Determination of boron as boric acid by automatic potentiometric titration

International Nuclear Information System (INIS)

Midgley, D.

1988-06-01

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

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

African Journals Online (AJOL)

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

Determination of uranium and plutonium in PFBR MOX fuel using automatic potentiometric titrator

International Nuclear Information System (INIS)

Kelkar, Anoop; Meena, D.L.; Singh, Mamta; Kapoor, Y.S.; Pabale, Sagar; Fulzele, Ajit; Das, D.K.; Behere, P.G.; Afzal, Mohd

2014-01-01

Present paper describes the automatic potentiometric method for the determination of uranium and plutonium in less complexing H 2 SO 4 with scaling down the reagent volumes 15-20 ml in order to minimize the waste generation

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

Science.gov (United States)

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

2015-01-01

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

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

International Nuclear Information System (INIS)

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

2015-01-01

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

Accurate and precise determination of 2-25mg amounts of uranium by means of a special automatic potentiometric titration

International Nuclear Information System (INIS)

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

1978-01-01

A precise and accurate potentiometric titration of 2-25 mg of uranium is described. The uranium is reduced to U(IV) according to the method of Eberle et al. [3], and titrated with 0.05 N potassium dichromate, using a platinum indicator electrode. During the sample preparation the walls of the titration vessel are cleaned by centrifugation. To avoid overshoot of the set point a special differentiator is described, that interrupts the titration until equilibrium is reached. The precision of the method is 0.02%, the accuracy is better than 0.04% rel. Each titration takes 5 min. (orig.) [de

Determination of milligram amounts of neptunium by potentiometric titration

International Nuclear Information System (INIS)

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

1981-01-01

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

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

Science.gov (United States)

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

2016-08-24

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

Potentiometric titration of free acid in uranium solutions

International Nuclear Information System (INIS)

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

1998-02-01

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

Potentiometric titration of free acid in uranium solutions

Energy Technology Data Exchange (ETDEWEB)

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

1998-02-01

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

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

Science.gov (United States)

Flowers, Paul A.

1997-07-01

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

A new approach to flow-batch titration. A monosegmented flow titrator with coulometric reagent generation and potentiometric or biamperometric detection.

Science.gov (United States)

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

2006-11-01

Monosegmented flow analysis (MSFA) has been used as a flow-batch system to produce a simple, robust, and mechanized titrator that enables true titrations to be performed without the use of standards. This paper also introduces the use of coulometry with monosegmented titration by proposing a versatile flow cell. Coulometric generation of the titrand is attractive for titrations performed in monosegmented systems, because the reagent can be added without increasing the volume of sample injected. Also, biamperomeric and potentiometric detection of titration end-points can increase the versatility of the monosegmented titrator. The cell integrates coulometric generation of the titrand with detection of end-point by potentiometry or biamperometry. The resulting titrator is a flow-batch system in which the liquid monosegment, constrained by the interfaces of the gaseous carrier stream, plays the role of a sample of known volume to be titrated. The system has been used for determination of ascorbic acid, by coulometric generation of I2 with biamperometric detection, and for determination of Fe(II), by coulometric generation of Ce(IV) with potentiometric detection of the end-point, both in feed supplements.

Potentiometric titration of molybdenum (6) with a cathode-polarized solid electrode

International Nuclear Information System (INIS)

Boeva, L.V.; Kimstach, V.A.; Bagdasarov, K.N.

1980-01-01

The possibility has been studied of using solid electrodes for potentiometric precipitation titration of molybdenum (6). A cathode-polarized electrode, electrochemically covered with a molybdenum blue layer, can be used as indicator electrode. The best results were obtained during deposition of molybdenum blue on a tungsten electrode. The mechanism of electrode work during titration has been investigated. A procedure has been developed of titration of molybdenum (6) in acid solutions using hydroxylamine N-aryl derivatives as titrants

Evaluation of an automatic uranium titration system

International Nuclear Information System (INIS)

Lewis, K.

1980-01-01

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

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

Science.gov (United States)

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

2010-06-11

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

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

International Nuclear Information System (INIS)

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

2010-01-01

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

Automation of potentiometric titration with a personal computer using ...

African Journals Online (AJOL)

sampling was designed and tested for automation of potentiometric titrations with personal ... automation permits us to carry out new types of experiments, such as those requiring ... have proved to be very useful in routine tasks but not in research, due to their ... This is done by a simple delay sub-routine in data acquisition.

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

Science.gov (United States)

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

2011-11-01

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

Method of semi-automatic high precision potentiometric titration for characterization of uranium compounds; Metodo de titulacao potenciometrica de alta precisao semi-automatizado para a caracterizacao de compostos de uranio

Energy Technology Data Exchange (ETDEWEB)

Cristiano, Barbara Fernandes G.; Dias, Fabio C.; Barros, Pedro D. de; Araujo, Radier Mario S. de; Delgado, Jose Ubiratan; Silva, Jose Wanderley S. da, E-mail: barbara@ird.gov.b, E-mail: fabio@ird.gov.b, E-mail: pedrodio@ird.gov.b, E-mail: radier@ird.gov.b, E-mail: delgado@ird.gov.b, E-mail: wanderley@ird.gov.b [Instituto de Radioprotecao e Dosimetria (IRD/CNEN-RJ), Rio de Janeiro, RJ (Brazil); Lopes, Ricardo T., E-mail: ricardo@lin.ufrj.b [Universidade Federal do Rio de Janeiro (LIN/COPPE/UFRJ), RJ (Brazil). Coordenacao dos Programas de Pos-Graduacao de Engenharia. Lab. de Instrumentacao Nuclear

2011-10-26

The method of high precision potentiometric titration is widely used in the certification and characterization of uranium compounds. In order to reduce the analysis and diminish the influence if the annalist, a semi-automatic version of the method was developed at the safeguards laboratory of the CNEN-RJ, Brazil. The method was applied with traceability guaranteed by use of primary standard of potassium dichromate. The standard uncertainty combined in the determination of concentration of total uranium was of the order of 0.01%, which is better related to traditionally methods used by the nuclear installations which is of the order of 0.1%

Determination of uranium and plutonium by sequential potentiometric titration

International Nuclear Information System (INIS)

Kato, Yoshiharu; Takahashi, Masao

1976-01-01

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

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

Science.gov (United States)

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

2014-12-16

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

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

OpenAIRE

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

2011-01-01

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

Non-euclidean simplex optimization. [Application to potentiometric titration of Pu

Energy Technology Data Exchange (ETDEWEB)

Silver, G.L.

1977-08-15

Geometric optimization techniques useful for studying chemical equilibrium traditionally rely upon principles of euclidean geometry, but such algorithms may also be based upon principles of a non-euclidean geometry. The sequential simplex method is adapted to the hyperbolic plane, and application of optimization to problems such as the potentiometric titration of plutonium is suggested.

Linear regression analysis of potentiometric titration data for asymmetric redox reactions

International Nuclear Information System (INIS)

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

1997-01-01

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

Determination of the total acidity in soft drinks using potentiometric sequential injection titration.

Science.gov (United States)

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

2002-12-06

A potentiometric SI titration system for the determination of total acidity in soft drinks is proposed. The concept is based on the aspiration of the acid soft drink sample between two base zones into a holding coil with the volume of the first base zone twice to that of the second one and channelled by flow reversal through a reaction coil to a potentiometric sensor. A solution of 0.1 mol l(-1) sodium chloride is used as ionic strength adjustment buffer in the carrier stream. The system has been applied to the analysis of some South African soft drinks having a total acidity level of about 0.2-0.3% (w/v). The method has a sample frequency of 45 samples per h with a linear range of 0.1 and 0.6% (w/v). It is easy to use, fully computerised, and gives the results that are comparable to both automated batch titration and manual titration.

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

Science.gov (United States)

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

2015-08-12

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

Determination of titanium and vanadium in aqueous solutions by potentiometric titration

International Nuclear Information System (INIS)

Sibirkin, A.A.; Elliev, Yu.E.

1996-01-01

Possibility of titanium and vanadium determination at their combined presence by bichromatometric chromometric titration with potentiometric indication of end point is shown. The technique is developed which allows to determine titanium and vanadium with relative standard derivation ±2% in amounts not less than 50 and 100 mg respectively

Potentiometric titrations of para and nitro substituted aromatic acids and their mixtures in methylethyl ketone

International Nuclear Information System (INIS)

Ozeroglu, C.; Karahan, M.

2011-01-01

In this study, it was the purpose to examine the potentiometric titrations of para and nitro substituted aromatic acids in methylethyl ketone (MEK) as a non-aqueous solvent. Good analytical results were obtained in determining the amount of each acid and the amounts of acids in their ternary mixtures by using 0.0964 N tetrabuthylammoniumhydroxyde (TBAH) as a standard titrant. Methylethyl ketone (MEK) which is a good solvent for many organic compounds and has a convenient liquid range of -86 to 80 deg. C was used for titration of the para and nitro substituted aromatic acids. A linear relationship has been found between pKa values of the para and nitro substituted aromatic acids in water and the half neutralization potential (HNP) values determined by potentiometric titration curves of the same acids in MEK. (author)

Characterization of Native and Modified Starches by Potentiometric Titration

OpenAIRE

Soto, Diana; Urdaneta, Jose; Pernia, Kelly

2014-01-01

The use of potentiometric titration for the analysis and characterization of native and modified starches is highlighted. The polyelectrolytic behavior of oxidized starches (thermal and thermal-chemical oxidation), a graft copolymer of itaconic acid (IA) onto starch, and starch esters (mono- and diester itaconate) was compared with the behavior of native starch, the homopolymer, and the acid employed as a graft monomer and substituent. Starch esters showed higher percentages of acidity, follo...

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

Science.gov (United States)

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

2002-09-01

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

The determination of 800 to 30 μg lead(II) by potentiometric titration with molybdate

International Nuclear Information System (INIS)

Campiglio, A.

1985-01-01

The determination of 800 to 30 μg Pb(II) by potentiometric titration with molybdate by using a lead(II)-selective electrode was investigated. Under suitable conditions, 800 to 300 μg Pb(II) in aqueous solution by automatic or manual titration with 4x10 -3 M molybdate can be determined with an accuracy of +-0.57% and +-0.45% and a precision of +-0.43% and 0.30% (standard deviation = 0.25% and 0.17%, resp.). For determining amounts of Pb(II) below 300 μg, a 2x10 -3 M molybdate solution has to be used. Although 300 to 100μg Pb(II) are determinable again in water with satisfactory results, the titration in 40% ethanol is however more reliable: in this medium, amounts of 300 to 30μg Pb(II) can be determined with an accuracy of +-1% and a precision of +-2% (standard deviation from 20 titrations of 100μg Pb(II)=0.60%). The titration of 300-800μg Pb(II) in water and of 30-300μg Pb(II) in 40% ethanol is also possible in 0.1 M NaNO 3 sub- snd 0.1 M NaClO 4 sub- medium and can be used in the lead determination in organic compounds after mineralization with HNO 3 sub-HClO 4 sub-H 2 O 2 . (Author)

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

Science.gov (United States)

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.

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

Science.gov (United States)

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

2012-06-01

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

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

Science.gov (United States)

Kufelnicki, A; Lis, S; Meinrath, G

2005-08-01

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

Method for linearizing the potentiometric curves of precipitation titration in nonaqueous and aqueous-organic solutions

International Nuclear Information System (INIS)

Bykova, L.N.; Chesnokova, O.Ya.; Orlova, M.V.

1995-01-01

The method for linearizing the potentiometric curves of precipitation titration is studied for its application in the determination of halide ions (Cl - , Br - , I - ) in dimethylacetamide, dimethylformamide, in which titration is complicated by additional equilibrium processes. It is found that the method of linearization permits the determination of the titrant volume at the end point of titration to high accuracy in the case of titration curves without a potential jump in the proximity of the equivalent point (5 x 10 -5 M). 3 refs., 2 figs., 3 tabs

Use of the potentiometric titration method to investigate heterogeneous systems including phosphorylated complexones

International Nuclear Information System (INIS)

Tereshin, G.S.; Kharitonova, L.K.; Kuznetsova, O.B.

1979-01-01

Heterogeneous systems Y(NO 3 ) 3 (YCl 3 )-Hsub(n)L-KNO 3 (KCl)-H 2 O are investigated by potentiometric titration (with coulomb-meter generation of oH - ions). Hsub(n)L is one of the following: oxyethylidendiphosphonic; aminobenzilidendiphosphonic; glycine-bis-methyl-phosphonic; nitrilotrimethylphosphonic (H 6 L) and ethylenediaminetetramethylphosphonic acids. The range of the exsistence of YHsub(nL3)LxyH 2 O has been determined. The possibility of using potentiometric titration for investigating heterogeneous systems is demonstrated by the stUdy of the system Y(NO 3 ) 3 -H 6 L-KOH-H 2 o by the method of residual concentration. The two methods have shown that at pH 3 LxyH 2 O; at pH=6, KYH 2 Lxy'H 2 O, and at pH=7, K 2 YHLxy''H 2 O. The complete solubility products of nitrilotrimethylphosphonates are evaluated

Differential potentiometric titration: development of a methodology for determining the point of zero charge of metal (hydr)oxides by one titration curve.

Science.gov (United States)

Bourikas, Kyriakos; Kordulis, Christos; Lycourghiotis, Alexis

2005-06-01

A new methodology is presented, called differential potentiometric titration (DPT), which allows the determination of the point of zero charge (pzc) of metal (hydr)oxides using only one potentiometric curve. By performing extensive simulations of potentiometric titrations for various model (hydr)oxides, we found that an inflection point in a H+(cons,surf) versus pH potentiometric curve (H+(cons,surf): hydrogen ions consumed on the surface of the (hydr)oxide) and a peak in the corresponding differential curve, dH+(cons,surf)/dpH versus pH, appear at a pH equal to the pzc assumed for a model (hydr)oxide. This distinguishable peak appears at the same position irrespective of the surface ionization and the interfacial model adopted as well as the assumed ionic strength. It was found that the aforementioned peak also appears in the high-resolution differential potentiometric curves experimentally determined for four oxides (SiO2, TiO2, gamma-Al2O3, and MgO) that are widely used in various environmental and other technological applications. The application of DPT to the above-mentioned oxides provided practically the same pzc values as the corresponding ones achieved by using four different techniques as well as the corresponding isoelectric point (iep) values determined by microelectrophoresis. Differences between the pzc and iep values determined using various techniques in the case of MgO were attributed to the increasing dissolution of this oxide as pH decreases and the adsorption of cations (Mg2+, Na+) on the MgO/electrolytic solution interface.

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

International Nuclear Information System (INIS)

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

1994-01-01

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

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

Science.gov (United States)

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

2009-10-15

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

Persistence length of carboxymethyl cellulose as evaluated from size exclusion chromatography and potentiometric titrations.

NARCIS (Netherlands)

Hoogendam, C.W.; Keizer, de A.; Cohen Stuart, M.A.; Bijsterbosch, B.H.; Smit, J.A.M.; Dijk, van J.A.P.P.; Horst, van der P.M.; Batelaan, J.G.

1998-01-01

The intrinsic persistence length of carboxymethyl cellulose (CMC) is determined by size exclusion chromatography in combination with multiangle laser light scattering (SEC-MALLS) as well as from potentiometric titrations. Samples with degree of substitution (ds) ranging from 0.75 to 1.25 were

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

Science.gov (United States)

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

2016-09-01

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

Calculating Equilibrium Constants in the SnCl2-H2O-NaOH System According to Potentiometric Titration Data

Science.gov (United States)

Maskaeva, L. N.; Fedorova, E. A.; Yusupov, R. A.; Markov, V. F.

2018-05-01

The potentiometric titration of tin chloride SnCl2 is performed in the concentration range of 0.00009-1.1 mol/L with a solution of sodium hydroxide NaOH. According to potentiometric titration data based on modeling equilibria in the SnCl2-H2O-NaOH system, basic equations are generated for the main processes, and instability constants are calculated for the resulting hydroxo complexes and equilibrium constants of low-soluble tin(II) compounds. The data will be of interest for specialists in the field of theory of solutions.

Determination of binding constants of cyclodextrin inclusion complexes with amino acids and dipeptides by potentiometric titration.

Science.gov (United States)

Kahle, Claudia; Holzgrabe, Ulrike

2004-10-01

Cyclodextrins are well known for their ability to separate enantiomers of drugs, natural products, and other chiral substances using HPLC, GC, or CE. The resolution of the enantiomers is due to the formation of diastereomeric complexes between the cyclodextrin and the pairs of enantiomers. The aim of this study was to determine the binding constants of the complexes between alpha- and beta-cyclodextrin and the enantiomers of a series of aliphatic and aromatic amino acids, and dipeptides, using a potentiometric titration method. The results of this method are compared to other methods, and correlated to findings in cyclodextrin-modified capillary electrophoresis and possible complex structures. Potentiometric titration was found to be an appropriate tool to determine the binding constants of cyclodextrin inclusion complexes.

Automation of potentiometric titration for the determination of uranium in nuclear fuel materials

International Nuclear Information System (INIS)

Kelkar, Anoop; Pandey, Ashish; Kapoor, Y.S.; Kumar, Manish; Singh, Mamta; Fulzele, Ajeet; Prakash, Amrit; Afzal, Mohd; Panakkal, J.P.

2010-01-01

Advanced Fuel Fabrication Facility is fabricating various types of mixed oxide fuels, namely for PHWR, BWR, FBTR and PFBR. Precise determination of uranium in MOX fuel sample is important to get desired burn up in the reactor. The modified Davies and Gray method is routinely used for the potentiometric titration of uranium

Determination of uranyl ion by potentiometric titration using an uranyl-selective electrode

International Nuclear Information System (INIS)

Nassory, N.S.

1990-01-01

A potentiometric titration of uranyl ion is described using an uranyl selective electrode based on a membrane containing a complex of UO 2 -bis[di-4-(1,1,3,3-tetramethylbutyl)phenyl phosphate] as an ion-exchanger and tritolyl phosphate as a solvent mediator. The titrations were carried out with various titrants: Sodium hydroxide, potassium fluoride and sodium salts of acetate, oxalate and citrate. The equivalence points were determined by Gran's method. Good results were obtained by using sodium oxalate as a titrant for the determination of uranium in several samples of ammonium diuranate. The results were quite comparable with those obtained by X-ray fluorescence spectrometry. (orig.)

Determination of boron as boric acid by automatic potentiometric titration using Gran plots [in pressurized water reactor coolant

International Nuclear Information System (INIS)

Midgley, D.; Gatford, C.

1989-11-01

Boron in PWR primary coolant and related waters may be determined as boric acid by titration with sodium hydroxide, using a glass electrode as a pH indicator. Earlier work has shown that this analysis can conveniently be carried out automatically with adequate precision and accuracy for routine use, although bias became apparent at the lowest concentrations tested. The latest titrators enable the titration data to be transformed mathematically to give two linear segments, before and after the end-point (Gran plots). The results are as precise as those from other titration methods (in which the end-point is found from the point of inflexion of a plot of pH against volume of titrant), but the bias at low concentrations is much reduced. This is achieved without extra time or involvement of the operator. (author)

Conductimetric and Potentiometric Titration of Some Hydroxylated Cinnamic Acids with Tetrabutylammonium Hydroxide in Non-Aqueous Media

OpenAIRE

AKTAŞ, A. Hakan; YAŞAR, Gülsüm; ALSANCAK, Güleren ÖZKAN

2001-01-01

In this study, four hydroxycinnamic acids, namely 3,4-dihydroxycinnamic acid, 4-hydroxycinnamic acid, 4-hydroxy --3- methoxycinnamic acid and 4-hydroxy-3,5-dimethoxycinnamic acid, were titrated conductimetrically and potentiometrically using triethylamine and tetrabutylammonium hydroxide in acetonitrile, 2-propanol, and pyridine solvents under a nitrogen atmosphere at 25 oC. In conductimetric titration with tetrabutylammonium hydroxide all of the compounds exhibited conventional s...

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

International Nuclear Information System (INIS)

Ganivet, Michel

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

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

NARCIS (Netherlands)

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

1984-01-01

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

Determination of arsenate and organic arsenic via potentiometric titration of its heteropoly anions.

Science.gov (United States)

Metelka, R; Slavíková, S; Vytras, K

2002-08-16

Determination of arsenate based on its conversion to molybdoarsenate heteropoly anions followed by potentiometric titration is described. The titration is realized on the ion-pairing principle using cetylpyridinium chloride (or an analogous titrant containing a lipophilic cation), and is monitored by a carbon paste electrode, although other liquid-polymeric membrane-based electrodes can also be used. Calibration plots of the titrant end-point consumption versus concentration of arsenic were constructed and used to evaluate the content of arsenic in aqueous samples. The method could be applied in the analyses of samples with quite low arsenic content (amounts approximately 10 mug As in 50 cm(3) could be titrated). Organic arsenic was determined analogously after the Schöniger combustion of the sample and conversion of its arsenic to arsenate.

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

Science.gov (United States)

Bratskaya, S; Golikov, A; Lutsenko, T; Nesterova, O; Dudarchik, V

2008-09-01

Charge characteristics of humic and fulvic acids of a different origin (inshore soils, peat, marine sediments, and soil (lysimetric) waters) were evaluated by means of two alternative methods - colloid titration and potentiometric titration. In order to elucidate possible limitations of the colloid titration as an express method of analysis of low content of humic substances we monitored changes in acid-base properties and charge densities of humic substances with soil depth, fractionation, and origin. We have shown that both factors - strength of acidic groups and molecular weight distribution in humic and fulvic acids - can affect the reliability of colloid titration. Due to deviations from 1:1 stoichiometry in interactions of humic substances with polymeric cationic titrant, the colloid titration can underestimate total acidity (charge density) of humic substances with domination of weak acidic functional groups (pK>6) and high content of the fractions with molecular weight below 1kDa.

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

International Nuclear Information System (INIS)

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

1990-01-01

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

Differential electrolytic potentiometric titration method for the determination of ciprofloxacin in drug formulations.

Science.gov (United States)

Abulkibash, Abdalla M; Sultan, Salah M; Al-Olyan, Abeer M; Al-Ghannam, Sheikha M

2003-10-17

A simple and rapid differential electrolytic potentiometric titration method for the determination of ciprofloxacin was developed. The work is based on the fast complexation reaction between iron(III) and ciprofloxacin in a ratio of 1:3, respectively, in sulfuric acid media of 0.09 mol dm(-3). Among the electrodes tested silver amalgam electrodes were found to be a suitable indicating system. By applying a current density of 0.5 muA cm(-2) to these electrodes and using iron(III) solution of 0.097 mol dm(-3) as a titrant, normal titration curves were obtained. The method was successfully applied for the determination of ciprofloxacin in drug formulations as low as 4.0 ppm.

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

Science.gov (United States)

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.

Potentiometric titration in a low volume of solution for rapid assay of uranium. Application to quantitative electro-reduction of uranium(VI)

International Nuclear Information System (INIS)

Sahoo, P.; Ananthanarayanan, R.; Murali, N.; Mallika, C.; Falix Lawrence; Kamachi Mudali, U.

2012-01-01

A simple, inexpensive PC based potentiometric titration technique for the assay of uranium using low volumes of sample aliquot (25-100 μL) along with all reagents (total volume of solution being less than 2.5 mL) is presented. The technique involves modification of the well known Davies and Gray Method recommended for assay of uranium(VI) in nuclear materials by introducing an innovative potentiometric titration device with a mini cell developed in-house. After appropriate chemical conditioning the titration is completed within a couple of minutes with display of online titration plot showing the progress of titration. The first derivative plot generated immediately after titration provides information of end point. The main advantage of using this technique is to carry out titration with minimum volumes of sample and reagents generating minimum volume of wastes after titration. The validity of the technique was evaluated using standard certified samples. This technique was applied for assay of uranium in a typical sample collected from fuel reprocessing laboratory. Further, the present technique was deployed in investigating the optimum conditions for efficient in situ production of U(IV). The precision in the estimation of uranium is highly satisfactory (RSD less than 1.0%). (author)

Statistical evaluation of an interlaboratory comparison for the determination of uranium by potentiometric titration

International Nuclear Information System (INIS)

Ketema, D.J.; Harry, R.J.S.; Zijp, W.L.

1990-09-01

Upon request of the ESARDA working group 'Low enriched uranium conversion - and fuel fabrication plants' an interlaboratory comparison was organized, to assess the precision and accuracy concerning the determination of uranium by the potentiometric titration method. This report presents the results of a statistical evaluation on the data of the first phase of this exercise. (author). 9 refs.; 5 figs.; 24 tabs

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

Science.gov (United States)

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

2010-08-01

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

Automatic titrator for high precision plutonium assay

International Nuclear Information System (INIS)

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

1986-01-01

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

Potentiometric and amperometric titration of ferrocene by cerium(4)

International Nuclear Information System (INIS)

Solomatin, V.T.

1985-01-01

Redox-potentials (E) of ferrocene (ferricenium-cation), Ce(4)/Ce(3) pairs are investigated and a possibility of regulating E value of these systems depending on the composition of water-organic media is shown. E value of Ce(4)/Ce(3) system decreases as increasing H 2 SO 4 concentration and CH 3 COOH mol share in the water-organic phase. Kinetic investigations of Ce(4)-ferrocene reactions shown that E constant value is achieved in 12-16 s depending on donor-acceptor properties of the solvent. Optimum conditions are chosen for potentiometric and amperometric titration of ferrocene by ceruium (4) in technological products. The method is versatile and permits to determine from tenths to dozens per cent of ferrocene

Estimation of uncertainty in pKa values determined by potentiometric titration.

Science.gov (United States)

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

2004-06-01

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

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

International Nuclear Information System (INIS)

Jiang Haiying; Cheng Ruoyu; Meng Xiujun

2014-01-01

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

Study on the use of solid electrodes for potentiometric titrations in non-aqueous solvents-I

International Nuclear Information System (INIS)

Fatibello Filho, O.; Carvalho, W.M. de; Capelato, M.D.; Bulhoes, L.O.S.; Almeida Neves, E.F. de

1984-01-01

Fatty acids and ethanolamines were titrated potentiometrically with tetrabutylammnonium hydroxide in methyl isobutyl ketone-isopropyl alcohol and with perchloric acid in ethanol, respectively. A study of utilization of Sb, Sn, W, PbO 2 , Ti and 316L stainless steel oxides - Ag/AgBr/Bu 4 NBr (x M)/solvent electrode systems have been investigated in comparison with the glass - Ag/AgBr/Bu 4 NBr (x M)/solvent system. The best performance was obtained using W, Sb, PbO 2 and Ti electrodes have yielded a larger potential shift than glass electrode for acid-base titration. (C.L.B.) [pt

Characterization of solid-solution interface by potentiometric titration and electrophoretic mobility

International Nuclear Information System (INIS)

Lindecker, C.; Drot, R.; Fourest, B.; Simoni, E.

1999-01-01

The study of nuclear waste storage in deep geological sites involves the understanding of processes which could produce a possible dispersion or retention of radioelements. The dispersion of solid particles in aqueous solution is consequently important to be characterized. In this bi-phased system it is necessary to determine the characteristics of the solid-solution interface. The method used of this study is the techniques of potentiometric titration applied to heterogeneous systems. The material studied were phosphate matrices which were synthesized in the laboratory. The dependence of their surface change upon the nature of the electrolytes was investigated

Concentration determination of methyl magnesium chloride and other Grignard reagents by potentiometric titration with in-line characterization of reaction species by FTIR spectroscopy.

Science.gov (United States)

Chen, Yadan; Wang, Tao; Helmy, Roy; Zhou, George X; LoBrutto, Rosario

2002-07-01

A potentiometric titration method for methyl magnesium chloride and other Grignard reagents based on the reaction with 2-butanol in THF has been developed and validated. The method employs a commercially available platinum electrode, using an electrolyte compatible with non-aqueous solvents. Well-defined titration curves were obtained, along with excellent method precision. The endpoint was precisely determined based on the first derivative of the titration curve. Different solvents such as THF, diethyl ether and methylene chloride provided similar results with regard to sharpness of the endpoint and method precision. The method was applied to a wide array of Grignard reagents including methyl magnesium bromide, ethyl magnesium chloride, propyl magnesium chloride, vinyl magnesium chloride, phenyl magnesium chloride, and benzyl magnesium chloride with similar precision and accuracy. Application of in-line FTIR was demonstrated for in situ monitoring of the titration reaction, allowing characterization of the reaction species. An authentic spectrum of the MeMgCl-THF complex was obtained using spectral subtraction and the vibrational absorbance bands were identified. FTIR also provided an alternative for detecting the titration endpoint, and the titration results so obtained, provided a cross-validation of the accuracy of the potentiometric titration.

Validation of analytical procedure of quantitative determination of 5,7-bis(meta-nitrophenylamino-4,6-dinitrobenzofuroxan by potentiometric titration

Directory of Open Access Journals (Sweden)

R. Sh. Markhabullina

2014-01-01

Full Text Available A new method of quantitative determination of the substance of 5,7-bis(meta-nitrophenylamino-4,6-dinitrobenzofuroxan using potentiometric titration method is developed. The method has high precision, reliability and sensitivity.

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

Science.gov (United States)

Hoffmann, W

1996-09-01

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

Potentiometric titration curves of aluminium salt solutions and its species conversion in the hydrolysis-polymerization course

Directory of Open Access Journals (Sweden)

Chenyi Wang

2008-12-01

Full Text Available A new concept of critical point is expounded by analysing the potentiometric titration curves of aluminium salt solutions under the moderate slow rate of base injection. The critical point is defined as the characteristic spot of the Al3+ salt solutions potentiometric titration curve, which is related to the experiment conditions. In addition, the changes of critical points reflect the influence of experiment conditions on the course of the hydrolysis-polymerization and the conversion of hydroxyl polynuclear aluminum species. According to the OH/Al mole ratio, the Al species can be divided into four regions quantitatively by three characteristic points on the titration curves: Part I, Al3+/Ala region, consist chiefly of Al3+ and mononuclear Al; Part II, the small/middle polynuclear Al region, including Al2-Al12; Part III, the large-size polynuclear aluminum region, consistent with predominantly Al13-Al54 and a little sol/gel Al(OH3; Part IV, the dissolving region of sol/gel Alc, only Al(OH 3 (aq or am and Al(OH4- species, which set up a base to study on the hydrolysis-polymerization of Al3+. At the same time, significant effects of total aluminum concentration, temperature, halide ion, silicate radical, and organic acid radical on the titration curves and its critical points were observed. Given the three critical points which demarcating the aluminum forms, we carry out a through investigation into the fundamental regulations of these factors’ influence, and offer a fresh train of thought to study the hydrolysis-polymerization of Al3+ in soil solutions.

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

Science.gov (United States)

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

2010-06-01

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

Evaluation of the performance of a metrohm titrator titrando-836 in potentiometric analysis of uranium for safeguards purposes

International Nuclear Information System (INIS)

Cristiano, Barbara Fernandes; Silva, Jose Wanderley S. da; Barros, Pedro Dionisio de; Araujo, Radier Mario S. de

2009-01-01

To achieve the requirements of the Brazilian State System of Accounting for and Control of Nuclear Materials - SSAC the Safeguards Laboratory of Brazilian Nuclear Energy Commission, LASAL, has been applying the 'Davies and Gray/NBL' method for Potentiometric determination of total uranium concentration in several forms of nuclear materials since 1984. To improve the accuracy and the repeatability the method uses as titrant, standard reference potassium dichromate NIST SRM 136e and the results are also corrected for bias with NBL CRM 112A uranium metal assay standard. This work describes the assays performed for validation of a Metrohm 836 potentiometric titrator acquired by LASAL in order to improve the analytical methodology of the laboratory. The titrator is attached to a Pt:Rh (90:10) as indicator electrode and a mercurous sulfate as the reference electrode. The evaluation of accuracy and repeatability were made by comparison, the results provided by the titrator with the certified value of standards and also by the participation in round robin program sponsored by New Brunswick Laboratory - NBL. The validation was done by a comparison of the performance between the Metrohm 836 and a Mettler - DL67 titrator which has currently been used by the laboratory. It included evaluation of the results of both equipment, the repeatability of the measurement, any systematic contributions and its uncertainties. (author)

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

Science.gov (United States)

Papanastasiou, G; Ziogas, I

1995-06-01

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

Determination of plutonium and uranium in the same aliquot by potentiometric titration

International Nuclear Information System (INIS)

Karekar, C.V.; Chander, Keshav; Nair, G.M.; Natarajan, P.R.

1986-01-01

A potentiometric titration method was developed for the determination of plutonium and uranium in the same aliquot in nitric acid medium. Plutonium was first determined by oxidation to Pu(VI) by fuming with HClO 4 . Pu(VI) was reduced to Pu(IV) with known excess of Fe(II). Uranium in the same solution was determined by reduction to U(IV) with Fe(II) in H 3 PO 4 medium. For the quantity of plutonium and uranium in the range of 3-5 mg per aliquot a precision of +-0.2% and +-0.4%, respectively, was obtained. (author)

Potentiometric and spectrophotometric titration study of interaction of tungstovanadophosphoric heteropolyacids with sodium hydroxide

International Nuclear Information System (INIS)

Borkoyakov, S.A.; Fisun, L.A.

1988-01-01

The methods of potentiometric and spectrophotometric titration are used to study H s+n PW 12-n V n O 40 (n=1,2) (P-W-V HPA) decomposition by sodium hydroxide. It is shown that at the first stage of heteropolyanion interaction with alkali (pH) > 4 P-W-V HPA structural reconstruction takes place. It is accompanied by the formation of complexes with a higher content of vanadium atoms stable at pH 4-7/ P-W-V HPA decomposition to initial salts occurs at pH > 8

Microprocessor-controlled system for automatic acquisition of potentiometric data and their non-linear least-squares fit in equilibrium studies.

Science.gov (United States)

Gampp, H; Maeder, M; Zuberbühler, A D; Kaden, T A

1980-06-01

A microprocessor-controlled potentiometric titration apparatus for equilibrium studies is described. The microprocessor controls the stepwise addition of reagent, monitors the pH until it becomes constant and stores the constant value. The data are recorded on magnetic tape by a cassette recorder with an RS232 input-output interface. A non-linear least-squares program based on Marquardt's modification of the Newton-Gauss method is discussed and its performance in the calculation of equilibrium constants is exemplified. An HP 9821 desk-top computer accepts the data from the magnetic tape recorder. In addition to a fully automatic fitting procedure, the program allows manual adjustment of the parameters. Three examples are discussed with regard to performance and reproducibility.

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

Science.gov (United States)

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

2013-07-15

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

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

International Nuclear Information System (INIS)

Yoshimura, Chozo; Miyamoto, Kiyoshige

1985-01-01

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

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

International Nuclear Information System (INIS)

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

2009-01-01

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

Interlaboratory comparison exercise for the determination of uranium by potentiometric titration (first phase)

International Nuclear Information System (INIS)

Verdingh, V.; Le Duigou, Y.

1991-01-01

Upon request of the Esarda working group on low-enriched uranium conversion and fuel fabrication plants an interlaboratory comparison was organized, to assess the precision and accuracy concerning the determination of uranium by the potentiometric titration method. This report presents the results of the first phase of this exercise (pure uranyl-nitrate solutions). The solutions used in this intercomparison have been certified for their uranium content by the CBNM, Geel. Comparison of the laboratory results with the certified values shows excellent, good and fairly good agreement for many of the participating laboratories. 10 tabs., 5 figs., 10 refs

Development of a Novel Solid-State Sensor Electrode Based on Titanium Thin Film as an Indicator Electrode in Potentiometric and Conductometric Acid-Base Titration in Aqueous Solution

OpenAIRE

Abu Ghalwa, Nasser

2012-01-01

A modified Ti/(SnO2 + Sb2O3) electrode was prepared by thermal deposition on titanium substrate and its use as indicator electrode to potentiometric and conductometric acid-base titration in aqueous solution at 298 K was developed. The E-pH curve is linear with slope of 0.0512 V/dec at 298 K. The standard potential of this electrode, E0, was determined with respect to the SCE as reference electrode. The recovery percentages for potentiometric and conductometric acid-base titration for acetic ...

Potentiometric determination of molybdenum

International Nuclear Information System (INIS)

Rusina, O.N.; Gorbatkova, B.Kh.

1977-01-01

Potentiometric titration by lead acetate is used to determine molybdenum in the form of molybdate ions. The behaviour of bimetallic electrode couples, i.e. tungsten-lead, platinum-lead, lead-carbon electrode, molybdenum-carbon electrode platinum-molibdenum has been investigated. The greatest jump of the potential in the finite point is observed for platinum-molybdenum electrode couple (150 mV/ml at pH 4.0-5.5). The limiting concentration of molybdenum in potentiometric titration by lead acetate is 2.8x10 -4 M. The measurements are accurate to within +-0.1%

Automated uranium titration system

International Nuclear Information System (INIS)

Takahashi, M.; Kato, Y.

1983-01-01

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

A nonaqueous potentiometric titration study of the dissociation of t-butyl methacrylate-methacrylic acid copolymers.

Science.gov (United States)

Nakatani, Kiyoharu; Yamashita, Jun; Sekine, Tomomi; Toriumi, Minoru; Itani, Toshiro

2003-05-01

The dissociation of t-butyl methacrylate-methacrylic acid copolymers in dimethyl sulfoxide was analyzed by a nonaqueous potentiometric titration technique. The negative logarithm of the dissociation constant of the monomer unit of a methacrylic acid (MAA) monotonously increased with the increasing degree of dissociation corresponding to the titrant/MAA amount ratio, and was highly influenced by the copolymerization ratio. The results are discussed in terms of the suppression of the dissociation of MAA by a neighboring charged methacrylate anion unit.

Four points function fitted and first derivative procedure for determining the end points in potentiometric titration curves: statistical analysis and method comparison.

Science.gov (United States)

Kholeif, S A

2001-06-01

A new method that belongs to the differential category for determining the end points from potentiometric titration curves is presented. It uses a preprocess to find first derivative values by fitting four data points in and around the region of inflection to a non-linear function, and then locate the end point, usually as a maximum or minimum, using an inverse parabolic interpolation procedure that has an analytical solution. The behavior and accuracy of the sigmoid and cumulative non-linear functions used are investigated against three factors. A statistical evaluation of the new method using linear least-squares method validation and multifactor data analysis are covered. The new method is generally applied to symmetrical and unsymmetrical potentiometric titration curves, and the end point is calculated using numerical procedures only. It outperforms the "parent" regular differential method in almost all factors levels and gives accurate results comparable to the true or estimated true end points. Calculated end points from selected experimental titration curves compatible with the equivalence point category of methods, such as Gran or Fortuin, are also compared with the new method.

Digital movie-based on automatic titrations.

Science.gov (United States)

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

2016-01-15

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

The binding of aluminum to mugineic acid and related compounds as studied by potentiometric titration.

Science.gov (United States)

Yoshimura, Etsuro; Kohdr, Hicham; Mori, Satoshi; Hider, Robert C

2011-08-01

The phytosiderophores, mugineic acid (MA) and epi-hydroxymugineic acid (HMA), together with a related compound, nicotianamine (NA), were investigated for their ability to bind Al(III). Potentiometric titration analysis demonstrated that MA and HMA bind Al(III), in contrast to NA which does not under normal physiological conditions. With MA and HMA, in addition to the Al complex (AlL), the protonated (AlLH) and deprotonated (AlLH(-1)) complexes were identified from an analysis of titration curves, where L denotes the phytosiderophore form in which all the carboxylate functions are ionized. The equilibrium formation constants of the Al(III) phytosiderophore complexes are much smaller than those of the corresponding Fe(III) complexes. The higher selectivity of phytosiderophores for Fe(III) over Al(III) facilitates Fe(III) acquisition in alkaline conditions where free Al(III) levels are higher than free Fe(III) levels.

Limitations of pH-potentiometric titration for the determination of the degree of deacetylation of chitosan.

Science.gov (United States)

Balázs, Nándor; Sipos, Pál

2007-01-15

The degree of deacetylation (DDA) of chitosan determines the biopolymer's physico-chemical properties and technological applications. pH-Potentiometric titration seems to offer a simple and convenient means of determining DDA. However, to obtain accurate pH-potentiometric DDA values, several factors have to be taken into consideration. We found that the moisture content of the air-dry chitosan samples can be as high as 15%, and a reasonable fraction of this humidity cannot be removed by ordinary drying. Corrections have to be made for the ash content, as in some samples it can be as high as 1% by weight. The method of equivalence point determination was also found to cause systematic variations in the results and in some samples extra acid as high as 1 mol% of the free amino content was also identified. To compensate for the latter effect, the second equivalence point of the titration has to be determined separately and the analytical concentration of the acid be corrected for it. All the corrections listed here are necessary to obtain DDA values that are in reasonable agreement with those obtained from (1)H NMR and IR spectroscopic measurements. The need for these corrections severely limits the usefulness of pH-metry for determining accurate DDA values and thus potentiometry is hardly able to compete with other standard spectroscopic procedures, that is, (1)H NMR spectroscopy.

Elucidation of the electronic spectrum changes of KA-Al3+ complex by potentiometric titration, FTIR, 13C NMR and quantum mechanics

International Nuclear Information System (INIS)

Piantavini, Mário S.; Gonçalves, Alan G.; Trindade, Ângela C.L.B.; Noseda, Miguel D.; Mercê, Ana L.R.; Pontarolo, Roberto; Machado, Antonio E.H.

2017-01-01

Kojic acid (KA) is an organic acid widely used in pharmaceutical industry, mainly as a skin lightening agent. Based on the ability of KA to form complexes with ions, we found the most possible kind of complex formed with cation aluminum. KA-Al 3+ complex structures were studied using potentiometric and spectrophotometric (UV) titrations, FTIR and 13 C NMR. The electronic spectroscopy showed that the KA-Al 3+ complexes absorb at higher wavelengths (λ max = 305 nm) than do the non-complexed KA (λ max = 269 nm), confirming complexation. The IR spectra of KA complexed and not complexed allowed to correlate the changes in the absorption of enol and carbonyl groups in absence and presence of Al 3+ in aqueous solutions. The complexation suggested by the potentiometric titration and FTIR spectroscopy are in accordance with the data obtained from NMR results. Calculations based on quantum mechanics were utilized to understand the differences found in the non complexed and complexed KAH electronic spectra. (author)

Gran method for end point anticipation in monosegmented flow titration

Directory of Open Access Journals (Sweden)

Aquino Emerson V

2004-01-01

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

Titulações potenciométricas de cátions metálicos tendo como eletrodo indicador o sistema Cu/Cu(II-EDTA Potentiometric titrations of metal cations with edta using the Cu/Cu(II-EDTA system as indicator electrode

Directory of Open Access Journals (Sweden)

Paulo H. Pereira da Silva

2008-01-01

Full Text Available In potentiometric titrations of metal cations with EDTA the Hg/HgY2- system is usually used to detect the end point. However, the use of mercury has been discouraged in analytical procedures due to its toxicity. In this work the Cu/CuY2- system was used as indicator electrode for potentiometric titrations of some metal cations with EDTA. The solutions of Cu2+, Cd2+, Mn2+, Co2+ and Zn2+ were titrated with Na2EDTA solution in the presence of a small concentration of the CuY2- complex using a copper wire as indicator electrode. The potentiometric titrations with the Cu/CuY2- system showed good correlation when compared with an Hg/HgY2- system.

A potentiometric titration method for the crystallization of drug-like organic molecules.

Science.gov (United States)

Du-Cuny, Lei; Huwyler, Jörg; Fischer, Holger; Kansy, Manfred

2007-09-05

It is generally accepted, that crystalline solids representing a low energy polymorph should be selected for development of oral dosage forms. As a consequence, efficient and robust procedures are needed at an early stage during drug discovery to prepare crystals from drug-like organic molecules. In contrast to the use of supersaturated solutions, we present a potentiometric crystallization procedure where saturated solutions are prepared in a controlled manner by pH-titration. Crystallization is carried out under defined conditions using the sample concentration and experimental pK(a) values as input parameters. Crystals of high quality were obtained for 11 drugs selected to demonstrate the efficiency and applicability of the new method. Technical improvements are suggested to overcome practical limitations and to enhance the possibility of obtaining crystals from molecules in their uncharged form.

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

International Nuclear Information System (INIS)

Zarzycki, Piotr P.; Rosso, Kevin M.

2009-01-01

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

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

Science.gov (United States)

Zarzycki, Piotr; Rosso, Kevin M

2009-06-16

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

Development of a Novel Solid-State Sensor Electrode Based on Titanium Thin Film as an Indicator Electrode in Potentiometric and Conductometric Acid-Base Titration in Aqueous Solution

Directory of Open Access Journals (Sweden)

Nasser Abu Ghalwa

2012-01-01

Full Text Available A modified Ti/(SnO2 + Sb2O3 electrode was prepared by thermal deposition on titanium substrate and its use as indicator electrode to potentiometric and conductometric acid-base titration in aqueous solution at 298 K was developed. The E-pH curve is linear with slope of 0.0512 V/dec at 298 K. The standard potential of this electrode, E0, was determined with respect to the SCE as reference electrode. The recovery percentages for potentiometric and conductometric acid-base titration for acetic acid against NaOH were calculated. The cell constant, specific conductance, and the molar conductance with dilution for some common electrolytes were measured.

Effect of temperature, solvent and nature of metal cations on the potentiometric titration S of iron oxide

International Nuclear Information System (INIS)

Tasleem, S.; Ishrat, B.

2008-01-01

A comprehensive study of the potentiometric titrations of iron oxide in the presence of CU/sub 2/ and Mg/sup 2/ were under taken under different experimental conditions of temperature and concentration of metal ions in aqueous and aqueous/organic mixed solvent. The adsorption of both the metal ions were observed to increase with the increase in pH and temperature of the system. The adsorbent iron oxide preferentially adsorbs transition metal as compared to alkaline earth metal ion. (author)

Construction and use of an optical semi-automatic titrator employing the technique of reflectance photometry

International Nuclear Information System (INIS)

Hwang, Hoon

2001-01-01

An optical semi-automatic titrator was constructed employing the technique of the reflectance spectrometry and was tested for the determination of the end points of the acid-base, precipitation, and EDTA titrations. And since the current optical semi-automatic titrator built on the principle of the reflectance spectrometry could be successfully used even for the determination of the end of the end point in the precipitation titration where the solid particles are formed during the titration process, it was found to be feasible that a completely automated optical titrator would be designed and built based on the current findings

Laboratory Automatic Titration of Chromium Plating and Electropolishing Solutions

National Research Council Canada - National Science Library

Sopok, Samuel

2001-01-01

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

Colloidal titration of aqueous zirconium solutions with poly(vinyl sulfate) by potentiometric endpoint detection using a toluidine blue selective electrode.

Science.gov (United States)

Sakurada, Osamu; Kato, Yasutake; Kito, Noriyoshi; Kameyama, Keiichi; Hattori, Toshiaki; Hashiba, Minoru

2004-02-01

Zirconium oxy-salts were hydrolyzed to form positively charged polymer or cluster species in acidic solutions. The zirconium hydrolyzed polymer was found to react with a negatively charged polyelectrolyte, such as poly(vinyl sulfate), and to form a stoichiometric polyion complex. Thus, colloidal titration with poly(vinyl sulfate) was applied to measure the zirconium concentration in an acidic solution by using a Toluidine Blue selective plasticized poly(vinyl chloride) membrane electrode as a potentiometric end-point detecting device. The determination could be performed with 1% of the relative standard deviation. The colloidal titration stoichiometry at pH < or = 2 was one mol of zirconium per equivalent mol of poly(vinyl sulfate).

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

Science.gov (United States)

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

2016-05-01

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

Determination of total acidity index in bioethanol by automated potentiometric titration; Determinacao do indice de acidez total em bioetanol por titulacao potenciometrica automatizada

Energy Technology Data Exchange (ETDEWEB)

Sobral, Sidney Pereira; Ribeiro, Carla de Matos; Fraga, Isabel Cristina Serta; Goncalves, Mary Ane [Instituto Nacional de Metrologia, Normalizacao e Qualidade Industrial (DIMCI/INMETRO), Duque de Caxias, RJ (Brazil). Diretoria de Metrologia Cientifica e Industrial], E-mail: spsobral@inmetro.gov.br

2009-07-01

This paper determines the total acidity index of bioethanol by volumetric titration with potentiometric detection. Also, viewing the optimization of the method, studies are exhibited related to the repeatable, besides the comparison with the colorimetric method with the objective to contribute to the certification of bioethanol reference materials.

Indirect potentiometric titration of ascorbic acid in pharmaceutical preparations using copper based mercury film electrode.

Science.gov (United States)

Abdul Kamal Nazer, Meeran Mohideen; Hameed, Abdul Rahman Shahul; Riyazuddin, Patel

2004-01-01

A simple and rapid potentiometric method for the estimation of ascorbic acid in pharmaceutical dosage forms has been developed. The method is based on treating ascorbic acid with iodine and titration of the iodide produced equivalent to ascorbic acid with silver nitrate using Copper Based Mercury Film Electrode (CBMFE) as an indicator electrode. Interference study was carried to check possible interference of usual excipients and other vitamins. The precision and accuracy of the method was assessed by the application of lack-of-fit test and other statistical methods. The results of the proposed method and British Pharmacopoeia method were compared using F and t-statistical tests of significance.

Natural monocrystalline pyrite as a sensor in non-aqueous solution Part I: Potentiometric titration of weak acids in, N,N-dimethylformamide, methylpyrrolidone and pyridine.

Science.gov (United States)

Mihajlović, Lj V; Mihajlović, R P; Antonijević, M M; Vukanović, B V

2004-11-15

The possibility of applying natural monocrystaline pyrite as a sensor for the potentiometric titration of weak acids in N,N-dimethylformamide, methylpyrrolidone and pyridine was investigated. The potential of this electrode in N,N-dimethylformamide, methylpyrrolidone and pyridine exhibits a sub-Nernst dependence. In N,N-dimethylformamide the slope (mV/pH) is 39.0 and in methylpyrrolidone it is 45.0. The potential jumps at the titration end-point obtained in the titration of weak acids are higher than those obtained by the application of a glass electrode as the indicator electrode The potential in the course of the titration and at the titration end-point (TEP) are rapidly established. Sodium methylate, potassium hydroxide and tetrabutylammonium hydroxide (TBAH) proved to be very suitable titrating agents for these titrations. The results obtained in the determination of the investigated weak acids deviate by 0.1-0.35% with respect to those obtained by using a glass electrode as the indicator electrode.

Use of the sulfide mineral pyrite as electrochemical sensor in non-aqueous solutions: potentiometric titration of weak acids in acetonitrile, propionitrile and benzonitrile.

Science.gov (United States)

Mihajlović, Ljiljana; Nikolić-Mandić, Snezana; Vukanović, Branislav; Mihajlović, Randel

2009-03-01

Natural monocrystalline pyrite as a new indicator electrode for the potentiometric titration of weak acids in acetonitrile, propionitrile and benzonitrile was studied. The investigated electrode showed a linear dynamic response for p-toluenesulfonic acid concentrations in the range from 0.1 to 0.001 M, with a Nernstian slope of 74 mV per decade. Sodium methylate, potassium hydroxide and tetrabutylammonium hydroxide (TBAH) proved to be very suitable titrating agent for this titration. The response time was less than (11 s) and the lifetime of the electrode is long. The advantages of the electrode are log-term stability, fast response, and reproducibility, while the sensor is easy to prepare and of low cost.

Use of linear regression for the processing of curves of differential potentiometric titration of a binary mixture of heterovalent ions using precipitation reactions

International Nuclear Information System (INIS)

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

2003-01-01

A method is proposed for the computer processing of curve of differential potentiometric titration of a binary mixture of heterovalent ions using precipitation reactions. The method is based on the transformation of the titration curve to segment-line characteristics, whose parameters (within the accuracy of the least-squares method) determine the sequence of the equivalence points and solubility products of the resulting precipitation. The method is applied to the titration of Ag(I)-Cd)II), Hg(II)-Te(IV), and Cd(II)-Te(IV) mixtures by a sodium diethyldithiocarbamate solution with membrane sulfide and glassy carbon indicator electrodes. For 4 to 11 mg of the analyte in 50 ml of the solution, RSD varies from 1 to 9% [ru

Use of marker ion and cationic surfactant plastic membrane electrode for potentiometric titration of cationic polyelectrolytes.

Science.gov (United States)

Masadome, Takashi; Imato, Toshihiko

2003-07-04

A plasticized poly (vinyl chloride) (PVC) membrane electrode sensitive to stearyltrimethylammonium (STA) ion is applied to the determination of cationic polyelectrolytes such as poly (diallyldimethylammonium chloride) (Cat-floc) by potentiometric titration, using a potassium poly (vinyl sulfate) (PVSK) solution as a titrant. The end-point of the titration is detected as the potential change of the plasticized PVC membrane electrode caused by decrease in the concentration of STA ion added to the sample solution as a marker ion due to the ion association reaction between the STA ion and PVSK. The effects of the concentration of STA ion, coexisting electrolytes in the sample solution and pH of the sample on the degree of the potential change at the end-point were examined. A linear relationship between the concentration of cationic polyelectrolyte and the end-point volume of the titrant exists in the concentration range from 2x10(-5) to 4x10(-4) N for Cat-floc, glycol chitosan, and methylglycol chitosan.

Programa de ajuste multiparamétrico de curvas de titulação potenciométricas de ácidos húmicos Multiparametric adjustment program of potentiometric titration curves of humic acids

Directory of Open Access Journals (Sweden)

Clausius Duque Gonçalves Reis

2010-04-01

Full Text Available Tendo em vista a dificuldade de determinação dos pontos de inflexão na curva de titulação potenciométrica de ácidos húmicos, por metodologias tradicionais, foi desenvolvido foi desenvolvido um programa na linguagem Delphi para ajuste multiparamétrico de dados de titulação potenciométrica. Para isso um processo iterativo para estimar as raízes de um polinômio, com base no método de Newton-Raphson, foi utilizado. Os dados das titulações potenciométricas de ácidos húmicos usados nas regressões foram obtidos em um sistema automatizado de titulação potenciométrica. O programa desenvolvido na linguagem Delphi permite maior versatilidade e facilidade de operação, com uma interação mais amigável com o usuário. As curvas de titulação potenciométricas ajustadas sobrepuseram-se quase que totalmente às curvas experimentais. Os valores de pKa e as percentagens de grupos tituláveis dos ácidos húmicos, parâmetros ajustáveis na regressão multiparamétrica, apresentaram valores comparáveis com dados da literatura.Regarding the difficulty of determining the inflection points in the potentiometric titration curve of humic acids by means of traditional methodologies, a Delphi program a Delphi program was developed for the multiparametric data adjustment in potentiometric titration. For this purpose, an iterative process was used, based on the Newton-Raphson method to estimate the roots of a polynomial. The humic acid potentiometric titration data, used in regressions, were obtained in an automated system of potentiometric titration. The program developed in Delphi language features greater versatility, ease of operation and better interaction with the user. The adjusted potentiometric titration curves overlap the experimental curves almost entirely. The pKa values and percentages of titrable groups of humic acids extracted from soil, adjustable parameters in the multiparametric regression, were comparable with those reported

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

Science.gov (United States)

Meites, T; Meites, L

1970-06-01

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

Symmetry Properties of Potentiometric Titration Curves.

Science.gov (United States)

Macca, Carlo; Bombi, G. Giorgio

1983-01-01

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

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

Science.gov (United States)

Pehrsson, L; Ingman, F

1977-02-01

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

Potentiometric determination of ibuprofen, indomethacin and naproxen using an artificial neural network calibration

Directory of Open Access Journals (Sweden)

A. HAKAN AKTAŞ

2008-01-01

Full Text Available In this study, three anti-inflammatory agents, namely ibuprofen, indomethacin and naproxen, were titrated potentiometrically using tetrabutylammonium hydroxide in acetonitrile solvent under a nitrogen atmosphere at 25 °C. MATLAB 7.0 software was applied for data treatment as a multivariate calibration tool in the potentiometric titration procedure. An artificial neural network (ANN was used as a multivariate calibration tool in the potentiometric titration to model the complex non-linear relationship between ibuprofen, indomethacin and naproxen concentrations and the millivolt (mV of the solutions measured after the addition of different volumes of the titrant. The optimized network predicted the concentrations of agents in synthetic mixtures. The results showed that the employed ANN can precede the titration data with an average relative error of prediction of less than 2.30 %.

Statistical analysis of differential potentiometric precipitation titration data for a mixture of three heterovalent ions using linear characteristics

International Nuclear Information System (INIS)

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

2003-01-01

A computer-based method is proposed for data processing in the successive potentiometric precipitation titration of a three-component mixture of differently charged ions. The method was tested on the data of the titration of an artificial solution containing a mixture of Cd(II), Hg(II), and Te(IV) with diethyldithiocarbamate using a chalcogenide Cd-selective or a glassy-carbon indicator electrodes and was used for an analysis of the main components in a semiconductor material, namely, a solid solution of mercury and cadmium tellurides. For concentrations of test ions in the model solution from 7.5 x 10 -3 to 3 x 10 -4 M, the RSD value varies from 0.01 to 0.3; the determination error does not exceed 6 %. The RSD value for the semiconductor alloy lies in the range from 0.002 to 0.01 [ru

Elucidation of the electronic spectrum changes of KA-Al{sup 3+} complex by potentiometric titration, FTIR, {sup 13}C NMR and quantum mechanics

Energy Technology Data Exchange (ETDEWEB)

Piantavini, Mário S.; Gonçalves, Alan G.; Trindade, Ângela C.L.B.; Noseda, Miguel D.; Mercê, Ana L.R.; Pontarolo, Roberto, E-mail: pontarolo@ufpr.br [Universidade Federal do Paraná (UFPR), Curitiba (Brazil); Machado, Antonio E.H. [Universidade Federal de Uberlândia (UFU), MG (Brazil)

2017-08-15

Kojic acid (KA) is an organic acid widely used in pharmaceutical industry, mainly as a skin lightening agent. Based on the ability of KA to form complexes with ions, we found the most possible kind of complex formed with cation aluminum. KA-Al{sup 3+} complex structures were studied using potentiometric and spectrophotometric (UV) titrations, FTIR and {sup 13}C NMR. The electronic spectroscopy showed that the KA-Al{sup 3+} complexes absorb at higher wavelengths (λ{sub max}= 305 nm) than do the non-complexed KA (λ{sub max}= 269 nm), confirming complexation. The IR spectra of KA complexed and not complexed allowed to correlate the changes in the absorption of enol and carbonyl groups in absence and presence of Al{sup 3+} in aqueous solutions. The complexation suggested by the potentiometric titration and FTIR spectroscopy are in accordance with the data obtained from NMR results. Calculations based on quantum mechanics were utilized to understand the differences found in the non complexed and complexed KAH electronic spectra. (author)

Surface Complexation Modeling in Variable Charge Soils: Charge Characterization by Potentiometric Titration

Directory of Open Access Journals (Sweden)

Giuliano Marchi

2015-10-01

Full Text Available ABSTRACT Intrinsic equilibrium constants of 17 representative Brazilian Oxisols were estimated from potentiometric titration measuring the adsorption of H+ and OH− on amphoteric surfaces in suspensions of varying ionic strength. Equilibrium constants were fitted to two surface complexation models: diffuse layer and constant capacitance. The former was fitted by calculating total site concentration from curve fitting estimates and pH-extrapolation of the intrinsic equilibrium constants to the PZNPC (hand calculation, considering one and two reactive sites, and by the FITEQL software. The latter was fitted only by FITEQL, with one reactive site. Soil chemical and physical properties were correlated to the intrinsic equilibrium constants. Both surface complexation models satisfactorily fit our experimental data, but for results at low ionic strength, optimization did not converge in FITEQL. Data were incorporated in Visual MINTEQ and they provide a modeling system that can predict protonation-dissociation reactions in the soil surface under changing environmental conditions.

Assessment of two theoretical methods to estimate potentiometric titration curves of peptides: comparison with experiment.

Science.gov (United States)

Makowska, Joanna; Bagiñska, Katarzyna; Makowski, Mariusz; Jagielska, Anna; Liwo, Adam; Kasprzykowski, Franciszek; Chmurzyñski, Lech; Scheraga, Harold A

2006-03-09

We compared the ability of two theoretical methods of pH-dependent conformational calculations to reproduce experimental potentiometric titration curves of two models of peptides: Ac-K5-NHMe in 95% methanol (MeOH)/5% water mixture and Ac-XX(A)7OO-NH2 (XAO) (where X is diaminobutyric acid, A is alanine, and O is ornithine) in water, methanol (MeOH), and dimethyl sulfoxide (DMSO), respectively. The titration curve of the former was taken from the literature, and the curve of the latter was determined in this work. The first theoretical method involves a conformational search using the electrostatically driven Monte Carlo (EDMC) method with a low-cost energy function (ECEPP/3 plus the SRFOPT surface-solvation model, assumming that all titratable groups are uncharged) and subsequent reevaluation of the free energy at a given pH with the Poisson-Boltzmann equation, considering variable protonation states. In the second procedure, molecular dynamics (MD) simulations are run with the AMBER force field and the generalized Born model of electrostatic solvation, and the protonation states are sampled during constant-pH MD runs. In all three solvents, the first pKa of XAO is strongly downshifted compared to the value for the reference compounds (ethylamine and propylamine, respectively); the water and methanol curves have one, and the DMSO curve has two jumps characteristic of remarkable differences in the dissociation constants of acidic groups. The predicted titration curves of Ac-K5-NHMe are in good agreement with the experimental ones; better agreement is achieved with the MD-based method. The titration curves of XAO in methanol and DMSO, calculated using the MD-based approach, trace the shape of the experimental curves, reproducing the pH jump, while those calculated with the EDMC-based approach and the titration curve in water calculated using the MD-based approach have smooth shapes characteristic of the titration of weak multifunctional acids with small differences

Detecting Levels of Polyquaternium-10 (PQ-10) via Potentiometric Titration with Dextran Sulphate and Monitoring the Equivalence Point with a Polymeric Membrane-Based Polyion Sensor.

Science.gov (United States)

Ferguson, Stephen A; Wang, Xuewei; Meyerhoff, Mark E

2016-08-07

Polymeric quaternary ammonium salts (polyquaterniums) have found increasing use in industrial and cosmetic applications in recent years. More specifically, polyquaternium-10 (PQ-10) is routinely used in cosmetic applications as a conditioner in personal care product formulations. Herein, we demonstrate the use of potentiometric polyion-sensitive polymeric membrane-based electrodes to quantify PQ-10 levels. Mixtures containing both PQ-10 and sodium lauryl sulfate (SLS) are used as model samples to illustrate this new method. SLS is often present in cosmetic samples that contain PQ-10 (e.g., shampoos, etc.) and this surfactant species interferes with the polyion sensor detection chemistry. However, it is shown here that SLS can be readily separated from the PQ-10/SLS mixture by use of an anion-exchange resin and that the PQ-10 can then be titrated with dextran sulphate (DS). This titration is monitored by potentiometric polyanion sensors to provide equivalence points that are directly proportional to PQ-10 concentrations.

Using Spectrophotometric Titrations To Characterize Humic Acid Reactivity at Environmental Concentrations

International Nuclear Information System (INIS)

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

2010-01-01

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

Using Spectrophotometric Titrations To Characterize Humic Acid Reactivity at Environmental Concentrations

Energy Technology Data Exchange (ETDEWEB)

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

2010-07-01

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

The determination of titratable acidity and total tannins in red wine

OpenAIRE

Rajković Miloš B.; Sredović Ivana D.

2009-01-01

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

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

Science.gov (United States)

Lenoir, Thomas; Manceau, Alain

2010-03-16

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

Quantitative Determination of NTA and Other Chelating Agents in Detergents by Potentiometric Titration with Copper Ion Selective Electrode.

Science.gov (United States)

Ito, Sana; Morita, Masaki

2016-01-01

Quantitative analysis of nitrilotriacetate (NTA) in detergents by titration with Cu 2+ solution using a copper ion selective electrode was achieved. This method tolerates a wide range of pH and ingredients in detergents. In addition to NTA, other chelating agents, having relatively lower stability constants toward Cu 2+ , were also qualified with sufficient accuracy by this analytical method for model detergent formulations. The titration process was automated by automatic titrating systems available commercially.

Thermodynamic analysis of Bacillus subtilis endospore protonation using isothermal titration calorimetry

Science.gov (United States)

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.

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

International Nuclear Information System (INIS)

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

2005-01-01

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

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

Science.gov (United States)

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.

Investigation of interaction of phosphorotungstenvanadium heteropolyacids with sodium hydroxide by the methods of calorimetric and potentiometric titration

International Nuclear Information System (INIS)

Ganelina, E.Sh.; Borgoyakov, S.A.

1985-01-01

Interaction of phosphorotungstenvanadium heteropolyacids (HPA) with alkali (NaOH) is studied by the methods of calorimetric and potentiometric titration. Three stages are singled out: 1) neutralization of ''strong'' hydrogen atoms with a constant thermal effect of 52.0+-1.6 kJ/mol; 2) neutralization of ''weak'' protons, which acidity constant is of order 10 -2 ; 3) interaction of NaOH with hydrogen atoms combined with the internal sphere of HPA, and completed by HPA destruction. The data obtained are compared with the results, calculating the composition of polymer particles inside HPA, and they are discussed from the view point of their micellar structure

Investigation of uranyl-ion hydrolysis in uranyl pertechnetate and uranyl perchlorates solutions by two-phases potentiometric titration method

International Nuclear Information System (INIS)

Volk, V.I.; Belikov, A.D.

1977-01-01

The applicability of the method of two-phase potentiometric titration for studying hydrolysis of multi-charge ions has been shown. Hydrolysis of uranyl-ion has been investigated and hydrolysis constants in the solutions of uranyl pertechnetate and perchlorate have been calculated equal to (6.2+-0.15)x10 -5 and (9.25+-0.5)10 -5 , respectively. Infrared spectra of the initial crystallohydrates of uranyl pertechnetate and perchlorate has been analyzed. The data on hydrolysis of an uranyl-ion and IR spectra of crystallohydrates of the investigated salts have revealed the ability of pertechnetate ion to complexing with an uranyl group

Determination of the biodiesel acidity index by potentiometric titration by using different methods; Determinacao do indice de acidez de biodiesel por titulacao potenciometrica utilizando-se diferentes metodos

Energy Technology Data Exchange (ETDEWEB)

Goncalves, Mary Ane; Sobral, Sidney Pereira; Borges, Paulo Paschoal [Instituto Nacional de Metrologia, Normalizacao e Qualidade Industrial (DIMCI/INMETRO), Duque de Caxias, RJ (Brazil). Diretoria de Metrologia Cientifica e Industrial], E-mail: magoncalves@inmetro.gov.br

2009-07-01

This work determined the index of the soybean/fat bio diesel through the potentiometric titration. Four different methods were used with variation of solvent and electrodes. The results were compared by F and t (Student) and it was verified that they were agreed in a 95% confidence interval.

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

NARCIS (Netherlands)

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

2006-01-01

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

Potentiometric titrations in anhydrous acetic acid

International Nuclear Information System (INIS)

Le Port, L.

1966-03-01

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

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

Science.gov (United States)

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

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

Science.gov (United States)

Scherrer, Robert A; Donovan, Stephen F

2009-04-01

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

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

Science.gov (United States)

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

2009-10-01

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

Comparison between amperometric and true potentiometric end-point detection in the determination of water by the Karl Fischer method.

Science.gov (United States)

Cedergren, A

1974-06-01

A rapid and sensitive method using true potentiometric end-point detection has been developed and compared with the conventional amperometric method for Karl Fischer determination of water. The effect of the sulphur dioxide concentration on the shape of the titration curve is shown. By using kinetic data it was possible to calculate the course of titrations and make comparisons with those found experimentally. The results prove that the main reaction is the slow step, both in the amperometric and the potentiometric method. Results obtained in the standardization of the Karl Fischer reagent showed that the potentiometric method, including titration to a preselected potential, gave a standard deviation of 0.001(1) mg of water per ml, the amperometric method using extrapolation 0.002(4) mg of water per ml and the amperometric titration to a pre-selected diffusion current 0.004(7) mg of water per ml. Theories and results dealing with dilution effects are presented. The time of analysis was 1-1.5 min for the potentiometric and 4-5 min for the amperometric method using extrapolation.

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

Science.gov (United States)

Duc, Myriam; Gaboriaud, Fabien; Thomas, Fabien

2005-09-01

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

Non-aqueous titration of benzotrifuroxan (BTF)

Energy Technology Data Exchange (ETDEWEB)

Selig, W.

1978-01-01

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

Determination of Carbonyl Functional Groups in Bio-oils by Potentiometric Titration: The Faix Method.

Science.gov (United States)

Black, Stuart; Ferrell, Jack R

2017-02-07

Carbonyl compounds present in bio-oils are known to be responsible for bio-oil property changes upon storage and during upgrading. Specifically, carbonyls cause an increase in viscosity (often referred to as 'aging') during storage of bio-oils. As such, carbonyl content has previously been used as a method of tracking bio-oil aging and condensation reactions with less variability than viscosity measurements. Additionally, carbonyls are also responsible for coke formation in bio-oil upgrading processes. Given the importance of carbonyls in bio-oils, accurate analytical methods for their quantification are very important for the bio-oil community. Potentiometric titration methods based on carbonyl oximation have long been used for the determination of carbonyl content in pyrolysis bio-oils. Here, we present a modification of the traditional carbonyl oximation procedures that results in less reaction time, smaller sample size, higher precision, and more accurate carbonyl determinations. While traditional carbonyl oximation methods occur at room temperature, the Faix method presented here occurs at an elevated temperature of 80 °C.

Determination of neptunium by redox titration

International Nuclear Information System (INIS)

Godbole, A.G.; Patil, S.K.

1979-01-01

A simple and quick method for the potentiometric determination of neptunium on the 2 to 5 mg scale has been developed. It consists of oxidation to Np(VI) by AgO or fuming with HClO 4 , destruction of excess of AgO by sulphamic acid, reduction of Np(VI) to Np(IV) with a slight excess of standard Fe(II) in 2M H 2 SO 4 and potentiometric titration of the excess of Fe(II) with standard Ce(IV). The precision is +- 0.5%. (author)

Chemical sensors and the development of potentiometric methods for liquid media analysis

International Nuclear Information System (INIS)

Vlasov, Yu.G.; Kolodnikov, V.V.; Ermolenko, Yu.E.; Mikhajlova, S.S.

1996-01-01

Aspects of applying indirect potentiometric determination to chemical analysis are considered. Among them are the standard and modified addition and subtraction methods, the multiple addition method, and potentiometric titration using ion-selective electrodes as indicators. These methods significantly extend the capabilities of ion-selective potentiometric analysis. Conditions for the applicability of the above-mentioned methods to various samples (Cd, REE, Th, iodides and others) are discussed using all available ion-selective electrodes as examples. 162 refs., 2 figs., 5 tabs

Potentiometric determination of milligram amounts of uranium by semiautomatic titrator

International Nuclear Information System (INIS)

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

1978-01-01

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

Potentiometric application of boron- and phosphorus-doped glassy carbon electrodes

Directory of Open Access Journals (Sweden)

ZORAN V. LAUSEVIC

2001-03-01

Full Text Available Acomparative study was carried out of the potentiometric application of boronand phosphorus-doped and undoped glassy carbon samples prepared at the same heat treatment temperature (HTT 1000°C. The electrochemical activities of the obtained electrode materials were investigated on the example of argentometric titrations. It was found that the electrochemical behaviour of the doped glassy carbon samples are very similar to a Sigri (undoped glassy carbon sample (HTT 2400°C. The experiments showed that the potentiometric response depends on the polarization mode, the nature of the sample, the pretreatment of the electrode surface, and the nature of the supporting electrolyte. The amounts of iodide, bromide, and of chloridewere determined to be 1.27 mg, 0.80 mg and 0.54 mg, respectively, with a maximum relative standard deviation of less than 1.1%. The obtained results are in good agreement with the results of comparative potentiometric titrations using a silver indicator electrode. The titrationmethod was applied to the indirect determination of pyridoxine hydrochloride, i.e., vitamin B6.

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

Science.gov (United States)

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.

Specification analysis of plutonium fuels : a potentiometric method for the determination of plutonium

International Nuclear Information System (INIS)

Vaidyanathan, S.; Natarajan, P.R.

1977-01-01

A potentiometric method for the routine determination of plutonium in the specification analysis of plutonium fuels is described. Plutonium is oxidized to Pu(VI) with AgO and Pu(VI) is reduced with Fe(II) after the destruction of excess AgO with sulphamic acid. The excess Fe(II) is titrated potentiometrically against K 2 Cr 2 O 7 , the titration being carried out by adding a concentrated titrant solution from a weight burette and a suitably diluted solution from another weight burette near the end. The overall relative standard deviation obtained in 326 analyses of a working standard solution by eight experimenters is 0.14 percent. (author)

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

Science.gov (United States)

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

2013-10-01

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

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

Science.gov (United States)

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, ΔG 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.

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

NARCIS (Netherlands)

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

1984-01-01

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

Determination of pKa values of alendronate sodium in aqueous solution by piecewise linear regression based on acid-base potentiometric titration.

Science.gov (United States)

Ke, Jing; Dou, Hanfei; Zhang, Ximin; Uhagaze, Dushimabararezi Serge; Ding, Xiali; Dong, Yuming

2016-12-01

As a mono-sodium salt form of alendronic acid, alendronate sodium presents multi-level ionization for the dissociation of its four hydroxyl groups. The dissociation constants of alendronate sodium were determined in this work by studying the piecewise linear relationship between volume of titrant and pH value based on acid-base potentiometric titration reaction. The distribution curves of alendronate sodium were drawn according to the determined pKa values. There were 4 dissociation constants (pKa 1 =2.43, pKa 2 =7.55, pKa 3 =10.80, pKa 4 =11.99, respectively) of alendronate sodium, and 12 existing forms, of which 4 could be ignored, existing in different pH environments.

Investigation of the interaction of iron(III) complexes with dAMP by ESI-MS, MALDI-MS and potentiometric titration: insights into synthetic nuclease behavior.

Science.gov (United States)

Fernandes, Christiane; Oliveira Moreira, Rafaela; Lube, Leonardo M; Horn, Adolfo; Szpoganicz, Bruno; Sherrod, Stacy; Russell, David H

2010-06-07

We report herein the characterization by electrospray ionization (ESI) mass spectrometry (MS), matrix assisted laser desorption ionization (MALDI-MS) and potentiometric titration of three iron(III) compounds: [Fe(III)(HPClNOL)Cl2]·NO3 (1), [Cl(HPClNOL)Fe(III)-(μ-O)-Fe(III)(HPClNOL)Cl]·Cl2·H2O (2) and [(SO4)(HPClNOL)Fe(III)-(μ-O)-Fe(III)(HPClNOL)(SO4)]·6H2O (3), where HPClNOL= 1-(bis-pyridin-2-ylmethyl-amino)-3-chloropropan-2-ol). Despite the fact that the compounds have distinct structures in solid state and non-buffered solution, all compounds present similar ESI and MALDI mass spectra in a buffered medium (pH 7.0). At this pH, the species [(PClNOL)Fe(III)-(μ-O)-Fe(III)(PClNOL)](2+) (m/z 354) was observed for all the compounds under investigation. Potentiometric titration confirms a similar behavior for all compounds, indicating that the dihydroxo form [(OH)(HPClNOL)Fe(III)-(μ-O)-Fe(III)(HPClNOL)(OH)](2+) is the major species at pH 7.0, for all the compounds. The products of the interaction between compounds (1), (2) and (3) and dAMP (2'-deoxyadenosine-5'-monophosphate) in a buffered medium (pH 7.0) were identified by MALDI-MS/MS. The fragmentation data obtained by MS/MS allow one to identify the nature of the interaction between the iron(III) compounds and dAMP, revealing the direct interaction between the iron center and phosphate groups.

Potentiometric titration of polyhexamethylene biguanide hydrochloride with potassium poly(vinyl sulfate) solution using a cationic surfactant-selective electrode.

Science.gov (United States)

Masadome, Takashi; Yamagishi, Yuichi; Takano, Masaki; Hattori, Toshiaki

2008-03-01

A potentiometric titration method using a cationic surfactant as an indicator cation and a plasticized poly(vinyl chloride) membrane electrode sensitive to the cationic surfactant is proposed for the determination of polyhexamethylene biguanide hydrochloride (PHMB-HCl), which is a cationic polyelectrolyte. A sample solution of PHMB-HCl containing an indicator cation (hexadecyltrimethylammonium ion, HTA) was titrated with a standard solution of an anionic polyelectrolyte, potassium poly(vinyl sulfate) (PVSK). The end-point was detected as a sharp potential change due to an abrupt decrease in the concentration of the indicator cation, HTA, which is caused by its association with PVSK. The effects of the concentrations of HTA ion and coexisting electrolytes in the sample solution on the degree of the potential change at the end-point were examined. A linear relationship between the concentration of PHMB-HCl and the end-point volume of the titrant exists in the concentration range from 2.0 x 10(-5) to 4.0 x 10(-4) M in the case that the concentration of HTA is 1.0 x 10(-5) M, and that from 1.0 x 10(-6) to 1.2 x 10(-5) M in the case that the concentration of HTA is 5.0 x 10(-6) M, respectively. The proposed method was applied to the determination of PHMB-HCl in some contact-lens detergents.

Potentiometric determination of free nitric-acid in trilaurylamine solutions containing plutonium nitrate

International Nuclear Information System (INIS)

Perez, J.J.; Saey, J.C.

1965-01-01

A potentiometric method of determination of the free nitric acid in trilaurylamine solutions containing plutonium or thorium nitrates is described. The potentiometric titration is carried out in a mixture of benzene and 1,2-dichloro ethane with a standard solution of trilaurylamine as the titrant. When thorium nitrate is present the metal complex is not dissociated then the titration has a single end-point. In the case of plutonium nitrate the partial dissociation of the plutonium complex corresponds to a second point. The experimental error in duplicate analyses of 50 samples is about 1 per cent for free acid concentrations in the range of 0,03 to 0,1 N and plutonium concentrations between 1 to 5 g/l. (authors) [fr

Potentiometric microdetermination of cadmium in organic compounds after oxygen flask combustion

International Nuclear Information System (INIS)

Campiglio, A.

1986-01-01

The sample is burnt in an oxygen flask and the combustion products are absorbed in 1Μ HNO 3 . After removal of interfering gases by boiling, the solution is transfered to the titration cell and neutralized with NaOH in the presence of methyl red; cd(II) is finally titrated potentiometrically in a buffered 50% ethanolic medium with 0.01Μ sodium diethyldithiocarbamate in 50% ethanol. A silver/sulphide ion-selective electrode and a double junction referenceelectrode containing a 10% KNO 3 solution in 26% ethanol in the outer compartment are used in combination with a Titroprocessor to detect the end point. The results obtained are very accurate and reproducible: the maximum error does not exceed 0.09%, the recovery of cadmium is in the range 99.67 to 99.95% and the rel. standard deviation is 0.05%. The potentiometric titration with diethyldithiocarbamate, which is useful to determine small Cd(II) amounts down to 30μg (2μg ml -1 ), as well as the oxygen flask combustion of organic cadmium compounds are discussed. (Author)

Relationship between potentiometric measurements, sensorial analysis, and some substances responsible for aroma degradation of white wines.

Science.gov (United States)

Silva Ferreira, A C; Oliveira, Carla; Hogg, T; Guedes de Pinho, P

2003-07-30

Oxidative degradation of white wines can be described sensorially as developing from a loss at positive aroma characteristics, through the development of negative aromas to a linel stage of chromatic alterations. This work attempts to relate the oxidation "status" evaluate by potentiometric titrations, with sensorial degradation and the levels of substances responsible for "off-flavors", such as methional and phenylacetaldehyde. The potentiometric titration employed measures the most powerful antioxidants of white wines (e.g., those which more rapidly consume oxygen). Considering that aromatic precedes chromatic degradation, resistance to oxidation (ROX) constitutes a useful indicator of resistance to oxidation. Sensorial degradation (ID), potentiometric measures, and volatiles were determined both in samples submitted to a "forced aging" protocol and normal aged white wines. High correlation values were observed between ROX and the ID, in both sets (r > 0.87). ID is better explained by ROX values than by the indicated wine age or by the "degree of browning" (Abs = 420 nm). It was also observed that in samples with ROX values higher than 10, the concentration of methional and phenylacetaldehyde were above their respective odor threshold. Finally, it was observed that there is a relationship between oxygen consumption and the respective ROX. Although these results seem very promising, they needed to be further complemented in order to estimate the shelf life of a white wine using potentiometric titrations.

Potentiometric studies on the complexes of tetracycline (TC) and oxytetracycline (OTC) with some metal ions

International Nuclear Information System (INIS)

Ghandour, M.A.; Azab, H.A.; Hassan, A.; Ali, A.M.

1992-01-01

The interaction of Cr(III), Mn(II), Fe(III), Co(II), Ni(II), Zn(II), Cd(II), Hg(II), Pb(II), Al(III), and UO 2 (II) ions with tetracycline (TC) were studied by potentiometric pH titrations. The formation constants of the different binary complexes formed in such systems have been determined at 25±0.1 deg C and μ=0.1 moll -1 (NaNO 3 ). Potentiometric pH equilibrium measurements have been made under the same conditions for the interaction of oxytetracycline (OTC) and Cu(II), Cd(II), Pb(II), and UO 2 (II). The formation of (1:1) binary complexes are inferred from the potentiometric pH titration curves. The protonation constants of TC and OTC were also determined under the same conditions and refined (ESAB2M computer program). The transition metal stability constants are consistent with the Irving-Williams series. (authors)

Fluorinated tripodal receptors for potentiometric chloride detection in biological fluids.

Science.gov (United States)

Pankratova, Nadezda; Cuartero, Maria; Jowett, Laura A; Howe, Ethan N W; Gale, Philip A; Bakker, Eric; Crespo, Gastón A

2018-01-15

Fluorinated tripodal compounds were recently reported to be efficient transmembrane transporters for a series of inorganic anions. In particular, this class of receptors has been shown to be suitable for the effective complexation of chloride, nitrate, bicarbonate and sulfate anions via hydrogen bonding. The potentiometric properties of urea and thiourea-based fluorinated tripodal receptors are explored here for the first time, in light of the need for reliable sensors for chloride monitoring in undiluted biological fluids. The ion selective electrode (ISE) membranes with tren-based tris-urea bis(CF 3 ) tripodal compound (ionophore I) were found to exhibit the best selectivity for chloride over major lipophilic anions such as salicylate ( [Formula: see text] ) and thiocyanate ( [Formula: see text] ). Ionophore I-based ISEs were successfully applied for chloride determination in undiluted human serum as well as artificial serum sample, the slope of the linear calibration at the relevant background of interfering ions being close to Nernstian (49.8±1.7mV). The results of potentiometric measurements were confirmed by argentometric titration. Moreover, the ionophore I-based ISE membrane was shown to exhibit a very good long-term stability of potentiometric performance over the period of 10 weeks. Nuclear magnetic resonance (NMR) titrations, potentiometric sandwich membrane experiments and density functional theory (DFT) computational studies were performed to determine the binding constants and suggest 1:1 complexation stoichiometry for the ionophore I with chloride as well as salicylate. Copyright © 2017 Elsevier B.V. All rights reserved.

Potentiometric sensing of nuclease activities and oxidative damage of single-stranded DNA using a polycation-sensitive membrane electrode.

Science.gov (United States)

Ding, Jiawang; Qin, Wei

2013-09-15

A simple, general and label-free potentiometric method to measure nuclease activities and oxidative DNA damage in a homogeneous solution using a polycation-sensitive membrane electrode is reported. Protamine, a linear polyionic species, is used as an indicator to report the cleavage of DNA by nucleases such as restriction and nonspecific nucleases, and the damage of DNA induced by hydroxyl radicals. Measurements can be done with a titration mode or a direct detection mode. For the potentiometric titration mode, the enzymatic cleavage dramatically affects the electrostatical interaction between DNA and protamine and thus shifts the response curve for the potentiometric titration of the DNA with protamine. Under the optimized conditions, the enzyme activities can be sensed potentiometrically with detection limits of 2.7×10(-4)U/µL for S1 nuclease, and of 3.9×10(-4)U/µL for DNase I. For the direct detection mode, a biocomplex between protamine and DNA is used as a substrate. The nuclease of interest cleaves the DNA from the protamine/DNA complex into smaller fragments, so that free protamine is generated and can be detected potentiometrically via the polycation-sensitive membrane electrode. Using a direct measurement, the nuclease activities could be rapidly detected with detection limits of 3.2×10(-4)U/µL for S1 nuclease, and of 4.5×10(-4)U/µL for DNase I. Moreover, the proposed potentiometric assays demonstrate the potential applications in the detection of hydroxyl radicals. It is anticipated that the present potentiometric strategy will provide a promising platform for high-throughput screening of nucleases, reactive oxygen species and the drugs with potential inhibition abilities. Copyright © 2013 Elsevier B.V. All rights reserved.

Potentiometric determination of uranium with cobalt (3) acetate as oxidimetric titrant

International Nuclear Information System (INIS)

Muhammad, H.; Ishrat, P.; Zyka, J.

1972-01-01

A potentiometric method for the determination of uranium through the reduction of hexavalent to tetravalent state and its potentiometric oxidation in 8 N sulphuric acid with standard cobalt (3)-acetate has been worked out. The method is quite accurate with the error not exceeding 1% for mg amounts. Moreover an apparatus for preservation of reduced solution of uranium and its delivery for titrations has been designed. The same apparatus can be used for reducing and preserving solutions of strong reducing titrants. (author)

Potentiometric determination of hexavalent uranium in uranium silicide samples

International Nuclear Information System (INIS)

Arlegui, Oscar

1999-01-01

The Chilean Nuclear Energy Commission's Department of Nuclear Materials has among its projects the production of fuels elements for nuclear reactors, and, therefore, the Chemical Analysis Laboratory must have a rapid and reliable method for uranium analysis, to control the uranium concentration during each stage of the production process. For this reason the Chilean Nuclear Energy Commission's Chemical Analysis Laboratory has validated a potentiometric method, which is a modification of the Davies and Gray method proposed by A.R. Eberle. This method uses the Potentiometric Titration Technique and is based on the direct and rapid reduction of uranium (VI) to Uranium (IV), in a concentrated phosphoric acid medium, with excess iron (II) used as a reducing agent. In this medium the excess iron (II) selectively oxidizes to iron (III) with nitric acid, using molybdenum (IV) as a catalyzer, the nitrous acid that is produced is eliminated by adding amidosulfuric acid. The solution is diluted with 1M sulfuric acid and the uranium (IV) obtained is titrated potentiometrically with potassium dichromate in the presence of vanadilic sulfate to obtain a better defined final titration point. The samples were softened with hydrochloric acid and nitric acid and later 50 ml were estimated in a 20% sulfuric acid medium. The analytical method was validated by comparing it with Certified Reference Material (C.R.M.) from the New Brunswick Laboratory (NBL), Metallic Uranium, CRM 112-A. The F Test and the T Test show that the value calculated is less than the tabulated value so the result is traceable to the reference material. The quantification limit, sensitivity, precision and accuracy were quantified for the method

Comparison of manual versus automatic continuous positive airway pressure titration and the development of a predictive equation for therapeutic continuous positive airway pressure in Chinese patients with obstructive sleep apnoea.

Science.gov (United States)

Luo, Jiaying; Xiao, Sichang; Qiu, Zhihui; Song, Ning; Luo, Yuanming

2013-04-01

Whether the therapeutic nasal continuous positive airway pressure (CPAP) derived from manual titration is the same as derived from automatic titration is controversial. The purpose of this study was to compare the therapeutic pressure derived from manual titration with automatic titration. Fifty-one patients with obstructive sleep apnoea (OSA) (mean apnoea/hypopnoea index (AHI) = 50.6 ± 18.6 events/h) who were newly diagnosed after an overnight full polysomnography and who were willing to accept CPAP as a long-term treatment were recruited for the study. Manual titration during full polysomnography monitoring and unattended automatic titration with an automatic CPAP device (REMstar Auto) were performed. A separate cohort study of one hundred patients with OSA (AHI = 54.3 ± 18.9 events/h) was also performed by observing the efficacy of CPAP derived from manual titration. The treatment pressure derived from automatic titration (9.8 ± 2.2 cmH(2)O) was significantly higher than that derived from manual titration (7.3 ± 1.5 cmH(2)O; P titration (54.3 ± 18.9 events/h before treatment and 3.3 ± 1.7 events/h after treatment; P titration pressure derived from REMstar Auto is usually higher than the pressure derived from manual titration. © 2013 The Authors. Respirology © 2013 Asian Pacific Society of Respirology.

Model compounds of humic acid and oxovanadium cations. Potentiometric titration and EPR spectroscopy studies

Directory of Open Access Journals (Sweden)

Mercê Ana Lucia Ramalho

1999-01-01

Full Text Available The stability constants and the isotropic EPR parameters Ao (hyperfine splitting constant and g o (g value were obtained by potentiometric titrations and EPR spectroscopy, respectively, of 85%v/v aqueous solutions of model compounds of humic acids - salicylic acid (SALA - and both nitrohumic acids, a laboratory artifact - nitrosalicylic acids, 3-nitrosalicylic acid (3-NSA, 5-nitrosalicylic acid (5-NSA and 3,5-dinitrosalicylic acid (3,5-DNSA and oxovanadium cations. It was possible to record EPR spectra of those model compounds and the ion VO2+ (V(IV, and the stability constants were obtained from a solution of VO3+ (V(V, the values for the logarithms of the stability constants ranging from 12.77 ± 0.04 to 7.06 ± 0.05 for the species ML, and from 9.90 ±0.04 to 4.06 ± 0.05 for the species ML2 according to the decrease in the acidity of the carboxylic and the hydroxyl groups in the aromatic ring of the model compounds studied as the -NO2 substituents were added. Species distribution diagrams were also obtained for the equilibria studied. The EPR parameters showed that as the logarithm of the overall stability constants increase, g o values also increase, while Ao values show a tendency to decrease.

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

Science.gov (United States)

Skic, Kamil; Boguta, Patrycja; Sokołowska, Zofia

2016-07-01

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

NABTIT-a computer program for non-aqueous acid-base titration.

Science.gov (United States)

Budevsky, O; Zikolova, T; Tencheva, J

1988-11-01

A program NABTIT written in BASIC has been developed for the treatment of data (ml/mV) obtained from potentiometric acid-base titrations in non-aqueous solvents. No preliminary information on equilibrium constants is required for the input. The treatment of the data is based on known equations and uses least-squares procedures. The essence of the method is to determine the equivalence volume (V(e)) accurately, and to use the data acquired by adding titrant after V(e) for the pH*-calibration of the non-aqueous potentiometric cell. As a by-product or the calculations, the pK* value of the substance titrated is also obtained, and in some cases the autoprotolysis constant of the medium (pK*(s)). Good agreement between experiment and theory was found in the treatment of data obtained for water and methanol-water mixtures.

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

International Nuclear Information System (INIS)

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

2010-01-01

In order to have a better understanding of the interactions of heavy metals with bacteria and minerals in soil and associated environments, isothermal titration calorimetry (ITC), potentiometric titration and equilibrium sorption experiments were conducted to investigate the adsorption behavior of Cu(II) by Bacillus thuringiensis, Pseudomonas putida and their composites with minerals. The interaction of montmorillonite with bacteria increased the reactive sites and resulted in greater adsorption for Cu(II) on their composites, while decreased adsorption sites and capacities for Cu(II) were observed on goethite-bacteria composites. A gram-positive bacterium B. thuringiensis played a more important role than a gram-negative bacterium P. putida in determining the properties of the bacteria-minerals interfaces. The enthalpy changes (ΔH ads ) from endothermic (6.14 kJ mol -1 ) to slightly exothermic (-0.78 kJ mol -1 ) suggested that Cu(II) is complexed with the anionic oxygen ligands on the surface of bacteria-mineral composites. Large entropies (32.96-58.89 J mol -1 K -1 ) of Cu(II) adsorption onto bacteria-mineral composites demonstrated the formation of inner-sphere complexes in the presence of bacteria. The thermodynamic data implied that Cu(II) mainly bound to the carboxyl and phosphoryl groups as inner-sphere complexes on bacteria and mineral-bacteria composites.

Coulometric titration of niobium in EDTA complexing solution

International Nuclear Information System (INIS)

Pannu, S.S.

1976-01-01

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

Determination of dissociation constants for coordination compounds of Cr(III) and Co(III) using potentiometric and spectrophotometric methods

International Nuclear Information System (INIS)

Chylewska, A.; Jacewicz, D.; Zarzeczanska, D.; Chmurzynski, L.

2008-01-01

The acid-base properties of analogous complex ions of chromium(III) and cobalt(III) in aqueous solution have been studied. The equilibrium constants for all metal complexes were determined by using potentiometric and spectrophotometric titration methods. First, dissociation constants for the studied complexes of Cr(III) and Co(III) were determined by means of the potentiometric titration method and using the STOICHIO computer programme. Then, pH-spectrophotometric titrations were performed and the OriginPro 7.5 computer programme was used to calculate the same constants. The measurements using both methods were carried out under the same conditions of temperature, T = 298.15 K, and over the same pH range 2.00-10.00, respectively. It turned out that the two methods used enabled us to obtain acidity constants in very good agreement

Determination of dissociation constants for coordination compounds of Cr(III) and Co(III) using potentiometric and spectrophotometric methods

Energy Technology Data Exchange (ETDEWEB)

Chylewska, A.; Jacewicz, D.; Zarzeczanska, D. [Department of Chemistry, University of Gdansk, Sobieskiego 18/19, 80-952 Gdansk (Poland); Chmurzynski, L. [Department of Chemistry, University of Gdansk, Sobieskiego 18/19, 80-952 Gdansk (Poland)], E-mail: lech@chem.univ.gda.pl

2008-08-15

The acid-base properties of analogous complex ions of chromium(III) and cobalt(III) in aqueous solution have been studied. The equilibrium constants for all metal complexes were determined by using potentiometric and spectrophotometric titration methods. First, dissociation constants for the studied complexes of Cr(III) and Co(III) were determined by means of the potentiometric titration method and using the STOICHIO computer programme. Then, pH-spectrophotometric titrations were performed and the OriginPro 7.5 computer programme was used to calculate the same constants. The measurements using both methods were carried out under the same conditions of temperature, T = 298.15 K, and over the same pH range 2.00-10.00, respectively. It turned out that the two methods used enabled us to obtain acidity constants in very good agreement.

Ruthenium determination in new composite materials by coulometric titration with generated iron(2)

International Nuclear Information System (INIS)

Butakova, N.A.; Oganesyan, L.B.

1983-01-01

A coulometric technique is developed for ruthenium (4) titration with generated iron (2) in a mixture of hydrochloric-, sulfuric- and phosphoric acids with potentiometric and biammetric indication of the final titration point. Bi (3), Pd (2), Nb (5), Pt (4) Pb (2), Rh (3) do not interfere with the titration. Together with Ru (4) titrated are Ir (4), V (5), Au (3). The method is applied to analyze commercial samples of ruthenium dioxides, lead- and bismuth ruthenites, ruthenium pentafluorides containing 30-80% of ruthenium. The Ssub(r) values do not exceed 0.002

Cell surface groups of two picocyanobacteria strains studied by zeta potential investigations, potentiometric titration, and infrared spectroscopy.

Science.gov (United States)

Dittrich, Maria; Sibler, Sabine

2005-06-15

In order to clarify the role of picocyanobacteria in aquatic biogeochemical processes (e.g., calcite precipitation), cell surface properties need to be investigated. An experimental study of the cell surface characteristics of two Synechococcus-type unicellular autotrophic picocyanobacterial strains was carried out. One strain was isolated from Lake Plon and contained phycocyanin, the other strain came from Lago Maggiore and was rich in phycoerythrin. Potentiometric titrations were conducted to determine the different types of sites present on the bacteria cell walls. Infrared spectroscopy allowed characterization of the various functional groups (RNH(2), RCOOH, ROH, RPO(2)) and investigations of zeta potential provided insight into the isoelectrical points of the strains. Titrations reveal three distinct sites on the bacterial surfaces of phycocyanin- and phycoerythrin-rich strains with pK values of 4.8+/-0.3/5.0+/-0.2, 6.6+/-0.2/6.7+/-0.4, and 8.8+/-0.1/8.7+/-0.2, corresponding to carboxyl, phosphate, and amine groups with surface densities of 2.6+/-0.4/7.4+/-1.6 x 10(-4), 1.9+/-0.5/4.4+/-0.8 x 10(-4), and 2.5+/-0.4/4.8+/-0.7 x 10(-4) mol/g of dry bacteria. The deprotonation constants are similar to those of bacterial strains and site densities are also within an order of magnitude of other strains. The phycoerythrin-rich strain had a higher number of binding sites than the phycocyanin-rich strain. The results showed that picocyanobacteria may adsorb either calcium cations or carbonate anions and therefore strongly influence the biogeochemical cycling of calcite in pelagic systems.

Implementation of the automated potentiometric titration method for total U at the CNEN Safeguard Laboratory, Brazil; Implementacao do metodo de titulacao potenciometrica automatizado para U total no Laboratorio de Salvaguardas da CNEN, Brasil

Energy Technology Data Exchange (ETDEWEB)

Cristiano, Barbara F.G.; Delgado, Jose U.; Araujo, Radier M.S. de; Silva, Jose W.S. da; Barros, Pedro D. de, E-mail: barbara@ird.gov.b [Instituto de Radioprotecao e Dosimetria (IRD/CNEN-RJ), Rio de Janeiro, RJ (Brazil)

2009-07-01

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

Online Automatic Titration of Chromic Acid in Chromium Plating Solutions and Phosphoric and Sulfuric Acids in Electropolishing Solutions

National Research Council Canada - National Science Library

Sopok, Samuel

1991-01-01

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

A new potentiometric method for the estimation of the rare earth elements

International Nuclear Information System (INIS)

Selig, W.S.

1988-01-01

Chinese workers recently described a new potentiometric method for lead using sodium tetraphenylborate (NaTPB) as a titrant. Based on a previous Chinese publication, the authors have recently developed a method for the estimation of the alkaline earth metals by sequential titration with NaTPB. In the present work, the authors report a similar method for the estimation of the rare earth elements, including Sc and Y. The sensing electrode is a spectrographic graphite rod, coated with a solution of poly(vinyl chloride) and dioctylphthalate in tetrahydrofuran as previously described. The reference electrode was a double-junction Ag/AgCl electrode. The titration system is controlled by a Tektronix 4051 graphics computer system. Single cations or mixtures up to 0.5 mequiv are determined by potentiometric titration with 0.05 N NaTPB, after formation of the oxonium cations by reaction with an aqueous solution of poly(ethylene glycol) (PEG). Best results are obtained with PEGs of molecular weights from 8,000 to 20,000. Sequential estimation of Pb + Ba, Sr, and Ca, and the sum of the rare earth elements is also reported, plus possible applications to Al, Ga, and anions precipitated by lead

Potentiometric studies on some ternary complexes of Nd(III), Sm(III), Gd(III) and Ho(III) with cyclohexanediaminetetraacetic acid as primary ligand

International Nuclear Information System (INIS)

Marathe, D.G.; Munshi, K.N.

1983-01-01

The formation constants of the ternary complexes of neodymium(III), samarium(III), gadlonium(III) and holmium(III) with cyclohexanediaminetetraacetic acid (CyDTA) as primary ligand and dihydroxynaphthalene (DHN), dihydroxynaphthalene-6-sulphonic acid (DHNSA) and cateechol-3,5-disulphonic acid (CDSA) as secondary ligands have been investigated by potentiometric titration technique. The secondary ligands have been investigated by potentiometric titration technique. The values of formation constants of 1:1:1 ternary chelates are reported at three different temperatures, and at a fixed ionic strength, μ = 0.1 M (NaClO 4 ). (author)

Coulometric titration of niobium in 1F sulfuric acid

International Nuclear Information System (INIS)

Pannu, S.S.

1975-01-01

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

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

International Nuclear Information System (INIS)

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

2004-01-01

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

Ni(III) - a new oxidant for the potentiometric determination of plutonium

International Nuclear Information System (INIS)

Gopinath, N.; Rama Rao, G.A.; Natarajan, P.R.

1986-01-01

Ni(III) was employed as an oxidant for the quantitative oxidation of plutonium to its hexavalent state and this makes possible to determine plutonium concentrations potentiometrically by the Fe(II)-dichromate redox titration method. The unreacted oxidant is completely reduced by sulphamic acid prior to the determination of plutonium. (author)

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

Energy Technology Data Exchange (ETDEWEB)

Fang Linchuan [State Key Laboratory of Agricultural Microbiology, Huazhong Agricultural University, Wuhan 430070 (China); Key Laboratory of Subtropical Agriculture and Environment, Ministry of Agriculture, College of Resources and Environment, Huazhong Agricultural University, Wuhan 430070 (China); Cai Peng; Li Pengxiang; Wu Huayong; Liang Wei; Rong Xingmin [Key Laboratory of Subtropical Agriculture and Environment, Ministry of Agriculture, College of Resources and Environment, Huazhong Agricultural University, Wuhan 430070 (China); Chen Wenli [State Key Laboratory of Agricultural Microbiology, Huazhong Agricultural University, Wuhan 430070 (China); Huang Qiaoyun, E-mail: qyhuang@mail.hzau.edu.cn [State Key Laboratory of Agricultural Microbiology, Huazhong Agricultural University, Wuhan 430070 (China); Key Laboratory of Subtropical Agriculture and Environment, Ministry of Agriculture, College of Resources and Environment, Huazhong Agricultural University, Wuhan 430070 (China)

2010-09-15

In order to have a better understanding of the interactions of heavy metals with bacteria and minerals in soil and associated environments, isothermal titration calorimetry (ITC), potentiometric titration and equilibrium sorption experiments were conducted to investigate the adsorption behavior of Cu(II) by Bacillus thuringiensis, Pseudomonas putida and their composites with minerals. The interaction of montmorillonite with bacteria increased the reactive sites and resulted in greater adsorption for Cu(II) on their composites, while decreased adsorption sites and capacities for Cu(II) were observed on goethite-bacteria composites. A gram-positive bacterium B. thuringiensis played a more important role than a gram-negative bacterium P. putida in determining the properties of the bacteria-minerals interfaces. The enthalpy changes ({Delta}H{sub ads}) from endothermic (6.14 kJ mol{sup -1}) to slightly exothermic (-0.78 kJ mol{sup -1}) suggested that Cu(II) is complexed with the anionic oxygen ligands on the surface of bacteria-mineral composites. Large entropies (32.96-58.89 J mol{sup -1} K{sup -1}) of Cu(II) adsorption onto bacteria-mineral composites demonstrated the formation of inner-sphere complexes in the presence of bacteria. The thermodynamic data implied that Cu(II) mainly bound to the carboxyl and phosphoryl groups as inner-sphere complexes on bacteria and mineral-bacteria composites.

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

Science.gov (United States)

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

2010-09-15

In order to have a better understanding of the interactions of heavy metals with bacteria and minerals in soil and associated environments, isothermal titration calorimetry (ITC), potentiometric titration and equilibrium sorption experiments were conducted to investigate the adsorption behavior of Cu(II) by Bacillus thuringiensis, Pseudomonas putida and their composites with minerals. The interaction of montmorillonite with bacteria increased the reactive sites and resulted in greater adsorption for Cu(II) on their composites, while decreased adsorption sites and capacities for Cu(II) were observed on goethite-bacteria composites. A gram-positive bacterium B. thuringiensis played a more important role than a gram-negative bacterium P. putida in determining the properties of the bacteria-minerals interfaces. The enthalpy changes (DeltaH(ads)) from endothermic (6.14 kJ mol(-1)) to slightly exothermic (-0.78 kJ mol(-1)) suggested that Cu(II) is complexed with the anionic oxygen ligands on the surface of bacteria-mineral composites. Large entropies (32.96-58.89 J mol(-1) K(-1)) of Cu(II) adsorption onto bacteria-mineral composites demonstrated the formation of inner-sphere complexes in the presence of bacteria. The thermodynamic data implied that Cu(II) mainly bound to the carboxyl and phosphoryl groups as inner-sphere complexes on bacteria and mineral-bacteria composites. Copyright 2010 Elsevier B.V. All rights reserved.

Potentiometric end point detection in the EDTA titrimetric determination of gallium

International Nuclear Information System (INIS)

Gopinath, N.; Renuka, M.; Aggarwal, S.K.

2001-01-01

Gallium is titrated in presence of known amount of Fe (III) with EDTA in HNO 3 solution at pH 2 to 3. The end point is detected potentiometrically employing a bright platinum wire - saturated calomel (SCE) reference electrode system, the redox couple being Fe (III) / Fe (II). Since Fe (III) is also titrated by EDTA, it is, therefore, subtracted from titre value to get the EDTA equivalent to gallium only. Precision and accuracy 0.2 to 0.4% was obtained in the results of gallium in the range of 8 to 2 mg. (author)

Accurate potentiometric determination of lipid membrane-water partition coefficients and apparent dissociation constants of ionizable drugs: electrostatic corrections.

Science.gov (United States)

Elsayed, Mustafa M A; Vierl, Ulrich; Cevc, Gregor

2009-06-01

Potentiometric lipid membrane-water partition coefficient studies neglect electrostatic interactions to date; this leads to incorrect results. We herein show how to account properly for such interactions in potentiometric data analysis. We conducted potentiometric titration experiments to determine lipid membrane-water partition coefficients of four illustrative drugs, bupivacaine, diclofenac, ketoprofen and terbinafine. We then analyzed the results conventionally and with an improved analytical approach that considers Coulombic electrostatic interactions. The new analytical approach delivers robust partition coefficient values. In contrast, the conventional data analysis yields apparent partition coefficients of the ionized drug forms that depend on experimental conditions (mainly the lipid-drug ratio and the bulk ionic strength). This is due to changing electrostatic effects originating either from bound drug and/or lipid charges. A membrane comprising 10 mol-% mono-charged molecules in a 150 mM (monovalent) electrolyte solution yields results that differ by a factor of 4 from uncharged membranes results. Allowance for the Coulombic electrostatic interactions is a prerequisite for accurate and reliable determination of lipid membrane-water partition coefficients of ionizable drugs from potentiometric titration data. The same conclusion applies to all analytical methods involving drug binding to a surface.

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

Science.gov (United States)

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.

Potentiometric study of rare earth complexing with trans-1,2-diaminocyclohexane-N,N'-dimalonic acid

International Nuclear Information System (INIS)

Smirnova, T.I.; Gorelov, I.P.

1980-01-01

Complexing of rare earths (Ln) and yttrium with trans-1,2-diaminocyclohexane-N, N'-dimalonic acid in aqueous solutions is studied using indirect potentiometric method with an aid of stationary mercury electrode and by the method of pH-potentiometric titration. It is shown that in the investigated solutions the LnL - and LnL 2 5- complexes are formed. At 25 deg C and ion force 0.1 stability constants of the complexes detected are determined [ru

Determination of the point-of-zero, charge of manganese oxides with different methods including an improved salt titration method

NARCIS (Netherlands)

Tan, W.F.; Lu, S.J.; Liu, F.; Feng, X.H.; He, J.Z.; Koopal, L.K.

2008-01-01

Manganese (Mn) oxides are important components in soils and sediments. Points-of-zero charge (PZC) of three synthetic Mn oxides (birnessite, cryptomelane, and todorokite) were determined by using three classical techniques (potentiometric titration or PT, rapid PT or R-PT, and salt titration or ST)

A Precise Method for Processing Data to Determine the Dissociation Constants of Polyhydroxy Carboxylic Acids via Potentiometric Titration.

Science.gov (United States)

Huang, Kaixuan; Xu, Yong; Lu, Wen; Yu, Shiyuan

2017-12-01

The thermodynamic dissociation constants of xylonic acid and gluconic acid were studied via potentiometric methods, and the results were verified using lactic acid, which has a known pKa value, as a model compound. Solutions of xylonic acid and gluconic acid were titrated with a standard solution of sodium hydroxide. The determined pKa data were processed via the method of derivative plots using computer software, and the accuracy was validated using the Gran method. The dissociation constants associated with the carboxylic acid group of xylonic and gluconic acids were determined to be pKa 1  = 3.56 ± 0.07 and pKa 1  = 3.74 ± 0.06, respectively. Further, the experimental data showed that the second deprotonation constants associated with a hydroxyl group of each of the two acids were pKa 2  = 8.58 ± 0.12 and pKa 2  = 7.06 ± 0.08, respectively. The deprotonation behavior of polyhydroxy carboxylic acids was altered using various ratios with Cu(II) to form complexes in solution, and this led to proposing a hypothesis for further study.

Determinação de ácido acéttico em amostra de vinagre adulterada com ácido clorídrico - um experimento integrado de titulação potenciométrica e condutométrica Determination of acetic acid in vinegar adulterated sample with cloridric acid - an experiment integrated of potentiometric and conductometric titrations

Directory of Open Access Journals (Sweden)

José Vinicius Martins

2010-01-01

Full Text Available The determination of acetic acid in vinegar adulterated sample using simultaneous potentiometric and condutometric titrations was used as an example of integrated experiment in instrumental analysis. An Excel® spreadsheet, which allows the entry of simultaneous data and the construction of the superimposed experimental curves (condutometric, potentiometric, first and second derivative potentiometric curve and, distribution diagrama of the acetic species as function of pH, was used as powerful tool to discuss the fundamental concepts involved in each technique and choose the best of them to quantify, without mutual interference, H3CCOOH and HCl in vinegar adulterated sample.

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

Science.gov (United States)

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

2017-01-01

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

The application of hydrogen-palladium electrode for potentiometric acid-base determinations in tetrahydrofuran

Directory of Open Access Journals (Sweden)

Jokić Anja B.

2013-01-01

Full Text Available The application of the hydrogen-palladium electrode (H2/Pd as the indicator electrode for the determination of relative acidity scale (Es, mV of tetrahydrofuran (THF and the potentiometric titrations of acids in this solvent was investigated. The relative acidity scale tetrahydrofuran was determined from the difference half-neutralization potentials of perchloric acid and tetrabutylammonium hydroxide (TBAH, which were measured by using both H2/Pd-SCE and glass-SCE electrode pairs. The experimentally obtained value of Es scale THF with a H2/Pd-SCE electrode pair was 1155 mV, and those obtained with glass-SCE electrode pair 880 mV. By using a H2/Pd indicator electrode, the individual acids (benzoic acid, palmitic acid, maleic acid, acetyl acetone, α-naphthol and two component acid mixtures (benzoic acid + α-naphthol, palmitic acid + α-naphthol, maleic acid + α-naphthol and maleic acid + ftalic acid were titrated with a standard solution of TBAH. In addition, sodium methylate and potassium hydroxide proved to be very suitable titrating agents for titrating of the individual acids and the acids in mixtures, respectively. The relative error of the determination of acids in mixture was less than 3%. The results are in agreement with those obtained by a conventional glass electrode. The advantages of H2/Pd electrode over a glass electrode in potentiometric acid-base determinations in tetrahydrofuran lie in the following: this electrode gives wider relative acidity scale THF, higher the potential jumps at the titration end-point and relatively fast response time; furthermore, it is very durable, simple to prepare and can be used in the titrations of small volumes. [Projekat Ministarstva nauke Republike Srbije, br.172051

Determination of lithium in organic matrix by potentiometric titration using fluoride ion selective electrode

International Nuclear Information System (INIS)

Govindan, R.; Alamelu, D.; Shah, Raju; Aggarwal, S.K.

2008-01-01

A method has been developed for the determination of lithium (Li) present in organic matrix containing hexa methylene tetramine (HMTA) and urea used in the sol-gel process for preparing lithium titanate microspheres, using fluoride ion selective electrode and potentiometric end point. Lithium is present in the wash solutions of the Sol-Gel process employed for the preparation of lithium titanate microspheres, proposed to be used in TBM (Test Blanket Module) of International Thermonuclear Experimental Reactor (ITER) project. Methods such as ICP-AES, AAS etc. used in aqueous solutions cannot be employed directly for lithium determination in organic matrix containing hexa methylene tetramine (HMTA), urea, NH 4 NO 3 , NH 4 Cl etc. A potentiometric method using a combination fluoride ion selective electrode for end point detection was developed and has been employed for lithium determination in the process streams from sol-gel process. The method is simple and rapid and an accuracy of about 0.5 % was achieved for the determination of Li in the range of 1 to 20 mg. The method is based on the complexation of Li by adding a known excess of NH 4 F solution, followed by potentiometric end point detection using fluoride ISE

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

Science.gov (United States)

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

2016-02-20

Potentiometric and spectrophotometric pH-titration of the multiprotic cytostatics bosutinib for dissociation constants determination were compared. Bosutinib treats patients with positive chronic myeloid leukemia. Bosutinib exhibits four protonatable sites in a pH range from 2 to 11, where two pK are well separated (ΔpK>3), while the other two are near dissociation constants. In the neutral medium, bosutinib occurs in the slightly water soluble form LH that can be protonated to the soluble cation LH4(3+). The molecule LH can be dissociated to still difficultly soluble anion L(-). The set of spectra upon pH from 2 to 11 in the 239.3-375.0nm was divided into two absorption bands: the first one from 239.3 to 290.5nm and the second from 312.3 to 375.0nm, which differ in sensitivity of chromophores to a pH change. Estimates of pK of the entire set of spectra were compared with those of both absorption bands. Due to limited solubility of bosutinib the protonation in a mixed aqueous-methanolic medium was studied. In low methanol content of 3-6% three dissociation constants can be reliably determined with SPECFIT/32 and SQUAD(84) and after extrapolation to zero content of methanol they lead to pKc1=3.43(12), pKc2=4.54(10), pKc3=7.56(07) and pKc4=11.04(05) at 25°C and pKc1=3.44(06), pKc2=5.03(08) pKc3=7.33(05) and pKc4=10.92(06) at 37°C. With an increasing content of methanol in solvent the dissociation of bosutinib is suppressed and the percentage of LH3(2+) decreases and LH prevails. From the potentiometric pH-titration at 25°C the concentration dissociation constants were estimated with ESAB pKc1=3.51(02), pKc2=4.37(02), pKc3=7.97(02) and pKc4=11.05(03) and with HYPERQUAD: pKc1=3.29(12), pKc2=4.24(10), pKc3=7.95(07) and pKc4=11.29(05). Copyright © 2015 Elsevier B.V. All rights reserved.

Potentiometric determination of trace amounts of volatile thiols in natural gas

International Nuclear Information System (INIS)

Farroha, S.M.; Habboush, A.E.; Kurthab, S.Y.

1986-01-01

A potentiometric titration method was developed for the determination of volatile thiols in natural gas. An apparatus was devised for the quantitative absorption of volatile thiols. The measurements were performed in an ethanolic ammonium buffer solution containing a known amount of silver nitrate as supporting electrolyte. The excess silver was precipitated by a known amount of potassium iodide. The excess of iodide was back titrated potentiometrically with a standard solution of silver nitrate. The direct titration of the excess silver ions with a standard solution of potassium iodide gave a poor accuracy compared with the back titration method. Iodide selective electrode was employed as an indicator electrode and a silver-silver chloride electrode as reference electrode. The accuracy and reproducibility of the method were established by preparing several synthetic samples in which ethanthiol containing from 346.61 to 12.11 μUg mercaptan sulfur was taken as standard nitrogen as carrier gas with an optimum flow rate of 31.5 L/hr. The results obtained expressed in the form of Grans plot showed an error ranging from 0.16 to 2.39% by weight and the relative standard deviation did not exceed 2.20%. The amount of mercaptan sulfur determined in Iraqi natural gas taken directly in a cylinder from Dora refinery, Baghdad, Iraq, and after six months of storage we 23.15 Ug/L and 21.25 Ug/L respectively with a relative standard deviation not exceeded 1%. The interferences of hydrogen sulfide could be eliminated by absorption in cadimium acetate containing solution. Other sulfur containing compounds e.g. disulfides, sulfoxides which may be present in natural gas do not interfere with the analysis

Determination of acid–base properties of HCl acid activated palygorskite by Potentiometrie titration

OpenAIRE

N. FriniSrasra; E.Srasra

2008-01-01

The surface acidity of raw and acid activated palygorskite clay were studied by acid-base potentiometric titration. The Gran plot method was applied for the hydroxide titration and the total surface site (Hs) and the average number of protons reacted per surface site (Z) of palygorskite samples at a given ionic strength were calculated. Acid treatment increases the clay acidity and modifies its surface charge. The point of zero charge value, determined by the common crossing point of Z vs pH ...

Linear titration plot for the determination of boron in the primary coolant of a pressurized water reactor

International Nuclear Information System (INIS)

Midgley, D.; Gatford, C.

1992-01-01

A linear titration plot method has been devised for the determination of boron as boric acid in partly neutralized solution, such as occurs in the primary coolant of pressurized water reactors. The total boron and the alkali in the sample are determined simultaneously. Although it is not essential to add mannitol in this method, it is more accurate when the solution is saturated with mannitol. Comparisons are made with other modes of titration: Gran plots, first and second differential potentiometric titrations and indicator titrations. None of these gives the total boron directly in partly neutralized solutions. (author)

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

International Nuclear Information System (INIS)

Kimuro, Shingo; Kirishima, Akira; Sato, Nobuaki

2015-01-01

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

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

Science.gov (United States)

2013-06-01

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

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

Science.gov (United States)

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

1995-03-01

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

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

International Nuclear Information System (INIS)

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

1982-01-01

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

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

Science.gov (United States)

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. 2010 Elsevier Inc. All rights reserved.

Complexometric consequent titration of bismuth-titanium mixtures in the μg-region

International Nuclear Information System (INIS)

Schaefer, H.

1975-01-01

A quantitative method is described for the determination of microquantities of bismuth and titanium. Both metals are determined complexometrically with EDTA and potentiometric equivalence point indication using a Cu-ion sensitive electrode in a consequent titration. The analysis is conducted as back-titration with standard Cu-solution. The relative error of the determination is 0.8% for bismuth (50-100 μg) and for titanium (10-30 μg) at 1.0%. Under the chosen conditions, it is possible to determine as little as 15 μg bismuth and 5 μg titanium by means of this procedure. (author)

[Comparison of different continuous positive airway pressure titration methods for obstructive sleep apnea hypopnea syndrome].

Science.gov (United States)

Li, Jingjing; Ye, Jingying; Zhang, Peng; Kang, Dan; Cao, Xin; Zhang, Yuhuan; Ding, Xiu; Zheng, Li; Li, Hongguang; Bian, Qiuli

2014-10-01

To explore whether there were differences between the results of automatic titration and the results of manual titration for positive airway pressure treatment in patients with obstructive sleep apnea hypopnea syndrome (OSAHS) and its influencing factors, the results might provide a theoretical basis for the rational use of two pressure titration methods. Sixty one patients with OSAHS were included in this study. All patients underwent a manual titration and an automatic titration within one week. The clinical informations, polysomnography data, and the results of both two titration of all patients were obtained for analysis. The overall apnea/hypopnea index was (63.1 ± 17.7)/h, with a range of 14.9/h to 110.4/h. The treatment pressure of manual titration was (8.4 ± 2.1) cmH(2)O, which was significantly lower than the treatment pressure of automatic titration, (11.5 ± 2.7) cmH(2)O (t = -9.797, P titration and manual titration), it was found that the pressure of automatic titration was significantly higher in patients with a ΔP > 3 cmH(2)O than in patients with a ΔP ≤ 3 cmH(2)O, which was (13.3 ± 2.3) cmH(2)O vs (10.0 ± 2.0) cmH(2)O (t = -6.159, P titration between these two groups, which was (8.6 ± 2.4) cmH(2)O vs (8.3 ± 2.0)cmH(2)O (P > 0.05). There was no significant difference in age, body mass index, neck circumference, abdomen circumference, apnea hypopnea index, and arterial oxygen saturation between these two groups. The treatment pressure of automatic titration is usually higher than that of manual titration. For patients with a high treatment pressure which is derived from automatic titration, a suggestion about manual titration could be given to decrease the potential treatment pressure of continuous positive airway pressure, which may be helpful in improving the comfortableness and the compliance of this treatment.

Potentiometric determination of sulfate with EDTA and the cupric-selective electrode

International Nuclear Information System (INIS)

Baumann, E.W.

1976-11-01

Sulfate was indirectly determined by precipitating sulfate as BaSO 4 and then dissolving BaSO 4 in excess ammoniacal EDTA. The excess EDTA was titrated potentiometrically with La 3+ . A cupric-selective electrode was used to detect the end point. About 10 -3 M SO 4 2- was determined in 3M HCl solutions of metal oxides with a relative standard deviation of 3.5 percent and a bias of +4 percent

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

Science.gov (United States)

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

2006-12-19

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

Automated back titration method to measure phosphate

International Nuclear Information System (INIS)

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

1987-01-01

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

Thermometric titrations of amines with nitrosyl perchlorate in acetonitrile solvent.

Science.gov (United States)

Gündüz, T; Kiliç, E; Cakirer, O

1996-05-01

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

A new potentiometric determination of hydrazine in the presence of uranium(IV)

International Nuclear Information System (INIS)

Singh, N.S.; Mohan, S.V.

1996-01-01

The present method describes the determination of hydrazine by making use of potentiometric titration technique. The underlying principle is back titration of unreacted excess cerium remaining after the complete oxidation of hydrazine. Standardized ferrous ammonium sulfate was used for titration. This method was applied to 'real samples' generated from a nuclear reprocessing plant wherein control of hydrazine is of paramount importance. The interference of U(IV), Cr(III), U(VI), nitrite, and chloride was studied and of all these ions the way to eliminate the interference of U(IV) was only attempted. The relative standard deviations (RSD) for synthetic as well as 'real samples' were determined. The method gives RSD of less than 1% in the range of 1 mg to 20 mg of hydrazine. The error in the range 3 mg to 17 mg was found to be less than 1%. (author). 5 refs., 3 tabs

pH-metric solubility. 2: correlation between the acid-base titration and the saturation shake-flask solubility-pH methods.

Science.gov (United States)

Avdeef, A; Berger, C M; Brownell, C

2000-01-01

The objective of this study was to compare the results of a normal saturation shake-flask method to a new potentiometric acid-base titration method for determining the intrinsic solubility and the solubility-pH profiles of ionizable molecules, and to report the solubility constants determined by the latter technique. The solubility-pH profiles of twelve generic drugs (atenolol, diclofenac.Na, famotidine, flurbiprofen, furosemide, hydrochlorothiazide, ibuprofen, ketoprofen, labetolol.HCl, naproxen, phenytoin, and propranolol.HCl), with solubilities spanning over six orders of magnitude, were determined both by the new pH-metric method and by a traditional approach (24 hr shaking of saturated solutions, followed by filtration, then HPLC assaying with UV detection). The 212 separate saturation shake-flask solubility measurements and those derived from 65 potentiometric titrations agreed well. The analysis produced the correlation equation: log(1/S)titration = -0.063(+/- 0.032) + 1.025(+/- 0.011) log(1/S)shake-flask, s = 0.20, r2 = 0.978. The potentiometrically-derived intrinsic solubilities of the drugs were: atenolol 13.5 mg/mL, diclofenac.Na 0.82 microg/mL, famotidine 1.1 mg/ mL, flurbiprofen 10.6 microg/mL, furosemide 5.9 microg/mL, hydrochlorothiazide 0.70 mg/mL, ibuprofen 49 microg/mL, ketoprofen 118 microg/mL, labetolol.HCl 128 microg/mL, naproxen 14 microg/mL, phenytoin 19 microg/mL, and propranolol.HCl 70 microg/mL. The new potentiometric method was shown to be reliable for determining the solubility-pH profiles of uncharged ionizable drug substances. Its speed compared to conventional equilibrium measurements, its sound theoretical basis, its ability to generate the full solubility-pH profile from a single titration, and its dynamic range (currently estimated to be seven orders of magnitude) make the new pH-metric method an attractive addition to traditional approaches used by preformulation and development scientists. It may be useful even to discovery

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

Science.gov (United States)

Kozak, Joanna; Wójtowicz, Marzena; Gawenda, Nadzieja; Kościelniak, Paweł

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. Copyright © 2011 Elsevier B.V. All rights reserved.

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

Science.gov (United States)

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

2007-09-01

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

Control of OSA during automatic positive airway pressure titration in a clinical case series: predictors and accuracy of device download data.

Science.gov (United States)

Huang, Hsin-Chia Carol; Hillman, David R; McArdle, Nigel

2012-09-01

To investigate the factors associated with physiologic control of obstructive sleep apnea (OSA) during automatic positive airway pressure (APAP) titration in a clinical series. To also assess the usefulness of apnea-hypopnea index (AHI) data downloaded from the APAP device (Dev AHI). Retrospective review of a consecutive series of patients with OSA who underwent APAP titration (Autoset Spirit, ResMed, Bella Vista, New South Wales, Australia ) with simultaneous polysomnographic (PSG) monitoring in the sleep laboratory. Tertiary sleep clinic. There were 190 consecutive patients with OSA referred for APAP titration. There were 58% of patients who achieved optimal or good control of OSA (titration PSG AHI titration. The independent predictors of titration PSG AHI were a history of cardiac disease and elevated central apnea and arousal indices during the diagnostic study. Although the median and interquartile range (IQR) AHI from the device (7.0, 3.9-11.6 events/hr) was only slightly less than the PSG AHI (7.8, 3.9-14.4 events/hr, P = 0.04) during titration, case-by-case agreement between the two measures was poor (chi-square titration is often poor, and close clinical follow-up is particularly needed in patients with a history of cardiac disease or with high arousal or central apnea indices on the diagnostic study. Device AHI does not reliably assess control during APAP titration, and PSG assessment may be required if clinical response to treatment is poor. The findings relate to the ResMed AutoSet device and may not apply to other devices.

Potentiometric studies on the complexes of tetracycline (TC) and oxytetracycline (OTC) with some metal ions. Potentiometrische Untersuchungen der Komplexe von Tetracyclin (TC) und Oxytetracyclin (OTC) mit einigen Metall-Ionen

Energy Technology Data Exchange (ETDEWEB)

Ghandour, M A; Azab, H A; Hassan, A; Ali, A M [Assiut Univ. (Egypt)

1992-01-01

The interaction of Cr(III), Mn(II), Fe(III), Co(II), Ni(II), Zn(II), Cd(II), Hg(II), Pb(II), Al(III), and UO[sub 2](II) ions with tetracycline (TC) were studied by potentiometric pH titrations. The formation constants of the different binary complexes formed in such systems have been determined at 25[+-]0.1 deg C and [mu]=0.1 moll[sup -1] (NaNO[sub 3]). Potentiometric pH equilibrium measurements have been made under the same conditions for the interaction of oxytetracycline (OTC) and Cu(II), Cd(II), Pb(II), and UO[sub 2](II). The formation of (1:1) binary complexes are inferred from the potentiometric pH titration curves. The protonation constants of TC and OTC were also determined under the same conditions and refined (ESAB2M computer program). The transition metal stability constants are consistent with the Irving-Williams series. (authors).

Redox behaviour of molybdenum in aqueous medium : a potentiometric study

International Nuclear Information System (INIS)

Sagi, S.R.; Mohan Rao, P.R.

1975-01-01

The nature of the two forms; of Mo(III) cationic-aquomolybdenum(III) (green) and anionic-chloromolybdate(III) (orange-red) has been investigated using various oxidants in hydrochloric acid mdeium, the oxidation steps being detected using a potentiometric method. The two species behave differently towards the various oxidants. The green form is a better reducing agent giving large breaks in potentials during redox titrations. The existence of the intermediate oxidation states Mosup(3.5) and Mosup(4.5) reported earlier has also been confirmed. (author)

Potentiometric study of Nd3+ chelates of substituted salicylhydroxamic acids

International Nuclear Information System (INIS)

Deshpande, R.G.; Jahagirdar, D.V.

1976-01-01

The interaction of Nd 3+ ion with salicylhydroxamic acid and 5-methyl, 5-chloro, 5-bromo, 5-nitro, 4-chloro, 4-bromo and 3-chloro salicylhydroxamic acids is investigated potentiometrically by Calvin-Bjerrum titration technique at 30 0 +- 0.1 0 and ionic strength μ=0.1 M(NaClO 4 ) in 50% v/v dioxane-water mixtures. Nd 3+ forms only 1:1 chelates with these ligands. The validity of the log K= apk + b relationship is examined for these chelates. (author)

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

Science.gov (United States)

Kiba, N; Takeuchi, T

1973-09-01

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

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

Science.gov (United States)

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

2011-07-15

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

Potentiometric determination of uranium in simulated Purex Process solutions by acidiometry

International Nuclear Information System (INIS)

Cohen, V.H.; Matsuda, H.T.; Araujo, B.F. de; Araujo, J.A. de

1983-01-01

A potentiometric methods for sequential free acidity and uranium determination in simulated Purex Process solutions is described. An oxalate solution or a mixture of fluoride-oxalate pellets were used as complexing agent for free titration. Following this first equivalent point, uranium is determined-by indirect titration of H + liberated in the peruanate reaction. Some elements present in the standard fuel elements with a burn-up of 33.000 Mwd/t, neutron flux of 3,2 x 10 13 n.cm -2 .s -1 and cooling time of two years were considered as interfering elements in uranium analyses. As a substitute of Pu-IV, Th(NO 3 ) 4 solution was used. The method can be applied to aqueous and organic (TBP/diluent) solutions with 2% precision and 2% accuracy. (Autor) [pt

Sequential potentiometric determination of uranium and plutonium in a single aliquot

International Nuclear Information System (INIS)

Rao, V.K.; Charyulu, M.M.; Natarajan, P.R.

1983-01-01

A method is reported for sequential potentiometric determination of uranium and plutonium present is an aliquot. Plutonium is first determined by oxidizing it to the hexavalent state with perchloric acid followed by iron(II) reduction and titration of excess ferrous iron with chromium(VI). Uranium is subsequently determined by reduction to the quadrivalent state using titanium(III) and titration with vanadium(V). The interference of plutonium and iron(II) is eliminated by the addition of a mixture containing sulfamic acid, nitric acid, and molybdenum(VI). The results of the analysis of mixture containing 3-5 mg quantities of uranium and plutonium are reliable with errors less than 0.3% and 0.2%, respectively. The application of the method for the analysis of mixtures containing various amounts of uranium and plutonium has been examined. (author)

Potentiometric determination of uranium in simulated Purex Process solutions by acidiometry

Energy Technology Data Exchange (ETDEWEB)

Cohen, V H; Matsuda, H T; Araujo, B.F. de; Araujo, J.A. de

1984-01-01

A potentiometric methods for sequential free acidity and uranium determination in simulated Purex Process solutions is described. An oxalate solution or a mixture of fluoride-oxalate pellets were used as complexing agent for free titration. Following this first equivalent point, uranium is determined-by indirect titration of H/sup +/ liberated in the peruanate reaction. Some elements present in the standard fuel elements with a burn-up of 33.000 Mwd/t, neutron flux of 3,2 x 10/sup 13/n.cm/sup -2/.s/sup -1/ and cooling time of two years were considered as interfering elements in uranium analyses. As a substitute of Pu-IV, Th(NO/sub 3/)/sub 4/ solution was used. The method can be applied to aqueous and organic (TBP/diluent) solutions with 2% precision and 2% accuracy. (Autor).

Stability constants of some Y(III)-complexes from potentiometric data

Energy Technology Data Exchange (ETDEWEB)

Pande, S P; Munshi, K N [Nagpur Univ. (India). Dept. of Chemistry

1975-06-01

Potentiometric studies have been carried out on the metal complexes of yttrium(III) with 5-sulphosalicylic acid 3,5-dinitro salicylic acid sodium 2,3-dihydroxynaphthalene-6-sulfonate, and nitroso-R-salt. The Calvin-Bjerrum pH-titration technique, as used by Iriving and Rossotti, has been applied to determine the stepwise protonation constants of the ligands and the formation constants of the complexes. The log K values have been computed by alternative methods, at three different temperatures at an ionic strength of 0.2M(NaClO/sub 4/).(author).

Experiments for quick and accurate thorium assay by means of potentiometric end point determination

International Nuclear Information System (INIS)

Mainka, E.; Coerdt, W.

1978-10-01

Two methods are described which allow quick thorium assay easily to be automated. In the potentiometric titration with NaF the ion sensitive fluoride electrode is used as the indicator. The analysis can be performed for pH values 3 to 4. Th(OH) 4 precipitation must be avoided although the acidity of the solution must not be too high since otherwise erroneous measurements will be obtained. In the complexometric thorium assay EDTA is used for titration and the indicator is the copper sensitive electrode. This method offers the advantage that the analysis can be performed in the presence of large amounts of uranium, which is excluded under the NaF method. (orig.) [de

Stuides on a Pb2+-selective electrode with a macrocyclic liquid membrane. Potentiometric determination of Pb2+ ions

Directory of Open Access Journals (Sweden)

MARIAN ISVORANU

2006-12-01

Full Text Available This paper presents experimental and theoretical data regarding the design, characterization and analytical applications of a non-expensive, liquid-membrane ion-selective electrode for Pb2+ ions. The membrane is a solution of the active complex formed by Pb2+ ions with dibenzo-18-crown-6-ionophore (DB-[18]-C-6 extracted in propylene carbonate (PC. The sucessful application of the developed electrode for the determination of Pb2+ ions in aqueos solution samples by direct potentiometry and potentiometric titration is presented. For the presented analytical results, there are insignificant systematic errors between the direct potentiometric method with the developed ion-selective electrode and atomic absorption spectrometry.

Potentiometric determination of the 'formal' hydrolysis ratio of aluminium species in aqueous solutions

International Nuclear Information System (INIS)

Fournier, Agathe C.; Shafran, Kirill L.; Perry, Carole C.

2008-01-01

The 'formal' hydrolysis ratio (h = C(OH - ) added /C(Al) total ) of hydrolysed aluminium-ions is an important parameter required for the exhaustive and quantitative speciation-fractionation of aluminium in aqueous solutions. This paper describes a potentiometric method for determination of the formal hydrolysis ratio based on an automated alkaline titration procedure. The method uses the point of precipitation of aluminium hydroxide as a reference (h = 3.0) in order to calculate the initial formal hydrolysis ratio of hydrolysed aluminium-ion solutions. Several solutions of pure hydrolytic species including aluminium monomers (AlCl 3 ), Al 13 polynuclear cluster ([Al 13 O 4 (OH) 24 (H 2 O) 12 ] 7+ ), Al 30 polynuclear cluster ([Al 30 O 8 (OH) 56 (H 2 O) 26 ] 18+ ) and a suspension of nanoparticulate aluminium hydroxide have been used as 'reference standards' to validate the proposed potentiometric method. Other important variables in the potentiometric determination of the hydrolysis ratio have also been optimised including the concentration of aluminium and the type and strength of alkali (Trizma-base, NH 3 , NaHCO 3 , Na 2 CO 3 and KOH). The results of the potentiometric analysis have been cross-verified by quantitative 27 Al solution nuclear magnetic resonance ( 27 Al NMR) measurements. The 'formal' hydrolysis ratio of a commercial basic aluminium chloride has been measured as an example of a practical application of the developed technique

A potentiometric study of (acid+base) equilibria in substituted 4-nitropyridine N-oxide systems in methanol and dimethyl sulfoxide

International Nuclear Information System (INIS)

Gurzynski, Lukasz; Puszko, Aniela; Makowski, Mariusz; Chmurzynski, Lech

2007-01-01

The acid dissociation constants for cationic acids conjugated with 4-nitropyridine N-oxides have been determined using potentiometric titration method. The measurements in the systems of thirteen 4-nitropyridine N-oxide derivatives were carried out in the polar amphiprotic methanol (MeOH) and in the aprotic protophilic dimethyl sulfoxide (DMSO). Likewise as in the polar aprotic protophobic solvents (acetonitrile, acetone) it was found that in MeOH for all N-oxides studied the pK a values were readily determinable, whereas in DMSO the pK a values were hardly determinable or indeterminable by using the potentiometric method. In addition, just like in our previous investigations it was revealed that the sequence of the pK a values of the cationic acids in methanol is the same as in the water and the values are lower than those determined in acetonitrile and acetone. Also, it was found that the phenomenon of cationic homoconjugation equilibria was not present in the systems involving 4-nitropyridine N-oxide derivatives in both solvents used. Furthermore, protonation energies, ΔE prot , and Gibbs free enthalpies, ΔG prot , in vacuo have been compared with acid dissociation constants (expressed as pK a MeOH values) of the protonated N-oxides determined by potentiometric titration in methanol to establish a correlation between these magnitudes

A potentiometric study of (acid+base) equilibria in substituted 4-nitropyridine N-oxide systems in methanol and dimethyl sulfoxide

Energy Technology Data Exchange (ETDEWEB)

Gurzynski, Lukasz [Department of General Chemistry, University of Gdansk, Sobieskiego 18, 80-952 Gdansk (Poland); Puszko, Aniela [Department of Organic Chemistry, School of Economics, Wroclaw (Poland); Makowski, Mariusz [Department of General Chemistry, University of Gdansk, Sobieskiego 18, 80-952 Gdansk (Poland); Chmurzynski, Lech [Department of General Chemistry, University of Gdansk, Sobieskiego 18, 80-952 Gdansk (Poland)]. E-mail: lech@chemik.chem.univ.gda.pl

2007-02-15

The acid dissociation constants for cationic acids conjugated with 4-nitropyridine N-oxides have been determined using potentiometric titration method. The measurements in the systems of thirteen 4-nitropyridine N-oxide derivatives were carried out in the polar amphiprotic methanol (MeOH) and in the aprotic protophilic dimethyl sulfoxide (DMSO). Likewise as in the polar aprotic protophobic solvents (acetonitrile, acetone) it was found that in MeOH for all N-oxides studied the pK{sub a} values were readily determinable, whereas in DMSO the pK{sub a} values were hardly determinable or indeterminable by using the potentiometric method. In addition, just like in our previous investigations it was revealed that the sequence of the pK{sub a} values of the cationic acids in methanol is the same as in the water and the values are lower than those determined in acetonitrile and acetone. Also, it was found that the phenomenon of cationic homoconjugation equilibria was not present in the systems involving 4-nitropyridine N-oxide derivatives in both solvents used. Furthermore, protonation energies, {delta}E{sub prot}, and Gibbs free enthalpies, {delta}G{sub prot}, in vacuo have been compared with acid dissociation constants (expressed as pK{sub a}{sup MeOH} values) of the protonated N-oxides determined by potentiometric titration in methanol to establish a correlation between these magnitudes.

Label-free and substrate-free potentiometric aptasensing using polycation-sensitive membrane electrodes.

Science.gov (United States)

Ding, Jiawang; Chen, Yan; Wang, Xuewei; Qin, Wei

2012-02-21

A potentiometric label-free and substrate-free (LFSF) aptasensing strategy which eliminates the labeling, separation, and immobilization steps is described in this paper. An aptamer binds specifically to a target molecule via reaction incubation, which could induce a change in the aptamer conformation from a random coil-like configuration to a rigid folded structure. Such a target binding-induced aptamer conformational change effectively prevents the aptamer from electrostatically interacting with the protamine binding domain. This could either shift the response curve for the potentiometric titration of the aptamer with protamine as monitored by a conventional polycation-sensitive membrane electrode or change the current-dependent potential detected by a protamine-conditioned polycation-sensitive electrode with the pulsed current-driven ion fluxes of protamine across the polymeric membrane. Using adenosine triphosphate (ATP) as a model analyte, the proposed concept offers potentiometric detection of ATP down to the submicromolar concentration range and has been applied to the determination of ATP in HeLa cells. In contrast to the current LFSF aptasensors based on optical detection, the proposed strategy allows the LFSF biosensing of aptamer/target binding events in a homogeneous solution via electrochemical transduction. It is anticipated that the proposed strategy will lay a foundation for development of potentiometric sensors for LFSF aptasensing of a variety of analytes where target binding-induced conformational changes such as the formation of folded structures and the opening of DNA hairpin loops are involved.

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

Science.gov (United States)

Zarzycki, Piotr; Thomas, Fabien

2006-10-15

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

The Davies-Gray titration for the assay of uranium in nuclear materials: a performance study

International Nuclear Information System (INIS)

Bickel, M.

1997-01-01

An interlaboratory comparison in two phases was organized to assess the precision and accuracy concerning the assay of uranium in nuclear materials by the potentiometric titration method. This contribution presents the results of this exercise in terms of method performance. Variations to be expected between different laboratories and within a single laboratory are estimated. In general, the method proved again very reliable. (orig.)

Determination of free acid in plutonium (IV) solutions - thermometrically, potentiometrically

International Nuclear Information System (INIS)

Williams, T.L.; Tucker, G.M.; Huff, G.A.; Jordan, L.G.

1981-09-01

The thermometric titration technique was found to offer certain advantages over potentiometry in the determination of free acid in Pu(IV) solutions. The thermometric technique was applied to the determination of free acid in plutonium nitrate solutions using potassium fluoride to suppress the hydrolytic interference of plutonium(IV). The results indicate that 0.2 to 2.0 milliequivalents of free acid can be determined with acceptable bias and precision in solutions containing up to 30 milligrams of plutonium. In contrast, neither the thermometric nor the potentiometric technique was suitable for samples containing more than eight milligrams of plutonium complexed with potassium oxalate

Development and validation of an alternative titration method for the determination of sulfate ion in indinavir sulfate

Directory of Open Access Journals (Sweden)

Breno de Carvalho e Silva

2005-02-01

Full Text Available A simple and rapid precipitation titration method was developed and validated to determine sulfate ion content in indinavir sulfate raw material. 0.1 mol L-1 lead nitrate volumetric solution was used as titrant employing potentiometric endpoint determination using a lead-specific electrode. The United States Pharmacopoeia Forum indicates a potentiometric method for sulfate ion quantitation using 0.1 mol L-1 lead perchlorate as titrant. Both methods were validated concerning linearity, precision and accuracy, yielding good results. The sulfate ion content found by the two validated methods was compared by the statistical t-student test, indicating that there was no statistically significant difference between the methods.

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

Science.gov (United States)

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

2003-07-01

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

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

Science.gov (United States)

Avdeef, A; Berger, C M

2001-12-01

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

pH Sensitivity of Si-C Linked Organic Monolayers on Crystalline Silicon Surfaces: Titration Experiments, Mott Schottky Analysis and Site-Binding Modeling

NARCIS (Netherlands)

Faber, E.J.; Sparreboom, W.; Groeneveld, W.; Smet, de L.C.P.M.; Bomer, J.; Olthuis, W.; Zuilhof, H.; Sudhölter, E.J.R.; Bergveld, P.; Berg, van den A.

2007-01-01

The electrochemical behavior of SiC linked organic monolayers is studied in electrolyte-insulator-Si devices, under conditions normally encountered in potentiometric biosensors, to gain fundamental knowledge on the behavior of such Si electrodes under practical conditions. This is done via titration

The use of kragten spreadsheets for uncertainty evaluation of uranium potentiometric analysis by the Brazilian Safeguards Laboratory

International Nuclear Information System (INIS)

Silva, Jose Wanderley S. da; Barros, Pedro Dionisio de; Araujo, Radier Mario S. de

2009-01-01

In safeguards, independent analysis of uranium content and enrichment of nuclear materials to verify operator's declarations is an important tool to evaluate the accountability system applied by nuclear installations. This determination may be performed by nondestructive (NDA) methods, generally done in the field using portable radiation detection systems, or destructive (DA) methods by chemical analysis when more accurate and precise results are necessary. Samples for DA analysis are collected by inspectors during safeguards inspections and sent to Safeguards Laboratory (LASAL) of the Brazilian Nuclear Energy Commission - (CNEN), where the analysis take place. The method used by LASAL for determination of uranium in different physical and chemical forms is the Davies and Gray/NBL using an automatic potentiometric titrator, which performs the titration of uranium IV by a standard solution of K 2 Cr 2 O 7 . Uncertainty budgets have been determined based on the concepts of the ISO 'Guide to the Expression of Uncertainty in Measurement' (GUM). In order to simplify the calculation of the uncertainty, a computational tool named Kragten Spreadsheet was used. Such spreadsheet uses the concepts established by the GUM and provides results that numerically approximates to those obtained by propagation of uncertainty with analytically determined sensitivity coefficients. The main parameters (input quantities) interfering on the uncertainty were studied. In order to evaluate their contribution in the final uncertainty, the uncertainties of all steps of the analytical method were estimated and compiled. (author)

Catalytic thermometric titrations in non-aqueous solvents by coulometrically generated titrant.

Science.gov (United States)

Vajgand, V J; Gaál, F F; Brusin, S S

1970-05-01

Catalytic thermometric titrations have been developed for tertiary amines and salts of organic acids in acetic and propionic anhydride with titrant coulometrically generated at a mercury and/or platinum anode, hydroquinone being added to the solution titrated if the platinum anode is used. The results obtained are compared with those obtained by coulometric titration with the end-point detected either photometrically or potentiometrically. On a élaboré des titrages thermométriques catalytiques pour les amines tertiaires et les sels d'acides organiques en anhydrides aétique et propionique avec l'agent de titrage engendré coulométriquement sur une anode de mercure et/ou platine, de l'hydroquinone étant ajoutée à la solution titrée si l'on emploie l'anode de platine. Les résultats obtenus sont comparés avec ceux obtenus par titrage coulométrique avec le point de fin de réaction détecté soit photométriquement soit potentioétriquement.

On-Board Monitoring of Engine Oil

Science.gov (United States)

2011-04-01

methods involve potentiometric and colorimetric titrations , respectively. For both tests, a titration solvent is prepared and added to the oil. The...ASTM D 2896 and ASTM D 4739 [17]. Both methods involve potentiometric titrations . ASTM D 2896 uses a stronger acid and more polar solvent than ASTM D...Petroleum Products by Potentiometric Titration ASTM D 4739 Standard Test Method for Base Number Determination by Potentiometric Titration Gas

A microcomputer-controlled system for titration analysis

NARCIS (Netherlands)

Boelema, Gerrit Jan

1982-01-01

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

Combinatorial screening of potentiometric Pb(II) sensors from polysulfoaminoanthraquinone solid ionophore.

Science.gov (United States)

Huang, Mei-Rong; Ding, Yong-Bo; Li, Xin-Gui

2014-03-10

A potentiometric Pb(II)-selective sensor was fabricated by a combinatorial screening of electrically conducting polysulfoaminoanthraquinone (PSA) nanoparticles as a solid ionophore, ion exchangers (oleic acid (OA) and NaTPB), plasticizers in a polyvinyl chloride (PVC) matrix, membrane thickness, inner filling ion species, and concentration. The membrane sensor with the composition of PSA/PVC/DOP (dioctyl phthalate)/OA (1.0:33:61:5.0) exhibited the best performance, including a slope of 29.3 mV decade(-1) in the concentration range 10(-6.3)-10(-1.6) M, detection limit of 1.6 × 10(-7) M, response time of 16 s, lifetime of five months, and good response reversibility. The proposed sensor has demonstrated good selectivity for Pb(II) over other monovalent, divalent and trivalent interfering ions, and could be used in a pH range of 3.62-5.22. The Pb(II) sensor has been successfully applied for the determination of Pb(II) concentration in real-world samples and also as an indicator electrode for potentiometric titration of lead ions.

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.

Science.gov (United States)

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

2010-01-05

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.

Desulfurization of Hydrocarbon Fuels at Ambient Conditions Using Supported Silver Oxide-Titania Sorbents

Science.gov (United States)

2010-12-13

Potentiometric titration ------------------------------------------------------------------ 27 II.10 Equilibrium isotherms...chemisorption ------------------------------------------------ 104 VI.1.5 Potentiometric titration ...Figure VI.7. The relationship between bronsted surface acidity measured by potentiometric titration and sulfur adsorption capacity using JP5 fuel (1172

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

Science.gov (United States)

Ivaska, A

1974-06-01

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

Potentiometric and ab initio studies of acid-base interactions of substituted 4-halo(Cl, Br)pyridine N-oxide systems

International Nuclear Information System (INIS)

Gurzynski, Lukasz; Puszko, Aniela; Makowski, Mariusz; Makowska, Joanna; Chmurzynski, Lech

2006-01-01

By using the potentiometric method, acidity constants have been determined in systems of tri- and tetra-substituted pyridine N-oxides. The potentiometric measurements in systems of four 4-chloropyridine N-oxide derivatives containing the chlorine atom at position 4 to the NO 2 group and four bromine counterparts were carried out in polar non-aqueous solvents, viz. amphiprotic methanol (MeOH) and aprotic protophilic dimethyl sulfoxide (DMSO). It was found that in all the systems studied the pK a values were readily determinable (as indicated by small standard deviations) in MeOH, whereas in DMSO large standard deviations were obtained making the pK a values either hardly determinable or indeterminable from potentiometric measurements. Furthermore, it was demonstrated that the acidity constants of protonated N-oxides studied in MeOH changed according to the sequence of their acidity constants in water. It was also found that in the polar solvents studied, i.e. in the amphiprotic methanol and the highly basic aprotic dimethyl sulfoxide, the cationic homo-conjugation equlibrium constants could not be determined using potentiometric method. Also, by using ab initio methods at the RHF and MP2 levels and the PCM model, utilizing the Gaussian 6-31++G** basis set, energies and Gibbs free energies of the protonation reactions of the N-oxides have been determined. The energy parameters have been compared with acidity constants of the protonated N-oxides determined by potentiometric titration in methanol to establish a correlation between these approaches

Potentiometric Determination of Phytic Acid and Investigations of Phytate Interactions with Some Metal Ions.

Science.gov (United States)

Marolt, Gregor; Pihlar, Boris

2015-01-01

Determination of correct amount (concentration) of phytic acid is of vital importance when dealing with protonation and/or metal complexation equilibria. A novel approach for precise and reliable assay of phytic acid, based on the difference between end points by potentiometric titration, has been presented. Twelve phytic acid protons are classified into three groups of acidity, which enables detection of 2 to 3 distinct equivalent points (EPs) depending on experimental conditions, e.g. counter-ion concentration. Using the differences between individual EPs enables correct phytate determination as well as identification of potential contamination and/or determination of initial protonation degree. Impact of uncertainty of phytate amount on the calculation of protonation constants has been evaluated using computer simulation program (Hyperquad2013). With the analysis of titration curves different binding sites on phytate ligand have been proposed for complexation of Ca2+ and Fe3+ ions.

Potentiometric and Conductometric Study of Aqueous Solutions of Lithium and Sodium Salts of Poly(thiophen-3-ylacetic acid).

Science.gov (United States)

Hostnik, Gregor; Vlachy, Vojko; Bondarev, Dmitrij; Jiří, Vohlídal; Cerar, Janez

2012-09-01

The title polymer, PTAA, practically free of ester groups was obtained by oxidative polymerization of methyl thiophen-3-ylacetate and subsequent basic hydrolysis of primary polymer. Poly(thiophen-3-ylacetic acid) has been thoroughly characterized by NMR, IR, Raman, and UV/Vis spectroscopy. The polyacid behavior during neutralization titrations with lithium and sodium hydroxides, carried out under nitrogen atmosphere, has been studied by conductometry and potentiometry. Henderson-Hasselbach plots of potentiometric titration curves show a break point at pH around 6, where the curve slope drops from 1.8 (at lower pH) to a value from 1.05 to 1.3 (at higher pH values). The UV/Vis spectra monitored during back titration show: (i) monotonous decrease of both λmax and εmax as pH decreases, (ii) the presence of the isosbestic point at 401 nm that can be ascribed to conformational transition of PTAA chains, and (iii) absence of the isosbestic point at 392 nm reported previously by other authors.

Potentiometric study of cadmium (2) complexing with chloride-ions in aqueous solutions of Mg(ClO/sub 4/, Cl)/sub 2/

Energy Technology Data Exchange (ETDEWEB)

Prokuev, V A; Belousov, E A

1985-05-01

By the method of potentiometric titration using cadmium amalgam electrode at ionic forces 1.0; 2.0; 3.0; 4.5; 6.0; 7.5 and 9.0 of (Mg(ClO/sub 4/)/sub 2/ general constants of cadmium chloride compleses stability are determined. By the Vasiliev extrapolation equation thermodynamic constants of CdClsub(n)sup(2-n) ion formation, where n=1-3 are evaluated.

Modern Directions for Potentiometric Sensors

Science.gov (United States)

Bakker, Eric; Chumbimuni-Torres, Karin

2009-01-01

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

Titulador potenciométrico automatizado baseado em sistema de fluxo monossegmentado Automated potentiometric titrator based in monosegmented flow system

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Edgard Moreira Ganzarolli

1999-02-01

Full Text Available A new automated system for acid-base flow titrations is proposed. In the operation mode, several sample to titrant volumetric ratios are injected in an air segmented plug. Five three way solenoid valves and three acrilic junctions, assembled in a hidrodynamic injection system, were accountable for the monosegmented reagents plug formation. A turbulent flow reactor was used for a perfect mix of reagents in the plug. The detector system employed a glass combined electrode fitted in an acrilic holder. Titrations of hydrochloric, nitric and acetic acids, in several concentrations, were performed with standard sodium hidroxide, for evaluation of the efficiency of the system. The relative standard deviation of the determinations was about ±0,5% and each titration was carried out in 3-4 minutes. A Quick BASIC 4.5® program was developed for the titrator control.

Potentiometric and ab initio studies of acid-base interactions of substituted 4-halo(Cl, Br)pyridine N-oxide systems

Energy Technology Data Exchange (ETDEWEB)

Gurzynski, Lukasz [Department of General Chemistry, University of Gdansk, Sobieskiego 18, 80-952 Gdansk (Poland); Puszko, Aniela [Department of Organic Chemistry, School of Economics, Wroclaw (Poland); Makowski, Mariusz [Department of General Chemistry, University of Gdansk, Sobieskiego 18, 80-952 Gdansk (Poland); Makowska, Joanna [Department of General Chemistry, University of Gdansk, Sobieskiego 18, 80-952 Gdansk (Poland); Chmurzynski, Lech [Department of General Chemistry, University of Gdansk, Sobieskiego 18, 80-952 Gdansk (Poland)]. E-mail: lech@chem.univ.gda.pl

2006-12-15

By using the potentiometric method, acidity constants have been determined in systems of tri- and tetra-substituted pyridine N-oxides. The potentiometric measurements in systems of four 4-chloropyridine N-oxide derivatives containing the chlorine atom at position 4 to the NO{sub 2} group and four bromine counterparts were carried out in polar non-aqueous solvents, viz. amphiprotic methanol (MeOH) and aprotic protophilic dimethyl sulfoxide (DMSO). It was found that in all the systems studied the pK {sub a} values were readily determinable (as indicated by small standard deviations) in MeOH, whereas in DMSO large standard deviations were obtained making the pK {sub a} values either hardly determinable or indeterminable from potentiometric measurements. Furthermore, it was demonstrated that the acidity constants of protonated N-oxides studied in MeOH changed according to the sequence of their acidity constants in water. It was also found that in the polar solvents studied, i.e. in the amphiprotic methanol and the highly basic aprotic dimethyl sulfoxide, the cationic homo-conjugation equlibrium constants could not be determined using potentiometric method. Also, by using ab initio methods at the RHF and MP2 levels and the PCM model, utilizing the Gaussian 6-31++G** basis set, energies and Gibbs free energies of the protonation reactions of the N-oxides have been determined. The energy parameters have been compared with acidity constants of the protonated N-oxides determined by potentiometric titration in methanol to establish a correlation between these approaches.

Coulometric-potentiometric determination of autoprotolysis constant and relative acidity scale of water

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Džudović Radmila M.

2010-01-01

Full Text Available The autoprotolysis constant and relative acidity scale of water were determined by applying the coulometric-potentiometric method and a hydrogen/palladium (H2/Pd generator anode. In the described procedure for the evaluation of autoprotolysis constant, a strong base generated coulometrically at the platinum cathode in situ in the electrolytic cell, in presence of sodium perchlorate as the supporting electrolyte, is titrated with hydrogen ions obtained by the anodic oxidation of hydrogen dissolved in palladium electrode. The titration was carried out with a glass-SCE electrode pair at 25.0±0.1°C. The value obtained pKw = 13.91 ± 0.06 is in agreement with literature data. The range of acidity scale of water is determined from the difference between the halfneutralization potentials of electrogenerated perchloric acid and that of sodium hydroxide in a sodium perchlorate medium. The halfneutralization potentials were measured using both a glass-SCE and a (H2/Pdind-SCE electrode pairs. A wider range of relative acidity scale of water was obtained with the glass-SCE electrode pair.

Fluoro-apatite surface composition in aqueous solution deduced from potentiometric, electrokinetic, and solubility measurements, and spectroscopic observations

International Nuclear Information System (INIS)

Chairat, C.; Oelkers, E.H.; Schott, J.; Lartigue, J.E.

2007-01-01

The surface chemistry of fluoro-apatite 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 fluoro-apatite (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 similar to 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. (authors)

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

Science.gov (United States)

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

1996-01-01

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

A General Simulator for Acid-Base Titrations

Science.gov (United States)

de Levie, Robert

1999-07-01

General formal expressions are provided to facilitate the automatic computer calculation of acid-base titration curves of arbitrary mixtures of acids, bases, and salts, without and with activity corrections based on the Davies equation. Explicit relations are also given for the buffer strength of mixtures of acids, bases, and salts.

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

Science.gov (United States)

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

1968-07-01

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

Determination of nitric acid in highly radioactive solutions by the method of coulometric titration

International Nuclear Information System (INIS)

Gromov, V.S.; Kuperman, A.Ya.; Smirnov, Yu.A.

1988-01-01

A procedure, a cell, and an electronic block have been developed for a long-distance determination of nitric acid in highly radioactive industrial solutions by coulometric titration under hot chamber conditions. A solution of a mixture of ammonium and potassium oxalates was used for the background and anoide electrolytes. This solution prevents the hydrolysis of the metal ions and appreciably decreases the rate of accumulation of the acid in the anode chamber of the cell. Titration with 0.1-0.5 A currents is carried out with internal generation of hydroxyl ions. The cell was prepared from a radiation-resistant and transparent material, poly(methyl methacrylate). The anode and cathode chambers were separated by a cellophane membrane, reinforced by a porous glass filter. By using the electronic coulometric block working together with a pH-meter (EV-74 or I-130) and with an automatic titration block (BAT-15), the titration can be carried out automatically, and the determination results can be obtained in a digital form

Direct potentiometric control of chloride-ion content in water coolant of nuclear reactors

International Nuclear Information System (INIS)

Moskvin, L.N.; Vilkov, N.Ya.; Krasnoperov, V.M.; Epimakhova, L.V.

1979-01-01

The work of automatic chloride measuring device designed for continuous determination of chloride-ion concentration in water coolants of nuclear power plants is investigated. A series of experiments have been performed to investigate a device with sensitive element in the form of potentiometric cell with two flowing porous metal silver electrodes (PSE), placed in series. A calibration circuit of chloride measuring devices and PSE is described. A comparison is made between the results obtained by means of automatic chloride measuring device and results of manual control of samples. A conclusion is drawn that automatic chloride measuring devices meet the requirements of nuclear power plants for methods and instruments of control of chloride-ions microconcentration. The development and implantation of automatic chloride-ion analizers will make the analytical control on nuclear power plants easier and make it possible to obtain more reliable information

Potentiometric and electrokinetic signatures of iron(II) interactions with (α,γ)-Fe2O3.

Science.gov (United States)

Toczydłowska, Diana; Kędra-Królik, Karolina; Nejbert, Krzysztof; Preočanin, Tajana; Rosso, Kevin M; Zarzycki, Piotr

2015-10-21

The electrochemical signatures of Fe(II) interactions with iron(III) oxides are poorly understood, despite their importance in controlling the amount of mobilized iron. Here, we report the potentiometric titration of α,γ-Fe2O3 oxides exposed to Fe(II) ions. We monitored in situ surface and ζ potentials, the ratio of mobilized ferric to ferrous, and the periodically analyzed nanoparticle crystal structure using X-ray diffraction. Electrokinetic potential reveals weak but still noticeable specific sorption of Fe(II) to the oxide surface under acidic conditions, and pronounced adsorption under alkaline conditions that results in a surface potential reversal. By monitoring the aqueous iron(II/III) fraction, we found that the addition of Fe(II) ions produces platinum electrode response consistent with the iron solubility-activity curve. Although, XRD analysis showed no evidence of γ-Fe2O3 transformations along the titration pathway despite iron cycling between aqueous and solid reservoirs, the magnetite formation cannot be ruled out.

PVC-membrane potentiometric sensors based on a recently synthesized Schiff base for Fe(III ion

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S. Yousef Ebrahimipur

2012-12-01

Full Text Available A potentiometric iron sensor based on the use 3-(2-diethylamino-ethylimino-1,3-dihydro-indol-2-one (DEDIO as an ionophore in poly(vinyl chloride (PVC matrix, is reported. The plasticized membrane sensor exhibits a Nernstian response for Fe(III ions over a wide concentration range (2.0 × 10-6 - 5.0 × 10-2 M with a super Nernstian slope of 26(plus or minus 1 mV per decade. It has a fast response time of less than 12 s and can be used for ten weeks without any considerable divergences in its potentials the electrode can be used in the pH range 4.5-8.0. The proposed sensor shows fairly good discriminating ability towards Fe(III ion in comparison with a large number of alkali, alkaline earth, transition and heavy metal ions. The sensor was used as indicator electrode in potentiometric titration of Fe(III ions vs. EDTA.DOI: http://dx.doi.org/10.4314/bcse.v26i1.7

A new oxidimetric reagent: potassium dichromate in a strong phosphoric acid medium--VII. Photometric titration of vanadium(IV) and of cerium(III) alone and in mixtures with iroN(II).

Science.gov (United States)

Rao, G G; Rao, P K

1967-01-01

Vanadium(IV) can be accurately titrated with potassium dichromate in media containing phosphoric acid of 3-12M concentration: the change in absorption of vanadium(IV) is followed in the region 660 mmicro using a red filter. It is more convenient to carry out the titration in 3M phosphoric acid because at higher concentrations chloride, nitrate, cerium(III) and manganese(II) may interfere. Photoelcetric titration is more convenient than potentiometric because the former can be made in a 3M phosphoric acid medium, whereas the latter is possible only in 12M phosphoric acid. The simultaneous differential photometric titration of iron(II) and vanadium(IV) is also possible. Conditions have been found for the photometric titration of cerium(III) and of cerium(III) plus iron(II). The titration is carried out (at 450 mmicro or with a blue filter) in about 10.5M phosphoric acid. Application of the method to a cerium mineral is considered.

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

Science.gov (United States)

Tôrres, Adamastor Rodrigues; Lyra, Wellington da Silva; de Andrade, Stéfani Iury Evangelista; Andrade, Renato Allan Navarro; da Silva, Edvan Cirino; Araújo, Mário César Ugulino; Gaião, Edvaldo da Nóbrega

2011-05-15

This work proposes the use of digital image-based method for determination of total acidity in red wines by means of acid-base titration without using an external indicator or any pre-treatment of the sample. Digital images present the colour of the emergent radiation which is complementary to the radiation absorbed by anthocyanines present in wines. Anthocyanines change colour depending on the pH of the medium, and from the variation of colour in the images obtained during titration, the end point can be localized with accuracy and precision. RGB-based values were employed to build titration curves, and end points were localized by second derivative curves. The official method recommends potentiometric titration with a NaOH standard solution, and sample dilution until the pH reaches 8.2-8.4. In order to illustrate the feasibility of the proposed method, titrations of ten red wines were carried out. Results were compared with the reference method, and no statistically significant difference was observed between the results by applying the paired t-test at the 95% confidence level. The proposed method yielded more precise results than the official method. This is due to the trivariate nature of the measurements (RGB), associated with digital images. Copyright © 2011 Elsevier B.V. All rights reserved.

Aqueous uranyl complexes. 3. Potentiometric measurements of the hydrolysis of uranyl(VI) ion at 25 degrees C

International Nuclear Information System (INIS)

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

1995-01-01

Potentiometric titrations of uranyl(VI) solutions were conducted using a standard glass/calomel electrode combination over the pH range 3 to 12 at 0.1 mol-kg -1 ionic strength with tetramethylammonium trifluoromethanesulfonate as the supporting electrolyte. The electrodes were calibrated directly on the hydrogen ion concentration scale during the initial stage of each titration. The species, UO 2 2+ , (UO 2 ) 2 (OH) 2 2+ , (UO 2 ) 3 (OH) 5 + , (UO 2 ) 3 (OH) 7 - , (UO 2 ) 3 (OH) 8 2- , and (UO 2 ) 3 (OH) 10 4- identified in an earlier Raman study were compatible with the analysis of the titration data. Based on this analysis and application of the extended Debye-Hueckel treatment, the polynuclear species indicated above were assigned overall formation constants at 25 degrees C and at infinite dilution of -5.51±0.04, -15.3±0.1, -27.77±0.09, -37.65±0.14, and -62.4±0.3, respectively. The results are discussed in reference to hydrolysis quotients reported in the literature for the first three species. Formation quotients for the last two species have not been reported previously

Liquid membrane ion-selective electrodes for potentiometric dosage of coper and nickel

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MARIA PLENICEANY

2005-02-01

Full Text Available This paper presents experimental and theoretical data regarding the preparation and characterization of three liquid-membrane electrodes, which have not been mentioned in the specialized literature so far. The active substances, the solutions of which in nitrobenzene formed the membranes on a graphite rod, are simple complex combinations of Cu(II and Ni(II ions with an organic ligand belonging to the Schiff base class: N-[2-thienylmethilidene]-2-aminoethanol (TNAHE. The Cu2+ -selective and Ni2+ -selective electrodes were used to determine the copper and nickel ions in aqueous solutions, both by direct potentiometry and by potentiometric titration with EDTA. They were also used for the determination of Cu2+ and Ni2+ ions in industrial waters by direct potentiometry.

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

Science.gov (United States)

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. Copyright © 2014 Elsevier B.V. All rights reserved.

Potentiometric investigations of molecular heteroconjugation equilibria of substituted phenol+n-butylamine systems in dimethyl sulfoxide

International Nuclear Information System (INIS)

Czaja, MaIgorzata; Baginska, Katarzyna; Kozak, Anna; Makowski, Mariusz; Chmurzynski, Lech

2005-01-01

Molecular heteroconjugation constants, K BHA DMSO and K AHB DMSO , expressed as their logarithms, have been determined by potentiometric titration for eleven substituted phenol+n-butylamine systems in a polar protophilic aprotic solvent, dimethyl sulfoxide (DMSO). An increasing tendency towards molecular heteroconjugation in these systems without proton transfer has been found with increasing pK a DMSO (HA), i.e., with decreasing phenol acidity. Moreover, a linear correlation has been established between the determined lgK BHA DMSO values and pK a DMSO (HA). Furthermore, overall stability constants, lgK o DMSO , could be correlated linearly with pK a DMSO (HA) values

Sorbents and Mechanisms of Removal

Science.gov (United States)

2010-08-21

potentiometric   titration ,   X-­‐ray  diffraction   and  FTIR   spectroscopy.  Results  of  breakthrough  tests  show  significant...thermogravimetric analyses, potentiometric titration and sorption of nitrogen. It was found that not only oxygen-containing groups but also sulfur-containing groups...using adsorption of nitrogen, XRD, FTIR, TA, and potentiometric titration . The results showed differences in the texture and chemistry of adsorbents

Potentiometric titration of uranium reduced by chromic salts in chloridic solutions; Titulacao potenciometrica de uranio reduzido por sais cromosos em solucoes cloridricas

Energy Technology Data Exchange (ETDEWEB)

Coutinho, C M.C.; Bastos, E T.R.

1986-06-01

The utilization of chromic salts for reducing the uranium (VI) from chloridic solutions, for potentiometric dosage is described. This method is used in the range of 0,002 to 1,0 M of uranium. (C.G.C.).

Potentiometric Membrane Sensors for Levamisole Determination

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Natalia Zubenya

2016-11-01

Full Text Available The ion pair (IP of levamisole with BiI4-(SbI4- for the levamisole-selective sensor with a PVC membrane containing - ions were developed. Thermal behavior of obtained IP was investigated by differential thermal analysis that would show the thermal stability and the character of the decomposition of the complex. The thermolysis of Lev+BiI4- IP undergoes three stages that fit a theoretical interpretation. the linearity ranges of levamisole sensors function are 7.9 ×10-6 – 1×10-1 (7.9 ×10-5 – 1×10-1 M. The Nernstian slope of                   50.6 – 53.4 mV pC−1 and detection limit of 5.0 × 10−5 – 1.5 × 10−4 M. The working range of pH is 2.8 – 6.0.     The efficiency of the use of electrodes for levamisole content control in pharmaceutical preparations was shown by direct potentiometry and potentiometric titration methods.

Permian potentiometric analysis

International Nuclear Information System (INIS)

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

Método potenciométrico para determinação de cobre em cachaça Potentiometric method for copper determination in sugarcane spirit

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Ivo L. Küchler

1999-06-01

Full Text Available 'Cachaça' is the Brazilian name for the spirit obtained from sugarcane. According to Brazilian regulations, it may be sold raw or with addition of sugar and may contain up to 5 mg/L of copper. Copper in "cachaça" was determined by titration with EDTA, using a homemade copper membrane electrode for end-point detection. It was found a pooled standard deviation of 0,057 mg/L and there was no significant difference between the results obtained by the potentiometric method and by flame atomic absorption spectrometry with standard addition. Among the 21 'cachaça' samples from 16 different brands analyzed, three overpassed the legal copper limit. For its characteristics of accuracy, precision, and speed, the potentiometric method may be employed advantageously in routine analysis, specially when low cost is a major concern.

Determination of U and Impurities Elements in The Uranium Tetra Fluoride by Potentiometric and Atomic Absorption Spectrophotometric Methods

International Nuclear Information System (INIS)

Putro Kasino, P

1998-01-01

The determination of u and impurities contents in the Uranium tetra fluoride (UF 4 )has been carried out by potentiometric titration using modified 'Davies-Gray' and atomic absorption spectrophotometric methods. Dissolution process of the powder sample using saturated Al 2 (SO 4 ) 3 solution introduced to determine UF 4 compound content in the UF 4 sample. The uranium Content in the obtained filtrate is analyzed by potentiometric. The impurities content is determined by ato-Mic absorption spectrophotometric using ammonium oxalate powder in introducing of the sample preparation. The experiment covered the observation on influence of stirring time of UF 4 sample dissolution in respect to separate UF 4 from its impurities in determination of uranium content. Also the effects of Ammonium Oxalate added and agitating time were observed deal with the sample preparation for the determination of Impurities content.The analysis result found that UF 4 content was 96.15 ± 0.04% the relative station 0.7%. However the best impurities determination was achieved by addition of ammonium oxalate powder and 15 Minutes of agitation time at temperature of 800 0 C

Potentiometric investigation of acid dissociation and anionic homoconjugation equilibria of substituted phenols in dimethyl sulfoxide

International Nuclear Information System (INIS)

Czaja, Malgorzata; Kozak, Anna; Makowski, Mariusz; Chmurzynski, Lech.

2003-01-01

Standard acidity constants, K a DMSO (HA), expressed as pK a DMSO (HA) values, and anionic homoconjugation constants, K DMSO AHA - , (in the form of lg K DMSO AHA - values) have been determined for 11 substituted phenol-phenolate systems a polar protophilic aprotic solvent, dimethyl sulfoxide (DMSO) with a potentiometric titration. A linear relationship has been determined between lg K DMSO AHA - and pK a DMSO (HA). The tendency towards anionic homoconjugation in these systems increases with increasing pK a DMSO (HA) that is with declining phenol acidity. The pK a DMSO (HA) are correlated with both pK a W (HA) water and other polar non-aqeous solvents

Potentiometric investigations of molecular heteroconjugation equilibria of substituted phenol+n-butylamine systems in dimethyl sulfoxide

Energy Technology Data Exchange (ETDEWEB)

Czaja, MaIgorzata [Department of General Chemistry, University of Gdansk, Sobieskiego 18, 80-952 Gdansk (Poland); Baginska, Katarzyna [Department of General Chemistry, University of Gdansk, Sobieskiego 18, 80-952 Gdansk (Poland); Kozak, Anna [Department of General Chemistry, University of Gdansk, Sobieskiego 18, 80-952 Gdansk (Poland); Makowski, Mariusz [Department of General Chemistry, University of Gdansk, Sobieskiego 18, 80-952 Gdansk (Poland); Chmurzynski, Lech [Department of General Chemistry, University of Gdansk, Sobieskiego 18, 80-952 Gdansk (Poland)]. E-mail: lech@chem.univ.gda.pl

2005-08-15

Molecular heteroconjugation constants, K{sub BHA}{sup DMSO} and K{sub AHB}{sup DMSO}, expressed as their logarithms, have been determined by potentiometric titration for eleven substituted phenol+n-butylamine systems in a polar protophilic aprotic solvent, dimethyl sulfoxide (DMSO). An increasing tendency towards molecular heteroconjugation in these systems without proton transfer has been found with increasing pK{sub a}{sup DMSO} (HA), i.e., with decreasing phenol acidity. Moreover, a linear correlation has been established between the determined lgK{sub BHA}{sup DMSO} values and pK{sub a}{sup DMSO} (HA). Furthermore, overall stability constants, lgK{sub o}{sup DMSO}, could be correlated linearly with pK{sub a}{sup DMSO} (HA) values.

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

Science.gov (United States)

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.

Potentiometric Zinc Ion Sensor Based on Honeycomb-Like NiO Nanostructures

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Magnus Willander

2012-11-01

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

A new oxidimetric reagent-potassium dichromate in a strong phosphoric acid medium-VIII Potentiometric titration of molybdenum(VI) and vanadium(V).

Science.gov (United States)

Muralikrishna, U; Rao, G G

1968-01-01

A new titrimetric method is described for the determination of molybdenum(VI) involving prior reduction to Mo(V) with an excess of Fe(II) in a concentrated phosphoric acid solution, followed by titration with dichromate. The titration can be done at room temperature and without protective atmosphere. Uranium interferes, but vanadium may be determined simultaneously.

The determination of boron and carbon in reactor grade boron carbide

International Nuclear Information System (INIS)

Crossley, D.; Wood, A.J.; McInnes, C.A.J.; Jones, I.G.

1978-09-01

The sealed tube method of dissolution at high temperature and pressure has been successfully applied in the analysis of reactor grade boron carbide for the determination of boron. A 50 mg sample of boron carbide is completely dissolved by heating with concentrated nitric acid in a sealed tube at 300 0 C. The boron content of the resultant sample solution is determined by the mannitol potentiometric titration method. The precision of the method for the determination of 2.5 mg of boron using the Harwell automatic potentiometric titrator is 0.2% (coefficient of variation). The carbon content of a boron carbide sample is determined by combustion of the sample at 1050 0 C in a stream of oxygen using vanadium pentoxide to ensure the complete oxidation of the sample. The carbon dioxide produced from the sample is measured manometrically and the precision of the method for the determination of 4 mg of carbon is 0.4% (coefficient of variation). (author)

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

Science.gov (United States)

Barbieri Gonzaga, Fabiano; Pereira Sobral, Sidney

2012-08-15

A new method is proposed for determining the acid number (AN) of biodiesel using coulometric titration with potentiometric detection, basically employing a potentiostat/galvanostat and an electrochemical cell containing a platinum electrode, a silver electrode, and a combination pH electrode. The method involves a sequential application of a constant current between the platinum (cathode) and silver (anode) electrodes, followed by measuring the potential of the combination pH electrode, using an isopropanol/water mixture as solvent and LiCl as the supporting electrolyte. A preliminary evaluation of the new method, using acetic acid for doping a biodiesel sample, showed an average recovery of 100.1%. Compared to a volumetric titration-based method for determining the AN of several biodiesel samples (ranging from about 0.18 to 0.95 mg g(-1)), the new method produced statistically similar results with better repeatability. Compared to other works reported in the literature, the new method presented an average repeatability up to 3.2 times better and employed a sample size up to 20 times smaller. Copyright © 2012 Elsevier B.V. All rights reserved.

Automated sample-processing and titration system for determining uranium in nuclear materials

International Nuclear Information System (INIS)

Harrar, J.E.; Boyle, W.G.; Breshears, J.D.; Pomernacki, C.L.; Brand, H.R.; Kray, A.M.; Sherry, R.J.; Pastrone, J.A.

1977-01-01

The system is designed for accurate, precise, and selective determination of from 10 to 180 mg of uranium in 2 to 12 cm 3 of solution. Samples, standards, and their solutions are handled on a weight basis. These weights, together with their appropriate identification numbers, are stored in computer memory and are used automatically in the assay calculations after each titration. The measurement technique (controlled-current coulometry) is based on the Davies-Gray and New Brunswick Laboratory method, in which U(VI) is reduced to U(IV) in strong H 3 PO 4 , followed by titration of the U(IV) with electrogenerated V(V). Solution pretreatment and titration are automatic. The analyzer is able to process 44 samples per loading of the sample changer, at a rate of 4 to 9 samples per hour. The system includes a comprehensive fault-monitoring system that detects analytical errors, guards against abnormal conditions which might cause errors, and prevents unsafe operation. A detailed description of the system, information on the reliability of the component subsystems, and a summary of its evaluation by the New Brunswick Laboratory are presented

Recovery of [CO2]T from Aqueous Bicarbonate using a Gas Permeable Membrane

Science.gov (United States)

2008-06-25

coulometer. For the potentiometric titrations , the entire 150 mL of the water/bicarbonate solution sample was collected and titrated with 0.2 M HCl...High Precision Determination of Titration Alkalinity and Total Carbon Dioxide Content of Sea Water by Potentiometric Titration . Deep-Sea Res. 1970...IL 60436) [8] or by strong acid titration [18,19]. All solutions for the coulometer were of reagent grade and purchased from UIC Inc. The lower

Automatic chemical determination facility for plutonium and uranium

International Nuclear Information System (INIS)

Benhamou, A.

1980-01-01

A proposal for a fully automated chemical determination system for uranium and plutonium in (U, Pu)O 2 mixed oxide fuel, from the solid sample weighing operation to the final result is described. The steps completed to data are described. These include: test sample preparation by weighing, potentiometer titration system, cleaning and drying of glassware after titration. The process uses a Mettler SR 10 Titrator System in conjunction with others automatized equipment in corse of realization. Precision may reach 0.02% and is generally better than 0.1%. Accuracy in within +-0.1% of manual determination results or titration standards [fr

Stanovení disociačních konstant vybraných polyaza derivátů

OpenAIRE

Hajduová, Jana

2010-01-01

Title: Determination of dissociation exponents of selected polyaza derivatives Annotation: The aim of this thesis is extimation of dissociation exponets of seclected polyaza derivatives by acid-base titration with potentiometric registration of titration curve. The titration curve was processed using Hyperquad 2006 software. The satisfactory agreement of determined values of dissociation exponents with literature data was found. Key words: dissociation exponent, potentiometric titration, poly...

Dysprosium selective potentiometric membrane sensor

Energy Technology Data Exchange (ETDEWEB)

Zamani, Hassan Ali, E-mail: haszamani@yahoo.com [Department of Applied Chemistry, Mashhad Branch, Islamic Azad University, Mashhad (Iran, Islamic Republic of); Faridbod, Farnoush; Ganjali, Mohammad Reza [Center of Excellence in Electrochemistry, Faculty of Chemistry, University of Tehran, Tehran (Iran, Islamic Republic of)

2013-03-01

A novel Dy(III) ion-selective PVC membrane sensor was made using a new synthesized organic compound, 3,4-diamino-N Prime -((pyridin-2-yl)methylene)benzohydrazide (L) as an excellent sensing element. The electrode showed a Nernstian slope of 19.8 {+-} 0.6 mV per decade in a wide concentration range of 1.0 Multiplication-Sign 10{sup -6}-1.0 Multiplication-Sign 10{sup -2} mol L{sup -1}, a detection limit of 5.5 Multiplication-Sign 10{sup -7} mol L{sup -1}, a short conditioning time, a fast response time (< 10 s), and high selectivity towards Dy(III) ion in contrast to other cations. The proposed sensor was successfully used as an indicator electrode in the potentiometric titration of Dy(III) ions with EDTA. The membrane sensor was also applied to the F{sup -} ion indirect determination of some mouth washing solutions and to the Dy{sup 3+} determination in binary mixtures. Highlights: Black-Right-Pointing-Pointer The novelty of this work is based on the high affinity of the ionophore toward the Dy{sup 3+} ions. Black-Right-Pointing-Pointer This technique is very simple, fast and inexpensive and it is not necessary to use sophisticated equipment. Black-Right-Pointing-Pointer The newly developed sensor is superior to the formerly reported Dy{sup 3+} sensors in terms of selectivity.

Plutonium estimation in the process solutions and oxide dissolved audit samplers by potentiometry using memo titrator

International Nuclear Information System (INIS)

Kumaraguru, K.; Shukla, Y.D.; Vijayan, K.; Ramamoorthy, N.; Jambunathan, U.; Kapoor, S.C.

1990-01-01

Potentiometric method is employed by using memotitrator coupled with combined electrode for the estimation of plutonium. The estimations are carried out on the process samples and the acid dissolved samples for auditing, in the concentration range of 5 g/l to 20 g/l. The chemical procedure is: i)oxidising plutonium to higher oxidation state by silver oxide, ii)reducing the same by adding excess ferrous, and iii)titrating potassium dichromate against the unreacted ferrous. The plutonium content is computed from ferrous consumed in the reaction. The average percentage error of the method is +/-0.27. The values obtained are in close agreement with those obtained by coulometry. (author)

Estimation of free acid content in lanthanide salt solution used for pH-potentiometric determination of their stability constants with organic ligands

International Nuclear Information System (INIS)

Zheltvaj, I.I.; Tishchenko, M.A.

1985-01-01

To improve the pH-potentiometric method for determining complex stability constants the possibility of alkalimetric titration of a free acid in the lanthanide perchlorate solution after binding metal ions by disodium salt of ethylene-diamine-tetraacetic acid is studied. The stability constants were determined from the difference between the total acid content after complexon addition and doubled metal cation content in the solution which has been preliminarily determined by the complexonometric method. It is shown that the alkaline (NaOH) equivalent quantities spent for free acid titration either in the absence or presence of the complexon is different. With increase of free acid content in the solution the difference in determinations with complexon and without it is somewhat reduced. Thus, the use of complexon contributes to a higher accuracy in determining the free acid, and in the first place in case of minor contents

Micellar and analytical implications of a new potentiometric PVC sensor based on neutral ion-pair complexes of dodecylmethylimidazolium bromide-sodium dodecylsulfate.

Science.gov (United States)

Sanan, Reshu; Mahajan, Rakesh Kumar

2013-03-15

With an aim to characterize the micellar aggregates of imidazolium based ionic liquids, a new potentiometric PVC sensor based on neutral ion-pair complexes of dodecylmethylimidazolium bromide-sodium dodecylsulfate (C12MeIm(+)DS(-)) has been developed. The electrode exhibited a linear response for the concentration range of 7.9×10(-5)-9.8×10(-3) M with a super-Nernstian slope of 92.94 mV/decade, a response time of 5 s and critical micellar concentration (cmc) of 10.09 mM for C12MeImBr. The performance of the electrode in investigating the cmc of C12MeImBr in the presence of two drugs [promazine hydrochloride (PMZ) and promethazine hydrochloride (PMT)] and three triblock copolymers (P123, L64 and F68) has been found to be satisfactory on comparison with conductivity measurements. Various micellar parameters have been evaluated for the binary mixtures of C12MeImBr with drugs and triblock copolymers using Clint's, Rubingh's, and Motomura's approach. Thus the electrode offers a simple, straightforward and relatively fast technique for the characterization of micellar aggregates of C12MeImBr, complementing existing conventional techniques. Further, the analytical importance of proposed C12MeIm(+)-ISE as end point indicator in potentiometric titrations and for direct determination of cationic surfactants [cetylpyridinium chloride (CPC), tetradecyltrimethylammonium bromide (TTAB), benzalkonium chloride (BC)] in some commercial products was judged by comparing statistically with classical two-phase titration methods. Copyright © 2013 Elsevier Inc. All rights reserved.

An online computer method for the potentiometric titration of mixtures of a strong and a weak acid

NARCIS (Netherlands)

Bos, M.

1977-01-01

A PDP-11 online computer method for the titration of mixtures or a strong and a weak acid is described.The method is based on multiparametric curve-fitting. One or the parameters found from the calculations is the dissociation constant of the weak acid, hence the method can be applied even when this

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

International Nuclear Information System (INIS)

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

2007-01-01

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

Potentiometric determination of chloride ions in circulating water systems of the Kirishinefteorgsintez production association

International Nuclear Information System (INIS)

Sukhova, N.S.; Skatina, L.I.

1993-01-01

The chloride content of circulating water and wastewater in industrial plants is one of the important indexes of contamination. The increasingly stringent sanitary and ecological requirements that have been imposed on wastewater are making it necessary to monitor the chloride content on a regular basis. It is difficult to use the mercurometric method of chloride determination that has been recommended for use in petroleum refineries in analyzing turbid of dark-colored waters with high contents of organic matter. Also, when the mercurometric method is used, accurate control of pH must be maintained in order to achieve good reproducibility of results. The authors are proposing a rapid method for monitoring the content of chloride ions in circulating water systems by potentiometric titration of a sample in a medium of glacial acetic acid by a 0.01 M solution of silver nitrate with the silver indicator electrode and a silver chloride auxiliary electrode EVL-1MZ, filled with a saturated solution of potassium nitrate. The potential is measured 30 sec after it has been established, in a type pH-121 potentiometer. The titration is performed from a microburette with a scale division of 0.02 cm 3 , with constant stirring of the test solution by means of a magnetic stirrer

Acid-base strengths in 1,2-dichloroethane

NARCIS (Netherlands)

Bos, M.; Dahmen, E.A.M.F.

1973-01-01

The pKa value of hydriodic acid in 1,2-dichloroethane was determined from conductivity measurements. A glass electrode was calibrated for dichloroethane in the potentiometric titration of hydriodic acid with tetramethylguanidine. From potentiometric titrations, the pKa values in dichloroethane of

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

Science.gov (United States)

Rao, G G; Rao, P K

1966-09-01

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

Potentiometric determination of acid dissociation constants (pKa) for human and veterinary antibiotics.

Science.gov (United States)

Qiang, Zhimin; Adams, Craig

2004-07-01

This work determined the acid dissociation constants (pKa) of 26 common human and veterinary antibiotics by potentiometric titration. Selected antibiotics consisted of sulfonamides, macrolides, tetracyclines, fluoroquinolones, and other miscellaneous antibiotics. After validation of analysis methods using phosphoric acid as a model compound, a second-derivative (delta2pH/deltaV2) method was primarily applied to determining pKa's from titration curves for most antibiotics due to its convenience and accuracy. For tetracyclines, however, a least-square non-linear regression method was developed to determine their pKa's because the second-derivative method cannot well distinguish the pKa,2 and pKa,3 of tetracyclines. Results indicate that the pKa values are approximately 2 and 5-7.5 for sulfonamides; 7.5-9 for macrolides; 3-4, 7-8 and 9-10 for tetracyclines; 3-4, 6, 7.5-9 and 10-11 for fluoroquinolones; while compound-specific for other miscellaneous antibiotics. The moieties corresponding to specific pKa's were identified based on chemical structures of antibiotics. In addition, the pKa's available in literature determined by various techniques are compiled in comparison with the values of this work. These results are expected to essentially facilitate the research on occurrence, fate and effects, analysis methods development, and control of antibiotics in various treatment operations.

Titulações espectrofotométricas de sistemas ácido-base utilizando extrato de flores contendo antocianinas Spectrophotometric titrations of acid-base systems using flower extracts containig anthocyanins

Directory of Open Access Journals (Sweden)

Mônica Souza Cortes

2007-08-01

Full Text Available Considering the attraction of the students' attention by the changes in the colors of vegetable crude extracts caused by the variation of the pH of the medium, the use of these different colors in order to demonstrate principles of spectrophotometric acid-base titrations using the crude extracts as indicators is proposed. The experimental setup consisted of a simple spectrophotometer, a homemade flow cell and a pump to propel the fluids along the system. Students should be stimulated to choose the best wavelength to monitor the changes in color during the titration. Since the pH of the equivalence point depends on the system titrated, the wavelength must be properly chosen to follow these changes, demonstrating the importance of the correct choice of the indicator. When compared with the potentiometric results, errors as low as 2% could be found using Rhododendron simsii (azalea or Tibouchina granulosa (Glory tree, quaresmeira as sources of the crude extracts.

Coulometric titrations of bases in propylene carbonate and g-butyrolactone using hydroquinone as the depolarizer and a quinhydrone indicator electrode

Directory of Open Access Journals (Sweden)

Z. D. STANIC

2000-08-01

Full Text Available The application of hydroquinone for the coulometric generation of hydrogen ions in propylene carbonate (PC and g-butyrolactone (GBL is described. The current-potential curves recorded for theid sepolarizer, titrated bases, indicator and the solvents used showed that the investigated depolarizer is oxidized at lower potentials than the oxidation potentials of other components in the solution. the hydrogen ions generated by the oxidation of hydroquinone were used for the titration of organic bases (triethylamine, n-butylamine, pyridine, quinoline, aniline, N,N’-diphenylguanidine, piperidine, and 2,2’-bipiridine in PC and GBL with visual (Crystal Violet as indicator and potentiometric end-point detection using a quinhydrone electrode as the indicator electrode. The quinhydrone added to the to be analyzed solution served both as a source of hydrogen ions and, together with the immersed platinum electrode, as a quinhydrone electrode. The relative error of the determination of the bases was about 1 %.

Microelectrode generator-collector systems for electrolytic titration: theoretical and practical considerations.

Science.gov (United States)

Bell, Christopher G; Seelanan, Parinya; O'Hare, Danny

2017-10-23

Electochemical generator-collector systems, where one electrode is used to generate a reagent, have a potentially large field of application in sensing and measurement. We present a new theoretical description for coplanar microelectrode disc-disc systems where the collector is passive (such as a potentiometric sensor) and the generator is operating at constant flux. This solution is then used to develop a leading order solution for such a system where the reagent reacts reversibly in solution, such as in acid-base titration, where a hydrogen ion flux is generated by electrolysis of water. The principal novel result of the theory is that such devices are constrained by a maximum reagent flux. The hydrogen ion concentration at the collector will only reflect the buffer capacity of the bulk solution if this constraint is met. Both mathematical solutions are evaluated with several microfabricated devices and reasonable agreement with theory is demonstrated.

Experience in usage of T-108 titrimetric laboratory unit for precision analysis of uranium-containing materials

International Nuclear Information System (INIS)

Ryzhinskij, M.V.; Bronzov, P.A.

1989-01-01

Possibilities of the T-108 device of potentiometric titration for precise determination of uranium in various uranium-containing materials are studied, the results being presented. Principle flowsheet of the device and the sequence of analytic procedure of uranium potentiometric titration are considered. U 3 O 8 , UO 2 and UF 4 were used as materials to be analyzed, state standard samples of K 2 Cr 2 O 7 -SSS 2215-81 and U 3 O 8 SSS 2396-83P- as standard samples. It is shown that relative standard deviation during titration using the T-108 device is mainly determined by the error of determination of the final titration point potention and it must not exceed 0.002 for uranium titration considered. The conclusion is made that the variant of potentiometric titration of uranium with the use of the T-108 device is not inferior in its accuracy to gravimetry and surpasses it in productivity and possibility of automation. 4 refs.; 2 figs.; 2 tabs

Highly selective potentiometric and colorimetric determinations of cobalt (II) ion using thiazole based ligands.

Science.gov (United States)

Singhal, Divya; Singh, Ashok Kumar; Upadhyay, Anjali

2014-12-01

New PVC-membrane electrodes were prepared by using 2-((thiazol-2-ylimino)methyl)phenol (L1) and 2-((thiazol-2-ylamino)methyl)phenol (L2) and explored as Co(II) selective electrodes. The effect of various plasticizers and anion excluder was studied in detail and improved performance was observed. It was found that the electrode based on L1 shows better response characteristics in comparison to L2. Optimum performance was observed for the membrane electrode having a composition of L1:NaTPB:DBP:PVC≡2:8:78:62 (w/w, mg). The performance of PME based on L1 was compared with that of CGE. The electrodes exhibit Nernstian slope for Co(II) ions with a limit of detection of 6.91×10(-7) mol L(-1) for PME and 7.94×10(-8) mol L(-1) for CGE. The response time for PME and CGE was found to be 15s and 12 s respectively. The potentiometric responses are independent in the pH range 3.0-9.0 for CGE. The CGE could be used for a period of 90 days. The CGE was used as an indicator electrode in potentiometric titration of EDTA with Co(2+) ion. Further the selectivity of the L1 and L2 was also confirmed by the UV-vis and colorimetric studies and found that L1 is more selective for Co(II) ion. Copyright © 2014 Elsevier B.V. All rights reserved.

Potentiometric chip-based multipumping flow system for the simultaneous determination of fluoride, chloride, pH, and redox potential in water samples.

Science.gov (United States)

Chango, Gabriela; Palacio, Edwin; Cerdà, Víctor

2018-08-15

A simple potentiometric chip-based multipumping flow system (MPFS) has been developed for the simultaneous determination of fluoride, chloride, pH, and redox potential in water samples. The proposed system was developed by using a poly(methyl methacrylate) chip microfluidic-conductor using the advantages of flow techniques with potentiometric detection. For this purpose, an automatic system has been designed and built by optimizing the variables involved in the process, such as: pH, ionic strength, stirring and sample volume. This system was applied successfully to water samples getting a versatile system with an analysis frequency of 12 samples per hour. Good correlation between chloride and fluoride concentration measured with ISE and ionic chromatography technique suggests satisfactory reliability of the system. Copyright © 2018 Elsevier B.V. All rights reserved.

Potentiometric investigations of (acid+base) equilibria in (n-butylamine+acetic acid) systems in binary (acetone+cyclohexane) solvent mixtures

International Nuclear Information System (INIS)

Czaja, MaIgorzata; Kozak, Anna; Makowski, Mariusz; Chmurzynski, Lech

2005-01-01

By using the potentiometric titration method, standard equilibrium constants have been determined of acid dissociation of molecular acid, K a (HA), cationic acid, K a (BH + ), of anionic and cationic homoconjugation, K AHA - andK BHB + , respectively, and of molecular heteroconjugation, K AHB (K BHA ), in (acid+base) systems without proton transfer consisting of n-butylamine and acetic acid in binary (acetone+cyclohexane) solvent mixtures. The results have shown that both the pK a (HA) and pK a (BH + ), as well as lgK AHA - values change non-linearly as a function of composition of the solvent mixture. On the other hand, standard molecular heteroconjugation constants without proton transfer do not depend on the cyclohexane content in the mixture, i.e. on solvent polarity

Potentiometric determination of free nitric-acid in trilaurylamine solutions containing plutonium nitrate; Dosage potentiometrique de l'acidite nitrique libre dans les solutions organiques de trilaurylamine

Energy Technology Data Exchange (ETDEWEB)

Perez, J J; Saey, J C [Commissariat a l' Energie Atomique, Fontenay-aux-Roses (France). Centre d' Etudes Nucleaires

1965-07-01

A potentiometric method of determination of the free nitric acid in trilaurylamine solutions containing plutonium or thorium nitrates is described. The potentiometric titration is carried out in a mixture of benzene and 1,2-dichloro ethane with a standard solution of trilaurylamine as the titrant. When thorium nitrate is present the metal complex is not dissociated then the titration has a single end-point. In the case of plutonium nitrate the partial dissociation of the plutonium complex corresponds to a second point. The experimental error in duplicate analyses of 50 samples is about 1 per cent for free acid concentrations in the range of 0,03 to 0,1 N and plutonium concentrations between 1 to 5 g/l. (authors) [French] Une methode potentiometrique de dosage de l'acidite nitrique libre dans les solutions de trilaurylamine contenant un complexe de plutonium ou de thorium est decrite. La potentiometrie est effectuee en prenant comme base titrante la trilaurylamine et comme milieu de dilution un melange de benzene et de 1,2 dichloroethane. Dans le cas du thorium, le complexe organometallique n'est pas deplace et la courbe de titrage presente un seul point d'inflexion. Dans le cas du plutonium le complexe est partiellement dissocie ce qui correspond a un second saut de potentiel. La moyenne des erreurs experimentales sur 50 echantillons doses a ete d'environ {+-} 1 pour cent sur l'acide libre. Les solutions experimentees contenaient de 0,03 a 0,1 N en acide et de 1 a 5 g/l en plutonium. (auteurs)

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

NARCIS (Netherlands)

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

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

Thermometric titration of sulphate.

Science.gov (United States)

Williams, M B; Janata, J

1970-06-01

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

Pseudo-indicator behaviour of platinum electrode explored for the potentiometric estimation of non-redox systems.

Science.gov (United States)

Raashid, Syed; Chat, Oyais Ahmad; Rizvi, Masood A; Bhat, Mohsin Ahmad; Khan, Badruddin

2012-11-15

A pseudo-indicator electrode based potentiometric method for estimation of non-redox metal ions is presented. In the proposed method, nature and concentration specific impact of analyte over the redox potential of ideally polarisable Pt/pregenerated-redox-couple interface forms the basis of quantification. Utility of the method in estimation of six non-redox metal ions viz. Zn(2+), Cu(2+), Ni(2+), Cd(2+), Pb(2+), Al(3+) in the concentration range of 10(-1)-10(-3) moldm(-3), individually and as binary mixtures is also presented. Three types of potentiometric behaviours, which we ascribe to the nature specific thermodynamic and kinetic aspects of metal-EDTA binding, were observed. While Cu(2+), Ni(2+), Pb(2+) and Al(3+) were found to bind EDTA efficiently, without exchanging Fe(3+); Zn(2+) and Cd(2+) were observed to replace Fe(3+) from EDTA. In contrast, Ca(2+) and Mg(2+) were found to show no binding affinity to EDTA in the pH range employed in the present work. The proposed method was also used to explore the reversibility and the Nernestian behaviour of ferricyanide/ferrocyanide redox couple through spectroelectrochemical titration of Zn(2+) with ferrocyanide. The presented method is presaged to be a reliable and low cost future replacement for costly and delicate ion selective electrodes (ISE) in the estimation of non-redox species like Zn(2+), Cu(2+), etc. Copyright © 2012 Elsevier B.V. All rights reserved.

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

Science.gov (United States)

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

2017-07-01

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

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

Science.gov (United States)

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.

Nuclear fuel technology - Determination of milligram amounts of plutonium in nitric acid solutions - Potentiometric titration with potassium dichromate after oxidation by Ce(IV) and reduction by Fe(II)

International Nuclear Information System (INIS)

2000-01-01

This International Standard describes a precise and accurate analytical method for determining 1 mg to 5 mg of plutonium per millilitre in nitric acid solutions. The method is very selective for plutonium. It is suitable for the direct determination of plutonium in materials ranging from pure product solutions, to solutions of mixed nuclear materials with a uranium/plutonium ratio up to 20:1. However, potential application to the assay of plutonium in solutions of irradiated nuclear fuels and solutions of mixed nuclear materials with uranium/plutonium ratios of 20:1 to 33:1 has not yet been documented. The method recommends that the aliquot be weighed and that the titration burettes be calibrated gravimetrically in order to obtain adequate precision and accuracy. This does not preclude using any alternative technique which can be shown to give an equivalent accuracy. As the reproducibility of the reaction conditions is important to maintain good performance, extensive automatization of the procedure is beneficial

Automatic photometric titration of fluoride with thorium nitrate and alizarin S as indicator

International Nuclear Information System (INIS)

Bliefert, C.; Sobek, M.

1978-01-01

The photometric titration of fluoride with thorium nitrate and Alizarin S as indicator has been automated and optimized for fluoride levels between 1 and 20mg/85ml solution. The interference of several ions has been investigated. This procedure is particularly useful for the determination of fluoride after fusion with peroxides as fluxing agents. (orig.) [de

Comparison of the clinical outcomes between unattended home APAP and polysomnography manual titration in obstructive sleep apnea patients.

Science.gov (United States)

Wongsritrang, Krongthong; Fueangkamloon, Sumet

2013-09-01

To compare the clinical outcomes and determine the difference in therapeutic pressure between Automatic positive airway pressure (APAP) and polysomnography manual titration. Fifty patients of obstructive sleep apnea (OSA), moderate to severe cases, were randomized into two groups of intervention: 95-percentile pressure derived from APAP titration and an optimal pressure derived from manual titration. Clinical outcomes were assessed before and after four weeks. The average 95-percentile pressure derived from APAP titration was 11.7 +/- 0.3 cmH2O with median mask leak 1.3 L/min. The average optimal pressure derived from manual titration was 8.2 +/- 0.3 cmH2O. Pearson correlation analysis showed weak positive correlation (r = 0.336, p = 0.017). The Epworth Sleepiness Score (ESS), Quality of life tests: PSQI (Pittsburg Sleep Quality Index), and SF-36 (Medical Outcomes Study 36-Item Short-Form Health Survey) were improved significantly in both groups, but there were no statistical significant differences between groups. An APAP titration is an effective method of pressure determination for conventional CPAP therapy and shows no difference in clinical outcomes comparing the standard titration.

Potentiometric Determination of Ketotifen Fumarate in Pharmaceutical Preparations and Urine Using Carbon Paste and PVC Membrane Selective Electrodes

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Eman Y. Z. Frag

2011-01-01

Full Text Available This study compares between unmodified carbon paste (CPE; the paste has no ion pair and polyvinyl chloride (PVC membrane selective electrodes that were used in potentiometric determination of ketotifen fumarate (KTF, where sodium tetraphenylborate (NaTPB was used as titrant. The performance characteristics of these sensors were evaluated according to IUPAC recommendations which reveal a fast, stable, and linear response for KTF over the concentration range of 10−7 to 10−2 mol L−1. The electrodes show Nernstian slope value of 52.51±0.20 and 51.51±0.25 mV decade−1 for CPE and PVC membrane electrodes at 30∘C, respectively. The potential is nearly stable over the pH range 3.0–6.0 and 2.0–7.0 for CPE and PVC membrane electrodes, respectively. Selectivity coefficient values towards different inorganic cations, sugars, and amino acids reflect high selectivity of the prepared electrodes. The electrodes responses at different temperatures were also studied, and long operational lifetime of 12 and 5 weeks for CPE and PVC membrane electrodes, respectively, were found. These are used for determination of ketotifen fumarate using potentiometric titration, calibration, and standard addition methods in pure samples, its pharmaceutical preparations (Zaditen tablets, and biological fluid (urine. The direct potentiometric determination of KTF using the proposed sensors gave recoveries % of 98.97±0.53 and 98.62±0.74 with RSD 1.42 and 0.63% for CPE and PVC membrane selective electrodes, respectively. Validation of the method shows suitability of the proposed sensors for use in quality control assessment of KTF. The obtained results were in a good agreement with those obtained using the reported spectrophotometric method.

Potentiometric determination of ketotifen fumarate in pharmaceutical preparations and urine using carbon paste and PVC membrane selective electrodes.

Science.gov (United States)

Frag, Eman Y Z; Mohamed, Gehad G; Khalil, Mohamed M; Hwehy, Mohammad M A

2011-01-01

This study compares between unmodified carbon paste (CPE; the paste has no ion pair) and polyvinyl chloride (PVC) membrane selective electrodes that were used in potentiometric determination of ketotifen fumarate (KTF), where sodium tetraphenylborate (NaTPB) was used as titrant. The performance characteristics of these sensors were evaluated according to IUPAC recommendations which reveal a fast, stable, and linear response for KTF over the concentration range of 10(-7) to 10(-2) mol L(-1). The electrodes show Nernstian slope value of 52.51 ± 0.20 and 51.51 ± 0.25 mV decade(-1) for CPE and PVC membrane electrodes at 30°C, respectively. The potential is nearly stable over the pH range 3.0-6.0 and 2.0-7.0 for CPE and PVC membrane electrodes, respectively. Selectivity coefficient values towards different inorganic cations, sugars, and amino acids reflect high selectivity of the prepared electrodes. The electrodes responses at different temperatures were also studied, and long operational lifetime of 12 and 5 weeks for CPE and PVC membrane electrodes, respectively, were found. These are used for determination of ketotifen fumarate using potentiometric titration, calibration, and standard addition methods in pure samples, its pharmaceutical preparations (Zaditen tablets), and biological fluid (urine). The direct potentiometric determination of KTF using the proposed sensors gave recoveries % of 98.97 ± 0.53 and 98.62 ± 0.74 with RSD 1.42 and 0.63% for CPE and PVC membrane selective electrodes, respectively. Validation of the method shows suitability of the proposed sensors for use in quality control assessment of KTF. The obtained results were in a good agreement with those obtained using the reported spectrophotometric method.

Use of EDTA for potentiometric back titration of rare earths and analysis of their mixtures

International Nuclear Information System (INIS)

Zayed, M.A.; Rizk, M.S.; Khalifa, H.; Omer, W.F.

1987-01-01

Advantage was taken of the stoichiometric reaction between mercury(II), rare earths, alkaline earths, heavy metal ions and EDTA in urotropine buffered media to determine rare earths by back-titration of excess EDTA in the course of estimating a variety of lanthanides or analysing their binary mixture with one of the alkaline earth metals by selective control of pH; or analysing their binary mixtures with heavy metals using fluoride as a good masking agent for rare earths; or analysing their ternary mixtures with both heavy and alkaline earth metals in two steps, one by selective control of pH and the other by masking of rare earths with fluoride at lower pH to estimate the heavy metal. The procedures given are simple, rapid and extremely reliable. 19 refs. (author)

Potentiometric determination of uranium in the presence of plutonium in Hsub(2)SOsub(4) medium

International Nuclear Information System (INIS)

Gopinath, N.; Rama Rao, G.A.; Manchanda, V.K.; Natarajan, P.R.

1985-01-01

The potentiometric determination of uranium is widely carried out in phosphoric acid medium to suppress the interferences of plutonium by complexation. Owing to the complexity of the recycling plutonium from the phosphate based waste involving manifold stages of separation, a method is proposed which does not use phosphoric acid. Uranium and plutonium are reduced to U(IV) and Pu(III) in IM Hsub(2)SOsub(4) by Ti(III), and NaNOsub(2) is chosen to selectively oxidize Pu(III) and the excess of Ti(III). The unreacted NaNOsub(2) is destroyed by sulphamic acid and excess Fe(III) is added following dilution. The euqivalent amount of Fe(II) thus liberated is titrated against standard Ksub(2)Crsub(2)Osub(7). RSD obtained for the determination of uranium (1-2 mg) is 0.3% with plutonium present up to 4.0 mg. (author)

SHORT COMMUNICATION POTENTIOMETRIC DETERMINATION ...

African Journals Online (AJOL)

a

SHORT COMMUNICATION. POTENTIOMETRIC DETERMINATION OF K+ IONS USING A K+-SELECTIVE. ELECTRODE WITH MACROCYCLIC LIQUID MEMBRANE. Cezar Spinu*, Marian Isvoranu, Maria Pleniceanu and Cristian Tigae. Faculty of Chemistry, University of Craiova, A.I. Cuza 13, Craiova, Romania. (Received ...

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

Science.gov (United States)

Pehrsson, L; Ingman, F; Johansson, S

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

Development of novel redox systems in potentiometry and its application to analytical chemistry

OpenAIRE

Teshima, Norio

1996-01-01

Potentiometric methods (potentiometry) embrace two types of analyses. One is known as analysis by direct potentiometric measurement using a pH glass electrode and/or an ion-selective electrode. The other type is potentiometric titration. The latter method can be applied ...

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

Science.gov (United States)

Gaál, F F; Abramović, B F

1985-07-01

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

Highly Selective and Sensitized Spectrophotometric Determination of Iron (3) Following Potentiometric Study

International Nuclear Information System (INIS)

Shokrollahi, A.; Ghaedi, M.; Rajabi, H.R.

2007-01-01

A simple, selective and sensitized spectrophotometric method for determination of trace amounts of Fe 3+ ion in tap and waste water solutions has been described. The spectrophotometric determination of Fe 3+ ion using Ferron in the presence of N,N-Dodecy trimethylammonium bromide (DTAB) has been carried out. The Beer's law is obeyed over the concentration range of 0.05-2.6 μg mL -1 of Fe 3+ ion with the relative standard deviation (RSD %) 3 L mol -1 cm -1 . Potentiometric pH titration has been used for prediction of protonation constants of ferron, and evaluating its stoichiometry and respective stability constant with Fe 3+ ion. As it is obvious the most likely species of ferron alone and its complexes are LH (log=7.64), LH 2 (logK=10.52), LH 3 (logK=11.74) and ML 2 (logβ= 23.68), ML 3 (logβ23.68), ML 3 H (logβ= 23.68), ML 3 H 2 (logβ= 23.68) and ML(OH) 2 (logβ=23.68) respectively

Carbon Nanotubes-Based Potentiometric Bio-Sensors for Determination of Urea

Directory of Open Access Journals (Sweden)

Ewa Jaworska

2015-07-01

Full Text Available The possibility of using disposable plastic-carbon potentiometric sensors as enzyme biosensors was examined. Urease enzyme was immobilized on poly(vinyl chloride based H+- or NH4+-selective membranes using cellulose acetate. This approach has resulted in a potentiometric response on changing the pH of the solution or NH4+ ion content due to an enzymatic reaction that occurs between urease and urea. Both types of potentiometric biosensors for urea were characterized by good analytical parameters as high sensitivity and fast response time.

LIGHT TITRATIONS

Science.gov (United States)

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

1926-01-01

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

An investigation of the functional groups on the surface of activated carbons

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MARYTE DERVINYTE

2004-05-01

Full Text Available Activated carbons were produced in the laboratory from wood using a 20-run Plackett–Burman experimental design for 19 factors. The obtained batches of activated carbon were analysed by potentiometric titration and FTIR spectroscopy to determine the surface functional groups. The results obtained by potentiometric titration displayed the distribution of individual acidity constants of those groups in the pK range. Considering this parameter, the surface functional groups were divided into carboxyl, lactone and phenol. The linear regression equations reflecting the influence of each operation used for the synthesis on the amount of these functional groups in the obtained activated carbons were generated. The FTIR spectra were used in parallel for the evaluation of the amount and the type of the surface functional groups. Relationships between the two data sets obtained by potentiometric titration and FTIR spectroscopy were evaluated by correlation analysis. It was established that the amount of surface functional groups determined by potentiometric titration positively correlates with the intensity of the peaks of hydrophilic functional groups in the FTIR spectra. At the same time, the negative correlation between potentiometrically determined amount of surface functional groups and the intensity of peaks of hydrophobic functional groups was observed. Most probably, these non-polar formations can take part in the interaction of carbon surface with H+/OH- ions and diminish the strength of existent functional groups.

Effect of Grafted Hydroquinone on the Acid-Base Properties of Poly(acrylic acid in the Presence of Copper (II

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Nabila Bensacia

2015-01-01

Full Text Available Potentiometric titration of poly(acrylic acid and hydroquinone-functionalized poly(acrylic acid was conducted in the presence of copper (II. The effects of hydroquinone functionalizing and copper (II complexing on the potentiometric titration of poly(acrylic acid were studied in an ionic environment and in its absence. Henderson-Hasselbalch equation was applied to assess its validity for this titration. Coordination number and the stability constants of the copper- (II-complexed polymers were determined, and results showed the formation of mostly monodentate and bidentate copper- (II-polymer complexes.

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

Science.gov (United States)

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.

Potentiometric investigations of (acid+base) equilibria in (n-butylamine+acetic acid) systems in binary (acetone+cyclohexane) solvent mixtures

Energy Technology Data Exchange (ETDEWEB)

Czaja, MaIgorzata [Department of General Chemistry, University of Gdansk, Sobieskiego 18, 80-952 Gdansk (Poland); Kozak, Anna [Department of General Chemistry, University of Gdansk, Sobieskiego 18, 80-952 Gdansk (Poland); Makowski, Mariusz [Department of General Chemistry, University of Gdansk, Sobieskiego 18, 80-952 Gdansk (Poland); Chmurzynski, Lech [Department of General Chemistry, University of Gdansk, Sobieskiego 18, 80-952 Gdansk (Poland)]. E-mail: lech@chem.univ.gda.pl

2005-08-15

By using the potentiometric titration method, standard equilibrium constants have been determined of acid dissociation of molecular acid, K{sub a}(HA), cationic acid, K{sub a}(BH{sup +}), of anionic and cationic homoconjugation, K{sub AHA{sup -}}andK{sub BHB{sup +}}, respectively, and of molecular heteroconjugation, K{sub AHB} (K{sub BHA}), in (acid+base) systems without proton transfer consisting of n-butylamine and acetic acid in binary (acetone+cyclohexane) solvent mixtures. The results have shown that both the pK{sub a}(HA) and pK{sub a}(BH{sup +}), as well as lgK{sub AHA{sup -}} values change non-linearly as a function of composition of the solvent mixture. On the other hand, standard molecular heteroconjugation constants without proton transfer do not depend on the cyclohexane content in the mixture, i.e. on solvent polarity.

A Novel Potentiometric Sensor Based on 1,2-Bis(N’-benzoylthioureido)benzene and Reduced Graphene Oxide for Determination of Lead (II) Cation in Raw Milk

International Nuclear Information System (INIS)

Abraham, Abigail Asha; Rezayi, Majid; Manan, Ninie S.A.; Narimani, Leila; Rosli, Ahmad Nazmi Bin; Alias, Yatimah

2015-01-01

We have developed a highly sensitive and selective potentiometric PVC-membrane sensor for lead (II) cation. A glassy carbon electrode (GCE) was modified with synthesized 1,2-Bis(N’-benzoylthioureido) benzene (BBTB) as an ionophore and reduced graphene oxide (RGO), and this material was characterized by scanning electron microscopy. The sensor shows sensitive and highly selective response to Pb(II) ion with a linear range from 6.31 × 10 −8 to 3.98 × 10 −2 M, Nernstian slope of 30.37 ± 0.62 mV per decade and a detection limit of 2.51 × 10 −8 M. The proposed sensor could be used in a pH range of 4.0–8.0. Selectivity coefficients were determined for known common cations by applying the match potential method (MPM). The sensor was successfully applied to monitor Pb(II) in raw milk and in potentiometric titration of Pb 2+ ions. The structure of BBTB ligand and its complexation with some common cations were investigated by using quantum mechanical DFT calculations. Lead (II) cation showed prominent affinity to the BBTB carrier

Potentiometric studies on ternary complexes involving some divalent transition metal ions, gallic acid and biologically abundant aliphatic dicarboxylic acids in aqueous solutions

Directory of Open Access Journals (Sweden)

Abdelatty Mohamed Radalla

2015-06-01

Full Text Available Formation of binary and ternary complexes of the divalent transition metal ions, Cu2+, Ni2+, Co2+ and Zn2+ with gallic acid and the biologically important aliphatic dicarboxylic acids (adipic, succinic, malic, malonic, maleic, tartaric and oxalic acids were investigated by means of the potentiometric technique at 25 °C and I = 0.10 mol dm−3 NaNO3. The acid-base properties of the ligands were investigated and discussed. The acidity constants of gallic acid and aliphatic dicarboxylic acids were determined and used for determining the stability constants of the binary and ternary complexes formed in the aqueous medium under the above experimental conditions. The formation of the different 1:1 and 1:2 binary complexes and 1:1:1 ternary complexes are inferred from the corresponding potentiometric pH-metric titration curves. The ternary complex formation was found to occur in a stepwise manner. The stability constants of these binary and ternary systems were calculated. The values of Δ log K, percentage of relative stabilization (%R.S. and log X were evaluated and discussed. The concentration distribution of the various complex species formed in solution was evaluated and discussed. The mode of chelation of ternary complexes formed was ascertained by conductivity measurements.

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

Science.gov (United States)

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

2013-05-01

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

Thermometric titration of beta-aryl-alpha-mercaptopropenoic acids and determination of the stoichiometry of their metal complexes.

Science.gov (United States)

Izquierdo, A; Carrasco, J

1981-05-01

Automatic thermometric titration was applied to some beta-aryl-alpha-mercaptopropenoic acids and the stoichiometry of their complexes with several metal ions was investigated. The heats of neutralization of the mercapto-acids with sodium hydroxide and the heats of their reaction with metal ions were calculated.

Ionization constants by curve fitting: determination of partition and distribution coefficients of acids and bases and their ions.

Science.gov (United States)

Clarke, F H; Cahoon, N M

1987-08-01

A convenient procedure has been developed for the determination of partition and distribution coefficients. The method involves the potentiometric titration of the compound, first in water and then in a rapidly stirred mixture of water and octanol. An automatic titrator is used, and the data is collected and analyzed by curve fitting on a microcomputer with 64 K of memory. The method is rapid and accurate for compounds with pKa values between 4 and 10. Partition coefficients can be measured for monoprotic and diprotic acids and bases. The partition coefficients of the neutral compound and its ion(s) can be determined by varying the ratio of octanol to water. Distribution coefficients calculated over a wide range of pH values are presented graphically as "distribution profiles". It is shown that subtraction of the titration curve of solvent alone from that of the compound in the solvent offers advantages for pKa determination by curve fitting for compounds of low aqueous solubility.

Detecting Levels of Polyquaternium-10 (PQ-10) via Potentiometric Titration with Dextran Sulphate and Monitoring the Equivalence Point with a Polymeric Membrane-Based Polyion Sensor

OpenAIRE

Ferguson, Stephen A.; Wang, Xuewei; Meyerhoff, Mark E.

2016-01-01

Polymeric quaternary ammonium salts (polyquaterniums) have found increasing use in industrial and cosmetic applications in recent years. More specifically, polyquaternium-10 (PQ-10) is routinely used in cosmetic applications as a conditioner in personal care product formulations. Herein, we demonstrate the use of potentiometric polyion-sensitive polymeric membrane-based electrodes to quantify PQ-10 levels. Mixtures containing both PQ-10 and sodium lauryl sulfate (SLS) are used as model sample...

A potentiometric study of molecular heteroconjugation equilibria in (n-butylamine+acetic acid) systems in binary (acetonitrile +1,4-dioxane) solvent mixtures

International Nuclear Information System (INIS)

Czaja, Malgorzata; Makowski, Mariusz; Chmurzynski, Lech

2006-01-01

By using the potentiometric method the following quantities have been determined: acidity constants of molecular acid, K a (HA), of cationic acid, K a (BH + ), anionic and cationic homoconjugation constants, K AHA - and K BHB + , respectively, as well as molecular heteroconjugation constants, K AHB , in (n-butylamine+acetic acid) systems without proton transfer in binary (acetonitrile+1,4-dioxane), AN+D, solvent mixtures. The results of these measurements have shown that the magnitudes of the molecular heteroconjugation constants do not depend on the 1,4-dioxane content in the mixed solvent, i.e., on solvent polarity. It has also been found that in the (acid+base) systems without proton transfer, the manner of carrying out the titration (direct B+HA vs. reverse HA+B) does not affect the magnitudes of the molecular heteroconjugation constants

Functions of chalcogenide electrodes in solutions of complexing reagents and interfering ions

International Nuclear Information System (INIS)

Kiyanskij, V.V.

1990-01-01

The possibility to modify chalcogenide electrodes and their behaviour in solutions of complexing reagents for the development of new methods of potentiometric titration has been studied. It is shown that complexing reagents (EDTA, cupferron, 8-hydroxyquinoline, sodium dithiocarbaminate) and Cu(2), Hg(2) produce a strong effect on the functions of Ag, Cu, Cd, Pb - selective electrodes, which is used for titration of potential-determining and non-potential-determining ions ions (Sr 2+ , La 3+ etc.) and also for modification of sulfide-selecting electrode. A method of potentiometric titration of sulfates and chlorides with modified Cd- and Ag-selective electrodes is suggested

Determination of uranium in uranium metal, uranium oxides, and uranyl nitrate solutions by potentiometric titration

International Nuclear Information System (INIS)

Tucker, H.L.; McElhaney, R.J.

1983-01-01

A simple, fast method for the determination of uranium in uranium metal, uranium oxides, and uranyl nitrate solutions has been adapted from the Davies-Gray volumetric method to meet the needs of Y-12. One-gram duplicate aliquots of uranium metal or uranium oxide are dissolved in 1:1 HNO 3 and concentrated H 2 SO 4 to sulfur trioxide fumes, and then diluted to 100-mL volume. Duplicate aliquots are then weighed for analysis. For uranyl nitrate samples, duplicate aliquots containing between 50 and 150 mg of U are weighed and analyzed directly. The weighed aliquot is transferred to a Berzelius beaker; 1.5 M sulfamic acid is added, followed in order by concentrated phosphoric acid, 1 M ferrous sulfate, and (after a 30-second interval) the oxidizing reagent. After a timed 3-minute waiting period, 100 mL of the 0.1% vanadyl sulfate-sulfuric acid mixture is added. The sample is then titrated past its endpoint with standard potassium dichromate, and the endpoint is determined by second derivative techniques on a mV/weight basis

Analysis of Aircraft Fuels and Related Materials

Science.gov (United States)

1982-09-01

content by the Karl Fischer method . Each 2040 solvent sample represented a different step in a clean-up procedure conducted by Aero Propulsion...izes a potentiometric titration with alcoholic silver nitrate. This method has a minimum detectability of 1 ppm. It has a re- peatability of 0.1 ppm... Method 163-80, which util- izes a potentiometric titration with alcoholic silver nitrate. This method has a minimum detectability of 1 ppm and has a

Determination of vanadium

International Nuclear Information System (INIS)

Stepin, V.V.; Kurbatova, V.I.; Fedorova, N.D.

1980-01-01

Titrimetric and potentiometric methods of vanadium determination in ferrovanadium are developed. The essence of the titrimetric method using phenylanthranilic acid as indicator is in the following. Ferrovanadium weighed amount is dissolved in H 2 SO 4 , vanadium is oxidated by potassium permanganate to V(5) and is titrated by a solution of double salt of sulfuric Fe(2) and ammonium in the presence of indicator. Potentiometric titration is carried out using the same indicator [ru

Optimization and plutonium equilibrium

International Nuclear Information System (INIS)

Silver, G.L.

1976-01-01

The sequential simplex method has been used to estimate the extent of disproportionation of tetravalent plutonium in dilute acid. A method for simulating potentiometric titrations is proposed, and this method suggests that the stoichiometric end point and the inflection point may not always correspond in the potentiometric titration of plutonium. A possible characteristic equation for the nitrite-plutonium reaction is illustrated, and the method of proportional equations is extended to the iron-plutonium reaction

Potentiometric detection of silver (I) ion based on carbon paste electrode modified with diazo-thiophenol-functionalized nanoporous silica gel

International Nuclear Information System (INIS)

Zhang Ting; Chai Yaqin; Yuan Ruo; Guo Junxiang

2012-01-01

For the first time, triazene compound functionalized silica gel was incorporated into carbon paste electrode for the potentiometric detection of silver (I) ion. A novel diazo-thiophenol-functionalized silica gel (DTPSG) was synthesized, and the presence of DTPSG acted as not only a paste binder, but also a reactive material. The electrode with optimum composition, exhibited an excellent Nernstian response to Ag + ion ranging from 1.0 × 10 −6 to 1.0 × 10 −1 M with a detection limit of 9.5 × 10 −7 M and a slope of 60.4 ± 0.2 mV dec −1 over a wide pH range (4.0–9.0) with a fast response time (50 s) at 25 °C. The electrode also showed a long-time stability, high selectivity and reproducibility. The response mechanism of the proposed electrode was investigated by using AC impedance. Moreover, the electrode was successfully applied for the determination of silver ions in radiology films, and for potentiometric titration of the mixture solution of Cl − and Br − ions. - Highlights: ► Functionalized silica gels have become promising materials. ► This work is the first attempt to apply triazene functionalized silica gel. ► The Functionalized silica gels were used to detect silver. ► The response of the previously reported papers are compared with this work. ► The result indicates the proposed electrode is better than reported Ag + electrodes.

Caracterização ácido-base da superfície de espécies mistas da alga Spirulina através de titulação potenciométrica e modelo de distribuição de sítios discretos Acid base characterization of the surface of mixed species of algae Spirulin by potentiometric titration and discrete site distribution model

Directory of Open Access Journals (Sweden)

Elizabete C. de Lima

1999-09-01

Full Text Available Acid base properties of mixed species of the microalgae Spirulina were studied by potentiometric titration in medium of 0.01 and 0.10 mols L-1 NaNO3 at 25.0±0.10 C using modified Gran functions or nonlinear regression techniques for data fitting. The discrete site distribution model was used, permitting the characterization of five classes of ionizable sites in both ionic media. This fact suggests that the chemical heterogeneity of the ionizable sites on the cell surface plays a major role on the acid-base properties of the suspension in comparison to electrostatic effects due to charge-charge interactions. The total of ionizable sites were 1.75±0.10 and 1.86±0.20 mmolsg-1 in ionic media of 0.01 and 0.10 mols L-1 NaNO3, respectively. A major contribution of carboxylic groups was observed with an average 34 and 22% of ionizable sites being titrated with conditional pcKa of 4.0 and 5.4, respectively. The remaining 44% of ionizable sites were divided in three classes with averaged conditional pcKa of 6.9, 8.7 and 10.12, which may be assigned respectively to imidazolic, aminic, and phenolic functionalities.

Synthesis of nano-sized hydrogen phosphate-imprinted polymer in acetonitrile/water mixture and its use as a recognition element of hydrogen phosphate selective all-solid state potentiometric electrode.

Science.gov (United States)

Alizadeh, Taher; Atayi, Khalil

2018-02-01

Herein, a new recipe is introduced for the preparation of hydrogen phosphate ion-imprinted polymer nanoparticles (nano-IIP) in acetonitrile/water (63.5:36.5) using phosphoric acid as the template. The nano-IIP obtained was used as the recognition element of a carbon paste potentiometric sensor. The IIP electrode showed a Nernstian response to hydrogen phosphate anion; whereas, the non-imprinted polymer (NIP)-based electrode had no considerable sensitivity to the anion. The presence of both methacrylic acid and vinyl pyridine in the IIP structure, as well as optimization of the functional monomers-template proportion, was found to be important to observe the sensing capability of the IIP electrode. The nano-IIP electrode showed a dynamic linear range of 1 × 10 -5 -1 × 10 -1  mol L-1, Nernstian slope of 30.6 ± (0.5) mV decade -1 , response time of 25 seconds, and detection limit of 4.0 × 10 -6  mol L -1 . The utility of the electrodes was checked by potentiometric titration of hydrogen phosphate with La 3+ solution. Copyright © 2017 John Wiley & Sons, Ltd.

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

International Nuclear Information System (INIS)

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

Automated spectrophotometric bicarbonate analysis in duodenal juice compared to the back titration method.

Science.gov (United States)

Erchinger, Friedemann; Engjom, Trond; Gudbrandsen, Oddrun Anita; Tjora, Erling; Gilja, Odd H; Dimcevski, Georg

2016-01-01

We have recently evaluated a short endoscopic secretin test for exocrine pancreatic function. Bicarbonate concentration in duodenal juice is an important parameter in this test. Measurement of bicarbonate by back titration as the gold standard method is time consuming, expensive and technically difficult, thus a simplified method is warranted. We aimed to evaluate an automated spectrophotometric method in samples spanning the effective range of bicarbonate concentrations in duodenal juice. We also evaluated if freezing of samples before analyses would affect its results. Patients routinely examined with short endoscopic secretin test suspected to have decreased pancreatic function of various reasons were included. Bicarbonate in duodenal juice was quantified by back titration and automatic spectrophotometry. Both fresh and thawed samples were analysed spectrophotometrically. 177 samples from 71 patients were analysed. Correlation coefficient of all measurements was r = 0.98 (p titration gold standard. This is a major simplification of direct pancreas function testing, and allows a wider distribution of bicarbonate testing in duodenal juice. Extreme values for Bicarbonate concentration achieved by the autoanalyser method have to be interpreted with caution. Copyright © 2016 IAP and EPC. Published by Elsevier India Pvt Ltd. All rights reserved.

Complex formation between uranium(VI) and α-D-glucose 1-phosphate

International Nuclear Information System (INIS)

Koban, A.; Geipel, G.; Bernhard, G.

2003-01-01

The complex formation of uranium(VI) with α-D-glucose 1-phosphate (C 6 H 11 O 6 PO 3 2- , G1P) was determined by time-resolved laser-induced fluorescence spectroscopy (TRLFS) at pH 4 and potentiometric titration in the pH range from 3 to 10. Both measurements show the formation of a 1 : 1 complex at lower pH values. The formation constant of UO 2 (C 6 H 11 O 6 PO 3 ) was calculated from TRLFS measurements to be log β 11 = 5.72±0.12, and from potentiometric titration log β 11 = 5.40±0.25, respectively. It was found by potentiometric titration that at higher pH values the complexation changes to a 1 : 2 complex. The stability constant for this complex was calculated to be log β 12 = 8.96±0.18. (orig.)

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

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Kellermeier, Matthias; Cölfen, Helmut; Gebauer, Denis

2013-01-01

Despite the importance of crystallization for various areas of research, our understanding of the early stages of the mineral precipitation from solution and of the actual mechanism of nucleation is still rather limited. Indeed, detailed insights into the processes underlying nucleation may enable a systematic development of novel strategies for controlling mineralization, which is highly relevant for fields ranging from materials chemistry to medicine. In this work, we describe experimental aspects of a quantitative assay, which relies on pH titrations combined with in situ metal ion potentiometry and conductivity measurements. The assay has originally been designed to study the crystallization of calcium carbonate, one of the most abundant biominerals. However, the developed procedures can also be readily applied to any compound containing cations for which ion-selective electrodes are available. Besides the possibility to quantitatively assess ion association prior to nucleation and to directly determine thermodynamic solubility products of precipitated phases, the main advantage of the crystallization assay is the unambiguous identification of the different stages of precipitation (i.e., prenucleation, nucleation, and early postnucleation) and the characterization of the multiple effects of additives. Furthermore, the experiments permit targeted access to distinct precursor species and intermediate stages, which thus can be analyzed by additional methods such as cryo-electron microscopy or analytical ultracentrifugation (AUC). Regarding ion association in solution, AUC detects entities significantly larger than simple ion pairs, so-called prenucleation clusters. Sedimentation coefficient values and distributions obtained for the calcium carbonate system are discussed in light of recent insights into the structural nature of prenucleation clusters. © 2013 Elsevier Inc. All rights reserved.

Determination of hydroxide in the presence of aluminate using a modified potentiometric titration

International Nuclear Information System (INIS)

Hanson, T.J.

1975-11-01

A procedure for the determination of hydroxide concentration in the presence of aluminate and other interfering ions was developed using the method of standard additions (or more specifically in this case, standard subtractions). The procedure called for titration with a strong acid which was added in equal increments at regular time intervals. The potential was recorded after each addition of acid. The data was plotted on Gran's Plot Paper, which is based on work done originally by Gran, or it was entered into a computer to determine the equivalence volume of the titrant. When used on many different samples in different matrices, the method gave results that were approximately 100 +- 1 percent of the calculated value. This was shown to be true even in systems containing aluminate [Al(OH) 4 - ], phosphate (PO 4 3- ), sulfate (SO 4 2- ), nitrate (NO 3 - ), nitrite (NO 2 - ), carbonate (CO 3 2- ), and other ions. The effect of these ions was shown to be negligible if the initial OH - concentration was at least 10 -3 M and barium chloride (BaCl 2 ) was added to complex the PO 4 3- and CO 3 2- ions. These ions were checked at levels of up to 3 M for Al(OH) 4 - and NO 3 - , 2 M for NO 2 - , and 1 M for SO 4 2- , PO 4 3- , and CO 3 2- . The method is applicable to radioactive as well as nonradioactive samples and any heat involved with a radioactive sample is insufficient to cause an error in the determination. On the basis of the work performed it was shown that the method was general enough to be run on a routine basis

Fabrication of new carbon paste electrodes based on gold nano-particles self-assembled to mercapto compounds as suitable ionophores for potentiometric determination of copper ions

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Rasoul Pourtaghavi Talemi

2013-12-01

Full Text Available In the present study, we investigate the potentiometric behavior of Cu2+ carbon paste electrodes based on two mercapto compounds 2-ethylmino-5-mercapto-1,3,4-thiadiazole (EAMT and 2-acetylamino-5-mercapto-1,3,4-thiadiazole (AAMT self-assembled on gold nano-paricle (GNP as ionophore. Then, the obtained results from the modified electrodes are compared. The self-assembled ionophores exhibit a high selectivity for copper ion (Cu2+, in which the sulfur and nitrogen atoms in their structure play a significant role as the effective coordination donor site for the copper ion. Among these electrodes, the best performance was obtained with the sensor with a EAMT/graphite powder/paraffin oil weight ratio of 4.0/68/28 with 200 µL of GNP which exhibits the working concentration range of 1.6×10−9 to 6.3×10−2 M and a nernstian slope of 28.9±0.4 mVdecade−1 of copper(II activity. The detection limit of electrode was 2.9(±0.2×10−10M and potential response was pH ; in other words, it was independent across the range of 2.8–6.3. The proposed electrode presented very good selectivity and sensitivity towards the Cu2+ ions over a wide variety of cations including alkali, alkaline earth, transition and heavy metal ions. Moreover, the proposed electrode was successfully applied as an indicator electrode in the potentiometric titration of Cu(II ions with EDTA and also the potentiometric determination of copper ions in spiked water samples.

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

Science.gov (United States)

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

2017-04-01

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

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

Science.gov (United States)

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.

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

Science.gov (United States)

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.

Comparison of Potentiometric and Gravimetric Methods for Determination of O/U Ratio

International Nuclear Information System (INIS)

Farida; Windaryati, L; Putro Kasino, P

1998-01-01

Comparison of determination O/U ratio by using potentiometric and gravimetric methods has been done. Those methods are simple, economical and having high precision and accuracy. Determination O/U ratio for UO 2 powder using potentiometric is carried out by adopting the davies-gray method. This technique is based on the redox reaction of uranium species such as U(IV) and U(VI). In gravimetric method,the UO 2 power as a sample is calcined at temperature of 900 C, and the weight of the sample is measured after calcination process. The t-student test show that there are no different result significantly between those methods. However, for low concentration in the sample the potentiometric method has a highed precision and accuracy compare to the gravimetric method. O/U ratio obtained is 2.00768 ± 0,00170 for potentiometric method 2.01089 ± 0,02395 for gravimetric method

A potentiometric study of molecular heteroconjugation equilibria in (n-butylamine+acetic acid) systems in binary (acetonitrile +1,4-dioxane) solvent mixtures

Energy Technology Data Exchange (ETDEWEB)

Czaja, Malgorzata [Department of General Chemistry, University of Gdansk, Sobieskiego 18, 80-952 Gdansk (Poland); Makowski, Mariusz [Department of General Chemistry, University of Gdansk, Sobieskiego 18, 80-952 Gdansk (Poland); Chmurzynski, Lech [Department of General Chemistry, University of Gdansk, Sobieskiego 18, 80-952 Gdansk (Poland)]. E-mail: lech@chem.univ.gda.pl

2006-05-15

By using the potentiometric method the following quantities have been determined: acidity constants of molecular acid, K{sub a}(HA), of cationic acid, K{sub a}(BH{sup +}), anionic and cationic homoconjugation constants, K{sub AHA{sup -}} and K{sub BHB{sup +}}, respectively, as well as molecular heteroconjugation constants, K{sub AHB}, in (n-butylamine+acetic acid) systems without proton transfer in binary (acetonitrile+1,4-dioxane), AN+D, solvent mixtures. The results of these measurements have shown that the magnitudes of the molecular heteroconjugation constants do not depend on the 1,4-dioxane content in the mixed solvent, i.e., on solvent polarity. It has also been found that in the (acid+base) systems without proton transfer, the manner of carrying out the titration (direct B+HA vs. reverse HA+B) does not affect the magnitudes of the molecular heteroconjugation constants.

Development and validation of alternative methods by non-aqueous acid-base titration and derivative ultraviolet spectrophotometry for quantification of sildenafil in raw material and tablets

Directory of Open Access Journals (Sweden)

Taízia Dutra Silva

2017-04-01

Full Text Available Sildenafil citrate (SILC is a potent phosphodiesterase-5 inhibitor used for erectile dysfunction and pulmonary hypertension. This study shows two simple, fast and alternative analytical methods for SILC determination by non-aqueous titration and by derivative ultraviolet spectrophotometry (DUS in active pharmaceutical ingredient and/or dosage forms. The quantitation method of SILC active pharmaceutical ingredient by non-aqueous acid-base titration was developed using methanol as solvent and 0.1 mol/L of perchloric acid in acetic acid as titrant. The endpoint was potentiometrically detected. The non-aqueous titration method shows satisfactory repeatability and intermediate precision (RSD 0.70-1.09%. The neutralization reaction occurred in the stoichiometric ratio 1:1 in methanol. The determination of SILC active pharmaceutical ingredient or dosage forms by DUS was developed in the linear range from 10 to 40 µg/mL, in 0.01 mol/L HCl, using the first order zero-peak method at λ 256 nm. The DUS method shows selectivity toward tablets excipients, appropriate linearity (R2 0.9996, trueness (recovery range 98.86-99.30%, repeatability and intermediate precision in three concentration levels (RSD 1.17-1.28%; 1.29-1.71%, respectively. Therefore, the methods developed are excellent alternatives to sophisticated instrumental methods and can be easily applied in any pharmaceutical laboratory routine due to simple and fast executions.

Titration Curves: Fact and Fiction.

Science.gov (United States)

Chamberlain, John

1997-01-01

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

Evaluation of the results from uranium chemical analysis by potentiometric tritation method for safeguards utilization through intercomparison programs

International Nuclear Information System (INIS)

Araujo, R.M.S. de; Almeida, S.G. de; Bezerra, J.H.B.; Silva, S.P. da

1990-01-01

It was analysed three samples of uranium, two of them of UO 2 -powder, provided by IAEA and one of UO 2 (NO 3 ) 2 - solution, provided by ECN. The goal was to verify the accuracy and precision of the method used in the routine determinations carried out at the laboratories who participate of the intercomparison exercises. The method used in the analyses performed at Laboratorio de Salvaguardas of CNEN was the potentiometric titration of Davies and Gray/NBL. It was concluded that the precisions lied in the range suitable to finalities of safeguards which are of the order of 0,05% or better. The accuracies were suitable to these purposes too. The larger deviation in relation to the certified value was equal to 0,062 of uranion and the minor equal to 0,0117% of the element. These values are comparable to which obtained by the best international laboratories which carried out this kind of analyses. (author) [pt

Potentiometric surface of the Upper Floridan aquifer in the St. Johns River water management district and vicinity, Florida, September 2005

Science.gov (United States)

Kinnaman, Sandra L.

2006-01-01

This map depicts the potentiometric surface of the Upper Floridan aquifer in the St. Johns River Water Management District and vicinity for September 2005. Potentiometric contours are based on water-level measurements collected at 643 wells during the period September 12-28, 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 springflow. 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.

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

Science.gov (United States)

Kinnaman, Sandra L.; Dixon, Joann F.

2009-01-01

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

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

Science.gov (United States)

Kinnaman, Sandra L.; Dixon, Joann F.

2009-01-01

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

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

Science.gov (United States)

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.

Potentiometric surface of the upper Floridan Aquifer in the St. Johns River Water Management District and vicinity, Florida, September, 2004

Science.gov (United States)

Kinnaman, Sandra L.

2005-01-01

Introduction: This map depicts the potentiometric surface of the Upper Floridan aquifer in the St. Johns River Water Management District and vicinity in September 2004. Potentiometric contours are based on water-level measurements collected at 608 wells during the period September 14-October 1, near the end of the wet season. The shapes of some contours have been 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. 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.

Potentiometric Surface of the Upper Floridan Aquifer in the St. Johns River Water Management District and Vicinity, Florida, May 2005

Science.gov (United States)

Kinnaman, Sandra L.

2006-01-01

INTRODUCTION This map depicts the potentiometric surface of the upper Floridan aquifer in the St. Johns River Water Management District and vicinity for May 2005. Potentiometric contours are based on water level measurements collected at 598 wens during the period May 5 - 31, near the end of the dry season. Some contours are inferred from previous potentiometric-surface maps with larger well networks. The potentiometric surface of the carbonate upper Floridan aquifer responds mainly to rainfall, and more locally, to ground water withdrawals. 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.

Potentiometric Surface of the Upper Floridan Aquifer in the St. Johns River Water Management District and Vicinity, Florida, May, 2004

Science.gov (United States)

Kinnaman, Sandra L.; Knowles, Leel

2004-01-01

INTRODUCTION This map depicts the potentiometric surface of the Upper Floridan aquifer in the St. Johns River Water Management District and vicinity in May 2001. Potentiometric contours are based on water-level measurements collected at 684 wells during the period May 2 - 30, near the end of the dry season. The shapes of some contours have been 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. 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.

Potentiometric Surface of the Upper Floridan Aquifer in the St. Johns River Water Management District and Vicinity, Florida, May 2006

Science.gov (United States)

Kinnaman, Sandra L.

2006-01-01

Introduction: This map depicts the potentiometric surface of the Upper Floridan aquifer in the St. Johns River Water Management District and vicinity for May 2006. Potentiometric contours are based on water-level measurements collected at 599 wells during the period May 14-31, near the end of the dry season. Some contours are inferred from previous potentiometric-surface maps with larger well networks. The potentiometric surface of the carbonate Upper Floridan aquifer responds mainly to rainfall, and more locally, to ground-water withdrawals and springflow. 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.

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

Science.gov (United States)

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 (titration of Ho(3+) ion solutions in certified reference materials, alloy samples and for the determination of the fluoride ion in two mouthwash preparations. Copyright © 2012 Elsevier B.V. All rights reserved.

Carbon paste electrode modified with silver thimerosal for the potentiometric flow injection analysis of silver(I)

Energy Technology Data Exchange (ETDEWEB)

Ibrahim, Hosny [Chemistry Department, Faculty of Science, Cairo University, Cairo (Egypt)]. E-mail: dr_hosny@yahoo.com

2005-07-27

The utility of carbon paste electrode modified with silver ethylmercurythiosalicylate (silver thimerosal) in both static mode and flow injection analysis (FIA) is demonstrated. The electrode was fully characterized in terms of composition, response time, thermal stability, usable pH and ionic strength ranges. It has been shown that diisononyl phthalate (DINP) acts as more suitable solvent mediator for preparation of the electrode, which exhibits linear response range to Ag(I) extending from 5.0 x 10{sup -7} to 1.0 x 10{sup -3} M with detection limit of 2.5 x 10{sup -7} M and Nernstian slope of 59.3 {+-} 1.0 mV/decade. The proposed chemically modified carbon paste electrode shows a very good selectivity for Ag(I) over a wide variety of metal ions and successfully used for the determination of the silver content of silver sulphadiazine (burning cream) and developed radiological films. The electrode was also used as an indicator electrode in the potentiometric titration of thiopental and thimerosal with AgNO{sub 3}.

Potentiometric detection of silver (I) ion based on carbon paste electrode modified with diazo-thiophenol-functionalized nanoporous silica gel

Energy Technology Data Exchange (ETDEWEB)

Zhang Ting; Chai Yaqin, E-mail: yqchai@swu.edu.cn; Yuan Ruo; Guo Junxiang

2012-07-01

For the first time, triazene compound functionalized silica gel was incorporated into carbon paste electrode for the potentiometric detection of silver (I) ion. A novel diazo-thiophenol-functionalized silica gel (DTPSG) was synthesized, and the presence of DTPSG acted as not only a paste binder, but also a reactive material. The electrode with optimum composition, exhibited an excellent Nernstian response to Ag{sup +} ion ranging from 1.0 Multiplication-Sign 10{sup -6} to 1.0 Multiplication-Sign 10{sup -1} M with a detection limit of 9.5 Multiplication-Sign 10{sup -7} M and a slope of 60.4 {+-} 0.2 mV dec{sup -1} over a wide pH range (4.0-9.0) with a fast response time (50 s) at 25 Degree-Sign C. The electrode also showed a long-time stability, high selectivity and reproducibility. The response mechanism of the proposed electrode was investigated by using AC impedance. Moreover, the electrode was successfully applied for the determination of silver ions in radiology films, and for potentiometric titration of the mixture solution of Cl{sup -} and Br{sup -} ions. - Highlights: Black-Right-Pointing-Pointer Functionalized silica gels have become promising materials. Black-Right-Pointing-Pointer This work is the first attempt to apply triazene functionalized silica gel. Black-Right-Pointing-Pointer The Functionalized silica gels were used to detect silver. Black-Right-Pointing-Pointer The response of the previously reported papers are compared with this work. Black-Right-Pointing-Pointer The result indicates the proposed electrode is better than reported Ag{sup +} electrodes.

Potentiometric investigation of acid dissociation and anionic homoconjugation equilibria of substituted phenols in dimethyl sulfoxide[Substituted phenols; Acid-base equilibria; Dimethyl sulfoxide (DMSO); Potentiometry

Energy Technology Data Exchange (ETDEWEB)

Czaja, Malgorzata; Kozak, Anna; Makowski, Mariusz; Chmurzynski, Lech. E-mail: lech@chemik.chem.univ.gda.pl

2003-10-01

Standard acidity constants, K{sub a}{sup DMSO} (HA), expressed as pK{sub a}{sup DMSO} (HA) values, and anionic homoconjugation constants, K{sup DMSO}{sub AHA{sup -}}, (in the form of lg K{sup DMSO}{sub AHA{sup -}} values) have been determined for 11 substituted phenol-phenolate systems a polar protophilic aprotic solvent, dimethyl sulfoxide (DMSO) with a potentiometric titration. A linear relationship has been determined between lg K{sup DMSO}{sub AHA{sup -}} and pK{sub a}{sup DMSO} (HA). The tendency towards anionic homoconjugation in these systems increases with increasing pK{sub a}{sup DMSO} (HA) that is with declining phenol acidity. The pK{sub a}{sup DMSO} (HA) are correlated with both pK{sub a}{sup W} (HA) water and other polar non-aqeous solvents.

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

NARCIS (Netherlands)

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

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

Open-Source Low-Cost Wireless Potentiometric Instrument for pH Determination Experiments

Science.gov (United States)

Jin, Hao; Qin, Yiheng; Pan, Si; Alam, Arif U.; Dong, Shurong; Ghosh, Raja; Deen, M. Jamal

2018-01-01

pH determination is an essential experiment in many chemistry laboratories. It requires a potentiometric instrument with extremely low input bias current to accurately measure the voltage between a pH sensing electrode and a reference electrode. In this technology report, we propose an open-source potentiometric instrument for pH determination…

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

Energy Technology Data Exchange (ETDEWEB)

Liang, Jintao [School of Life and Environmental Sciences, Guilin University of Electronic Technology, Guilin, Guangxi 541004 (China); Guangxi Experiment Center of Information Sciences, Guilin University of Electronic Technology, Guilin, Guangxi 541004 (China); Guan, Mingyuan; Huang, Guoyin; Qiu, Hengming; Chen, Zhengcheng [School of Life and Environmental Sciences, Guilin University of Electronic Technology, Guilin, Guangxi 541004 (China); Li, Guiyin, E-mail: liguiyin01@163.com [School of Life and Environmental Sciences, Guilin University of Electronic Technology, Guilin, Guangxi 541004 (China); Guangxi Experiment Center of Information Sciences, Guilin University of Electronic Technology, Guilin, Guangxi 541004 (China); Huang, Yong, E-mail: huangyong503@126.com [School of Life and Environmental Sciences, Guilin University of Electronic Technology, Guilin, Guangxi 541004 (China); Guangxi Experiment Center of Information Sciences, Guilin University of Electronic Technology, Guilin, Guangxi 541004 (China)

2016-06-01

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

Development of destructive methods of burn-up determination and their application on WWER type nuclear fuels

International Nuclear Information System (INIS)

Hermann, A.; Stephan, H.; Nebel, D.

1984-03-01

Results are described of a cooperation between the Central Institute of Nuclear Research Rossendorf and the Radium Institute 'V.G. Chlopin' Leningrad in the field of destructive burn-up determination. Laboratory methods of burn-up determination using the classical monitors 137 Cs, 106 Ru, 148 Nd and isotopes of heavy metals (U, Pu) as well as the usefulness of 90 Sr, stable isotopes of Ru and Mo as monitors are dealt with. The analysis of the fuel components uranium (spectrophotometry, potentiometric titration, mass-spectrometric isotope dilution) and plutonium (spectrophotometry, coulometric titration, mass- and alpha-spectrometric isotope dilution) is fully described. Possibilities of increasing the reproducibility (automatic adjusting of measurement conditions) and the sensibility (ion impuls counting) of mass-spectrometric measurements are proposed and applied to a precise determination of Am and Cm isotopic composition. The methods have been used for burn-up analysis of spent WWER (especially WWER-440) fuel. (author)

Chemical processes at the surface of various clays on acid-base titration

International Nuclear Information System (INIS)

Park, K. K.; Park, Y. S.; Jung, E. C.

2010-01-01

The chemical reaction of radionuclides at the interface between groundwater and geological mineral is an important process determining their retardation of transport through groundwater flow in a nuclear waste disposal. Clay minerals are major components of soil and argillaceous rock, and some of them are considered to be important base materials in the design of high-level nuclear waste repository due to their large swelling, low-permeability, large surface area, and strong and large sorption of radionuclides. Clay materials are phyllosilicates containing accessory minerals such as metal oxides, hydroxides, oxyhydroxides. Their structures are condensed 1:1 or 2:1 layers of tetrahedral SiO 3/2 OH and octahedral Al(OH) 6/2 sheets. An accurate knowledge about the properties of clay surface is required as a parameter for a long-term estimation of radionuclide retardation effects. Electric surface charge is a primary property determining ion exchange and surface complexation of radionuclides on its surface. The sources of electric surface charge are a permanent structural negative charge on a basal plane and a dissociable charge at an edge surface. Investigation of proton sorption is a prerequisite to the understanding of radionuclide sorption. The reactions on a permanently charged site and on an edge site are measured by an electrokinetic measurement and by potentiometric titration, respectively. However, side reactions such as complexation, proton/cation exchange, dissolution, hydrolysis, precipitation and re adsorption, and the reaction of secondary minerals hinder an experimental measurement of accurate acid-base properties. This presentation describes the pH change on dispersing various clays in water and adding acid, base or Eu(III) ion to these solutions, and the effect of Eu(III) ion on acid-base titration of clay solutions

Chemical processes at the surface of various clays on acid-base titration

Energy Technology Data Exchange (ETDEWEB)

Park, K. K.; Park, Y. S.; Jung, E. C. [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of)

2010-10-15

The chemical reaction of radionuclides at the interface between groundwater and geological mineral is an important process determining their retardation of transport through groundwater flow in a nuclear waste disposal. Clay minerals are major components of soil and argillaceous rock, and some of them are considered to be important base materials in the design of high-level nuclear waste repository due to their large swelling, low-permeability, large surface area, and strong and large sorption of radionuclides. Clay materials are phyllosilicates containing accessory minerals such as metal oxides, hydroxides, oxyhydroxides. Their structures are condensed 1:1 or 2:1 layers of tetrahedral SiO{sub 3/2}OH and octahedral Al(OH){sub 6/2} sheets. An accurate knowledge about the properties of clay surface is required as a parameter for a long-term estimation of radionuclide retardation effects. Electric surface charge is a primary property determining ion exchange and surface complexation of radionuclides on its surface. The sources of electric surface charge are a permanent structural negative charge on a basal plane and a dissociable charge at an edge surface. Investigation of proton sorption is a prerequisite to the understanding of radionuclide sorption. The reactions on a permanently charged site and on an edge site are measured by an electrokinetic measurement and by potentiometric titration, respectively. However, side reactions such as complexation, proton/cation exchange, dissolution, hydrolysis, precipitation and re adsorption, and the reaction of secondary minerals hinder an experimental measurement of accurate acid-base properties. This presentation describes the pH change on dispersing various clays in water and adding acid, base or Eu(III) ion to these solutions, and the effect of Eu(III) ion on acid-base titration of clay solutions

Potentiometric Surface of the Upper Floridan Aquifer in the St. Johns River Water Management District and Vicinity, Florida, September 2006

Science.gov (United States)

Kinnaman, Sandra L.; Dixon, Joann F.

2007-01-01

Introduction This map depicts the potentiometric surface of the Upper Floridan aquifer in the St. Johns River Water Management District and vicinity for September 2006. Potentiometric contours are based on water-level measurements collected at 571 wells during the period September 11-29, near the end of the wet season. Some contours are inferred from previouspotentiometric-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.

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

Science.gov (United States)

Kinnaman, Sandra L.; Dixon, Joann F.

2007-01-01

Introduction This map depicts the potentiometric surface of the Upper Floridan aquifer in the St. Johns River Water Management District and vicinity for May 2007. Potentiometric contours are based on water-level measurements collected at 566 wells during the period May 4-June 11 near the end of the dry season, however most of the water level data for this map were collected by the U.S. Geological Survey during the period May 21-25, 2007. 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.

Derivatives of imidopyrophosphoric acids as extractants. Part I. The preparation and fundamental constants of tetraalkylimidopyrophosphoric acids

International Nuclear Information System (INIS)

Preez, J.G.H. du; Knabl, K.U.; Krueger, L.; Brecht, B.J.A.M. van

1992-01-01

Improved methods for the preparation of imidotetraalkylpyrophosphates are reported. The dissociation constant of the water soluble tetraethyl analogue was determined by potentiometric titration. The values for the partition constant and aggregation constant of the tetradodecyl analogue were determined by two phase EMF potentiometric titration of which the data were processed through a sophisticated general optimization technique. The application of this method also made it possible to obtain a species distribution curve of the organic phase in terms of variation of pH in the aqueous phase. 17 refs., 7 figs., 4 tabs

Risks and Benefits of Rapid Clozapine Titration.

Science.gov (United States)

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

2016-05-18

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

Risks and benefits of rapid clozapine titration

Directory of Open Access Journals (Sweden)

Jeannie D. Lochhead

2016-05-01

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

A novel, fast responding, low noise potentiometric sensor containing a carbon-based polymeric membrane for measuring surfactants in industrial and environmental applications.

Science.gov (United States)

Samardžić, Mirela; Galović, Olivera; Hajduković, Mateja; Sak-Bosnar, Milan

2017-01-01

A new high-sensitivity potentiometric sensor for anionic surfactants was fabricated using the dimethyldioctadecylammonium-tetraphenylborate (DDA-TPB) ion associate as an ionophore that was incorporated into a liquid PVC membrane. Carbon powder was used for immobilization of the ionophore in the membrane, thus significantly reducing its ohmic resistance and reducing its signal drift. The sensor exhibits a sub-Nernstian response for both dodecylbenzenesulfonate (DBS) and dodecyl sulfate (DS) in H 2 O (55.3 and 58.5mV/decade of activity, respectively) in a range between 3.2×10 -7 and 4.6×10 -3 M for DS and 2.5×10 -7 and 1.2×10 -3 M for DBS. The sensor also exhibited a sub-Nernstian response for DS and DBS in 10mM Na 2 SO 4 (55.4 and 57.7mV/decade of activity, respectively) between 2.5×10 -7 and 4.6×10 -3 M for DS and 1.5×10 -7 and 8.8×10 -4 M for DBS. The detection limits for DS and DBS in H 2 O were 2.5×10 -7 and 2.0×10 -7 M and in 10mM Na 2 SO 4 the detection limits were 2.5×10 -7 and 1.2×10 -7 M, respectively. The response time of the sensor was less than 5s for changes at higher concentration levels (above 1×10 -4 M) in both water and 10mM Na 2 SO 4. At lower concentrations (below 1×10 -5 M) the response times were 8 and 6s in water and 10mM Na 2 SO 4 , respectively. The signal drift of the sensor was 1.2mV/hour. The new carbon-based sensor exhibited excellent selectivity performance for DS over almost all of the anions commonly present in commercial formulations and it was successfully employed as an end-point detector in potentiometric titrations of anionic surfactants in a pH range from 3 to 12. Three-component mixtures containing sodium alkanesulfonate (C 10 , C 12 and C 14 ) were successfully differentially titrated. Copyright © 2016 Elsevier B.V. All rights reserved.

Potentiometric-surface map, 1993, Yucca Mountain and vicinity, Nevada

International Nuclear Information System (INIS)

Tucci, P.; Burkhardt, D.J.

1995-01-01

The revised potentiometric surface map here, using mainly 1993 average water levels, updates earlier maps of this area. Water levels are contoured with 20-m intervals, with additional 0.5-m contours in the small-gradient area SE of Yucca Mountain. Water levels range from 728 m above sea level SE of Yucca to 1,034 m above sea level north of Yucca. Potentiometric levels in the deeper parts of the volcanic rock aquifer range from 730 to 785 m above sea level. The potentiometric surface can be divided into 3 regions: A small gradient area E and SE of Yucca, a moderate-gradient area on the west side of Yucca, and a large-gradient area to the N-NE of Yucca. Water levels from wells at Yucca were examined for yearly trends (1986-93) using linear least-squares regression. Of the 22 wells, three had significant positive trends. The trend in well UE-25 WT-3 may be influenced by monitoring equipment problems. Tends in USW WT-7 and USW WTS-10 are similar; both are located near a fault west of Yucca; however another well near that fault exhibited no significant trend

Potentiometric determination of iodides in urine

International Nuclear Information System (INIS)

Gikolaev, B.A.; Primakova, L.N.; Rakhman'ko, E.M.

1996-01-01

Variants of potentiometric method: determination using a calibrations plot, the Gran method, and the double addition method are considered. The method of double additions of the test solution to the reference one is suggested as the most favorable method of determining iodides in urine under clinical laboratory conditions. Refs. 5, tabs. 2

[Titration comparative study of TOPINA Tablets in patients with localization related epilepsy: double-blind comparative study by rapid and slow titration methods].

Science.gov (United States)

Kaneko, Sunao; Inoue, Yushi; Sasagawa, Mutsuo; Kato, Masaaki

2012-04-01

To compare the tolerability and efficacy of two titration methods (rapid and slow titration) for TOPINA Tablets with different dosages and periods of escalation, a double-blind comparative study was conducted in patients with localization-related epilepsy. A total of 183 patients were randomized to either rapid titration (initial dosage 100 mg/day increased by 100-200 mg at weekly intervals) or to slow titration (initial dosage 50 mg/day increased in 50 mg/day increments at weekly intervals). TOPINA Tablets were administered for 12 weeks to the maximum dosage of 400 mg/day. The incident of adverse events leading to treatment interruptions or withdrawals was 18.9% in rapid titration and 14.8% in slow titration, with no statistical significance (p = 0.554). The incident of adverse events and adverse reactions of slow titration was slightly lower than that of rapid titration. The common adverse events and adverse reactions reported in the two titration methods were comparable and were well tolerated. On the other hand, the efficacy of slow titration, percent reduction in seizure rate and responder rate, was comparable with that of rapid titration. In conclusion, there were no significant differences of therapeutic response to TOPINA Tablets between the two titration methods.

An estimated potentiometric surface of the Death Valley region, Nevada and California, developed using geographic information system and automated interpolation techniques

International Nuclear Information System (INIS)

D'Agnese, F.A.; Faunt, C.C.; Turner, A.K.

1998-01-01

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

Coulometric titration at low temperatures-nonstoichiometric silver selenide

OpenAIRE

Beck, Gesa K.; Janek, Jürgen

2003-01-01

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

On rhenium (7) state in aqueous solutions

International Nuclear Information System (INIS)

Sinyakova, G.S.

1979-01-01

The methods of spectrophotometry, electric conductivity and potentiometric titration have been used in studying the interaction in the system Re(7)-H 3 O + -H 2 O. It has been found that sodium perrhenate and perrhenic acid dissociate on dilution but not the way typical of binary electrolytes. Perrhenic acid is a mixture of the acids HReO 4 and H 5 ReO 6 . The two acids do not undergo differential titration. The conventional ionization constant, as calculated from the data of potentiometric titration, K 1 =(2.34+-0.52)x10 -2 . A step-wise dissociation of the H 4 ReO 6 - anion has been found, K 2 =(2.04+-0.30)x10 -8 , K 3 =(4.90+-0.20)x10 -12

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

Science.gov (United States)

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

2016-12-01

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

Comparison of Efficacy and Tolerance of Automatic Continuous Positive Airway Pressure Devices With the Optimum Continuous Positive Airway Pressure.

Science.gov (United States)

Tommi, George; Aronow, Wilbert S; Sheehan, John C; McCleay, Matthew T; Meyers, Patrick G

Patients diagnosed with obstructive sleep apnea syndrome were randomly placed on automatic continuous positive airway pressure (ACPAP) for 2 hours followed by manual titration for the rest of the night. One hundred sixty-one patients entered the study, with at least 50 patients titrated with each of 3 ACPAP devices. The optimum continuous positive airway pressure (CPAP) was defined as the lowest pressure with an apnea-hypoxia index of ≤5/hr, which ranged from 4 cm to 18 cm. Success with ACPAP was approximately 60%-80% when the optimum CPAP was 4-6 cm but fell to below 30% if the optimum CPAP was ≥8 cm (P = 0.001). Average ACPAP ranged from 2 to 10 cm below the optimum level if the optimum CPAP was ≥8 cm. Patients who responded to a low CPAP but deteriorated on higher pressures failed to respond to any of the automatic devices. We recommend that CPAP titration be performed manually before initiation of ACPAP in patients with obstructive sleep apnea. The basal pressure for ACPAP should be the optimum pressure obtained by manual titration. Limits on the upper level of ACPAP may be necessary for patients who deteriorate on higher positive pressures.

Determination of the O/U ratio in uranium dioxide pellets

International Nuclear Information System (INIS)

Kuvik, V.; Krtil, J.; Moravec, A.

1982-01-01

The potentiometric titration method for the determination of the O/U ratio in pellets is verified. The sample is dissolved in purified conc. phosphoric acid at increased pressure and temperature under argon atmosphere. U(VI) content is determined by bipotentiometric titration with ferrous ions. An automated recording of titration curves is performed. The precision and the accuracy of analysis are estimated. (author)

Potentiometric studies on quaternary complexes of dioxouranium(VI)

Energy Technology Data Exchange (ETDEWEB)

Kumari, Vinod; Chaturvedi, G K [Agra Coll., (India). Chemical Laboratories

1979-10-01

The formation of quaternary complexes of dioxouranium(VI) with three different organic acids (OX, MALN and SA, SSA, TAR or TMA) has been inferred from the potentiometric studies. The formation constants for the resulting triligand complexes have been evaluated.

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

Science.gov (United States)

Kinnaman, Sandra L.; Dixon, Joann F.

2008-01-01

This map depicts the potentiometric surface of the Upper Floridan aquifer in the St. Johns River Water Management District and vicinity for May 2008. Potentiometric contours are based on water-level measurements collected at 567 wells during the period May 6-May 27, near the end of the dry season. Some contours are inferred from previous potentiometric-surface maps with larger well networks. The potentiometric surface of the carbonate Upper Floridan aquifer responds mainly to rainfall, and more locally, to ground-water withdrawals and spring flow. Potentiometric-surface highs generally correspond to topographic highs where the aquifer is recharged. Springs and areas of diffuse upward leakage naturally discharge water from the aquifer and are most prevalent along the St. Johns River. Areas of discharge are reflected by depressions in the potentiometric surface. Ground-water withdrawals locally have lowered the potentiometric surface. Ground water in the Upper Floridan aquifer generally flows from potentiometric highs to potentiometric lows in a direction perpendicular to the contours. Measured values of the potentiometric surface ranged from 7 feet below NGVD29 near Fernandina Beach, Florida, to 124 feet above NGVD29 in Polk County, Florida. The average water level of the network in May 2008 was about 1 foot lower than the average in September 2007 following below-average rainfall during the dry season of 2007-08. Seasonal differences in network average water levels generally range from 4 to 6 feet. For 457 wells with previous measurements, May 2008 levels ranged from about 19 feet below to about 11 feet above September 2007 water levels. The average water level of the network in May 2008 was about 1 foot higher than the average in May 2007. For 544 wells with previous measurements, May 2008 levels ranged from about 8 feet below to about 13 feet above May 2007 water levels. Long-term hydrographs of ground-water levels for continuous and periodic wells are available

Up-titration of allopurinol in patients with gout.

Science.gov (United States)

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

2014-08-01

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

Urea potentiometric enzymatic biosensor based on charged biopolymers and electrodeposited polyaniline.

Science.gov (United States)

Lakard, Boris; Magnin, Delphine; Deschaume, Olivier; Vanlancker, Guilhem; Glinel, Karine; Demoustier-Champagne, Sophie; Nysten, Bernard; Jonas, Alain M; Bertrand, Patrick; Yunus, Sami

2011-06-15

A potentiometric biosensor based on urease was developed for the quantitative determination of urea concentration in aqueous solutions for biomedical applications. The urease was either physisorbed onto an electrodeposited polyaniline film (PANI), or immobilized on a layer-by-layer film (LbL) assembled over the PANI film, that was obtained by the alternate deposition of charged polysaccharides (carboxymethylpullulan (CMP) and chitosan (CHI)). In the latter case, the urease (Urs) enzyme was either physically adsorbed or covalently grafted to the LbL film using carbodiimide coupling reaction. Potentiometric responses of the enzymatic biosensors were measured as a function of the urea concentration in aqueous solutions (from 10(-6) to 10(-1) mol L(-1) urea). Very high sensitivity and short response time were observed for the present biosensor. Moreover, a stability study showed a higher stability over time for the potentiometric response of the sensor with the enzyme-grafted LbL film, testifying for the protective nature of the polysaccharide coating and the interest of covalent grafting. Copyright © 2011 Elsevier B.V. All rights reserved.

Complexação da tetraciclina, da oxitetraciclina e da clortetraciclina com o catião cobre (II. Estudo potenciométrico Tetracycline, oxytetracycline and chlortetracycline complexation with copper (II. Potentiometric study

Directory of Open Access Journals (Sweden)

Cristina M. C. M. Couto

2000-08-01

Full Text Available Stability constants of complexes formed by copper (II with three different tetracyclines (tetracycline, oxytetracycline and chlortetracycline have been determined potentiometrically with an automatic system in aqueous medium at 25,0 ± 0,2 ºC and I = 0,1 mol L-1 NaNO3. The protonation constants of the three tetracyclines were also determined under the same conditions. The distribution of the complexes was then simulated at therapeutic levels of the drugs.

Non-aqueous titration of hydroxamic acids.

Science.gov (United States)

Stamey, T W; Christian, R

1966-01-01

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

Improving the limits of detection in potentiometric sensors

NARCIS (Netherlands)

Bent, Van Der J.F.; Puik, E.C.N.; Tong, H.D.; Rijn, Van C.J.M.

2015-01-01

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

Creation of Vapor/Gas Impermeable Coatings for CB Hardening of Existing Structures

Science.gov (United States)

2013-04-05

Standard Test Method for Hydroxyl Groups Using Reaction with p-Toluenesulfonyl Isocyanate and Potentiometric Titration with Tetrabutylammonium...setup The structures of some resins produced as a result of the syntheses were confirmed by titration of their reactive terminal groups. This work...was conducted on a Mettler-Toledo DL-55 titrator . It must be noted that, as all the produced resins were new compounds that had never been

Fulltext PDF

Indian Academy of Sciences (India)

classroom discussion emphasizes the effect of titrated volume in potentiometric titrations. Nature Watch has always been the most popular section and, here Sindhu Radhakrishna traces the social behaviour of the slender Loris, a nocturnal prosimian found in India. She recounts the story of the various perils which threaten ...

Determination of substances by radiothermometric titration

International Nuclear Information System (INIS)

Tolgyessy, J.; Lesny, J.

1976-01-01

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

Investigation into transformations of Ru(4) and Os(4) hexafluorocomplexes in aqueous solutions

International Nuclear Information System (INIS)

Shipachev, V.A.; Zemskov, S.V.

1982-01-01

Using the methods of spectrophotometry, 19 NMR and potentiometric titration the study of activation processes of hexafluorocomplexes [RuF 6 ] 2- and Cl - ion substitution for F - in them is carried out. It is shown that Cl - substitution for F - in [RuF 6 ] 2 is limited by the stage of replacement of the first fluorine in the inner sphere, and intermediate mixed forms are less stable. Hydrolytic interactions with formation of polymer oxohydroxofluoride ions in solutions are of great importance in the chemistry of the compounds. The data of potentiometric titration of [RuF 6 ] 2- solutions with reducers point to the formation of Ru(3) aquohydroxocomplexes of indefinite composition

Propriedades ácido-base e de complexação de ácidos húmico e fúlvico isolados de vermicomposto Acid/base and complexation properties of humic and fulvic acids isolated from vermicompost

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Sandro de Miranda Colombo

2007-10-01

Full Text Available Proton binding properties of humic and fulvic acids were studied by potentiometric titration. Carboxylic groups were the predominant ionizable sites in comparison to phenolic and amine groups. Total acidity of fulvic acid was 12 x 10-3 mol g-1, a number significantly higher than that obtained for humic acid (5.2 x 10-3 mol g-1. Copper ion binding was evaluated at pH 4, 5 and 6 by potentiometric titration with an ion selective electrode for Cu(II. Differential stability constants and complexation capacities were systematically higher for humic acid, despite its lower number of ionizable sites in comparison with fulvic acid.

Potentiometric-level monitoring program, Mississippi and Louisiana: Annual status report for fiscal year 1985

International Nuclear Information System (INIS)

1986-10-01

Potentiometric-level data presented in this report were collected at 82 wells in Mississippi and Louisiana from October 1984 through September 1985. These wells are located near Richton and Cypress Creek Domes in Mississippi and Vacherie dome in Louisiana. Three wells were reinstated to the program during this period. Two previously destroyed wells were deleted from the program. Protective barriers were installed around 26 shallow borings in Mississippi. Cursory analysis of the data in Mississippi indicated minimal, if any, change in potentiometric level during the past year in the Citronelle, Hattiesburg, Cockfield, Sparta, and Wilcox Formations. A slight decline, on the order of 0.3 meter (1 foot), occurred during the past year in well MCCG-1, which is screened in the caprock of Cypress Creek Dome. The potentiometric level in well MRIG-9, in the caprock of Richton Dome, stabilized during fiscal year 1985 following 5 years of increase. The Catahoula Formation experienced a continuing decline of about 0.3 meter/year (1 foot/year). Well MH-5C, screened in the Cook Mountain Formation, showed a continuing, long-term, upward trend on the order of 1.5 meters (4.9 feet) during the past year. The potentiometric level of well MH-8C, screened in the Cook Mountain Formation, stabilized during fiscal year 1985, following 5 years of large annual increases. Wells screened in the Austin Formation in Louisiana showed a downward trend of 0.3 to 1 meter (1 to 3.3 feet) during fiscal year 1985. Other formations in Louisiana generally showed no change in potentiometric level

A Tabular Approach to Titration Calculations

Science.gov (United States)

Lim, Kieran F.

2012-01-01

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

Anion binding in the C3v-symmetric cavity of a protonated tripodal amine receptor: potentiometric and single crystal X-ray studies.

Science.gov (United States)

Bose, Purnandhu; Ravikumar, I; Ghosh, Pradyut

2011-11-07

Tris(2-aminoethyl)amine (tren) based pentafluorophenyl-substituted tripodal L, tris[[(2,3,4,5,6-pentafluorobenzyl)amino]ethyl]amine receptor is synthesized in good yield and characterized by single crystal X-ray diffraction analysis. Detailed structural aspects of binding of different anionic guests toward L in its triprotonated form are examined thoroughly. Crystallographic results show binding of fluoride in the C(3v)-symmetric cavity of [H(3)L](3+) where spherical anion fluoride is in tricoordinated geometry via (N-H)(+)···F interaction in the complex [H(3)L(F)]·[F](2)·2H(2)O, (3). In the case of complexes [H(3)L(OTs)]·[OTs](2), (4) and [H(3)L(OTs)]·[NO(3)]·[OTs], (5), tetrahedral p-toluenesulphonate ion is engulfed in the cavity of [H(3)L](3+) via (N-H)(+)···O interactions. Interestingly, complex [(H(3)L)(2)(SiF(6))]·[BF(4)](4)·CH(3)OH·H(2)O, (6) shows encapsulation of octahedral hexafluorosilicate in the dimeric capsular assembly of two [H(3)L](3+) units, via a number of (N-H)(+)···F interactions. The kinetic parameters of L upon binding with different anions are evaluated using a potentiometric study in solution state. The potentiometric titration experiments in a polar protic methanol/water (1:1 v/v) binary solvent system show high affinity of the receptor toward more basic fluoride and acetate anions, with a lesser affinity for other inorganic anions (e.g., chloride, bromide, nitrate, sulfate, dihydrogenphosphate, and p-toluenesulphonate). © 2011 American Chemical Society

Automated titration method for use on blended asphalts

Science.gov (United States)

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

2012-08-07

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

Quantitative determination of americium and curium in solutions using potassium tungstophosphate

International Nuclear Information System (INIS)

Chistyakov, V.M.; Baranov, A.A.; Erin, E.A.; Timoaeev, G.A.

1990-01-01

Two methods of americium (4) and curium (4) titration-replacement and redox ones - have been considered. According to the replacement method thorium nitrate solution was used as a titrant and the final point of titration was determined spectophotometrically. Using the method developed, on the basis of experimental data, the composition of thorium (4) complex with potassium tungstophosphate was determined. In case of the redox titration sodium nitrite was used, and the final titration point was indicated either spectrophotometrically or potentiometrically

A Porphyrin Based Potentiometric Sensor for Zn2+ Determination

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H. Lang

2003-07-01

Full Text Available PVC based membranes of disodium salt of porphyrin 3,7,12,17-tetramethyl-8, 13-divinyl 2,18-porphine dipropionic acid (I as ionophore with sodium tetra phenyl borate (NaTPB as anion excluder and dibutyl phthalate (DBP, dioctyl phthalate (DOP, dibutyl butyl phosphonate (DBBP, tris(2- ethyl hexylphosphate (TEP, tri-n-butylphosphate (TBP and 1- chloronaphthalene (CN as plasticizing solvent mediators were prepared and constructed for determination of Zn(II. The PVC based membrane of (I with DBBP as plasticizer and having anion excluder, NaTPB in the ratio PVC: I: NaTPB: DBBP (150: 10: 2: 200 gave the best results in terms of working concentration range (1.3×10-5-1.0 ×10-1M with a Nernstian slope (30.0 mV/decade of activity. The useful pH range of the sensor is 3.0 –7.4, beyond which a drift in potential was observed. The response time of the sensor is 10s and the lifetime was about 2 months during which it could be used without any measurable divergence. It had good stability and reproducibility. The membrane worked satisfactorily in non-aqueous medium up to 40% (v/v non-aqueous content. The selectivity coefficient values indicate that the electrode is highly selective for Zn2+ over a number of other cations except Na+ and Cd2+. Although Na+ and Cd2+ are likely to cause some interference, they would not interfere if present at the concentrations < 1 ×10-5 and < 5 ×10-5 M, respectively. The electrode has been used as an indicator electrode to determine the end point in the potentiometric titration of Zn2+ with EDTA.

PVC-Membrane Potentiometric Electrochemical Sensor Based on 2-(4-Oxopentan-2-ylideneaminoisoindoline-1,3-dione for Selective Determination of Holmium(III

Directory of Open Access Journals (Sweden)

Hassan Ali Zamani

2011-01-01

Full Text Available 2-(4-Oxopentan-2-ylideneamino isoindoline-1,3-dione (OID was found to be a suitable neutral ionophore in the fabrication of a highly selective Ho3+ membrane sensor. The electrode has a near-Nernstian slope of 19.6±0.5 mV per decade with a wide concentration range between 1.0×10-6 and 1.0×10-2 mol/L in the pH range of 3.5–8.8, having a fast response time (∼5 s and a detection limit of 5.8×10-7 mol/L. This electrode presented very good selectivity and sensitivity towards the Ho3+ ions over a wide variety of cations, including alkali, alkaline earth, transition and heavy metal ions. The practical utility of the electrode has been demonstrated by its use as an indicator electrode for the potentiometric titration of a Ho3+ solution with EDTA and for the determination of Ho3+ ions concentration in mixtures of two and three different ions.

Design and evaluation of potentiometric principles for bladder volume monitoring: a preliminary study.

Science.gov (United States)

Chen, Shih-Ching; Hsieh, Tsung-Hsun; Fan, Wen-Jia; Lai, Chien-Hung; Chen, Chun-Lung; Wei, Wei-Feng; Peng, Chih-Wei

2015-06-01

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 design principles and animal experience gathered from this research can serve as a basis for developing new implantable bladder sensors in the future.

pH-Induced precipitation behavior of weakly basic compounds: determination of extent and duration of supersaturation using potentiometric titration and correlation to solid state properties.

Science.gov (United States)

Hsieh, Yi-Ling; Ilevbare, Grace A; Van Eerdenbrugh, Bernard; Box, Karl J; Sanchez-Felix, Manuel Vincente; Taylor, Lynne S

2012-10-01

To examine the precipitation and supersaturation behavior of ten weak bases in terms of the relationship between pH-concentration-time profiles and the solid state properties of the precipitated material. Initially the compound was dissolved at low pH, followed by titration with base to induce precipitation. Upon precipitation, small aliquots of acid or base were added to induce slight subsaturation and supersaturation respectively and the resultant pH gradient was determined. The concentration of the unionized species was calculated as a function of time and pH using mass and charge balance equations. Two patterns of behavior were observed in terms of the extent and duration of supersaturation arising following an increase in pH and this behavior could be rationalized based on the crystallization tendency of the compound. For compounds that did not readily crystallize, an amorphous precipitate was formed and a prolonged duration of supersaturation was observed. For compounds that precipitated to crystalline forms, the observed supersaturation was short-lived. This study showed that supersaturation behavior has significant correlation with the solid-state properties of the precipitate and that pH-metric titration methods can be utilized to evaluate the supersaturation behavior.

An Olfactory Indicator for Acid-Base Titrations.

Science.gov (United States)

Flair, Mark N.; Setzer, William N.

1990-01-01

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

Fe (III - Galactomannan Solid and Aqueous Complexes: Potentiometric, EPR Spectroscopy and Thermal Data

Directory of Open Access Journals (Sweden)

Mercê Ana L. R.

2001-01-01

Full Text Available Galactomannans can be employed in food industries to modify the final rheological properties of the products. Since they are not absorbed by the living organisms they can also be used in dietary foods. The equilibria involving the interactions of Fe(III and galactomannans and arabinogalactan of several leguminous plants were characterized by potentiometric titrations and EPR spectroscopy. The log of the equilibrium constants for the formation of ML species, where M is the metal ion and L is the monomeric unit of the biopolymers, were 15.4, 14.1 and 18.5, for the galactomannans of C. fastuosa, L. leucocephala and S. macranthera, respectively. Log K values for protonated species (MHL were 3.1, 3.3, and were not detected for the galactomannan of S. macranthera. The log K values for the formation of ML2 were 14.1, 13.3 and 15.2, respectively. Early formation of insoluble products in the equilibrium with arabinogalactan and Fe(III prevented acquisition of reliable data. The solid complexes assays showed a great dipolar interaction between two Fe(III ions in the inner structure of the biopolymer which increased as the degree of substitution of the galactomannan decreased, and also showed the resulting thermal stability. The complexes impart a new possibility of providing essential metal ions in dietary foods since decomplexation of the complexes can occur at different pH values existing in the human body.

Linear Titration Curves of Acids and Bases.

Science.gov (United States)

Joseph, N R

1959-05-29

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

Novel titration method for surface-functionalised silica

Energy Technology Data Exchange (ETDEWEB)

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

2011-01-15

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

Novel titration method for surface-functionalised silica

International Nuclear Information System (INIS)

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

2011-01-01

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

Reduction and determination of dixanthogens.

Science.gov (United States)

Prasad, M S

1971-06-01

A convenient method for the reduction and determination of dixaathogen has been developed. It is based on the quantitative reaction of dixanthogen with zinc amalgam to form xanthate; the latter can be determined by iodine titration, potentiometric titration with silver nitrate or by spectrophotometry at 310 mmu. Dixanthogen can be determined in mixtures containing xanthate, by titration of aliquots with and without reduction. Higher dixanthogens can also be determined, and flotation liquors analysed.

Potentiometric Surface of the Magothy Aquifer in Southern Maryland, September 2007

Science.gov (United States)

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.

Potencialidades do dióxido de chumbo eletrodepositado como sensor potenciométrico Potentialities of electrodeposited lead dioxide as a potentiometric sensor

Directory of Open Access Journals (Sweden)

Milton Duffles Capelato

1998-07-01

Full Text Available This paper proposes an experiment to be performed in both instrumental analysis and experimental physical-chemistry curricular disciplines in order to open options to develop challenging basic research activities. Thus the experimental procedures and the results obtained in the preparation of electrodeposited lead dioxide onto graphite and its evaluation as potentiometric sensor for H3O+ and Pb2+ ions, are presented. The data obtained in acid-base titrations were compared with those of the traditional combination glass electrode at the same conditions. Although a linear sub-Nernstian response to free hydrogen ions was observed for the electrodeposited PbO2 electrode, a good agreement was obtained between them. Working as lead(II sensing electrode, the PbO2 showed a linear sub-Nernstian behavior at total Pb2+ concentrations ranging from 3,5 x 10-4 to 3,0 x 10-2 mol/L in nitrate media. For the redox couple PbO2/Pb(II the operational slope converges to the theoretical one, as the acidity of the working solution increases.

Automated electronic tongue based on potentiometric sensors for the determination of a trinary anionic surfactant mixture.

Science.gov (United States)

Cortina, Montserrat; Ecker, Christina; Calvo, Daniel; del Valle, Manuel

2008-01-22

An automated electronic tongue consisting of an array of potentiometric sensors and an artificial neural network (ANN) has been developed to resolve mixtures of anionic surfactants. The sensor array was formed by five different flow-through sensors for anionic surfactants, based on poly(vinyl chloride) membranes having cross-sensitivity features. Feedforward multilayer neural networks were used to predict surfactant concentrations. As a great amount of information is required for the correct modelling of the sensors response, a sequential injection analysis (SIA) system was used to automatically provide it. Dodecylsulfate (DS(-)), dodecylbenzenesulfonate (DBS(-)) and alpha-alkene sulfonate (ALF(-)) formed the three-analyte study case resolved in this work. Their concentrations varied from 0.2 to 4mM for ALF(-) and DBS(-) and from 0.2 to 5mM for DS(-). Good prediction ability was obtained with correlation coefficients better than 0.933 when the obtained values were compared with those expected for a set of 16 external test samples not used for training.

Electrochemical properties of actinides in molten chlorides

International Nuclear Information System (INIS)

Lambertin, D.; Lacquement, J.; Sanchez, S.; Picard, G.

2000-01-01

The chemical properties of plutonium and cerium chlorides have been studied in the fused CaCl 2 -NaCl equimolar mixture at 550 deg. C using a tungsten working electrode and a pO 2- indicator electrode. The standard potential of Pu(III)/Pu was determined using cyclic voltammetry. The solubility product of Pu 2 O 3 was calculated by potentiometric titration. The standard potential of Ce(III)/Ce have been determined by a potentiometry method. Potentiometric titrations of Ce(III) have been shown the existence of a soluble cerium oxychloride. All these data allowed us to draw the potential-pO 2- diagram which summarises the properties of plutonium and cerium compounds in the melt. (authors)

Enhancing Natural Attenuation through Bioaugmentation with Aerobic Bacteria that Degrade cis-1,2-Dichloroethene

Science.gov (United States)

2010-01-01

Studies with Site Groundwater ............................................................ 25  5.2.2  Titration Studies...Figure 4-4: Potentiometric Map of the Columbia Aquifer Figure 4-5: Shallow Groundwater TCE Plume Figure 4-6: Shallow Groundwater cDCE Plume Figure 4-7...west. Shallow groundwater typically ranges from 2 to 7 ft below ground surface (bgs) (CH2M HILL, 2008). A potentiometric map for the Columbia

Potentiometric determination of moxifloxacin in some pharmaceutical formulation using PVC membrane sensors.

Science.gov (United States)

Hefnawy, Mohammed M; Homoda, Atef M; Abounassif, Mohammed A; Alanazi, Amer M; Al-Majed, Abdulrahaman; Mostafa, Gamal A

2014-01-01

The construction and electrochemical response characteristics of Poly (vinyl chloride) membrane sensors for moxifloxacin HCl (MOX) are described. The sensing membranes incorporate ion association complexes of moxifloxacin cation and sodium tetraphenyl borate (NaTPB) (sensor 1), phosphomolybdic acid (PMA) (sensor 2) or phosphotungstic acid (PTA) (sensor 3) as electroactive materials. The sensors display a fast, stable and near-Nernstian response over a relative wide moxifloxacin concentration range (1 × 10(-2) - 4.0 × 10(-6), 1 × 10(-2) - 5.0 × 10(-6), 1 × 10(-2) - 5.0 × 10(-6) M), with detection limits of 3 × 10(-6), 4 × 10(-6) and 4.0 × 10(-6) M for sensor 1, 2 and 3, respectively over a pH range of 6.0 - 9.0. The sensors show good discrimination of moxifloxacin from several inorganic and organic compounds. The direct determination of 400 μg/ml of moxifloxacin show an average recovery of 98.5, 99.1 and 98.6% and a mean relative standard deviation of 1.8, 1.6 and 1.8% for sensors 1, 2 and 3 respectively. The proposed sensors have been applied for direct determination of moxifloxacin in some pharmaceutical preparations. The results obtained by determination of moxifloxacin in tablets using the proposed sensors are comparable favorably with those obtained using the US Pharmacopeia method. The sensors have been used as indicator electrodes for potentiometric titration of moxifloxacin.

NBL-Davies-Gray weight titration method

International Nuclear Information System (INIS)

Hassell, C.

1981-01-01

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

A novel method for the determination of the degree of deacetylation of chitosan by coulometric titration.

Science.gov (United States)

Wang, Chao; Yuan, Fang; Pan, Jiabao; Jiao, Shining; Jin, Ling; Cai, Hongwei

2014-09-01

A novel method to determine the degree of deacetylation of chitosan is described. In this method, the coulometric titrant OH- is generated by the electrolysis of water. The OH- reacted with the residual hydrochloric acid in chitosan solution and the degree of deacetylation was obtained by Faraday's law. The optimized experimental parameters in this study were 1.0 mol/L KCl as supporting electrolyte, 15.00 mA as the intensity of constant current, composite glass electrode as indicating electrode couples, double platinum generated electrode-platinum wire auxiliary electrode as working electrode pairs, pH 3.80 as the titration end-point. The degree of deacetylation in the four samples, which varied from 70 to 95% were measured. The results were similar to those from 1H NMR and the standard deviations were lower than 0.5%. With merit of simplicity, convenience, quickness, high accuracy and precision, automatic detection of titration end-point and low-cost, the proposed method will be very useful in the industrial production. Copyright © 2014 Elsevier B.V. All rights reserved.

A Urea Potentiometric Biosensor Based on a Thiophene Copolymer

Directory of Open Access Journals (Sweden)

Cheng-Yuan (Kevin Lai

2017-03-01

Full Text Available A potentiometric enzyme biosensor is a convenient detector for quantification of urea concentrations in industrial processes, or for monitoring patients with diabetes, kidney damage or liver malfunction. In this work, poly(3-hexylthiophene-co-3-thiopheneacetic acid (P(3HT-co-3TAA was chemically synthesized, characterized and spin-coated onto conductive indium tin oxide (ITO glass electrodes. Urease (Urs was covalently attached to the smooth surface of this copolymer via carbodiimide coupling. The electrochemical behavior and stability of the modified Urs/P(3HT-co-3TAA/ITO glass electrode were investigated by cyclic voltammetry, and the bound enzyme activity was confirmed by spectrophotometry. Potentiometric response studies indicated that this electrode could determine the concentration of urea in aqueous solutions, with a quasi-Nernstian response up to about 5 mM. No attempt was made to optimize the response speed; full equilibration occurred after 10 min, but the half-time for response was typically <1 min.

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

Science.gov (United States)

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.

Students' integration of multiple representations in a titration experiment

Science.gov (United States)

Kunze, Nicole M.

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

The potentiometric and laser RAMAN study of the hydrolysis of uranyl chloride under physiological conditions and the effect of systematic and random errors on the hydrolysis constants

International Nuclear Information System (INIS)

Deschenes, L.L.; Kramer, G.H.; Monserrat, K.J.; Robinson, P.A.

1986-12-01

The hydrolysis of uranyl ions in 0.15 mol/L (Na)C1 solution at 37 degrees Celsius has been studied by potentiometric titration. The results were consistent with the formation of (UO 2 ) 2 (OH) 2 , (UO 2 ) 3 (OH) 4 , (UO 2 ) 3 (OH) 5 and (UO 2 ) 4 (OH) 7 . The stability constants, which were evaluated using a version of MINIQUAD, were found to be: log β 22 = -5.693 ± 0.007, log β 34 = -11.499 ± 0.024, log β 35 = -16.001 ± 0.050, log β 47 = -21.027 ± 0.051. Laser Raman spectroscopy has been used to identify the products including (UO 2 ) 4 (OH) 7 species. The difficulties in identifying the chemical species in solution and the effect of small errors on this selection has also been investigated by computer simulation. The results clearly indicate that small errors can lead to the selection of species that may not exist

Acid-basic and complexation properties of a sedimentary humic acid. A study on the Barra Bonita reservoir of Tietê river, São Paulo State, Brazil

Directory of Open Access Journals (Sweden)

Abate Gilberto

2001-01-01

Full Text Available Acid-base and complexation properties of humic acid (HA isolated from a river sediment were studied by potentiometric titration, adopting the discrete site distribution model and the modified Gran functions for data fitting. Six classes of titratable groups were characterized, with pKa values between 2.4 and 10.2. Carboxylic groups accounted for 66% of the total of ionizable sites. The complexing properties were studied with regard to Cu2+, Pb2+, Cd2+ and Zn2+ ions by potentiometric titration using Cu ion selective electrode, or amalgam electrodes (Pb, Cd and Zn. The data treatment by the Scatchard method revealed two binding sites for copper and lead and one binding site for cadmium and zinc. The average stability constants were in the following order: log KHA-Cu > log KHA-Pb > log KHA-Cd @ log KHA-Zn, while the complexing capacity order, Cc, was: Pb > Cu > Cd @ Zn.

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

Science.gov (United States)

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

2013-06-15

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

Titration in the treatment of the more troubled patient.

Science.gov (United States)

Winer, J A; Ornstein, E D

2001-01-01

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

Titrimetric determination of ruthenium

International Nuclear Information System (INIS)

Velichko, V.V.; Belyaeva, T.I.; Kudinova, V.K.; Usatenko, Yu.I.

1978-01-01

Titration of ruthenium(4) hydrochloric-acid solutions with Mohr's salt, hydroquinone, and thiourea has been studied with the use of biampero- and potentiometric indication of the titration end point (t.e.p.) Potentiometric and amperometric indication of the t.e.p. is applicable when Ru(4) concentration is from 20 to 6000 mkg in 20 ml of the titrated solution; biamperometric indication can be used at a concentration of 5-1000 mkg in the same volume. It has been established that titration of Ru(4) (in the form of the Na 2 RuCl 6 solution) with Mohr's salt is not hindered by the presence of 1000-fold excess of alkaline and alkali-earth metals, Al, Ti(4), Mn(2), Cr(3), Fe(3), Co, Ni, Cu, Zn, Ga, Ge(4), As, Se, Mo(6), Cd, In, and Te; 100-fold excess of Rh, Pd, W, Bi, and Sn; 10-fold excess of Ag, Au, Pt, Hg, Os. Along with Ru(4) titrated are Ir(4), Te(3), V(5), and Ce(4). Selectivity of hydroquinone and thiourea is lower. Titrimetric procedure of determining ruthenium has been tested for ruthenium alloy containing cobalt tungsten. It cannot be recommended for analysis of the samples which dissolve in aqua regia

Potentiometric perchlorate determination at nanomolar concentrations in vegetables.

Science.gov (United States)

Leoterio, Dilmo M S; Paim, Ana Paula S; Belian, Mônica F; Galembeck, André; Lavorante, André F; Pinto, Edgar; Amorim, Célia G; Araújo, Alberto N; Montenegro, Maria C B S M

2017-07-15

In this work, an expeditious method based on the multi-commutated flow-analysis concept with potentiometric detection is proposed to perform determinations of the emergent contaminant perchlorate in vegetable matrices down to nanomolar concentration. To accomplish the task, a tubular shaped potentiometric sensor selective to perchlorate ion was constructed with a PVC membrane containing 12mmol/kg of the polyamine bisnaphthalimidopropyl-4,4'-diaminodiphenylmethane and 2-nitrophenyl phenyl ether 68% (w/w) as plasticizer casted on a conductive epoxy resin. Under optimal flow conditions, the sensor responded linearly in the concentration range of 6.3×10 -7 -1.0×10 -3 mol/L perchlorate. In order to extend the determinations to lower concentrations (4.6(±1.3)×10 -10 mol/L perchlorate), a column packed with 70mg of sodium 2,5,8,11,14-pentaoxa-1-silacyclotetradecane-polymer was coupled to the flow-system thus enabling prior pre-concentration of the perchlorate. The proposed procedure provides a simpler alternative for the determination of perchlorate in foods, nowadays only allowed by sophisticated and expensive equipment and laborious methods. Copyright © 2017 Elsevier Ltd. All rights reserved.

Geostatistical analysis of potentiometric data in Wolfcamp aquifer of the Palo Duro Basin, Texas

International Nuclear Information System (INIS)

Harper, W.V.; Furr, J.M.

1986-04-01

This report details a geostatistical analysis of potentiometric data from the Wolfcamp aquifer in the Palo Duro Basin, Texas. Such an analysis is a part of an overall uncertainty analysis for a high-level waste repository in salt. Both an expected potentiometric surface and the associated standard error surface are produced. The Wolfcamp data are found to be well explained by a linear trend with a superimposed spherical semivariogram. A cross-validation of the analysis confirms this. In addition, the cross-validation provides a point-by-point check to test for possible anomalous data

Potentiometric Surface of the Magothy Aquifer in Southern Maryland, September 2009

Science.gov (United States)

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.

Improved Performance of the Potentiometric Biosensor for the Determination of Creatinine

DEFF Research Database (Denmark)

Andersen, Jens Enevold Thaulov; Rasmussen, Claus/Dallerup; Zachau-Christiansen, Birgit

2007-01-01

The development of potentiometric biosensors for the determination of creatinine is attractive because it is a frequently analysed species in clinical chemistry. Contemporary methods of analysing creatinine engage chemicals harmful to the environment and generate large volumes of waste disposals....... By introducing a membrane-based potentiometric biosensor with immobilised creatinine deaminase, the measurements can be performed by miniaturised portable devices that are easy to handle and allow rapid analysis at a minimum consumption of chemicals. Thus, the enzymatic creatinine biosensors was revisited...... performed by flow injection analysis (FIA) showed that the response time could be lowered to approx. 30 sec. using sample volumes of 30 L. Interferences were corrected for by application of the Nicolsky-Eisenman equation thus allowing determination of creatinine in matrices resembling those of clinical...

Rapid clozapine titration in treatment-refractory bipolar disorder.

Science.gov (United States)

Ifteni, Petru; Correll, Christoph U; Nielsen, Jimmi; Burtea, Victoria; Kane, John M; Manu, Peter

2014-09-01

Clozapine is effective in treatment-refractory bipolar disorder (BD). Guidelines recommend slow titration to prevent seizures, hypotension and myocarditis, but this stance is not supported by comparative data. To evaluate the safety and effectiveness of rapid clozapine titration in BD. Analysis of a consecutive cohort of treatment-refractory BD patients with mixed/manic episode admitted on alternate days to one of two units of a psychiatric hospital. On one unit, clozapine was started at 25mg followed by 25-50mg as needed every 6h (maximum=100mg/day) on day 1, followed by increases of 25-100mg/day. On the other unit, clozapine was initiated with 25mg in day 1, followed by increases of 25-50mg/day. The primary outcome was the number of days from starting clozapine until readiness for discharge, adjusted in logistic regression for the number of antipsychotics tried during the hospitalization, psychotropic co-treatments and presence of psychotic features. Patients subject to rapid (N=44) and standard (N=23) titration were similar in age, gender, smoking status, body mass index, illness severity at baseline and discharge, and highest clozapine dose. Clozapine was discontinued due to hypotension (N=1) and pneumonia (N=1) during rapid titration, and for excessive sedation (N=1) in each titration group. The number of hospital days from starting clozapine until readiness for discharge was 3.8 days shorter in the rapid titration group (12.7±6.3 vs. 16.5±5.8, p=0.0077). Rapid clozapine titration appeared safe and effective for treatment-refractory BD. The potential for shorter hospital stays justifies prospective trials of this method. Copyright © 2014 Elsevier B.V. All rights reserved.

Surface stoichiometry of zinc sulfide and its effect on the adsorption behaviors of xanthate

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Wang Meng

2011-11-01

Full Text Available Abstract In this paper, the surface stoichiometry, acid-base properties as well as the adsorption of xanthate at ZnS surfaces were studied by means of potentiometric titration, adsorption and solution speciation modeling. The surface proton binding site was determined by using Gran plot to evaluate the potentiometric titration data. Testing results implied that for stoichiometric surfaces of zinc sulfide, the proton and hydroxide determine the surface charge. For the nonstoichiometric surfaces, the surface charge is controlled by proton, hydroxide, zinc and sulfide ions depending on specific conditions. The xanthate adsorption decreases with increasing solution pH, which indicates an ion exchange reaction at the surfaces. Based on experimental results, the surface protonation, deprotonation, stoichiometry and xanthate adsorption mechanism were discussed.

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

Science.gov (United States)

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

2016-01-01

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

Differential Binding Models for Direct and Reverse Isothermal Titration Calorimetry.

Science.gov (United States)

Herrera, Isaac; Winnik, Mitchell A

2016-03-10

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

Complexometric determination of trivalent rare earths and actinides with diethylene-triaminepentaacetic acid

International Nuclear Information System (INIS)

Timofeev, G.A.; Simakin, G.A.; Baklanova, P.F.; Kuznetsov, G.F.; Ivanov, V.I.

1976-01-01

Optimal conditions have been found for the separate quantitative determination of 200 to 500 mcg of trivalent Eu, La, Nd, Pr, Am and Cm by complexometric titration with diethylenetriaminepentaacetic acid. The final titration point (FTP) has been determined by using one of the following three methods, namely by visual inspection with the aid of xylene orange as an indicator, spectrophotometrically at pH 4.5-4.7 with xylene orange and potentiometrically at pH 4.0-5.5 through the backward titration of the excess complexone with the solution of Fe(3) in HNO 3 . The relative standard errors Ssub(r)=0.004 (Eu), 0.011 Cm with the visual indication of FTP; Ssub(r)=0.005 (Am) with the spectrophotometric indication of FTP; Ssub(r)=0.0O9 (Eu), 0.011 (Pr) and 0.02 (Am) with the potentiometric indication of FTP. Determination of trivalent lanthanides and actinoids is adversely affected by tetravalent actinoids, Zr, U(6), Hg(2) and Fe(3). Titration conditions chosen have been checked in the analysis of the mixture containing the sum of trivalent rare earths, Am and Cm [ru

Simple and Automated Coulometric Titration of Acid Using Nonisolated Electrodes

Science.gov (United States)

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

2011-01-01

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

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

Science.gov (United States)

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 design and application of virtual ion meter based on LABVIEW 8.0.

Science.gov (United States)

Meng, Hu; Li, Jiangyuan; Tang, Yonghuai

2009-08-01

The virtual ion meter is developed based on LABVIEW 8.0 by homemade adjusting circuit, data acquisition (DAQ) board, and computer. This note provides details of the structure of testing system and flow chart of DAQ program. This virtual instrument system is applied to multitask testing such as determining rate constant of second-order reaction by pX, pX potentiometric titration, determining oscillating reaction by potential, etc. The result of application indicates that this test system not only has function of real-time data acquiring, displaying, storage, but also realizes remote monitoring and controlling test-control spots through internet, automatic analyzing and processing of data, reporting of result according to the different testing task; moreover, the veracity and repeatability of data processing result are higher than the results of manual data processing.

A Closer Look at Acid-Base Olfactory Titrations

Science.gov (United States)

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

2005-01-01

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

Silver ion recognition using potentiometric sensor based on recently synthesized isoquinoline-1,3-dione derivatives

Directory of Open Access Journals (Sweden)

AJAR KAMAL

2012-08-01

Full Text Available The four derivatives of isoquinoline-1,3-dione based on β-lactum (I-IV, have been explored as neutral ionophores for preparing poly(vinylchloride based polymeric membrane electrodes (PME selective to silver(I ions. The addition of sodium tetraphenylborate (NaTPB and dioctylsebacate (DOS as a plasticizer was found to improve the performance of ion selective electrodes. The best performance was obtained with PME-1 based on ionophore I having composition: ionophore (9.2 mg, PVC (100.1 mg, DOS (201.1 mg and NaTPB (1.5 mg in 5 mL tetrahydrofuran. The electrode response was linear with Nernstian slope of 58.44 mV/decade in the concentration range of 1.0 x 10-1 M to 5.0 x 10-6 M and detection limit of 5.83 x 10-6 M. It performs satisfactorily over wide pH range of 1.0-5.5. The proposed sensor can be used over a period of more than three months without any significant drift in potential and shows good selectivity to silver(I ion over a number of cations especially with no interference of mercury(II ions. Sharp end point was obtained when the sensor was used as an indicator electrode for the potentiometric titration of silver(I ions with chloride ions and therefore this electrode (PME-1 could be used for quantitative determination of silver(I ion in synthetic water, silver foil and dental amalgam samples.

Potentiometric Sensor for Gadolinium(III Ion Based on Zirconium(IV Tungstophosphate as an Electroactive Material

Directory of Open Access Journals (Sweden)

Harish K. Sharma

2009-01-01

Full Text Available A new inorganic ion exchanger has been synthesized namely Zirconium(IV tungstophosphate [ZrWP]. The synthesized exchanger was characterized using ion exchange capacity and distribution coefficient (Kd. For further studies, exchanger with 0.35 meq/g ion-exchange capacity was selected. Electrochemical studies were carried out on the ion exchange membranes using epoxy resin as a binder. In case of ZrWP, the membrane having the composition; Zirconium(IV tugstophosphate (40% and epoxy resin (60% exhibits best performance. The membrane works well over a wide range of concentration from 1×10-5 to 1×10-1 M of Gd(III ion with an over- Nernstian slope of 30 mv/ decade. The response time of the sensor is 15 seconds. For this membrane, effect of internal solution has been studied and the electrode was successfully used in partially non-aqueous media too. Fixed interference method and matched potential method has been used for determining selectivity coefficient with respect to alkali, alkaline earth, some transition and rare earth metal ions that are normally present along with Gd(III in its ores. The electrode can be used in the pH range 4.0-10.0 for 10-1 M and 3.0-7.0 for 10-2 M concentration of target ion. These sensors have been used as indicator electrodes in the potentiometric titration of Gd(III ion against EDTA and oxalic acid.

Extended Abstracts, International Society of Electrochemistry (36th) Held at Salamanca, Spain on 23-28 September 1985.

Science.gov (United States)

1985-09-28

potentiometric titration of cimeti- dine with HC1O 4 using the Gran graphic method to estimate the end point. Polarographic Behaviour of Ranitidine In the...solutions: Before each experiment, the H20 content in LiCl04 + MeOR is determined (144 wg/ml) by Karl Fischer cou- lometer (Acquavit-Tacussel). After the... method . The potentiometric selectivity coefficients towards monovalent cations were reasonable good. The response curves are presented in Figure 3, when

Potentiometric assay for hydrogenocarbonate in natural waters

OpenAIRE

Milla González, Miguel

2008-01-01

Potentiometry is often used for the determination of hydrogenocarbonate in natural water samples. In this exercise, a volume V of the titrant HCl is required for the potentiometric analysis of the mentioned species in 50 mL of water sample. The titrant concentration is M molar. The user should calculate the concentration of hydrogenocarbonate and express it either in mg/L or in g/L of calcium carbonate by building up the corresponding stoichiometric expressions. All results entered in the sys...

Spectrophotometric titration of sulfates in the presence of zirconium

International Nuclear Information System (INIS)

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

1978-01-01

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

Green chemistry volumetric titration kit for pharmaceutical formulations: Econoburette

Directory of Open Access Journals (Sweden)

Man Singh

2009-08-01

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

Studies on potassium chlorate as a primary oxidimetric reagent.

Science.gov (United States)

Murty, C R; Rao, G G

1972-01-01

Conditions have been established for the use of potassium chlorate as a primary oxidizing agent in the direct titration of vanadium(III), tin(II) and titanium(III) with visual or potentiometric end-points.

Parameters for Efficient Fuel Cell Catalyst Structures

Science.gov (United States)

2011-04-03

concentration which varies for several reactions generating or consuming protons. The SECPM offers this possibility due to the potentiometric ...applied to the Pd/H electrode in order to remove excess surface hydrogen and relieve concentration gradients [56]. Titration experiments in order to...Figure 10: Titration curve of Pd/H electrode. OCP vs. time This experiment was also done adding alkaline NaOH electrolyte in different amounts and

Screen-printed sensor for batch and flow injection potentiometric chromium(VI) monitoring

Energy Technology Data Exchange (ETDEWEB)

Sanchez-Moreno, Raul A.; Gismera, M.J.; Sevilla, M.T.; Procopio, Jesus R. [Facultad de Ciencias, Universidad Autonoma de Madrid, Departamento de Quimica Analitica y Analisis Instrumental, Madrid (Spain)

2010-05-15

A disposable screen-printed electrode was designed and evaluated for direct detection of chromium(VI) in batch and flow analysis. The carbon screen-printed electrode was modified with a graphite-epoxy composite. The optimal graphite-epoxy matrix contains 37.5% graphite powder, 12.5% diphenylcarbohydrazide, a selective compound for chromium(VI), and 50% epoxy resin. The principal analytical parameters of the potentiometric response in batch and flow analysis were optimized and calculated. The screen-printed sensor exhibits a response time of 20 {+-} 1 s. In flow analysis, the analytical frequency of sampling is 70 injections per hour using 0.1 M NaNO{sub 3} solution at pH 3 as the carrier, a flow rate of 2.5 mL.min{sup -1}, and an injection sample volume of 0.50 mL. The sensor shows potentiometric responses that are very selective for chromium(VI) ions and optimal detection limits in both static mode (2.1 x 10{sup -7} M) and online analysis (9.4 x 10{sup -7} M). The disposable potentiometric sensor was employed to determine toxicity levels of chromium(VI) in mineral, tap, and river waters by flow-injection potentiometry and batch potentiometry. Chromium(VI) determination was also carried out with successful results in leachates from municipal solid waste landfills. (orig.)

Potentiometric surfaces of the intermediate aquifer system, west-central Florida, May, 1993

Science.gov (United States)

Mularoni, R.A.

1994-01-01

The intermediate aquifer system underlies a 5000-sq-mi area including De Soto, Sarasota, Hardee, Manatee, and parts of Charlotte, Hillsborough, Highlands, and Polk Counties, Florida. It is overlain by the surf@cial aquifer system and underlain by the Floridan aquifer system. The potentiometric surface of the intermediate aquifer system was mapped by determining the altitude of water levels in a network of wells and represented on a map by contours that connect points of equal altitude. This map represents water-level conditions near the end of the spring dry season when ground- water withdrawals for agricultural use were high. The cumulative rainfall for the study area was 4.84 inches above normal for the period from June 1992 to May 1993. Hydrographs for selected wells indicated that the annual and seasonal fluctuations of the water levels were generally large (greater than 15 feet) in the central interior region where water demand for irrigation is high during the fall and spring. Seasonal fluctuations were smaller in the northern recharge area where water use is predominantly for public supply. Water levels measured in May 1993 for the composite intermediate aquifer potentiometric surface were lower than those measured in May or September 1992. A cone of depression exists in the potentiometric surface for the composite aquifer system at Warm Mineral Springs, which is a natural discharge point from this system.

Comparison of Ho and Y complexation data obtained by electromigration methods, potentiometry and spectrophotometry

International Nuclear Information System (INIS)

Vinsova, H.; Koudelkova, M.; Ernestova, M.; Jedinakova-Krizova, V.

2003-01-01

Many of holmium and yttrium complex compounds of both organic and inorganic origin have been studied recently from the point of view of their radiopharmaceutical behavior. Complexes with Ho-166 and Y-90 can be either directly used as pharmaceutical preparations or they can be applied in a conjugate form with selected monoclonal antibody. Appropriate bifunctional chelation agents are necessary in the latter case for indirect binding of monoclonal antibody and selected radionuclide. Our present study has been focused on the characterization of radionuclide (metal) - ligand interaction using various analytical methods. Electromigration methods (capillary electrophoresis, capillary isotachophoresis), potentiometric titration and spectrophotometry have been tested from the point of view of their potential to determine conditional stability constants of holmium and yttrium complexes. A principle of an isotachophoretic determination of stability constants is based on the linear relation between logarithms of stability constant and a reduction of a zone of complex. For the calculation of thermodynamic constants using potentiometry it was necessary at first to determine the protonation constants of acid. Those were calculated using the computer program LETAGROP Etitr from data obtained by potentiometric acid-base titration. Consequently, the titration curves of holmium and yttrium with studied ligands and protonation constants of corresponding acid were applied for the calculation of metal-ligand stability constants. Spectrophotometric determination of stability constants of selected systems was based on the titration of holmium and yttrium nitrate solutions by Arsenazo III following by the titration of metal-Arsenazo III complex by selected ligand. Data obtained have been evaluated using the computation program OPIUM. Results obtained by all analytical methods tested in this study have been compared. It was found that direct potentiometric titration technique could not be

New applications of corrosion measurements by titration (CMT)

DEFF Research Database (Denmark)

Bech-Nielsen, Gregers

1998-01-01

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

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

Science.gov (United States)

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

2014-05-01

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

''Titration'' polymerization of monovinylacetylene

NARCIS (Netherlands)

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

1996-01-01

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

Potentiometric Surface of the Upper Floridan Aquifer, West-Central Florida, September 2006

Science.gov (United States)

Ortiz, A.G.

2007-01-01

The Floridan aquifer system consists of the Upper and Lower Floridan aquifers separated by the middle confining unit. The middle confining unit and the Lower Floridan aquifer in west-central Florida generally contain highly mineralized water. The water-bearing units containing freshwater are herein referred to as the Upper Floridan aquifer. The Upper Floridan aquifer is the principal source of water in the Southwest Florida Water Management District and is used for major public supply, domestic use, irrigation, and brackish water desalination in coastal communities (Southwest Florida Water Management District, 2000). This map report shows the potentiometric surface of the Upper Floridan aquifer measured in September 2006. The potentiometric surface is an imaginary surface connecting points of equal altitude to which water will rise in tightly cased wells that tap a confined aquifer system (Lohman, 1979). This map represents water-level conditions near the end of the wet season, when ground-water levels usually are at an annual high and withdrawals for agricultural use typically are low. The cumulative average rainfall of 46.06 inches for west-central Florida (from October 2005 through September 2006) was 6.91 inches below the historical cumulative average of 52.97 inches (Southwest Florida Water Management District, 2006). Historical cumulative averages are calculated from regional rainfall summary reports (1915 to most recent complete calendar year) and are updated monthly by the Southwest Florida Water Management District. This report, prepared by the U.S. Geological Survey in cooperation with the Southwest Florida Water Management District, is part of a semi-annual series of Upper Floridan aquifer potentiometric-surface map reports for west-central Florida. Potentiometric-surface maps have been prepared for January 1964, May 1969, May 1971, May 1973, May 1974, and for each May and September since 1975. Water-level data are collected in May and September each

Potentiometric Surface of the Upper Floridan Aquifer, West-Central Florida, September 2007

Science.gov (United States)

Ortiz, A.G.

2008-01-01

The Floridan aquifer system consists of the Upper and Lower Floridan aquifers separated by the middle confining unit. The middle confining unit and the Lower Floridan aquifer in west-central Florida generally contain highly mineralized water. The water-bearing units containing fresh water are herein referred to as the Upper Floridan aquifer. The Upper Floridan aquifer is the principal source of water in the Southwest Florida Water Management District and is used for major public supply, domestic use, irrigation, and brackish water desalination in coastal communities (Southwest Florida Water Management District, 2000). This map report shows the potentiometric surface of the Upper Floridan aquifer measured in September 2007. The potentiometric surface is an imaginary surface connecting points of equal altitude to which water will rise in tightly-cased wells that tap a confined aquifer system (Lohman, 1979). This map represents water-level conditions near the end of the wet season, when ground-water levels usually are at an annual high and withdrawals for agricultural use typically are low. The cumulative average rainfall of 39.50 inches for west-central Florida (from October 2006 through September 2007) was 13.42 inches below the historical cumulative average of 52.92 inches (Southwest Florida Water Management District, 2007). Historical cumulative averages are calculated from regional rainfall summary reports (1915 to most recent complete calendar year) and are updated monthly by the Southwest Florida Water Management District. This report, prepared by the U.S. Geological Survey in cooperation with the Southwest Florida Water Management District, is part of a semi-annual series of Upper Floridan aquifer potentiometric-surface map reports for west-central Florida. Potentiometric-surface maps have been prepared for January 1964, May 1969, May 1971, May 1973, May 1974, and for each May and September since 1975. Water-level data are collected in May and September each

Potentiometric surface of the Upper Floridan aquifer, west-central Florida, September 2005

Science.gov (United States)

Ortiz, A.G.

2006-01-01

The Floridan aquifer system consists of the Upper and Lower Floridan aquifers separated by the middle confining unit. The middle confining unit and the Lower Floridan aquifer in west-central Florida generally contain highly mineralized water. The water-bearing units containing freshwater are herein referred to as the Upper Floridan aquifer. The Upper Floridan aquifer is the principal source of water in the Southwest Florida Water Management District 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 2005. 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 55.19 inches for west-central Florida (from October 2004 through September 2005) was 2.00 inches above the historical cumulative average of 53.19 inches (Southwest Florida Water Management District, 2005). Historical cumulative averages are calculated from regional rainfall summary reports (1915 to 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

Potentiometric Surface of the Upper Floridan Aquifer, West-Central Florida, May 2007

Science.gov (United States)

Ortiz, A.G.

2008-01-01

The Floridan aquifer system consists of the Upper and Lower Floridan aquifers separated by the middle confining unit. The middle confining unit and the Lower Floridan aquifer in west-central Florida generally contain highly mineralized water. The water-bearing units containing fresh water are herein referred to as the Upper Floridan aquifer. The Upper Floridan aquifer is the principal source of water in the Southwest Florida Water Management District and is used for major public supply, domestic use, irrigation, and brackish water desalination in coastal communities (Southwest Florida Water Management District, 2000). This map report shows the potentiometric surface of the Upper Floridan aquifer measured in May 2007. The potentiometric surface is an imaginary surface connecting points of equal altitude to which water will rise in tightly-cased wells that tap a confined aquifer system (Lohman, 1979). This map represents water-level conditions near the end of the dry season, when ground-water levels usually are at an annual low and withdrawals for agricultural use typically are high. The cumulative average rainfall of 41.21 inches for west-central Florida (from June 2006 through May 2007) was 11.63 inches below the historical cumulative average of 52.84 inches (Southwest Florida Water Management District, 2007). Historical cumulative averages are calculated from regional rainfall summary reports (1915 to most recent complete calendar year) and are updated monthly by the Southwest Florida Water Management District. This report, prepared by the U.S. Geological Survey in cooperation with the Southwest Florida Water Management District, is part of a semi-annual series of Upper Floridan aquifer potentiometric-surface map reports for west-central Florida. Potentiometric-surface maps have been prepared for January 1964, May 1969, May 1971, May 1973, May 1974, and for each May and September since 1975. Water-level data are collected in May and September each year to show the

Determination of the Acidity of Oils Using Paraformaldehyde as a Thermometric End-Point Indicator

Directory of Open Access Journals (Sweden)

Carneiro Mário J. D.

2002-01-01

Full Text Available The determination of the acidity of oils by catalytic thermometric titrimetry using paraformaldehyde as the thermometric end-point indicator was investigated. The sample solvent was a 1:1 (v/v mixture of toluene and 2-propanol and the titrant was 0.1 mol L-1 aqueous sodium hydroxide. Paraformaldehyde, being insoluble in the sample solvent, does not present the inconvenience of other indicators that change the properties of the solvent due to composition changes. The titration can therefore be done effectively in the same medium as the standard potentiometric and visual titration methods. The results of the application of the method to both non-refined and refined oils are presented herein. The proposed method has advantages in relation to the potentiometric method in terms of speed and simplicity.

An efficient ab initio DFT and PCM assessment of the potentiometric selectivity of a salophen type Schiff base.

Science.gov (United States)

Demir, Serkan; Yilmaz, Hakan; Dilimulati, Maowulidan; Andaç, Müberra

2014-06-01

As a neutral carrier component for the preparation of a potentiometric membrane sensor, the affinity and selectivity of the salophen type Schiff base ligand obtained by 1:2 condensation of 2.3-diaminopyridine with salicylaldehyde toward a series of common cations has been fully examined by DFT/B3LYP and integral equation formalism polarizable continum model (IEF-PCM or only given with PCM as default input in the computations) in combination with the experimental data. Both the potentiometric measurements and DFT calculations have exhibited that the ionophore shows appreciable selectivity for Cu(2+) ion over other cations. Four different approaches where the last three are the modified version of each other have been evaluated and compared with potentiometric data. Based upon the results of comparison among the approaches suggested to verify the selective behavior of ionophore toward Cu(2+), PCM implemented approach having a whole computational groundwork has given well-matched results with the observed data and with the method augmented with experimental hydration energies. The foremost interferences were detected by determining potentiometric selectivity coefficients for each metal ion relative to Cu(2+) and compared to the results obtained by the DFT calculations.

Colloid Titration--A Rapid Method for the Determination of Charged Colloid.

Science.gov (United States)

Ueno, Keihei; Kina, Ken'yu

1985-01-01

"Colloid titration" is a volumetric method for determining charged polyelectrolytes in aqueous solutions. The principle of colloid titration, reagents used in the procedure, methods of endpoint detection, preparation of reagent solutions, general procedure used, results obtained, and pH profile of colloid titration are considered. (JN)

Molecular dynamics simulation of potentiometric sensor response: the effect of biomolecules, surface morphology and surface charge.

Science.gov (United States)

Lowe, B M; Skylaris, C-K; Green, N G; Shibuta, Y; Sakata, T

2018-05-10

The silica-water interface is critical to many modern technologies in chemical engineering and biosensing. One technology used commonly in biosensors, the potentiometric sensor, operates by measuring the changes in electric potential due to changes in the interfacial electric field. Predictive modelling of this response caused by surface binding of biomolecules remains highly challenging. In this work, through the most extensive molecular dynamics simulation of the silica-water interfacial potential and electric field to date, we report a novel prediction and explanation of the effects of nano-morphology on sensor response. Amorphous silica demonstrated a larger potentiometric response than an equivalent crystalline silica model due to increased sodium adsorption, in agreement with experiments showing improved sensor response with nano-texturing. We provide proof-of-concept that molecular dynamics can be used as a complementary tool for potentiometric biosensor response prediction. Effects that are conventionally neglected, such as surface morphology, water polarisation, biomolecule dynamics and finite-size effects, are explicitly modelled.

A new sensor for thermometric titrations.

Science.gov (United States)

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

2007-01-15

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

The fluorimetric titration of zirconium in the ppm-range

International Nuclear Information System (INIS)

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

1976-01-01

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

Analysis of the Purity of Cetrimide by Titrations

DEFF Research Database (Denmark)

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

2006-01-01

. Titration by perchloric acid showed a 99.69 ± 0.05 % purity of cetrimide and titration by silver nitrate showed a 99.85% ± 0.05 % purity while the traditional assay method predicted a purity of only 97.1 ± 0.4. It was found that the discrepancy could be identified as differences in selectivity during...

Thermodynamic study of complexation of thorium with pyridine monocarboxylates by calorimetry and DFT calculations

International Nuclear Information System (INIS)

Rama Mohana Rao, D.; Rawat, Neetika; Sawant, R.M.; Tomar, B.S.; Manna, D.; Ghanty, T.K.

2013-01-01

Stability constants of Th(IV) complexes with pyridine mono-carboxylates, namely, picolinate, nicotinate and isonicotinate have been determined following potentiometric titration of the metal ion and ligand mixtures with NaOH solution of known concentration. These data were used during the analysis of the calorimetric titration data to obtain the enthalpy of complexation reactions. The experimental data have been compared with that obtained from the DFT based theoretical calculations. (author)

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

Science.gov (United States)

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.

Determination of the stability constants of 2-hydroxyl-1-naphthalidene-monoethanol-amine complexes with Pr/sup 3 +/, Nd/sup 3 +/, Gd/sup 3 +/, Dy/sup 3 +/ and Y/sup 3 +/

Energy Technology Data Exchange (ETDEWEB)

Mayadeo, M S; Ganti, R L; Rao, A P [Ramnarain Ruia Coll., Bombay (India)

1981-01-01

The successive stability constants of the complexes of 2-hydroxy-1-naphthalidene-monoethanolamine with various trivalent metal ions have been determined potentiometrically following the Calvin-Bjerrum pH titration technique as adopted by Irving and Rossotti.

Thermometric Titration for Rapid Determination of Trace Water in Jet Fuel

Directory of Open Access Journals (Sweden)

Jian-Qiang Hu

2017-01-01

Full Text Available Water content in jet fuels is detected by thermometric titration (TMT, and the optimal detected system is 2,2-dimethoxypropane as titrant, cyclohexane and isopropanol as titration solvents, and methanesulfonic acid as catalyst in this method. The amounts of oil, concentration and delivery rate of titrant, volumes, and the reliability and accuracy of thermometric titration were emphasized. The results show that the accuracy, validity, and reliability of TMT are excellent by different indicated spiked water contents. The obtained results between TMT and Karl Fischer titration have been proven to be in accord. But, the duration of titration merely spends 3–5 min in the whole process, greatly shortening the detected time. Therefore, rapid and accurate determination of trace water in a jet fuel can be realized by TMT.

Solid-state potentiometric biosensors for pH quantification in biological samples

NARCIS (Netherlands)

Ivan, M.G.; Wiegersma, S.; Sweelssen, J.; Saalmink, M.; Boersma, A.

2011-01-01

This paper reports on manufacturing and characterization of an all-solid-state potentiometric sensor aimed at monitoring pH in dialysate or blood plasma for patients who undergo dialysis. The sensing polymer-based membrane, coated on top of the Au working electrodes, contains a polymer matrix -