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Sample records for acid titration method

  1. A simple method for the titration of multicomponent acid-base mixtures.

    PubMed

    Moisio, T; Heikonen, M

    1996-01-01

    A titration method has been developed to analyze acid mixtures, in which the pK values differed by 0.5 to 1 pH units. Instead of the use of equivalence points a buffer capacity curve is numerically derived from the titration curve resulting in a presentation similar to chromatograms and spectra. The consumption of the NaOH titrant is determined within pH intervals of 0.2-0.6 units around the pK values of the components. The buffer capacity measured is expressed as the consumption of NaOH over the pH interval. The amounts of compounds are found from these results using simple models of chemometrics. The method has been applied to a mixture of formic and acetic acids with concentrations of 0-3 mmol/20 ml with an error of 0-0.05 mmol. Furthermore a curve-fitting method based on a theoretical equation of buffer capacity can be applied with an error slightly larger than with the previous method. In this case, the pK values were also computed. For titrations beyond the pH range 4-10, the buffer capacity of water has to be subtracted from the titration results. The whole procedure requires including the computations about 3-6 min.

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

    PubMed

    Barbieri Gonzaga, Fabiano; Pereira Sobral, Sidney

    2012-08-15

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

  3. Nanopore Back Titration Analysis of Dipicolinic Acid

    PubMed Central

    Han, Yujing; Zhou, Shuo; Wang, Liang; Guan, Xiyun

    2015-01-01

    Here we report a novel label-free nanopore back titration method for the detection of dipicolinic acid, a marker molecule for bacterial spores. By competitive binding of the target analyte and a large ligand probe to metal ions, dipicolinic acid could be sensitively and selectively detected. This nanopore back titration approach should find useful applications in the detection of other species of medical, biological, or environmental importance if their direct detection is difficult to achieve. PMID:25074707

  4. Linear Titration Curves of Acids and Bases.

    PubMed

    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.

  5. Acidic range titration of HEWL using a constant-pH molecular dynamics method.

    PubMed

    Machuqueiro, Miguel; Baptista, António M

    2008-07-01

    In this work, we present the first application to a protein of the stochastic constant-pH molecular dynamics (MD) method with the inclusion of proton tautomerism. The acidic titration of HEWL was performed under different conditions. Both generalized reaction field (GRF) and particle mesh Ewald (PME) methods were used in the treatment of the long range electrostatics and, even though the PME simulations revealed to be more stable, the better results were obtained using GRF (pK(a) RMSD of 0.82 for GRF and 1.13 for PME). The results using PME at different dielectric constants (2, 4, and 8) also revealed that there was no significant improvement in pK(a)'s prediction upon increasing the dielectric constant. The secondary structure analysis of HEWL revealed a remarkably stable protein in the acidic pH range. The beta-sheet strands (unlike the alpha-helices) seem to be destabilized upon pH decrease, suggesting that the beta-domain is less stable than the alpha-domain. The four principal alpha-helices were also ordered according to their stability in the acidic pH range and the results (4 < 1 < 2 approximately = 3) were consistent with the ones obtained in thermal denaturation studies.

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

    USGS Publications Warehouse

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

    1996-01-01

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

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

    PubMed

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

    2011-05-15

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

  8. Development of High-purity Certified Reference Materials for 17 Proteinogenic Amino Acids by Traceable Titration Methods.

    PubMed

    Kato, Megumi; Yamazaki, Taichi; Kato, Hisashi; Eyama, Sakae; Goto, Mari; Yoshioka, Mariko; Takatsu, Akiko

    2015-01-01

    To ensure the reliability of amino acid analyses, the National Metrology Institute of Japan of the National Institute of Advanced Industrial Science and Technology (NMIJ/AIST) has developed high-purity certified reference materials (CRMs) for 17 proteinogenic amino acids. These CRMs are intended for use as primary reference materials to enable the traceable quantification of amino acids. The purity of the present CRMs was determined based on two traceable methods: nonaqueous acidimetric titration and nitrogen determination by the Kjeldahl method. Since neither method could distinguish compounds with similar structures, such as amino acid-related impurities, impurities were thoroughly quantified by combining several HPLC methods, and subtracted from the obtained purity of each method. The property value of each amino acid was calculated as a weighted mean of the corrected purities by the two methods. The uncertainty of the property value was obtained by combining measurement uncertainties of the two methods, a difference between the two methods, the uncertainty from the contribution of impurities, and the uncertainty derived from inhomogeneity. The uncertainty derived from instability was considered to be negligible based on stability monitoring of some CRMs. The certified value of each amino acid, property value with uncertainty, was given for both with or without enantiomeric separation.

  9. Sequential injection titration method using second-order signals: determination of acidity in plant oils and biodiesel samples.

    PubMed

    del Río, Vanessa; Larrechi, M Soledad; Callao, M Pilar

    2010-06-15

    A new concept of flow titration is proposed and demonstrated for the determination of total acidity in plant oils and biodiesel. We use sequential injection analysis (SIA) with a diode array spectrophotometric detector linked to chemometric tools such as multivariate curve resolution-alternating least squares (MCR-ALS). This system is based on the evolution of the basic specie of an acid-base indicator, alizarine, when it comes into contact with a sample that contains free fatty acids. The gradual pH change in the reactor coil due to diffusion and reaction phenomenona allows the sequential appearance of both species of the indicator in the detector coil, recording a data matrix for each sample. The SIA-MCR-ALS method helps to reduce the amounts of sample, the reagents and the time consumed. Each determination consumes 0.413ml of sample, 0.250ml of indicator and 3ml of carrier (ethanol) and generates 3.333ml of waste. The frequency of the analysis is high (12 samples h(-1) including all steps, i.e., cleaning, preparing and analysing). The utilized reagents are of common use in the laboratory and it is not necessary to use the reagents of perfect known concentration. The method was applied to determine acidity in plant oil and biodiesel samples. Results obtained by the proposed method compare well with those obtained by the official European Community method that is time consuming and uses large amounts of organic solvents.

  10. Linear titration plots for polyfunctional weak acids and bases.

    PubMed

    Midgley, D; McCallum, C

    1976-04-01

    Procedures are derived for obtaining the equivalence volumes in the potentiometric titrations of polyfunctional weak acids and weak bases by a linear titration plot method. The effect of errors in the equilibrium constants on the accuracy is considered. A Fortran program is available to do the calculations.

  11. Thermometric titration of acids in pyridine.

    PubMed

    Vidal, R; Mukherjee, L M

    1974-04-01

    Thermometric titration of HClO(4), HI, HNO(3), HBr, picric acid o-nitrobenzoic acid, 2,4- and 2,5-dinitrophenol, acetic acid and benzoic acid have been attempted in pyridine as solvent, using 1,3-diphenylguanidine as the base. Except in the case of 2,5-dinitrophenol, acetic acid and benzoic acid, the results are, in general, reasonably satisfactory. The approximate molar heats of neutralization have been calculated.

  12. The acid-base titration of montmorillonite

    NASA Astrophysics Data System (ADS)

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

    2003-12-01

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

  13. Comparison of the serial dilution indicator and intragastric titration methods for measurement of meal-stimulated gastric acid secretion in man.

    PubMed

    Hogan, D L; Turken, D; Stern, A I; Isenberg, J I

    1983-11-01

    Two in vivo methods that permit quantitation of gastric acid secretion immediately after the meal are currently in use: intragastric titration and the serial dilution indicator method. During intragastric titration, intragastric pH is artificially maintained at 5.5 to 7 by the continuous addition of alkali to the gastric contents, while during serial dilution the intragastric pH is permitted to seek its natural pH. This study compared gastric acid secretion and serum gastrin in response to a liquid protein meal measured by both techniques in 10 subjects. Mean (+/- SE) 3-hr acid outputs were almost identical (53.6 +/- 6.0 mmol/3 hr with intragastric titration and 52.0 +/- 8.5 mmol/3 hr with serial dilution indicator). Furthermore, 30 min secretory responses in individual subjects were highly correlated (r = 0.98 +/- 0.01, P less than 0.001). Also, in spite of intragastric pH being less than 1.5 by 90 min after the meal during the serial dilution method, total integrated serum gastrin concentrations after the meal were similar (intragastric titration = 20.6 +/- 7.3 ng min/ml versus serial dilution indicator = 23.5 +/- 9.8 ng min/ml) and individual 30-min gastrins during the two separate tests were highly correlated (r = 0.80 +/- 0.06, P less than 0.01). It is concluded that both meal-stimulated gastric acid secretion and serum gastrin concentrations as measured by intragastric titration and by the serial dilution indicator method produced similar results.

  14. Determination of Acidity Constants by Gradient Flow-Injection Titration

    ERIC Educational Resources Information Center

    Conceicao, Antonio C. L.; Minas da Piedade, Manuel E.

    2006-01-01

    A three-hour laboratory experiment, designed for an advanced undergraduate course in instrumental analysis that illustrates the application of the gradient chamber flow-injection titration (GCFIT) method with spectrophotometric detection to determine acidity constants is presented. The procedure involves the use of an acid-base indicator to obtain…

  15. An Olfactory Indicator for Acid-Base Titrations.

    ERIC Educational Resources Information Center

    Flair, Mark N.; Setzer, William N.

    1990-01-01

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

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

    ERIC Educational Resources Information Center

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

    2011-01-01

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

  17. The Acid-Base Titration of a Very Weak Acid: Boric Acid

    ERIC Educational Resources Information Center

    Celeste, M.; Azevedo, C.; Cavaleiro, Ana M. V.

    2012-01-01

    A laboratory experiment based on the titration of boric acid with strong base in the presence of d-mannitol is described. Boric acid is a very weak acid and direct titration with NaOH is not possible. An auxiliary reagent that contributes to the release of protons in a known stoichiometry facilitates the acid-base titration. Students obtain the…

  18. 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.

    PubMed

    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.

  19. Coulometric titration of bases in acetic acid and acetonitrile media.

    PubMed

    Vajgand, V J; Mihajlović, R

    1969-09-01

    The working conditions and the results for coulometric titration of milligram amounts of some bases in 0.1M sodium perchlorate in a mixture of acetic acid and acetic anhydride (1:6), are given. Determinations were made both by coulometric back-titration or direct titration at the platinum anode. Back-titration was done in the catholyte, by coulometric titration of the excess of added perchloric acid. The titration end-point was detected photometrically with Crystal Violet as indicator. The direct titration of bases was done at the platinum anode, in the same electrolyte, to which hydroquinone was added as anode depolarizer and as the source of hydrogen ions, Malachite Green being used as indicator. Similarly, bases can be determined in acetonitrile if sodium perchlorate, hydroquinone and Malachite Green are added to the solvent. Errors are below 1 %, and the precision is satisfactory.

  20. Acid Base Titrations in Nonaqueous Solvents and Solvent Mixtures

    NASA Astrophysics Data System (ADS)

    Barcza, Lajos; Buvári-Barcza, Ágnes

    2003-07-01

    The acid base determination of different substances by nonaqueous titrations is highly preferred in pharmaceutical analyses since the method is quantitative, exact, and reproducible. The modern interpretation of the reactions in nonaqueous solvents started in the last century, but several inconsistencies and unsolved problems can be found in the literature. The acid base theories of Brønsted Lowry and Lewis as well as the so-called solvent theory are outlined first, then the promoting (and leveling) and the differentiating effects are discussed on the basis of the hydrogen-bond concept. Emphasis is put on the properties of formic acid and acetic anhydride since their importance is increasing.

  1. A Closer Look at Acid-Base Olfactory Titrations

    ERIC Educational Resources Information Center

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

    2005-01-01

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

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

    PubMed

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

    2008-09-01

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

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

    PubMed

    Papanastasiou, G; Ziogas, I

    1995-06-01

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

  4. Potentiometric titration and equivalent weight of humic acid

    USGS Publications Warehouse

    Pommer, A.M.; Breger, I.A.

    1960-01-01

    The "acid nature" of humic acid has been controversial for many years. Some investigators claim that humic acid is a true weak acid, while others feel that its behaviour during potentiometric titration can be accounted for by colloidal adsorption of hydrogen ions. The acid character of humic acid has been reinvestigated using newly-derived relationships for the titration of weak acids with strong base. Re-interpreting the potentiometric titration data published by Thiele and Kettner in 1953, it was found that Merck humic acid behaves as a weak polyelectrolytic acid having an equivalent weight of 150, a pKa of 6.8 to 7.0, and a titration exponent of about 4.8. Interdretation of similar data pertaining to the titration of phenol-formaldehyde and pyrogallol-formaldehyde resins, considered to be analogs for humic acid by Thiele and Kettner, leads to the conclusion that it is not possible to differentiate between adsorption and acid-base reaction for these substances. ?? 1960.

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

    PubMed

    Maskula, S; Nyman, J; Ivaska, A

    2000-05-31

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

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

    ERIC Educational Resources Information Center

    McClendon, Michael

    1984-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2000-09-01

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

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

    PubMed

    Liao, Lifu; Yang, Jing; Yuan, Jintao

    2007-05-15

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

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

    PubMed

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

    2015-08-12

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

  10. Differential titration of bases in glacial acetic acid.

    PubMed

    Castellano, T; Medwick, T; Shinkai, J H; Bailey, L

    1981-01-01

    A study of bases in acetic acid and their differential titration was carried out. The overall basicity constants for 20 bases were measured in acetic acid, and the differential titration of five binary mixtures of variable delta pKb values in acetic acid was followed using a glass electrode-modified calomel electrode system. Agreement with literature values was good. A leveling diagram was constructed that indicated that bases stronger than aqueous pKb 10 are leveled to an acetous pKb 5.69, whereas weaker bases are not leveled but instead exhibit their own intrinsic basicity, with the acetous pKb to aqueous pKb values being linearly related (slope 1.18, correlation coefficient 0.962). A minimum acetous delta pKb of four units is required for the satisfactory differential titration of two bases in acetic acid.

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

    NASA Technical Reports Server (NTRS)

    Meites, L.

    1978-01-01

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

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

    PubMed

    Burakowski, Andrzej; Gliński, Jacek

    2014-01-01

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

  13. Using Spreadsheets to Produce Acid-Base Titration Curves.

    ERIC Educational Resources Information Center

    Cawley, Martin James; Parkinson, John

    1995-01-01

    Describes two spreadsheets for producing acid-base titration curves, one uses relatively simple cell formulae that can be written into the spreadsheet by inexperienced students and the second uses more complex formulae that are best written by the teacher. (JRH)

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

    PubMed Central

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

    1990-01-01

    An automatic system for acid-base titrations by electrogeneration of H+ and OH- ions, with potentiometric end-point detection, was developed. The system includes a PC-compatible computer for instrumental control, data acquisition and processing, which allows up to 13 samples to be analysed sequentially with no human intervention. The system performance was tested on the titration of standard solutions, which it carried out with low errors and RSD. It was subsequently applied to the analysis of various samples of environmental and nutritional interest, specifically waters, soft drinks and wines. PMID:18925283

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

    PubMed

    Söderman, Olle; Jönsson, Bengt; Olofsson, Gerd

    2006-02-23

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

  16. Determination of tertiary amines and salts of organic acids in acetic acid by catalytic thermometric titration.

    PubMed

    Vajgand, V J; Gaál, F F

    1967-03-01

    A new method of determination of tertiary amines and salts of organic adds in acetic acid solution, to which about 2 % of water and 8% acetic anhydride are added, is described. After the equivalence point, the excess of perchloric acid catalyses the exothermic reaction of water with acetic anhydride. The end-point is determined from the graph of temperature against volume of added titrant. If a slightly soluble compound is produced during the titration, the precision of the new method is superior to that of the potentiometric method.

  17. Analysis of a mixture of a known and an unknown weak acid by titration to a preset pH.

    PubMed

    Livaska, A

    1975-12-01

    The preset-pH titration method has been used to indicate the presence of a second acid when the titration curve (pH vs. volume of added titrant) seems to indicate only one acid. By use of the method even small amounts of propionic acid can be detected in an acetic acid solution despite the small value of Delta log K(H)(HA) = 0.18. Binary mixtures of acids may bs analysed when one acid is known, and log k(H)(HA) for the unknown acid may be found. Acetic acid, as the known acid, has been determined together with hydrochloric, mandelic, hydroxyacetic or boric acid or ammonium ion, with an error of about 1%. The method can be used in some cases for titration of ternary mixtures of one known and two unknown acids. Only the sum of the unknown acids can then be determined together with the known acid.

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

    PubMed

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

    2002-09-01

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

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

    PubMed

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

    1993-01-01

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

  20. Determination of berkelium by the method of spectrophotometric titration

    SciTech Connect

    Frolova, L.M.; Vityutnev, V.M.; Vasil'ev, V.M.

    1987-01-01

    The method that the authors propose consists of the following: berkelium is oxidized electrochemically, spectrophotometric titration of berkelium(IV) by a solution of the reducing agent is performed, and the amount of berkelium(IV) is determined according to the volume of the titrant, and considering the degree of oxidation of berkelium(III) to berkelium(IV), the total berkelium content in the sample is also determined. In this case the necessity for preliminary determination of the molar extinction coefficient of berkelium(IV) under the experimental conditions falls away. Moreover, the radiometric method of determining the berkelium content is not used. Successful titration requires selection of a reagent which, on the one hand, would rapidly reduce berkelium(VI), but on the other hand, neither itself nor the reaction products would interfere with the measurement of the optical density of berkelium(IV). As is well known, berkelium(IV) is quantitatively and rapidly reduced by hydrogen peroxide (10, 11), hydroxylamine (11), and nitrous acid (9). After preliminary experiments, they selected hydrogen peroxide and sodium nitrite as the titrants.

  1. Macromolecular competition titration method accessing thermodynamics of the unmodified macromolecule-ligand interactions through spectroscopic titrations of fluorescent analogs.

    PubMed

    Bujalowski, Wlodzimierz; Jezewska, Maria J

    2011-01-01

    Analysis of thermodynamically rigorous binding isotherms provides fundamental information about the energetics of the ligand-macromolecule interactions and often an invaluable insight about the structure of the formed complexes. The Macromolecular Competition Titration (MCT) method enables one to quantitatively obtain interaction parameters of protein-nucleic acid interactions, which may not be available by other methods, particularly for the unmodified long polymer lattices and specific nucleic acid substrates, if the binding is not accompanied by adequate spectroscopic signal changes. The method can be applied using different fluorescent nucleic acids or fluorophores, although the etheno-derivatives of nucleic acid are especially suitable as they are relatively easy to prepare, have significant blue fluorescence, their excitation band lies far from the protein absorption spectrum, and the modification eliminates the possibility of base pairing with other nucleic acids. The MCT method is not limited to the specific size of the reference nucleic acid. Particularly, a simple analysis of the competition titration experiments is described in which the fluorescent, short fragment of nucleic acid, spanning the exact site-size of the protein-nucleic acid complex, and binding with only a 1:1 stoichiometry to the protein, is used as a reference macromolecule. Although the MCT method is predominantly discussed as applied to studying protein-nucleic acid interactions, it can generally be applied to any ligand-macromolecule system by monitoring the association reaction using the spectroscopic signal originating from the reference macromolecule in the presence of the competing macromolecule, whose interaction parameters with the ligand are to be determined.

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

    PubMed

    Coelho, Lúcia H G; Gutz, Ivano G R

    2006-03-15

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

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

    PubMed

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

    2003-11-01

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

  4. Interaction between bisphenol A and tannic Acid: Spectroscopic titration approach

    NASA Astrophysics Data System (ADS)

    Omoike, Anselm; Brandt, Benjamin

    2011-06-01

    The interaction between tannic acid (TA) and bisphenol A (BPA), an endocrine disruptor, was studied by absorption and fluorescence titration techniques. The binding constants and corresponding thermodynamic parameters at different temperatures (294, 296, 298, 300 and 303 K) were determined. The intrinsic fluorescence of BPA was strongly quenched by TA and the quenching mechanism is attributed to static quenching. The thermodynamic data revealed that the formation of TA-BPA complex was exothermic, entropic-driven, and spontaneous. Furthermore, hydrogen and van der Waals interactions seem to be the major driving forces for the formation of the nonfluorescent TA-BPA complex.

  5. Interaction between bisphenol A and tannic acid: spectroscopic titration approach.

    PubMed

    Omoike, Anselm; Brandt, Benjamin

    2011-06-01

    The interaction between tannic acid (TA) and bisphenol A (BPA), an endocrine disruptor, was studied by absorption and fluorescence titration techniques. The binding constants and corresponding thermodynamic parameters at different temperatures (294, 296, 298, 300 and 303 K) were determined. The intrinsic fluorescence of BPA was strongly quenched by TA and the quenching mechanism is attributed to static quenching. The thermodynamic data revealed that the formation of TA-BPA complex was exothermic, entropic-driven, and spontaneous. Furthermore, hydrogen and van der Waals interactions seem to be the major driving forces for the formation of the nonfluorescent TA-BPA complex.

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

    PubMed

    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.

  7. Determination of free acidic and alkaline residues of protein via moving reaction boundary titration in microdevice electrophoresis.

    PubMed

    Wang, Hou-yu; Li, Si; Tang, Yun-yun; Dong, Jing-yu; Fan, Liu-yin; Cao, Cheng-xi

    2013-06-21

    As two important physico-chemical parameters, the acidic and alkaline residues of protein are of evident significance for the evaluation of protein properties and the design of relevant separation and analysis. However, there is still no electrophoretic method used for the direct detection of free acidic and alkaline residues of protein. Herein, we developed the concepts of moving reaction boundary (MRB) and MRB titration, relevant MRB titration theory, and the method of microdevice electrophoresis for the determination of free acidic and alkaline residues of protein. In the MRB titration, the boundary was created with acid or alkali and target protein immobilized via highly cross-linked polyacrylamide gel (PAG). It was theoretically revealed that the number of free acidic or alkaline residues of protein was as a function of MRB displacement in the electrophoretic titration system. As a proof of concept, seven model proteins were chosen for the determination of acidic or alkaline residues of protein via MRB titration. The results showed that the numbers of free acidic and alkaline residues of proteins detected were in good agreement with those obtained from the relevant amino sequences in the NCBI database, demonstrating the feasibility of the developed concept, theory and technique. The general methodology of MRB titration has potential application for inexpensive, facilitative and informative protein structure analysis of free acidic or alkaline residues of protein.

  8. Sequential injection redox or acid-base titration for determination of ascorbic acid or acetic acid.

    PubMed

    Lenghor, Narong; Jakmunee, Jaroon; Vilen, Michael; Sara, Rolf; Christian, Gary D; Grudpan, Kate

    2002-12-06

    Two sequential injection titration systems with spectrophotometric detection have been developed. The first system for determination of ascorbic acid was based on redox reaction between ascorbic acid and permanganate in an acidic medium and lead to a decrease in color intensity of permanganate, monitored at 525 nm. A linear dependence of peak area obtained with ascorbic acid concentration up to 1200 mg l(-1) was achieved. The relative standard deviation for 11 replicate determinations of 400 mg l(-1) ascorbic acid was 2.9%. The second system, for acetic acid determination, was based on acid-base titration of acetic acid with sodium hydroxide using phenolphthalein as an indicator. The decrease in color intensity of the indicator was proportional to the acid content. A linear calibration graph in the range of 2-8% w v(-1) of acetic acid with a relative standard deviation of 4.8% (5.0% w v(-1) acetic acid, n=11) was obtained. Sample throughputs of 60 h(-1) were achieved for both systems. The systems were successfully applied for the assays of ascorbic acid in vitamin C tablets and acetic acid content in vinegars, respectively.

  9. [Acids in coffee. XI. The proportion of individual acids in the total titratable acid].

    PubMed

    Engelhardt, U H; Maier, H G

    1985-07-01

    22 acids in ground roast coffees and instant coffees were determined by GLC of their silyl derivatives (after preseparation by gel electrophoresis) or isotachophoresis. The contribution to the total acidity (which was estimated by titration to pH 8 after cation exchange of the coffee solutions) was calculated for each individual acid. The mentioned acids contribute with 67% (roast coffee) and 72% (instant coffee) to the total acidity. In the first place citric acid (12.2% in roast coffee/10.7% in instant coffee), acetic acid (11.2%/8.8%) and the high molecular weight acids (8%/9%) contribute to the total acidity. Also to be mentioned are the shares of chlorogenic acids (9%/4.8%), formic acid (5.3%/4.6%), quinic acid (4.7%/5.9%), malic acid (3.9%/3%) and phosphoric acid (2.5%/5.2%). A notable difference in the contribution to total acidity between roast and instant coffee was found for phosphoric acid and pyrrolidonecarboxylic acid (0.7%/1.9%). It can be concluded that those two acids are formed or released from e.g. their esters in higher amounts than other acids during the production of instant coffee.

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

    PubMed

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

    2011-04-01

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

  11. Developing a multipoint titration method with a variable dose implementation for anaerobic digestion monitoring.

    PubMed

    Salonen, K; Leisola, M; Eerikäinen, T

    2009-01-01

    Determination of metabolites from an anaerobic digester with an acid base titration is considered as superior method for many reasons. This paper describes a practical at line compatible multipoint titration method. The titration procedure was improved by speed and data quality. A simple and novel control algorithm for estimating a variable titrant dose was derived for this purpose. This non-linear PI-controller like algorithm does not require any preliminary information from sample. Performance of this controller is superior compared to traditional linear PI-controllers. In addition, simplification for presenting polyprotic acids as a sum of multiple monoprotic acids is introduced along with a mathematical error examination. A method for inclusion of the ionic strength effect with stepwise iteration is shown. The titration model is presented with matrix notations enabling simple computation of all concentration estimates. All methods and algorithms are illustrated in the experimental part. A linear correlation better than 0.999 was obtained for both acetate and phosphate used as model compounds with slopes of 0.98 and 1.00 and average standard deviations of 0.6% and 0.8%, respectively. Furthermore, insensitivity of the presented method for overlapping buffer capacity curves was shown.

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

    PubMed

    Campbell, B H; Meites, L

    1974-02-01

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

  13. A Dating Analogy for Acid-Base Titration Problems

    NASA Astrophysics Data System (ADS)

    Delorenzo, Ronald

    1995-11-01

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

  14. 40 CFR Appendix A to Part 425 - Potassium Ferricyanide Titration Method

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 31 2013-07-01 2013-07-01 false Potassium Ferricyanide Titration..., App. A Appendix A to Part 425—Potassium Ferricyanide Titration Method Source The potassium ferricyanide titration method is based on method SLM 4/2 described in “Official Method of Analysis,” Society...

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

    ERIC Educational Resources Information Center

    Boblick, John M.

    1971-01-01

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

  16. Colloid Titration--A Rapid Method for the Determination of Charged Colloid.

    ERIC Educational Resources Information Center

    Ueno, Keihei; Kina, Ken'yu

    1985-01-01

    "Colloid titration" is a volumetric method for determining charged polyelectrolytes in aqueous solutions. The principle of colloid titration, reagents used in the procedure, methods of endpoint detection, preparation of reagent solutions, general procedure used, results obtained, and pH profile of colloid titration are considered. (JN)

  17. Instrumentation and Automated Photometric Titration Procedure for Total Acidity Determination in Red Wine Employing a Multicommuted Flow System

    PubMed Central

    Garcia, Ausberta Jesus Cabezas; Reis, Boaventura F.

    2006-01-01

    An automated procedure for photometric titration of red wine and associated instrumentation is described. The procedure was based on the flow-batch approach implemented employing multicommutation. The photometric detection was carried out using a homemade LED-based photometer. The mixing device, LED, and photodetector were attached to the titration chamber in order to form a compact and small-sized unit. The flow system comprised an automatic injector and three-way solenoid valves, which were controlled by a microcomputer through an electronic interface card. The software, written in Quick BASIC 4.5, was designed with abilities to accomplish all steps of the titration procedure including data acquisition and real-time processing to decide about the course of titration in the following step and so forth, until the titration endpoint was reached. The usefulness of the proposed titration system was demonstrated by analyzing red wine samples. When results were compared with those obtained using the AOAC reference method, no significant difference was observed at the 95% confidence level. A relative standard deviation of ca  2% (n=9 ) was obtained when processing a typical red wine sample containing 7.3 gl -1 total acidity expressed as tartaric acid. PMID:17671625

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

    PubMed

    Avdeef, A; Berger, C M

    2001-12-01

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

  19. [Titration comparative study of TOPINA Tablets in patients with localization related epilepsy: double-blind comparative study by rapid and slow titration methods].

    PubMed

    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.

  20. Automated titration method for use on blended asphalts

    DOEpatents

    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.

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

    PubMed

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

    2015-01-01

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

  2. Evaluation of the number of ionogenic groups of inulinase by acid-base titration.

    PubMed

    Kovaleva, T A; Holyavka, M G; Rezvan, S G; Kozhedub, S V

    2008-06-01

    Acid base titration showed that Aspergillus awamori inulinase includes 178 asparaginic and glutamic acid residues, 20 histidine, 10 serine, and 34 lysine and tyrosine residues. Denaturation temperature for this enzyme was calculated using analysis of the proportion of stabilizing and destabilizing amino acids in the molecule.

  3. Difference in amounts between titratable acid and total carboxylic acids produced by oral streptococci during sugar metabolism.

    PubMed

    Iwami, Y; Hata, S; Takahashi, N; Yamada, T

    1989-01-01

    The acid produced by the resting cells of Streptococcus mutants NCTC 10449 and HS 6 and S. sanguis ATCC 10556 during sugar metabolism was estimated with a pH-stat and a carboxylic acid analyzer. Lactic, formic, acetic, pyruvic, and carbonic acids were detected in the reaction mixtures, but propionic, citric, succinic, iso-butyric, butyric, iso-valeric, and valeric acids were not detected. The amount of titratable acid estimated by alkaline titration with the pH-stat was larger than the amount of total carboxylic acids estimated with the carboxylic acid analyzer. The difference in quantity between the titratable and the total carboxylic acids increased significantly with an increase in the period of incubation with sugar. Moreover, the value of the alkaline titration of standard lactic, formic, acetic, and pyruvic acids was equal to the amount analyzed with the carboxylic acid analyzer. The results indicated that these two streptococci produced not only these carboxylic acids but also other acid(s), possibly non-carboxylic acid(s), during their sugar metabolism.

  4. 40 CFR Appendix A to Part 425 - Potassium Ferricyanide Titration Method

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... Method A Appendix A to Part 425 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED..., App. A Appendix A to Part 425—Potassium Ferricyanide Titration Method Source The potassium... buffered sulfide solution is titrated with standard potassium ferricyanide solution in the presence of...

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

    SciTech Connect

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

    2013-01-01

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

  6. Linear titration plots for the analysis of mixtures of three weak acids or bases.

    PubMed

    Midgley, D; McCallum, C

    1984-06-01

    Linearly related functions have been derived which enable mixtures of three weak acids or bases in solution to be analysed by means of pH-titration data. This theory has been tested with data from the titration of a variety of mixtures of acids. The data required for the functions are pH, volume of titrant, the equilibrium constants relevant to the mixture, and an independently determined equivalence volume. This may be the equivalence volume for one of the components of the mixture or the sum of the equivalence volumes for any two or all three of the components. It is immaterial how this equivalence volume is obtained, but it is usually possible to obtain the total equivalence volume from data in another part of the same titration curve (when a large excess of titrant has been added).

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

    PubMed Central

    Tavčar, Eva; Turk, Erika; Kreft, Samo

    2012-01-01

    The most commonly used technique for water content determination is Karl-Fischer titration with electrometric detection, requiring specialized equipment. When appropriate equipment is not available, the method can be performed through visual detection of a titration endpoint, which does not enable an analysis of colored samples. Here, we developed a method with spectrophotometric detection of a titration endpoint, appropriate for moisture determination of colored samples. The reaction takes place in a sealed 4 ml cuvette. Detection is performed at 520 nm. Titration endpoint is determined from the graph of absorbance plotted against titration volume. The method has appropriate reproducibility (RSD = 4.3%), accuracy, and linearity (R2 = 0.997). PMID:22567558

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

    PubMed

    Gemene, Kebede L; Bakker, Eric

    2008-05-15

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

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

    PubMed

    Cui, Leyu; Puerto, Maura; López-Salinas, José L; Biswal, Sibani L; Hirasaki, George J

    2014-11-18

    The methylene blue (MB) two-phase titration method is a rapid and efficient method for determining the concentrations of anionic surfactants. The point at which the aqueous and chloroform phases appear equally blue is called Epton's end point. However, many inorganic anions, e.g., Cl(-), NO3(-), Br(-), and I(-), can form ion pairs with MB(+) and interfere with Epton's end point, resulting in the failure of the MB two-phase titration in high-salinity brine. Here we present a method to extend the MB two-phase titration method for determining the concentration of various cationic surfactants in both deionized water and high-salinity brine (22% total dissolved solid). A colorless end point, at which the blue color is completely transferred from the aqueous phase to the chloroform phase, is proposed as titration end point. Light absorbance at the characteristic wavelength of MB is measured using a spectrophotometer. When the absorbance falls below a threshold value of 0.04, the aqueous phase is considered colorless, indicating that the end point has been reached. By using this improved method, the overall error for the titration of a permanent cationic surfactant, e.g., dodecyltrimethylammonium bromide, in deionized (DI) water and high-salinity brine is 1.274% and 1.322% with limits of detection (LOD) of 0.149 and 0.215 mM, respectively. Compared to the traditional acid-base titration method, the error of this improved method for a switchable cationic surfactant, e.g., tertiary amine surfactant (Ethomeen C12), is 2.22% in DI water and 0.106% with LOD of 0.369 and 0.439 mM, respectively.

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

    NASA Astrophysics Data System (ADS)

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

    2016-05-01

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

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

    PubMed

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

    2008-09-10

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

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

    PubMed

    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.

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

    PubMed

    Karita, Shingo; Kaneta, Takashi

    2014-12-16

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

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

    PubMed

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

    2003-07-01

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

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

    PubMed

    Ivaska, A

    1974-06-01

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

  16. Liquefaction of Douglas Fir wood slurries: titration of acids and anions in aqueous product and feed slurries

    SciTech Connect

    Davis, H.G.

    1981-03-01

    After hydrolytic pretreatment, wood slurries contain substantial amounts of organic acids. Additional acids are produced during the liquefaction step whether or not there is prehydrolysis. The acids have pH's in the range of about 3 to 5 and are easily titrated potentiometrically with sodium hydroxide. Anions present in neutralized slurry or in aqueous product can be titrated with hydrogen chloride solution with appropriate corrections for sulfate if present, and for excess titrant at the low pH of the endpoint.

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

    PubMed

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

    2006-11-01

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

  18. Acid-base titration of melanocortin peptides: evidence of Trp rotational conformers interconversion.

    PubMed

    Fernandez, Roberto M; Vieira, Renata F F; Nakaie, Clóvis R; Lamy, M Teresa; Ito, Amando S

    2005-01-01

    Tryptophantime-resolved fluorescence was used to monitor acid-base titration properties of alpha-melanocyte stimulating hormone (alpha-MSH) and the biologically more potent analog [Nle4, D-Phe7]alpha -MSH (NDP-MSH), labeled or not with the paramagnetic amino acid probe 2,2,6,6-tetramthylpiperidine-N-oxyl-4-amino-4-carboxylic acid (Toac). Global analysis of fluorescence decay profiles measured in the pH range between 2.0 and 11.0 showed that, for each peptide, the data could be well fitted to three lifetimes whose values remained constant. The less populated short lifetime component changed little with pH and was ascribed to Trp g+ chi1 rotamer, in which electron transfer deactivation predominates over fluorescence. The long and intermediate lifetime preexponential factors interconverted along that pH interval and the result was interpreted as due to interconversion between Trp g- and trans chi1 rotamers, driven by conformational changes promoted by modifications in the ionization state of side-chain residues. The differences in the extent of interconversion in alpha-MSH and NDP-MSH are indicative of structural differences between the peptides, while titration curves suggest structural similarities between each peptide and its Toac-labeled species, in aqueous solution. Though less sensitive than fluorescence, the Toac electron spin resonance (ESR) isotropic hyperfine splitting parameter can also monitor the titration of side-chain residues located relatively far from the probe.

  19. Voltammetric iodometric titration of ascorbic acid with dead-stop end-point detection in fresh vegetables and fruit samples.

    PubMed

    Verdini, R A; Lagier, C M

    2000-07-01

    The present work describes a method for determining ascorbic acid, which combines iodometry with a voltammetric technique to detect the end point of the titration. In addition, the validity of the method applied to natural vegetable or fruit samples was assessed. The results were compared with those obtained by an accurate method such as HPLC using UV detection. Similar values of ascorbic acid for different natural samples were obtained by means of this approach (p > 0.05). The limit of quantification was 0.1 mg. This technique presents the advantage of other electroanalytical methods such as avoiding filtration or ultracentrifugation steps, with the additional benefit of using the platinum electrodes, which are routinely used in the laboratory. These facts allow a rapid and efficient quantification of ascorbic acid with very low cost of reagents and equipment.

  20. Effect of temperature on the acid-base properties of the alumina surface: microcalorimetry and acid-base titration experiments.

    PubMed

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

    2006-06-15

    Sorption reactions on natural or synthetic materials that can attenuate the migration of pollutants in the geosphere could be affected by temperature variations. Nevertheless, most of the theoretical models describing sorption reactions are at 25 degrees C. To check these models at different temperatures, experimental data such as the enthalpies of sorption are thus required. Highly sensitive microcalorimeters can now be used to determine the heat effects accompanying the sorption of radionuclides on oxide-water interfaces, but enthalpies of sorption cannot be extracted from microcalorimetric data without a clear knowledge of the thermodynamics of protonation and deprotonation of the oxide surface. However, the values reported in the literature show large discrepancies and one must conclude that, amazingly, this fundamental problem of proton binding is not yet resolved. We have thus undertaken to measure by titration microcalorimetry the heat effects accompanying proton exchange at the alumina-water interface at 25 degrees C. Based on (i) the surface sites speciation provided by a surface complexation model (built from acid-base titrations at 25 degrees C) and (ii) results of the microcalorimetric experiments, calculations have been made to extract the enthalpic variations associated respectively to first and second deprotonation of the alumina surface. Values obtained are deltaH1 = 80+/-10 kJ mol(-1) and deltaH2 = 5+/-3 kJ mol(-1). In a second step, these enthalpy values were used to calculate the alumina surface acidity constants at 50 degrees C via the van't Hoff equation. Then a theoretical titration curve at 50 degrees C was calculated and compared to the experimental alumina surface titration curve. Good agreement between the predicted acid-base titration curve and the experimental one was observed.

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

    PubMed

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

    2009-10-01

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

  2. A nine-point pH titration method to determine low-concentration VFA in municipal wastewater.

    PubMed

    Ai, Hainan; Zhang, Daijun; Lu, Peili; He, Qiang

    2011-01-01

    Characterization of volatile fatty acid (VFA) in wastewater is significant for understanding the wastewater nature and the wastewater treatment process optimization based on the usage of Activated Sludge Models (ASMs). In this study, a nine-point pH titration method was developed for the determination of low-concentration VFA in municipal wastewater. The method was evaluated using synthetic wastewater containing VFA with the concentration of 10-50 mg/l and the possible interfering buffer systems of carbonate, phosphate and ammonium similar to those in real municipal wastewater. In addition, the further evaluation was conducted through the assay of real wastewater using chromatography as reference. The results showed that the recovery of VFA in the synthetic wastewater was 92%-102 and the coefficient of variance (CV) of reduplicate measurements 1.68%-4.72%. The changing content of the buffering substances had little effect on the accuracy of the method. Moreover, the titration method was agreed with chromatography in the determination of VFA in real municipal wastewater with R(2)= 0.9987 and CV =1.3-1.7. The nine-point pH titration method is capable of satisfied determination of low-concentration VFA in municipal wastewater.

  3. Sulfur in graphite by combustion-iodometric titration method

    SciTech Connect

    Not Available

    1981-01-01

    The method covers the determination of sulfur in graphite in the concentration range of 1 to 200 ..mu..g/g in a l-g sample or 5 to 1000 ..mu..g/g in a 0.2-g sample. The method includes a discussion of interferences, apparatus, reagents and materials, procedure, calculations, and precision. (JMT)

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

    ERIC Educational Resources Information Center

    Gilbert, George L., Ed.

    1979-01-01

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

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

    SciTech Connect

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

    2008-01-01

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

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

    PubMed

    Maslarska, Vania; Tencheva, Jasmina; Budevsky, Omortag

    2003-01-01

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

  7. MOISTURE IN COTTON BY THE KARL FISCHER TITRATION REFERENCE METHOD

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Moisture is a critical parameter that influences many aspects of cotton fiber from harvesting and ginning to various fiber properties. Because of their importance, reference moisture methods that are more accurate than the existing oven-drying techniques and relatively easy to generate results are ...

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

    NASA Technical Reports Server (NTRS)

    Sprengnether, Michele; Prinn, Ronald G.

    1994-01-01

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

  9. Rapid air titration method for determining SO/sub 2/ concentration in inhalation chambers

    SciTech Connect

    Snyder, E.A.; Palmes, E.D.

    1985-06-01

    A rapid air titration method for determining SO/sub 2/ concentration in inhalation chambers has been validated using the pararosaniline-formaldehyde (PRA) method of West and Gaeke. This air-titration (iodate) method is an adaptation of iodometric methods using a starch indicator. Potassium iodate and an excess of potassium iodide are used in the reaction. Sampling is completed in ten minutes or less and concentration is calculated by use of a simple formula. Linear equations were derived over the range of concentrations from 0.5 to 100 ppm SO/sub 2/ for uncorrected iodate bubbler results, data corrected for tandem bubbler concentrations and data corrected for mean iodate bubbler efficiency. Linear correlation with the PRA method over this range was 0.999 for all three sets of data.

  10. Isothermal titration calorimetry - a new method for the quantification of microbial degradation of trace pollutants.

    PubMed

    Mariana, F; Buchholz, F; Harms, H; Yong, Z; Yao, J; Maskow, T

    2010-07-01

    The environmental fate and, in particular, biodegradation rates of hydrophobic organic compounds (HOC) are of high interest due to the ubiquity, persistence, and potential health effects of these compounds. HOC tend to interact with bioreactor materials and sampling devices and are frequently volatile, so that conventionally derived degradation parameters are often biased. We report on the development and validation of a novel calorimetric approach that serves to gain real time information on the kinetics and the physiology of HOC bioconversion in aqueous systems while overcoming weaknesses of conventional biodegradation experiments. Soil bacteria Mycobacterium frederiksbergense LB501T, Rhodococcus erythropolis K2-3 and Pseudomonas putida G7 were exposed to pulsed titrations of dissolved anthracene, 4-(2,4-dichlorophenoxy)butyric acid or naphthalene, respectively, and the thermal responses were monitored. The combinations of strains and pollutants were selected as examples for complete and partial biodegradation and complete degradation with storage product formation, respectively. Heat production signals were interpreted thermodynamically and in terms of Michaelis-Menten kinetics. The half-saturation constant k(D) and the degradation rate r(D)(Max) were derived. Comparison with conventional methods shows the suitability to extract kinetic degradation parameters of organic trace pollutants from simple ITC experiments, while thermodynamic interpretation provided further information about the metabolic fate of HOC compounds.

  11. Interaction of gymnemic acid with cyclodextrins analyzed by isothermal titration calorimetry, NMR and dynamic light scattering.

    PubMed

    Izutani, Yusuke; Kanaori, Kenji; Imoto, Toshiaki; Oda, Masayuki

    2005-12-01

    The physiological phenomenon that the antisweet taste effect of gymnemic acid (GA) is diminished by application of gamma-cyclodextrin (gamma-CD) to the mouth was evaluated at the molecular level using isothermal titration calorimetry, NMR and dynamic light scattering. These analyses showed that GA specifically binds to gamma-CD. Thermodynamic analysis using isothermal titration calorimetry revealed that the association constant of GA and gamma-CD is 10(5)-10(6) m(-1) with favorable enthalpy and entropy changes. The heat capacity change was negative and large, despite the change in accessible surface area upon binding being small. These thermodynamics indicate that the binding is dominated by hydrophobic interactions, which is in agreement with inclusion complex formation of gamma-CD. In addition, NMR measurements showed that in solution the spectra of GA are broad and sharpened by the addition of gamma-CD, indicating that unbound GA is in a water-soluble aggregate that is dispersed when it forms a complex with gamma-CD. Dynamic light scattering showed that the average diameter of unbound GA is > 30 nm and that of GA and gamma-CD complex is 2.2 nm, similar to unbound gamma-CD, supporting the aggregate property of GA and the inclusion complexation of GA by gamma-CD.

  12. Canadian Tire Money: An Analogy for Use When Discussing Weak Acid Strong Base Titrations

    NASA Astrophysics Data System (ADS)

    Last, Arthur M.

    2003-12-01

    A simple analogy can often provide an instructor with a means of helping students to understand an unfamiliar concept. An analogy involving money can be particularly helpful as most students have experience in dealing with a range of financial transactions in their everyday lives. In this article, use is made of the practice of one well-known Canadian retail chain in returning to its customers a small percentage of an item's purchase price in the form of imitation bank notes that can subsequently be spent in the chain's stores. An analogy is drawn between this practice and the determination of the pKa of a weak acid by titrating it with a strong base, taking into account the hydrolysis of the anion produced.

  13. 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).

    PubMed

    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.

  14. Flow cytometry as an improved method for the titration of Chlamydiaceae and other intracellular bacteria.

    PubMed

    Käser, T; Pasternak, J A; Hamonic, G; Rieder, M; Lai, K; Delgado-Ortega, M; Gerdts, V; Meurens, F

    2016-05-01

    Chlamydiaceae is a family of intracellular bacteria causing a range of diverse pathological outcomes. The most devastating human diseases are ocular infections with C. trachomatis leading to blindness and genital infections causing pelvic inflammatory disease with long-term sequelae including infertility and chronic pelvic pain. In order to enable the comparison of experiments between laboratories investigating host-chlamydia interactions, the infectious titer has to be determined. Titer determination of chlamydia is most commonly performed via microscopy of host cells infected with a serial dilution of chlamydia. However, other methods including fluorescent ELISpot (Fluorospot) and DNA Chip Scanning Technology have also been proposed to enumerate chlamydia-infected cells. For viruses, flow cytometry has been suggested as a superior alternative to standard titration methods. In this study we compared the use of flow cytometry with microscopy and Fluorospot for the titration of C. suis as a representative of other intracellular bacteria. Titer determination via Fluorospot was unreliable, while titration via microscopy led to a linear read-out range of 16 - 64 dilutions and moderate reproducibility with acceptable standard deviations within and between investigators. In contrast, flow cytometry had a vast linear read-out range of 1,024 dilutions and the lowest standard deviations given a basic training in these methods. In addition, flow cytometry was faster and material costs were lower compared to microscopy. Flow cytometry offers a fast, cheap, precise, and reproducible alternative for the titration of intracellular bacteria like C. suis. © 2016 International Society for Advancement of Cytometry.

  15. Titration Curves: Fact and Fiction.

    ERIC Educational Resources Information Center

    Chamberlain, John

    1997-01-01

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

  16. Investigation of the formation of peroxide in. gamma. -irradiated polyethylene by the method of iodometric titration

    SciTech Connect

    Savost'yanov, V.S.; Kritskaya, D.A.; Ponomarev, A.N.

    1986-09-01

    The concentrations of hydroperoxides (HP) and dialkyl peroxides (DAP) in polyethylene (PE) powder, ..gamma.. irradiated in air at 295 K at a dose of 0.22-2.8 J/(kg x sec) up to doses of 16-300 kJ/kg, were determined by various methods of iodometric titration. Under the indicated conditions, the HP concentration reached 0.18 mole/kg, DPA 0.07 mole/kg, G /SUB HP/ was 8.3 1/100 eV; G /SUB GP/ ..integral..I /SUP -0.5/ . On the basis of the total absence of grafting of acrylamide onto ..gamma..-irradiated PE after reduction during titration of HP in it, it was concluded that grafted polymerization is initiated by the radicals of thermal decomposition of HP in PE.

  17. Amperometric, Bipotentiometric, and Coulometric Titration.

    ERIC Educational Resources Information Center

    Stock, John T.

    1984-01-01

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

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

    Technology Transfer Automated Retrieval System (TEKTRAN)

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

  19. Assembling and Using an LED-Based Detector to Monitor Absorbance Changes during Acid-Base Titrations

    ERIC Educational Resources Information Center

    Santos, Willy G.; Cavalheiro, E´der T. G.

    2015-01-01

    A simple photometric assembly based in an LED as a light source and a photodiode as a detector is proposed in order to follow the absorbance changes as a function of the titrant volume added during the course of acid-base titrations in the presence of a suitable visual indicator. The simplicity and low cost of the electronic device allow the…

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

    SciTech Connect

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

    2008-01-01

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

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

    PubMed

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

    2008-11-01

    Many geochemical reactions that control aqueous metal concentrations are directly affected by solution pH. However, changes in solution pH are strongly buffered by various aqueous phase and solid phase precipitation/dissolution and adsorption/desorption reactions. The ability to predict acid-base behavior of the soil-solution system is thus critical to predict metal transport under variable pH conditions. This studywas undertaken to develop a practical generic geochemical modeling approach to predict aqueous and solid phase concentrations of metals and anions during conditions of acid or base additions. The method of Spalding and Spalding was utilized to model soil buffer capacity and pH-dependent cation exchange capacity by treating aquifer solids as a polyprotic acid. To simulate the dynamic and pH-dependent anion exchange capacity, the aquifer solids were simultaneously treated as a polyprotic base controlled by mineral precipitation/ dissolution reactions. An equilibrium reaction model that describes aqueous complexation, precipitation, sorption and soil buffering with pH-dependent ion exchange was developed using HydroGeoChem v5.0 (HGC5). Comparison of model results with experimental titration data of pH, Al, Ca, Mg, Sr, Mn, Ni, Co, and SO4(2-) for contaminated sediments indicated close agreement suggesting that the model could potentially be used to predictthe acid-base behavior of the sediment-solution system under variable pH conditions.

  2. Estimating iron and aluminum content of acid mine discharge from a north-central Pennsylvania coal field by use of acidity titration curves

    USGS Publications Warehouse

    Ott, A.N.

    1986-01-01

    Determination of acidity provides a value that denotes the quantitative capacity of the sample water to neutralize a strong base to a particular pH. However, much additional information can be obtained from this determination if a titration curve is constructed from recorded data of titrant increments and their corresponding pH values. The curve can be used to identify buffer capabilities, the acidity with respect to any pH value within the curve limit, and, in the case of acid mine drainage from north-central Pennsylvania, the identification and estimation of the concentration of dissolved ferrous iron, ferric iron, and aluminum. Through use of titration curves, a relationship was observed for the acid mine drainage between: (1) the titratable acidity (as milligrams per liter calcium carbonate) to pH 4.0 and the concentration of dissolved ferric iron; and (2) the titratable acidity (as milligrams per liter calcium carbonate) from pH 4.0 to 5.0 and the concentration of dissolved aluminum. The presence of dissolved ferrous iron can be detected by the buffering effect exhibited in the area between pH 5.5 to 7.5. The concentration of ferrous iron is estimated by difference between the concentrations of ferric iron in an oxidized and unoxidized sample. Interferences in any of the titrations from manganese, magnesium, and aluminate, appear to be negligible within the pH range of interest.

  3. Characterization of molecularly imprinted polymers using a new polar solvent titration method.

    PubMed

    Song, Di; Zhang, Yagang; Geer, Michael F; Shimizu, Ken D

    2014-07-01

    A new method of characterizing molecularly imprinted polymers (MIPs) was developed and tested, which provides a more accurate means of identifying and measuring the molecular imprinting effect. In the new polar solvent titration method, a series of imprinted and non-imprinted polymers were prepared in solutions containing increasing concentrations of a polar solvent. The polar solvent additives systematically disrupted the templation and monomer aggregation processes in the prepolymerization solutions, and the extent of disruption was captured by the polymerization process. The changes in binding capacity within each series of polymers were measured, providing a quantitative assessment of the templation and monomer aggregation processes in the imprinted and non-imprinted polymers. The new method was tested using three different diphenyl phosphate imprinted polymers made using three different urea functional monomers. Each monomer had varying efficiencies of templation and monomer aggregation. The new MIP characterization method was found to have several advantages. To independently verify the new characterization method, the MIPs were also characterized using traditional binding isotherm analyses. The two methods appeared to give consistent conclusions. First, the polar solvent titration method is less susceptible to false positives in identifying the imprinting effect. Second, the method is able to differentiate and quantify changes in binding capacity, as measured at a fixed guest and polymer concentration, arising from templation or monomer aggregation processes in the prepolymerization solution. Third, the method was also easy to carry out, taking advantage of the ease of preparing MIPs.

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

    PubMed

    Zikolov, P; Zikolova, T; Budevsky, O

    1976-08-01

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

  5. Electrostatic calculations of amino acid titration and electron transfer, Q-AQB-->QAQ-B, in the reaction center.

    PubMed Central

    Beroza, P; Fredkin, D R; Okamura, M Y; Feher, G

    1995-01-01

    The titration of amino acids and the energetics of electron transfer from the primary electron acceptor (QA) to the secondary electron acceptor (QB) in the photosynthetic reaction center of Rhodobacter sphaeroides are calculated using a continuum electrostatic model. Strong electrostatic interactions between titrating sites give rise to complex titration curves. Glu L212 is calculated to have an anomalously broad titration curve, which explains the seemingly contradictory experimental results concerning its pKa. The electrostatic field following electron transfer shifts the average protonation of amino acids near the quinones. The pH dependence of the free energy between Q-AQB and QAQ-B calculated from these shifts is in good agreement with experiment. However, the calculated absolute free energy difference is in severe disagreement (by approximately 230 meV) with the observed experimental value, i.e., electron transfer from Q-A to QB is calculated to be unfavorable. The large stabilization energy of the Q-A state arises from the predominantly positively charged residues in the vicinity of QA in contrast to the predominantly negatively charged residues near QB. The discrepancy between calculated and experimental values for delta G(Q-AQB-->QAQ-B) points to limitations of the continuum electrostatic model. Inclusion of other contributions to the energetics (e.g., protein motion following quinone reduction) that may improve the agreement between theory and experiment are discussed. PMID:7647231

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

    SciTech Connect

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

    2010-01-01

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

  7. Surface characteristic changes of dental ceramics after cyclic immersion in acidic agents and titratable acidity.

    PubMed

    Junpoom, Peerapong; Kukiattrakoon, Boonlert; Hengtrakool, Chanothai

    2010-12-01

    The potential erosive effect of acidic food, sour fruits and drinks on all-ceramic restorations used in dentistry has not been clearly documented. Surface characteristic changes have been evaluated and compared for disc-shaped specimens (diameter 12.0 mm and thickness 2.0 mm) of fluorapatite-leucite and fluorapatite ceramics using various storage agents (deionized water, citrate buffer solution, pineapple juice, green mango juice, cola soft drink and 4% acetic acid). Immersion in pineapple juice, green mango juice, cola soft drink and 4% acetic acid for 16 hours produce significant increases in surface roughness for both types of ceramics investigated.

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

    NASA Astrophysics Data System (ADS)

    Sung, Lung-Yu; Lu, Chia-Jung

    2014-09-01

    This study introduced a quantitative method that can be used to measure the concentration of analytes directly from a single-beam spectrum of open-path Fourier Transform Infrared Spectroscopy (OP-FTIR). The peak shapes of the analytes in a single-beam spectrum were gradually canceled (i.e., "titrated") by dividing an aliquot of a standard transmittance spectrum with a known concentration, and the sum of the squared differential synthetic spectrum was calculated as an indicator for the end point of this titration. The quantity of a standard transmittance spectrum that is needed to reach the end point can be used to calculate the concentrations of the analytes. A NIST traceable gas standard containing six known compounds was used to compare the quantitative accuracy of both this titration method and that of a classic least square (CLS) using a closed-cell FTIR spectrum. The continuous FTIR analysis of industrial exhausting stack showed that concentration trends were consistent between the CLS and titration methods. The titration method allowed the quantification to be performed without the need of a clean single-beam background spectrum, which was beneficial for the field measurement of OP-FTIR. Persistent constituents of the atmosphere, such as NH3, CH4 and CO, were successfully quantified using the single-beam titration method with OP-FTIR data that is normally inaccurate when using the CLS method due to the lack of a suitable background spectrum. Also, the synthetic spectrum at the titration end point contained virtually no peaks of analytes, but it did contain the remaining information needed to provide an alternative means of obtaining an ideal single-beam background for OP-FTIR.

  9. pH Titratable Superparamagnetic Iron Oxide for Improved Nanoparticle Accumulation in Acidic Tumor Microenvironments

    PubMed Central

    Crayton, Samuel H.; Tsourkas, Andrew

    2011-01-01

    A wide variety of nanoparticle platforms are being developed for the diagnosis and treatment of malignancy. While many of these are passively targeted or rely on receptor-ligand interactions, metabolically directed nanoparticles provide a complementary approach. It is known that both primary and secondary events in tumorigensis alter the metabolic profile of developing and metastatic cancers. One highly conserved metabolic phenotype is a state of up-regulated glycolysis and reduced use of oxidative phosphorylation, even when oxygen tension is not limiting. This metabolic shift, termed the Warburg effect, creates a “hostile” tumor microenvironment with increased levels of lactic acid and low extracellular pH. In order to exploit this phenomenon and improve the delivery of nanoparticle platforms to a wide variety of tumors, a pH-responsive iron oxide nanoparticle was designed. Specifically, glycol chitosan (GC), a water-soluble polymer with pH titratable charge, was conjugated to the surface of superparamagnetic iron oxide nanoparticles (SPIO) to generate a T2*-weighted MR contrast agent that responds to alterations in its surrounding pH. Compared to control nanoparticles that lack pH sensitivity, these GC-SPIO nanoparticles demonstrated potent pH-dependent cellular association and MR contrast in vitro. In murine tumor models GC-SPIO also generated robust T2*-weighted contrast, which correlated with increased delivery of the agent to the tumor site, measured quantitatively by inductively coupled plasma mass spectrometry. Importantly, the increased delivery of GC-SPIO nanoparticles cannot be solely attributed to the commonly observed enhanced permeability and retention effect, since these nanoparticles have similar physical properties and blood circulation times as control agents. PMID:22035454

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

    PubMed

    Weinreich, Wenke; Acker, Jörg; Gräber, Iris

    2007-03-30

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

  11. Aggregation property of glycyrrhizic acid and its interaction with cyclodextrins analyzed by dynamic light scattering, isothermal titration calorimetry, and NMR.

    PubMed

    Izutani, Yusuke; Kanaori, Kenji; Oda, Masayuki

    2014-06-17

    The structural properties of glycyrrhizic acid, a sweet-tasting constituent of Glycyrrhiza glabra, and its interaction with cyclodextrins were analyzed using dynamic light scattering, isothermal titration calorimetry, and NMR. The dynamic light scattering and NMR studies showed that glycyrrhizic acid forms a water-soluble aggregate that disperses upon the addition of γ-cyclodextrin. The high sweetness of glycyrrhizic acid can be closely correlated with this aggregation, because the multimers of glycyrrhizic acid can simultaneously bind to the sweet taste receptors on the human tongue. The isothermal titration calorimetry experiments demonstrated that γ-cyclodextrin binds to glycyrrhizic acid more strongly than β-cyclodextrin, however, both reactions are accompanied by a favorable change in binding entropy. Considering the large negative change in heat capacity that is observed during the binding of γ-cyclodextrin, the main driving force for the binding is hydrophobic interactions with dehydration, which is typical for inclusion complex. NMR experiments showed that γ-cyclodextrin interacts with the central part of the aglycone moiety, not the glucuronic acid moieties, resulting in high binding affinity. It should also be noted that the two distinct complexes of glycyrrhizic acid with γ-cyclodextrin would exist in aqueous solution.

  12. Development and validation of a nonaqueous titration with perchloric acid to determine sparfloxacin in tablets.

    PubMed

    Marona, H R; Schapoval, E E

    2001-09-01

    A simple, rapid and inexpensive method for the determination of sparfloxacin in tablets is described. The procedure is based on the use of volumetric dosage in a nonaqueous medium in glacial acetic acid with 0.1 M perchloric acid. The method validation yielded good results and included precision and accuracy. It was also found that the excipients in the commercial tablet preparation did not interfere with the assay.

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

    PubMed

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

    1997-11-01

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

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

    ERIC Educational Resources Information Center

    Dungey, Keenan E.; Epstein, Paul

    2007-01-01

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

  15. Alternative methods of titrating continuous positive airway pressure: a large multicenter study.

    PubMed

    Masa, Juan F; Jiménez, Antonio; Durán, Joaquín; Capote, Francisco; Monasterio, Carmen; Mayos, Mercedes; Terán, Joaquín; Hernández, Lourdes; Barbé, Ferrán; Maimó, Andrés; Rubio, Manuela; Montserrat, José M

    2004-12-01

    Standard practice for continuous positive airway pressure (CPAP) treatment in sleep apnea and hypopnea syndrome (SAHS) requires pressure titration during attended laboratory polysomnography. However, polysomnographic titration is expensive and time-consuming. The aim of this study was to ascertain, in a large sample of CPAP-naive patients, whether CPAP titration performed by an unattended domiciliary autoadjusted CPAP device or with a predicted formula was as effective as CPAP titration performed by full polysomnography. The main outcomes were the apnea-hypopnea index and the subjective daytime sleepiness. We included 360 patients with SAHS requiring CPAP treatment. Patients were randomly allocated into three groups: standard, autoadjusted, and predicted formula titration with domiciliary adjustment. The follow-up period was 12 weeks. With CPAP treatment, the improvement in subjective sleepiness and apnea-hypopnea index was very similar in the three groups. There were no differences in the objective compliance of CPAP treatment and in the dropout rate of the three groups at the end of the follow-up. Autoadjusted titration at home and predicted formula titration with domiciliary adjustment can replace standard titration. These procedures could lead to considerable savings in cost and to significant reductions in the waiting list.

  16. A one-step colorimetric acid-base titration sensor using a complementary color changing coordination system.

    PubMed

    Cho, Hui Hun; Kim, Si Hyun; Heo, Jun Hyuk; Moon, Young Eel; Choi, Young Hun; Lim, Dong Cheol; Han, Kwon-Hoon; Lee, Jung Heon

    2016-06-21

    We report the development of a colorimetric sensor that allows for the quantitative measurement of the acid content via acid-base titration in a single-step. In order to create the sensor, we used a cobalt coordination system (Co-complex sensor) that changes from greenish blue colored Co(H2O)4(OH)2 to pink colored Co(H2O)6(2+) after neutralization. Greenish blue and pink are two complementary colors with a strong contrast. As a certain amount of acid is introduced to the Co-complex sensor, a portion of greenish blue colored Co(H2O)4(OH)2 changes to pink colored Co(H2O)6(2+), producing a different color. As the ratio of greenish blue and pink in the Co-complex sensor is determined by the amount of neutralization reaction occurring between Co(H2O)4(OH)2 and an acid, the sensor produced a spectrum of green, yellow green, brown, orange, and pink colors depending on the acid content. In contrast, the color change appeared only beyond the end point for normal acid-base titration. When we mixed this Co-complex sensor with different concentrations of citric acid, tartaric acid, and malic acid, three representative organic acids in fruits, we observed distinct color changes for each sample. This color change could also be observed in real fruit juice. When we treated the Co-complex sensor with real tangerine juice, it generated diverse colors depending on the concentration of citric acid in each sample. These results provide a new angle on simple but quantitative measurements of analytes for on-site usage in various applications, such as in food, farms, and the drug industry.

  17. Sequential injection titration with spectrophotometric detection for the assay of acidity in fruit juices.

    PubMed

    Jakmunee, Jaroon; Rujiralai, Thitima; Grudpan, Kate

    2006-01-01

    A simple sequential injection analysis (SIA) with spectrophotometric detection for an assay of acidity in fruit juice was investigated. An alkaline reagent (sodium hydroxide), a sample and an indicator (phenolphthalein) were first aspirated and stacked as adjacent zones in a holding coil. With flow reversal through a reaction coil to the detector, zone penetration occurred, leading to a neutralization reaction that caused a decrease in the color intensity of the indicator being monitored for absorbance at 552 nm. The effects of various parameters were studied. Linear calibration graphs for acidities of 0.2 - 1.0 and 0.5 - 2.5% w/v citric acid as a standard, with a relative standard deviation of 1% (acidity of 0.3 - 0.6% w/v as citric acid, n=11) and a sample throughput of 30 samples h(-1), were achieved. The developed method was validated by a standard titrimetric method for assaying the acidity of fruit juice samples.

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

    SciTech Connect

    Black, Stuart; Ferrell, Jack R.

    2017-01-01

    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 degrees C.

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

    PubMed

    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.

  20. Photometric titration of small quantities of metals with ethylenediaminetetra-acetic acid.

    PubMed

    Belcher, R; Crossland, B; Fennell, T R

    1969-09-01

    A commercially available photometric titration apparatus has been used for the determination ofAl, Ba, Bi, Ca, Cd, Co, Mg, Mn, Ni and Zn in the 4-20 mug range and of Hg in the 16-32 mug range. Pooled standard deviations (32 determinations) of between 0.09 and 0.15 mug were found for all the metals except Ba (0.20 mug) and Hg (0.44 mug, 24 determinations).

  1. Accurate Three States Model for Amino Acids with Two Chemically Coupled Titrating Sites in Explicit Solvent Atomistic Constant pH Simulations and pKa Calculations.

    PubMed

    Dobrev, Plamen; Donnini, Serena; Groenhof, Gerrit; Grubmüller, Helmut

    2017-01-10

    Correct protonation of titratable groups in biomolecules is crucial for their accurate description by molecular dynamics simulations. In the context of constant pH simulations, an additional protonation degree of freedom is introduced for each titratable site, allowing the protonation state to change dynamically with changing structure or electrostatics. Here, we extend previous approaches for an accurate description of chemically coupled titrating sites. A second reaction coordinate is used to switch between two tautomeric states of an amino acid with chemically coupled titratable sites, such as aspartate (Asp), glutamate (Glu), and histidine (His). To this aim, we test a scheme involving three protonation states. To facilitate charge neutrality as required for periodic boundary conditions and Particle Mesh Ewald (PME) electrostatics, titration of each respective amino acid is coupled to a "water" molecule that is charged in the opposite direction. Additionally, a force field modification for Amber99sb is introduced and tested for the description of carboxyl group protonation. Our three states model is tested by titration simulations of Asp, Glu, and His, yielding a good agreement, reproducing the correct geometry of the groups in their different protonation forms. We further show that the ion concentration change due to the neutralizing "water" molecules does not significantly affect the protonation free energies of the titratable groups, suggesting that the three states model provides a good description of biomolecular dynamics at constant pH.

  2. Liquid-liquid interfaces as potentiometric ion-sensors-I The n-butanol-water interface as indicating sensor for the potentiometric titration of some acids and bases.

    PubMed

    Liteanu, C; Mioşcu, M

    1972-07-01

    The property that liquid-liquid interfaces modify their electrical charge as a function of the composition of the two phases in contact has been used to detect the end-points in a series of acid-base titrations in the aqueous phase. Although the titration curves are not classical in shape, the equivalence points can be located if the solutions are not too dilute. Good results for concentrations down to 10(-3)N have been obtained. The electrode has a fast response. The influence of surface-active substances on the titration has also been investigated.

  3. A protocol analysis of the influence of technology on students' actions, verbal commentary, and thought processes during the performance of acid-base titrations

    NASA Astrophysics Data System (ADS)

    Nakhleh, Mary B.; Krajcik, Joseph S.

    We investigated students' initial and final understanding of acid-base concepts and their concurrent thought processes and actions during the process of acid-base titrations. Here we report students' actions and thought processes while titrating. Different levels of information were presented by three technologies: chemical indicators, pH meters, and microcomputer-based laboratories. We speculated that the level of information would influence students' actions and thought processes, as expressed in verbal commentary. Data were collected from 14 secondary chemistry students. Each student used one technology to titrate a strong acid, a weak acid, and a polyprotic acid with a strong base. They verbalized their thoughts while titrating. Students then graphed pH versus volume of base and discussed the titration with the investigator. Verbal commentaries were coded and analyzed for patterns in actions and for frequency of statement categories. Drawings were analyzed for shape, scale, and direction; discussions were analyzed for understanding of acid-base neutralization. We found that the technology's level of information affected the focus of students' observations. The microcomputer group focused primarily on the graph; other groups exhibited multiple foci. We speculate the screen display functions as an auxiliary short-term memory. The discussion data also reveal that students held three main ideas about how acids and bases behave when mixed. Implications for instruction are discussed.

  4. Reference test methods for total water in lint cotton by Karl Fischer Titration and low temperature distillation

    Technology Transfer Automated Retrieval System (TEKTRAN)

    In a study of comparability of total water contents (%) of conditioned cottons by Karl Fischer Titration (KFT) and Low Temperature Distillation (LTD) reference methods, we demonstrated a match of averaged results based on a large number of replications and weighing the test specimens at the same tim...

  5. Repeated dose titration versus age-based method in electroconvulsive therapy: a pilot study.

    PubMed

    Aten, Jan Jaap; Oudega, Mardien; van Exel, Eric; Stek, Max L; van Waarde, Jeroen A

    2015-06-01

    In electroconvulsive therapy (ECT), a dose titration method (DTM) was suggested to be more individualized and therefore more accurate than formula-based dosing methods. A repeated DTM (every sixth session and dose adjustment accordingly) was compared to an age-based method (ABM) regarding treatment characteristics, clinical outcome, and cognitive functioning after ECT. Thirty-nine unipolar depressed patients dosed using repeated DTM and 40 matched patients treated with ABM were compared. Montgomery-Åsberg Depression Rating Scale (MADRS) and Mini-Mental State Examination (MMSE) were assessed at baseline and at the end of the index course, as well as the total number of ECT sessions. Both groups were similar regarding age, sex, psychotic features, mean baseline MADRS, and median baseline MMSE. At the end of the index course, the two methods showed equal outcome (mean end MADRS, 11.6 ± 8.3 in DTM and 9.5 ± 7.6 in ABM (P = 0.26); median end MMSE, 28 (25-29) and 28 (25-29.8), respectively (P = 0.81). However, the median number of all ECT sessions differed 16 (11-22) in DTM versus 12 (10-14.8) in ABM; P = 0.02]. Using regression analysis, dosing method and age were independently associated with the total number of ECT sessions, with less sessions needed in ABM (P = 0.02) and in older patients (P = 0.001). In this comparative cohort study, ABM and DTM showed equal outcome for depression and cognition. However, the median ECT course duration in repeated DTM appeared longer. Additionally, higher age was associated with shorter ECT courses regardless of the dosing method. Further prospective studies are needed to confirm these findings.

  6. Effects of dairy factory, milk casein content and titratable acidity on coagulation properties in Trentingrana dairy industry.

    PubMed

    Penasa, Mauro; Toffanin, Valentina; Cologna, Nicola; Cassandro, Martino; De Marchi, Massimo

    2016-05-01

    The objective of the present study was to investigate the effect of environmental factors, milk casein content and titratable acidity on milk coagulation properties (MCP) of samples routinely collected in the Trento province (northeast Italy) under field conditions. Rennet coagulation time (RCT, min), curd-firming time (k20, min) and curd firmness (a30, mm) were determined by Formagraph on 14 971 samples from 635 herds associated to 17 dairy factories. Besides MCP, fat, protein, and casein percentages, titratable acidity (TA), and somatic cell and bacterial counts were available. A standardised index of milk aptitude to coagulate (IAC) was derived using information of RCT and a30. An analysis of variance was conducted on MCP and IAC using a fixed effects linear model. Approximately 3% of milk samples did not form a curd within the testing time (30 min) and k20 was missing for 26% of milks. The percentage of samples without information on k20 largely differed among dairy factories (1·7-20·9%). Significant differences were estimated between the best and the worst dairy factory for RCT (-2 min), k20 (-1·2 min), a30 (+3·4 mm) and IAC (+2·6 points). Milk casein content and TA were important factors in explaining the variation of MCP and IAC, supporting the central role of these two traits on technological properties. The Trento province is heterogeneous in terms of dairy systems and this could explain the differences among dairy factories.

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

    NASA Astrophysics Data System (ADS)

    Skic, Kamil; Boguta, Patrycja; Sokołowska, Zofia

    2016-07-01

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

  8. Filtrates & Residues: Olfactory Titration.

    ERIC Educational Resources Information Center

    Wood, John T.; Eddy, Roberta M.

    1996-01-01

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

  9. The interaction of phenolic acids with Fe(III) in the presence of citrate as studied by isothermal titration calorimetry.

    PubMed

    Yang, Senpei; Bai, Guangling; Chen, Lingli; Shen, Qun; Diao, Xianmin; Zhao, Guanghua

    2014-08-15

    Under physiological conditions, exogenous chelators such as polyphenols might interact with non-protein bound ferric complexes, such as Fe(III)-citrate. Additionally, Fe(III) and citrate are widely distributed in various fruits and vegetables which are also rich in phenolic acids. In this study, we focus on the interaction between phenolic acids (gallic acid, methyl gallate and protocatechuic acid) and Fe(III) in the presence of excessive citrate by isothermal titration calorimetry (ITC) for thermodynamic studies, and stopped-flow absorption spectrometry for fast kinetic studies. Results reveal that all of these three phenolic acids can bind to the Fe(III) with the same stoichiometry (3:1). Moreover, the binding constants of these three compounds with Fe(III) are greatly dependent on ligand structure, and are much higher than that of Fe(III)-citrate. Based on their stoichiometry and superhigh binding constants, it is most likely that these three phenolic acids can displace the citrate to bind with one iron(III) ion to form a stable octahedral geometric structure, albeit at different rates. These findings shed light on the interaction between phenolic acids and Fe(III) in the presence of citrate under either physiological conditions or in a food system.

  10. Postoperative intravenous morphine titration.

    PubMed

    Aubrun, F; Mazoit, J-X; Riou, B

    2012-02-01

    Relief of acute pain during the immediate postoperative period is an important task for anaesthetists. Morphine is widely used to control moderate-to-severe postoperative pain and the use of small i.v. boluses of morphine in the post-anaesthesia care unit allows a rapid titration of the dose needed for adequate pain relief. The essential principle of a titration regimen must be to adapt the morphine dose to the pain level. Although morphine would not appear to be the most appropriate choice for achieving rapid pain relief, this is the sole opioid assessed in many studies of immediate postoperative pain management using titration. More than 90% of the patients have pain relief using a protocol of morphine titration and the mean dose required to obtain pain relief is 12 (7) mg, after a median of four boluses. Sedation is frequent during i.v. morphine titration and should be considered as a morphine-related adverse event and not evidence of pain relief. The incidence of ventilatory depression is very low when the criteria to limit the dose of i.v. morphine are enforced. Morphine titration can be used with caution in elderly patients, in children, or in obese patients. In practice, i.v. morphine titration allows the physician to meet the needs of individual patients rapidly and limits the risk of overdose making this method the first step in postoperative pain management.

  11. 40 CFR Appendix A to Part 425 - Potassium Ferricyanide Titration Method

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... MDL. Spike recovery must be 40 to 120 percent for the analysis of a particular matrix type to be... swirl gently. Let stand for two minutes, add 10 ml. of a 30 percent zinc sulfate solution, and titrate.... Preparation of ferrous dimethylglyoxime indicator solution: Mix 10 ml. 0.6 percent ferrous sulfate, 50 ml....

  12. 40 CFR Appendix A to Part 425 - Potassium Ferricyanide Titration Method

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... MDL. Spike recovery must be 40 to 120 percent for the analysis of a particular matrix type to be... swirl gently. Let stand for two minutes, add 10 ml. of a 30 percent zinc sulfate solution, and titrate.... Preparation of ferrous dimethylglyoxime indicator solution: Mix 10 ml. 0.6 percent ferrous sulfate, 50 ml....

  13. Comparison of the surface ion density of silica gel evaluated via spectral induced polarization versus acid-base titration

    NASA Astrophysics Data System (ADS)

    Hao, Na; Moysey, Stephen M. J.; Powell, Brian A.; Ntarlagiannis, Dimitrios

    2016-12-01

    Surface complexation models are widely used with batch adsorption experiments to characterize and predict surface geochemical processes in porous media. In contrast, the spectral induced polarization (SIP) method has recently been used to non-invasively monitor in situ subsurface chemical reactions in porous media, such as ion adsorption processes on mineral surfaces. Here we compare these tools for investigating surface site density changes during pH-dependent sodium adsorption on a silica gel. Continuous SIP measurements were conducted using a lab scale column packed with silica gel. A constant inflow of 0.05 M NaCl solution was introduced to the column while the influent pH was changed from 7.0 to 10.0 over the course of the experiment. The SIP measurements indicate that the pH change caused a 38.49 ± 0.30 μS cm- 1 increase in the imaginary conductivity of the silica gel. This increase is thought to result from deprotonation of silanol groups on the silica gel surface caused by the rise in pH, followed by sorption of Na+ cations. Fitting the SIP data using the mechanistic model of Leroy et al. (Leroyet al., 2008), which is based on the triple layer model of a mineral surface, we estimated an increase in the silica gel surface site density of 26.9 × 1016 sites m- 2. We independently used a potentiometric acid-base titration data for the silica gel to calibrate the triple layer model using the software FITEQL and observed a total increase in the surface site density for sodium sorption of 11.2 × 1016 sites m- 2, which is approximately 2.4 times smaller than the value estimated using the SIP model. By simulating the SIP response based on the calibrated surface complexation model, we found a moderate association between the measured and estimated imaginary conductivity (R2 = 0.65). These results suggest that the surface complexation model used here does not capture all mechanisms contributing to polarization of the silica gel captured by the SIP data.

  14. Development of a new certified reference material of diosgenin using mass balance approach and Coulometric titration method.

    PubMed

    Gong, Ningbo; Zhang, Baoxi; Hu, Fan; Du, Hui; Du, Guanhua; Gao, Zhaolin; Lu, Yang

    2014-12-01

    Certified reference materials (CRMs) can be used as a valuable tool to validate the trueness of measurement methods and to establish metrological traceability of analytical results. Diosgenin has been selected as a candidate reference material. Characterization of the material relied on two different methods, mass balance method and Coulometric titration method (CT). The certified value of diosgenin CRM is 99.80% with an expanded uncertainty of 0.37% (k=2). The new CRM of diosgenin can be used to validate analytical methods, improve the accuracy of measurement data and control the quality of diosgenin in relevant pharmaceutical formulations.

  15. Effects of freezing and the cryoprotectant lactobionic acid in the structure of GlnK protein evaluated by circular dichroism (CD) and isothermal titration calorimetry (ITC).

    PubMed

    Misugi, Cíntia Tiemi; Savi, Lizandra Kamradt; Iwankiw, Patrícia Kanczewski; Masson, Maria Lucia; de Oliveira, Marco Aurélio Schüler; Igarashi-Mafra, Luciana; Mafra, Marcos Rogério

    2017-01-01

    Freezing is a widely applied method in food preservation. The technique has negative effects on sensory and textural properties of some foods. In this study the effects of the freeze-thaw process and lactobionic acid (LBA) as a cryoprotectant on GlnK protein solution were evaluated by circular dichroism (CD) analysis and isothermal titration calorimetry (ITC). The freeze-thaw cycles caused changes in GlnK conformation and interactions with small ligands (adenosine triphosphate, ATP). CD assay demonstrated changes in the molar ellipticity values of the samples subjected to freezing, indicating conformational changes to the GlnK protein. Additionally, ITC analysis indicated that the freeze-thaw process caused changes in the interaction properties of GlnK with its ligand ATP. LBA cryoprotectant activity was also evaluated and with both of the techniques it was demonstrated that the compound prevented the damage caused by the freeze-thaw process, thereby maintaining the characteristics of the samples.

  16. Microscale Titration in Schools Titration Competition.

    ERIC Educational Resources Information Center

    Clark, Michael J.

    1998-01-01

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

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

    PubMed

    Scherrer, Robert A; Donovan, Stephen F

    2009-04-01

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

  18. Determination of soluble solids content and titratable acidity of intact fruit and juice of Satsuma mandarin using a hand-held NIR instrument in transmittance mode

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Determination of soluble solids content (SSC) and titratable acidity (TA) of intact fruit and juice of Satsuma mandarin was investigated using a hand-held NIR instrument “NIR-Gun” in transmittance mode. The resulting calibration equation measured SSC of intact fruit and juice with a standard error o...

  19. Analysis of aqueous solutions by near-infrared spectrometry (NIRS) II. Titrations of weak and very weak acids with strong bases

    NASA Astrophysics Data System (ADS)

    Molt, K.; Niemöller, A.; Cho, Y. J.

    1997-06-01

    The titrations of acetic and phosphoric acid with NaOH were observed by NIR-spectrometry. The measured spectra can be evaluated quantitatively for calibration of the H +-and OH --concentration. The NIRS errors with respect to the prediction of the pH and the equivalence point are discussed.

  20. Volumetric Titrations Using Electrolytically Generated Reagents for the Determination of Ascorbic Acid and Iron in Dietary Supplement Tablets: An Undergraduate Laboratory Experiment

    ERIC Educational Resources Information Center

    Scanlon, Christopher; Gebeyehu, Zewdu; Griffin, Kameron; Dabke, Rajeev B.

    2014-01-01

    An undergraduate laboratory experiment for the volumetric quantitative analysis of ascorbic acid and iron in dietary supplement tablets is presented. Powdered samples of the dietary supplement tablets were volumetrically titrated against electrolytically generated reagents, and the mass of dietary reagent in the tablet was determined from the…

  1. Determination of Carbonyl Groups in Pyrolysis Bio-oils Using Potentiometric Titration: Review and Comparison of Methods

    SciTech Connect

    Black, Stuart; Ferrell, Jack R.

    2016-01-06

    Carbonyl compounds present in bio-oils are known to be responsible for bio-oil property changes upon storage and during upgrading. 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. 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 in this study, 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. Some compounds such as carbohydrates are not measured by the traditional method (modified Nicolaides method), resulting in low estimations of the carbonyl content. Furthermore, we have shown that reaction completion for the traditional method can take up to 300 hours. The new method presented here (the modified Faix method) reduces the reaction time to 2 hours, uses triethanolamine (TEA) in the place of pyridine, and requires a smaller sample size for the analysis. Carbonyl contents determined using this new method are consistently higher than when using the traditional titration methods.

  2. Determination of Carbonyl Groups in Pyrolysis Bio-oils Using Potentiometric Titration: Review and Comparison of Methods

    DOE PAGES

    Black, Stuart; Ferrell, Jack R.

    2016-01-06

    Carbonyl compounds present in bio-oils are known to be responsible for bio-oil property changes upon storage and during upgrading. 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. 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 in this study, we present a modification of the traditional carbonyl oximation procedures that results inmore » less reaction time, smaller sample size, higher precision, and more accurate carbonyl determinations. Some compounds such as carbohydrates are not measured by the traditional method (modified Nicolaides method), resulting in low estimations of the carbonyl content. Furthermore, we have shown that reaction completion for the traditional method can take up to 300 hours. The new method presented here (the modified Faix method) reduces the reaction time to 2 hours, uses triethanolamine (TEA) in the place of pyridine, and requires a smaller sample size for the analysis. Carbonyl contents determined using this new method are consistently higher than when using the traditional titration methods.« less

  3. Competitive virus assay method for titration of noncytopathogenic bovine viral diarrhea viruses (END⁺ and END⁻ viruses).

    PubMed

    Muhsen, Mahmod; Ohi, Kota; Aoki, Hiroshi; Ikeda, Hidetoshi; Fukusho, Akio

    2013-03-01

    A new, reliable and secure virus assay method, named the competitive virus assay (CVA) method, has been established for the titration of bovine viral diarrhea viruses (BVDVs) that either show the exaltation of Newcastle disease virus (END) phenomenon or heterologous interference phenomenon (but not the END phenomenon). This method is based on the principle of (1) homologous interference between BVDVs, by using BVDV RK13/E(-) or BVDV RK13/E(+) strains as competitor virus, and (2) END phenomenon and heterologous interference, by using attenuated Newcastle disease virus (NDV) TCND strain as challenge virus. In titration of BVDV END(+) and BVDV END(-) viruses, no significant difference in estimated virus titer was observed between CVA and conventional methods. CVA method demonstrated comparable levels of sensitivity and accuracy as conventional END and interference methods, which require the use of a velogenic Miyadera strain of NDV and vesicular stomatitis virus (VSV), both of which are agents of high-risk diseases. As such, the CVA method is a safer alternative, with increased bio-safety and bio-containment, through avoidance of virulent strains that are commonly employed with conventional methods.

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

    Technology Transfer Automated Retrieval System (TEKTRAN)

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

  5. Molecular Characterization of the Gas-Particle Interface of Soot Sampled from a Diesel Engine Using a Titration Method.

    PubMed

    Tapia, A; Salgado, M S; Martín, María Pilar; Lapuerta, M; Rodríguez-Fernández, J; Rossi, M J; Cabañas, B

    2016-03-15

    Surface functional groups of two different types of combustion aerosols, a conventional diesel (EN 590) and a hydrotreated vegetable oil (HVO) soot, have been investigated using heterogeneous chemistry (i.e., gas-particle surface reactions). A commercial sample of amorphous carbon (Printex XE2-B) was analyzed as a reference substrate. A Knudsen flow reactor was used to carry out the experiments under molecular flow conditions. The selected gases for the titration experiments were: N(CH3)3 for the identification of acidic sites, NH2OH for the presence of carbonyl groups, CF3COOH and HCl for basic sites of different strength, and O3 and NO2 for reducing groups. Reactivity with N(CH3)3 indicates a lower density of acidic functionalities for Printex XE2-B in relation to diesel and HVO soot. Results for NH2OH experiments indicates that commercial amorphous carbon exhibits a lower abundance of available carbonyl groups at the interface compared to the results from diesel and HVO soot, the latter being the one with the largest abundance of carbonyl functions. Reactions with acids indicate the presence of weak basic oxides on the particle surface that preferentially interact with the strong acid CF3COOH. Finally, reactions with O3 and NO2 reveal that diesel and especially HVO have a significantly higher reactivity with both oxidizers compared to that of Printex XE2-B because they have more reducing sites by roughly a factor of 10 and 30, respectively. The kinetics of titration reactions have also been investigated.

  6. Amperometric, Bipotentiometric, and Coulometric Titration.

    ERIC Educational Resources Information Center

    Stock, John T.

    1980-01-01

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

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

    DOEpatents

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

    1998-02-24

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

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

    DOEpatents

    Smith, Douglas D.; Hiller, John M.

    1998-01-01

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

  9. Colorblindness and Titrations with Visual Indicators.

    ERIC Educational Resources Information Center

    Diehl, Harvey; And Others

    1985-01-01

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

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

    SciTech Connect

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

    2013-01-01

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

  11. Coarse-grained modeling of the titration and conductance behavior of aqueous fullerene hexa malonic acid (FHMA) solutions.

    PubMed

    Allison, Stuart A; Wu, Hengfu; Moyher, Avery; Soegiarto, Linda; Truong, Bi; Nguyen, Duy; Nguyen, Tam; Park, Donghyun

    2014-03-20

    The coarse-grained continuum primitive model is developed and used to characterize the titration and electrical conductance behavior of aqueous solutions of fullerene hexa malonic acid (FHMA). The spherical FHMA molecule, a highly charged electrolyte with an absolute valence charge as large as 12, is modeled as a dielectric sphere in Newtonian fluid, and electrostatics are treated numerically at the level of the non-linear Poisson-Boltzmann equation. Transport properties (electrophoretic mobilities and conductances) of the various charge states of FHMA are numerically computed using established numerical algorithms. For reasonable choices of the model parameters, good agreement between experiment (published literature) and modeling is achieved. In order to accomplish this, however, a moderate degree of specific binding of principal counterion and FHMA must be included in the modeling. It should be emphasized, however, that alternative explanations are possible. This comparison is made at 25 °C for both Na(+) and Ca(2+) principal counterions. The model is also used to characterize the different charge states and degree of counterion binding to those charge states as a function of pH.

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

    PubMed

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

    2007-09-01

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

  13. Calcium-buffering effects of gluconate and nucleotides, as determined by a novel fluorimetric titration method

    PubMed Central

    Woehler, Andrew; Lin, Kun-Han; Neher, Erwin

    2014-01-01

    Significantly more Ca2+ influx is required for eliciting release of neurotransmitter during whole cell patch clamp recording in the Calyx of Held, when gluconate with 3 mm free ATP is used as pipette filling solution, as compared to a methanesulfonate-based solution with excess Mg2+. This reduction in efficiency of Ca2+ in eliciting release is due to low-affinity Ca2+ binding of both gluconate and ATP2− anions. To study these effects we developed a simple fluorimeteric titration procedure, which reports the dissociation constant, KD, of a given Ca2+ indicator dye, multiplied by 1 plus the sum of Ca2+ binding ratios of any anions, which act as low-affinity Ca2+ ligands. For solutions without Ca2+ binding anions we find KD values for Fura2FF ranging from 11.5 ± 1.7 to 15.6 ± 7.47 μm depending on the dominant anion used. For Fura6F and KCl-based solutions we find KD = 17.8 ± 1.3 μm. For solutions with gluconate as the main anion and for solutions that contain nucleotides, such as ATP and GTP, we find much higher values for the product. Assuming that the KD of the indicator dye is equal to that of KCl-based solutions we calculate the summed Ca2+ binding ratios and find a value of 3.55 for a solution containing 100 mm potassium gluconate and 4 mm ATP. Gluconate contributes a value of 1.75 to this number, while the contribution of ATP depends strongly on the presence of Mg2+ and varies from 0.8 (with excess Mg2+) to 13.8 (in the presence of 3 mm free ATP). Methanesulfonate has negligible Ca2+ binding capacity. These results explain the reduced efficiency of Ca2+ influx in the presence of gluconate or nucleotides, as these anions are expected to intercept Ca2+ ions at short distance. PMID:25194050

  14. Quantitative estimation of diphtheria and tetanus toxoids. 6. Use of different antibody titration methods for evaluation of immunogenicity in animals during potency assay of diphtheria toxoid.

    PubMed

    Lyng, J; Heron, I

    1992-06-01

    Two diphtheria toxoid preparations were compared in potency assays in guinea-pigs using different methods for evaluation of the responses to vaccination. The methods used were the direct skin challenge (Schick test) and ELISA and VERO cell titration of antibodies. The different evaluation methods resulted in the same relative potencies between the toxoids. It was observed that when first-vaccination sera were compared with a second-vaccination serum, the relative antibody concentration depended on whether ELISA or VERO cell titration was used.

  15. Coulometric titration of urea with electrogenerated hypobromite.

    PubMed

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

    2013-01-01

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

  16. Neutron absorptiometric titration.

    PubMed

    Tölgyessy, J; Varga, S; Dillinger, P

    1967-03-01

    A method is outlined for detection of two-phase titration end-points by means of an abrupt change in the neutron-absorption characteristics of one of the phases. One of the components of the precipitate must have a large neutron absorption cross-section, and the disappearance or appearance of neutron absorption by the supernatant liquid from the precipitation reaction then marks the completion of precipitation.

  17. Responses of grape berry anthocyanin and titratable acidity to the projected climate change across the Western Australian wine regions.

    PubMed

    Barnuud, Nyamdorj N; Zerihun, Ayalsew; Mpelasoka, Freddie; Gibberd, Mark; Bates, Bryson

    2014-08-01

    More than a century of observations has established that climate influences grape berry composition. Accordingly, the projected global climate change is expected to impact on grape berry composition although the magnitude and direction of impact at regional and subregional scales are not fully known. The aim of this study was to assess potential impacts of climate change on levels of berry anthocyanin and titratable acidity (TA) of the major grapevine varieties grown across all of the Western Australian (WA) wine regions. Grape berry anthocyanin and TA responses across all WA wine regions were projected for 2030, 2050 and 2070 by utilising empirical models that link these berry attributes and climate data downscaled (to ∼5 km resolution) from the csiro_mk3_5 and miroc3_2_medres global climate model outputs under IPCC SRES A2 emissions scenario. Due to the dependence of berry composition on maturity, climate impacts on anthocyanin and TA levels were assessed at a common maturity of 22 °Brix total soluble solids (TSS), which necessitated the determination of when this maturity will be reached for each variety, region and warming scenario, and future period. The results indicate that both anthocyanin and TA levels will be affected negatively by a warming climate, but the magnitude of the impacts will differ between varieties and wine regions. Compared to 1990 levels, median anthocyanins concentrations are projected to decrease, depending on global climate model, by up to 3-12 % and 9-33 % for the northern wine regions by 2030 and 2070, respectively while 2-18 % reductions are projected in the southern wine regions for the same time periods. Patterns of reductions in the median Shiraz berry anthocyanin concentrations are similar to that of Cabernet Sauvignon; however, the magnitude is lower (up to 9-18 % in southern and northern wine regions respectively by 2070). Similarly, uneven declines in TA levels are projected across the study regions. The largest reductions

  18. Simultaneous determination of equilibrium constants and enthalpy changes by titration calorimetry: Methods, instruments, and uncertainties.

    PubMed

    Hansen, Lee D; Fellingham, Gilbert W; Russell, Donald J

    2011-02-15

    Calorimetric methods have been used to determine equilibrium constants since 1937, but no comprehensive review of the various calorimeters and methods has been done previously. This article reports methods for quantitative comparison of the capabilities of calorimeters for simultaneous determination of equilibrium constants and enthalpy changes, for determining optimal experimental conditions, and for assessing the effects of systematic and random errors on the accuracy and precision of equilibrium constants and enthalpy changes determined by this method.

  19. Comparison of methods for acid quantification: impact of resist components on acid-generating efficiency

    NASA Astrophysics Data System (ADS)

    Cameron, James F.; Fradkin, Leslie; Moore, Kathryn; Pohlers, Gerd

    2000-06-01

    Chemically amplified deep UV (CA-DUV) positive resists are the enabling materials for manufacture of devices at and below 0.18 micrometer design rules in the semiconductor industry. CA-DUV resists are typically based on a combination of an acid labile polymer and a photoacid generator (PAG). Upon UV exposure, a catalytic amount of a strong Bronsted acid is released and is subsequently used in a post-exposure bake step to deprotect the acid labile polymer. Deprotection transforms the acid labile polymer into a base soluble polymer and ultimately enables positive tone image development in dilute aqueous base. As CA-DUV resist systems continue to mature and are used in increasingly demanding situations, it is critical to develop a fundamental understanding of how robust these materials are. One of the most important factors to quantify is how much acid is photogenerated in these systems at key exposure doses. For the purpose of quantifying photoacid generation several methods have been devised. These include spectrophotometric methods, ion conductivity methods and most recently an acid-base type titration similar to the standard addition method. This paper compares many of these techniques. First, comparisons between the most commonly used acid sensitive dye, tetrabromophenol blue sodium salt (TBPB) and a less common acid sensitive dye, Rhodamine B base (RB) are made in several resist systems. Second, the novel acid-base type titration based on the standard addition method is compared to the spectrophotometric titration method. During these studies, the make up of the resist system is probed as follows: the photoacid generator and resist additives are varied to understand the impact of each of these resist components on the acid generation process.

  20. A study of pH-dependent photodegradation of amiloride by a multivariate curve resolution approach to combined kinetic and acid-base titration UV data.

    PubMed

    De Luca, Michele; Ioele, Giuseppina; Mas, Sílvia; Tauler, Romà; Ragno, Gaetano

    2012-11-21

    Amiloride photostability at different pH values was studied in depth by applying Multivariate Curve Resolution Alternating Least Squares (MCR-ALS) to the UV spectrophotometric data from drug solutions exposed to stressing irradiation. Resolution of all degradation photoproducts was possible by simultaneous spectrophotometric analysis of kinetic photodegradation and acid-base titration experiments. Amiloride photodegradation showed to be strongly dependent on pH. Two hard modelling constraints were sequentially used in MCR-ALS for the unambiguous resolution of all the species involved in the photodegradation process. An amiloride acid-base system was defined by using the equilibrium constraint, and the photodegradation pathway was modelled taking into account the kinetic constraint. The simultaneous analysis of photodegradation and titration experiments revealed the presence of eight different species, which were differently distributed according to pH and time. Concentration profiles of all the species as well as their pure spectra were resolved and kinetic rate constants were estimated. The values of rate constants changed with pH and under alkaline conditions the degradation pathway and photoproducts also changed. These results were compared to those obtained by LC-MS analysis from drug photodegradation experiments. MS analysis allowed the identification of up to five species and showed the simultaneous presence of more than one acid-base equilibrium.

  1. Development of Conductivity Method as an Alternative to Titration for Hydrolytic Resistance Testing Used for Evaluation of Glass Vials Used in Pharmaceutical Industry.

    PubMed

    Fujimori, Kiyoshi; Lee, Hans; Phillips, Joseph; Nashed-Samuel, Yasser

    The European Pharmacopeia surface test to analyze the hydrolytic resistance is a common industrial method to understand and ensure the quality of produced glass vials. Hydrolytic resistance is evaluated by calculating the alkalinity of water extract from autoclaved vials by titration. As an alternative to this titration technique, a conductivity technique was assessed, which directly measures the ions in the water extract. A conductivity meter with a 12 mm diameter electrode was calibrated with a 100 μS/cm conductivity standard and carryover minimized by rinsing the probe in a water beaker per analysis. The limit of quantification at 1 μS/cm was determined as having a signal-to-noise ratio of 3 compared with the water blank. The conductivity method was selective for glass-composing elements (boron, sodium, aluminum, silicon, potassium, and calcium) within the vial extract. Accuracies of spiked conductivity standard within the range of 1 to 100 μS/cm were ±7% and had linearity with coefficient of determination (R(2)) of ≥0.9999. Intraday precision had a relative standard deviation (RSD) (n = 5) of ≤6% for spiked conductivity standard within the range of 1 to 100 μS/cm. Interday precision had a RSD (n = 4) of ≤6% for 10 vials from three glass vial lots. Conductivity of water extracts from nine sets of seven lots of glass vials had a precise linear relationship [R(2) = 0.9876, RSD = 1% (n = 9)] with titration volumes of the same lots. Conductivity results in μS/cm could be converted to titration volumes in milliliters by a conversion factor of 0.0275. The simplicity, sample stability, and individual vial analysis of the conductivity technique were more advantageous than the current titration technique.

  2. Does the commonly used pH-stat method with back titration really quantify the enzymatic digestibility of lipid drug delivery systems? A case study on solid lipid nanoparticles (SLN).

    PubMed

    Heider, Martha; Hause, Gerd; Mäder, Karsten

    2016-12-01

    Enzymatic digestion of lipid drug carriers is very important. Commonly, pancreatin induced formation of fatty acids is monitored by the pH-stat method, which provides a fast, but unspecific readout. However, according to the literature, the pKa values of long chain fatty acids are strongly dependent on the local environment and might vary between 4.2 and 10.15. The high pKa values would lead to an incomplete detection of the lipid digestion and false results. In order to investigate these issues in more detail, we produced cetyl palmitate solid lipid nanoparticles (CP-SLN) stabilized with poloxamer 188 or polysorbate 80. The digestion of CP-SLN was investigated by two different and independent readouts. A HPTLC assay was used in addition to the pH-stat method (with or without back titration). An incomplete digestion of CP-SLN was observed with all methods. Partial digestion of polysorbate 80 contributed to the formation of fatty acids. Depending on the investigated system and the experimental conditions (FaSSIF or FeSSIF) the results of both readout methods were comparable or not. For example, in FeSSIF conditions, the values detected by HPTLC were roughly twice as high as the pH-stat results. Our findings on solid lipids agree with data from Helbig et al. on lipid emulsions, where a gas chromatography method detected much higher values than the pH-stat assay (Food Hydrocoll. 28 (2012) 10-19). The results of our pH-stat experiments with back titration at different pH values showed increased values for fatty acids from pH 7.5 to pH 10. The values obtained by back titration at high pH values (pH 9 or higher) did exceed the digestion values measured by HPTLC. Therefore, we conclude that the pH-stat method might give the same results as more specific reference methods, but it might also both under- (without back titration) or overestimate (with back titration) the enzymatic digestion of lipid drug delivery systems. A further outcome of our study was the proof that

  3. Reference method for total water in lint cotton by automated oven drying combined with volumetric Karl Fischer titration

    Technology Transfer Automated Retrieval System (TEKTRAN)

    In a preliminary study to measure total water in lint cotton we demonstrated that volumetric Karl Fischer Titration of moisture transported by a carrier gas from an attached small oven is more accurate than standard oven drying in air. The objective of the present study was to assess the measuremen...

  4. Method for isolating nucleic acids

    SciTech Connect

    Hurt, Jr., Richard Ashley; Elias, Dwayne A.

    2015-09-29

    The current disclosure provides methods and kits for isolating nucleic acid from an environmental sample. The current methods and compositions further provide methods for isolating nucleic acids by reducing adsorption of nucleic acids by charged ions and particles within an environmental sample. The methods of the current disclosure provide methods for isolating nucleic acids by releasing adsorbed nucleic acids from charged particles during the nucleic acid isolation process. The current disclosure facilitates the isolation of nucleic acids of sufficient quality and quantity to enable one of ordinary skill in the art to utilize or analyze the isolated nucleic acids for a wide variety of applications including, sequencing or species population analysis.

  5. Digital movie-based on automatic titrations.

    PubMed

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

    2016-01-15

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

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

    USGS Publications Warehouse

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

    1985-01-01

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

  7. Systemic errors in quantitative polymerase chain reaction titration of self-complementary adeno-associated viral vectors and improved alternative methods.

    PubMed

    Fagone, Paolo; Wright, J Fraser; Nathwani, Amit C; Nienhuis, Arthur W; Davidoff, Andrew M; Gray, John T

    2012-02-01

    Self-complementary AAV (scAAV) vector genomes contain a covalently closed hairpin derived from a mutated inverted terminal repeat that connects the two monomer single-stranded genomes into a head-to-head or tail-to-tail dimer. We found that during quantitative PCR (qPCR) this structure inhibits the amplification of proximal amplicons and causes the systemic underreporting of copy number by as much as 10-fold. We show that cleavage of scAAV vector genomes with restriction endonuclease to liberate amplicons from the covalently closed terminal hairpin restores quantitative amplification, and we implement this procedure in a simple, modified qPCR titration method for scAAV vectors. In addition, we developed and present an AAV genome titration procedure based on gel electrophoresis that requires minimal sample processing and has low interassay variability, and as such is well suited for the rigorous quality control demands of clinical vector production facilities.

  8. Nucleic Acid Detection Methods

    DOEpatents

    Smith, Cassandra L.; Yaar, Ron; Szafranski, Przemyslaw; Cantor, Charles R.

    1998-05-19

    The invention relates to methods for rapidly determining the sequence and/or length a target sequence. The target sequence may be a series of known or unknown repeat sequences which are hybridized to an array of probes. The hybridized array is digested with a single-strand nuclease and free 3'-hydroxyl groups extended with a nucleic acid polymerase. Nuclease cleaved heteroduplexes can be easily distinguish from nuclease uncleaved heteroduplexes by differential labeling. Probes and target can be differentially labeled with detectable labels. Matched target can be detected by cleaving resulting loops from the hybridized target and creating free 3-hydroxyl groups. These groups are recognized and extended by polymerases added into the reaction system which also adds or releases one label into solution. Analysis of the resulting products using either solid phase or solution. These methods can be used to detect characteristic nucleic acid sequences, to determine target sequence and to screen for genetic defects and disorders. Assays can be conducted on solid surfaces allowing for multiple reactions to be conducted in parallel and, if desired, automated.

  9. Nucleic acid detection methods

    DOEpatents

    Smith, C.L.; Yaar, R.; Szafranski, P.; Cantor, C.R.

    1998-05-19

    The invention relates to methods for rapidly determining the sequence and/or length a target sequence. The target sequence may be a series of known or unknown repeat sequences which are hybridized to an array of probes. The hybridized array is digested with a single-strand nuclease and free 3{prime}-hydroxyl groups extended with a nucleic acid polymerase. Nuclease cleaved heteroduplexes can be easily distinguish from nuclease uncleaved heteroduplexes by differential labeling. Probes and target can be differentially labeled with detectable labels. Matched target can be detected by cleaving resulting loops from the hybridized target and creating free 3-hydroxyl groups. These groups are recognized and extended by polymerases added into the reaction system which also adds or releases one label into solution. Analysis of the resulting products using either solid phase or solution. These methods can be used to detect characteristic nucleic acid sequences, to determine target sequence and to screen for genetic defects and disorders. Assays can be conducted on solid surfaces allowing for multiple reactions to be conducted in parallel and, if desired, automated. 18 figs.

  10. [The titration of double bonds in fatty acids of blood plasma in patients in testing of glucose tolerance].

    PubMed

    Titov, V N; Sazhina, N N; Evteeva, N M; Aripovskiĭ, A V; Tkhagalizhokova, E M

    2015-01-01

    The article deals with per oral glucose tolerance test applied to 20 patients with arterial hypertension. The blood plasma was analyzed to detect content of individual fatty acids, double bounds, glucose, insulin and metabolites of fatty acids. In patients with different resistance to insulin content of non-etherized fatty acids decreased approximatively up to 3 times. Without insulin resistance secretion of insulin in 2 hours after glucose load increased up to 3 times and content of individual fatty acids decreases in greater extent. Under insulin resistance secretion of insulin increases up to 8 times and decreasing of content of fatty acids is less expressed. The decrease in blood plasma of content of oleic and linoleic fatty acids and double bounds reflects effectiveness of effect of insulin--blockade of hydrolysis of triglycerides in subcutaneous adipocytes. The concentration of insulin positively correlates with initial content of palmitic fatty acid in the pool of lipids of blood plasma.

  11. Identification of Weak Acids and Bases by Titration with Primary Standards. A Modern Version of an Old Analytical Chemistry Experiment.

    ERIC Educational Resources Information Center

    Thompson, Robert Q.

    1988-01-01

    Describes a laboratory exercise in which acid dissociation constants and molecular weights are extracted from sample data and the sample is identified. Emphasizes accurate volumetric work while bringing to practice the concepts of acid-base equilibria, activity coefficients, and thermodynamic constants. (CW)

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

    NASA Astrophysics Data System (ADS)

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

    2010-06-01

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

  13. A high-throughput microtiter plate based method for the determination of peracetic acid and hydrogen peroxide.

    PubMed

    Putt, Karson S; Pugh, Randall B

    2013-01-01

    Peracetic acid is gaining usage in numerous industries who have found a myriad of uses for its antimicrobial activity. However, rapid high throughput quantitation methods for peracetic acid and hydrogen peroxide are lacking. Herein, we describe the development of a high-throughput microtiter plate based assay based upon the well known and trusted titration chemical reactions. The adaptation of these titration chemistries to rapid plate based absorbance methods for the sequential determination of hydrogen peroxide specifically and the total amount of peroxides present in solution are described. The results of these methods were compared to those of a standard titration and found to be in good agreement. Additionally, the utility of the developed method is demonstrated through the generation of degradation curves of both peracetic acid and hydrogen peroxide in a mixed solution.

  14. Stability constants of some metal complexes of triethylenetetraminehexa-acetic acid and complexometric titration of rare earths and other metals.

    PubMed

    Soucek, D A; Cheng, K L; Droll, H A

    1968-08-01

    The stability constants of some non-protonated 1:1 metal complexes of triethylenetetraminehexa-acetic acid are reported; log K values are Cd 19.8, Co(II) 20.4, Ni 19.9, Pb 19.5, Sm(III) 24.3, Zn 20.1.

  15. Micro coulometric titration in a liquid drop.

    PubMed

    Kanyanee, Tinakorn; Fuekhad, Pongwasin; Grudpan, Kate

    2013-10-15

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

  16. Derivative analysis of potentiometric titration data to obtain protonation constants

    SciTech Connect

    Chen, J.F.; Xia, Y.X.; Choppin, G.R.

    1996-11-15

    A methodology is described to calibrate glass electrodes and to analyze potentiometric titration data to calculate protonation constants. The analysis uses the variation of dV/dpH with titrant addition in terms of two physical parameters which involve the concentrations of H{sup +}, OH{sup -}, and H{sub m}A. The data for titration of acetic acid and 8-hydroxyquinoline in 0.10-5.0 m NaCl media are analyzed by this method to obtain the stoichiometric protonation constants of the acids, the ionization constants of water, and the parameters s and b in the pH electrode calibration equation, pcH = spH{sub m} + b, where pcH = -log[H{sup +}], pH{sub m} is the pH meter reading. 31 refs., 3 figs., 6 tabs.

  17. [Sources of error in the European Pharmacopoeia assay of halide salts of organic bases by titration with alkali].

    PubMed

    Kószeginé, S H; Ráfliné, R Z; Paál, T; Török, I

    2000-01-01

    A short overview has been given by the authors on the titrimetric assay methods of halide salts of organic bases in the pharmacopoeias of greatest importance. The alternative procedures introduced by the European Pharmacopoeia Commission some years ago to replace the non-aqueous titration with perchloric acid in the presence of mercuric acetate have also been presented and evaluated. The authors investigated the limits of applicability and the sources of systematic errors (bias) of the strongly preferred titration with sodium hydroxide in an alcoholic medium. To assess the bias due to the differences between the results calculated from the two inflexion points of the titration curves and the two real endpoints corresponding to the strong and weak acids, respectively, the mathematical analysis of the titration curve function was carried out. This bias, generally negligible when the pH change near the endpoint of the titration is more than 1 unit, is the function of the concentration, the apparent pK of the analyte and the ionic product of water (ethanol) in the alcohol-water mixtures. Using the validation data gained for the method with the titration of ephedrine hydrochloride the authors analysed the impact of carbon dioxide in the titration medium on the additive and proportional systematic errors of the method. The newly introduced standardisation procedure of the European Pharmacopoeia for the sodium hydroxide titrant to decrease the systematic errors caused by carbon dioxide has also been evaluated.

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

    NASA Astrophysics Data System (ADS)

    Kunze, Nicole M.

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

  19. Successive determination of praseodymium and ytterbium by coulometric complexometric titration

    SciTech Connect

    Chun-Nian, S.; Jing-Ci, L.; Qi-Dao, N.; Mou-Sen, C.

    1982-06-01

    A method is described for the successive coulometric complexometric titration of microgram levels of light and heavy rare earth elements. The total amount of light and heavy rare earth elements is titrated by electrogenerating titrant EDTA on the mercury pool as a cathode. Then, the mercury pool is switched as an anode, electrogenerating Hg/sup 2 +/, and is used to titrate EDTA which is displaced from its light rare earth elements complex by malic acid that has been added prior to the electrogenerating Hg/sup 2 +/. The heavy rare earth elements can be determined from the total rare earth elements minus the result of displacement titration of EDTA which is equivalent to the light rare earth elements. A 10-30 ..mu..g sample of light and heavy rare earth elements (Pr and Yb, La and Lu, Nd and Tm) can be determined successively. Errors and standard deviation are not more than 2.5% and 0.20, respectively. 2 tables, 5 figures.

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

    PubMed

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

    2005-06-01

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

  1. Titration Calculations with Computer Algebra Software

    ERIC Educational Resources Information Center

    Lachance, Russ; Biaglow, Andrew

    2012-01-01

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

  2. Comparative assessment of the methods for exchangeable acidity measuring

    NASA Astrophysics Data System (ADS)

    Vanchikova, E. V.; Shamrikova, E. V.; Bespyatykh, N. V.; Zaboeva, G. A.; Bobrova, Yu. I.; Kyz"yurova, E. V.; Grishchenko, N. V.

    2016-05-01

    A comparative assessment of the results of measuring the exchangeable acidity and its components by different methods was performed for the main mineral genetic horizons of texturally-differentiated gleyed and nongleyed soddy-podzolic and gley-podzolic soils of the Komi Republic. It was shown that the contents of all the components of exchangeable soil acidity determined by the Russian method (with potassium chloride solution as extractant, c(KCl) = 1 mol/dm3) were significantly higher than those obtained by the international method (with barium chloride solution as extractant, c(BaCl2) = 0.1 mol/dm3). The error of the estimate of the concentration of H+ ions extracted with barium chloride solution equaled 100%, and this allowed only qualitative description of this component of the soil acidity. In the case of the extraction with potassium chloride, the error of measurements was 50%. It was also shown that the use of potentiometric titration suggested by the Russian method overestimates the results of soil acidity measurement caused by the exchangeable metal ions (Al(III), Fe(III), and Mn(II)) in comparison with the atomic emission method.

  3. Standard test method for water in lint cotton by oven evaporation combined with volumetric Karl Fischer Titration

    Technology Transfer Automated Retrieval System (TEKTRAN)

    The referenced test method for total water content and water regain in lint cotton was developed by USDA scientists in New Orleans at the request of the cotton industry. The method covers the determination of the total water (free and bound) in raw and lint cotton at moisture equilibrium from con...

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

    PubMed

    Herrera, Isaac; Winnik, Mitchell A

    2016-03-10

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

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

    PubMed

    Bezáková, Zelmíra; Stankovičová, Mária

    2013-12-01

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

  6. Probing the binding mechanisms of α-tocopherol to trypsin and pepsin using isothermal titration calorimetry, spectroscopic, and molecular modeling methods.

    PubMed

    Li, Xiangrong; Ni, Tianjun

    2016-06-01

    α-Tocopherol is a required nutrient for a variety of biological functions. In this study, the binding of α-tocopherol to trypsin and pepsin was investigated using isothermal titration calorimetry (ITC), steady-state and time-resolved fluorescence measurements, circular dichroism (CD) spectroscopy, and molecular modeling methods. Thermodynamic investigations reveal that α-tocopherol binds to trypsin/pepsin is synergistically driven by enthalpy and entropy. The fluorescence experimental results indicate that α-tocopherol can quench the fluorescence of trypsin/pepsin through a static quenching mechanism. The binding ability of α-tocopherol with trypsin/pepsin is in the intermediate range, and one molecule of α-tocopherol combines with one molecule of trypsin/pepsin. As shown by circular dichroism (CD) spectroscopy, α-tocopherol may induce conformational changes of trypsin/pepsin. Molecular modeling displays the specific binding site and gives information about binding forces and α-tocopherol-tryptophan (Trp)/tyrosine (Tyr) distances. In addition, the inhibition rate of α-tocopherol on trypsin and pepsin was studied. The study provides a basic data set for clarifying the binding mechanisms of α-tocopherol with trypsin and pepsin and is helpful for understanding its biological activity in vivo.

  7. Implementation of coulometric titration system at constant current for developing of certified materials as primary standards

    NASA Astrophysics Data System (ADS)

    Suarez, H.; Cristancho, R.; Peralta, F.; Torres, H.

    2017-01-01

    Coulometry is a primary method for measuring high purity substances. This is used to certify the primary reference materials required in a chemical analysis process. This paper describes the coulometric titration system developed by the National Metrology Institute (NMI) of Colombia for the certification of hydrochloric acid 0.1mol/kg reference materials. In addition, it also shows preliminary studies for future development of potassium chloride (KCl) and ethylenediaminetetraacetic acid disodium salt (EDTA-Na2) certification.

  8. Isothermal Titration Calorimetry: Assisted Crystallization of RNA-Ligand Complexes.

    PubMed

    Da Veiga, Cyrielle; Mezher, Joelle; Dumas, Philippe; Ennifar, Eric

    2016-01-01

    The success rate of nucleic acids/ligands co-crystallization can be significantly improved by performing preliminary biophysical analyses. Among suitable biophysical approaches, isothermal titration calorimetry (ITC) is certainly a method of choice. ITC can be used in a wide range of experimental conditions to monitor in real time the formation of the RNA- or DNA-ligand complex, with the advantage of providing in addition the complete binding profile of the interaction. Following the ITC experiment, the complex is ready to be concentrated for crystallization trials. This chapter describes a detailed experimental protocol for using ITC as a tool for monitoring RNA/small molecule binding, followed by co-crystallization.

  9. A computer-controlled potentiometric/spectrophotometric titrator

    PubMed Central

    Stong, John D.

    1988-01-01

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

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

    PubMed

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

    2004-01-01

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

  11. [Detection of urinary organic acids by gradual titration of pH 2,0-7,4. Significance for the assessment of the litho-protective characteristic of the examined urine].

    PubMed

    Leskovar, P; Hartung, R; Hropot, M; Huber, H; Friedl, H; Wellnhofer, E; Steffek, D; Schöninger, R

    1981-08-01

    The role of organic acids in urine is not sufficiently known until today. From our detailed in vitro studies it can be concluded that some of them are highly efficacious in the inhibition of Ca-oxalate and Ca-phosphate crystal growth. Moreover, some of them showed, as acids and as salts, a strong lytic effect on stone-forming crystals and native stone-material. By the oral application to rats, concentrations preventing any precipitation out of meta- and instable Ca-oxalate solutions could be achieved. The renal excretion was controlled by the stepwise titration of preacidified urinary samples from pH 2.0 to 7.4 and the lithoprotective character of urine estimated by the Ca2+-binding capacity.

  12. Laboratory installation for the study of atomic-oxygen and ozone detectors and certain methodological aspects concerning the determination of oxygen-atom concentration by the methods of NO and NO2 titration

    NASA Astrophysics Data System (ADS)

    Bromberg, D. V.; Perov, S. P.

    A laboratory installation is described which can be used to study various characteristics of atomic oxygen and ozone in the pressure range from 0.01 to 50 Pa. The installation can be used to calibrate rocketborne sensors intended for measurements in the middle atmosphere. Systematic and random errors connected with the determination of oxygen-atom concentration by the NO2 and NO titration methods are examined.

  13. Nucleic acid arrays and methods of synthesis

    DOEpatents

    Sabanayagam, Chandran R.; Sano, Takeshi; Misasi, John; Hatch, Anson; Cantor, Charles

    2001-01-01

    The present invention generally relates to high density nucleic acid arrays and methods of synthesizing nucleic acid sequences on a solid surface. Specifically, the present invention contemplates the use of stabilized nucleic acid primer sequences immobilized on solid surfaces, and circular nucleic acid sequence templates combined with the use of isothermal rolling circle amplification to thereby increase nucleic acid sequence concentrations in a sample or on an array of nucleic acid sequences.

  14. Choice of chemical conditions in order to obtain linear titration curves in potentiometry.

    PubMed

    Johansson, A

    1975-12-01

    In the titration of an acid HA with a strong base, [HA] diminishes, on the whole, in proportion to the addition of titrant. However, [HA] = K(HA)[H] [A], and if [A] is kept constant [HA] will be proportional to [H]. Therefore if [H] instead of [HA] is plotted against ml of titrant added, one obtains a linear titration curve. [A] is kept constant by addition of NaA before titration in such high concentration that the formation of A can be neglected during the titration. When an acid stronger than acetic acid is titrated, sodium acetate can be used as the added salt. Even mixtures of adds, mono- or polybasic, then yield'straight titration curves since one is in fact titrating acetic acid in the presence of excess of acetate. For weaker acids sodium sulphite is used. In the oxidation-reduction titration of, for example, ferrous iron with permanganate, the potential measured is dependent on the ratio [Fe(2+)]/[Fe(3+)]. If [Fe(3+)] is kept constant by the addition of ferric chloride before the titration, the potential win be dependent only on [Fe(2+)]. Since this diminishes in proportion to the added volume of titrant, straight titration curves can be obtained in this case also. No correction for dilution should be made.

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

    PubMed

    Wójtowicz, Marzena; Kozak, Joanna; Kościelniak, Paweł

    2007-09-26

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

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

    PubMed

    Zarzycki, Piotr; Thomas, Fabien

    2006-10-15

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

  17. Alkylated lariat ethers as solvent extraction reagents: Surveying the extraction of alkali metals by bis-t-octylbenzo-14-crown-4-acetic acid by use of potentiometric two-phase titration

    SciTech Connect

    Sachleben, R.A.; Moyer, B.A.; Case, F.I.; Garmon, S.A.

    1993-01-01

    Two-phase potentiometric titrimetry was used to survey the extraction of alkali metal cations from aqueous chloride solution by the lipophilic, ionizable lariat ether bis-(t-octylbenzo)-14-crown-4-acetic acid (BOB14C4AA) in o-xylene. Analysis of the data indicates that ion-exchange extraction by the crown-carboxylic acid at low loading (i.e., low conversion of BOB14C4AA to its salt form) is stronger for lithium ion than for the other alkali metals. Little or no selectivity occurs at high loadings. In comparison with the long-chain carboxylic acid 2-methyl-2-heptylnonanoic acid (HMHN), BOB14C4AA extracts lithium and sodium at significantly lower pH; in the loading range of 0.1 to 0.7, the pH shift is 1.4-1.8 pH units for sodium ion and 1.7-2.3 pH units for lithium ion. The titration data are interpreted in terms of aggregated organic-phase species. In the case of lithium extraction, clear evidence was found for a species in which neutral BOB14C4AA participates in the organic-phase complexation of the metal cation.

  18. Photometric method for determination of acidity constants through integral spectra analysis.

    PubMed

    Zevatskiy, Yuriy Eduardovich; Ruzanov, Daniil Olegovich; Samoylov, Denis Vladimirovich

    2015-04-15

    An express method for determination of acidity constants of organic acids, based on the analysis of the integral transmittance vs. pH dependence is developed. The integral value is registered as a photocurrent of photometric device simultaneously with potentiometric titration. The proposed method allows to obtain pKa using only simple and low-cost instrumentation. The optical part of the experimental setup has been optimized through the exclusion of the monochromator device. Thus it only takes 10-15 min to obtain one pKa value with the absolute error of less than 0.15 pH units. Application limitations and reliability of the method have been tested for a series of organic acids of various nature.

  19. Photometric method for determination of acidity constants through integral spectra analysis

    NASA Astrophysics Data System (ADS)

    Zevatskiy, Yuriy Eduardovich; Ruzanov, Daniil Olegovich; Samoylov, Denis Vladimirovich

    2015-04-01

    An express method for determination of acidity constants of organic acids, based on the analysis of the integral transmittance vs. pH dependence is developed. The integral value is registered as a photocurrent of photometric device simultaneously with potentiometric titration. The proposed method allows to obtain pKa using only simple and low-cost instrumentation. The optical part of the experimental setup has been optimized through the exclusion of the monochromator device. Thus it only takes 10-15 min to obtain one pKa value with the absolute error of less than 0.15 pH units. Application limitations and reliability of the method have been tested for a series of organic acids of various nature.

  20. Kinetic titration series with biolayer interferometry.

    PubMed

    Frenzel, Daniel; Willbold, Dieter

    2014-01-01

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

  1. Proton-binding study of standard and reference fulvic acids, humic acids, and natural organic matter

    NASA Astrophysics Data System (ADS)

    Ritchie, Jason D.; Perdue, E. Michael

    2003-01-01

    The acid-base properties of 14 standard and reference materials from the International Humic Substances Society (IHSS) were investigated by potentiometric titration. Titrations were conducted in 0.1 M NaCl under a nitrogen atmosphere, averaging 30 min from start to finish. Concentrations of carboxyl groups and phenolic groups were estimated directly from titration curves. Titration data were also fit to a modified Henderson-Hasselbalch model for two classes of proton-binding sites to obtain "best fit" parameters that describe proton-binding curves for the samples. The model was chosen for its simplicity, its ease of implementation in computer spreadsheets, and its excellent ability to describe the shapes of the titration curves. The carboxyl contents of the IHSS samples are in the general order: terrestrial fulvic acids > aquatic fulvic acids > Suwannee River natural organic matter (NOM) > aquatic humic acids > terrestrial humic acids. Overall, fulvic acids and humic acids have similar phenolic contents; however, all of the aquatically derived samples have higher phenolic contents than the terrestrially derived samples. The acid-base properties of reference Suwannee River NOM are surprisingly similar to those of standard Suwannee River humic acid. Results from titrations in this study were compared with other published results from both direct and indirect titrations. Typically, carboxyl contents for the IHSS samples were in agreement with the results from both methods of titration. Phenolic contents for the IHSS samples were comparable to those determined by direct titrations, but were significantly less than estimates of phenolic content that were based on indirect titrations with Ba(OH) 2 and Ca(OAc) 2. The average phenolic-to-carboxylic ratio of the IHSS samples is approximately 1:4. Models that assume a 1:2 ratio of phenolic-to-carboxylic groups may overestimate the relative contribution of phenolic groups to the acid-base chemistry of humic substances.

  2. Determination of component concentrations in mixtures of weak and strong acids and bases by linear algebraic methods.

    PubMed

    Ivaska, A; Nagypál, I

    1980-09-01

    A general expression for transforming potentiometric titration curves of mixtures of weak acids into a system of linear equations is derived. The solution of the linear equations gives directly the concentrations of the components. This linear transformation method is illustrated by the analysis of mixtures of weak acids with overlapping dissociation equilibria. The possible presence of a strong acid or strong base in the mixture can also be detected and its concentration simultaneously determined. The method can also be used for analysis of an ampholyte and solutions containing a weak acid and its conjugate base. For example a mixture of hydroxyacetic acid (pK approximately 3.6), acetic acid (pK approximately 4.6) and hydroxylamine hydrochloride (pK approximately 6) was analysed in the presence of strong acid with an average relative error of approximately 2%.

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

    USGS Publications Warehouse

    Shapiro, L.; Brannock, W.W.

    1955-01-01

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

  4. Probing the thermodynamics of protein-lipid interactions by isothermal titration calorimetry.

    PubMed

    Swamy, Musti J; Sankhala, Rajeshwer S

    2013-01-01

    Isothermal titration calorimetry is a highly sensitive technique for the study of molecular interactions. This method has been applied quite extensively to investigate the interaction of proteins with small ligands, other proteins, and nucleic acids as well as with drugs and metal ions. In this chapter, we describe the application of ITC for the investigation of thermodynamics of protein-lipid interaction. A number of parameters such as enthalpy of binding (ΔH), entropy of binding (ΔS), association constant (K (a)), binding stoichiometry (n), and free energy of binding (ΔG) can be obtained from a single calorimetric titration, providing a complete thermodynamic characterization of the interaction. The method is described in detail taking the major protein of the bovine seminal plasma, PDC-109, which exhibits a high preference for interaction with choline-containing lipids, as an example. The method can be applied to investigate the thermodynamics of the interaction of other soluble proteins with lipid membranes.

  5. [Indirect hemagglutination inhibition reactions as a method of titrating immune serums. V. Application of the reaction to the quantitative determination of immunoglobulins A, M and G in human blood sera].

    PubMed

    Konikova, R E; Semenova, B N; Noskov, F S; Shakhanina, K L; Malkina, L A

    1975-01-01

    The authors present the results of using the indirect hemagglutination inhibition test (IHIT) for quantitative determination of A, M and G immunoglobulins in the blood sera of humans in comparison with the method of radial immunodiffusion in agar (RID) after Mancini. The results of IHIT were no less precise and reproducible than those of RID. The significance of the correlation coefficient of grades after Spirman constituted greater than 99.9% for both tests. On this basis a conclusion was made that, having a number of advantages over RID, IHIT could be recommended for quantitative titration of immunoglobulins of various classes.

  6. Well acidizing compositions and method

    SciTech Connect

    Gardener, T.R.; Dill, W.R.; Ford, W.G.F.; King, K.L.

    1991-07-23

    This patent describes a concentrate which forms an acid internal microemulsion well treatment composition when added to an acid treatment fluid. It comprises in the range of from about 20% to about 98% by weight of a hydrocarbon carrier fluid; in the range of from about 1% to about 50% by weight of an alkyl alcohol having in the range of from about 4 to 18 carbon atoms; and in the range of from about 1% to about 50% by weight of an emulsifying agent comprising at least one compound selected from the group consisting of amine salts having ester or amide linkages and propoxylated alcohols, each of the components being different compounds or different mixtures of compounds.

  7. Ionic equilibria in neutral amphiprotic solvents of low dielectric constant: Titration curves.

    PubMed

    Bosch, E; Rosés, M

    1989-06-01

    Titration curves have been simulated for the titration of acids, bases and salts in neutral amphiprotic solvents such as isopropyl and tert-butyl alcohols. Ranges of pK values and acid concentrations have been examined. The incomplete dissociation of salts, which increases the acid or basic strength, has been found to be the major factor modifying the shape of the curve and the pH break. The theoretical predictions have been checked by titrating several series of acids and good agreement has been obtained between computed and experimental results.

  8. Method for sequencing nucleic acid molecules

    DOEpatents

    Korlach, Jonas; Webb, Watt W.; Levene, Michael; Turner, Stephen; Craighead, Harold G.; Foquet, Mathieu

    2006-05-30

    The present invention is directed to a method of sequencing a target nucleic acid molecule having a plurality of bases. In its principle, the temporal order of base additions during the polymerization reaction is measured on a molecule of nucleic acid, i.e. the activity of a nucleic acid polymerizing enzyme on the template nucleic acid molecule to be sequenced is followed in real time. The sequence is deduced by identifying which base is being incorporated into the growing complementary strand of the target nucleic acid by the catalytic activity of the nucleic acid polymerizing enzyme at each step in the sequence of base additions. A polymerase on the target nucleic acid molecule complex is provided in a position suitable to move along the target nucleic acid molecule and extend the oligonucleotide primer at an active site. A plurality of labelled types of nucleotide analogs are provided proximate to the active site, with each distinguishable type of nucleotide analog being complementary to a different nucleotide in the target nucleic acid sequence. The growing nucleic acid strand is extended by using the polymerase to add a nucleotide analog to the nucleic acid strand at the active site, where the nucleotide analog being added is complementary to the nucleotide of the target nucleic acid at the active site. The nucleotide analog added to the oligonucleotide primer as a result of the polymerizing step is identified. The steps of providing labelled nucleotide analogs, polymerizing the growing nucleic acid strand, and identifying the added nucleotide analog are repeated so that the nucleic acid strand is further extended and the sequence of the target nucleic acid is determined.

  9. Method for sequencing nucleic acid molecules

    DOEpatents

    Korlach, Jonas; Webb, Watt W.; Levene, Michael; Turner, Stephen; Craighead, Harold G.; Foquet, Mathieu

    2006-06-06

    The present invention is directed to a method of sequencing a target nucleic acid molecule having a plurality of bases. In its principle, the temporal order of base additions during the polymerization reaction is measured on a molecule of nucleic acid, i.e. the activity of a nucleic acid polymerizing enzyme on the template nucleic acid molecule to be sequenced is followed in real time. The sequence is deduced by identifying which base is being incorporated into the growing complementary strand of the target nucleic acid by the catalytic activity of the nucleic acid polymerizing enzyme at each step in the sequence of base additions. A polymerase on the target nucleic acid molecule complex is provided in a position suitable to move along the target nucleic acid molecule and extend the oligonucleotide primer at an active site. A plurality of labelled types of nucleotide analogs are provided proximate to the active site, with each distinguishable type of nucleotide analog being complementary to a different nucleotide in the target nucleic acid sequence. The growing nucleic acid strand is extended by using the polymerase to add a nucleotide analog to the nucleic acid strand at the active site, where the nucleotide analog being added is complementary to the nucleotide of the target nucleic acid at the active site. The nucleotide analog added to the oligonucleotide primer as a result of the polymerizing step is identified. The steps of providing labelled nucleotide analogs, polymerizing the growing nucleic acid strand, and identifying the added nucleotide analog are repeated so that the nucleic acid strand is further extended and the sequence of the target nucleic acid is determined.

  10. Determining enzyme kinetics via isothermal titration calorimetry.

    PubMed

    Demarse, Neil A; Killian, Marie C; Hansen, Lee D; Quinn, Colette F

    2013-01-01

    Isothermal titration calorimetry (ITC) has emerged as a powerful tool for determining the thermodynamic properties of chemical or physical equilibria such as protein-protein, ligand-receptor, and protein-DNA binding interactions. The utility of ITC for determining kinetic information, however, has not been fully recognized. Methods for collecting and analyzing data on enzyme kinetics are discussed here. The step-by-step process of converting the raw heat output rate into the kinetic parameters of the Michaelis-Menten equation is explicitly stated. The hydrolysis of sucrose by invertase is used to demonstrate the capability of the instrument and method.

  11. Studying Current-Potential Curves Using a Bipotentiometric Lodometric Back-Titration for the Determination of Ascorbic Acid in Fruits and Vegetables

    ERIC Educational Resources Information Center

    Verdini, Roxana A.; Lagier, Claudia M.

    2004-01-01

    Voltammetry principles are introduced to students by means of a bipotentiometric method to determine vitamin C in fruits and vegetables. The aim is to draw attention to voltammetric methods, particular to the study of current-potential curves, stressing the potential applicability in areas of food quality control.

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

    PubMed

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

    2013-01-01

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

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

    PubMed

    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.

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

    ERIC Educational Resources Information Center

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

    2004-01-01

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

  15. Fast coarse-grained model for RNA titration

    NASA Astrophysics Data System (ADS)

    Barroso da Silva, Fernando Luís; Derreumaux, Philippe; Pasquali, Samuela

    2017-01-01

    A new numerical scheme for RNA (ribonucleic acid) titration based on the Debye-Hückel framework for the salt description is proposed in an effort to reduce the computational costs for further applications to study protein-RNA systems. By means of different sets of Monte Carlo simulations, we demonstrated that this new scheme is able to correctly reproduce the experimental titration behavior and salt pKa shifts. In comparison with other theoretical approaches, similar or even better outcomes are achieved at much lower computational costs. The model was tested on the lead-dependent ribozyme, the branch-point helix, and the domain 5 from Azotobacter vinelandii Intron 5.

  16. An elevated temperature titration calorimeter

    SciTech Connect

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

    1991-06-01

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

  17. Wang-Landau Reaction Ensemble Method: Simulation of Weak Polyelectrolytes and General Acid-Base Reactions.

    PubMed

    Landsgesell, Jonas; Holm, Christian; Smiatek, Jens

    2017-02-14

    We present a novel method for the study of weak polyelectrolytes and general acid-base reactions in molecular dynamics and Monte Carlo simulations. The approach combines the advantages of the reaction ensemble and the Wang-Landau sampling method. Deprotonation and protonation reactions are simulated explicitly with the help of the reaction ensemble method, while the accurate sampling of the corresponding phase space is achieved by the Wang-Landau approach. The combination of both techniques provides a sufficient statistical accuracy such that meaningful estimates for the density of states and the partition sum can be obtained. With regard to these estimates, several thermodynamic observables like the heat capacity or reaction free energies can be calculated. We demonstrate that the computation times for the calculation of titration curves with a high statistical accuracy can be significantly decreased when compared to the original reaction ensemble method. The applicability of our approach is validated by the study of weak polyelectrolytes and their thermodynamic properties.

  18. Characterization of Titratable Amphiphiles in Lipid Membranes by Fluorescence Spectroscopy.

    PubMed

    Pierrat, Philippe; Lebeau, Luc

    2015-11-17

    Understanding the ionization behavior of lipid membranes is a key parameter for successful development of lipid-based drug delivery systems. Accurate determination of the ionization state of a titratable species incorporated in a lipid bilayer however requires special care. Herein we investigated the behavior of titratable lipids in liposomes by fluorescence spectroscopy and determined which extrinsic parameters-i.e., besides those directly related to their molecular structure-determine their ionization state. Two fluorescent dyes, TNS and R18, have been used to investigate basic and acidic titratable lipids, respectively. Our results suggest that the titration behavior of the ionizable lipid in the membrane is more sensitive to the composition of the membrane and to its physical state than to the presence of solutes in the aqueous phase. Essentially overlooked in earlier studies on ionizable lipid assemblies, the concentration of the titratable lipid in the membrane was found to have a major effect on the ionization state of the lipid polar head. This may result in a shift in the apparent pKa value which may be as large as two pKa units and cannot be satisfactorily predicted.

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

    PubMed

    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.

  20. Titration of Isolated Cell Walls of Lemna minor L 1

    PubMed Central

    Morvan, Claudine; Demarty, Maurice; Thellier, Michel

    1979-01-01

    A theoretical model has been built to bypass the equation of titration of the cell wall. This equation, which is an extension of the Henderson-Hasselbach equation, underlines the importance of the exchange constant, the ionic strength as well as the rate of neutralization. The model is restricted to the case when the ionization degree is equal to the neutralization degree. The shape of the titration curve is shown to be strongly dependent on the valency of the base used. Experimental results have shown that isolated cell walls bear at least two kinds of sites. The first sites which are titrated after a short time of equilibration are attributed to polyuronic acids (capacity: 0.3 milliequivalents per gram fresh cell walls). The second sites, are obtained after a long time of equilibration (capacity: 1.2 to 1.3 milliequivalents per gram, fresh cell walls). Titrations have been performed with different bases [KOH, NaOH, and Ca(OH)2] and under different ionic strengths. The results obtained with NaOH and KOH do not exhibit any difference of selectivity. Conversely, the sites have a much bigger affinity for the Ca2+ ions than for the monovalent ones. The apparent pKa of the uronic acids was estimated to lie between 3.0 and 3.4; this is consistent with the values obtained with polyuronic acid solutions. PMID:16660868

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

    NASA Astrophysics Data System (ADS)

    Last, Arthur M.

    1998-09-01

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

  2. Methods for analyzing nucleic acid sequences

    DOEpatents

    Korlach, Jonas; Webb, Watt W.; Levene, Michael; Turner, Stephen; Craighead, Harold G.; Foquet, Mathieu

    2011-05-17

    The present invention is directed to a method of sequencing a target nucleic acid. The method provides a complex comprising a polymerase enzyme, a target nucleic acid molecule, and a primer, wherein the complex is immobilized on a support Fluorescent label is attached to a terminal phosphate group of the nucleotide or nucleotide analog. The growing nucleic acid strand is extended by using the polymerase to add a nucleotide analog to the nucleic acid strand. The nucleotide analog added to the oligonucleotide primer as a result of the polymerizing step is identified. The time duration of the signal from labeled nucleotides or nucleotide analogs that become incorporated is distinguished from freely diffusing labels by a longer retention in the observation volume for the nucleotides or nucleotide analogs that become incorporated than for the freely diffusing labels.

  3. Phenolic acid esterases, coding sequences and methods

    DOEpatents

    Blum, David L.; Kataeva, Irina; Li, Xin-Liang; Ljungdahl, Lars G.

    2002-01-01

    Described herein are four phenolic acid esterases, three of which correspond to domains of previously unknown function within bacterial xylanases, from XynY and XynZ of Clostridium thermocellum and from a xylanase of Ruminococcus. The fourth specifically exemplified xylanase is a protein encoded within the genome of Orpinomyces PC-2. The amino acids of these polypeptides and nucleotide sequences encoding them are provided. Recombinant host cells, expression vectors and methods for the recombinant production of phenolic acid esterases are also provided.

  4. A Low-Cost Device for Automatic Photometric Titrations

    NASA Astrophysics Data System (ADS)

    Rocha, Fábio R. P.; Reis, Boaventura F.

    2000-02-01

    Electronics is an important topic in chemistry courses. However, the introduction of basic concepts is often difficult and the lab instruments are frequently seen as "black boxes". To address this problem, we propose the construction of a simple, low-cost (about $150 U.S.) automatic photometric titrator employing a light-emitting diode (LED) and a phototransistor. The electronic circuit can be assembled by the students themselves. The device was employed to implement a common procedure in chemical labs, making feasible the introduction of concepts related to electronics in undergraduate chemistry courses. The titrator is able to work automatically, since a feedback system permits stopping the addition of titrant solution when the end-point is achieved. With this demonstration, it can be stressed that automatic procedures can be implemented without expensive instruments. Additionally, a classical procedure becomes more attractive to the students and its importance to chemical analysis can be emphasized. The feasibility of the titrator was demonstrated by acid-base titrations of HCl solutions with NaOH in the presence of phenolphthalein and by iodimetric determination of ascorbic acid in vitamin C tablets and lemon juice. Precise results (0.7% relative standard deviation, n = 10) in agreement at the 95% confidence level with those attained by a conventional procedure were obtained.

  5. Determination of free acid by standard addition method in potassium thiocyanate

    SciTech Connect

    Baumann, E W

    1982-06-01

    The free acid content of solutions containing hydrolyzable ions has been determined potentiometrically by a standard addition method. Two increments of acid are added to the sample in 1M potassium thiocyanate solution. The sample concentration is calculated by solution of three simultaneous Nernst equations. The method has been demonstrated for solutions containing Al/sup 3 +/, Cr/sup 3 +/, Fe/sup 3 +/, Hg/sup 2 +/, Ni/sup 2 +/, Th/sup 4 +/, or UO/sub 2//sup 2 +/ with a metal-to-acid ratio of < 2.5. The method is suitable for determination of 10 ..mu..moles acid in 10 mL total volume. The accuracy can be judged from the agreement of the Nernst slopes found in the presence and absence of hydrolyzable ions. The relative standard deviation is < 2.5%. The report includes a survey of experiments with thermometric, pH, and Gran plot titrations in a variety of complexants, from which the method was evolved. Also included is a literature survey of sixty references, a discussion of the basic measurements, and a complete analytical procedure.

  6. Risks and Benefits of Rapid Clozapine Titration

    PubMed Central

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

    2016-01-01

    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. PMID:27403276

  7. Risks and Benefits of Rapid Clozapine Titration.

    PubMed

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

    2016-05-18

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

  8. Molecular Titration Promotes Oscillations and Bistability in Minimal Network Models with Monomeric Regulators.

    PubMed

    Cuba Samaniego, Christian; Giordano, Giulia; Kim, Jongmin; Blanchini, Franco; Franco, Elisa

    2016-04-15

    Molecular titration is emerging as an important biochemical interaction mechanism within synthetic devices built with nucleic acids and the CRISPR/Cas system. We show that molecular titration in the context of feedback circuits is a suitable mechanism to enhance the emergence of oscillations and bistable behaviors. We consider biomolecular modules that can be inhibited or activated by input monomeric regulators; the regulators compete with constitutive titrating species to determine the activity of their target. By tuning the titration rate and the concentration of titrating species, it is possible to modulate the delay and convergence speed of the transient response, and the steepness and dead zone of the stationary response of the modules. These phenomena favor the occurrence of oscillations when modules are interconnected to create a negative feedback loop; bistability is favored in a positive feedback interconnection. Numerical simulations are supported by mathematical analysis showing that the capacity of the closed loop systems to exhibit oscillations or bistability is structural.

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

    PubMed

    Zhai, Jingying; Xie, Xiaojiang; Bakker, Eric

    2015-08-18

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

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

    PubMed

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

    2010-01-05

    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.

  11. Isothermal Titration Calorimetry Can Provide Critical Thinking Opportunities

    ERIC Educational Resources Information Center

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

    2016-01-01

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

  12. Isothermal Titration Calorimetry to Characterize Enzymatic Reactions.

    PubMed

    Mazzei, Luca; Ciurli, Stefano; Zambelli, Barbara

    2016-01-01

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

  13. A Tabular Approach to Titration Calculations

    ERIC Educational Resources Information Center

    Lim, Kieran F.

    2012-01-01

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

  14. Determination of free acid by standard addition method in potassium thiocyanate

    SciTech Connect

    Not Available

    1981-06-01

    An analytical method for determination of free acidity in all SRP process solutions has been developed. Free acidity was successfully determined in solutions of nitric acid and the nitrates of aluminum, chromium(III), iron(III), mercury(II), nickel(II), thorium, and uranium(VI), at metal-to-acid ratios <2.5. Sample requirements, instrumentation, and mode of operation are similar to those currently used in the Laboratories Department free acid procedures. The simple procedure would be suitable for automation and microprocessor control. The method consists of two additions of known increments of acid into a solution containing the sample aliquot (10 ..mu..moles free acid) and 10 mL 1M potassium thiocyanate. The potential is determined in the initial solution and after each addition with a glass electrode and pH meter. The sample concentration is calculated by solution of three simultaneous Nernst equations. Two programs for this iterative computation are available: one written for the PDP-15 computer and another for a Hewlett-Packard 67 (or 97) programmable calculator. The accuracy of the result is verified by a slope that approximates the theoretical Nernst value. The relative standard deviation is <2.5%. This memorandum includes a survey of experiments with thermometric, pH, and Gran plot titrations in a variety of complexants, from which this particular system and technique logically evolved. The appendix includes a literature survey of sixty references, a discussion of the basic measurements, and a complete analytical procedure. The final step for completion of this RTA is training and consultation at the convenience of the Laboratories Department for demonstration of the method with process samples.

  15. Method for the production of dicarboxylic acids

    DOEpatents

    Nghiem, Nhuan Phu; Donnelly, Mark; Millard, Cynthia S.; Stols, Lucy

    1999-01-01

    The present invention is an economical fermentation method for the production of carboxylic acids comprising the steps of a) inoculating a medium having a carbon source with a carboxylic acid-producing organism; b) incubating the carboxylic acid-producing organism in an aerobic atmosphere to promote rapid growth of the organism thereby increasing the biomass of the organism; c) controllably releasing oxygen to maintain the aerobic atmosphere; d) controllably feeding the organism having increased biomass with a solution containing the carbon source to maintain the concentration of the carbon source within the medium of about 0.5 g/L up to about 1 g/L; e) depriving the aerobic atmosphere of oxygen to produce an anaerobic atmosphere to cause the organism to undergo anaerobic metabolism; f) controllably feeding the organism having increased biomass a solution containing the carbon source to maintain the concentration of the carbon source within the medium of .gtoreq.1 g/L; and g) converting the carbon source to carboxylic acids using the anaerobic metabolism of the organism.

  16. Method for the production of dicarboxylic acids

    DOEpatents

    Nghiem, N.P.; Donnelly, M.; Millard, C.S.; Stols, L.

    1999-02-09

    The present invention is an economical fermentation method for the production of carboxylic acids comprising the steps of (a) inoculating a medium having a carbon source with a carboxylic acid-producing organism; (b) incubating the carboxylic acid-producing organism in an aerobic atmosphere to promote rapid growth of the organism thereby increasing the biomass of the organism; (c) controllably releasing oxygen to maintain the aerobic atmosphere; (d) controllably feeding the organism having increased biomass with a solution containing the carbon source to maintain the concentration of the carbon source within the medium of about 0.5 g/l up to about 1 g/l; (e) depriving the aerobic atmosphere of oxygen to produce an anaerobic atmosphere to cause the organism to undergo anaerobic metabolism; (f) controllably feeding the organism having increased biomass a solution containing the carbon source to maintain the concentration of the carbon source within the medium of {>=}1 g/l; and (g) converting the carbon source to carboxylic acids using the anaerobic metabolism of the organism. 7 figs.

  17. Use of an in vivo titration method to study a global regulator: effect of varying Lrp levels on expression of gltBDF in Escherichia coli.

    PubMed Central

    Borst, D W; Blumenthal, R M; Matthews, R G

    1996-01-01

    Most studies of global regulatory proteins are performed in vitro or involve phenotypic comparisons between wild-type and mutant strains. We report the use of strains in which the gene for the leucine-responsive regulatory protein (lrp) is transcribed from isopropyl-beta-D-thiogalactopyranoside (IPTG)-inducible promoters for the purpose of continuously varying the in vivo concentration of Lrp. To obtain a broad range of Lrp concentrations, strains were employed that contained the lrp fusion either in the chromosome (I. C. Blomfield, P. J. Calie, K. J. Eberhardt, M. S. McClain, and B. I. Eisenstein, J. Bacteriol. 175:27-36, 1993) or on a multicopy plasmid. Western blot (immunoblot) analysis with polyclonal antiserum to Lrp confirmed that Lrp levels could be varied more than 70-fold by growing the strains in glucose minimal 3-(N-morpholino)propanesulfonic acid (MOPS) medium containing different amounts of IPTG. Expression of an Lrp-regulated gltB::lacZ operon fusion was measured over this range of Lrp concentrations. beta-Galactosidase activity rose with increasing Lrp levels up to the level of Lrp found in wild-type strains, at which point expression is maximal. The presence of leucine in the medium increased the level of Lrp necessary to achieve half-maximal expression of the gltB::lacZ fusion, as predicted by earlier in vitro studies (B. R. Ernsting, J. W. Denninger, R. M. Blumenthal, and R. G. Matthews, J. Bacteriol. 175:7160-7169, 1993). Interestingly, levels of Lrp greater than those in wild-type cells interfered with activation of gltB::lacZ expression. The growth rate of cultures correlated with the intracellular Lrp concentration: levels of Lrp either lower or higher than wild-type levels resulted in significantly slower growth rates. Thus, the level of Lrp in the cell appears to be optimal for rapid growth in minimal medium, and the gltBDF control region is designed to give maximal expression at this Lrp level. PMID:8955313

  18. Applications of isothermal titration calorimetry in protein science.

    PubMed

    Liang, Yi

    2008-07-01

    During the past decade, isothermal titration calorimetry (ITC) has developed from a specialist method for understanding molecular interactions and other biological processes within cells to a more robust, widely used method. Nowadays, ITC is used to investigate all types of protein interactions, including protein-protein interactions, protein-DNA/RNA interactions, protein-small molecule interactions and enzyme kinetics; it provides a direct route to the complete thermodynamic characterization of protein interactions. This review concentrates on the new applications of ITC in protein folding and misfolding, its traditional application in protein interactions, and an overview of what can be achieved in the field of protein science using this method and what developments are likely to occur in the near future. Also, this review discusses some new developments of ITC method in protein science, such as the reverse titration of ITC and the displacement method of ITC.

  19. Asphalt compatibility testing using the automated Heithaus titration test

    SciTech Connect

    Pauli, A.T.

    1996-12-31

    The Heithaus titration test or variations of the test have been used for over 35 years to predict compatibilities of blends of asphalts from different crude sources. Asphalt compatibility is determined from three calculated parameters that measure the state of peptization of an asphalt or asphalt blend. The parameter p{sub a} is a measure of the peptizability of the asphaltenes. The parameter p{sub a} is a measure of the peptizing power of the maltenes, and the parameter P, derived from p{sub a} and p{sub o} values, is a measure of the overall state of peptization of the asphalt or asphalt blend. In Heithaus original procedure, samples of asphalt were dissolved in toluene and titrated with n-heptane in order to initiate flocculation. The onset of flocculation was detected either by photography or by spotting a filter paper with a small amount of the titrated solution. Recently, an {open_quotes}automated{close_quotes} procedure, after Hotier and Robin, has been developed for use with asphalt. In the automated method UV-visible spectrophotometric detection measures the onset of flocculation as a peak with the percent transmittance plotted as a function of the volume of titrating solvent added to a solution of asphalt. The automated procedure has proven to be less operator dependent and much faster than the original Heithaus procedure. Results from the automated procedure show the data to be consistent with results from the original, {open_quotes}classical{close_quotes} Heithaus procedure.

  20. Titration of gold nanoparticles in phase extraction.

    PubMed

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

    2015-12-07

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

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

    PubMed

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

    2016-05-01

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

  2. Analysis of heavy oils: Method development and application to Cerro Negro heavy petroleum detailed separation and analysis of acidic compounds

    SciTech Connect

    Green, J.B.; Yu, S.K.T.; Green, J.A.; Doughty, D.A.; Vogh, J.W.; Grigsby, R.D.

    1989-10-01

    An HPLC method for fractionation of whole acid concentrates into nominal compound class subfractions is described. The method utilizes silica columns and gradient elution with eluents containing a strong base, tetramethyl-ammonium hydroxide. The performance of the method is evaluated through analysis of subfractions obtained from a coal liquid, Wilmington, CA, petroleum and Cerro Negro heavy oil. Methods developed specifically for analysis of whole acid concentrates and subfractions are described in detail. These include: (1) an infrared method for determination of total hydroxyl and carboxyl groups after their conversion to trifluoroacetate and 2,2,2-trifluoresters, respectively. (2) an NMR method for functional group analysis based on methylation of acidic groups with {sup 13}C-enriched methyl iodide, (3) a nonaqueous titration procedure employing the potassium salt of dimethyl sulfoxide as a titrant for acidic compounds, (4) GC/MS analysis of hydroxyaromatic compounds after their conversion to trifluoroacetate esters, and (5) probe microdistillation high resolution mass spectrometric analysis of acid fractions exhibiting low volatility. 146 refs., 38 figs., 27 tabs.

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

    PubMed

    Tanaka, Hideji; Baba, Tsutomu

    2005-10-15

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

  4. Aquaporin-4 antibody titration in NMO patients treated with rituximab

    PubMed Central

    Marnetto, Fabiana; Granieri, Letizia; Capobianco, Marco; Bertolotto, Antonio

    2016-01-01

    Objective: We undertook an observational retrospective study to investigate the usefulness of aquaporin-4 (AQP4) antibodies (Ab) titration in the management of patients with neuromyelitis optica (NMO) treated with rituximab (RTX) by studying (1) the correlation between AQP4-Ab titer and disease activity, (2) the influence of RTX on antibody levels, and (3) the association between AQP4-Ab levels and responsiveness to RTX. Methods: A cell-based assay was used for AQP4-Ab titration in 322 serum samples from 7 patients with NMO treated with RTX (median follow-up 65 months), according to a treatment-to-target approach. Serum samples were collected every month following standardized procedures. Results: (1) In group analysis, AQP4-Ab titers correlated with the disease activity, showing higher titers during and preceding relapses than during remission. However, in individual analysis, an increase in AQP4-Ab titers and CD19+ B cells did not always precede a relapse. (2) A reduction of AQP4-Ab titers in the short-term and long-term period was observed during RTX treatment. (3) Reduction of AQP4-Ab titers was observed in responder patients both 3 months after RTX infusion and in the long-term follow-up. In one nonresponder patient, AQP4-Ab levels never decreased during the treatment period. Conclusions: Titration of AQP4-Abs could be useful in the clinical management of patients with NMO treated with RTX: titration before each reinfusion and 3 months after each reinfusion may provide information about responsiveness to RTX. Although a relationship among AQP4-Ab levels, disease activity, and response to RTX was observed, the usefulness of AQP4-Ab titration to predict relapses is limited. PMID:28054001

  5. Method of increasing conversion of a fatty acid to its corresponding dicarboxylic acid

    DOEpatents

    Craft, David L.; Wilson, C. Ron; Eirich, Dudley; Zhang, Yeyan

    2004-09-14

    A nucleic acid sequence including a CYP promoter operably linked to nucleic acid encoding a heterologous protein is provided to increase transcription of the nucleic acid. Expression vectors and host cells containing the nucleic acid sequence are also provided. The methods and compositions described herein are especially useful in the production of polycarboxylic acids by yeast cells.

  6. Titration of vaccinia virus by intravenous injection of chick embryos

    PubMed Central

    Kaplan, C.

    1960-01-01

    The final test of a smallpox vaccine is its capacity to prevent the disease from developing in inoculated individuals. This capacity, however, cannot be measured directly, so that other methods of assessing the efficacy of vaccine have had to be developed. A laboratory method—pock counting on the chorio-allantoic membrane of chick embryos—has recently been shown to provide a reasonably reliable estimate of the number of infective units in a given vaccine. In this paper, the author compares this pock-counting method with another method—titration by intravenous injection of chick embryos. He concludes that, although the reproducibility of titrations by intravenous injection compares very favourably with that obtained by chorio-allantoic inoculation, the former method would not be advantageous for the assay of vaccines, since it is very time-consuming and since differences in virulence might obscure comparisons between the efficacy of vaccines. PMID:14404376

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

    SciTech Connect

    Selig, W.

    1982-04-01

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

  8. Titration of hydrophobic polyelectrolytes using Monte Carlo simulations.

    PubMed

    Ulrich, Serge; Laguecir, Abohachem; Stoll, Serge

    2005-03-01

    The conformation and titration curves of weak (or annealed) hydrophobic polyelectrolytes have been examined using Monte Carlo simulations with screened Coulomb potentials in the grand canonical ensemble. The influence of the ionic concentration pH and presence of hydrophobic interactions has been systematically investigated. A large number of conformations such as extended, pearl-necklace, cigar-shape, and collapsed structures resulting from the subtle balance of short-range hydrophobic attractive interactions and long-range electrostatic repulsive interactions between the monomers have been observed. Titration curves were calculated by adjusting the pH-pK(0) values (pK(0) represents the intrinsic dissociation constant of an isolated monomer) and then calculating the ionization degree alpha of the polyelectrolyte. Important transitions related to cascades of conformational changes were observed in the titration curves, mainly at low ionic concentration and with the presence of strong hydrophobic interactions. We demonstrated that the presence of hydrophobic interactions plays an important role in the acid-base properties of a polyelectrolyte in promoting the formation of compact conformations and hence decreasing the polyelectrolyte degree of ionization for a given pH-pK(0) value.

  9. Calibrationless determination of creatinine and ammonia by coulometric flow titration.

    PubMed

    He, Z K; Fuhrmann, B; Spohn, U

    2000-08-01

    A precise and sensitive working microflow titration procedure was developed to determine creatinine and ammonia in urine samples. This procedure is based on enzymatic conversion of creatinine, gas diffusional membrane separation of the released ammonia into an acid acceptor stream, and coulometric titration of ammonia with hypobromite. The hypobromite is formed after the electrogeneration of bromine in an electrolyte containing 1.0 M NaBr and 0.1 M sodium borate adjusted to pH 8.5. The electrolysis current follows a triangle-programmed current-time course. An amperometric flow detector records the resulting mirror symmetrical titration curves, which show two equivalence points. The analyte concentration is calculated from the time difference between the equivalence points. For quantitative conversion of creatinine and quantitative separation of present and released ammonia no calibration is necessary to get accurate results. Both ammonia/ammonium and creatinine were determined in the range between 2 microM and 2 mM with relative standard deviations between 3.0 and 1.0% (n = 5). High recoveries were obtained for the analysis of diluted urine samples for both creatinine and ammonia.

  10. Monitoring RNA-ligand interactions using isothermal titration calorimetry.

    PubMed

    Gilbert, Sunny D; Batey, Robert T

    2009-01-01

    Isothermal titration calorimetry (ITC) is a biophysical technique that measures the heat evolved or absorbed during a reaction to report the enthalpy, entropy, stoichiometry of binding, and equilibrium association constant. A significant advantage of ITC over other methods is that it can be readily applied to almost any RNA-ligand complex without having to label either molecule and can be performed under a broad range of pH, temperature, and ionic concentrations. During our application of ITC to investigate the thermodynamic details of the interaction of a variety of compounds with the purine riboswitch, we have explored and optimized experimental parameters that yield the most useful and reproducible results for RNAs. In this chapter, we detail this method using the titration of an adenine-binding RNA with 2,6-diaminopurine (DAP) as a practical example. Our insights should be generally applicable to observing the interactions of a broad range of molecules with structured RNAs.

  11. Potentiometric titration of heterocyclic nitrogen bases in non-aqueous media.

    PubMed

    Rao, K C; Naidu, P R

    1972-11-01

    Pyridine, quinoline, isoquinoline, acridine, alpha-picoline, beta-picoline, gamma-picoline and 2,6-lutidine have been titrated potentio-metrically (calomel and glass electrodes), with chlorosulphonic acid in methyl ethyl ketone-acetic acid (1:1) medium, with an error of less than 1%.

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

    Technology Transfer Automated Retrieval System (TEKTRAN)

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

  13. Precise coulometric titration of sodium thiosulfate and development of potassium iodate as a redox standard.

    PubMed

    Asakai, Toshiaki; Murayama, Mariko; Tanaka, Tatsuhiko

    2007-09-15

    In this paper, we determine the effective purity of potassium iodate as a redox standard with a certified value linked to the international system of units (SI units). Concentration measurement of sodium thiosulfate solution was performed by precise coulometric titration with electrogenerated iodine, and an assay of potassium iodate was carried out by gravimetric titration based on the reductometric factor of sodium thiosulfate assigned by coulometry. The accuracy of the coulometric titration method was evaluated by examining the current efficiency of iodine electrogeneration, stability of sodium thiosulfate solutions and dependence on the amount of sodium thiosulfate solution used. The measurement procedure for gravimetric titration of potassium iodate with sodium thiosulfate was validated based on determination of a reference material of known purity (potassium dichromate determined by coulometry with electrogenerated ferrous ions) using the same gravimetric method. Solutions of 0.2 and 0.5mol/L sodium thiosulfate were stable over 17 days without stabilizer. Investigation of the dependency of titration results on the amount of sodium thiosulfate solution used showed no significant effects, no evidence of diffusion of the sample, and no effect of contamination appearing during the experiment. Precise coulometric titration of sodium thiosulfate achieved a relative standard deviation of less than 0.005% under repeating conditions (six measurements). For gravimetric titration, the results obtained for the effective purity of potassium dichromate were sufficiently close to its certified value to allow confirmation of the validity of the gravimetric titration was confirmed. The relative standard deviation of gravimetric titration for potassium iodate was less than 0.011% (nine measurements), and a redox standard with a certified value linked to SI units was developed.

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

    USGS Publications Warehouse

    Wahlberg, James S.; Skinner, Dwight L.; Rader, Lewis F.

    1956-01-01

    A new method for determining uranium in samples containing 0.05 percent or more U3O8, using titanous sulfate as reducing agent, is much shorter, faster, and has fewer interferences than conventional methods using reductor columns. The sample is dissolved with sulfuric, nitric, perchloric, and hydrofluoric acids. Elements that would otherwise form insoluble fluorides are kept in solution by complexing the fluoride ion with boric acid. A precipitation is made with cupferron to remove interfering elements. The solution is filtered to remove the precipitated cupferrates instead of extracting them with chloroform as is usually done. Filtration is preferred to extraction because any niobium that may be in solution forms an insoluble cupferrate that may be removed by filtering but is very difficult to extract with chloroform. Excess cupferron is destroyed by oxidizing with nitric and perchloric acids, and evaporating to dense fumes of sulfuric acid. The uranium is reduced to U(IV) by the addition of titanous sulfate, with cupric sulfate used as an indicator of the completeness of the reduction. Metallic copper is formed when all the uranium is reduced. The reduced copper is then reoxidized by the addition of mercuric perchlorate, an excess of ferric sulfate added, and the solution titrated immediately with standard ceric sulfate with ferroin as an indicator. Precision of the method compared favorable with methods in common use, both for uranium ores and for most types of uranium-rich materials.

  15. Copper and cobalt complexes of octadentate azamacrocycles: spectrophotometric titration, stopped-flow kinetics and crystallographic study.

    PubMed

    Ozay, Hava; Baran, Yakup; Ishii, Youichi

    2011-12-01

    Details of complex formation kinetics are reported for tetrakis(2-hydroxyethyl) substituted cyclen (L(1)) and cyclam (L(2)) with Cu(II) and Co(II). Stopped-flow kinetics and spectroscopic titration methods were employed for the activation parameters and stability constants, respectively. X-ray studies revealed that the pendant 2-hydroxyethyl groups are not equivalent: two are folded over the macrocycle and maintained by intramolecular hydrogen bonds while the others are extended and pointed away from the macrocyclic cavity. Complex formation kinetics and spectroscopic titration were performed in aqueous acidic buffer solutions. Thermodynamic and kinetic parameters revealed that the ring size of the macrocycles plays an extremely important role for each metal ion studied. Stopped-flow kinetic measurements explained the mechanism of the complex formation process of both Cu(II) and Co(II) which proceed in outer-sphere interactions with ligands. There are two steps in the complex formation of the system studied. The initial step is a second order reaction between the metal ion and macrocycle with a second order rate constant.

  16. Advances in nucleic acid-based detection methods.

    PubMed Central

    Wolcott, M J

    1992-01-01

    Laboratory techniques based on nucleic acid methods have increased in popularity over the last decade with clinical microbiologists and other laboratory scientists who are concerned with the diagnosis of infectious agents. This increase in popularity is a result primarily of advances made in nucleic acid amplification and detection techniques. Polymerase chain reaction, the original nucleic acid amplification technique, changed the way many people viewed and used nucleic acid techniques in clinical settings. After the potential of polymerase chain reaction became apparent, other methods of nucleic acid amplification and detection were developed. These alternative nucleic acid amplification methods may become serious contenders for application to routine laboratory analyses. This review presents some background information on nucleic acid analyses that might be used in clinical and anatomical laboratories and describes some recent advances in the amplification and detection of nucleic acids. PMID:1423216

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

    PubMed

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

    2005-06-14

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

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

    PubMed

    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

  19. Ozone Cross-Section Measurement by Gas Phase Titration.

    PubMed

    Viallon, Joële; Moussay, Philippe; Flores, Edgar; Wielgosz, Robert I

    2016-11-01

    Elevated values of ground-level ozone damage health, vegetation, and building materials and are the subject of air quality regulations. Levels are monitored by networks using mostly ultraviolet (UV) absorption instruments, with traceability to standard reference photometers, relying on the UV absorption of ozone at the 253.65 nm line of mercury. We have redetermined the ozone cross-section at this wavelength based on gas phase titration (GPT) measurements. This is a well-known chemical method using the reaction of ozone (O3) with nitrogen monoxide (NO) resulting in nitrogen dioxide (NO2) and oxygen (O2). The BIPM GPT facility uses state-of-the-art flow measurement, chemiluminescence for NO concentration measurements, a cavity phase shift analyzer (CAPS) for NO2 measurements, and a UV ozone analyzer. The titration experiment is performed over the concentration range 100-500 nmol/mol, with NO and NO2 reactants/calibrants diluted down from standards with nominal mole fractions of 50 μmol/mol. Accurate measurements of NO, NO2, and O3 mole fractions allow the calculation of ozone absorption cross section values at 253.65 nm, and we report a value of 11.24 × 10(-18) cm(2) molecule(-1) with a relative expanded uncertainty of 1.8% (coverage factor k = 2) based on nitrogen monoxide titration values and a value of 11.22 × 10(-18) cm(2) molecule(-1) with a relative expanded uncertainty of 1.4% (coverage factor k = 2) based on nitrogen dioxide titration values. The excellent agreement between these values and recently published absorption cross-section measurements directly on pure ozone provide strong evidence for revising the conventionally accepted value of ozone cross section at 253.65 nm.

  20. Method for nucleic acid isolation using supercritical fluids

    SciTech Connect

    Nivens, David E.; Applegate, Bruce M.

    1999-01-01

    A method for detecting the presence of a microorganism in an environmental sample involves contacting the sample with a supercritical fluid to isolate nucleic acid from the microorganism, then detecting the presence of a particular sequence within the isolated nucleic acid. The nucleic acid may optionally be subjected to further purification.

  1. Method for nucleic acid isolation using supercritical fluids

    DOEpatents

    Nivens, D.E.; Applegate, B.M.

    1999-07-13

    A method is disclosed for detecting the presence of a microorganism in an environmental sample involves contacting the sample with a supercritical fluid to isolate nucleic acid from the microorganism, then detecting the presence of a particular sequence within the isolated nucleic acid. The nucleic acid may optionally be subjected to further purification. 4 figs.

  2. Virtual Titrator: A Student-Oriented Instrument.

    ERIC Educational Resources Information Center

    Ritter, David; Johnson, Michael

    1997-01-01

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

  3. Isothermal Titration Calorimetry in the Student Laboratory

    ERIC Educational Resources Information Center

    Wadso, Lars; Li, Yujing; Li, Xi

    2011-01-01

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

  4. Method for identifying and quantifying nucleic acid sequence aberrations

    DOEpatents

    Lucas, J.N.; Straume, T.; Bogen, K.T.

    1998-07-21

    A method is disclosed for detecting nucleic acid sequence aberrations by detecting nucleic acid sequences having both a first and a second nucleic acid sequence type, the presence of the first and second sequence type on the same nucleic acid sequence indicating the presence of a nucleic acid sequence aberration. The method uses a first hybridization probe which includes a nucleic acid sequence that is complementary to a first sequence type and a first complexing agent capable of attaching to a second complexing agent and a second hybridization probe which includes a nucleic acid sequence that selectively hybridizes to the second nucleic acid sequence type over the first sequence type and includes a detectable marker for detecting the second hybridization probe. 11 figs.

  5. Method for identifying and quantifying nucleic acid sequence aberrations

    DOEpatents

    Lucas, Joe N.; Straume, Tore; Bogen, Kenneth T.

    1998-01-01

    A method for detecting nucleic acid sequence aberrations by detecting nucleic acid sequences having both a first and a second nucleic acid sequence type, the presence of the first and second sequence type on the same nucleic acid sequence indicating the presence of a nucleic acid sequence aberration. The method uses a first hybridization probe which includes a nucleic acid sequence that is complementary to a first sequence type and a first complexing agent capable of attaching to a second complexing agent and a second hybridization probe which includes a nucleic acid sequence that selectively hybridizes to the second nucleic acid sequence type over the first sequence type and includes a detectable marker for detecting the second hybridization probe.

  6. Continuous-flow free acid monitoring method and system

    DOEpatents

    Strain, James E.; Ross, Harley H.

    1981-01-01

    A free acid monitoring method and apparatus is provided for continuously measuring the excess acid present in a process stream. The disclosed monitoring system and method is based on the relationship of the partial pressure ratio of water and acid in equilibrium with an acid solution at constant temperature. A portion of the process stream is pumped into and flows through the monitor under the influence of gravity and back to the process stream. A continuous flowing sample is vaporized at a constant temperature and the vapor is subsequently condensed. Conductivity measurements of the condensate produces a nonlinear response function from which the free acid molarity of the sample process stream is determined.

  7. Continuous-flow free acid monitoring method and system

    DOEpatents

    Strain, J.E.; Ross, H.H.

    1980-01-11

    A free acid monitoring method and apparatus is provided for continuously measuring the excess acid present in a process stream. The disclosed monitoring system and method is based on the relationship of the partial pressure ratio of water and acid in equilibrium with an acid solution at constant temperature. A portion of the process stream is pumped into and flows through the monitor under the influence of gravity and back to the process stream. A continuous flowing sample is vaporized at a constant temperature and the vapor is subsequently condensed. Conductivity measurements of the condensate produces a nonlinear response function from which the free acid molarity of the sample process stream is determined.

  8. Sulfuric acid thermoelectrochemical system and method

    DOEpatents

    Ludwig, Frank A.

    1989-01-01

    A thermoelectrochemical system in which an electrical current is generated between a cathode immersed in a concentrated sulfuric acid solution and an anode immersed in an aqueous buffer solution of sodium bisulfate and sodium sulfate. Reactants consumed at the electrodes during the electrochemical reaction are thermochemically regenerated and recycled to the electrodes to provide continuous operation of the system.

  9. Methods of refining and producing isomerized fatty acid esters and fatty acids from natural oil feedstocks

    DOEpatents

    Snead, Thomas E.; Cohen, Steven A.; Gildon, Demond L.; Beltran, Leslie V.; Kunz, Linda A.; Pals, Tessa M.; Quinn, Jordan R; Behrends, Jr., Raymond T.; Bernhardt, Randal J.

    2016-07-05

    Methods are provided for refining natural oil feedstocks and producing isomerized esters and acids. The methods comprise providing a C4-C18 unsaturated fatty ester or acid, and isomerizing the fatty acid ester or acid in the presence of heat or an isomerization catalyst to form an isomerized fatty ester or acid. In some embodiments, the methods comprise forming a dibasic ester or dibasic acid prior to the isomerizing step. In certain embodiments, the methods further comprise hydrolyzing the dibasic ester to form a dibasic acid. In certain embodiments, the olefin is formed by reacting the feedstock in the presence of a metathesis catalyst under conditions sufficient to form a metathesized product comprising olefins and esters, separating the olefins from the esters in the metathesized product, and transesterifying the esters in the presence of an alcohol to form a transesterified product having unsaturated esters.

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

    NASA Astrophysics Data System (ADS)

    Ebling, A. M.; Schijf, J.

    2008-12-01

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

  11. Reaction titration: a convenient method for titering reactive hydride agents (Red-Al, LiAlH4, DIBALH, L-Selectride, NaH, and KH) by No-D NMR spectroscopy.

    PubMed

    Hoye, Thomas R; Aspaas, Andrew W; Eklov, Brian M; Ryba, Troy D

    2005-05-26

    The concentration of reactive metal hydride (Met-H) reducing agents can be determined (in < or = 20 min) using No-D NMR spectroscopy. The method involves (i) reacting Met-H with an excess of p-methoxybenzaldehyde, (ii) quenching with excess acetic acid, (iii) recording the No-D NMR spectrum of this homogeneous mixture, and (iv) deducing the concentration of Met-H from the % conversion (as measured by integration). By a conceptually related method, the titer of the basic alkali metal hydrides KH and NaH can also be determined.

  12. Boron containing amino acid compounds and methods for their use

    DOEpatents

    Glass, John D.; Coderre, Jeffrey A.

    2000-01-01

    The present invention provides new boron containing amino acid compounds and methods for making these compounds by contacting melphalan or another nitrogen mustard derivative and sodium borocaptate. The present invention also provides a method of treating a mammal having a tumor by administering to the mammal a therapeutically effective amount of the new boron containing amino acid compounds.

  13. Boron containing amino acid compounds and methods for their use

    SciTech Connect

    Glass, J.D.; Coderre, J.A.

    2000-01-25

    The present invention provides new boron containing amino acid compounds and methods for making these compounds by contacting melphalan or another nitrogen mustard derivative and sodium borocaptate. The present invention also provides a method of treating a mammal having a tumor by administering to the mammal a therapeutically effective amount of the new boron containing amino acid compounds.

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

    PubMed

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

    2005-10-15

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

  15. Acid-base properties of titanium-antimony oxides catalysts

    SciTech Connect

    Zenkovets, G.A.; Paukshtis, E.A.; Tarasova, D.V.; Yurchenko, E.N.

    1982-06-01

    The acid-base properties of titanium-antimony oxide catalysts were studied by the methods of back titration and ir spectroscopy. The interrelationship between the acid-base and catalytic properties in the oxidative ammonolysis of propylene was discussed. 3 figures, 1 table.

  16. Mutant fatty acid desaturase and methods for directed mutagenesis

    DOEpatents

    Shanklin, John; Whittle, Edward J.

    2008-01-29

    The present invention relates to methods for producing fatty acid desaturase mutants having a substantially increased activity towards substrates with fewer than 18 carbon atom chains relative to an unmutagenized precursor desaturase having an 18 carbon chain length specificity, the sequences encoding the desaturases and to the desaturases that are produced by the methods. The present invention further relates to a method for altering a function of a protein, including a fatty acid desaturase, through directed mutagenesis involving identifying candidate amino acid residues, producing a library of mutants of the protein by simultaneously randomizing all amino acid candidates, and selecting for mutants which exhibit the desired alteration of function. Candidate amino acids are identified by a combination of methods. Enzymatic, binding, structural and other functions of proteins can be altered by the method.

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

    PubMed Central

    Wu, Grace; Wollen, Alec; Himley, Stephen; Austin, Glenn; Delarosa, Jaclyn; Izadnegahdar, Rasa; Ginsburg, Amy Sarah; Zehrung, Darin

    2017-01-01

    Background Continuous oxygen treatment is essential for managing children with hypoxemia, but access to oxygen in low-resource countries remains problematic. Given the high burden of pneumonia in these countries and the fact that flow can be gradually reduced as therapy progresses, oxygen conservation through routine titration warrants exploration. Aim To determine the amount of oxygen saved via titration during oxygen therapy for children with hypoxemic pneumonia. Methods Based on published clinical data, we developed a model of oxygen flow rates needed to manage hypoxemia, assuming recommended flow rate at start of therapy, and comparing total oxygen used with routine titration every 3 minutes or once every 24 hours versus no titration. Results Titration every 3 minutes or every 24 hours provided oxygen savings estimated at 11.7% ± 5.1% and 8.1% ± 5.1% (average ± standard error of the mean, n = 3), respectively. For every 100 patients, 44 or 30 kiloliters would be saved—equivalent to 733 or 500 hours at 1 liter per minute. Conclusions Ongoing titration can conserve oxygen, even performed once-daily. While clinical validation is necessary, these findings could provide incentive for the routine use of pulse oximeters for patient management, as well as further development of automated systems. PMID:28234903

  18. Potentiometric/turbidometric titration of antiperspirant actives.

    PubMed

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

    2003-01-01

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

  19. Acetoclastic methanogenic activity measurement by a titration bioassay.

    PubMed

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

    2002-01-05

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

  20. Compositions and method for controlling precipitation when acidizing sour wells

    SciTech Connect

    Dill, W.R.; Walker, M.L.

    1990-08-21

    This patent describes a method of treating a sour well penetrating a subterranean formation. It comprises: introducing into the well a treating fluid comprising an acid solution having a pH below 1.9, an iron sequestering agent comprising at least one compound selected from the group consisting of aminopolycarboxylic acids, hydroxycarboxylic acids, cyclic polyethers and derivatives of the acids and ethers, present in an amount of from about 0.25 to about 5 percent by weight of the acid solution, and a sulfide modifier comprising at least one compound selected from the group consisting of an aldehyde, acetal, hemiacetal and any other compound capable of forming aldehydes in the acid solution, present in an amount of from about 0.25 to about 5 percent of the acid solution; and treating the subterranean formation with the treating fluid.

  1. Fluorometric Method for Determination of Uric Acid in Flour

    DTIC Science & Technology

    1980-07-01

    of the excreta of adult Tribolium used in this study for natural infestation, accumulates in infested products providing a quantitative measure of past...by Adult Tribolium 8 4 FLUOROMETRIC METHOD FOR DETERMINATION OF URIC ACID IN FLOUR Introduction Chemical and microanalytical techniques have been...determining uric acid content.’ Approximately 18% of the total excreta from Tribolium confusum is uric acid.2 Various investigators have established

  2. Human jagged polypeptide, encoding nucleic acids and methods of use

    DOEpatents

    Li, Linheng; Hood, Leroy

    2000-01-01

    The present invention provides an isolated polypeptide exhibiting substantially the same amino acid sequence as JAGGED, or an active fragment thereof, provided that the polypeptide does not have the amino acid sequence of SEQ ID NO:5 or SEQ ID NO:6. The invention further provides an isolated nucleic acid molecule containing a nucleotide sequence encoding substantially the same amino acid sequence as JAGGED, or an active fragment thereof, provided that the nucleotide sequence does not encode the amino acid sequence of SEQ ID NO:5 or SEQ ID NO:6. Also provided herein is a method of inhibiting differentiation of hematopoietic progenitor cells by contacting the progenitor cells with an isolated JAGGED polypeptide, or active fragment thereof. The invention additionally provides a method of diagnosing Alagille Syndrome in an individual. The method consists of detecting an Alagille Syndrome disease-associated mutation linked to a JAGGED locus.

  3. 40 CFR 425.03 - Sulfide analytical methods and applicability.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... Provisions § 425.03 Sulfide analytical methods and applicability. (a) The potassium ferricyanide titration... the potassium ferricyanide titration method for the determination of sulfide in wastewaters...

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

    PubMed

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

    2009-07-15

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

  5. Method for incorporating radioactive phosphoric acid solutions in concrete

    DOEpatents

    Wolf, G.A.; Smith, J.W.; Ihle, N.C.

    1982-07-08

    A method for incorporating radioactive phosphoric acid solutions in concrete is described wherein the phosphoric acid is reacted with Ca(OH)/sub 2/ to form a precipitate of hydroxyapatite and the hydroxyapatite is mixed with Portland cement to form concrete.

  6. Method for incorporating radioactive phosphoric acid solutions in concrete

    DOEpatents

    Wolf, Gary A [Kennewick, WA; Smith, Jeffrey W [Lancaster, OH; Ihle, Nathan C [Walla Walla, WA

    1984-01-01

    A method for incorporating radioactive phosphoric acid solutions in concrete is described wherein the phosphoric acid is reacted with Ca(OH).sub.2 to form a precipitate of hydroxyapatite and the hydroxyapatite is mixed with portland cement to form concrete.

  7. Titrimetric and photometric methods for determination of hypochlorite in commercial bleaches.

    PubMed

    Jonnalagadda, Sreekanth B; Gengan, Prabhashini

    2010-01-01

    Two methods, simple titration and photometric methods for determination of hypochlorite are developed, based its reaction with hydrogen peroxide and titration of the residual peroxide by acidic permanganate. In the titration method, the residual hydrogen peroxide is estimated by titration with standard permanganate solution to estimate the hypochlorite concentration. The photometric method is devised to measure the concentration of remaining permanganate, after the reaction with residual hydrogen peroxide. It employs 4 ranges of calibration curves to enable the determination of hypochlorite accurately. The new photometric method measures hypochlorite in the range 1.90 x 10(-3) to 1.90 x 10(-2) M, with high accuracy and with low variance. The concentrations of hypochlorite in diverse commercial bleach samples and in seawater which is enriched with hypochlorite were estimated using the proposed method and compared with the arsenite method. The statistical analysis validates the superiority of the proposed method.

  8. The origin of multiply sigmoid curves of pH-dependence. The partitioning of groups among titration pK values.

    PubMed

    Dixon, H B; Clarke, S D; Smith, G A; Carne, T K

    1991-08-15

    An acid, HnA, with n ionizing groups is known to have the same titration curve as an equimolar mixture of n hypothetical monobasic acids, whose dissociation constants are known as the 'titration constants' of the real acid. We show that the pH-dependence of any property of HnA is also represented by the sum of one-site titration curves, characterized by these same titration constants. Since one such property is the degree of dissociation of one of the dissociating groups, a fraction of each group shows each of the various titration pK values, so that the group partitions among them. The n groups therefore share the same n titration pK values but differ in the fractions belonging to each. The one H+ ion per molecule that titrates with each pK is thus made up of the fractions, one from each group, that share this pK value. A group may possess a single pK value, in that it contributes virtually all of this pK and almost nothing to the others, only if either (1) in titrates in a different pH range from the other groups or (2) its affinity for H+ is unaffected by their ionization state.

  9. The influence of mechanochemical modification on prevention of toxic ability of humic acids towards phenanthrene in aquatic environment

    NASA Astrophysics Data System (ADS)

    Shekhovtsova, N. S.; Maltseva, E. V.; Glyzina, T. S.; Ovchinnikova, I. S.

    2015-11-01

    The aim of the research work is to quantify interaction between phenanthrene with modified humic acids in aquatic environment. The changes in the structure and properties of humic acids after modifications were studied with 1H NMR spectroscopy and potentiometric titration methods. Our research demonstrates that the application of thiourea as a modified agent increases the binding capacity of humic acids towards phenanthrene.

  10. Methods and compositions for efficient nucleic acid sequencing

    DOEpatents

    Drmanac, Radoje

    2006-07-04

    Disclosed are novel methods and compositions for rapid and highly efficient nucleic acid sequencing based upon hybridization with two sets of small oligonucleotide probes of known sequences. Extremely large nucleic acid molecules, including chromosomes and non-amplified RNA, may be sequenced without prior cloning or subcloning steps. The methods of the invention also solve various current problems associated with sequencing technology such as, for example, high noise to signal ratios and difficult discrimination, attaching many nucleic acid fragments to a surface, preparing many, longer or more complex probes and labelling more species.

  11. Methods and compositions for efficient nucleic acid sequencing

    DOEpatents

    Drmanac, Radoje

    2002-01-01

    Disclosed are novel methods and compositions for rapid and highly efficient nucleic acid sequencing based upon hybridization with two sets of small oligonucleotide probes of known sequences. Extremely large nucleic acid molecules, including chromosomes and non-amplified RNA, may be sequenced without prior cloning or subcloning steps. The methods of the invention also solve various current problems associated with sequencing technology such as, for example, high noise to signal ratios and difficult discrimination, attaching many nucleic acid fragments to a surface, preparing many, longer or more complex probes and labelling more species.

  12. Validation of two methods for fatty acids analysis in eggs.

    PubMed

    Mazalli, Mônica R; Bragagnolo, Neura

    2007-05-01

    A comparative study between two methods (lipid extraction followed by saponification and methylation, and direct methylation) to determine the fatty acids in egg yolk was evaluated. Direct methylation of the samples resulted in lower fatty acid content and greater variation in the results than the lipid extraction followed by saponification and methylation. The low repeatability observed for the direct HCl methylation method was probably due to a less efficient extraction and conversion of the fatty acids into their methyl esters as compared to the same procedure starting with the lipid extract. As the lipid extraction followed by esterification method was shown to be more precise it was validated using powdered egg certified as reference material (RM 8415, NIST) and applied to samples of egg, egg enriched with polyunsaturated omega-3 fatty acids (n-3 PUFA), and commercial spray-dried whole egg powder.

  13. Fatty acids determination in Bronte pistachios by gas chromatographic method.

    PubMed

    Pantano, Licia; Lo Cascio, Giovanni; Alongi, Angelina; Cammilleri, Gaetano; Vella, Antonio; Macaluso, Andrea; Cicero, Nicola; Migliazzo, Aldo; Ferrantelli, Vincenzo

    2016-10-01

    A gas chromatographic with flame ionization detector (GC-MS FID) method for the identification and quantification of fatty acids based on the extraction of lipids and derivatisation of free acids to form methyl esters was developed and validated. The proposed method was evaluated to a number of standard FAs, and Bronte pistachios samples were used for that purpose and to demonstrate the applicability of the proposed method. In this regard, repeatability, mean and standard deviation of the analytical procedure were calculated. The results obtained have demonstrated oleic acid as the main component of Bronte pistachios (72.2%) followed by linoleic acid (13.4%) and showed some differences in composition with respect to Tunisian, Turkish and Iranian pistachios.

  14. A rapid automated procedure for laboratory and shipboard spectrophotometric measurements of seawater alkalinity: continuously monitored single-step acid additions

    NASA Astrophysics Data System (ADS)

    Liu, X.; Byrne, R. H.; Lindemuth, M.; Easley, R. A.; Patsavas, M. C.

    2012-12-01

    An automated system for shipboard and laboratory alkalinity measurements is presented. The simple system, which consists of a Dosimat titrator to deliver acid volumetrically and a USB 4000 spectrophotometer to monitor the titration progress, provides fast, precise and accurate measurements of total alkalinity for oceanographic research. The analytical method is based on single-point HCl titrations of seawater samples of a known volume; bromol cresol purple is used as an indicator to determine the final pH. Field data from an Arctic cruise demonstrates accuracy and precision around 1 micro mol/kg and a sample processing rate of 6 min per sample.

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

    PubMed

    Price, Randi; Wan, Ping

    2010-01-01

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

  16. Acid-base properties of water-soluble organic matter of forest soils, studied by the pK-spectroscopy method.

    PubMed

    Shamrikova, E V; Ryazanov, M A; Vanchikova, E V

    2006-11-01

    Using the potentiometric titration and pK spectroscopy method, acid-base properties of water-soluble organic matter of forest soils have been studied. Five acidic classes composed of different substances with pK(a) values around 3.6; 4.8; 6.7; 8.7 and 9.7 have been identified. Testing the properties of soluble soil fraction, it is to be taken into account that when it is isolated from non-soluble soil matter, some water-soluble substances remain in soil and do not pass into the solution. Most firmly adsorbed in soil are water-soluble components with pK(a) 9.6-9.8.

  17. A visual detection of protein content based on titration of moving reaction boundary electrophoresis.

    PubMed

    Wang, Hou-Yu; Guo, Cheng-Ye; Guo, Chen-Gang; Fan, Liu-Yin; Zhang, Lei; Cao, Cheng-Xi

    2013-04-24

    A visual electrophoretic titration method was firstly developed from the concept of moving reaction boundary (MRB) for protein content analysis. In the developed method, when the voltage was applied, the hydroxide ions in the cathodic vessel moved towards the anode, and neutralized the carboxyl groups of protein immobilized via highly cross-linked polyacrylamide gel (PAG), generating a MRB between the alkali and the immobilized protein. The boundary moving velocity (V(MRB)) was as a function of protein content, and an acid-base indicator was used to denote the boundary displacement. As a proof of concept, standard model proteins and biological samples were chosen for the experiments to study the feasibility of the developed method. The experiments revealed that good linear calibration functions between V(MRB) and protein content (correlation coefficients R>0.98). The experiments further demonstrated the following merits of developed method: (1) weak influence of non-protein nitrogen additives (e.g., melamine) adulterated in protein samples, (2) good agreement with the classic Kjeldahl method (R=0.9945), (3) fast measuring speed in total protein analysis of large samples from the same source, and (4) low limit of detection (0.02-0.15 mg mL(-1) for protein content), good precision (R.S.D. of intra-day less than 1.7% and inter-day less than 2.7%), and high recoveries (105-107%).

  18. Measuring Multivalent Binding Interactions by Isothermal Titration Calorimetry.

    PubMed

    Dam, Tarun K; Talaga, Melanie L; Fan, Ni; Brewer, Curtis F

    2016-01-01

    Multivalent glycoconjugate-protein interactions are central to many important biological processes. Isothermal titration calorimetry (ITC) can potentially reveal the molecular and thermodynamic basis of such interactions. However, calorimetric investigation of multivalency is challenging. Binding of multivalent glycoconjugates to proteins (lectins) often leads to a stoichiometry-dependent precipitation process due to noncovalent cross-linking between the reactants. Precipitation during ITC titration severely affects the quality of the baseline as well as the signals. Hence, the resulting thermodynamic data are not dependable. We have made some modifications to address this problem and successfully studied multivalent glycoconjugate binding to lectins. We have also modified the Hill plot equation to analyze high quality ITC raw data obtained from multivalent binding. As described in this chapter, ITC-driven thermodynamic parameters and Hill plot analysis of ITC raw data can provide valuable information about the molecular mechanism of multivalent lectin-glycoconjugate interactions. The methods described herein revealed (i) the importance of functional valence of multivalent glycoconjugates, (ii) that favorable entropic effects contribute to the enhanced affinities associated with multivalent binding, (iii) that with the progression of lectin binding, the microscopic affinities of the glycan epitopes of a multivalent glycoconjugate decrease (negative cooperativity), (iv) that lectin binding to multivalent glycoconjugates, especially to mucins, involves internal diffusion jumps, (bind and jump) and (v) that scaffolds of glycoconjugates influence their entropy of binding.

  19. Measuring the Kinetics of Molecular Association by Isothermal Titration Calorimetry.

    PubMed

    Vander Meulen, Kirk A; Horowitz, Scott; Trievel, Raymond C; Butcher, Samuel E

    2016-01-01

    The real-time power response inherent in an isothermal titration calorimetry (ITC) experiment provides an opportunity to directly analyze association kinetics, which, together with the conventional measurement of thermodynamic quantities, can provide an incredibly rich description of molecular binding in a single experiment. Here, we detail our application of this method, in which interactions occurring with relaxation times ranging from slightly below the instrument response time constant (12.5 s in this case) to as large as 600 s can be fully detailed in terms of both the thermodynamics and kinetics. In a binding titration scenario, in the most general case an injection can reveal an association rate constant (kon). Under more restrictive conditions, the instrument time constant-corrected power decay following each injection is simply an exponential decay described by a composite rate constant (kobs), from which both kon and the dissociation rate constant (koff) can be extracted. The data also support the viability of this exponential approach, for kon only, for a slightly larger set of conditions. Using a bimolecular RNA folding model and a protein-ligand interaction, we demonstrate and have internally validated this approach to experiment design, data processing, and error analysis. An updated guide to thermodynamic and kinetic regimes accessible by ITC is provided.

  20. Characterization of protein-protein interactions by isothermal titration calorimetry.

    PubMed

    Velazquez-Campoy, Adrian; Leavitt, Stephanie A; Freire, Ernesto

    2015-01-01

    The analysis of protein-protein interactions has attracted the attention of many researchers from both a fundamental point of view and a practical point of view. From a fundamental point of view, the development of an understanding of the signaling events triggered by the interaction of two or more proteins provides key information to elucidate the functioning of many cell processes. From a practical point of view, understanding protein-protein interactions at a quantitative level provides the foundation for the development of antagonists or agonists of those interactions. Isothermal Titration Calorimetry (ITC) is the only technique with the capability of measuring not only binding affinity but the enthalpic and entropic components that define affinity. Over the years, isothermal titration calorimeters have evolved in sensitivity and accuracy. Today, TA Instruments and MicroCal market instruments with the performance required to evaluate protein-protein interactions. In this methods paper, we describe general procedures to analyze heterodimeric (porcine pancreatic trypsin binding to soybean trypsin inhibitor) and homodimeric (bovine pancreatic α-chymotrypsin) protein associations by ITC.

  1. Titration of chaos with added noise

    PubMed Central

    Poon, Chi-Sang; Barahona, Mauricio

    2001-01-01

    Deterministic chaos has been implicated in numerous natural and man-made complex phenomena ranging from quantum to astronomical scales and in disciplines as diverse as meteorology, physiology, ecology, and economics. However, the lack of a definitive test of chaos vs. random noise in experimental time series has led to considerable controversy in many fields. Here we propose a numerical titration procedure as a simple “litmus test” for highly sensitive, specific, and robust detection of chaos in short noisy data without the need for intensive surrogate data testing. We show that the controlled addition of white or colored noise to a signal with a preexisting noise floor results in a titration index that: (i) faithfully tracks the onset of deterministic chaos in all standard bifurcation routes to chaos; and (ii) gives a relative measure of chaos intensity. Such reliable detection and quantification of chaos under severe conditions of relatively low signal-to-noise ratio is of great interest, as it may open potential practical ways of identifying, forecasting, and controlling complex behaviors in a wide variety of physical, biomedical, and socioeconomic systems. PMID:11416195

  2. Phenol-Sulfuric Acid Method for Total Carbohydrates

    NASA Astrophysics Data System (ADS)

    Nielsen, S. Suzanne

    The phenol-sulfuric acid method is a simple and rapid colorimetric method to determine total carbohydrates in a sample. The method detects virtually all classes of carbohydrates, including mono-, di-, oligo-, and polysaccharides. Although the method detects almost all carbohydrates, the absorptivity of the different carbohydrates varies. Thus, unless a sample is known to contain only one carbohydrate, the results must be expressed arbitrarily in terms of one carbohydrate.

  3. Electroanalytical measurements without electrolytes: conducting polymers as probes for redox titration in non-conductive organic media.

    PubMed

    Lange, Ulrich; Mirsky, Vladimir M

    2012-09-26

    Electroanalytical methods have been applied only in conducting media. An application of conducting polymers allows to overcome this limitation. If such material is in electrochemical equilibrium with dissolved redox active species, its electrical conductivity depends on the redox potential of these species. Therefore, conductometric measurements with conducting polymers can provide about the same information as classical redox electrodes. The approach was applied for redox titration. Equivalent points obtained by this titration in aqueous and organic electrolytes were identical. Then the approach was applied for determination of bromine number by redox titration in non-conducting organic phase.

  4. Multiwavelength spectrophotometric determination of acidity constants of some azo dyes

    NASA Astrophysics Data System (ADS)

    Shamsipur, Mojtaba; Maddah, Bozorgmehr; Hemmateenejad, Bahram; Rouhani, Shohreh; Haghbeen, Kamaladin; Alizadeh, Kamal

    2008-06-01

    A multiwavelength spectrophotometric titration method was applied to study the acidity constants of some azo dyes in water. The UV-vis absorption spectra of azo dye solutions were recorded in the course of their pH-metric titration with a standard base solution. The protolytic equilibrium constants, spectral profiles, concentration diagrams and also the number of components have been calculated. The quantitative effects of the substituents on the acidity of the studied azo dyes were investigated by the linear free energy relationship (LFER) using Hammet sigma constant ( σ) and field and resonance effects of Kamlet and Taft ( f and ℜ, respectively).

  5. Multiwavelength spectrophotometric determination of acidity constants of some azo dyes.

    PubMed

    Shamsipur, Mojtaba; Maddah, Bozorgmehr; Hemmateenejad, Bahram; Rouhani, Shohreh; Haghbeen, Kamaladin; Alizadeh, Kamal

    2008-06-01

    A multiwavelength spectrophotometric titration method was applied to study the acidity constants of some azo dyes in water. The UV-vis absorption spectra of azo dye solutions were recorded in the course of their pH-metric titration with a standard base solution. The protolytic equilibrium constants, spectral profiles, concentration diagrams and also the number of components have been calculated. The quantitative effects of the substituents on the acidity of the studied azo dyes were investigated by the linear free energy relationship (LFER) using Hammet sigma constant (sigma) and field and resonance effects of Kamlet and Taft (f and Re, respectively).

  6. Fast and selective determination of total protein in milk powder via titration of moving reaction boundary electrophoresis.

    PubMed

    Guo, Cheng-ye; Wang, Hou-yu; Liu, Xiao-ping; Fan, Liu-yin; Zhang, Lei; Cao, Cheng-xi

    2013-05-01

    In this paper, moving reaction boundary titration (MRBT) was developed for rapid and accurate quantification of total protein in infant milk powder, from the concept of moving reaction boundary (MRB) electrophoresis. In the method, the MRB was formed by the hydroxide ions and the acidic residues of milk proteins immobilized via cross-linked polyacrylamide gel (PAG), an acid-base indicator was used to denote the boundary motion. As a proof of concept, we chose five brands of infant milk powders to study the feasibility of MRBT method. The calibration curve of MRB velocity versus logarithmic total protein content of infant milk powder sample was established based on the visual signal of MRB motion as a function of logarithmic milk protein content. Weak influence of nonprotein nitrogen (NPN) reagents (e.g., melamine and urea) on MRBT method was observed, due to the fact that MRB was formed with hydroxide ions and the acidic residues of captured milk proteins, rather than the alkaline residues or the NPN reagents added. The total protein contents in infant milk powder samples detected via the MRBT method were in good agreement with those achieved by the classic Kjeldahl method. In addition, the developed method had much faster measuring speed compared with the Kjeldahl method.

  7. Method for enhancing amidohydrolase activity of fatty acid amide hydrolase

    SciTech Connect

    John, George; Nagarajan, Subbiah; Chapman, Kent; Faure, Lionel; Koulen, Peter

    2016-10-25

    A method for enhancing amidohydrolase activity of Fatty Acid Amide Hydrolase (FAAH) is disclosed. The method comprising administering a phenoxyacylethanolamide that causes the enhanced activity. The enhanced activity can have numerous effects on biological organisms including, for example, enhancing the growth of certain seedlings. The subject matter disclosed herein relates to enhancers of amidohydrolase activity.

  8. Method to produce succinic acid from raw hydrolysates

    DOEpatents

    Donnelly, Mark I.; Sanville-Millard, Cynthia Y.; Nghiem, Nhuan Phu

    2004-06-01

    A method for producing succinic acid from industrial-grade hydrolysates is provided, comprising supplying an organism that contains mutations for the genes ptsG, pflB, and ldhA, allowing said organism to accumulate biomass, and allowing said organism to metabolize the hydrolysate. Also provided is a bacteria mutant characterized in that it produces succinic acid from substrate contained in industrial-grade hydrolysate in a ratio of between 0.6:1 and 1.3:1 succinic acid to substrate.

  9. Determination of organic acids by CE and CEC methods.

    PubMed

    Klampfl, Christian W

    2007-10-01

    A comprehensive overview of the analysis of low-molecular-mass organic acids employing electromigration methods in the capillary format is given. This review includes papers published since 2003 and can be seen as an update of the review paper published by Galli et al. in 2003. Tables included in this review contain application papers describing the determination of organic acids from a variety of fields like the analysis of food and beverages, environmental samples, samples from clinical origin, and from natural products.

  10. Nucleic acid amplification: Alternative methods of polymerase chain reaction

    PubMed Central

    Fakruddin, Md; Mannan, Khanjada Shahnewaj Bin; Chowdhury, Abhijit; Mazumdar, Reaz Mohammad; Hossain, Md. Nur; Islam, Sumaiya; Chowdhury, Md. Alimuddin

    2013-01-01

    Nucleic acid amplification is a valuable molecular tool not only in basic research but also in application oriented fields, such as clinical medicine development, infectious diseases diagnosis, gene cloning and industrial quality control. A comperehensive review of the literature on the principles, applications, challenges and prospects of different alternative methods of polymerase chain reaction (PCR) was performed. PCR was the first nucleic acid amplification method. With the advancement of research, a no of alternative nucleic acid amplification methods has been developed such as loop mediated isothermal amplification, nucleic acid sequence based amplification, strand displacement amplification, multiple displacement amplification. Most of the alternative methods are isothermal obviating the need for thermal cyclers. Though principles of most of the alternate methods are relatively complex than that of PCR, they offer better applicability and sensitivity in cases where PCR has limitations. Most of the alternate methods still have to prove themselves through extensive validation studies and are not available in commercial form; they pose the potentiality to be used as replacements of PCR. Continuous research is going on in different parts of the world to make these methods viable technically and economically. PMID:24302831

  11. Nucleic acid amplification: Alternative methods of polymerase chain reaction.

    PubMed

    Fakruddin, Md; Mannan, Khanjada Shahnewaj Bin; Chowdhury, Abhijit; Mazumdar, Reaz Mohammad; Hossain, Md Nur; Islam, Sumaiya; Chowdhury, Md Alimuddin

    2013-10-01

    Nucleic acid amplification is a valuable molecular tool not only in basic research but also in application oriented fields, such as clinical medicine development, infectious diseases diagnosis, gene cloning and industrial quality control. A comperehensive review of the literature on the principles, applications, challenges and prospects of different alternative methods of polymerase chain reaction (PCR) was performed. PCR was the first nucleic acid amplification method. With the advancement of research, a no of alternative nucleic acid amplification methods has been developed such as loop mediated isothermal amplification, nucleic acid sequence based amplification, strand displacement amplification, multiple displacement amplification. Most of the alternative methods are isothermal obviating the need for thermal cyclers. Though principles of most of the alternate methods are relatively complex than that of PCR, they offer better applicability and sensitivity in cases where PCR has limitations. Most of the alternate methods still have to prove themselves through extensive validation studies and are not available in commercial form; they pose the potentiality to be used as replacements of PCR. Continuous research is going on in different parts of the world to make these methods viable technically and economically.

  12. Evaluation of acidity estimation methods for mine drainage, Pennsylvania, USA.

    PubMed

    Park, Daeryong; Park, Byungtae; Mendinsky, Justin J; Paksuchon, Benjaphon; Suhataikul, Ratda; Dempsey, Brian A; Cho, Yunchul

    2015-01-01

    Eighteen sites impacted by abandoned mine drainage (AMD) in Pennsylvania were sampled and measured for pH, acidity, alkalinity, metal ions, and sulfate. This study compared the accuracy of four acidity calculation methods with measured hot peroxide acidity and identified the most accurate calculation method for each site as a function of pH and sulfate concentration. Method E1 was the sum of proton and acidity based on total metal concentrations; method E2 added alkalinity; method E3 also accounted for aluminum speciation and temperature effects; and method E4 accounted for sulfate speciation. To evaluate errors between measured and predicted acidity, the Nash-Sutcliffe efficiency (NSE), the coefficient of determination (R (2)), and the root mean square error to standard deviation ratio (RSR) methods were applied. The error evaluation results show that E1, E2, E3, and E4 sites were most accurate at 0, 9, 4, and 5 of the sites, respectively. Sites where E2 was most accurate had pH greater than 4.0 and less than 400 mg/L of sulfate. Sites where E3 was most accurate had pH greater than 4.0 and sulfate greater than 400 mg/L with two exceptions. Sites where E4 was most accurate had pH less than 4.0 and more than 400 mg/L sulfate with one exception. The results indicate that acidity in AMD-affected streams can be accurately predicted by using pH, alkalinity, sulfate, Fe(II), Mn(II), and Al(III) concentrations in one or more of the identified equations, and that the appropriate equation for prediction can be selected based on pH and sulfate concentration.

  13. Retardation signal for fluorescent determination of total protein content via rapid and sensitive chip moving reaction boundary electrophoretic titration.

    PubMed

    Wang, Houyu; Shi, Yongting; Yan, Jian; Dong, Jingyu; Li, Si; Xiao, Hua; Xie, Haiyang; Fan, Liu-Yin; Cao, Cheng-Xi

    2014-03-18

    A novel concept and theory of moving reaction boundary (MRB) retardation signal (RMRB) was advanced for determination of total protein content via MRB electrophoretic titration (MRBET). The theoretical results revealed that the retardation extent of boundary displacment, viz., the RMRB value, was as a function of protein content. Thus, the RMRB value of a sample could be used to determine its total protein content according to the relevant calibration curve. To demonstrate the concept and theoretical results, a novel microdevice was designed for the relevant experiments of MRBET. The microdevice has 30 identical work cells, each of which is composed of five ultrashort single microchannels (5 mm). In the microdevice, fluorescein isothiocyanate (FITC) was used to denote MRB motion and RMRB value for the first time, the polyacrylamide gel (PAG) containing protein sample was photopolymerized in microchannels, and the MRB was created with acid or alkali and target protein sample. As compared to the classic Kjeldahl method and conventional MRBET performed in glass tube, the developed titration chip has the following merits: good sensitivity (0.3-0.4 μg/mL vs 150-200 μg/mL of protein concentration, 0.6-0.8 ng vs 30-2000 μg of absolute protein content), rapid analysis (20-60 s vs 15-200 min), and portable low-power (15 V vs 200 V).

  14. The evaluation method for antiplatelet effect of acetylsalicylic acid.

    PubMed

    Yokoyama, Haruko; Mastumura, Takashi; Soeda, Shinji; Suzuki, Yuji; Watanabe, Masayuki; Kashiwakura, Emiko; Saso, Takayuki; Ikeda, Noriyuki; Tokuoka, Kentaro; Kitagawa, Yasuhisa; Yamada, Yasuhiko

    2014-12-01

    Reduced platelet aggregation by acetylsalicylic acid administration has been associated with adverse outcomes in patients with thrombotic diseases, thus it is important to determine aspirin resistance in those cases. The antiplatelet effect of acetylsalicylic acid is rarely measured, but it has many problems. The aim of this study was to find the evaluation method for antiplatelet effect after administration of acetylsalicylic acid. We developed a particle counting method based upon laser light scattering, and utilized the platelet aggregation agonists, collagen, at 0.25, 0.5 and 1.0 μg/mL, and adenosine diphosphate (ADP), at 0.5, 1.0 and 2.0 μM, to determine their effective concentrations. Seventeen healthy volunteers were administered acetylsalicylic acid at 162 mg/day, with platelet aggregation determined before and 20 min after administration. In all subjects, the rate of platelet aggregation induced by 1.0 μg/mL of collagen before taking acetylsalicylic acid was the highest value obtained, while 20 min after acetylsalicylic acid administration, aggregation induced by collagen at 1.0 μg/mL was significantly decreased as compared to before administration. As for the other concentrations of collagen and all those of ADP tested, platelet aggregation was either not significantly induced before taking acetylsalicylic acid or the rate of aggregation was not significantly decreased after taking acetylsalicylic acid. Our results indicate that collagen at 1.0 μg/mL is appropriate as a platelet aggregation agonist for evaluating the antiplatelet effect of acetylsalicylic acid. Thus, it is useful that the measurement is performed only once.

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

    PubMed

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

    2016-06-01

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

  16. Methods And Devices For Characterizing Duplex Nucleic Acid Molecules

    DOEpatents

    Akeson, Mark; Vercoutere, Wenonah; Haussler, David; Winters-Hilt, Stephen

    2005-08-30

    Methods and devices are provided for characterizing a duplex nucleic acid, e.g., a duplex DNA molecule. In the subject methods, a fluid conducting medium that includes a duplex nucleic acid molecule is contacted with a nanopore under the influence of an applied electric field and the resulting changes in current through the nanopore caused by the duplex nucleic acid molecule are monitored. The observed changes in current through the nanopore are then employed as a set of data values to characterize the duplex nucleic acid, where the set of data values may be employed in raw form or manipulated, e.g., into a current blockade profile. Also provided are nanopore devices for practicing the subject methods, where the subject nanopore devices are characterized by the presence of an algorithm which directs a processing means to employ monitored changes in current through a nanopore to characterize a duplex nucleic acid molecule responsible for the current changes. The subject methods and devices find use in a variety of applications, including, among other applications, the identification of an analyte duplex DNA molecule in a sample, the specific base sequence at a single nulceotide polymorphism (SNP), and the sequencing of duplex DNA molecules.

  17. A Full Automatic Device for Sampling Small Solution Volumes in Photometric Titration Procedure Based on Multicommuted Flow System

    PubMed Central

    Borges, Sivanildo S.; Vieira, Gláucia P.; Reis, Boaventura F.

    2007-01-01

    In this work, an automatic device to deliver titrant solution into a titration chamber with the ability to determine the dispensed volume of solution, with good precision independent of both elapsed time and flow rate, is proposed. A glass tube maintained at the vertical position was employed as a container for the titrant solution. Electronic devices were coupled to the glass tube in order to control its filling with titrant solution, as well as the stepwise solution delivering into the titration chamber. The detection of the titration end point was performed employing a photometer designed using a green LED (λ=545 nm) and a phototransistor. The titration flow system comprised three-way solenoid valves, which were assembled to allow that the steps comprising the solution container loading and the titration run were carried out automatically. The device for the solution volume determination was designed employing an infrared LED (λ=930 nm) and a photodiode. When solution volume delivered from proposed device was within the range of 5 to 105 μl, a linear relationship (R = 0.999) between the delivered volumes and the generated potential difference was achieved. The usefulness of the proposed device was proved performing photometric titration of hydrochloric acid solution with a standardized sodium hydroxide solution and using phenolphthalein as an external indicator. The achieved results presented relative standard deviation of 1.5%. PMID:18317510

  18. Isothermal Titration Calorimetry of Chiral Polymeric Nanoparticles.

    PubMed

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

    2015-09-01

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

  19. An equilibrium model for ligand-modified micellar-enhanced ultrafiltration. Selective separation of metal ions using iminoacetic substituted polyamines and a theoretical model for the titration behavior of polyamines

    SciTech Connect

    Dharmawardana, Udeni Rajaratna

    1992-01-01

    This thesis consists of three chapters. Chapter 1, An equilibrium model for ligand-modified micellar-enhanced ultrafiltration, describes a theoretical model and experimental investigations which used the semi-equilibrium-dialysis method with N-n-dodecyl iminodiacetic acid as the ligand. In Chapter 2, Selective separation of metal ions using iminoacetic substituted polyamines, polyamines with a substituted ligand group are synthesized and used in investigating selective separation of copper ions from aqueous solution. In Chapter 3, A theoretical model for the titration behavior of polyamines, a novel approach to explain the titration behavior of polymeric amines based on the binding behavior of counterions is described. The application of this study is to the investigation of inexpensive and efficient methods of industrial waste water treatment.

  20. A method to attenuate U(VI) mobility in acidic waste plumes using humic acids

    SciTech Connect

    Wan, J.; Dong, W.; Tokunaga, T.K.

    2011-02-01

    Acidic uranium (U) contaminated plumes have resulted from acid-extraction of plutonium during the Cold War and from U mining and milling operations. A sustainable method for in-situ immobilization of U under acidic conditions is not yet available. Here, we propose to use humic acids (HAs) for in-situ U immobilization in acidic waste plumes. Our laboratory batch experiments show that HA can adsorb onto aquifer sediments rapidly, strongly and practically irreversibly. Adding HA greatly enhanced U adsorption capacity to sediments at pH below 5.0. Our column experiments using historically contaminated sediments from the Savannah River Site under slow flow rates (120 and 12 m/y) show that desorption of U and HA were non-detectable over 100 pore-volumes of leaching with simulated acidic groundwaters. Upon HA-treatment, 99% of the contaminant [U] was immobilized at pH < 4.5, compared to 5% and 58% immobilized in the control columns at pH 3.5 and 4.5, respectively. These results demonstrated that HA-treatment is a promising in-situ remediation method for acidic U waste plumes. As a remediation reagent, HAs are resistant to biodegradation, cost effective, nontoxic, and easily introducible to the subsurface.

  1. [Determination of total protein content in soya-bean milk via visual moving reaction boundary titration].

    PubMed

    Guo, Chengye; Wang, Houyu; Zhang, Lei; Fan, Liuyin; Cao, Chengxi

    2013-11-01

    A visual, rapid and accurate moving reaction boundary titration (MRBT) method was used for the determination of the total protein in soya-bean milk. During the process, moving reaction boundary (MRB) was formed by hydroxyl ions in the catholyte and soya-bean milk proteins immobilized in polyacrylamide gel (PAG), and an acid-base indicator was used to denote the boundary motion. The velocity of MRB has a relationship with protein concentration, which was used to obtain a standard curve. By paired t-test, there was no significant difference of the protein content between MRBT and Kjeldahl method at 95% confidence interval. The procedure of MRBT method required about 10 min, and it had linearity in the range of 2.0-14.0 g/L, low limit of detection (0.05 g/L), good precision (RSD of intra-day < 1.90% and inter-day < 4.39%), and high recoveries (97.41%-99.91%). In addition, non-protein nitrogen (NPN) such as melamine added into the soya-bean milk had weak influence on MRBT results.

  2. A GC-ECD method for estimation of free and bound amino acids, gamma-aminobutyric acid, salicylic acid, and acetyl salicylic acid from Solanum lycopersicum (L.).

    PubMed

    Meher, Hari Charan; Gajbhiye, Vijay T; Singh, Ghanendra

    2011-01-01

    A gas chromatograph with electron capture detection method for estimation of selected metabolites--amino acids (free and bound), gamma-aminobutyric acid (GABA), salicylic acid (SA), and acetyl salicylic acid (ASA) from tomato--is reported. The method is based on nitrophenylation of the metabolites by 1-fluoro-2, 4-dinitrobenzene under aqueous alkaline conditions to form dinitophenyl derivatives. The derivatives were stable under the operating conditions of GC. Analysis of bound amino acids comprised perchloric acid precipitation of protein, alkylation (carboxymethylation) with iodoacetic acid, vapor-phase hydrolysis, and derivatization with 1-fluoro-2,4-dinitrobenzene in that order. The metabolites were resolved in 35 min, using a temperature-programmed run. The method is rapid, sensitive, and precise. It easily measured the typical amino acids (aspartate, asparagine, glutamate, glutamine, alanine, leucine, lysine, and phenylalanine) used for identification and quantification of a protein, resolved amino acids of the same mass (leucine and isoleucine), satisfactorily measured sulfur amino acid (methionine, cystine, and cysteine), and quantified GABA, SA, and ASA, as well. The developed method was validated for specificity, linearity, and precision. It has been applied and recommended for estimation of 25 metabolites from Solanum lycopersicum (L.).

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

    ERIC Educational Resources Information Center

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

    2012-01-01

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

  4. Potentiometric titration of bisarenechromium compounds with an ion-selective electrode

    SciTech Connect

    Gur'ev, I.A.; Gur'eva, Z.M.; Sankova, E.V.; Sirotkin, N.I.

    1986-06-10

    A liquid-membrane ion-selective electrode was developed for determining bisbenzene-chromium and its electrochemical and analytical characteristics studied. Methods have also been developed for determining bisarenechromium compounds in the industrial product and its waste waters by potentiometric titration with sodium tetraphenylborate solution.

  5. Method for preparing 6-.beta.-halopenicillanic acids

    DOEpatents

    Hansen, Erik I.; Kran-Nielsen, Mogens P.; Von Daehne, Welf

    1989-01-01

    The present invention relates to a new and improved method for the preparation of a compound of the formula I ##STR1## in which R stands for halogen, giving rise to high yields of substantially pure 6.beta.-halopenicillanic acids, obtained in one step.

  6. Predicting proton titration in cationic micelle and bilayer environments

    NASA Astrophysics Data System (ADS)

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

    2014-08-01

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

  7. Predicting proton titration in cationic micelle and bilayer environments

    SciTech Connect

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

    2014-08-28

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

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

    ERIC Educational Resources Information Center

    Belle-Oudry, Deirdre

    2008-01-01

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

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

    ERIC Educational Resources Information Center

    Fulton, Robert; And Others

    1986-01-01

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

  10. pH Static Titration: A Quasistatic Approach

    ERIC Educational Resources Information Center

    Michalowski, Tadeusz; Toporek, Marcin; Rymanowski, Maciej

    2007-01-01

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

  11. An analytical method for the measurement of acid metabolites of tryptophan-NAD pathway and related acids in urine.

    PubMed

    Liao, Xiangjun; Zhu, Jiping; Rubab, Mamoona; Feng, Yong-Lai; Poon, Raymond

    2010-04-15

    An analytical method has been developed for the measurements of five urinary acids namely, quinolinic acid, picolinic acid, nicotinic acid, 2-pyridylacetic acid and 3-pyridylacetic acid. The high performance liquid chromatograph-electrospray ionization mass spectrometry was operated in positive polarity under selected ion monitoring mode, with a column flow rate of 0.2 ml/min and an injection volume of 20 microl. The method used isotope-labelled picolinic acid (PA-d(4)) and nicotinic acid (NA-d(4)) as internal standards for the quantification. The sample preparation involved parallel use of two different types of mixed-mode solid phase extraction cartridges (Strata-X-AW for the extraction of quinolinic acid, and Strata-X-C for the remaining acids). Quantitative analysis of five target acids in several human and rat urine samples showed that the levels of acids were relatively uniform among rats while larger variations were observed for human samples.

  12. A simplified method for estimation of jarosite and acid-forming sulfates in acid mine wastes.

    PubMed

    Li, Jun; Smart, Roger St C; Schumann, Russell C; Gerson, Andrea R; Levay, George

    2007-02-01

    In acid base accounting (ABA) estimates of acid mine wastes, the acid potential (AP) estimate can be improved by using the net carbonate value (NCV) reactive sulfide S method rather than total S assay methods but this does not give recovery of potentially acid producing ferrous and ferric sulfates present in many wastes. For more accurate estimation of AP, an effective, site-specific method to quantify acid sulfate salts, such as jarosite and melanterite, in waste rocks has been developed and tested on synthetic and real wastes. The SPOCAS (acid sulfate soils) methods have been modified to an effective, rapid method to speciate sulfate forms in different synthetic waste samples. A three-step sequential extraction procedure has been established. These steps are: (1) argon-purged water extraction (3 min) to extract soluble Fe(II) salts (particularly melanterite), epsomite and gypsum (<10 wt.%), (2) roasting at 550 degrees C (1 h) to remove sulfur from pyrite and other reactive sulfides, (3) HCl extraction (4 M, 30 min) for determination of jarosites. Products (solid and aqueous) have been characterized at each step including the jarosite decomposition process in Step 2 where temperature control is critical to avoid S loss. The sequential extraction procedure was used to quantitatively determine melanterite, epsomite, gypsum, pyrite and jarosite concentrations in a synthetic waste sample containing these mineral phases at 5 wt.% in quartz, and also tested using a tailings waste sample to quantitatively determine epsomite, gypsum and jarosite contents. The method is applicable to most waste samples including those with non-pyrite sulfides but for samples containing significant amounts of sulfur (>1 wt.% S) as copper sulfides, the second step of roasting needs to be excluded from the procedure with an increased time of 4 M HCl extraction to 16 h for jarosite determination.

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

    PubMed

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

    2002-02-01

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

  14. Zinc sorption to three gram-negative bacteria: combined titration, modeling, and EXAFS study.

    PubMed

    Guiné, V; Spadini, L; Sarret, G; Muris, M; Delolme, C; Gaudet, J P; Martins, J M F

    2006-03-15

    The acid-base and Zn sorption properties of three bacteria, Cupriavidus metallidurans CH34, Pseudomonas putida ATCC12633, and Escherichia coli K12DH5alpha, were investigated through an original combination of extended X-ray absorption fine structure (EXAFS) spectroscopy and equilibrium titration studies. Acid-base titration curves of the three strains were fitted with a model accounting for three conceptual reactive sites: an acidic (carboxyl and/or phosphodiester), a neutral (phosphomonoester), and a basic (amine and/or hydroxyl) group. Calculated proton and Zn equilibrium constants and site densities compare with literature data. The nature of Zn binding sites was studied by EXAFS spectroscopy. Phosphoester, carboxyl, and unexpectedly sulfhydryl ligands were identified. Their proportions depended on Zn loading and bacterial strain and were consistent with the titration results. These findings were compared to the structure and site density of the major cell wall components. It appeared that the cumulated theoretical site density of these structures (<2 Zn nm(-2)) was much lower than the total site density of the investigated strains (16-56 Zn nm(-2)). These results suggest a dominant role of extracellular polymeric substances in Zn retention processes, although Zn binding to inner cell components cannot be excluded.

  15. Hydrogen-ion titration studies on erythrocyte membranes.

    PubMed Central

    Hallam, C; Wrigglesworth, J M

    1976-01-01

    1. H+ titration was used to detect the presence of ionizable groups on human erythrocyte plasma membranes. Between pH2.9 and 11.3, two significant peaks of H+ association/dissociation occur in the differential from of the titration curve, one at pH3. 1. And the other at pH10.3. 2. After disruption of membrane structure by exposure to high pH or by the addition of sodium dodecyl sulphate, maxima of H+ association/dissociation were seen at pH3.1,4.3,6.5,10.3 and 10.7. 3. Spectrophotometric assay and selective chemical treatments were used to identify several of the titratable residues. 4. The degree of eleectrostatic interaction between titratable charged groups was investigated by comparing the titration characteristics of the membranes before and after modification of membrane structure. PMID:8038

  16. Determination of L- Ascorbic Acid in Plasma by Voltammetric Method

    PubMed Central

    Behfar, Abdol Azim; Sadeghi, Nafiseh; Jannat, Behrooz; Oveisi, Mohammad Reza

    2010-01-01

    Voltammetric techniques have been considered as important methods among the analytical techniques used for the identification and determination of trace concentrations of many biological molecules such as L-ascorbic acid (AA). L-ascorbic acid is an electro-active molecule, though it is difficult to determine its value directly with a majority of electrodes made of carbon and transition metals, because of electrode surface problems. The present study is based on I-E curves for AA analysis at various pH. Furthermore, the effects of the presence of other electro-active substances; such as copper, as well as the effect of the sweep rate of potential will be studied. The present study is based on analysis of the current-voltage curves for L-ascorbic acid at varying pH and sweep rate scan values. An analysis was also carried out to measure the influence of the concentration of some electro active species. The peak height of the first oxidation wave is used for L-ascorbic acid assay. L-ascorbic acid was determined in aqueous media by linear-scan voltammetry on a gold electrode; ranging between (1-175 μg/mL). In biologic samples, for elimination of uric acid or some sugars and effects, a significant interference of copper ions whose presence reduces the height of the L-ascorbic acid oxidation peak was used. The optimum pH and sweep rate were 3.2 and 7500mV/s, respectively. Under these conditions, the detection limit of the method was 0.3 μg/mL. Repeatability of the method based on relative standard deviation (RSD) 50, 10 and 1 μg/mL concentrations was 0.83, 2.1 and 10.3%, respectively. The calibration curve was linear over the range 1-175μg/mL (r2 = 0.9977, p < 0.001). The advantage of this method lies in the fact that the use of copper eliminates the interference of different substances such as uric acid. PMID:24363717

  17. Method comparison study for weak acid dissociation cyanide analysis.

    PubMed

    Evans, Joseph D; Thompson, Leslie; Clark, Patrick J; Beckman, Scott W

    2003-02-01

    Method comparison studies of two different methods for the analysis of weak acid dissociable (WAD) cyanide revealed analytical flaws and/or matrix interference problems with both procedures. EPA "draft" method 1677 using a Perstorp 3202 CN analyzer was compared to Standard Method 4500 CN I. It was discovered that the Perstorp analyzer produced more precise and more accurate results once appropriate and necessary procedural steps from the EPA draft method were modified. Comparison of these two methods, was based on "real world" samples collected from a mine-tailing solution. The mine-tailing solution contained high concentrations of cyanide and metals. Inconsistencies in method procedures were traced to sulfide interferences and high concentrations of WAD metals. Conclusions were based upon a large sample base collected from a mine site over a 90-day period.

  18. Acid pre-treatment method for in situ ore leaching

    DOEpatents

    Mallon, R.G.; Braun, R.L.

    1975-10-28

    An acid leaching method is described for the recovery of a desired element from a subterranean rubblized body of primary ore containing the element and also having associated therewith a carbonate mineral wherein the rubblized ore body is flooded with an aqueous acidic solution in order to release carbon dioxide from the associated carbonate mineral. After a substantial portion of the available carbon dioxide is released and removed from the ore body, as by venting to the atmosphere, an oxidizing gas is introduced into the flooded, rubblized ore to oxidize the ore and form an acid leach solution effective in the presence of the dissolved oxidizing gas to dissolve the ore and cause the desired element to go into solution. The leach solution is then circulated to the surface where the metal values are recovered therefrom.

  19. Titration and hysteresis in epigenetic chromatin silencing

    NASA Astrophysics Data System (ADS)

    Dayarian, Adel; Sengupta, Anirvan M.

    2013-06-01

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

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

    NASA Technical Reports Server (NTRS)

    Demore, W. B.; Patapoff, M.

    1976-01-01

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

  1. Method for liquid chromatographic extraction of strontium from acid solutions

    DOEpatents

    Horwitz, E. Philip; Dietz, Mark L.

    1992-01-01

    A method and apparatus for extracting strontium and technetium values from biological, industrial and environmental sample solutions using a chromatographic column is described. An extractant medium for the column is prepared by generating a solution of a diluent containing a Crown ether and dispersing the solution on a resin substrate material. The sample solution is highly acidic and is introduced directed to the chromatographic column and strontium or technetium is eluted using deionized water.

  2. Method and apparatus for staining immobilized nucleic acids

    DOEpatents

    Ramsey, J. Michael; Foote, Robert S.; Jacobson, Stephen C.

    2000-01-01

    A method for staining immobilized nucleic acids includes the steps of affixing DNA probes to a solid substrate, moving target DNA material into proximity with the DNA probes, whereby the target DNA hybridized with specific ones of the DNA probes, and moving a fluorescent dye into proximity with the hybridized target DNA, whereby the fluorescent dye binds to the hybridized DNA to enable subsequent detection of fluorescence.

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

    PubMed

    Zhai, Jingying; Xie, Xiaojiang; Bakker, Eric

    2015-12-15

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

  4. Properties of nanocellulose isolated from corncob residue using sulfuric acid, formic acid, oxidative and mechanical methods.

    PubMed

    Liu, Chao; Li, Bin; Du, Haishun; Lv, Dong; Zhang, Yuedong; Yu, Guang; Mu, Xindong; Peng, Hui

    2016-10-20

    In this work, nanocellulose was extracted from bleached corncob residue (CCR), an underutilized lignocellulose waste from furfural industry, using four different methods (i.e. sulfuric acid hydrolysis, formic acid (FA) hydrolysis, 2,2,6,6-tetramethylpiperidine-1-oxyl (TEMPO)-mediated oxidation, and pulp refining, respectively). The self-assembled structure, morphology, dimension, crystallinity, chemical structure and thermal stability of prepared nanocellulose were investigated. FA hydrolysis produced longer cellulose nanocrystals (CNCs) than the one obtained by sulfuric acid hydrolysis, and resulted in high crystallinity and thermal stability due to its preferential degradation of amorphous cellulose and lignin. The cellulose nanofibrils (CNFs) with fine and individualized structure could be isolated by TEMPO-mediated oxidation. In comparison with other nanocellulose products, the intensive pulp refining led to the CNFs with the longest length and the thickest diameter. This comparative study can help to provide an insight into the utilization of CCR as a potential source for nanocellulose production.

  5. A New Indirect Spectrofluorimetric Method for Determination of Ascorbic Acid with 2,4,6-Tripyridyl-S-Triazine in Pharmaceutical Samples.

    PubMed

    Klepo, Lejla; Copra-Janicijevic, Amira; Kukoc-Modun, Lea

    2016-01-19

    Ascorbic acid (AA) is a water-soluble vitamin which shows no fluorescence. However, in reaction with iron(III), AA is oxidised to dehydroascorbic acid and iron(III) is reduced to iron(II) which forms a complex with 2,4,6-tripyridyl-S-triazine (TPTZ) in buffered medium. The relative fluorescence intensity of the resulting Fe(TPTZ)₂(2+) complex can be measured at excitation and emission wavelengths of 393 and 790 nm, respectively. Based on this data, a new indirect spectrofluorimetric method for the determination of AA in pharmaceutical samples was proposed. Influence of the reaction conditions, such as acidity of acetic buffer, concentration of TPTZ and iron(III), reaction time and instrumental parameters were investigated in detail. The linear range was from 5.4 × 10(-4) to 5.4 × 10(-6) mol·L(-1) (R = 0.9971). The LOD was 7.7 × 10(-7) mol·L(-1) and LOQ was 2.3 × 10(-4) mol·L(-1). Fourteen pharmaceutical samples containing various amounts of AA were analysed. Influences of potential interfering substances were also examined. Analysis of commercial pharmaceutical formulations showed good correlation with the nominal values given by the manufacturers and with the results obtained by a titration method. The proposed method can be applied in routine quality control in the pharmaceutical industry due to its sensitivity, simplicity, selectivity and low cost.

  6. Mycolic Acid Index Susceptibility Method for Mycobacterium tuberculosis

    PubMed Central

    Viader-Salvadó, José M.; Garza-González, Elvira; Valdez-Leal, Ramón; de los Angeles del Bosque-Moncayo, M.; Tijerina-Menchaca, Rolando; Guerrero-Olazarán, Martha

    2001-01-01

    A rapid drug susceptibility test to measure the susceptibility of Mycobacterium tuberculosis to isoniazid (INH) and rifampin (RIF) using clinical isolates and a newly defined mycolic acid index (MAI) was evaluated. A total of 200 clinical isolates of M. tuberculosis were tested for susceptibility or resistance to INH and RIF by the MAI susceptibility and indirect-proportion methods. Overall, there was agreement between the two methods for 398 (99.5%) of the 400 total tests. Specifically, the sensitivity of the MAI susceptibility method for INH and RIF was 97.6 and 100%, respectively. The specificity and positive predictive value were 100% for both drugs, and the negative predictive value for INH and RIF was 98.3 and 100%, respectively. In conclusion, the MAI susceptibility method described here can be used for rapid drug susceptibility testing of M. tuberculosis clinical isolates within 5 days after clinical isolates are incubated in the presence or absence of an antituberculosis drug. PMID:11427584

  7. A microarray-based method to perform nucleic acid selections.

    PubMed

    Aminova, Olga; Disney, Matthew D

    2010-01-01

    This method describes a microarray-based platform to perform nucleic acid selections. Chemical ligands to which a nucleic acid binder is desired are immobilized onto an agarose microarray surface; the array is then incubated with an RNA library. Bound RNA library members are harvested directly from the array surface via gel excision at the position on the array where a ligand was immobilized. The RNA is then amplified via RT-PCR, cloned, and sequenced. This method has the following advantages over traditional resin-based Systematic Evolution of Ligands by Exponential Enrichment (SELEX): (1) multiple selections can be completed in parallel on a single microarray surface; (2) kinetic biases in the selections are mitigated since all RNA binders are harvested from an array via gel excision; (3) the amount of chemical ligand needed to perform a selection is minimized; (4) selections do not require expensive resins or equipment; and (5) the matrix used for selections is inexpensive and easy to prepare. Although this protocol was demonstrated for RNA selections, it should be applicable for any nucleic acid selection.

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

    USGS Publications Warehouse

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

    1957-01-01

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

  9. Hydroxyapatite-phosphonoformic acid hybrid compounds prepared by hydrothermal method

    NASA Astrophysics Data System (ADS)

    Turki, Thouraya; Othmani, Masseoud; Bantignies, Jean-Louis; Bouzouita, Khaled

    2014-01-01

    Hydroxyapatites were prepared in the presence of different amounts of phosphonoformic acid (PFA) via the hydrothermal method. The obtained powders were characterized through chemical analysis, XRD, IR, 31P MAS-NMR, TEM, and TG-TDA. The XRD showed that the PFA did not affect the apatite composition. Indeed, only a reduction of the crystallite size was noted. After grafting of PFA, the IR spectroscopy revealed the appearance of new bands belonging to HPO42- and carboxylate groups of the apatite and organic moiety, respectively. Moreover, the 31P MAS-NMR spectra exhibited a peak with a low intensity assigned to the terminal phosphonate group of the organic moiety in addition to that of the apatite. Based on these results, a reaction mechanism involving the surface hydroxyl groups (tbnd Casbnd OH) of the apatite and the carboxyl group of the acid was proposed.

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

    ERIC Educational Resources Information Center

    Hodder, A. P. W.

    1983-01-01

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

  11. Microscope Titration and Extraction of DNA from Liver.

    ERIC Educational Resources Information Center

    Mayo, Lois T.; And Others

    1993-01-01

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

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

    PubMed

    Mazzei, Luca; Ciurli, Stefano; Zambelli, Barbara

    2014-04-04

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

  13. Method for the isolation of citric acid and malic acid in Japanese apricot liqueur for carbon stable isotope analysis.

    PubMed

    Akamatsu, Fumikazu; Hashiguchi, Tomokazu; Hisatsune, Yuri; Oe, Takaaki; Kawao, Takafumi; Fujii, Tsutomu

    2017-02-15

    A method for detecting the undeclared addition of acidic ingredients is required to control the authenticity of Japanese apricot liqueur. We developed an analytical procedure that minimizes carbon isotope discrimination for measurement of the δ(13)C values of citric and malic acid isolated from Japanese apricot liqueur. Our results demonstrated that freeze-drying is preferable to nitrogen spray-drying, because it does not significantly affect the δ(13)C values of citric acid and results in smaller isotope discrimination for malic acid. Both 0.1% formic acid and 0.2% phosphoric acid are acceptable HPLC mobile phases for the isolation of citric and malic acid, although the δ(13)C values of malic acid exhibited relatively large variation compared with citric acid following isolation using either mobile phase. The developed procedure allows precise δ(13)C measurements of citric and malic acid isolated from Japanese apricot liqueur.

  14. Exact analysis of competition ligand binding by displacement isothermal titration calorimetry.

    PubMed

    Sigurskjold, B W

    2000-01-15

    A rigorous method for the least-squares nonlinear regression analysis of displacement isothermal titration calorimetric data is presented. The method can fit the binding isotherm of a ligand which is competitively inhibited in its binding by another bound ligand to a molecule with n identical and independent binding sites. There are no other assumptions for the method and no approximations. Analysis of previously published data of the strong binding of acarbose to glucoamylase is presented as an example. The regression equations have been programmed for the Origin software supplied with the widely used titration calorimeters from Microcal, Inc., and an Origin Function Definition File with instructions is freely available from the author upon e-mail request.

  15. Simple quantification of surface carboxylic acids on chemically oxidized multi-walled carbon nanotubes

    NASA Astrophysics Data System (ADS)

    Gong, Hyejin; Kim, Seong-Taek; Lee, Jong Doo; Yim, Sanggyu

    2013-02-01

    The surface of multi-walled carbon nanotube (MWCNT) was chemically oxidized using nitric acid and sulfuric-nitric acid mixtures. Thermogravimetric analysis, transmission electron microscopy and infrared spectroscopy revealed that the use of acid mixtures led to higher degree of oxidation. More quantitative identification of surface carboxylic acids was carried out using X-ray photoelectron spectroscopy (XPS) and acid-base titration. However, these techniques are costly and require very long analysis times to promptly respond to the extent of the reaction. We propose a much simpler method using pH measurements and pre-determined pKa value in order to estimate the concentration of carboxylic acids on the oxidized MWCNT surfaces. The results from this technique were consistent with those obtained from XPS and titration, and it is expected that this simple quantification method can provide a cheap and fast way to monitor and control the oxidation reaction of MWCNT.

  16. Enzyme kinetics determined by single-injection isothermal titration calorimetry.

    PubMed

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

    2015-04-01

    The purposes of this paper are (a) to examine the effect of calorimeter time constant (τ) on heat rate data from a single enzyme injection into substrate in an isothermal titration calorimeter (ITC), (b) to provide information that can be used to predict the optimum experimental conditions for determining the rate constant (k2), Michaelis constant (KM), and enthalpy change of the reaction (ΔRH), and (c) to describe methods for evaluating these parameters. We find that KM, k2 and ΔRH can be accurately estimated without correcting for the calorimeter time constant, τ, if (k2E/KM), where E is the total active enzyme concentration, is between 0.1/τ and 1/τ and the reaction goes to at least 99% completion. If experimental conditions are outside this domain and no correction is made for τ, errors in the inferred parameters quickly become unreasonable. A method for fitting single-injection data to the Michaelis-Menten or Briggs-Haldane model to simultaneously evaluate KM, k2, ΔRH, and τ is described and validated with experimental data. All four of these parameters can be accurately inferred provided the reaction time constant (k2E/KM) is larger than 1/τ and the data include enzyme saturated conditions.

  17. Rational Catalyst Design of Titanium-Silica Materials Aided by Site-Specific Titration Tools

    NASA Astrophysics Data System (ADS)

    Eaton, Todd Robert

    Silica-supported titanium materials are widely used for thermocatalytic applications such as hydroxylation of alkanes and aromatics, oxidation of alcohols and ethers, ammoximation of carbonyls, and sulfoxidations, while Ti-based materials are widely studied for photocatalytic applications such as photo-oxidation of organic substrates and photo-reduction of CO 2. However, the underlying phenomena of how to synthesize, identify, and control the active structures in these materials is not well understood because of the narrow scope of previous work. Studies of titanium-based catalysts typically focus on materials where the metal is present as either highly-dispersed Ti cations or in bulk crystalline TiO2 form, neglecting the numerous and potentially useful intermediate structures. Furthermore, these works typically focus on a single synthesis technique and rely upon bulk characterization techniques to understand the materials. Here rigorous titanium-silica synthesis-structure-function relationships are established by examining several different synthetic method and utilizing characterization techniques that enable an atomic-level understanding of the materials. The materials studied span the range from isolated Ti cations to clustered TiOx domains, polymeric TiO x domains, anatase-like 2D TiO2 domains, and 3D crystalline TiO2. Tools to quantify accessible TiO x and tetrahedral Ti sites are developed, utilizing the selective titration of titanium with phenylphosphonic acid (PPA). Catalytic properties are probed with the photocatalytic oxidation of benzyl alcohol and the thermocatalytic epoxidation of cis-cyclooctene with H2O2 . PPA titration data indicate that the rate of benzyl alcohol photo-oxidation is independent of titanium coordination, while the rate of alkene epoxidation with H2O2 is proportional to the number of tetrahedral titanium sites on the catalyst. PPA titration data also enables the estimation of TiO2 particle size and reveals an important distinction

  18. Cholinium-amino acid based ionic liquids: a new method of synthesis and physico-chemical characterization.

    PubMed

    De Santis, Serena; Masci, Giancarlo; Casciotta, Francesco; Caminiti, Ruggero; Scarpellini, Eleonora; Campetella, Marco; Gontrani, Lorenzo

    2015-08-28

    In the present work we report the synthesis and physico-chemical characterization in terms of the viscosity and density of a wide series of cholinium-amino acid based room temperature ionic liquids ([Ch][AA] RTILs). 18 different amino acids were used to obtain 14 room temperature ILs. Among the most common AAs, only valine did not form an RTIL but it is a liquid above 80 °C. With respect to the methods reported in the literature we propose a synthesis based on potentiometric titration which has several advantages such as shorter preparation time, stoichiometry within ±1%, very high yields (close to 100%), high reproducibility, and no use of organic solvents, thus being more environmentally friendly. We tried to prepare dianionic ILs with some AAs with two potentially ionisable groups but in all cases the salts were solids at room temperature. All the ILs were characterized by (1)H NMR to confirm the stoichiometry. Physico-chemical properties such as density, viscosity, refractive index and conductivity were measured as a function of temperature and correlated with empirical equations. The values were compared with the data already reported in the literature for some [Ch][AA] ILs. The thermal expansion coefficient αp and the molar volume Vm were also calculated from the experimental density values. Due to the high number of AAs explored and their structural heterogeneity we have been able to find some interesting correlations between the data obtained and the structural features of the AAs in terms of the alkyl chain length, hydrogen bonding ability, stacking and cyclization. Some parameters were also found to be in good agreement with those reported for other ILs. We think that these data can give an important contribution to the understanding of the structure-property relationship of ILs because they focused on the structural effect of the anions, while most data in the literature are focussed on the cations.

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

    PubMed

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

    2006-11-15

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

  20. Simple method of isolating humic acids from organic soils

    NASA Astrophysics Data System (ADS)

    Ahmed, O.

    2009-04-01

    Humic substances particularly humic acids (HA) play a major role in soil conditioning e.g. erosion control, soil cation exchange capacity, complexation of heavy metal ions and pesticides, carbon and nitrogen cycles, plant growth and reduction of ammonia volatilization from urea. Humified substances such as coal, composts, and peat soils have substantial amounts of HA but the isolation of these acids is expensive, laborious, and time consuming. Factors that affect the quality and yield of HA isolated from these materials include extraction, fractionation, and purification periods. This work developed a simple, rapid, and cost effective method of isolating HA from peat soils. There was a quadratic relationship between extraction period and HA yield. Optimum extraction period was estimated at 4 h instead of the usual range of 12 to 48 h. There was no relationship between fractionation period and HA yield. As such 2 h instead of the usual range of 12 to 24 h fractionation period could be considered optimum. Low ash content (5%), remarkable reduction in K, coupled with the fact that organic C, E4/E6, carboxylic COOH, phenolic OH, and total acidity values of the HA were consistent with those reported by other authors suggest that the HA dealt with were free from mineral matter. This was possible because the distilled water used to purify the HA served as Bronsted-Lowry acid during the purification process of the HA. Optimum purification period using distilled waster was 1 h instead of the usual range of 1 and 7 days (uses HF and HCl and dialysis). Humic acids could be isolated from tropical peat soils within 7 h (i.e. 4 h extraction, 2 h fractionation, and 1 h purification) instead of the existing period of 2 and 7 days. This could facilitate the idea of producing organic fertilizers such as ammonium-humate and potassium-humate from humified substances since techniques devised in this study did not alter the true nature of the HA. Besides, the technique is rapid, simple

  1. Method for production of petroselinic acid and OMEGA12 hexadecanoic acid in transgenic plants

    DOEpatents

    Ohlrogge, John B.; Cahoon, Edgar B.; Shanklin, John; Somerville, Christopher R.

    1995-01-01

    The present invention relates to a process for producing lipids containing the fatty acid petroselinic acid in plants. The production of petroselinic acid is accomplished by genetically transforming plants which do not normally accumulate petroselinic acid with a gene for a .omega.12 desaturase from another species which does normally accumulate petroselinic acid.

  2. Method for production of petroselinic acid and OMEGA12 hexadecanoic acid in transgenic plants

    DOEpatents

    Ohlrogge, J.B.; Cahoon, E.B.; Shanklin, J.; Somerville, C.R.

    1995-07-04

    The present invention relates to a process for producing lipids containing the fatty acid, petroselinic acid, in plants. The production of petroselinic acid is accomplished by genetically transforming plants which do not normally accumulate petroselinic acid with a gene for a {omega}12 desaturase from another species which does normally accumulate petroselinic acid. 19 figs.

  3. Method of Identifying a Base in a Nucleic Acid

    DOEpatents

    Fodor, Stephen P. A.; Lipshutz, Robert J.; Huang, Xiaohua

    1999-01-01

    Devices and techniques for hybridization of nucleic acids and for determining the sequence of nucleic acids. Arrays of nucleic acids are formed by techniques, preferably high resolution, light-directed techniques. Positions of hybridization of a target nucleic acid are determined by, e.g., epifluorescence microscopy. Devices and techniques are proposed to determine the sequence of a target nucleic acid more efficiently and more quickly through such synthesis and detection techniques.

  4. Physical methods of nucleic acid transfer: general concepts and applications

    PubMed Central

    Villemejane, Julien; Mir, Lluis M

    2009-01-01

    Physical methods of gene (and/or drug) transfer need to combine two effects to deliver the therapeutic material into cells. The physical methods must induce reversible alterations in the plasma membrane to allow the direct passage of the molecules of interest into the cell cytosol. They must also bring the nucleic acids in contact with the permeabilized plasma membrane or facilitate access to the inside of the cell. These two effects can be achieved in one or more steps, depending upon the methods employed. In this review, we describe and compare several physical methods: biolistics, jet injection, hydrodynamic injection, ultrasound, magnetic field and electric pulse mediated gene transfer. We describe the physical mechanisms underlying these approaches and discuss the advantages and limitations of each approach as well as its potential application in research or in preclinical and clinical trials. We also provide conclusions, comparisons, and projections for future developments. While some of these methods are already in use in man, some are still under development or are used only within clinical trials for gene transfer. The possibilities offered by these methods are, however, not restricted to the transfer of genes and the complementary uses of these technologies are also discussed. As these methods of gene transfer may bypass some of the side effects linked to viral or biochemical approaches, they may find their place in specific clinical applications in the future. This article is part of a themed section on Vector Design and Drug Delivery. For a list of all articles in this section see the end of this paper, or visit: http://www3.interscience.wiley.com/journal/121548564/issueyear?year=2009 PMID:19154421

  5. Conductometric simultaneous determination of acetic acid, monochloroacetic acid and trichloroacetic acid using orthogonal signal correction-partial least squares.

    PubMed

    Ghorbani, R; Ghasemi, J; Abdollahi, B

    2006-04-17

    A simultaneous conductometric titration method for determination of mixtures of acetic acid, monochloroacetic acid and trichloroacetic acid based on the multivariate calibration partial least squares is proposed. It is possible to obtain an adjustable model to relate squared concentration values of the mixtures used in the calibration range by conductance. The effect of orthogonal signal correction (OSC) as a preprocessing technique used to remove the information unrelated to the target variables is studied. The calibration model was build using conductometric titrations data of 16 mixtures of three acids. The concentration matrix was designed by a orthogonal design. The root mean squares error of prediction (RMSEP) for acetic acid, monochloroacetic acid and trichloroacetic acid with and without OSC were 0.08, 0.30 and 0.08, and 0.15, 0.40 and 0.18, respectively. The results obtained by OSC-PLS are better than the PLS and this indicate the successful application of the OSC filter as a good preprocessing method in multivariate calibration methods. The proposed procedure allows the simultaneous determination of these acids, in the synthetic mixtures.

  6. Determination of the catalytic activity of binuclear metallohydrolases using isothermal titration calorimetry.

    PubMed

    Pedroso, Marcelo M; Ely, Fernanda; Lonhienne, Thierry; Gahan, Lawrence R; Ollis, David L; Guddat, Luke W; Schenk, Gerhard

    2014-03-01

    Binuclear metallohydrolases are a large and diverse family of enzymes that are involved in numerous metabolic functions. An increasing number of members find applications as drug targets or in processes such as bioremediation. It is thus essential to have an assay available that allows the rapid and reliable determination of relevant catalytic parameters (k cat, K m, and k cat/K m). Continuous spectroscopic assays are frequently only possible by using synthetic (i.e., nonbiological) substrates that possess a suitable chromophoric marker (e.g., nitrophenol). Isothermal titration calorimetry, in contrast, affords a rapid assay independent of the chromophoric properties of the substrate-the heat associated with the hydrolytic reaction can be directly related to catalytic properties. Here, we demonstrate the efficiency of the method on several selected examples of this family of enzymes and show that, in general, the catalytic parameters obtained by isothermal titration calorimetry are in good agreement with those obtained from spectroscopic assays.

  7. Method for producing labeled single-stranded nucleic acid probes

    DOEpatents

    Dunn, John J.; Quesada, Mark A.; Randesi, Matthew

    1999-10-19

    Disclosed is a method for the introduction of unidirectional deletions in a cloned DNA segment. More specifically, the method comprises providing a recombinant DNA construct comprising a DNA segment of interest inserted in a cloning vector, the cloning vector having an f1 endonuclease recognition sequence adjacent to the insertion site of the DNA segment of interest. The recombinant DNA construct is then contacted with the protein pII encoded by gene II of phage f1 thereby generating a single-stranded nick. The nicked DNA is then contacted with E. coli Exonuclease III thereby expanding the single-stranded nick into a single-stranded gap. The single-stranded gapped DNA is then contacted with a single-strand-specific endonuclease thereby producing a linearized DNA molecule containing a double-stranded deletion corresponding in size to the single-stranded gap. The DNA treated in this manner is then incubated with DNA ligase under conditions appropriate for ligation. Also disclosed is a method for producing single-stranded DNA probes. In this embodiment, single-stranded gapped DNA, produced as described above, is contacted with a DNA polymerase in the presence of labeled nucleotides to fill in the gap. This DNA is then linearized by digestion with a restriction enzyme which cuts outside the DNA segment of interest. The product of this digestion is then denatured to produce a labeled single-stranded nucleic acid probe.

  8. Compositions and method for controlling precipitation when acidizing sour wells

    SciTech Connect

    Dill, W.R.; Walker, M.L.

    1989-12-19

    This patent describes an acidizing composition for treating a sour well. It comprises: a base acid solution having an initial ph below 1.9; an iron sequestering agent to combine with iron present in the solution comprising at least one compound selected from the group consisting of aminopolycarboxylic acids, hydroxycarboxylic acids, cyclic polyethers and derivatives of the acids and ethers present in an amount of from about 0.25 to about 5 percent by weight of the acid solution; and a sulfide modifier to combine with sulfides present in the solution comprising at least one member selected from the group consisting of an aldehyde, acetal, hemiacetal and any other compound capable of forming an aldehyde in solution, present in an amount of from about 1 to about 4 percent by weight of the acid solution, whereby precipitation of ferric hydroxide, ferrous sulfide and elemental sulfur is inhibited as acid spending occurs.

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

    PubMed

    You, T J; Bashford, D

    1995-11-01

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

  10. Quantitative RT-PCR for titration of replication-defective recombinant Semliki Forest virus.

    PubMed

    Puglia, Ana L P; Rezende, Alexandre G; Jorge, Soraia A C; Wagner, Renaud; Pereira, Carlos A; Astray, Renato M

    2013-11-01

    Virus titration may constitute a drawback in the development and use of replication-defective viral vectors like Semliki Forest virus (SFV). The standardization and validation of a reverse transcription quantitative PCR (qRT-PCR) method for SFV titration is presented here. The qRT-PCR target is located within the nsp1 gene of the non-structural polyprotein SFV region (SFV RNA), which allows the strategy to be used for several different recombinant SFV constructs. Titer determinations were carried out by performing virus titration and infection assays with SFVs containing an RNA coding region for the rabies virus glycoprotein (RVGP) or green fluorescent protein (GFP). Results showed that the standardized qRT-PCR is applicable for different SFV constructs, and showed good reproducibility. To evaluate the correlation between the amount of functional SFV RNA in a virus lot and its infectivity in BHK-21 cell cultures, a temperature mediated titer decrease was performed and successfully quantitated by qRT-PCR. When used for cell infection at the same multiplicity of infection (MOI), the temperature treated SFV-RVGP samples induced the same levels of RVGP expression. Similarly, when different SFV-GFP lots with different virus titers, as accessed by qRT-PCR, were used for cell infection at the same MOI, the cultures showed comparable amounts of fluorescent cells. The data demonstrate a good correlation between the amount of virus used for infection, as measured by its SFV RNA, and the protein synthesis in the cells. In conclusion, the qRT-PCR method developed here is accurate and enables the titration of replication-defective SFV vectors, an essential aid for viral vector development as well as for establishment of production bioprocesses.

  11. In situ synthesis carbonated hydroxyapatite layers on enamel slices with acidic amino acids by a novel two-step method.

    PubMed

    Wu, Xiaoguang; Zhao, Xu; Li, Yi; Yang, Tao; Yan, Xiujuan; Wang, Ke

    2015-09-01

    In situ fabrication of carbonated hydroxyapatite (CHA) remineralization layer on an enamel slice was completed in a novel, biomimetic two-step method. First, a CaCO3 layer was synthesized on the surface of demineralized enamel using an acidic amino acid (aspartic acid or glutamate acid) as a soft template. Second, at the same concentration of the acidic amino acid, rod-like carbonated hydroxyapatite was produced with the CaCO3 layer as a sacrificial template and a reactant. The morphology, crystallinity and other physicochemical properties of the crystals were characterized using field emission scanning electron microscopy (FESEM), Fourier transform infrared spectrometry (FTIR), X-ray diffraction (XRD) and energy-dispersive X-ray analysis (EDAX), respectively. Acidic amino acid could promote the uniform deposition of hydroxyapatite with rod-like crystals via absorption of phosphate and carbonate ions from the reaction solution. Moreover, compared with hydroxyapatite crystals coated on the enamel when synthesized by a one-step method, the CaCO3 coating that was synthesized in the first step acted as an active bridge layer and sacrificial template. It played a vital role in orienting the artificial coating layer through the template effect. The results show that the rod-like carbonated hydroxyapatite crystals grow into bundles, which are similar in size and appearance to prisms in human enamel, when using the two-step method with either aspartic acid or acidic glutamate (20.00 mmol/L).

  12. AMDTreat 5.0+ with PHREEQC titration module to compute caustic chemical quantity, effluent quality, and sludge volume

    USGS Publications Warehouse

    Cravotta, Charles A.; Means, Brent P; Arthur, Willam; McKenzie, Robert M; Parkhurst, David L.

    2015-01-01

    Alkaline chemicals are commonly added to discharges from coal mines to increase pH and decrease concentrations of acidity and dissolved aluminum, iron, manganese, and associated metals. The annual cost of chemical treatment depends on the type and quantities of chemicals added and sludge produced. The AMDTreat computer program, initially developed in 2003, is widely used to compute such costs on the basis of the user-specified flow rate and water quality data for the untreated AMD. Although AMDTreat can use results of empirical titration of net-acidic or net-alkaline effluent with caustic chemicals to accurately estimate costs for treatment, such empirical data are rarely available. A titration simulation module using the geochemical program PHREEQC has been incorporated with AMDTreat 5.0+ to improve the capability of AMDTreat to estimate: (1) the quantity and cost of caustic chemicals to attain a target pH, (2) the chemical composition of the treated effluent, and (3) the volume of sludge produced by the treatment. The simulated titration results for selected caustic chemicals (NaOH, CaO, Ca(OH)2, Na2CO3, or NH3) without aeration or with pre-aeration can be compared with or used in place of empirical titration data to estimate chemical quantities, treated effluent composition, sludge volume (precipitated metals plus unreacted chemical), and associated treatment costs. This paper describes the development, evaluation, and potential utilization of the PHREEQC titration module with the new AMDTreat 5.0+ computer program available at http://www.amd.osmre.gov/.

  13. 40 CFR Appendix A to Subpart Ddd... - Free Formaldehyde Analysis of Insulation Resins by the Hydroxylamine Hydrochloride Method

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... this method is the titration of the hydrochloric acid that is liberated when hydroxylamine... prestandardized pH meter, 1.0 N hydrochloric acid, 0.1 N hydrochloric acid, and 0.1 N sodium hydroxide. 5.5Add 50... adjusted to 4.00. 4.3Hydrochloric acid solution, 1.0 N and 0.1 N. 4.4Sodium hydroxide solution, 0.1 N....

  14. 40 CFR Appendix A to Subpart Ddd... - Free Formaldehyde Analysis of Insulation Resins by the Hydroxylamine Hydrochloride Method

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... this method is the titration of the hydrochloric acid that is liberated when hydroxylamine... prestandardized pH meter, 1.0 N hydrochloric acid, 0.1 N hydrochloric acid, and 0.1 N sodium hydroxide. 5.5Add 50... adjusted to 4.00. 4.3Hydrochloric acid solution, 1.0 N and 0.1 N. 4.4Sodium hydroxide solution, 0.1 N....

  15. Method of preparing and using and composition for acidizing subterranean formations

    SciTech Connect

    Dill, W.R.

    1984-08-21

    A composition and method of acidizing or fracturing a subterranean formation comprises contacting the formation with a composition comprising an acid, urea, and a selected gelling agent. The urea is present in an amount sufficient to extend the viscous stability of the gelled acid composition in comparison to the acid and gelling agent alone.

  16. HPLC method for the simultaneous quantification of the major organic acids in Angeleno plum fruit

    NASA Astrophysics Data System (ADS)

    Wang, Yanwei; Wang, Jing; Cheng, Wei; Zhao, Zhilei; Cao, Jiankang

    2014-08-01

    A method was developed to profile major organic acids in Angeleno fruit by high performance liquid chromatography. Organic acids in plum were extracted by water with ultra- sonication at 50°C for 30 min. The extracts were chromatographed on Waters Atlantis T3 C18 column (4.6 mm×250 mm, 5 μm) with 0.01mol/L sulfuric acid and water as mobile phase, and flow rate was 0.5 ml/min. The column temperature was 40C, and chromatography was monitored by a diode array detector at 210 nm. The result showed that malic acid, citric acid, tartaric acid, oxalic acid, pyruvic acid, acetic acid, succinic acid in Angeleno plum, and the malic acid was the major organic acids. The coefficient of determination of the standard calibration curve is R2 > 0.999. The organic acids recovery ranged from 99.11% for Malic acid to 106.70% for Oxalic acid, and CV (n=6) ranged from 0.95% for Malic acid to 6.23% for Oxalic acid, respectively. The method was accurate, sensitive and feasible in analyzing the organic acids in Angeleno plum.

  17. Titration of selected bases in benzene-acetonitrile binary solvent system.

    PubMed

    Amirjahed, K; al-Khamis, K I

    1980-10-01

    The benzene-acetonitrile binary solvent system was used in the determination of the half-neutralization potentials (hnp) of selected bases varying widely in basicity (pKb). The solvent mixtures had specific dielectric constants (Dm). The hnp values of the bases determined in a solvent of a specific Dm value were related to the corresponding pKb values. The slopes of these linear relationships were related to Dm values. A certain mixture of the binary solvent system was selected, and successful differentiating titration of various base mixtures was demonstrated in this medium. The delta hnp/delta pK versus Dm data for acids were compared with those of bases in the benzene-acetonitrile binary solvent system. The resulting data on bases were compared with previously published data on acids, and the present report describes the behavior of acids and bases in the entire composition spectrum of the benzene-acetonitrile binary solvent system.

  18. Isothermal titration calorimetric analysis of the interaction between cationic lipids and plasmid DNA.

    PubMed

    Lobo, B A; Davis, A; Koe, G; Smith, J G; Middaugh, C R

    2001-02-01

    The effects of buffer and ionic strength upon the enthalpy of binding between plasmid DNA and a variety of cationic lipids used to enhance cellular transfection were studied using isothermal titration calorimetry at 25.0 degrees C and pH 7.4. The cationic lipids DOTAP (1,2-dioleoyl-3-trimethyl ammonium propane), DDAB (dimethyl dioctadecyl ammonium bromide), DOTAP:cholesterol (1:1), and DDAB:cholesterol (1:1) bound endothermally to plasmid DNA with a negligible proton exchange with buffer. In contrast, DOTAP: DOPE (L-alpha-dioleoyl phosphatidyl ethanolamine) (1:1) and DDAB:DOPE (1:1) liposomes displayed a negative enthalpy and a significant uptake of protons upon binding to plasmid DNA at neutral pH. These findings are most easily explained by a change in the apparent pKa of the amino group of DOPE upon binding. Complexes formed by reverse addition methods (DNA into lipid) produced different thermograms, sizes, zeta potentials, and aggregation behavior, suggesting that structurally different complexes were formed in each titration direction. Titrations performed in both directions in the presence of increasing ionic strength revealed a progressive decrease in the heat of binding and an increase in the lipid to DNA charge ratio at which aggregation occurred. The unfavorable binding enthalpy for the cationic lipids alone and with cholesterol implies an entropy-driven interaction, while the negative enthalpies observed with DOPE-containing lipid mixtures suggest an additional contribution from changes in protonation of DOPE.

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

    PubMed

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

    2014-12-16

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

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

    SciTech Connect

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

    1997-03-01

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

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

    NASA Technical Reports Server (NTRS)

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

    1990-01-01

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

  2. Universal nucleic acids sample preparation method for cells, spores and their mixture

    DOEpatents

    Bavykin, Sergei [Darien, IL

    2011-01-18

    The present invention relates to a method for extracting nucleic acids from biological samples. More specifically the invention relates to a universal method for extracting nucleic acids from unidentified biological samples. An advantage of the presently invented method is its ability to effectively and efficiently extract nucleic acids from a variety of different cell types including but not limited to prokaryotic or eukaryotic cells and/or recalcitrant organisms (i.e. spores). Unlike prior art methods which are focused on extracting nucleic acids from vegetative cell or spores, the present invention effectively extracts nucleic acids from spores, multiple cell types or mixtures thereof using a single method. Important that the invented method has demonstrated an ability to extract nucleic acids from spores and vegetative bacterial cells with similar levels effectiveness. The invented method employs a multi-step protocol which erodes the cell structure of the biological sample, isolates, labels, fragments nucleic acids and purifies labeled samples from the excess of dye.

  3. Fast high-throughput method for the determination of acidity constants by capillary electrophoresis: I. Monoprotic weak acids and bases.

    PubMed

    Fuguet, Elisabet; Ràfols, Clara; Bosch, Elisabeth; Rosés, Martí

    2009-04-24

    A new and fast method to determine acidity constants of monoprotic weak acids and bases by capillary zone electrophoresis based on the use of an internal standard (compound of similar nature and acidity constant as the analyte) has been developed. This method requires only two electrophoretic runs for the determination of an acidity constant: a first one at a pH where both analyte and internal standard are totally ionized, and a second one at another pH where both are partially ionized. Furthermore, the method is not pH dependent, so an accurate measure of the pH of the buffer solutions is not needed. The acidity constants of several phenols and amines have been measured using internal standards of known pK(a), obtaining a mean deviation of 0.05 pH units compared to the literature values.

  4. Separating acetic acid from furol (furfural) by electrodialysis method

    SciTech Connect

    Guan, S.F.; Li, C.S. Ye, S.T.; Shen, S.Y.; Wang, Y.T.; Yu, S.H.

    1981-01-01

    Furfural production by hydrolysis of fibrous plant materials is accompanied by formation of acetic acid in amounts depending on the material used. The amount of acetic formed in the hydrolysis of the fruit shell of oil-tea camellia (Camellia oleosa) (an oilseed-bearing tree) is equal to the amount of furfural. The acetic acid can be separated from the furfural and concentrated to 10% by electrodialysis. A smaller amount of furfural is separated with acetic acid.

  5. [Photometric micro-titration model of DPPH radicals scavenging activity and its application].

    PubMed

    Gao, Yun-tao; Wei, Wei; Ye, Li-qing; Li, Xiao-fen; Liu, Ping; Zhang, Hong-jiao; Yang, Lu; Yu, Jiao-jiao; Cha, Jia-wei

    2015-02-01

    In the present paper, the stoichiometric ratio (R) for the interreaction of DPPH radicals with the antoxidant was employed as a evaluation index for DPPH radicals scavenging activity of antioxidants. This evaluation index was related only with the stoichiometric relationship between DPPH radicals and the antioxidant, not the relationship with the initial DPPH amount and the volume of sample, which could offer a solution for the problem of poor comparability of EC50 under different conditions. A novel photometric micro-titration method was proposed for the determination of the stoichiometric ratio (R) for the interreaction of DPPH radicals with the antoxidant. The titration equation was established based on the absorbance difference (deltaA) of DPPH radicals in the titration process and the added amount of antoxidant. The stoichiometric ratio (R) for the reaction of DPPH radicals with the addition amount of antoxidant was determined by the titration equation obtained, while, the DPPH median elimination concentration (EC50) of antoxidant can be calculated by the stoichiometric ratio (R). The above photometric micro-titration model was verified using rutin as DPPH radicals scavenger. As experiment results, the stoichiometric ratio (R) of DPPH radicals to rutin was determined to be in the range of 1.817-1.846. The calculated value of EC50 was 1.196 x 10(-3), 2.392 x 10(-3), 4.819 x 10(-3) and 7.292 x 10(-3) mg x mL(-1) for 1.12 x 10(-7), 2.24 x 10(-7), 4.48 x 10(-7) and 6.72 x 10(-7) mol of the additon amount of DPPH radicals, respectively. The proposed method has better precision and reliability with smaller amount of sample than conventional method. While, the obtained stoichiometric ratio value (R) of rutin was employed to calculate the rutin median elimination concentration for DPPH EC50) according to the conditions as reported in the literatures, and the calculated results were consistent with that reported in the literatures.

  6. Ionization behavior of polyphosphoinositides determined via the preparation of pH titration curves using solid-state 31P NMR.

    PubMed

    Graber, Zachary T; Kooijman, Edgar E

    2013-01-01

    Detailed knowledge of the degree of ionization of lipid titratable groups is important for the evaluation of protein-lipid and lipid-lipid interactions. The degree of ionization is commonly evaluated by acid-base titration, but for lipids localized in a multicomponent membrane interface this is not a suitable technique. For phosphomonoester-containing lipids such as the polyphosphoinositides, phosphatidic acid, and ceramide-1-phosphate, this is more conveniently accomplished by (31)P NMR. Here, we describe a solid-state (31)P NMR procedure to construct pH titration curves to determine the degree of ionization of phosphomonoester groups in polyphosphoinositides. This procedure can also be used, with suitable sample preparation conditions, for other important signaling lipids. Access to a solid-state, i.e., magic angle spinning, capable NMR spectrometer is assumed. The procedures described here are valid for a Bruker instrument, but can be adapted for other spectrometers as needed.

  7. Coulometric titration of ruthenium and iridium by the generated hydroquinone

    SciTech Connect

    Organeysan, L.S.; Butakova, N.A.

    1986-05-10

    This paper studies the electrogeneration of hydroquinone from solutions of quinone on platinum and glass-carbon electrodes in HC1 and H/sub 2/SO/sub 4/ media of different concentrations, to select the optimal conditions for the coulometric titration of Ru(IV) and Ir(IV).

  8. Method for analyzing nucleic acids by means of a substrate having a microchannel structure containing immobilized nucleic acid probes

    DOEpatents

    Ramsey, J. Michael; Foote, Robert S.

    2002-01-01

    A method and apparatus for analyzing nucleic acids includes immobilizing nucleic probes at specific sites within a microchannel structure and moving target nucleic acids into proximity to the probes in order to allow hybridization and fluorescence detection of specific target sequences.

  9. Method for analyzing nucleic acids by means of a substrate having a microchannel structure containing immobilized nucleic acid probes

    DOEpatents

    Ramsey, J. Michael; Foote, Robert S.

    2003-12-09

    A method and apparatus for analyzing nucleic acids includes immobilizing nucleic probes at specific sites within a microchannel structure and moving target nucleic acids into proximity to the probes in order to allow hybridization and fluorescence detection of specific target sequences.

  10. Non-intercalative, deoxyribose binding of boric acid to calf thymus DNA.

    PubMed

    Ozdemir, Ayse; Gursaclı, Refiye Tekiner; Tekinay, Turgay

    2014-05-01

    The present study characterizes the effects of the boric acid binding on calf thymus DNA (ct-DNA) by spectroscopic and calorimetric methods. UV-Vis absorbance spectroscopy, circular dichroism (CD) spectroscopy, transmission electron microscopy (TEM), isothermal titration calorimetry (ITC), and Fourier transform infrared (FT-IR) spectroscopy were employed to characterize binding properties. Changes in the secondary structure of ct-DNA were determined by CD spectroscopy. Sizes and morphologies of boric acid-DNA complexes were determined by transmission electron microscopy (TEM). The kinetics of boric acid binding to calf thymus DNA (ct-DNA) was investigated by isothermal titration calorimetry (ITC). ITC results revealed that boric acid exhibits a moderate affinity to ct-DNA with a binding constant (K a) of 9.54 × 10(4) M(-1). FT-IR results revealed that boric acid binds to the deoxyribose sugar of DNA without disrupting the B-conformation at tested concentrations.

  11. A Novel Method for Presenting the Amino Acids in an Introductory Biochemistry Course.

    ERIC Educational Resources Information Center

    Kuehl, LeRoy

    1978-01-01

    Introduces an approach to teaching amino acids that employs the use of a poem containing information on the structure and properties of amino acids, and of slides illustrating the poem. Student response to the method was positive. (MA)

  12. Method for removing acid gases from a gaseous stream

    DOEpatents

    Gorin, Everett; Zielke, Clyde W.

    1981-01-01

    In a process for hydrocracking a heavy aromatic polynuclear carbonaceous feedstock containing reactive alkaline constituents to produce liquid hydrocarbon fuels boiling below about 475.degree. C. at atmospheric pressure by contacting the feedstock with hydrogen in the presence of a molten metal halide catalyst, thereafter separating a gaseous stream containing hydrogen, at least a portion of the hydrocarbon fuels and acid gases from the molten metal halide and regenerating the molten metal halide, thereby producing a purified molten metal halide stream for recycle to the hydrocracking zone, an improvement comprising; contacting the gaseous acid gas, hydrogen and hydrocarbon fuels-containing stream with the feedstock containing reactive alkaline constituents to remove acid gases from the acid gas containing stream. Optionally at least a portion of the hydrocarbon fuels are separated from gaseous stream containing hydrogen, hydrocarbon fuels and acid gases prior to contacting the gaseous stream with the feedstock.

  13. Energy recovery method and system for combined sulphuric acid and phosphoric acid manufacturing plant

    SciTech Connect

    Cameron, G. M.; Orlando, J. V.

    1985-01-22

    In conventional processes for manufacturing phosphoric acid, sulphuric acid is reacted with phosphate rock to produce weak phosphoric acid which is concentrated using steam from the associated sulphuric acid manufacturing operation. Low grade heat from the absorbers and drier of the sulphuric acid manufacturing plant has been wasted. According to the invention waste heat from the drier and one or more absorbers of the sulphuric acid manufacturing plant is used in all the evaporators of the phosphoric acid plant. The evaporators all operate at low pressures and their heaters are arranged in series, to enable the heat to be used at the relatively low temperatures available. The valuable steam is thus freed for other uses.

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

    NASA Astrophysics Data System (ADS)

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

    2011-10-01

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

  15. Method for nucleic acid hybridization using single-stranded DNA binding protein

    DOEpatents

    Tabor, Stanley; Richardson, Charles C.

    1996-01-01

    Method of nucleic acid hybridization for detecting the presence of a specific nucleic acid sequence in a population of different nucleic acid sequences using a nucleic acid probe. The nucleic acid probe hybridizes with the specific nucleic acid sequence but not with other nucleic acid sequences in the population. The method includes contacting a sample (potentially including the nucleic acid sequence) with the nucleic acid probe under hybridizing conditions in the presence of a single-stranded DNA binding protein provided in an amount which stimulates renaturation of a dilute solution (i.e., one in which the t.sub.1/2 of renaturation is longer than 3 weeks) of single-stranded DNA greater than 500 fold (i.e., to a t.sub.1/2 less than 60 min, preferably less than 5 min, and most preferably about 1 min.) in the absence of nucleotide triphosphates.

  16. Nucleic acid detection system and method for detecting influenza

    DOEpatents

    Cai, Hong; Song, Jian

    2015-03-17

    The invention provides a rapid, sensitive and specific nucleic acid detection system which utilizes isothermal nucleic acid amplification in combination with a lateral flow chromatographic device, or DNA dipstick, for DNA-hybridization detection. The system of the invention requires no complex instrumentation or electronic hardware, and provides a low cost nucleic acid detection system suitable for highly sensitive pathogen detection. Hybridization to single-stranded DNA amplification products using the system of the invention provides a sensitive and specific means by which assays can be multiplexed for the detection of multiple target sequences.

  17. Method for producing 3-hydroxypropionic acid and other products

    DOEpatents

    Lynch, Michael D.; Gill, Ryan T.; Lipscomb, Tanya E.W.

    2016-08-30

    This invention relates to metabolically engineered microorganism strains, such as bacterial strains, in which there is an increased utilization of malonyl-CoA for production of a chemical product, which includes 3-hydroxypropionic acid.

  18. Methods for producing 3-hydroxypropionic acid and other products

    DOEpatents

    Lynch, Michael D.; Gill, Ryan T.; Lipscomb, Tanya E. W.

    2016-07-12

    This invention relates to metabolically engineered microorganism strains, such as bacterial strains, in which there is an increased utilization of malonyl-CoA for production of a chemical product, which includes 3-hydroxypropionic acid.

  19. Determination of Calcium in Dietary Supplements: Statistical Comparison of Methods in the Analytical Laboratory

    ERIC Educational Resources Information Center

    Garvey, Sarah L.; Shahmohammadi, Golbon; McLain, Derek R.; Dietz, Mark L.

    2015-01-01

    A laboratory experiment is described in which students compare two methods for the determination of the calcium content of commercial dietary supplement tablets. In a two-week sequence, the sample tablets are first analyzed via complexometric titration with ethylenediaminetetraacetic acid and then, following ion exchange of the calcium ion present…

  20. Simple and reliable method for determination of oxygen content in high- Tc copper oxides

    NASA Astrophysics Data System (ADS)

    Maeno, Yoshiteru; Teraoka, Hideki; Matsukuma, Kuniko; Yoshida, Koji; Sugiyama, Kimihiko; Nakamura, Fumihiko; Fujita, Toshizo

    1991-12-01

    We present the details of a simple and reliable iodine-titration method suited for high- Tc copper oxides, in which the use of a solution of ammonium acetate and acetic acid as a buffer agent substantially improves the operation. The results applied to La 2- xM xCuO 4- δ (M = Ba, Sr and Ca) are presented.

  1. Materials and methods for efficient lactic acid production

    DOEpatents

    Zhou, Shengde; Ingram, Lonnie O'Neal; Shanmugam, Keelnatham T.; Yomano, Lorraine; Grabar, Tammy B.; Moore, Jonathan C.

    2009-12-08

    The present invention provides derivatives of ethanologenic Escherichia coli K011 constructed for the production of lactic acid. The transformed E. coli of the invention are prepared by deleting the genes that encode competing pathways followed by a growth-based selection for mutants with improved performance. These transformed E. coli are useful for providing an increased supply of lactic acid for use in food and industrial applications.

  2. Materials and methods for efficient lactic acid production

    SciTech Connect

    Zhou, Shengde; Ingram, Lonnie O'Neal; Shanmugam, Keelnatham T; Yomano, Lorraine; Grabar, Tammy B; Moore, Jonathan C

    2013-04-23

    The present invention provides derivatives of Escherichia coli constructed for the production of lactic acid. The transformed E. coli of the invention are prepared by deleting the genes that encode competing pathways followed by a growth-based selection for mutants with improved performance. These transformed E. coli are useful for providing an increased supply of lactic acid for use in food and industrial applications.

  3. Application of isothermal titration calorimeter for screening bitterness-suppressing molecules of quinine.

    PubMed

    Zhang, Yifan; Zhu, Youwei; Zhao, Na; Wu, Jinhui; Hu, Yiqiao

    2016-01-01

    Bitterness-suppressing molecules have drawn ever-increasing attention these years for some unique advantages like low molecular weight, tastelessness and no interference on drug bioavailability. L-Arg was reported to suppress the bitterness of quinine, and we happened to find that the suppressing effects could be demonstrated by isothermal titration calorimeter (ITC). In this study, we investigated the possibility of using ITC to screen bitterness-suppressing molecules for quinine. Among the amino acids we screened, L-Lys bond quinine with high affinity. The results of ITC correlated well with the results of human sensory experiments. L-Arg and L-Lys could suppress the bitterness of quinine while other amino acids could not. Therefore, ITC has the potential to screen bitterness-suppressing molecules.

  4. Comparative Oxidative Stability of Fatty Acid Alkyl Esters by Accelerated Methods

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Several fatty acid alkyl esters were subjected to accelerated methods of oxidation, including EN 14112 (Rancimat method) and pressurized differential scanning calorimetry (PDSC). Structural trends elucidated from both methods that improved oxidative stability included decreasing the number of doubl...

  5. Validation of a multi-analyte HPLC-DAD method for determination of uric acid, creatinine, homovanillic acid, niacinamide, hippuric acid, indole-3-acetic acid and 2-methylhippuric acid in human urine.

    PubMed

    Remane, Daniela; Grunwald, Soeren; Hoeke, Henrike; Mueller, Andrea; Roeder, Stefan; von Bergen, Martin; Wissenbach, Dirk K

    2015-08-15

    During the last decades exposure sciences and epidemiological studies attracts more attention to unravel the mechanisms for the development of chronic diseases. According to this an existing HPLC-DAD method for determination of creatinine in urine samples was expended for seven analytes and validated. Creatinine, uric acid, homovanillic acid, niacinamide, hippuric acid, indole-3-acetic acid, and 2-methylhippuric acid were separated by gradient elution (formate buffer/methanol) using an Eclipse Plus C18 Rapid Resolution column (4.6mm×100mm). No interfering signals were detected in mobile phase. After injection of blank urine samples signals for the endogenous compounds but no interferences were detected. All analytes were linear in the selected calibration range and a non weighted calibration model was chosen. Bias, intra-day and inter-day precision for all analytes were below 20% for quality control (QC) low and below 10% for QC medium and high. The limits of quantification in mobile phase were in line with reported reference values but had to be adjusted in urine for homovanillic acid (45mg/L), niacinamide 58.5(mg/L), and indole-3-acetic acid (63mg/L). Comparison of creatinine data obtained by the existing method with those of the developed method showing differences from -120mg/L to +110mg/L with a mean of differences of 29.0mg/L for 50 authentic urine samples. Analyzing 50 authentic urine samples, uric acid, creatinine, hippuric acid, and 2-methylhippuric acid were detected in (nearly) all samples. However, homovanillic acid was detected in 40%, niacinamide in 4% and indole-3-acetic acid was never detected within the selected samples.

  6. Expenditures associated with dose titration at initiation of therapy in patients with major depressive disorder: a retrospective analysis of a large managed care claims database.

    PubMed

    Camacho, Fabian; Kong, Meg C; Sheehan, David V; Balkrishnan, Rajesh

    2010-08-01

    OBJECTIVE.: Although selective serotonin reuptake inhibitors (SSRIs) are considered cost-effective medications for patients with major depressive disorder (MDD), significant dosage adjustments are often necessary when treatment is initiated. Our study was conducted to examine whether dose titration for SSRIs at initiation of therapy was associated with a greater use of health care resources and higher costs. STUDY DESIGN.: A retrospective database analysis was conducted. METHODS.: A nationally representative cohort of individuals with MDD was identified in a large managed care claims database between January 1, 2004, and December 31, 2006. A study-specific titration algorithm was used to identify patients who underwent dose titration, compared with those who did not, within the first eight weeks of initiating SSRI therapy. We calculated propensity scores and identified a 1:1 matched cohort of titration versus non-titration patients. We used univariate and multivariate statistical tests to compare the mean number of therapeutic days, health care service utilization, and expenditures between the two groups during the first eight weeks (56 days) of treatment and six months (180 days) after treatment began. RESULTS.: Over the first eight weeks, the titration cohort had a 32% decrease in the adjusted mean number of therapeutic days (38 vs. 56, respectively; P < 0.001), a 50% increase in depression-related outpatient visits (1.8 vs. 1.2; P < 0.001), a 38% increase in depression-related outpatient costs ($137 vs. $81; P ≤ 0.001), an increase in antidepressant pharmacy costs ($139 vs. $61; P < 0.001), and a 64% increase in psychiatric visits (0.69 vs. 0.42; P = 0.001), compared with the matched non-titration cohort. These differences were consistent among individual SSRI groups as well as during the six-month period. CONCLUSION.: Patients undergoing dose titration of SSRIs at the beginning of therapy consumed more medical resources and spent more days receiving a

  7. Study on the interaction of morphine chloride with deoxyribonucleic acid by fluorescence method

    NASA Astrophysics Data System (ADS)

    Li, J. F.; Dong, C.

    2009-01-01

    The mode and mechanism of the interaction of morphine chloride, an important alkaloid compound to calf thymus deoxyribonucleic acid (ct DNA) was investigated from absorption and fluorescence titration techniques. Hypochromic effect was founded in the absorption spectra of morphine when concentration of DNA increased. The decreased fluorescence study revealed non-cooperative binding of the morphine to DNA with an affinity of 3.94 × 10 3 M -1, and the stoichiometry of binding was characterized to be about one morphine molecule per nucleotide. Stern-Volmer plots at different temperatures proved that the quenching mechanism was static. Ferrocyanide quenching study showed that the magnitude of KSV of the bound morphine was lower than that of the free one. In addition, it was found that ionic strength could affect the binding of morphine and DNA. Fluorescence polarization and denatured DNA studies also applied strong evidences that morphine molecule was partially intercalated between every alternate base pairs of ct DNA. As observed from above experiments, intercalation was well supported as the binding mode of morphine and ct DNA.

  8. Remedial methods for intergranular attack of alloy 600 tubing. Volume 3. Boric acid and acetic acid remedial methods. Final report

    SciTech Connect

    Rubright, M.M.

    1986-06-01

    An important cause of recent tube degradation in recirculating pressurized water reactor (PWR) steam generators with open tube/tubesheet crevices is intergranular attack (IGA) of alloy 600 tubing in the crevice region. The attack appears to occur on the hot leg tubing because of high concentrations of caustic species formed from remnants of past phosphate water treatment, combined with materials from inleakage from freshwater-cooled condensers. The concept of using neutralizers to modify the aggressiveness of the crevice environment was examined. It appears that this can be accomplished by neutralizing the caustic species with an acid. Two ways to apply the acid are by off-line flushing during plant shutdown and by on-line treatment during operation. The substance that appears to be most suitable for off-line flushing is acetic acid, with boric acid as a second choice. Concentrations should be in the range of from 1000 to 5000 ppM. The addition of 1000 to 5000 ppM of a non-ionic detergent in the flush solution should improve penetration of the crevice. Use of preflush lancing to remove sludge on the tubesheet will also help by reducing acid consumption. The requirements for materials to be used in on-line treatment are more stringent because of possible interaction with other components in the secondry system. Boric acid is the only substance that has operational experience. A series of tests are proposed to investigate the behavior of acetic acid and boric acid on tubesheet sludge, on tubesheet/support plate material, and on alloy 600/tubesheet couples. Similarly, areas of uncertainty of on-line treatment with boric acid are its effect on tubesheet/support plate materials and on the rest of the secondary system. 23 refs.

  9. Characterization and quantification of N-(3-aminopropyl)-N-dodecyl-1,3-propanediamine biocide by NMR, HPLC/MS and titration techniques.

    PubMed

    Mondin, Andrea; Bogialli, Sara; Venzo, Alfonso; Favaro, Gabriella; Badocco, Denis; Pastore, Paolo

    2014-01-01

    The present paper reports the determination of the tri-amine N-(3-aminopropyl)-N-dodecyl-1,3-propanediamine (TA) present in a raw material called LONZABAC used to formulate various, widely used commercial biocides. The active principle, TA, is present in LONZABAC together with other molecules at lower concentration levels. Three independent analytical approaches, namely solution NMR spectroscopy, liquid chromatography coupled to high resolution mass spectrometry (LC/HRMS) and acid-base titration in mixed solvent, were used to overcome the problem of the non-availability of the active principle as high purity standard. NMR analysis of raw material, using a suitable internal standard, evidenced in all analyzed lots the presence of the active principle, the N-dodecyl-1,3-propanediamine (DA) and the n-dodecylamine (MA) and the absence of non-organic, NMR-inactive species. NMR peak integration led to a rough composition of the MA:DA:TA as 1:9:90. The LC/HRMS analysis allowed the accurate determination of DA and MA and confirmed in all samples the presence of the TA, which was estimated by difference: MA=1.4±0.3%, DA=11.1±0.7%, TA=87.5±1.3%. The obtained results were used to setup an easy, rapid and cheap acid-base titration method able to furnish a sufficiently accurate evaluation of the active principle both in the raw material and in diluted commercial products. For the raw material the results were: TA+MA=91.1±0.8% and DA-MA=8.9±0.8%, statistically coherent with LC/MS ones. The LC/MS approach demonstrated also its great potentialities to recognize trace of the biocide components both in environmental samples and in the formulated commercial products.

  10. Scopolamine Effects Under a Titrating-Delayed-Nonmatching-to-Position Procedure

    ERIC Educational Resources Information Center

    Porritt, M.; Poling, A.

    2008-01-01

    In a study of working memory, the performance of rats under titrating-delayed-nonmatching- to-position (TDNMTP) procedures was examined. Overall accuracy and the number of trials completed were inversely related to titration value, whereas the highest delay attained was directly related to titration value. When given intraperitoneally,…

  11. Analysis of Secondary Structure and Self-Assembly of Amelogenin by Variable Temperature Circular Dichroism and Isothermal Titration Calorimetry

    PubMed Central

    Lakshminarayanan, Rajamani; Yoon, Il; Hegde, Balachandra G.; Daming, Fan; Du, Chang; Moradian-Oldak, Janet

    2009-01-01

    Amelogenin is a proline-rich enamel matrix protein known to play an important role in the oriented growth of enamel crystals. Amelogenin self-assembles to form nanospheres and higher order structures mediated by hydrophobic interactions. This study aims to obtain a better insight into the relationship between primary-secondary structure and self-assembly of amelogenin by applying computational and biophysical methods. Variable temperature circular dichroism studies indicated that under physiological pH recombinant full-length porcine amelogenin contains unordered structures in equilibrium with polyproline type II (PPII) structure, the latter being more populated at lower temperatures. Increasing the concentration of rP172 resulted in the promotion of folding to an ordered β-structured assembly. Isothermal titration calorimetry dilution studies revealed that, at all temperatures, self-assembly is entropically driven due to the hydrophobic effect and the molar heat of assembly (ΔHA) decreases with temperature. Using a computational approach, a profile of domains in the amino acid sequence that have a high propensity to assemble and to have PPII structures has been identified. We conclude that the assembly properties of amelogenin are due to complementarity between the hydrophobic and PPII helix prone regions. PMID:19274734

  12. Method for promoting specific alignment of short oligonucleotides on nucleic acids

    DOEpatents

    Studier, F. William; Kieleczawa, Jan; Dunn, John J.

    1996-01-01

    Disclosed is a method for promoting specific alignment of short oligonucleotides on a nucleic acid polymer. The nucleic acid polymer is incubated in a solution containing a single-stranded DNA-binding protein and a plurality of oligonucleotides which are perfectly complementary to distinct but adjacent regions of a predetermined contiguous nucleotide sequence in the nucleic acid polymer. The plurality of oligonucleotides anneal to the nucleic acid polymer to form a contiguous region of double stranded nucleic acid. Specific application of the methods disclosed include priming DNA synthesis and template-directed ligation.

  13. Improved Segmented-Flow Tracer-Monitored Titration for Automated Measurement of Total Alkalinity in Seawater

    NASA Astrophysics Data System (ADS)

    Spaulding, R. S.; Hales, B.; Beck, J. C.; Degrandpre, M. D.

    2008-12-01

    The four measurable inorganic carbon parameters commonly measured as part of oceanic carbon cycle studies are total dissolved inorganic carbon (DIC), total alkalinity (AT), hydrogen ion concentration (pH) and partial pressure of CO2 (pCO2). AT determination is critical for anthropogenic CO2 inventory calculations and for quantifying CaCO3 saturation. Additionally, measurement of AT in combination with one other carbonate parameter can be used to describe the inorganic carbon equilibria. Current methods for measuring AT require calibrated volumetric flasks and burettes, gravimetry, or precise flow measurements. These methods also require analysis times of ˜15 min and sample volumes of ˜200 mL, and sample introduction is not automated, resulting in labor-intensive measurements and low temporal resolution. The Tracer Monitored Titration (TMT) system was previously developed at the University of Montana for AT measurements. The TMT is not dependent on accurate gravimetric, volumetric or flow rate measurements because it relies on a pH-sensitive indicator (tracer) to track the amount of titrant added to the sample. Sample and a titrant-indicator mixture are mechanically stirred in an optical flow cell and pH is calculated using the indicator equilibrium constant and the spectrophotometrically determined concentrations of the acid and base forms of the indicator. AT is then determined using these data in a non-linear least squares regression of the AT mass and proton balances. The precision and accuracy of the TMT are 2 and 4 micromol per kg in 16 min using 110-mL of sample. The TMT is dependent on complete mixing of titrant with the sample and accurate absorbance measurements. We have developed the segmented-flow TMT (SF- TMT) to improve on these aspects and decrease sample analysis time. The TMT uses segmented flow instead of active mixing and a white LED instead of a tungsten-halogen light source. Air is added to the liquid flow stream, producing segments of liquid

  14. Solubility of dicalcium phosphate dihydrate by solid titration.

    PubMed

    Pan, H-B; Darvell, B W

    2009-01-01

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

  15. Determination of aqueous acid-dissociation constants of aspartic acid using PCM/DFT method

    NASA Astrophysics Data System (ADS)

    Sang-Aroon, Wichien; Ruangpornvisuti, Vithaya

    Determination of acid-dissociation constants, pKa, of aspartic acid in aqueous solution, using density functional theory calculations combined with the conductor-like polarizable continuum model (CPCM) and with integral-equation-formalism polarizable continuum model (IEFPCM) based on the UAKS and UAHF radii, was carried out. The computed pKa values derived from the CPCM and IEFPCM with UAKS cavity model of bare structures of the B3LYP/6-31+G(d,p)-optimized tetrahydrated structures of aspartic acid species are mostly close to the experimental pKa values.0

  16. Measuring the sequence-affinity landscape of antibodies with massively parallel titration curves

    PubMed Central

    Adams, Rhys M; Mora, Thierry; Walczak, Aleksandra M; Kinney, Justin B

    2016-01-01

    Despite the central role that antibodies play in the adaptive immune system and in biotechnology, much remains unknown about the quantitative relationship between an antibody’s amino acid sequence and its antigen binding affinity. Here we describe a new experimental approach, called Tite-Seq, that is capable of measuring binding titration curves and corresponding affinities for thousands of variant antibodies in parallel. The measurement of titration curves eliminates the confounding effects of antibody expression and stability that arise in standard deep mutational scanning assays. We demonstrate Tite-Seq on the CDR1H and CDR3H regions of a well-studied scFv antibody. Our data shed light on the structural basis for antigen binding affinity and suggests a role for secondary CDR loops in establishing antibody stability. Tite-Seq fills a large gap in the ability to measure critical aspects of the adaptive immune system, and can be readily used for studying sequence-affinity landscapes in other protein systems. DOI: http://dx.doi.org/10.7554/eLife.23156.001 PMID:28035901

  17. A review on methods of recovery of acid(s) from spent pickle liquor of steel industry.

    PubMed

    Ghare, N Y; Wani, K S; Patil, V S

    2013-04-01

    Pickling is the process of removal of oxide layer and rust formed on metal surface. It also removes sand and corrosion products from the surface of metal. Acids such as sulfuric acid, hydrochloric acid are used for pickling. Hydrofluoric acid-Nitric acid mixture is used for stainless steel pickling. Pickling solutions are spent when acid concentration in pickling solutions decreases by 75-85%, which also has metal content up to 150-250 g/ dm3. Spent pickling liquor (SPL) should be dumped because the efficiency of pickling decreases with increasing content of dissolved metal in the bath. The SPL content depends on the plant of origin and the pickling method applied there. SPL from steel pickling in hot-dip galvanizing plants contains zinc(II), iron, traces of lead, chromium. and other heavy metals (max. 500 mg/dm3) and hydrochloric acid. Zinc(II) passes tothe spent solution after dissolution of this metal from zinc(II)-covered racks, chains and baskets used for transportation of galvanized elements. Unevenly covered zinc layers are usually removed in another pickling bath. Due to this, zinc(II) concentration increases even up to 110 g/dm3, while iron content may reach or exceed even 80 g/dm3 in the same solution. This review presents an overview on different aspects of generation and treatment of SPL with recourse to recovery of acid for recycling. Different processes are described in this review and higher weightage is given to membrane processes.

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

    PubMed

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

    2014-01-01

    The most commonly used chondroitin sulfate (CS) assay method is cetylpyridinium chloride (CPC) titration. Cellulose acetate membrane electrophoresis (CAME) is the technique used for detection of impurities in the U.S. Pharmacopeia's CS monograph. Because CPC titration is a relatively nonspecific quantitative technique, the apparent amount of CS as determined by CPC titration alone may not reflect the true amount of CS due to possible interference with the CPC assay by impurities that contain CPC titratable functional groups. When CAME is used in conjunction with CPC titration, certain non-CS and adulterants can be visualized and estimated, and a true value for CS can be assigned once the presence of these non-CS impurities has been ruled out. This study examines conjunct application of CPC and CAME in ascertaining CS assay and purity in the presence of certain adulterants. These include propylene glycol alginate sulfate sodium, known in commerce as alginic sodium diester (ASD), and Zero One (Z1), a water-soluble agent newly reported in the CS marketplace and subsequently identified as sodium hexametaphosphate. ASD, Z1, and CS are similar in physical appearance and solubility in water and ethanol. They are also titratable anions and form ionic pairs with CPC, therefore interfering with the CPC titration assay for CS CAME separates these adulterants from each other and from CS by differences in their electrophoretic mobility. CAME is able to detect these impurities in CS at levels as low as 0.66% by weight. Although it is recommended that a method for detecting impurities (e.g., CAME) be used in cormbination with relatively nonspecific assay methods such as CPC titration, this is seldom done in practice. Assay results for CS derived fromn CPC titration may, therefore, be misleading, leaving the CS supply chain vulnerable to adulteration. In this study, the authors investigated ASD and Z1 adulteration of CS and developed an electrophoretic separation of these

  19. Improved method for extracting lanthanides and actinides from acid solutions

    DOEpatents

    Horwitz, E.P.; Kalina, D.G.; Kaplan, L.; Mason, G.W.

    1983-07-26

    A process for the recovery of actinide and lanthanide values from aqueous acidic solutions uses a new series of neutral bi-functional extractants, the alkyl(phenyl)-N,N-dialkylcarbamoylmethylphosphine oxides. The process is suitable for the separation of actinide and lanthanide values from fission product values found together in high-level nuclear reprocessing waste solutions.

  20. Microtubule-associated proteins and tubulin interaction by isothermal titration calorimetry.

    PubMed

    Tsvetkov, P O; Barbier, P; Breuzard, G; Peyrot, V; Devred, F

    2013-01-01

    Microtubules play an important role in a number of vital cell processes such as cell division, intracellular transport, and cell architecture. The highly dynamic structure of microtubules is tightly regulated by a number of stabilizing and destabilizing microtubule-associated proteins (MAPs), such as tau and stathmin. Because of their importance, tubulin-MAPs interactions have been extensively studied using various methods that provide researchers with complementary but sometimes contradictory thermodynamic data. Isothermal titration calorimetry (ITC) is the only direct thermodynamic method that enables a full thermodynamic characterization (stoichiometry, enthalpy, entropy of binding, and association constant) of the interaction after a single titration experiment. This method has been recently applied to study tubulin-MAPs interactions in order to bring new insights into molecular mechanisms of tubulin regulation. In this chapter, we review the technical specificity of this method and then focus on the use of ITC in the investigation of tubulin-MAPs binding. We describe technical issues which could arise during planning and carrying out the ITC experiments, in particular with fragile proteins such as tubulin. Using examples of stathmin and tau, we demonstrate how ITC can be used to gain major insights into tubulin-MAP interaction.

  1. Thermochemical comparisons of homogeneous and heterogeneous acids and bases. 1. Sulfonic acid solutions and resins as prototype Broensted acids

    SciTech Connect

    Arnett, E.M.; Haaksma, R.A.; Chawla, B.; Healy, M.H.

    1986-08-06

    Heats of ionization by thermometric titration for a series of bases (or acids) can be used to compare solid acids (or bases) with liquid analogues bearing the same functionalities in homogeneous solutions. The method is demonstrated for Broensted acids by reacting a series of substituted nitrogen bases with solutions of p-toluenesulfonic acid (PTSA) in acetonitrile and with suspensions of the microporous polymeric arylsulfonic acid resin-Dowex 50W-X8 in the same solvent. Under well-controlled anhydrous conditions there is a good correlation (r = 0.992) between the heats of reaction of the bases with the homogeneous and heterogeneous acid systems, but the homogeneous system gives a more exothermic interaction by 3-4 kcal mol/sup -1/ for a series of 29 substituted pyrimidines, anilines, and some other amines. This difference may be attributed to homohydrogen bonding interactions between excess acid and sulfonate anion sites which are more restricted geometrically in the resin than in solution. Other factors which affect the enthalpy change for the acid-base interaction are the acid/base ratio, the water content of the sulfonic acid, the solvent, and the resin structure (e.g., microporous vs. macroporous). Steric hindrance in the base does not differentiate solid from homogeneous acid. In addition to the use of titration calorimetry, heats of immersion are reported for the Dowex-arylsulfonic acid resins and the Nafion-perfluorinated sulfonic acid resin in a series of basic liquids. The results are compared with each other and with those from a previous study of several varieties of coal.

  2. Methods for point-of-care detection of nucleic acid in a sample

    DOEpatents

    Bearinger, Jane P.; Dugan, Lawrence C.

    2015-12-29

    Provided herein are methods and apparatus for detecting a target nucleic acid in a sample and related methods and apparatus for diagnosing a condition in an individual. The condition is associated with presence of nucleic acid produced by certain pathogens in the individual.

  3. STATISTICAL VALIDATION OF SULFATE QUANTIFICATION METHODS USED FOR ANALYSIS OF ACID MINE DRAINAGE

    EPA Science Inventory

    Turbidimetric method (TM), ion chromatography (IC) and inductively coupled plasma atomic emission spectrometry (ICP-AES) with and without acid digestion have been compared and validated for the determination of sulfate in mining wastewater. Analytical methods were chosen to compa...

  4. Stepwise determination of quaternary ammonium salts and aromatic amines in pharmaceuticals by ion association titration.

    PubMed

    Sakai, T

    2001-12-01

    A stepwise titrimetric method has been developed for the simultaneous determination of pharmaceutical quaternary ammonium salts (R4N+) and aromatic amines (R3N). The method is based on the solvent extraction of R4N+ and R3NH+ with an ion association reagent. Sodium tetrakis(4-fluorophenyl)borate and sodium tetraphenylborate were used as titrants and potassium tetrabromophenolphthalein ethyl ester (TBPE) was used as an indicator. The ion associate which formed between R4N+ ion and TBPE made a blue color in 1,2-dichloroethane, while the ion associate formed between R3NH+ and TBPE showed a red-violet one. Sample solutions containing quaternary ammonium and/or amine compounds were titrated with sodium tetrakis(4-fluorophenyl)borate or sodium tetraphenylborate. When one drop of excess titrant was added, the color of the organic phase turned from blue or red-violet to yellow at the equivalence point. On the other hand, in the mixture of R4N+ and R3N, the color changed from blue to red-violet at the first equivalence point, and then its color turned to yellow at the second equivalence point. The quaternary ammonium compound and aromatic amine in pharmaceuticals could be simultaneously and successfully determined by the proposed titration method.

  5. Standard test method for acidity of distillation residues or hydrocarbon liquids

    SciTech Connect

    Not Available

    1980-01-01

    This method covers the qualitative determination of the acidity of the distillation residue from a gasoline. The sample of distillation residue or hydrocarbon liquid is shaken with water and the aqueous layer tested for acidity to methyl orange. Some petroleum products are treated with mineral acid as part of the refining procedure. Obviously, any residual mineral acid in a petroleum product is undesirable. The absence of a positive indication in the test for acidity of the distillation residue or aqueous extract of a hydrocarbon liquid is an assurance of the care used in refining the fuel or solvent.

  6. Method for construction of bacterial strains with increased succinic acid production

    DOEpatents

    Donnelly, Mark I.; Sanville-Millard, Cynthia; Chatterjee, Ranjini

    2000-01-01

    A fermentation process for producing succinic acid is provided comprising selecting a bacterial strain that does not produce succinic acid in high yield, disrupting the normal regulation of sugar metabolism of said bacterial strain, and combining the mutant bacterial strain and selected sugar in anaerobic conditions to facilitate production of succinic acid. Also provided is a method for changing low yield succinic acid producing bacteria to high yield succinic acid producing bacteria comprising selecting a bacterial strain having a phosphotransferase system and altering the phosphotransferase system so as to allow the bacterial strain to simultaneously metabolize different sugars.

  7. Effects of fixed or self-titrated dosages of Sativex on cannabis withdrawal and cravings

    PubMed Central

    Trigo, Jose M.; Lagzdins, Dina; Rehm, Jürgen; Selby, Peter; Gamaleddin, Islam; Fischer, Benedikt; Barnes, Allan J.; Huestis, Marilyn A.; Le Foll, Bernard

    2016-01-01

    Background There is currently no pharmacological treatment approved for cannabis dependence. In this proof of concept study, we assessed the feasibility/effects of fixed and self-titrated dosages of Sativex (1:1, Δ9-tetrahydrocannabinol (THC)/cannabidiol (CBD)) on craving and withdrawal from cannabis among nine community-recruited cannabis-dependent subjects. Methods Participants underwent an 8-week double-blind placebo-controlled trial (an ABACADAE design), with four smoke as usual conditions (SAU) (A) separated by four cannabis abstinence conditions (B–E), with administration of either self-titrated/fixed doses of placebo or Sativex (up to 108 mg THC/100 mg CBD). The order of medication administration during abstinence conditions was randomized and counterbalanced. Withdrawal symptoms and craving were assessed using the Cannabis Withdrawal Scale (CWS), Marijuana Withdrawal Checklist (MWC) and Marijuana Craving Questionnaire (MCQ). Medication use was assessed during the study by means of self-reports, vial weight control, toxicology and metabolite analysis. Cannabis use was assessed by means of self-reports. Results High fixed doses of Sativex were well tolerated and significantly reduced cannabis withdrawal during abstinence, but not craving, as compared to placebo. Self-titrated doses were lower and showed limited efficacy as compared to high fixed doses. Participants reported a significantly lower “high” following Sativex or placebo as compared to SAU conditions. Cannabis/medication use along the study, as per self-reports, suggests compliance with the study conditions. Conclusions The results found in this proof of concept study warrant further systematic exploration of Sativex as a treatment option for cannabis withdrawal and dependence. PMID:26925704

  8. Method for extracting lanthanides and actinides from acid solutions

    DOEpatents

    Horwitz, E. Philip; Kalina, Dale G.; Kaplan, Louis; Mason, George W.

    1985-01-01

    A process for the recovery of actinide and lanthanide values from aqueous acidic solutions with an organic extractant having the formula: ##STR1## where .phi. is phenyl, R.sup.1 is a straight or branched alkyl or alkoxyalkyl containing from 6 to 12 carbon atoms and R.sup.2 is an alkyl containing from 3 to 6 carbon atoms. The process is suitable for the separation of actinide and lanthanide values from fission product values found together in high level nuclear reprocessing waste solutions.

  9. Kinetic Monte Carlo method applied to nucleic acid hairpin folding.

    PubMed

    Sauerwine, Ben; Widom, Michael

    2011-12-01

    Kinetic Monte Carlo on coarse-grained systems, such as nucleic acid secondary structure, is advantageous for being able to access behavior at long time scales, even minutes or hours. Transition rates between coarse-grained states depend upon intermediate barriers, which are not directly simulated. We propose an Arrhenius rate model and an intermediate energy model that incorporates the effects of the barrier between simulated states without enlarging the state space itself. Applying our Arrhenius rate model to DNA hairpin folding, we demonstrate improved agreement with experiment compared to the usual kinetic Monte Carlo model. Further improvement results from including rigidity of single-stranded stacking.

  10. Luminol as a fluorescent acid-base indicator.

    PubMed

    Erdey, L; Buzás, I; Vigh, K

    1966-03-01

    The acid and base dissociation constants of luminol are determined at various ionic strengths. The transition interval occurs at pH 7.7-9.0, therefore luminol is a fluorescent indicator for the titration of strong and weak acids and strong bases. Its value as an indicator is established by titrating milk, red wine and cherry juice.

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

    PubMed

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

    2016-07-01

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

  12. Nonaqueous titration of amino groups in polymeric matrix of plant cell walls.

    PubMed

    Meychik, N R; Nikolaeva, Yu I; Ermakov, I P

    2009-08-01

    Nonaqueous titration was used for detection of free amino groups in the polymeric matrix of plant cell walls. The content of amino groups varied in the range 0.54-0.91 and total nitrogen in the range 1.0-4.2 mmol per gram dry mass of cell walls depending on the plant species. However, these data on the high content of free amino groups do not correlate with the present day concept that the nitrogen fraction in charged amino groups in plant cell wall proteins, which are assumed to be mainly amino groups of lysine and arginine residues, is about 10%. It is supposed that most detected free amino groups belong to the hydroxy-amino acids hydroxyproline and tyrosine that can be bound at the hydroxyl group with the carbohydrate part of glycoprotein or another structural cell wall polymer.

  13. Applications of isothermal titration calorimetry in biophysical studies of G-quadruplexes.

    PubMed

    Pagano, Bruno; Mattia, Carlo Andrea; Giancola, Concetta

    2009-07-02

    G-quadruplexes are higher-order nucleic acids structures formed by G-rich sequences that are stabilized by tetrads of hydrogen-bonded guanine bases. Recently, there has been growing interest in the study of G-quadruplexes because of their possible involvement in many biological processes. Isothermal titration calorimetry (ITC) has been proven to be a useful tool to study the energetic aspects of G-quadruplex interactions. Particularly, ITC has been applied many times to determine the thermodynamic properties of drug-quadruplex interactions to screening among various drugs and to address drug design. In the present review, we will focus on the ITC studies of G-quadruplex structures and their interaction with proteins and drugs and the most significant results will be discussed.

  14. Investigation of amine-buffered amide reagents for coulometric Karl Fischer titration.

    PubMed

    Larsson, William; Cedergren, Anders

    2009-06-15

    Formamide (FA), N-methylformamide (NMF), and dimethylformamide (DMF), were evaluated as solvents for coulometric Karl Fischer (KF) reagents in combination with several amine bases. Except for the effect of the iodine species (iodine or triiodide), the pH of the reagent and the position of the sulfur dioxide/hydrogen sulfite equilibrium were found to be the main factors explaining the large difference in the observed reaction rates between water and the KF reagent in these solvents. Acid-base titrations showed that hydrogen sulfite is the main sulfur reactant in these media. The results will be of great importance in finding suitable combinations of base and solvent with respect to stoichiometry, side reactions caused by active carbonyl compounds, and reagent stability.

  15. Method for high specific bioproductivity of .alpha.,.omega.-alkanedicarboxylic acids

    DOEpatents

    Mobley, David Paul; Shank, Gary Keith

    2000-01-01

    This invention provides a low-cost method of producing .alpha.,.omega.-alkanedicarboxylic acids. Particular bioconversion conditions result in highly efficient conversion of fatty acid, fatty acid ester, or alkane substrates to diacids. Candida tropicalis AR40 or similar yeast strains are grown in a medium containing a carbon source and a nitrogen source at a temperature of 31.degree. C. to 38.degree. C., while additional carbon source is continuously added, until maximum cell growth is attained. Within 0-3 hours of this point, substrate is added to the culture to initiate conversion. An .alpha.,.omega.-alkanedicarboxylic acid made according to this method is also provided.

  16. Determination of Dornic Acidity as a Method to Select Donor Milk in a Milk Bank

    PubMed Central

    Garcia-Lara, Nadia Raquel; Escuder-Vieco, Diana; Chaves-Sánchez, Fernando; De la Cruz-Bertolo, Javier; Pallas-Alonso, Carmen Rosa

    2013-01-01

    Abstract Background Dornic acidity may be an indirect measurement of milk's bacteria content and its quality. There are no uniform criteria among different human milk banks on milk acceptance criteria. The main aim of this study is to report the correlation between Dornic acidity and bacterial growth in donor milk in order to validate the Dornic acidity value as an adequate method to select milk prior to its pasteurization. Materials and Methods From 105 pools, 4-mL samples of human milk were collected. Dornic acidity measurement and culture in blood and McConkey's agar cultures were performed. Based on Dornic acidity degrees, we classified milk into three quality categories: top quality (acidity <4°D), intermediate (acidity between 4°D and 7°D), and milk unsuitable to be consumed (acidity ≥8°D). Spearman's correlation coefficient was used to perform statistical analysis. Results Seventy percent of the samples had Dornic acidity under 4°D, and 88% had a value under 8°D. A weak positive correlation was observed between the bacterial growth in milk and Dornic acidity. The overall discrimination performance of Dornic acidity was higher for predicting growth of Gram-negative organisms. In milk with Dornic acidity of ≥4°D, such a measurement has a sensitivity of 100% for detecting all the samples with bacterial growth with Gram-negative bacteria of over 105 colony-forming units/mL. Conclusions The correlation between Dornic acidity and bacterial growth in donor milk is weak but positive. The measurement of Dornic acidity could be considered as a simple and economical method to select milk to pasteurize in a human milk bank based in quality and safety criteria. PMID:23373435

  17. Dissolution behavior of Caldag lateritic nickel ore subjected to a sequential organic acid leaching method

    NASA Astrophysics Data System (ADS)

    Kursunoglu, Sait; Kaya, Muammer

    2015-11-01

    The dissolution behavior of Caldag lateritic nickel ore subjected to a sequential organic acid leaching method was investigated. The effects of the type of organic acid, acid concentration, leaching time, and leaching temperature on the lateritic nickel ore were examined. Organic acids were used individually prior to sequential leaching. Citric acid was more effective than the other two acids for the selective leaching of nickel and cobalt. An increase in the citric acid concentration negligibly affected the dissolution of the metals, whereas temperature exhibited a strong beneficial effect. Oxalic acid was determined to be the most appropriate organic acid for the second leaching step. After 8 h (4 h + 4 h) of leaching with organic acids (0.5 M citric + 0.5 M oxalic) in sequence at 90°C, 89.63% Ni, 82.89% Co, and 69.63% Fe were leached from the lateritic nickel ore. A sequential citric + oxalic acid leaching method could represent a viable alternative for the dissolution of metals from lateritic nickel ore.

  18. Solution Equilibrium Titration for High-Throughput Affinity Estimation of Unpurified Antibodies and Antibody Fragments.

    PubMed

    Della Ducata, Daniela; Jaehrling, Jan; Hänel, Cornelia; Satzger, Marion; Wolber, Meike; Ostendorp, Ralf; Pabst, Stefan; Brocks, Bodo

    2015-12-01

    The generation of therapeutic antibodies with extremely high affinities down to the low picomolar range is today feasible with state-of-the art recombinant technologies. However, reliable and efficient identification of lead candidates with the desired affinity from a pool of thousands of antibody clones remains a challenge. Here, we describe a high-throughput procedure that allows reliable affinity screening of unpurified immunoglobulin G or antibody fragments. The method is based on the principle of solution equilibrium titration (SET) using highly sensitive electrochemiluminescence as a readout system. Because the binding partners are not labeled, the resulting KD represents a sound approximation of the real affinity. For screening, diluted bacterial lysates or cell culture supernatants are equilibrated with four different concentrations of a soluble target molecule, and unbound antibodies are subsequently quantified on 384-well Meso Scale Discovery (MSD) plates coated with the respective antigen. For determination of KD values from the resulting titration curves, fit models deduced from the law of mass action for 1:1 and 2:1 binding modes are applied to assess hundreds of interactions simultaneously. The accuracy of the method is demonstrated by comparing results from different screening campaigns from affinity optimization projects with results from detailed affinity characterization.

  19. Isoelectric focusing and titration curves in biomedicine and in agrofood industries: a multimedia teaching program.

    PubMed

    Cade-Treyer, D; Cade, A; Darjo, A; Jouvion-Moreno, M

    1996-03-01

    The aim of this 45 min, 60 megabyte, modular program is to initiate students, scientists and engineers of biotechnology, biomedicine and agrofood industries into isoelectric focusing (IEF) and titration curves for analytical (e.g. IEF, zone electrophoresis, isotachophoresis, electrotransfer) and preparative (e.g. ion-exchange chromatography, chromatofocusing) application of charge-dependent methods. For advanced teaching, the following theoretical and practical aspects may be of interest: pH gradient engineering, IEF resolving power, generation of pH gradient, sample-ampholyte interactions, pH gradient drift, immobilized pH gradients (IPG), IPG-two-dimensional (2-D) electrophoresis, preparative methods with multi-compartments and IPG membranes, capillary IEF, isozyme analysis, etc.). The program associates fixed and animated drawings, and computer-assisted simulations, with spoken and written commentaries (in English). It is illustrated with numerous IEF gel patterns and titration curves and some video sequences to be run on a multimedia PC with MS Windows 3.1 (or later releases) as the only software. The linear presentation of the program may be used directly on the PC, or may be projected on a screen from the PC, for small classes or for a larger audience (200 persons). Its development as an interactive multimedia program is in progress and will soon be available on the Internet.

  20. Methods of emulsifying linoleic acid in biohydrogenation studies in vitro may bias the resulting fatty acid profiles.

    PubMed

    Khiaosa-ard, Ratchaneewan; Leiber, Florian; Soliva, Carla R

    2010-07-01

    The effects of three emulsifying methods on ruminal fatty acid biohydrogenation (BH) in vitro were compared. Using a static in-vitro gas test system, four replicates of each treatment were incubated in buffered ruminal fluid. Hemicellulose (300 mg dry matter) was supplemented either with or without linoleic acid (9c12c-18:2, 5% in diet dry matter) and incubated for 4 and 24 h. Three methods of emulsifying 9c12c-18:2 were tested: (1) ethanol, (2) Tween 80, and (3) sonication. The products were then compared to non-emulsified 9c12c-18:2. Out of the three emulsifying methods tested, ethanol and sonication resulted in stable 9c12c-18:2 emulsions, indicating good 9c12c-18:2 distribution, while the Tween 80 emulsion was less stable. BH was strongly inhibited by treating 9c12c-18:2 with ethanol and sonication at different steps of the BH-pathway, resulting in changed concentrations of certain BH intermediates. The fatty acid profile generated from the major BH-pathways of 9c12c-18:2 with Tween 80 was comparable to that without emulsification after 24 h of incubation. We conclude that it is not recommended to emulsify lipids before incubating them in vitro when investigating fatty acid BH. If emulsification of 9c12c-18:2 is necessary, Tween 80 seems to be the method that interferes least with BH.

  1. A Simple Spectrophotometric Method for the Determination of Thiobarbituric Acid Reactive Substances in Fried Fast Foods.

    PubMed

    Zeb, Alam; Ullah, Fareed

    2016-01-01

    A simple and highly sensitive spectrophotometric method was developed for the determination of thiobarbituric acid reactive substances (TBARS) as a marker for lipid peroxidation in fried fast foods. The method uses the reaction of malondialdehyde (MDA) and TBA in the glacial acetic acid medium. The method was precise, sensitive, and highly reproducible for quantitative determination of TBARS. The precision of extractions and analytical procedure was very high as compared to the reported methods. The method was used to determine the TBARS contents in the fried fast foods such as Shami kebab, samosa, fried bread, and potato chips. Shami kebab, samosa, and potato chips have higher amount of TBARS in glacial acetic acid-water extraction system than their corresponding pure glacial acetic acid and vice versa in fried bread samples. The method can successfully be used for the determination of TBARS in other food matrices, especially in quality control of food industries.

  2. Method of making a sealed lead-acid battery with a gel electrolyte and sealed lead-acid storage battery made according to this method

    SciTech Connect

    Chreitzberg, A.M.; Chiacchio, F.J.

    1987-08-18

    A method is described of making a sealed lead-acid storage battery having a plurality of electrodes and a gel electrolyte consisting substantially of sulfuric acid and a gelling agent, comprising the steps of: (a) activating a dry unformed battery by filling the battery with sulfuric acid, (b) maintaining the battery on open circuit or a period of time sufficient to chemically bond sulphuric acid as sulfate to the electrodes and lower the specific gravity of the acid to the desired gelling value, (c) dumping the free acid from the battery, (d) adding a solution of gelling agent and sulfuric acid to fill the battery to the normal formation level, (e) formation charging the battery by applying a constant charge current of 5-16 A/100 Ah for an input of 200-300 Ah/lb. positive active material whereby gelling of the electrolyte is effected, (f) when formation is complete, removing excess liquid, if any, to top of electrodes, and (g) sealing the battery with a pressure relief valve.

  3. Comparison of GC-MS and FTIR methods for quantifying naphthenic acids in water samples.

    PubMed

    Scott, Angela C; Young, Rozlyn F; Fedorak, Phillip M

    2008-11-01

    The extraction of bitumen from the oil sands in Canada releases toxic naphthenic acids into the process-affected waters. The development of an ideal analytical method for quantifying naphthenic acids (general formula C(n)H(2n+Z)O(2)) has been impeded by the complexity of these mixtures and the challenges of differentiating naphthenic acids from other naturally-occurring organic acids. The oil sands industry standard FTIR method was compared with a newly-developed GC-MS method. Naphthenic acids concentrations were measured in extracts of surface and ground waters from locations within the vicinity of and away from the oil sands deposits and in extracts of process-affected waters. In all but one case, FTIR measurements of naphthenic acids concentrations were greater than those determined by GC-MS. The detection limit of the GC-MS method was 0.01 mg L(-1) compared to 1 mg L(-1) for the FTIR method. The results indicated that the GC-MS method is more selective for naphthenic acids, and that the FTIR method overestimates their concentrations.

  4. All-Atom Continuous Constant pH Molecular Dynamics With Particle Mesh Ewald and Titratable Water.

    PubMed

    Huang, Yandong; Chen, Wei; Wallace, Jason A; Shen, Jana

    2016-11-08

    Development of a pH stat to properly control solution pH in biomolecular simulations has been a long-standing goal in the community. Toward this goal recent years have witnessed the emergence of the so-called constant pH molecular dynamics methods. However, the accuracy and generality of these methods have been hampered by the use of implicit-solvent models or truncation-based electrostatic schemes. Here we report the implementation of the particle mesh Ewald (PME) scheme into the all-atom continuous constant pH molecular dynamics (CpHMD) method, enabling CpHMD to be performed with a standard MD engine at a fractional added computational cost. We demonstrate the performance using pH replica-exchange CpHMD simulations with titratable water for a stringent test set of proteins, HP36, BBL, HEWL, and SNase. With the sampling time of 10 ns per replica, most pKa's are converged, yielding the average absolute and root-mean-square deviations of 0.61 and 0.77, respectively, from experiment. Linear regression of the calculated vs experimental pKa shifts gives a correlation coefficient of 0.79, a slope of 1, and an intercept near 0. Analysis reveals inadequate sampling of structure relaxation accompanying a protonation-state switch as a major source of the remaining errors, which are reduced as simulation prolongs. These data suggest PME-based CpHMD can be used as a general tool for pH-controlled simulations of macromolecular systems in various environments, enabling atomic insights into pH-dependent phenomena involving not only soluble proteins but also transmembrane proteins, nucleic acids, surfactants, and polysaccharides.

  5. Methods for immobilizing nucleic acids on a gel substrate

    SciTech Connect

    Mirzabekov, A.D.; Proudnikov, D.Y.; Timofeev, E.N.; Kochetkova, S.V.; Florentiev, V.L.; Shick, V.V.

    1999-11-09

    A method for labeling oligonucleotide molecules, and for immobilizing oligonucleotide and DNA molecules is provided comprising modifying the molecules to create a chemically active group, and contacting activated fluorescent dyes to the region. A method for preparing an immobilization substrate is also provided comprising modifying a gel to contain desired functional groups which covalently interact with certain moieties of the oligonucleotide molecules. A method for immobilizing biomolecules and other molecules within a gel by copolymerization of allyl-substituted oligonucleotides, DNA and proteins with acrylamide is also provided.

  6. Methods for immobilizing nucleic acids on a gel substrate

    DOEpatents

    Mirzabekov, Andrei Darievich; Proudnikov, Dimitri Y.; Timofeev, Edward N.; Kochetkova, Svetlana V.; Florentiev, Vladimir L.; Shick, Valentine V.

    1999-01-01

    A method for labeling oligonucleotide molecules, and for immobilizing oligonucleotide and DNA molecules is provided comprising modifying the molecules to create a chemically active group, and contacting activated fluorescent dyes to the region. A method for preparing an immobilization substrate is also provided comprising modifying a gel to contain desired functional groups which covalently interact with certain moieties of the oligonucleotide molecules. A method for immobilizing biomolecules and other molecules within a gel by copolymerization of allyl-substituted oligonucleotides, DNA and proteins with acrylamide is also provided.

  7. Hydrofluoric acid-resistant composite window and method for its fabrication

    DOEpatents

    Ostenak, C.A.; Mackay, H.A.

    1985-07-18

    A hydrofluoric acid-resistant composite window and method for its fabrication are disclosed. The composite window comprises a window having first and second sides. The first side is oriented towards an environment containing hydrofluoric acid. An adhesive is applied to the first side. A layer of transparent hydrofluoric acid-resistant material, such as Mylar, is applied to the adhesive and completely covers the first side. The adhesive is then cured.

  8. A Nucleic Acid Probe and Method for the Detection of Shigella and Enteroinvasive E. coli Bacteria.

    DTIC Science & Technology

    This invention relates to nucleic acid probes and a method for the rapid detection of Shigella and enteroinvasive Escherichia coli, the causative agents of bacterial dysentery, by use of a nucleic acid hybridization probe, equivalent to a plasmid DNA region encoding one of 4 specific invasion-associated, peptides of all strains of Shigella and enterinvasive E . coli , in a nucleic acid hybridization reaction with a clinical specimen containing dysentery bacteria.

  9. Hydrofluoric acid-resistant composite window and method for its fabrication

    DOEpatents

    Ostenak, Carl A.; Mackay, Harold A.

    1987-01-01

    A hydrofluoric acid-resistant composite window and method for its fabrication are disclosed. The composite window comprises a window having first and second sides. The first side is oriented towards an environment containing hydrofluoric acid. An adhesive is applied to the first side. A layer of transparent hydrofluoric acid-resistant material, such as Mylar, is applied to the adhesive and completely covers the first side. The adhesive is then cured.

  10. Label-Free Determination of the Dissociation Constant of Small Molecule-Aptamer Interaction by Isothermal Titration Calorimetry.

    PubMed

    Vogel, Marc; Suess, Beatrix

    2016-01-01

    Isothermal titration calorimetry (ITC) is a powerful label-free technique to determine the binding constant as well as thermodynamic parameters of a binding reaction and is therefore well suited for the analysis of small molecule-RNA aptamer interaction. We will introduce you to the method and present a protocol for sample preparation and the calorimetric measurement. A detailed note section will point out useful tips and pitfalls.

  11. A novel method for isolating and analyzing organic acids in biological cultures

    SciTech Connect

    Polman, K.

    1995-12-31

    Fermentatively produced organic acids have significant potential as chemical feedstocks for the production of various commodity materials. Such acids include acetic and succinic acids. Fermentations frequently result in the simultaneous production of two or more organic acids, and often other fermentation products as well. This necessitates separation of these products from each other, so that quantification and purification can be achieved. A multitude of methodologies for the identification, purification, and quantitation of organic acids has been developed and described; both liquid and gas chromatography have been used for such separations. High-performance liquid chromatography (HPLC) media used for the separation of organic acids have included C18 columns, Aminex HPX-87H (ion-moderated partition resin), TEAP-Si 100 Polyol (strongly basic anion-exchange resin), Dowex 1 (cation-exchange column), Shodex Ionpak KC811, and others. Methodologies for HPLC analysis of organic acids also vary in these aspects: (1) Sample pretreatment (e.g., pretreatment with Sep-Pak C18 cartridges or with DEAE-Sephadex); (2) Mobile-phase composition (e.g., dilute sulfuric acid or formic acid); and (3) Method of organic acid detection (e.g., refractive index or light absorption). In this study, we present a methodology for isolating and quantifying organic acids found in fermentation broths. The methodology is simple, utilizes dual separation chemistries to effect an enhanced separation capacity, and is durable in terms of HPLC column life.

  12. Graphene oxide for acid catalyzed-reactions: Effect of drying process

    NASA Astrophysics Data System (ADS)

    Gong, H. P.; Hua, W. M.; Yue, Y. H.; Gao, Z.

    2017-03-01

    Graphene oxides (GOs) were prepared by Hummers method through various drying processes, and characterized by XRD, SEM, FTIR, XPS and N2 adsorption. Their acidities were measured using potentiometric titration and acid-base titration. The catalytic properties were investigated in the alkylation of anisole with benzyl alcohol and transesterification of triacetin with methanol. GOs are active catalysts for both reaction, whose activity is greatly affected by their drying processes. Vacuum drying GO exhibits the best performance in transesterification while freezing drying GO is most active for alkylation. The excellent catalytic behavior comes from abundant surface acid sites as well as proper surface functional groups, which can be obtained by selecting appropriate drying process.

  13. Thermal and acid tolerant beta-xylosidases, genes encoding, related organisms, and methods

    DOEpatents

    Thompson, David N.; Thompson, Vicki S.; Schaller, Kastli D.; Apel, William A.; Lacey, Jeffrey A.; Reed, David W.

    2011-04-12

    Isolated and/or purified polypeptides and nucleic acid sequences encoding polypeptides from Alicyclobacillus acidocaldarius and variations thereof are provided. Further provided are methods of at least partially degrading xylotriose and/or xylobiose using isolated and/or purified polypeptides and nucleic acid sequences encoding polypeptides from Alicyclobacillus acidocaldarius and variations thereof.

  14. Thermal and acid tolerant beta xylosidases, arabinofuranosidases, genes encoding, related organisms, and methods

    SciTech Connect

    Thompson, David N; Thompson, Vicki S; Schaller, Kastli D; Apel, William A; Reed, David W; Lacey, Jeffrey A

    2013-04-30

    Isolated and/or purified polypeptides and nucleic acid sequences encoding polypeptides from Alicyclobacillus acidocaldarius and variations thereof are provided. Further provided are methods of at least partially degrading xylotriose, xylobiose, and/or arabinofuranose-substituted xylan using isolated and/or purified polypeptides and nucleic acid sequences encoding polypeptides from Alicyclobacillus acidocaldarius and variations thereof.

  15. Outpatient titration of carbidopa/levodopa enteral suspension (Duopa).

    PubMed

    Pahwa, Rajesh; Lyons, Kelly E

    2017-05-01

    Carbidopa/levodopa enteral suspension (CLES; Duopa) is a suspension or gel formulation of carbidopa/levodopa that is approved by the USA Food and Drug Administration for the treatment of advanced Parkinson's disease patients with motor fluctuations. CLES is delivered at a constant rate continuously throughout the day into the jejunum through an infusion pump via a PEG-J tube implanted surgically. The efficacy of CLES was established in the USA based on a randomized, double-blind, double-dummy, active controlled, parallel group and 12-week study, in which mean daily OFF time was reduced by 4.0 h, compared to 1.9 h with oral immediate release carbidopa/levodopa. The CLES hardware consists of a cassette containing the drug, a pump to deliver the drug and tubing to connect the PEG-J to the pump. It is critical to understand the appropriate conversion of the carbidopa/levodopa daily dosages to the CLES dosage and how to program the pump and titrate CLES to achieve the most effective dose. We describe one methodology for patient selection, outpatient titration and pump programming.

  16. Isothermal titration calorimetry: general formalism using binding polynomials.

    PubMed

    Freire, Ernesto; Schön, Arne; Velazquez-Campoy, Adrian

    2009-01-01

    The theory of the binding polynomial constitutes a very powerful formalism by which many experimental biological systems involving ligand binding can be analyzed under a unified framework. The analysis of isothermal titration calorimetry (ITC) data for systems possessing more than one binding site has been cumbersome because it required the user to develop a binding model to fit the data. Furthermore, in many instances, different binding models give rise to identical binding isotherms, making it impossible to discriminate binding mechanisms using binding data alone. One of the main advantages of the binding polynomials is that experimental data can be analyzed by employing a general model-free methodology that provides essential information about the system behavior (e.g., whether there exists binding cooperativity, whether the cooperativity is positive or negative, and the magnitude of the cooperative energy). Data analysis utilizing binding polynomials yields a set of binding association constants and enthalpy values that conserve their validity after the correct model has been determined. In fact, once the correct model is validated, the binding polynomial parameters can be immediately translated into the model specific constants. In this chapter, we describe the general binding polynomial formalism and provide specific theoretical and experimental examples of its application to isothermal titration calorimetry.

  17. A microfabrication-based approach to quantitative isothermal titration calorimetry.

    PubMed

    Wang, Bin; Jia, Yuan; Lin, Qiao

    2016-04-15

    Isothermal titration calorimetry (ITC) directly measures heat evolved in a chemical reaction to determine equilibrium binding properties of biomolecular systems. Conventional ITC instruments are expensive, use complicated design and construction, and require long analysis times. Microfabricated calorimetric devices are promising, although they have yet to allow accurate, quantitative ITC measurements of biochemical reactions. This paper presents a microfabrication-based approach to integrated, quantitative ITC characterization of biomolecular interactions. The approach integrates microfabricated differential calorimetric sensors with microfluidic titration. Biomolecules and reagents are introduced at each of a series of molar ratios, mixed, and allowed to react. The reaction thermal power is differentially measured, and used to determine the thermodynamic profile of the biomolecular interactions. Implemented in a microdevice featuring thermally isolated, well-defined reaction volumes with minimized fluid evaporation as well as highly sensitive thermoelectric sensing, the approach enables accurate and quantitative ITC measurements of protein-ligand interactions under different isothermal conditions. Using the approach, we demonstrate ITC characterization of the binding of 18-Crown-6 with barium chloride, and the binding of ribonuclease A with cytidine 2'-monophosphate within reaction volumes of approximately 0.7 µL and at concentrations down to 2mM. For each binding system, the ITC measurements were completed with considerably reduced analysis times and material consumption, and yielded a complete thermodynamic profile of the molecular interaction in agreement with published data. This demonstrates the potential usefulness of our approach for biomolecular characterization in biomedical applications.

  18. Using Conductivity Measurements to Determine the Identities and Concentrations of Unknown Acids: An Inquiry Laboratory Experiment

    ERIC Educational Resources Information Center

    Smith, K. Christopher; Garza, Ariana

    2015-01-01

    This paper describes a student designed experiment using titrations involving conductivity measurements to identify unknown acids as being either HCl or H[subscript 2]SO[subscript 4], and to determine the concentrations of the acids, thereby improving the utility of standard acid-base titrations. Using an inquiry context, students gain experience…

  19. Method Optimization of Deoxyribonucleic Acid (DNA) Thin Films for Biotronics

    DTIC Science & Technology

    2011-09-01

    Added to the Spin-coater ......................................................................4 3.3 Comparison of Spin - Coating Speed and Sample...precipitate after centrifugation. ..............................3 Figure 3. Diagram of spin - coating method. First, the DNA-CTMA solution was pipetted onto... spin - coating speeds. ...................................................................................................................6 Figure 5

  20. Method for replicating an array of nucleic acid probes

    DOEpatents

    Cantor, C.R.; Przetakiewicz, M.; Smith, C.L.; Sano, T.

    1998-08-18

    The invention relates to the replication of probe arrays and methods for replicating arrays of probes which are useful for the large scale manufacture of diagnostic aids used to screen biological samples for specific target sequences. Arrays created using PCR technology may comprise probes with 5{prime}- and/or 3{prime}-overhangs. 16 figs.

  1. Method for replicating an array of nucleic acid probes

    DOEpatents

    Cantor, Charles R.; Przetakiewicz, Marek; Smith, Cassandra L.; Sano, Takeshi

    1998-01-01

    The invention relates to the replication of probe arrays and methods for replicating arrays of probes which are useful for the large scale manufacture of diagnostic aids used to screen biological samples for specific target sequences. Arrays created using PCR technology may comprise probes with 5'- and/or 3'-overhangs.

  2. A survey of the year 2002 literature on applications of isothermal titration calorimetry.

    PubMed

    Cliff, Matthew J; Ladbury, John E

    2003-01-01

    Isothermal titration calorimetry (ITC) is becoming widely accepted as a key instrument in any laboratory in which quantification of biomolecular interactions is a requisite. The method has matured with respect to general acceptance and application development over recent years. The number of publications on ITC has grown exponentially over the last 10 years, reflecting the general utility of the method. Here all the published works of the year 2002 in this area have been surveyed. We review the broad range of systems to which ITC is being directed and classify these into general areas highlighting key publications of interest. This provides an overview of what can be achieved using this method and what developments are likely to occur in the near future.

  3. Signal processing with a summing operational amplifier in multicomponent potentiometric titrations.

    PubMed

    Parczewski, A

    1987-06-01

    It has been proved that application of two indicator electrodes connected to the ordinary titration apparatus through an auxiliary electronic device (a summing operational amplifier) significantly extends the scope of multicomponent potentiometric titrations in which the analytes are determined simultaneously from a single titration curve. For each analyte there is a corresponding potential jump on the titration curve. By application of the proposed auxiliary device, the sum of the electrode potentials is measured. The device also enables the relative sizes of the potential jumps at the end-points on the titration curve to be varied. The advantages of the proposed signal processing are exemplified by complexometric potentiometric titrations of Fe(III) and Cu(II) in mixtures, with a platinum electrode and a copper ion-selective electrode as the indicator electrodes.

  4. Fused liposome and acid induced method for liposome fusion

    SciTech Connect

    Huang, L.; Connor, J.

    1988-12-06

    This patent describes a method of fusing liposomes. It comprises: preparing a suspension of liposomes containing at least one lipid which has a tendency to form the inverted hexagonal phase and at least 20 mol percent of palmitoylhomocysteine; and in the absence of externally added divalent cations, proteins or other macromolecules, acidifying the liposome suspension to reduce the pH of the liposomes to below pH 7, such that at least about 20% of the liposomes fuse to one another.

  5. Stress degradation studies and stability-indicating TLC-densitometric method of glycyrrhetic acid

    PubMed Central

    2013-01-01

    Background Glycyrrhetic acid, a pentacyclic triterpenoid, possesses a broad range of pharmacological activities and serves as template to synthesize many bioactive drugs. This paper describes a simple, accurate, and sensitive stability-indicating TLC densitometric method for the determination of glycyrrhetic acid and its degradation product as per the ICH guidelines. Results Separation was carried out on TLC aluminium sheet pre-coated with silica gel 60F254 using chloroform, methanol and formic acid (9:0.9:0.1, v/v). Compact spot for glycyrrhetic acid was found at Rf value of 0.42 ± 0.03. Densitometric analysis was carried out in the absorbance mode at λmax 254 nm. Glycyrrhetic acid was found to be stable to the exposure of base, neutral, oxidation, dry heating treatment and wet heating treatment, but showed degradation under acidic and photochemical conditions. Moreover, fragmentation pattern of glycyrrhetic acid was developed by using a positive ion electrospray ionization quadrupole time-of-flight mass spectrometry (ESI-QqTOF-MS/MS) hybrid instrument. A photo-degraded product was characterized through comparison of mass spectrometric studies with glycyrrhetic acid. Conclusion The developed stability-indicating TLC-densitometric method can be applied for routine analysis of glycyrrhetic acid in the presence of its degradation products. PMID:23327365

  6. Theoretical curves in indicator photometric titration of monodentate polyatomic ligands by metal ions

    SciTech Connect

    Kuznetsov, V.V.; Shamanskii, V.A.

    1986-03-20

    On the basis of the law of mass action and material balance conditions, theoretical equations have been derived for the curves obtained in indicator photometric titration of anionic ligands by metal ions for the cases of formation of complexes ML, M/sub 2/L, and ML/sub 2/. Correspondence between theoretical and experimental titration curves has been demonstrated, thus making it possible to explain the factual material and to use reactions of low-stability complex formation in photometric titrations.

  7. Caprylic acid precipitation method for impurity reduction: an alternative to conventional chromatography for monoclonal antibody purification.

    PubMed

    Brodsky, Yan; Zhang, Cheng; Yigzaw, Yinges; Vedantham, Ganesh

    2012-10-01

    We report the use of caprylic acid based impurity precipitation as (1) an alternative method to polishing chromatography techniques commonly used for monoclonal antibody purification and (2) an impurity reduction step prior to harvesting the bioreactor. This impurity reduction method was tested with protein A purified antibodies and with cell culture fluid. First, the operational parameters influencing precipitation of host cell proteins and high molecular weight aggregate in protein A pools were investigated. When used as a polishing step, the primary factor affecting purification and yield was determined to be pH. Caprylic acid precipitation was comparable to polishing IEX chromatography in reducing host cell protein and aggregate levels. A virus reduction study showed complete clearance of a model retrovirus during caprylic acid precipitation of protein A purified antibody. Caprylic acid mediated impurity precipitation in cell culture showed that the impurity clearance was generally insensitive to pH and caprylic acid concentration whereas yield was a function of caprylic acid concentration. Protein A purification of caprylic acid precipitated cell culture fluid generated less turbid product pool with reduced levels of host cell proteins and high molecular weight aggregate. The results of this study show caprylic acid precipitation to be an effective purification method that can be incorporated into a production facility with minimal cost as it utilizes existing tanks and process flow. Eliminating flow through chromatography polishing step can provide process intensification by avoiding the process tank volume constraints for high titer processes.

  8. HPLC method for amino acids profile in biological fluids and inborn metabolic disorders of aminoacidopathies.

    PubMed

    Babu, S V Suresh; Shareef, M M; Shetty, A Pavan Kumar; Shetty, K Taranath

    2002-07-01

    Quantification of total and individual amino acids in biological fluids such as plasma, urine and cerebrospinal fluid has an important diagnostic implication in laboratory medicine. The present paper describes protocols for the assay of total amino acids by modified method based on dinitrophenyl and HPLC profile involving pre-column derivatization with o-pthalaldehyde (OPA) derivatization, respectively. The method, based on the alkylation of-SH groups prior to OPA derivatization of amino acids followed by reverse phase high performance liquid chromatography, provide a comprehensive profile of more than twenty amino acids (including-SH group containing) in a single run lasting about 45 minutes. The present study, apart from establishing the normal profile of amino acids in plasma of Indian sub population, also presents HPLC profile for some of the rare amino acidopathies.

  9. Development of a Rapid and Confirmatory Method to Identify Ganoderic Acids in Ganoderma Mushrooms

    PubMed Central

    Qi, Ying; Zhao, Lingling; Sun, Hao H.

    2012-01-01

    To examine the composition of lanostanoids in Ganoderma lucidum, we have developed a liquid chromatography–mass spectrometry (LC–MS) method by using the ganoderic acids isolated in our laboratory as reference standards. The identity of 14 peaks in the high performance liquid chromatogram (HPLC) of G. lucidum has been confirmed. By using the HPLC retention times of these ganoderic acids and their mass fragmentation patterns established in this paper, one can use LC–MS to analyze G. lucidum without requiring the reference standards of these 14 ganoderic acids. Subsequently, only the HPLC–UV method would be needed to analyze routine samples of G. lucidum. PMID:22586399

  10. Closed cycle ion exchange method for regenerating acids, bases and salts

    DOEpatents

    Dreyfuss, Robert M.

    1976-01-01

    A method for conducting a chemical reaction in acidic, basic, or neutral solution as required and then regenerating the acid, base, or salt by means of ion exchange in a closed cycle reaction sequence which comprises contacting the spent acid, base, or salt with an ion exchanger, preferably a synthetic organic ion-exchange resin, so selected that the counter ions thereof are ions also produced as a by-product in the closed reaction cycle, and then regenerating the spent ion exchanger by contact with the by-product counter ions. The method is particularly applicable to closed cycle processes for the thermochemical production of hydrogen.

  11. Convenient method of simultaneously analyzing aluminum and magnesium in pharmaceutical dosage forms using californium-252 thermal neutron activation.

    PubMed

    Landolt, R R; Hem, S L

    1983-05-01

    A commercial antacid suspension containing aluminum hydroxide and magnesium hydroxide products was used as a model sample to study the use of a californium-252 thermal neutron activation as a method for quantifying aluminum content as well as for the simultaneous assay of aluminum and magnesium. A 3.5-micrograms californium-252 source was used for the activation, and the induced aluminum-28 and magnesium-27 activity was simultaneously measured by sodium iodide crystal gamma-ray spectrometry using dual single-channel analyzers and scalers. The antacid suspension was contained in a chamber designed with the unique capability of serving as the container for counting the induced radioactivity in addition to being the irradiation chamber itself. Ten replicate irradiations were performed, and the precision was compared with 10 replicate analyses of the antacid suspension using the official ethylenediaminetetraacetic acid titration method. For aluminum the precision was 1.4 versus 0.62% for the titration method. For the magnesium the precision was 5.3 versus 0.79% for the titration method. This pilot study demonstrated that use of more intense californium-252 sources, which are commonly available, would provide a method that is competitive with the ethylenediaminetetraacetic acid titration method in precision and in other aspects as well.

  12. Determination of chemical oxygen demand (COD) using ultrasound digestion and oxidation-reduction potential-based titration.

    PubMed

    Kim, Hyunook; Lim, Honglae; Colosimo, Mark F

    2007-09-01

    A new method for determining wastewater chemical oxygen demand (COD) using ultrasonic digestion and titration based on oxidation reduction potential (ORP) was developed. COD values of potassium hydrogen phthalate solution obtained by ultrasonic digestion were well matched with those obtained using Standard Methods. When applied to determine COD of real wastewater collected from a local treatment plant, results from the new method were within 80% to 90% of those obtained using Standard Methods. Nonetheless, the proposed strategy has the potential to be implemented into an online COD analyzing system.

  13. Sensitivity of the acid-base properties of clays to the methods of preparation and measurement. 1. Literature review.

    PubMed

    Duc, Myriam; Gaboriaud, Fabien; Thomas, Fabien

    2005-09-01

    Measuring and modeling the surface charge of clays, and more especially smectites, has become an important issue in the use of bentonites as a waste confinement material aimed at retarding migration of water and solutes. Therefore, many studies of the acid-base properties of montmorillonite have appeared recently in the literature, following older studies principally devoted to cation exchange. It is striking that beyond the consensus about the complex nature of the surface charge of clays, there are many discrepancies, especially concerning the dissociable charge, that prevents intercomparison among the published data. However, a general trend is observed regarding the absence of common intersection point on raw titration curves at different ionic strengths. Analysis of the literature shows that these discrepancies originate from the experimental procedures for the preparation of the clays and for the quantification of their surface charge. The present work is an attempt to understand how these procedures can impact the final results. Three critical operations can be identified as having significant effects on the surface properties of the studied clays. The first one is the preparation of purified clay from the raw material: the use of acid or chelation treatments, and the repeated washings in deionized water result in partial dissolution of the clays. Then storage of the purified clay in dry or wet conditions strongly influences the equilibria in the subsequent experiments respectively by precipitation or enhanced dissolution. The third critical operation is the quantification of the surface charge by potentiometric titration, which requires the use of strong acids and bases. As a consequence, besides dissociation of surface sites, many secondary titrant consuming reactions were described in the literature, such as cation exchange, dissolution, hydrolysis, or precipitation. The cumulated effects make it difficult to derive proper dissociation constants, and to

  14. Graft polymerization of acrylic acid and methacrylic acid onto poly(vinylidene fluoride) powder in presence of metallic salt and sulfuric acid

    NASA Astrophysics Data System (ADS)

    Deng, Bo; Yu, Yang; Zhang, Bowu; Yang, Xuanxuan; Li, Linfan; Yu, Ming; Li, Jingye

    2011-02-01

    Poly(vinylidene fluoride) (PVDF) powder was grafted with acrylic acid (AAc) or methacrylic acid (MAA) by the pre-irradiation induced graft polymerization technique. The presence of graft chains was proven by FT-IR spectroscopy. The degree of grafting (DG) was calculated by the acid-base back titration method. The synergistic effect of acid and Mohr's salt on the grafting kinetics was examined. The results indicated that adding sulfuric acid and Mohr's salt simultaneously in AAc or MAA solutions led to a strong enhancement in the degree of grafting. The grafted PVDF powder was cast into microfiltration (MF) membranes using the phase inversion method and some properties of the obtained MF membranes were characterized.

  15. Improved gas chromatography-flame ionization detector analytical method for the analysis of epoxy fatty acids.

    PubMed

    Mubiru, Edward; Shrestha, Kshitij; Papastergiadis, Antonios; De Meulenaer, Bruno

    2013-11-29

    In this study an improved method for analysis of epoxy fatty acids is reported. Data obtained from analysis of polar fatty acids has previously been presented, but due to the high number of compounds that co-elute in the polar fraction, the resultant chromatograms are complex which may lead to compromising the accuracy of the data. A three steps separation of fatty acid methyl esters (FAMEs) by solid-phase extraction (SPE) on a silica gel column to remove hydroxy fatty acid interferences was proposed. This approach is opposed to a two step separation procedure that has been often used to prevent analytical interferences caused by non-altered fatty acids. A gas chromatograph with a flame ionization detector (GC-FID) equipped with a polar CP-Sil 88™ column was used. Quantification was based on the use of methyl nonadecanoate (C19:0), as an internal standard. Individual mono epoxy fatty acids were well separated without co-eluting compounds. The optimized method was finally applied to screen epoxy fatty acids in 37 fresh oil samples. Results obtained for the total epoxy fatty acids were in the range 0.03-2mgg(-1) of oil with repeatability coefficient of variation (CV) ranging from 2.8 to 9.9% for duplicate analysis showing that the results obtained are repeatable.

  16. [New method of near infrared spectra analysis for the content of acid soluble lignin of Acacia].

    PubMed

    Liu, Sheng

    2014-01-01

    The near infrared spectra analysis model of the content of the acid soluble lignin and the model of the content of the Klason lignin were built by the iterative method separately at first. The results show that the prediction effect of the content of the Klason lignin is obviously better than that of the acid soluble lignin. Different from usual methods of building near infrared spectra analysis model, the approximate linear relation between the contents of the acid soluble lignin and the contents of the Klason lignin was used. Combined with the near infrared spectroscopy data of multi-wavelength, twenty sub models of prediction of the content of the acid soluble lignin were built with the help of the Klason lignin content whose prediction effect is better than that of the acid soluble lignin. By calculating the weighted mean value of the prediction values of these sub models, the new prediction value of the content of the acid soluble lignin of each acacia specimen was obtained at last. The prediction error of the new model is obviously less than that of the model built by the iterative method. It is possible that the method of modeling in the paper can be used to some chemical component contents when the predictions of them by usual methods are not very effective, and the effects of the near infrared spectra analysis of them will be improved.

  17. A hydrophilic interaction chromatography-tandem mass spectrometry method for amino acid profiling in mussels.

    PubMed

    Tsochatzis, Emmanouil D; Begou, Olga; Gika, Helen G; Karayannakidis, Panayotis D; Kalogiannis, Stavros

    2017-03-15

    A UHPLC-HILIC-tandem MS method has been developed and validated for the quantification of 21 amino acids (20 protein amino acids and cystine) in their free form (FAA) and as protein constituents (total amino acids, TAA) in a rich protein food matrix such as lyophilized mussels (Mytilus galloprovincialis) samples. FAA were analyzed after suspending the samples in the presence of trichloroacetic acid in order to prevent dissolving the proteins, while TAA were determined after acid hydrolysis with 6M HCl in the presence of 4% v/v thioglycolic acid as a reducing agent. In hydrolysed samples 17 amino acids could be determined since tryptophan, cysteine, cystine and asparagine were degraded during acid hydrolysis. Linear regression coefficients (R(2)) were above 0.99 for all amino acids. Accuracy and precision, expressed as recovery (%) and relative standard deviation (RSD, %) were in acceptable levels, ranging from 78.2 to 123.3% and below 15%, respectively for both FAA and TAA. Uncertainty was also below 12% for FAA and below 22% for TAA. Sensitivity of the method was high with LOD values ranging from 0.003 to 0.034g/100g for FAA and 0.001 to 0.004g/100g for TAA, while LOQ ranged from 0.009 to 0.104g/100g for FAA and 0.002 to 0.011g/100g for TAA. The method proved to be a fast and reliable tool for acquiring information on free and total amino acids profile in high protein content foodstuffs such as mussels.

  18. A new end-point for ELISA titrations.

    PubMed

    Vidal, José

    2004-01-01

    This report describes a new ELISA procedure based on end-point titrations. This end-point ELISA takes advantage of the change of color intensity that occurs when peroxidase-containing wells of an ELISA plate are revealed with diaminobenzidine-nickel and further intensification with silver: as antibody concentration and, therefore, peroxidase concentration, decreased, the color became stronger in some wells and, afterwards (i.e., at lower antibody and peroxidase concentrations), the color faded toward clear background. It is proposed that the reciprocal of the sample dilution at which the color intensifies can be used as a measure of the sample antibody content. This report verifies the validity and precision of that procedure.

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

    NASA Astrophysics Data System (ADS)

    Sowa, S.; Kondo, A. E.

    2003-05-01

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

  20. Ultrasensitivity by Molecular Titration in Spatially Propagating Enzymatic Reactions

    PubMed Central

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

    2013-01-01

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

  1. Analysis of an Oxygen Bleach: A Redox Titration Lab

    NASA Astrophysics Data System (ADS)

    Copper, Christine L.; Koubek, Edward

    2001-05-01

    An experiment is presented which allows students to balance an oxidation-reduction reaction equation and use the reaction to analyze a consumer product. The experiment calls for students to balance the reaction of H2O2 and MnO4- two different ways (one assuming that H2O2 is the oxygen source and a second assuming that MnO4- is the oxygen source). They then determine which of these balanced equations has the correct stoichiometry by titrating a standard H2O2 solution with KMnO4. Finally, they use the correct balanced equation to determine the mass percent of H2O2 in a commercially available, "environmentally friendly" oxygen bleach solution.

  2. Isothermal titration calorimetry of ion-coupled membrane transporters.

    PubMed

    Boudker, Olga; Oh, SeCheol

    2015-04-01

    Binding of ligands, ranging from proteins to ions, to membrane proteins is associated with absorption or release of heat that can be detected by isothermal titration calorimetry (ITC). Such measurements not only provide binding affinities but also afford direct access to thermodynamic parameters of binding--enthalpy, entropy and heat capacity. These parameters can be interpreted in a structural context, allow discrimination between different binding mechanisms and guide drug design. In this review, we introduce advantages and limitations of ITC as a methodology to study molecular interactions of membrane proteins. We further describe case studies where ITC was used to analyze thermodynamic linkage between ions and substrates in ion-coupled transporters. Similar type of linkage analysis will likely be applicable to a wide range of transporters, channels, and receptors.

  3. Isothermal titration calorimetry of membrane proteins - progress and challenges.

    PubMed

    Rajarathnam, Krishna; Rösgen, Jörg

    2014-01-01

    Integral membrane proteins, including G protein-coupled receptors (GPCR) and ion channels, mediate diverse biological functions that are crucial to all aspects of life. The knowledge of the molecular mechanisms, and in particular, the thermodynamic basis of the binding interactions of the extracellular ligands and intracellular effector proteins is essential to understand the workings of these remarkable nanomachines. In this review, we describe how isothermal titration calorimetry (ITC) can be effectively used to gain valuable insights into the thermodynamic signatures (enthalpy, entropy, affinity, and stoichiometry), which would be most useful for drug discovery studies, considering that more than 30% of the current drugs target membrane proteins. This article is part of a Special Issue entitled: Structural and biophysical characterisation of membrane protein-ligand binding.

  4. Microextraction method of medium and long chain fatty acids from milk.

    PubMed

    Añorve-Morga, Javier; Castañeda-Ovando, Araceli; Cepeda-Saez, Alberto; Archibold, Armando Durant; Jaimez-Ordaz, Judith; Contreras-López, Elizabeth; González-Olivares, Luis Guillermo; Rodríguez-Rodríguez, José Luis

    2015-04-01

    The aim of this research was to develop a method for microextraction and quantification of long and medium chain fatty acids from milk. The proposed method was carried out on three steps: (1) lipids extraction from 10 μL of whole or skimmed milk containing omega-3 fatty acids (FAs) during 12, 24, 48, 72 and 96 h, in 2 mL chloroform: methanol mixture (2:1); (2) acid methylation of FAs; and (3) quantification of FAs methyl esters by gas chromatography. Using this method, the percentage recovery of FAs was higher (67% for whole and 85% for skimmed milk) compared with AOAC method 905.02 recovery (49% and 83%, respectively). Good reproducibility and repeatability (<3%) were obtained. The method developed can be useful for researching and in routine quality control. Additionally, it is simpler, faster and cheaper than the reference procedure since it requires minimum sample and solvents volume as well as fewer steps.

  5. Effects of calcium phosphate precipitation method on acid resistance to apatite powder and bovine tooth.

    PubMed

    Suge, Toshiyuki; Kawasaki, Akiko; Ishikawa, Kunio; Matsuo, Takashi; Ebisu, Shigeyuki

    2008-07-01

    The aims of this study were to evaluate the effects of CPP method on the crystallinity of apatite powder and on the acid resistance of bovine enamel. Crystallinity degrees of apatite powder before and after CPP treatment were measured by powder X-ray diffraction analysis. Polished bovine enamel specimens treated with CPP method or NaF were immersed in a lactic acid solution for up to five days. The demineralized depth of enamel was measured with a surface roughness analyzer. XRD peaks became sharper after the CPP treatment, indicating an increased crystallinity of the apatite powder. The demineralized depth of bovine enamel treated with CPP method was shallower than that of enamel treated with NaF. Results of this study revealed that the CPP method increased the crystallinity of apatite powder and the acid resistance of enamel. Therefore, the CPP method would be useful not only for treating dentin hypersensitivity, but also for the prevention of dental caries.

  6. Real-time PCR-based infectivity assay for the titration of turkey hemorrhagic enteritis virus, an adenovirus, in live vaccines.

    PubMed

    Mahsoub, Hassan M; Evans, Nicholas P; Beach, Nathan M; Yuan, Lijuan; Zimmerman, Kurt; Pierson, Frank W

    2017-01-01

    The current in vitro titration method for turkey hemorrhagic enteritis virus (THEV) is the end-point dilution assay (EPD) in suspension cell culture (CC). This assay is subjective and results in high variability among vaccine lots. In this study, a new in vitro infectivity method combining a SYBR Green I-based qPCR assay and CC was developed for titration of live hemorrhagic enteritis (HE) CC vaccines. The qPCR was used to determine the virus genome copy number (vGCN) of the internalized virus particles following inoculation of susceptible RP19 cells with 1 vaccine label dose. The measured vGCN represents the number of infectious viral particles (IVP) per 1 dose. This method was used to compare 9 vaccine lots from 3 companies in the United States. Significant lot-to-lot variations within the same company and among the various companies were found in genomic and qPCR-based infectious titer per label dose. A positive linear relationship was found between qPCR infectious titer and genomic titer. Further, considerable variations in CCID50 titers were found among tested vaccine lots, indicating the high variability of the current titration methods. The new method provides an alternative to classical titration assays and can help reduce variation among HE vaccine products.

  7. Characterization of relative abundance of lactic acid bacteria species in French organic sourdough by cultural, qPCR and MiSeq high-throughput sequencing methods.

    PubMed

    Michel, Elisa; Monfort, Clarisse; Deffrasnes, Marion; Guezenec, Stéphane; Lhomme, Emilie; Barret, Matthieu; Sicard, Delphine; Dousset, Xavier; Onno, Bernard

    2016-12-19

    In order to contribute to the description of sourdough LAB composition, MiSeq sequencing and qPCR methods were performed in association with cultural methods. A panel of 16 French organic bakers and farmer-bakers were selected for this work. The lactic acid bacteria (LAB) diversity of their organic sourdoughs was investigated quantitatively and qualitatively combining (i) Lactobacillus sanfranciscensis-specific qPCR, (ii) global sequencing with MiSeq Illumina technology and (iii) molecular isolates identification. In addition, LAB and yeast enumeration, pH, Total Titratable Acidity, organic acids and bread specific volume were analyzed. Microbial and physico-chemical data were statistically treated by Principal Component Analysis (PCA) and Hierarchical Ascendant Classification (HAC). Total yeast counts were 6 log10 to 7.6 log10CFU/g while LAB counts varied from 7.2 log10 to 9.6 log10CFU/g. Values obtained by L. sanfranciscensis-specific qPCR were estimated between 7.2 and 10.3 log10CFU/g, except for one sample at 4.4 log10CFU/g. HAC and PCA clustered the sixteen sourdoughs into three classes described by their variables but without links to bakers' practices. L. sanfranciscensis was the dominant species in 13 of the 16 sourdoughs analyzed by Next Generation Sequencing (NGS), by the culture dependent method this species was dominant only in only 10 samples. Based on isolates identification, LAB diversity was higher for 7 sourdoughs with the recovery of L. curvatus, L. brevis, L. heilongjiangensis, L. xiangfangensis, L. koreensis, L. pontis, Weissella sp. and Pediococcus pentosaceus, as the most representative species. L. koreensis, L. heilongjiangensis and L. xiangfangensis were identified in traditional Asian food and here for the first time as dominant in organic sourdough. This study highlighted that L. sanfranciscensis was not the major species in 6/16 sourdough samples and that a relatively high LAB diversity can be observed in French organic sourdough.

  8. Substituent effects on axle binding in amide pseudorotaxanes: comparison of NMR titration and ITC data with DFT calculations.

    PubMed

    Kaufmann, Lena; Dzyuba, Egor V; Malberg, Friedrich; Löw, Nora L; Groschke, Matthias; Brusilowskij, Boris; Huuskonen, Juhani; Rissanen, Kari; Kirchner, Barbara; Schalley, Christoph A

    2012-08-14

    The binding behaviour of differently substituted diamide axle molecules to Hunter/Vögtle tetralactam macrocycles was studied with a combination of NMR titration, isothermal titration calorimetry (ITC) experiments and calculations employing density functional theory (DFT), along with dispersion-corrected exchange-correlation functionals. Guests with alkyl or alkenyl chains attached to the diamide carbonyl groups have a significantly higher binding affinity to the macrocycle than guests with benzoyl amides and their substituted analogues. While the binding of the benzoyl and alkenyl substituted axles is enthalpically driven, the alkyl-substituted guest binds mainly because of a positive binding entropy. The electronic effects of para-substituents at the benzoyl moieties have an influence on the binding affinities. Electron donating substituents increase, while electron-withdrawing substituents decrease the binding energies. The binding affinities obtained from both NMR titration and ITC experiments correlate well with each other. The substituent effects observed in the experimental data are reflected in adiabatic interaction energies calculated with density functional methods. The calculated structures also agree well with pseudorotaxane crystal structures.

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

    PubMed

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

    2006-01-01

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

  10. Penta- and hexa-coordinate ferric hemoglobins display distinct pH titration profiles measured by Soret peak shifts.

    PubMed

    Uppal, Sheetal; Kumar, Amit; Shandilya, Manish; Mukhi, Nitika; Singh, Amit Kumar; Kateriya, Suneel; Kaur, Jagreet; Kundu, Suman

    2016-10-01

    Hemoglobins with diverse characteristics have been identified in all kingdoms of life. Their ubiquitous presence indicates that these proteins play important roles in physiology, though function for all hemoglobins are not yet established with certainty. Their physiological role may depend on their ability to bind ligands, which in turn is dictated by their heme chemistry. However, we have an incomplete understanding of the mechanism of ligand binding for these newly discovered hemoglobins and the measurement of their kinetic parameters depend on their coordination at the heme iron. To gain insights into their functional role, it is important to categorize the new hemoglobins into either penta- or hexa-coordinated varieties. We demonstrate that simple pH titration and absorbance measurements can determine the coordination state of heme iron atom in ferric hemoglobins, thus providing unambiguous information about the classification of new globins. This method is rapid, sensitive and requires low concentration of protein. Penta- and hexa-coordinate hemoglobins displayed distinct pH titration profiles as observed in a variety of hemoglobins. The pentacoordinate distal histidine mutant proteins of hexacoordinate hemoglobins and ligand-bound hexacoordinate forms of pentacoordinate hemoglobins reverse the pH titration profiles, thus validating the sensitivity of this spectroscopic technique.

  11. Dose-Titrated Vasopressin V2 Receptor Antagonist Improves Renoprotection in a Mouse Model for Autosomal Dominant Polycystic Kidney Disease

    PubMed Central

    Zittema, Debbie; Versteeg, Irina B.; Gansevoort, Ron T.; van Goor, Harry; de Heer, Emile; Veraar, Kimberley A.M.; Peters, Dorien J.M.; Meijer, Esther

    2016-01-01

    Background In autosomal dominant polycystic kidney disease, renoprotective treatment with a vasopressin V2 receptor antagonist (V2RA) is given in a fixed dose (FD). Disease progression and drug habituation could diminish treatment efficacy. We investigated whether the renoprotective effect of the V2RA can be improved by dose titration of the V2RA aiming to maintain aquaresis at a high level. Methods The V2RA OPC-31260 was administered to Pkd1-deletion mice in an FD (0.1%) or in a titrated dose (TD, up to 0.8% when drinking volume dropped). Total kidney weight (TKW) and cyst ratio were investigated and compared to non-treated Pkd1-deletion mice. Treatment was started early or late (21 or 42 days postnatal). Results Water intake was significantly higher throughout the experiment in the TD compared to the FD group. FD treatment that was initiated early reduced TKW and cyst ratio but lost its renoprotective effect later during the experiment. In contrast, TD treatment was able to maintain the renoprotective effect. TD treatment, however, was also associated with a higher early termination rate in comparison with FD treatment. Late start of treatment (FD or TD) did not show a renoprotective effect. Conclusions Titration of a V2RA aimed to maintain aquaresis at a high level showed a better renoprotective effect compared to FD administration. However, this treatment regimen was poorly tolerated and did not overcome treatment unresponsiveness when started later in the disease. PMID:27578560

  12. Method for determination of fatty acids in bovine colostrum using GC-FID.

    PubMed

    Yurchenko, S; Sats, A; Poikalainen, V; Karus, A

    2016-12-01

    Bovine colostrum is potentially valuable source of essential fatty acids (FAs), but so far only few studies have made the effort to estimate FA composition of this potential resource. The aim of current research was to fill this gap with selecting and validating an accurate procedure for the analysis of the composition of the FAs in bovine colostrum. We used colostrum samples of Holstein-Friesian cattle from Märja experimental farm as a test material. The validated method includes derivatization, in which FAs are sent through esterification with the acidic catalyst boron trifluoride. Formed methyl esters of fatty acids (FAMEs) were analysed using GC-FID. The obtained LOD and the LOQ of FAMEs were 0.11-0.68 and 0.37-2.27ppm, respectively. The analysis of fortified samples showed very good and similar recoveries, indicating that the method proposed here can be routinely used for determination and investigation of the fatty acids in dairy products.

  13. Enantiomer labelling, a method for the quantitative analysis of amino acids.

    PubMed

    Frank, H; Nicholson, G J; Bayer, E

    1978-12-21

    Enantiomer labelling a method for the quntitative analysis of optically active natural compounds by gas chromatography, involves the use of the unnatural enantiomer as an internal standard. With Chirasil-Val, a chiral stationary phase that is thermally stable up to up to 240 degrees, the enantiomers of amino acids and a variety of other compounds can be separated and quantitated. Incomplete recovery from the sample, incomplete derivatization, hydrolysis and thermal decomposition of the derivative and shifting response factors can be compensated for by adding the unnatural enantiomer. The accuracy of amino acid analysis by enantiomer labelling is equal or superior to that of hitherto known methods. The procedure affords a complete analysis of peptides with respect to both amino acid composition and the optical purity of each amino acid.

  14. Spectrophotometric method for determination and kinetics of amino acids through their reaction with syringaldehyde

    NASA Astrophysics Data System (ADS)

    Medien, H. A. A.

    1998-02-01

    A spectrophotometric method is described for the determination of amino acids. The method is based on the reaction between amino acids and syringaldehyde at pH 9.0, by which a color is developed with maximum absorption at 420 nm in aqueous methyl alcohol. The absorption of the product obeys Beer's law within the concentration range of 0.025-0.5 mM of original amino acid. The kinetics of the reaction follows overall second order kinetics, first order in each of the reactants. The rates of the reaction were investigated as a function of pH of the reaction medium and structure of the amino compounds. Logarithms of the second-order rate constants increased with amino acid anion concentration as the pH was increased. The mechanisms of the reaction have been discussed.

  15. A method for analysis of vanillic acid in polar ice cores

    NASA Astrophysics Data System (ADS)

    Grieman, M. M.; Greaves, J.; Saltzman, E. S.

    2015-02-01

    Biomass burning generates a wide range of organic compounds that are transported via aerosols to the polar ice sheets. Vanillic acid is a product of conifer lignin combustion, which has previously been observed in laboratory and ambient biomass burning aerosols. In this study a method was developed for analysis of vanillic acid in melted polar ice core samples. Vanillic acid was chromatographically separated using reversed-phase liquid chromatography (HPLC) and detected using electrospray ionization-triple quadrupole mass spectrometry (ESI-MS/MS). Using a 100 μL injection loop and analysis time of 4 min, we obtained a detection limit of 77 ppt (parts per trillion by mass) and an analytical precision of ±10%. Measurements of vanillic acid in Arctic ice core samples from the Siberian Akademii Nauk core are shown as an example application of the method.

  16. Methods and kits for nucleic acid analysis using fluorescence resonance energy transfer

    DOEpatents

    Kwok, Pui-Yan; Chen, Xiangning

    1999-01-01

    A method for detecting the presence of a target nucleotide or sequence of nucleotides in a nucleic acid is disclosed. The method is comprised of forming an oligonucleotide labeled with two fluorophores on the nucleic acid target site. The doubly labeled oligonucleotide is formed by addition of a singly labeled dideoxynucleoside triphosphate to a singly labeled polynucleotide or by ligation of two singly labeled polynucleotides. Detection of fluorescence resonance energy transfer upon denaturation indicates the presence of the target. Kits are also provided. The method is particularly applicable to genotyping.

  17. Methods of staining target chromosomal DNA employing high complexity nucleic acid probes

    DOEpatents

    Gray, Joe W.; Pinkel, Daniel; Kallioniemi, Ol'li-Pekka; Kallioniemi, Anne; Sakamoto, Masaru

    2006-10-03

    Methods and compositions for staining based upon nucleic acid sequence that employ nucleic acid probes are provided. Said methods produce staining patterns that can be tailored for specific cytogenetic analyses. Said probes are appropriate for in situ hybridization and stain both interphase and metaphase chromosomal material with reliable signals. The nucleic acid probes are typically of a complexity greater than 50 kb, the complexity depending upon the cytogenetic application. Methods and reagents are provided for the detection of genetic rearrangements. Probes and test kits are provided for use in detecting genetic rearrangements, particularly for use in tumor cytogenetics, in the detection of disease related loci, specifically cancer, such as chronic myelogenous leukemia (CML), retinoblastoma, ovarian and uterine cancers, and for biological dosimetry. Methods and reagents are described for cytogenetic research, for the differentiation of cytogenetically similar but genetically different diseases, and for many prognostic and diagnostic applications.

  18. Study of acid diffusion behaves form PAG by using top coat method

    NASA Astrophysics Data System (ADS)

    Sekiguchi, Atsushi; Matsumoto, Yoko

    2014-03-01

    Our past research on measurements of simulation parameters for ArF resists focused on establishing methods for measuring the following parameters:[1]-[4] • Development parameters[1] • PEB parameters[2] • Dill's ABC parameters[3] • Quencher parameter[4] We entered these parameters into a lithography simulator and performed ArF resist simulations.We then explored ways to optimize the ArF resist material and process. This paper reports on our study of methods for measuring the diffusion length of acid generated from PAG during exposures. In our experiment, we applied a PAG-containing top coat (TC) material (second layer) to a PAG-free ArF resist (first layer), then performed the exposure and PEB processes. The acid generated in the TC during the exposure diffused into the ArF resist in the lower layer (first layer) when PEB was performed. The process of developing this sample removed the TC in the second layer and the parts of the first layer into which the acid had diffused.We obtained the acid diffusion length based on the quantity of film removed by the development. We calculated the acid diffusion coefficient after varying the exposure value and repeating the measurement. For this report, we also performed measurements to determine how differences in PAG anion size, amount of quencher additive, and PEB temperature affected the acid diffusion coefficient.We entered the measurements obtained into the PROLITH simulator and explored the effects of acid diffusion on pattern profile.

  19. An HPLC method for the determination of selected amino acids in human embryo culture medium.

    PubMed

    Drábková, Petra; Andrlová, Lenka; Kanďár, Roman

    2017-02-01

    A method for the determination of selected amino acids in culture medium using HPLC with fluorescence detection is described. Twenty hours after intra-cytoplasmic sperm injection, one randomly selected zygote was transferred to the culture medium. After incubation (72 h after fertilization), the culture medium in which the embryo was incubated and blank medium was immediately stored at -80°C. Filtered medium samples were derivatized with ortho-phthalaldehyde (naphthalene-2,3-dicarboxaldehyde), forming highly fluorescent amino acids derivatives. Reverse-phase columns (LichroCART, Purospher STAR RP18e or Ascentis Express C18 ) were used for the separation. The derivatives were analyzed by gradient elution with a mobile phase containing ethanol and sodium dihydrogen phosphate. The analytical performance of this method is satisfactory for all amino acids; the intra-assay coefficients of variation were <10% and quantitative recoveries were between 95.5 and 104.4%. Changes in the levels of selected amino acids before and after human embryo cultivation were observed. After embryo incubation, the levels of all amino acids in the medium were increased, apart from aspartate and asparagine. After the cultivation of some embryos, amino acids which were not part of the medium were detected. Low amino acids turnover was observed in some embryos.

  20. Alternate method of source preparation for alpha spectrometry: No electrodeposition, no hydrofluoric acid

    DOE PAGES

    Kurosaki, Hiromu; Mueller, Rebecca J.; Lambert, Susan B.; ...

    2016-07-15

    An alternate method of preparing actinide alpha counting sources was developed in place of electrodeposition or lanthanide fluoride micro-precipitation. The method uses lanthanide hydroxide micro-precipitation to avoid the use of hazardous hydrofluoric acid. Lastly, it provides a quicker, simpler, and safer way of preparing actinide alpha counting sources in routine, production-type laboratories that process many samples daily.