or a closed-loop automated titration system (n = 557). Patient groups were not significantly different in age, weight, or height. Moreover, the types of surgical procedures were comparable: primary coronary artery bypass grafting, 59.2% and 58.9%, manual group versus automated group; repeat coronary artery bypass grafting, 10.5% and 8.6%, respectively; valve procedures, 11.3% and 15.1%, respectively; and other cardiac procedures, 19.0% and 17.4%, respectively (all p = not significant). The automated group showed a significant reduction in the number of hypertensive episodes per patient (1.8 +/- 0.2 versus 0.6 +/- 0.07; p = 0.0001. At the same time, the number of hypotensive episodes per patient was reduced with automated closed-loop titration (0.40 +/- 0.05 versus 0.30 +/- 0.03; p = 0.02). Chest tube drainage (866 +/- 37 mL versus 693 +/- 23 mL [mean +/- standard error of the mean]; p = 0.0001), percentage of patients receiving transfusion (40.0% versus 33.0%; p = 0.02), and total amount transfused (2.4 +/- 0.12 units versus 2.0 +/- 0.10 units; p = 0.0003) were all reduced significantly by the use of an automated titration system.(ABSTRACT TRUNCATED AT 250 WORDS) PMID:1510519

  20. Kinetic titration with differential thermometric determination of the end-point.

    PubMed

    Sajó, I

    1968-06-01

    A method has been described for the determination of concentrations below 10(-4)M by applying catalytic reactions and using thermometric end-point determination. A reference solution, identical with the sample solution except for catalyst, is titrated with catalyst solution until the rates of reaction become the same, as shown by a null deflection on a galvanometer connected via bridge circuits to two opposed thermistors placed in the solutions. PMID:18960338

  1. Reduction of sample volume and waste generation in acid/base titrations using microelectrodes

    SciTech Connect

    Ekechukwu, A.A.

    1996-03-22

    The Analytical Development Section (ADS) has developed microelectrode methods for use with pH titrations and pH determinations. These microelectrode methods offer increased sensitivity and enable analyses to be done with smaller sample and buffer volumes than are used with standard size electrodes. This report establishes the technical validity of the methods and describes the application of these methods to decreased detection limits, decreased waste generation, and decreased radiation exposure.

  2. Equivalence-point electromigration acid-base titration via moving neutralization boundary electrophoresis.

    PubMed

    Yang, Qing; Fan, Liu-Yin; Huang, Shan-Sheng; Zhang, Wei; Cao, Cheng-Xi

    2011-04-01

    In this paper, we developed a novel method of acid-base titration, viz. the electromigration acid-base titration (EABT), via a moving neutralization boundary (MNR). With HCl and NaOH as the model strong acid and base, respectively, we conducted the experiments on the EABT via the method of moving neutralization boundary for the first time. The experiments revealed that (i) the concentration of agarose gel, the voltage used and the content of background electrolyte (KCl) had evident influence on the boundary movement; (ii) the movement length was a function of the running time under the constant acid and base concentrations; and (iii) there was a good linearity between the length and natural logarithmic concentration of HCl under the optimized conditions, and the linearity could be used to detect the concentration of acid. The experiments further manifested that (i) the RSD values of intra-day and inter-day runs were less than 1.59 and 3.76%, respectively, indicating similar precision and stability in capillary electrophoresis or HPLC; (ii) the indicators with different pK(a) values had no obvious effect on EABT, distinguishing strong influence on the judgment of equivalence-point titration in the classic one; and (iii) the constant equivalence-point titration always existed in the EABT, rather than the classic volumetric analysis. Additionally, the EABT could be put to good use for the determination of actual acid concentrations. The experimental results achieved herein showed a new general guidance for the development of classic volumetric analysis and element (e.g. nitrogen) content analysis in protein chemistry. PMID:21462222

  3. Conformation and hydrogen ion titration of proteins: a continuum electrostatic model with conformational flexibility.

    PubMed Central

    You, T J; Bashford, D

    1995-01-01

    A new method for including local conformational flexibility in calculations of the hydrogen ion titration of proteins using macroscopic electrostatic models is presented. Intrinsic pKa values and electrostatic interactions between titrating sites are calculated from an ensemble of conformers in which the positions of titrating side chains are systematically varied. The method is applied to the Asp, Glu, and Tyr residues of hen lysozyme. The effects of different minimization and/or sampling protocols for both single-conformer and multi-conformer calculations are studied. For single-conformer calculations it is found that the results are sensitive to the choice of all-hydrogen versus polar-hydrogen-only atomic models and to the minimization protocol chosen. The best overall agreement of single-conformer calculations with experiment is obtained with an all-hydrogen model and either a two-step minimization process or minimization using a high dielectric constant. Multi-conformational calculations give significantly improved agreement with experiment, slightly smaller shifts between model compound pKa values and calculated intrinsic pKa values, and reduced sensitivity of the intrinsic pKa calculations to the initial details of the structure compared to single-conformer calculations. The extent of these improvements depends on the type of minimization used during the generation of conformers, with more extensive minimization giving greater improvements. The ordering of the titrations of the active-site residues, Glu-35 and Asp-52, is particularly sensitive to the minimization and sampling protocols used. The balance of strong site-site interactions in the active site suggests a need for including site-site conformational correlations. Images FIGURE 1 PMID:8580316

  4. Comparison of ozone determinations by ultraviolet photometry and gas-phase titration

    NASA Technical Reports Server (NTRS)

    Demore, W. B.; Patapoff, M.

    1976-01-01

    A comparison of ozone determinations based on ultraviolet absorption photometry and gas-phase titration (GPT) shows good agreement between the two methods. Together with other results, these findings indicate that three candidate reference methods for ozone, UV photometry, IR photometry, and GPT are in substantial agreement. However, the GPT method is not recommended for routine use by air pollution agencies for calibration of ozone monitors because of susceptibility to experimental error.

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

    PubMed

    Karita, Shingo; Kaneta, Takashi

    2014-12-16

    Rapid and simple acid-base titration was accomplished using a novel microfluidic paper-based analytical device (?PAD). The ?PAD was fabricated by wax printing and consisted of ten reservoirs for reaction and detection. The reaction reservoirs contained various amounts of a primary standard substance, potassium hydrogen phthalate (KHPth), whereas a constant amount of phenolphthalein was added to all the detection reservoirs. A sample solution containing NaOH was dropped onto the center of the ?PAD and was allowed to spread to the reaction reservoirs where the KHPth neutralized it. When the amount of NaOH exceeded that of the KHPth in the reaction reservoirs, unneutralized hydroxide ion penetrated the detection reservoirs, resulting in a color reaction from the phenolphthalein. Therefore, the number of the detection reservoirs with no color change determined the concentration of the NaOH in the sample solution. The titration was completed within 1 min by visually determining the end point, which required neither instrumentation nor software. The volumes of the KHPth and phenolphthalein solutions added to the corresponding reservoirs were optimized to obtain reproducible and accurate results for the concentration of NaOH. The ?PADs determined the concentration of NaOH at orders of magnitude ranging from 0.01 to 1 M. An acid sample, HCl, was also determined using Na2CO3 as a primary standard substance instead of KHPth. Furthermore, the ?PAD was applicable to the titrations of nitric acid, sulfuric acid, acetic acid, and ammonia solutions. The ?PADs were stable for more than 1 month when stored in darkness at room temperature, although this was reduced to only 5 days under daylight conditions. The analysis of acidic hot spring water was also demonstrated in the field using the ?PAD, and the results agreed well with those obtained by classic acid-base titration. PMID:25423320

  6. The ?-phosphorus hyperfine coupling constant in nitroxide: part 3: titration of water by electron paramagnetic resonance.

    PubMed

    Audran, Gérard; Bosco, Lionel; Brémond, Paul; Butscher, Teddy; Franconi, Jean-Michel; Marque, Sylvain R A; Mellet, Philippe; Parzy, Elodie; Santelli, Maurice; Thiaudière, Eric

    2015-12-14

    Recently, we showed that the phosphorus hyperfine coupling constant aP? of persistent cyclic nitroxides decreased with the normalized polarity Reichardt's constant E. Thus, we investigated the changes in aP? in binary mixtures of solvents. The sensitivity of aP? to the solvent was high enough to allow us to perform water titration in THF, 1,4-dioxane, and acetonitrile by EPR. Accuracies of a few percent were achieved. PMID:26395177

  7. Hydrogen ion titrations of the anodic and cathodic haemoglobin components of the European eel Anguilla anguilla.

    PubMed

    Brauner, C J; Weber, R E

    1998-09-01

    H+ titrations were conducted on the separated haemoglobin components of eel Anguilla anguilla in both the oxygenated and deoxygenated states. In anodic haemoglobin, the addition of GTP, and to a lesser extent C1-, increased the magnitude of the Haldane effect and shifted its maximum value into the in vivo pH range. Of the 22 histidine residues in the anodic component, only approximately seven were titratable, presumably the beta-chain residues at positions 41, 97, 109 and 146 (helical positions C7, FG4, G11 and HC3, respectively). In cathodic haemoglobin, a small negative Haldane effect was observed at pH values between 6.8 and 8.5 which disappeared in the presence of GTP (molar ratio 3:1 GTP:haemoglobin tetramer). GTP had virtually no effect on the buffer value at fixed oxygenation status, and the lowest buffer value was observed at in vivo pH values. No titratable histidine residues were observed in the cathodic component, indicating that all 14 histidines in this component are buried. We conclude that the anodic component, which constitutes two-thirds of the haemoglobin in the eel, plays the predominant role in CO2 transport and pH homeostasis in vivo. PMID:9698585

  8. Analysis of dose-response in flexible dose titration clinical studies.

    PubMed

    Xu, Xu Steven; Yuan, Min; Nandy, Partha

    2012-01-01

    Assessing dose-response from flexible-dose clinical trials (e.g., titration or dose escalation studies) is challenging and often problematic due to the selection bias caused by 'titration-to-response'. We investigate the performance of a dynamic linear mixed-effects (DLME) model and marginal structural model (MSM) in evaluating dose-response from flexible-dose titration clinical trials via simulations. The simulation results demonstrated that DLME models with previous exposure as a time-varying covariate may provide an unbiased and efficient estimator to recover exposure-response relationship from flexible-dose clinical trials. Although the MSM models with independent and exchangeable working correlations appeared to be able to recover the right direction of the dose-response relationship, it tended to over-correct selection bias and overestimated the underlying true dose-response. The MSM estimators were also associated with large variability in the parameter estimates. Therefore, DLME may be an appropriate modeling option in identifying dose-response when data from fixed-dose studies are absent or a fixed-dose design is unethical to be implemented. PMID:22407972

  9. EPR monitored redox titration of the cofactors of Saccharomyces cerevisiae Nar1.

    PubMed

    Hagedoorn, Peter-Leon; van der Weel, Laura; Hagen, Wilfred R

    2014-01-01

    Electron Paramagnetic Resonance (EPR) monitored redox titrations are a powerful method to determine the midpoint potential of cofactors in proteins and to identify and quantify the cofactors in their detectable redox state. The technique is complementary to direct electrochemistry (voltammetry) approaches, as it does not offer information on electron transfer rates, but does establish the identity and redox state of the cofactors in the protein under study. The technique is widely applicable to any protein containing an electron paramagnetic resonance (EPR) detectable cofactor. A typical titration requires 2 ml protein with a cofactor concentration in the range of 1-100 µM. The protein is titrated with a chemical reductant (sodium dithionite) or oxidant (potassium ferricyanide) in order to poise the sample at a certain potential. A platinum wire and a Ag/AgCl reference electrode are connected to a voltmeter to measure the potential of the protein solution A set of 13 different redox mediators is used to equilibrate between the redox cofactors of the protein and the electrodes. Samples are drawn at different potentials and the Electron Paramagnetic Resonance spectra, characteristic for the different redox cofactors in the protein, are measured. The plot of the signal intensity versus the sample potential is analyzed using the Nernst equation in order to determine the midpoint potential of the cofactor. PMID:25490157

  10. Automated spectrophotometric analyzer for rapid single-point titration of seawater total alkalinity.

    PubMed

    Li, Quanlong; Wang, Fengzhen; Wang, Zhaohui Aleck; Yuan, Dongxing; Dai, Minhan; Chen, Jinshun; Dai, Junwei; Hoering, Katherine A

    2013-10-01

    An automated analyzer was developed to achieve fast, precise, and accurate measurements of seawater total alkalinity (AT) based on single-point titration and spectrophotometric pH detection. The single-point titration was carried out in a circulating loop, which allowed the titrant (hydrochloric acid and bromocresol green solution) and a seawater sample to mix at a constant volume ratio. The dissolved CO2 in the sample-titrant mixture was efficiently removed by an inline CO2 remover, which consists of a gas-permeable tubing (Teflon AF2400) submerged in a sodium hydroxide (NaOH) solution. The pH of the mixture was then measured with a custom-made spectrophotometric detection system. The analyzer was calibrated against multiple certified reference materials (CRMs) with different AT values. The analyzer features a sample throughput time of 6.5 min with high precision (±0.33-0.36 ?mol kg(-1); n = 48) and accuracy (-0.33 ± 0.99 ?mol kg(-1); n = 10). Intercomparison to a traditional open-cell AT titrator showed overall good agreement of 0.88 ± 2.03 ?mol kg(-1) (n = 22). The analyzer achieved excellent stability without recalibration over 11 days, during which time 320 measurements were made with a total running time of over 40 h. Because of its small size, low power consumption requirements, and its ability to be automated, the new analyzer can be adapted for underway and in situ measurements. PMID:23968512

  11. Statistical mechanical model of coupled transcription from multiple promoters due to transcription factor titration

    PubMed Central

    Rydenfelt, Mattias; Cox, Robert Sidney; Garcia, Hernan; Phillips, Rob

    2014-01-01

    Transcription factors (TFs) with regulatory action at multiple promoter targets is the rule rather than the exception, with examples ranging from the cAMP receptor protein (CRP) in E. coli that regulates hundreds of different genes simultaneously to situations involving multiple copies of the same gene, such as plasmids, retrotransposons, or highly replicated viral DNA. When the number of TFs heavily exceeds the number of binding sites, TF binding to each promoter can be regarded as independent. However, when the number of TF molecules is comparable to the number of binding sites, TF titration will result in correlation (“promoter entanglement”) between transcription of different genes. We develop a statistical mechanical model which takes the TF titration effect into account and use it to predict both the level of gene expression for a general set of promoters and the resulting correlation in transcription rates of different genes. Our results show that the TF titration effect could be important for understanding gene expression in many regulatory settings. PMID:24580252

  12. Statistical mechanical model of coupled transcription from multiple promoters due to transcription factor titration

    NASA Astrophysics Data System (ADS)

    Rydenfelt, Mattias; Cox, Robert Sidney, III; Garcia, Hernan; Phillips, Rob

    2014-01-01

    Transcription factors (TFs) with regulatory action at multiple promoter targets is the rule rather than the exception, with examples ranging from the cAMP receptor protein (CRP) in E. coli that regulates hundreds of different genes simultaneously to situations involving multiple copies of the same gene, such as plasmids, retrotransposons, or highly replicated viral DNA. When the number of TFs heavily exceeds the number of binding sites, TF binding to each promoter can be regarded as independent. However, when the number of TF molecules is comparable to the number of binding sites, TF titration will result in correlation (“promoter entanglement”) between transcription of different genes. We develop a statistical mechanical model which takes the TF titration effect into account and use it to predict both the level of gene expression for a general set of promoters and the resulting correlation in transcription rates of different genes. Our results show that the TF titration effect could be important for understanding gene expression in many regulatory settings.

  13. Titration of biologically active amyloid-β seeds in a transgenic mouse model of Alzheimer's disease.

    PubMed

    Morales, Rodrigo; Bravo-Alegria, Javiera; Duran-Aniotz, Claudia; Soto, Claudio

    2015-01-01

    Experimental evidence in animal models suggests that misfolded Amyloid-β (Aβ) spreads in disease following a prion-like mechanism. Several properties characteristics of infectious prions have been shown for the induction of Aβ aggregates. However, a detailed titration of Aβ misfolding transmissibility and estimation of the minimum concentration of biologically active Aβ seeds able to accelerate pathological changes has not yet been performed. In this study, brain extracts from old tg2576 animals were serially diluted and intra-cerebrally injected into young subjects from the same transgenic line. Animals were sacrificed several months after treatment and brain slices were analyzed for amyloid pathology. We observed that administration of misfolded Aβ was able to significantly accelerate amyloid deposition in young mice, even when the original sample was diluted a million times. The titration curve obtained in this experiment was compared to the natural Aβ load spontaneously accumulated by these mice overtime. Our findings suggest that administration of the largest dose of Aβ seeds led to an acceleration of pathology equivalent to over a year. These results show that active Aβ seeds present in the brain can seed amyloidosis in a titratable manner, similarly as observed for infectious prions. PMID:25879692

  14. Role of DNA binding sites and slow unbinding kinetics in titration-based oscillators

    PubMed Central

    Karapetyan, Sargis; Buchler, Nicolas E.

    2016-01-01

    Genetic oscillators, such as circadian clocks, are constantly perturbed by molecular noise arising from the small number of molecules involved in gene regulation. One of the strongest sources of stochasticity is the binary noise that arises from the binding of a regulatory protein to a promoter in the chromosomal DNA. In this study, we focus on two minimal oscillators based on activator titration and repressor titration to understand the key parameters that are important for oscillations and for overcoming binary noise. We show that the rate of unbinding from the DNA, despite traditionally being considered a fast parameter, needs to be slow to broaden the space of oscillatory solutions. The addition of multiple, independent DNA binding sites further expands the oscillatory parameter space for the repressor-titration oscillator and lengthens the period of both oscillators. This effect is a combination of increased effective delay of the unbinding kinetics due to multiple binding sites and increased promoter ultrasensitivity that is specific for repression. We then use stochastic simulation to show that multiple binding sites increase the coherence of oscillations by mitigating the binary noise. Slow values of DNA unbinding rate are also effective in alleviating molecular noise due to the increased distance from the bifurcation point. Our work demonstrates how the number of DNA binding sites and slow unbinding kinetics, which are often omitted in biophysical models of gene circuits, can have a significant impact on the temporal and stochastic dynamics of genetic oscillators. PMID:26764732

  15. Calorimetry, activity, and micro-FTIR analysis of CO chemisorption, titration, and oxidation on supported Pt

    NASA Technical Reports Server (NTRS)

    Sermon, Paul A.; Self, Valerie A.; Vong, Mariana S. W.; Wurie, Alpha T.

    1990-01-01

    The value of in situ analysis on CO chemisorption, titration and oxidation over supported Pt catalysts using calorimetry, catalytic and micro-FTIR methods is illustrated using silica- and titania-supported samples. Isothermal CO-O and O2-CO titrations have not been widely used on metal surfaces and may be complicated if some oxide supports are reduced by CO titrant. However, they can illuminate the kinetics of CO oxidation on metal/oxide catalysts since during such titrations all O and CO coverages are scanned as a function of time. There are clear advantages in following the rates of the catalyzed CO oxidation via calorimetry and gc-ms simultaneously. At lower temperatures the evidence they provide is complementary. CO oxidation and its catalysis of CO oxidation have been extensively studied with hysteresis and oscillations apparent, and the present results suggest the benefits of a combined approach. Silica support porosity may be important in defining activity-temperature hysteresis. FTIR microspectroscopy reveals the chemical heterogeneity of the catalytic surfaces used; it is interesting that the evidence with regard to the dominant CO surface species and their reactivities with regard to surface oxygen for present oxide-supported Pt are different from those seen on graphite-supported Pt.

  16. Role of DNA binding sites and slow unbinding kinetics in titration-based oscillators

    NASA Astrophysics Data System (ADS)

    Karapetyan, Sargis; Buchler, Nicolas E.

    2015-12-01

    Genetic oscillators, such as circadian clocks, are constantly perturbed by molecular noise arising from the small number of molecules involved in gene regulation. One of the strongest sources of stochasticity is the binary noise that arises from the binding of a regulatory protein to a promoter in the chromosomal DNA. In this study, we focus on two minimal oscillators based on activator titration and repressor titration to understand the key parameters that are important for oscillations and for overcoming binary noise. We show that the rate of unbinding from the DNA, despite traditionally being considered a fast parameter, needs to be slow to broaden the space of oscillatory solutions. The addition of multiple, independent DNA binding sites further expands the oscillatory parameter space for the repressor-titration oscillator and lengthens the period of both oscillators. This effect is a combination of increased effective delay of the unbinding kinetics due to multiple binding sites and increased promoter ultrasensitivity that is specific for repression. We then use stochastic simulation to show that multiple binding sites increase the coherence of oscillations by mitigating the binary noise. Slow values of DNA unbinding rate are also effective in alleviating molecular noise due to the increased distance from the bifurcation point. Our work demonstrates how the number of DNA binding sites and slow unbinding kinetics, which are often omitted in biophysical models of gene circuits, can have a significant impact on the temporal and stochastic dynamics of genetic oscillators.

  17. The development of a continuous isothermal titration calorimetric method for equilibrium studies.

    PubMed

    Markova, Natalia; Hallén, Dan

    2004-08-01

    A continuous isothermal titration calorimetry (cITC) method for microcalorimeters has been developed. The method is based on continuous slow injection of a titrant into the calorimetric vessel. The experimental time for a cITC binding experiment is 12-20 min and the number of data points obtained is on the order of 1000. This gives an advantage over classical isothermal titration calorimetry (ITC) binding experiments that need 60-180 min to generate 20-30 data points. The method was validated using two types of calorimeters, which differ in calorimetric principle, geometry, stirring, and way of delivering the titrant into the calorimetric vessel. Two different experimental systems were used to validate the method: the binding of Ba(2+) to 18-crown-6 and the binding of cytidine 2'-monophosphate to RNAse A. Both systems are used as standard test systems for titration calorimetry. Computer simulations show that the dynamic range for determination of equilibrium constants can be increased by three orders of magnitude compared to that of classical ITC, making it possible to determine high affinities. Simulations also show an improved possibility to elucidate the actual binding model from cITC data. The simulated data demonstrate that cITC makes it easier to discriminate between different thermodynamic binding models due to the higher density of data points obtained from one experiment. PMID:15245999

  18. Trade-offs in Engineering Sugar Utilization Pathways for Titratable Control

    PubMed Central

    2015-01-01

    Titratable systems are common tools in metabolic engineering to tune the levels of enzymes and cellular components as part of pathway optimization. For nonmodel microorganisms with limited genetic tools, inducible sugar utilization pathways offer built-in titratable systems. However, these pathways can exhibit undesirable single-cell behaviors that hamper the uniform and tunable control of gene expression. Here, we applied mathematical modeling and single-cell measurements of l-arabinose utilization in Escherichia coli to systematically explore how sugar utilization pathways can be altered to achieve desirable inducible properties. We found that different pathway alterations, such as the removal of catabolism, constitutive expression of high-affinity or low-affinity transporters, or further deletion of the other transporters, came with trade-offs specific to each alteration. For instance, sugar catabolism improved the uniformity and linearity of the response at the cost of requiring higher sugar concentrations to induce the pathway. Within these alterations, we also found that a uniform and linear response could be achieved with a single alteration: constitutively expressing the high-affinity transporter. Equivalent modifications to the d-xylose utilization pathway yielded similar responses, demonstrating the applicability of our observations. Overall, our findings indicate that there is no ideal set of typical alterations when co-opting natural utilization pathways for titratable control and suggest design rules for manipulating these pathways to advance basic genetic studies and the metabolic engineering of microorganisms for optimized chemical production. PMID:24735079

  19. Utilizing the virus-induced blocking of apoptosis in an easy baculovirus titration method

    PubMed Central

    Niarchos, Athanasios; Lagoumintzis, George; Poulas, Konstantinos

    2015-01-01

    Baculovirus-mediated protein expression is a robust experimental technique for producing recombinant higher-eukaryotic proteins because it combines high yields with considerable post-translational modification capabilities. In this expression system, the determination of the titer of recombinant baculovirus stocks is important to achieve the correct multiplicity of infection for effective amplification of the virus and high expression of the target protein. To overcome the drawbacks of existing titration methods (e.g., plaque assay, real-time PCR), we present a simple and reliable assay that uses the ability of baculoviruses to block apoptosis in their host cells to accurately titrate virus samples. Briefly, after incubation with serial dilutions of baculovirus samples, Sf9 cells were UV irradiated and, after apoptosis induction, they were viewed via microscopy; the presence of cluster(s) of infected cells as islets indicated blocked apoptosis. Subsequently, baculovirus titers were calculated through the determination of the 50% endpoint dilution. The method is simple, inexpensive, and does not require unique laboratory equipment, consumables or expertise; moreover, it is versatile enough to be adapted for the titration of every virus species that can block apoptosis in any culturable host cells which undergo apoptosis under specific conditions. PMID:26490731

  20. Utilizing the virus-induced blocking of apoptosis in an easy baculovirus titration method.

    PubMed

    Niarchos, Athanasios; Lagoumintzis, George; Poulas, Konstantinos

    2015-01-01

    Baculovirus-mediated protein expression is a robust experimental technique for producing recombinant higher-eukaryotic proteins because it combines high yields with considerable post-translational modification capabilities. In this expression system, the determination of the titer of recombinant baculovirus stocks is important to achieve the correct multiplicity of infection for effective amplification of the virus and high expression of the target protein. To overcome the drawbacks of existing titration methods (e.g., plaque assay, real-time PCR), we present a simple and reliable assay that uses the ability of baculoviruses to block apoptosis in their host cells to accurately titrate virus samples. Briefly, after incubation with serial dilutions of baculovirus samples, Sf9 cells were UV irradiated and, after apoptosis induction, they were viewed via microscopy; the presence of cluster(s) of infected cells as islets indicated blocked apoptosis. Subsequently, baculovirus titers were calculated through the determination of the 50% endpoint dilution. The method is simple, inexpensive, and does not require unique laboratory equipment, consumables or expertise; moreover, it is versatile enough to be adapted for the titration of every virus species that can block apoptosis in any culturable host cells which undergo apoptosis under specific conditions. PMID:26490731