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Sample records for systems spectrometric potentiometric

  1. Potentiometric and spectrometric study: Copper(II), nickel(II) and ...

    Indian Academy of Sciences (India)

    taking potentially tridentate ligands, viz. L-cysteine, L-threonine, salicylglycinate and salicylvalinate, three metal ions (Cu2+, Ni2+ and Zn2+) and imidazole. The aqueous coordination chemistry of simple imidazolate bridged metal complexes is explored using. pH-potentiometric and UV/Vis spectroscopic techniques.

  2. System for Gamma an X rays fluorescence spectrometric

    International Nuclear Information System (INIS)

    Alonso Abad, D.; Arista Romeu, E.; Bolanos Perez, L. and others

    1997-01-01

    A system for spectrometry of gamma or fluorescence X rays is presented. It sis composed by a Si(Li) semiconductors detector, a charge sensitive preamplifier, a high voltage power supply, a spectrometric amplifier and a monolithic 1024 channels multichannel analyzers or an IBM compatible 4096 channels add - on- card multichannel analyzer. The system can be configured as a 1024 or 4096 channels gamma or fluorescent X rays spectrometer

  3. Gamma spectrometric system based on the personal computer Pravetz-83

    International Nuclear Information System (INIS)

    Yanakiev, K; Grigorov, T.; Vuchkov, M.

    1985-01-01

    A gamma spectrometric system based on a personal microcomputer Pravets-85 is described. The analog modules are NIM standard. ADC data are stored in the memory of the computer via a DMA channel and a real-time data processing is possible. The results from a series of tests indicate that the performance of the system is comparable with that of comercially avalable computerized spectrometers Ortec and Canberra

  4. A flow-through potentiometric sensor for an integrated microdialysis system

    NARCIS (Netherlands)

    Pijanowska, D.; Pijanowska, D.G.; Sprenkels, A.J.; van der Linden, H.J.; Bergveld, Piet; van den Berg, Albert; Olthuis, Wouter

    2003-01-01

    In this paper, the performance of a flow-through potentiometric sensor based on a semi-permeable dialysis tubing implemented in silicon, is presented. The sensor is designed as part of a lab-on-a-chip system and has been successfully incorporated into an integrated microdialysis system. Results of a

  5. A flow-through potentiometric sensor for an integrated microdialysis system

    NARCIS (Netherlands)

    Pijanowska, D.G.; Sprenkels, A.J.; van der Linden, H.J.; Olthuis, Wouter; Bergveld, Piet; van den Berg, Albert

    2004-01-01

    In this paper, the performance of a flow-through potentiometric sensor based on a semi-permeable dialysis tubing implemented in silicon, is presented. The sensor is designed as part of a lab-on-a-chip system and has been successfully incorporated into an integrated microdialysis system. Results of a

  6. Disposable Miniaturized Screen‐Printed pH and Reference Electrodes for Potentiometric Systems

    DEFF Research Database (Denmark)

    Musa, Arnaud Emmanuel; del Campo, Francisco Javier; Abramova, Natalia

    2011-01-01

    This work describes the development of a miniaturized potentiometric system comprising a miniaturized quasi‐reference electrode (QRE) coupled to a solid‐state ion‐selective electrode (ISE) for the monitoring of pH. We describe the optimization of materials and fabrication processes including scre...

  7. Actively shielded low level gamma - spectrometric system

    International Nuclear Information System (INIS)

    Mrdja, D.; Bikit, I.; Forkapic, S.; Slivka, J.; Veskovic, M.

    2005-01-01

    The results of the adjusting and testing of the actively shielded low level gamma-spectrometry system are presented. The veto action of the shield reduces the background in the energy region of 50 keV to the 2800 keV for about 3 times. (author) [sr

  8. Potentiometric, spectrometric, thermal and conductimetric studies on some 3-phenyl-4-(arylazo)-5-pyrazolones and their complexes with divalent cobalt metal ion

    Science.gov (United States)

    Hassib, H. B.; Abdel-Latif, S. A.

    2003-09-01

    3-phenyl-4-arylazo-5-pyrazolones (I-IV) have been synthesized and characterized by elemental, infrared (IR), ultraviolet and visible spectra (UV-Vis), proton nuclear magnetic resonance ( 1H NMR) and Mass spectra. It has been proved that these compounds exhibit a keto-enol tautomerism in solution. The donor character of the substituent increases the enol form. The ionization constants of the investigated ligands have been determined potentiometrically and found to decrease in the order OCH 3(IV)>CH 3(III)>H(I)>Cl(II). The Co(II) complexes of the investigated 3-phenyl-4-arylazo-5-pyrazolones (I-IV) have been prepared and characterized by elemental and thermal analyses as well as by IR, UV-Vis, electronic transition, potentiometric, conductimetric and magnetic measurements. The data suggest octahedral geometry for Co(II) (1:1) complexes and tetrahedral for Co(II) (2:3) complexes.

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

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

    Science.gov (United States)

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

    2012-05-15

    An automated flow injection potentiometric (FIP) system with electronic tongue detection (ET) is used for the monitoring of biosorption processes of heavy metals on vegetable wastes. Grape stalk wastes are used as biosorbent to remove Cu(2+) ions in a fixed-bed column configuration. The ET is formed by a 5-sensor array with Cu(2+) and Ca(2+)-selective electrodes and electrodes with generic response to heavy-metals, plus an artificial neural network response model of the sensor's cross-response. The real-time monitoring of both the Cu(2+) and the cation exchanged and released (Ca(2+)) in the effluent solution is performed by using flow-injection potentiometric electronic tongue system. The coupling of the electronic tongue with automation features of the flow-injection system allows us to accurately characterize the Cu(2+) ion-biosorption process, through obtaining its breakthrough curves, and the profile of the Ca(2+) ion release. In parallel, fractions of the extract solution are analysed by spectroscopic techniques in order to validate the results obtained with the reported methodology. The sorption performance of grape stalks is also evaluated by means of well-established sorption models. Copyright © 2012 Elsevier B.V. All rights reserved.

  11. Direct correlation between potentiometric and impedance biosensing of antibody-antigen interactions using an integrated system

    Science.gov (United States)

    Tsai, Meng-Yen; Creedon, Niamh; Brightbill, Eleanor; Pavlidis, Spyridon; Brown, Billyde; Gray, Darren W.; Shields, Niall; Sayers, Ríona; Mooney, Mark H.; O'Riordan, Alan; Vogel, Eric M.

    2017-08-01

    A fully integrated system that combines extended gate field-effect transistor (EGFET)-based potentiometric biosensors and electrochemical impedance spectroscopy (EIS)-based biosensors has been demonstrated. This integrated configuration enables the sequential measurement of the same immunological binding event on the same sensing surface and consequently sheds light on the fundamental origins of sensing signals produced by FET and EIS biosensors, as well as the correlation between the two. Detection of both the bovine serum albumin (BSA)/anti-BSA model system in buffer solution and bovine parainfluenza antibodies in complex blood plasma samples was demonstrated using the integrated biosensors. Comparison of the EGFET and EIS sensor responses reveals similar dynamic ranges, while equivalent circuit modeling of the EIS response shows that the commonly reported total impedance change (ΔZtotal) is dominated by the change in charge transfer resistance (Rct) rather than surface capacitance (Csurface). Using electrochemical kinetics and the Butler-Volmer equation, we unveil that the surface potential and charge transfer resistance, measured by potentiometric and impedance biosensors, respectively, are, in fact, intrinsically linked. This observation suggests that there is no significant gain in using the FET/EIS integrated system and leads to the demonstration that low-cost EGFET biosensors are sufficient as a detection tool to resolve the charge information of biomolecules for practical sensing applications.

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

    International Nuclear Information System (INIS)

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

    1979-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2005-08-15

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

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

    Directory of Open Access Journals (Sweden)

    Ching-Hsing Luo

    2011-09-01

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

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

    Science.gov (United States)

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

    2011-01-01

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

  16. Permian potentiometric analysis

    International Nuclear Information System (INIS)

    Devary, J.L.

    1983-09-01

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

  17. Potentiometric studies of acid-base interactions in substituted 4-nitropyridine N-oxide systems

    International Nuclear Information System (INIS)

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

    2006-01-01

    (Acid+base) equilibrium constants, involving the acidity (pK a AC ) and cationic homoconjugation constants (in the form of lgK BHB + AC ), have been determined by the potentiometric method in 13 systems formed by substituted 4-nitropyridine N-oxides in the polar aprotic solvent, acetone (AC). The derivatives covered a wide range of proton-acceptor properties and inherent diversified tendencies towards formation of hydrogen-bonded homocomplexed cations. In addition, the constant values (expressed as pK a AN andlgK BHB + AN ) for two of the systems studied, N-oxides of 2-methylamino- and 2-ethylamino-4-nitropyridine, were determined in acetonitrile (AN). The acidity constants in the non-aqueous media studied have been found to change in line with their substituent effects and the sequence of acidity changes in water. The values of the cationic homoconjugation constants increased with increasing basicity of the N-oxides and decreased with increasing solvent basicity

  18. Potentiometric studies of acid-base interactions in substituted 4-nitropyridine N-oxide systems

    Energy Technology Data Exchange (ETDEWEB)

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

    2006-05-15

    (Acid+base) equilibrium constants, involving the acidity (pK{sub a}{sup AC}) and cationic homoconjugation constants (in the form of lgK{sub BHB{sup +}}{sup AC}), have been determined by the potentiometric method in 13 systems formed by substituted 4-nitropyridine N-oxides in the polar aprotic solvent, acetone (AC). The derivatives covered a wide range of proton-acceptor properties and inherent diversified tendencies towards formation of hydrogen-bonded homocomplexed cations. In addition, the constant values (expressed as pK{sub a}{sup AN}andlgK{sub BHB{sup +}}{sup AN}) for two of the systems studied, N-oxides of 2-methylamino- and 2-ethylamino-4-nitropyridine, were determined in acetonitrile (AN). The acidity constants in the non-aqueous media studied have been found to change in line with their substituent effects and the sequence of acidity changes in water. The values of the cationic homoconjugation constants increased with increasing basicity of the N-oxides and decreased with increasing solvent basicity.

  19. Calibration facilities of airborne, surface and borehole gamma ray spectrometric survey systems

    International Nuclear Information System (INIS)

    Sarma, C.V.R.; Raghuwanshi, S.S.; Sreehari, R.; Johri, N.K.

    2009-01-01

    The gamma-ray spectrometric surveys for uranium exploration are based upon the detection of gamma-rays emitted by the primordial radio nuclides of Uranium (Bi-214), Thorium (Tl-208) and K-40. However, the instrumentation with gamma radiation detectors for surface, airborne, borehole surveys requires to be calibrated for processing of field acquired data. Various calibration procedures are being adopted for this purpose in Atomic Minerals Directorate for Exploration and Research in India and elsewhere in the world. The airborne and portable gamma-ray spectrometric survey systems are calibrated on indigenously constructed and suitably spiked concrete calibration pads at the Civil Airport at Nagpur, India over very low activity zone of Deccan traps. Using these pads sensitivities and Compton scattering factors are computed for these systems. For the calibration of gamma-ray borehole logging probes, concretized boreholes have been constructed at premises of AMD Headquarters Hyderabad which are called the primary standards. The concentrations of these standards and results found for the sensitivities of different probes and systems are given in Table 1 thru Table 5. These calibration standards at Hyderabad and Nagpur are now the National facilities and are being constantly used for calibration purposes not only for the gamma ray spectrometers designed by AMD, but also for the imported gamma ray spectrometric systems acquired by various other organizations in India. This paper describes the details of these calibration facilities. There are two more calibration facilities for airborne gamma-ray spectrometric survey systems which are located at Devarakonda, A.P. and Mahalarbadi in Maharashtra, The concentrations of U, Th, K of Devarakonda Test Strip, A.P. are given in Table 2. (author)

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2006-12-15

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

  2. Flow injection potentiometric system for the simultaneous determination of inositol phosphates and phosphate: phosphorus nutritional evaluation on seeds and grains.

    Science.gov (United States)

    Parra, Aleix; Ramon, Meritxell; Alonso, Julián; Lemos, Sherlan G; Vieira, Edivan C; Nogueira, Ana R A

    2005-10-05

    A simple flow injection potentiometric (FIP) system, which uses a tubular cobalt electrode, has been developed for phosphorus nutritional evaluation of seeds and grains. Inorganic phosphorus, P(i), is determined using a 1 x 10(-2) mol.L(-1) potassium phthalate buffer solution adjusted at pH 4. A sensitivity of 47 mV/decade and an operating range from 10 to 1000 mg.L(-1) (1 x 10(-4)-1 x 10(-2) M) of dihydrogen phosphate are obtained. The inositol phosphates amount, which is referred to the organic phosphorus, P(org), is directly determined from extracts using a 1 x 10(-2) mol.L(-1) Tris-HCl buffer solution adjusted at pH 8. A sensitivity of 127 mV/decade and an operating range of 10-1000 mg.L(-1) (2.5 x 10(-4)-5 x 10(-3) M) of P(org) (expressed as inositol hexakisphosphoric acid monocalcium) are achieved. Some samples of seed and grain are analyzed by an ICP-OES and a spectrophotometric method to compare results to the developed flow system; no significant differences at the 95% confidence level are observed using a paired t test. Other samples such as animal nursing feed, soybean meal, and corn are also analyzed with the proposed FIP system, showing a good correlation to the ICP-OES values.

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-02-15

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

  5. A Portable Low-Power Acquisition System with a Urease Bioelectrochemical Sensor for Potentiometric Detection of Urea Concentrations

    Directory of Open Access Journals (Sweden)

    Wei-Jhe Ma

    2016-04-01

    Full Text Available This paper presents a portable low-power battery-driven bioelectrochemical signal acquisition system for urea detection. The proposed design has several advantages, including high performance, low cost, low-power consumption, and high portability. A LT1789-1 low-supply-voltage instrumentation amplifier (IA was used to measure and amplify the open-circuit potential (OCP between the working and reference electrodes. An MSP430 micro-controller was programmed to process and transduce the signals to the custom-developed software by ZigBee RF module in wireless mode and UART in able mode. The immobilized urease sensor was prepared by embedding urease into the polymer (aniline-co-o-phenylenediamine polymeric matrix and then coating/depositing it onto a MEMS-fabricated Au working electrode. The linear correlation established between the urea concentration and the potentiometric change is in the urea concentrations range of 3.16 × 10−4 to 3.16 × 10−2 M with a sensitivity of 31.12 mV/log [M] and a precision of 0.995 (R2 = 0.995. This portable device not only detects urea concentrations, but can also operate continuously with a 3.7 V rechargeab-le lithium-ion battery (500 mA·h for at least four days. Accordingly, its use is feasible and even promising for home-care applications.

  6. Groundwater Flow Systems at the Nevada Test Site, Nevada: A Synthesis of Potentiometric Contours, Hydrostratigraphy, and Geologic Structures

    Energy Technology Data Exchange (ETDEWEB)

    Fenelon, Joseph M.; Sweetkind, Donald S.; Laczniak, Randell J.

    2010-01-25

    gradients between aquifer types are downward throughout most of the study area; however, flow from the alluvial-volcanic aquifer into the underlying carbonate aquifer, where both aquifers are present, is believed to be minor because of an intervening confining unit. Limited exchange of water between aquifer types occurs by diffuse flow through the confining unit, by focused flow along fault planes, or by direct flow where the confining unit is locally absent. Interflow between regional aquifers is evaluated and mapped to define major flow paths. These flow paths delineate tributary flow systems, which converge to form intermediate and regional flow systems. The implications of these flow systems in controlling transport of radionuclides away from the underground test areas at the Nevada Test Site are briefly discussed. Additionally, uncertainties in the delineation of aquifers, the development of potentiometric contours, and the identification of flow systems are identified and evaluated. Eleven tributary flow systems and three larger flow systems are mapped in the Nevada Test Site area. Flow systems within the alluvial-volcanic aquifer dominate the western half of the study area, whereas flow systems within the carbonate aquifer are most prevalent in the southeastern half of the study area. Most of the flow in the regional alluvial-volcanic aquifer that moves through the underground testing area on Pahute Mesa is discharged to the land surface at springs and seeps in Oasis Valley. Flow in the regional carbonate aquifer is internally compartmentalized by major geologic structures, primarily thrust faults, which constrain flow into separate corridors. Contaminants that reach the regional carbonate aquifer from testing areas in Yucca and Frenchman Flats flow toward downgradient discharge areas through the Alkali Flat-Furnace Creek Ranch or Ash Meadows flow systems and their tributaries.

  7. Groundwater Flow Systems at the Nevada Test Site, Nevada: A Synthesis of Potentiometric Contours, Hydrostratigraphy, and Geologic Structures

    Science.gov (United States)

    Fenelon, Joseph M.; Sweetkind, Donald S.; Laczniak, Randell J.

    2010-01-01

    gradients between aquifer types are downward throughout most of the study area; however, flow from the alluvial-volcanic aquifer into the underlying carbonate aquifer, where both aquifers are present, is believed to be minor because of an intervening confining unit. Limited exchange of water between aquifer types occurs by diffuse flow through the confining unit, by focused flow along fault planes, or by direct flow where the confining unit is locally absent. Interflow between regional aquifers is evaluated and mapped to define major flow paths. These flow paths delineate tributary flow systems, which converge to form intermediate and regional flow systems. The implications of these flow systems in controlling transport of radionuclides away from the underground test areas at the Nevada Test Site are briefly discussed. Additionally, uncertainties in the delineation of aquifers, the development of potentiometric contours, and the identification of flow systems are identified and evaluated. Eleven tributary flow systems and three larger flow systems are mapped in the Nevada Test Site area. Flow systems within the alluvial-volcanic aquifer dominate the western half of the study area, whereas flow systems within the carbonate aquifer are most prevalent in the southeastern half of the study area. Most of the flow in the regional alluvial-volcanic aquifer that moves through the underground testing area on Pahute Mesa is discharged to the land surface at springs and seeps in Oasis Valley. Flow in the regional carbonate aquifer is internally compartmentalized by major geologic structures, primarily thrust faults, which constrain flow into separate corridors. Contaminants that reach the regional carbonate aquifer from testing areas in Yucca and Frenchman Flats flow toward downgradient discharge areas through the Alkali Flat-Furnace Creek Ranch or Ash Meadows flow systems and their tributaries.

  8. Using Potentiometric Free Drug Sensors to Determine the Free Concentration of Ionizable Drugs in Colloidal Systems

    DEFF Research Database (Denmark)

    Tran, Thuy; Chakraborty, Anjan; Xi, Xi

    2018-01-01

    The present study investigates the use of free drug sensors (FDS) to measure free ionized drug concentrations in colloidal systems, including micellar solutions, emulsions, and lipid formulations during in vitro lipolysis. Diphenhydramine hydrochloride (DPH) and loperamide hydrochloride (LOP) were...... selected as model drugs. Self-diffusion nuclear magnetic resonance studies were performed and confirmed the entrapment of drugs in micelles in Brij 35 and sodium taurodeoxycholate (TDC)/phosphatidylcholine (PC) micellar solutions. The FDS measurements indicated that with a constant level of drug...

  9. Characterization of HPGe gamma spectrometric detectors systems for Instrumental Neutron Activation Analysis (INAA) at the Colombian Geological Survey

    Energy Technology Data Exchange (ETDEWEB)

    Sierra, O., E-mail: osierra@sgc.gov.co; Parrado, G., E-mail: gparrado@sgc.gov.co; Cañón, Y.; Porras, A.; Alonso, D.; Herrera, D. C.; Peña, M., E-mail: mlpena@sgc.gov.co; Orozco, J. [Colombian Geological Survey, Nuclear Affairs Technical Division, Neutron Activation Analysis Laboratory, Bogota D. C. (Colombia)

    2016-07-07

    This paper presents the progress made by the Neutron Activation Analysis (NAA) laboratory at the Colombian Geological Survey (SGC in its Spanish acronym), towards the characterization of its gamma spectrometric systems for Instrumental Neutron Activation Analysis (INAA), with the aim of introducing corrections to the measurements by variations in sample geometry. Characterization includes the empirical determination of the interaction point of gamma radiation inside the Germanium crystal, through the application of a linear model and the use of a fast Monte Carlo N-Particle (MCNP) software to estimate correction factors for differences in counting efficiency that arise from variations in sample density between samples and standards.

  10. AUTOMATION OF POTENTIOMETRIC TITRATION WITH A ...

    African Journals Online (AJOL)

    An IBM compatible interface card system with infrared source-detector data sampling was designed and tested for automation of potentiometric titrations with personal computers without continuous measurement of the volume of the titrant. The device with other appropriate apparatus and setup was tested for determination ...

  11. Redox equilibria in the In(III)-In(I)-In system in aqueous KBr solutions, I. potentiometric and coulometric study

    International Nuclear Information System (INIS)

    Malyszko, E.; Malyszko, J.

    1993-01-01

    The reproportionation of In(I) ions in acidic potassium bromide solutions was studied by means of the coulometric and potentiometric method. The formal potentials of the In(III)/In(I), In(III)/In and In(I)/In redox couples as well as the equilibrium constants of the reaction In(III) + 2 In 3 In(I) were determined at a background electrolyte concentration ranging from 1 to 4 mol dm -3 . Based on the experimental results, a scheme of the reproportionation reaction was proposed with regard to the participation of bromide ions. In addition, the diffusion coefficient of In(I) ions was determined using the chronopotentiometric technique

  12. Potentiometric and spectrometric study: Copper (II), nickel (II) and ...

    Indian Academy of Sciences (India)

    hetero-binuclear complexes; imidazole; metal(II); equilibrium study. Abstract. Equilibrium and solution structural study of mixed-metal-mixed-ligand complexes of Cu(II), Ni(II) and Zn(II) with L-cysteine, L-threonine and imidazole are conducted in ...

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

    International Nuclear Information System (INIS)

    Czaja, Malgorzata; Makowski, Mariusz; Chmurzynski, Lech

    2006-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2006-05-15

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

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2005-08-15

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

  17. Potentiometric titration with polarized electrodes

    International Nuclear Information System (INIS)

    Chikryzova, E.G.

    1977-01-01

    Based on the analysis of the works carried out during 1911-75 consideration is given to the present state of the method of potentiometric titration with polarized electrodes. The material is generalized in the tabular form indicating the elments of interest, titration conditions and the objects to be analyzed. The list and classification of the potentiometric titration methods intended for determining organic and inorganic substances are presented

  18. Spectrometric techniques 4

    CERN Document Server

    Vanasse, George A

    2013-01-01

    Spectrometric Techniques, Volume IV discusses three widely diversified areas of spectrometric techniques. The book focuses on three spectrometric methods. Chapter 1 discusses the phenomenology and applications of Coherent Anti-Stokes Raman Spectroscopy (CARS), the most commonly used optical technique that exploit the Raman effect. The second chapter is concerned with diffraction gratings and mountings for the Vacuum Ultraviolet Spectral Region. Chapter 3 accounts the uses of mass spectrometry, detectors, types of spectrometers, and ion sources. Physicists and chemists will find the book a go

  19. First derivative potentiometric and spectrophotometric ...

    African Journals Online (AJOL)

    This study sets out to provide simple, inexpensive and sensitive analytical techniques for the assay of cimetidine in tablet dosage forms using first derivative potentiometric and UV-spectrophotometric techniques, with a view to providing simple, sensitive and cost-effective analytical methods. Ten brands of cimetidine tablets ...

  20. Hydrothermal carbonization of biomass residues: mass spectrometric characterization for ecological effects in the soil-plant system.

    Science.gov (United States)

    Jandl, Gerald; Eckhardt, Kai-Uwe; Bargmann, Inge; Kücke, Martin; Greef, Jörg-Michael; Knicker, Heike; Leinweber, Peter

    2013-01-01

    Hydrochars, technically manufactured by hydrothermal carbonization (HTC) of biomass residues, are recently tested in high numbers for their suitability as feedstock for bioenergy production, the bioproduct industry, and as long-term carbon storage in soil, but ecological effects in the soil-plant system are not sufficiently known. Therefore, we investigated the influence of different biomass residues and process duration on the molecular composition of hydrochars, and how hydrochar addition to soils affected the germination of spring barley ( L.) seeds. Samples from biomass residues and the corresponding hydrochars were analyzed by pyrolysis-field ionization mass spectrometry (Py-FIMS) and gaseous emissions from the germination experiments with different soil-hydrochar mixtures by gas chromatography/mass spectrometry (GC/MS). The molecular-level characterization of various hydrochars by Py-FIMS clearly showed that the kind of biomass residue influenced the chemical composition of the corresponding hydrochars more strongly than the process duration. In addition to various detected possible toxic substances, two independent mass spectrometric methods (Py-FIMS and GC/MS) indicated long C-chain aliphatic compounds which are typically degraded to the C-unit ethylene that can evoke phytotoxic effects in high concentrations. This showed for the first time possible chemical compounds to explain toxic effects of hydrochars on plant growth. It is concluded that the HTC process did not result in a consistent product with defined chemical composition. Furthermore, possible toxic effects urgently need to be investigated for each individual hydrochar to assess effects on the soil organic matter composition and the soil biota before hydrochar applications as an amendment on agricultural soils. Copyright © by the American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America, Inc.

  1. New miniaturized alpha/beta spectrometric system for the surface contamination monitoring and radon personal dosimeter

    International Nuclear Information System (INIS)

    Streil, T.; Oeser, V.; Holfeld, G.

    1998-01-01

    The heart of the new miniaturized alpha/beta spectroscopic system is a Smart Card MCA having a 12 bit resolution and a 32 bit memory for each channel with the size of a cheque card. The system consists of a single or up to 12 alpha spectrometers in a battery powered casing with connectors for direct detector/amplifier module plugging. Surface contamination in the order of 1 Bq/cm 2 of 239 Pu can be measured. (M.D.)

  2. Simulation for photon detection in spectrometric system of high purity (HPGe) using MCNPX code

    International Nuclear Information System (INIS)

    Correa, Guilherme Jorge de Souza

    2013-01-01

    The Brazilian National Commission of Nuclear Energy defines parameters for classification and management of radioactive waste in accordance with the activity of materials. The efficiency of a detection system is crucial to determine the real activity of a radioactive source. When it's possible, the system's calibration should be performed using a standard source. Unfortunately, there are only a few cases that it can be done this way, considering the difficulty of obtaining appropriate standard sources for each type of measurement. So, computer simulations can be performed to assist in calculating of the efficiency of the system and, consequently, also auxiliary the classification of radioactive waste. This study aims to model a high purity germanium (HPGe) detector with MCNPX code, approaching the spectral values computationally obtained of the values experimentally obtained for the photopeak of 137 Cs. The approach will be made through changes in outer dead layer of the germanium crystal modeled. (author)

  3. Automated on-line liquid–liquid extraction system for temporal mass spectrometric analysis of dynamic samples

    Energy Technology Data Exchange (ETDEWEB)

    Hsieh, Kai-Ta; Liu, Pei-Han [Department of Applied Chemistry, National Chiao Tung University, 1001 University Rd, Hsinchu, 300, Taiwan (China); Urban, Pawel L. [Department of Applied Chemistry, National Chiao Tung University, 1001 University Rd, Hsinchu, 300, Taiwan (China); Institute of Molecular Science, National Chiao Tung University, 1001 University Rd, Hsinchu, 300, Taiwan (China)

    2015-09-24

    Most real samples cannot directly be infused to mass spectrometers because they could contaminate delicate parts of ion source and guides, or cause ion suppression. Conventional sample preparation procedures limit temporal resolution of analysis. We have developed an automated liquid–liquid extraction system that enables unsupervised repetitive treatment of dynamic samples and instantaneous analysis by mass spectrometry (MS). It incorporates inexpensive open-source microcontroller boards (Arduino and Netduino) to guide the extraction and analysis process. Duration of every extraction cycle is 17 min. The system enables monitoring of dynamic processes over many hours. The extracts are automatically transferred to the ion source incorporating a Venturi pump. Operation of the device has been characterized (repeatability, RSD = 15%, n = 20; concentration range for ibuprofen, 0.053–2.000 mM; LOD for ibuprofen, ∼0.005 mM; including extraction and detection). To exemplify its usefulness in real-world applications, we implemented this device in chemical profiling of pharmaceutical formulation dissolution process. Temporal dissolution profiles of commercial ibuprofen and acetaminophen tablets were recorded during 10 h. The extraction-MS datasets were fitted with exponential functions to characterize the rates of release of the main and auxiliary ingredients (e.g. ibuprofen, k = 0.43 ± 0.01 h{sup −1}). The electronic control unit of this system interacts with the operator via touch screen, internet, voice, and short text messages sent to the mobile phone, which is helpful when launching long-term (e.g. overnight) measurements. Due to these interactive features, the platform brings the concept of the Internet-of-Things (IoT) to the chemistry laboratory environment. - Highlights: • Mass spectrometric analysis normally requires sample preparation. • Liquid–liquid extraction can isolate analytes from complex matrices. • The proposed system automates

  4. Automated on-line liquid–liquid extraction system for temporal mass spectrometric analysis of dynamic samples

    International Nuclear Information System (INIS)

    Hsieh, Kai-Ta; Liu, Pei-Han; Urban, Pawel L.

    2015-01-01

    Most real samples cannot directly be infused to mass spectrometers because they could contaminate delicate parts of ion source and guides, or cause ion suppression. Conventional sample preparation procedures limit temporal resolution of analysis. We have developed an automated liquid–liquid extraction system that enables unsupervised repetitive treatment of dynamic samples and instantaneous analysis by mass spectrometry (MS). It incorporates inexpensive open-source microcontroller boards (Arduino and Netduino) to guide the extraction and analysis process. Duration of every extraction cycle is 17 min. The system enables monitoring of dynamic processes over many hours. The extracts are automatically transferred to the ion source incorporating a Venturi pump. Operation of the device has been characterized (repeatability, RSD = 15%, n = 20; concentration range for ibuprofen, 0.053–2.000 mM; LOD for ibuprofen, ∼0.005 mM; including extraction and detection). To exemplify its usefulness in real-world applications, we implemented this device in chemical profiling of pharmaceutical formulation dissolution process. Temporal dissolution profiles of commercial ibuprofen and acetaminophen tablets were recorded during 10 h. The extraction-MS datasets were fitted with exponential functions to characterize the rates of release of the main and auxiliary ingredients (e.g. ibuprofen, k = 0.43 ± 0.01 h −1 ). The electronic control unit of this system interacts with the operator via touch screen, internet, voice, and short text messages sent to the mobile phone, which is helpful when launching long-term (e.g. overnight) measurements. Due to these interactive features, the platform brings the concept of the Internet-of-Things (IoT) to the chemistry laboratory environment. - Highlights: • Mass spectrometric analysis normally requires sample preparation. • Liquid–liquid extraction can isolate analytes from complex matrices. • The proposed system automates the

  5. Data set for mass spectrometric analysis of recombinant human serum albumin from various expression systems

    Directory of Open Access Journals (Sweden)

    Daryl G.S. Smith

    2015-09-01

    Full Text Available Human serum albumin (HSA is a versatile and important protein for the pharmaceutical industry (Fanali et al., Mol. Aspects Med. 33(3 (2012 209–290. Due to the potential transmission of pathogens from plasma sourced albumin, numerous expression systems have been developed to produce recombinant HSA (rHSA (Chen et al., Biochim. Biophys. Acta (BBA—Gen. Subj. 1830(12 (2013 5515–5525; Kobayashi, Biologicals 34(1 (2006 55–59. Based on our previous study showing increased glycation of rHSA expressed in Asian rice (Frahm et al., J. Phys. Chem. B 116(15 (2012 4661–4670, both supplier-to-supplier and lot-to-lot variability of rHSAs from a number of expression systems were evaluated using reversed phase liquid chromatography linked with MS and MS/MS analyses. The data are associated with the research article ‘Determination of Supplier-to-Supplier and Lot-to-Lot Variability in Glycation of Recombinant Human Serum Albumin Expressed in Oryza sativa’ where further analysis of rHSA samples with additional biophysical methods can be found (Frahm et al., PLoS ONE 10(9 (2014 e109893. We determined that all rHSA samples expressed in rice showed elevated levels of arginine and lysine hexose glycation compared to rHSA expressed in yeast, suggesting that the extensive glycation of the recombinant proteins is a by-product of either the expression system or purification process and not a random occurrence.

  6. Analog-to-digital conversion of spectrometric data in information-control systems of activation analysis

    International Nuclear Information System (INIS)

    Mamonov, E.I.

    1972-01-01

    Analogue-digital conversion (ADC) techniques in nuclear radiation spectrometer channels is a most important link of information control systems in activation analysis. For the development of the ADC of spectrometer channels logico-structural methods of increasing the capacity, procedures for boosting frequency modes and improving the accuracy are promising. Procedures are suggested for increasing the ADC capacity. Insufficient stability and noticeable non-linearity of the spectrometer channel can be corrected at the information processing stage if their regularities are known. Capacity limitations make the development of ADC featuring high stability, capacity and linearity quite urgent

  7. Reconstruction of neutron spectra using neural networks starting from the Bonner spheres spectrometric system

    International Nuclear Information System (INIS)

    Ortiz R, J.M.; Martinez B, M.R.; Arteaga A, T.; Vega C, H.R.; Hernandez D, V.M.; Manzanares A, E.

    2005-01-01

    The artificial neural networks (RN) have been used successfully to solve a wide variety of problems. However to determine an appropriate set of values of the structural parameters and of learning of these, it continues being even a difficult task. Contrary to previous works, here a set of neural networks is designed to reconstruct neutron spectra starting from the counting rates coming from the detectors of the Bonner spheres system, using a systematic and experimental strategy for the robust design of multilayer neural networks of the feed forward type of inverse propagation. The robust design is formulated as a design problem of Taguchi parameters. It was selected a set of 53 neutron spectra, compiled by the International Atomic Energy Agency, the counting rates were calculated that would take place in a Bonner spheres system, the set was arranged according to the wave form of those spectra. With these data and applying the Taguchi methodology to determine the best parameters of the network topology, it was trained and it proved the same one with the spectra. (Author)

  8. Potentiometric-surface altitude of the confined aquifer, Wood River Valley aquifer system, south-central Idaho, October 2012.

    Data.gov (United States)

    Department of the Interior — Water levels in 93 wells completed in the Wood River Valley aquifer system were measured during October 22–24, 2012; these wells are part of a network established...

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

    Directory of Open Access Journals (Sweden)

    Edgard Moreira Ganzarolli

    1999-02-01

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

  10. Towards an automatic lab-on-valve-ion mobility spectrometric system for detection of cocaine abuse.

    Science.gov (United States)

    Cocovi-Solberg, David J; Esteve-Turrillas, Francesc A; Armenta, Sergio; de la Guardia, Miguel; Miró, Manuel

    2017-08-25

    A lab-on-valve miniaturized system integrating on-line disposable micro-solid phase extraction has been interfaced with ion mobility spectrometry for the accurate and sensitive determination of cocaine and ecgonine methyl ester in oral fluids. The method is based on the automatic loading of 500μL of oral fluid along with the retention of target analytes and matrix clean-up by mixed-mode cationic/reversed-phase solid phase beads, followed by elution with 100μL of 2-propanol containing (3% v/v) ammonia, which are online injected into the IMS. The sorptive particles are automatically discarded after every individual assay inasmuch as the sorptive capacity of the sorbent material is proven to be dramatically deteriorated with reuse. The method provided a limit of detection of 0.3 and 0.14μgL -1 for cocaine and ecgonine methyl ester, respectively, with relative standard deviation values from 8 till 14% with a total analysis time per sample of 7.5min. Method trueness was evaluated by analyzing oral fluid samples spiked with cocaine at different concentration levels (1, 5 and 25μgL -1 ) affording relative recoveries within the range of 85±24%. Fifteen saliva samples were collected from volunteers and analysed following the proposed automatic procedure, showing a 40% cocaine occurrence with concentrations ranging from 1.3 to 97μgL -1 . Field saliva samples were also analysed by reference methods based on lateral flow immunoassay and gas chromatography-mass spectrometry. The application of this procedure to the control of oral fluids of cocaine consumers represents a step forward towards the development of a point-of-care cocaine abuse sensing system. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Chemometric analysis of MALDI mass spectrometric images of three-dimensional cell culture systems.

    Science.gov (United States)

    Weaver, Eric M; Hummon, Amanda B; Keithley, Richard B

    2015-09-07

    As imaging mass spectrometry (IMS) has grown in popularity in recent years, the applications of this technique have become increasingly diverse. Currently there is a need for sophisticated data processing strategies that maximize the information gained from large IMS data sets. Traditional two-dimensional heat maps of single ions generated in IMS experiments lack analytical detail, yet manual analysis of multiple peaks across hundreds of pixels within an entire image is time-consuming, tedious and subjective. Here, various chemometric methods were used to analyze data sets obtained by matrix-assisted laser desorption/ionization (MALDI) IMS of multicellular spheroids. HT-29 colon carcinoma multicellular spheroids are an excellent in vitro model system that mimic the three dimensional morphology of tumors in vivo . These data are especially challenging to process because, while different microenvironments exist, the cells are clonal which can result in strong similarities in the mass spectral profiles within the image. In this proof-of-concept study, a combination of principal component analysis (PCA), clustering methods, and linear discriminant analysis was used to identify unique spectral features present in spatially heterogeneous locations within the image. Overall, the application of these exploratory data analysis tools allowed for the isolation and detection of proteomic changes within IMS data sets in an easy, rapid, and unsupervised manner. Furthermore, a simplified, non-mathematical theoretical introduction to the techniques is provided in addition to full command routines within the MATLAB programming environment, allowing others to easily utilize and adapt this approach.

  12. Mass spectrometric imaging of in vivo protein and lipid adsorption on biodegradable vascular replacement systems.

    Science.gov (United States)

    Fröhlich, Sophie M; Eilenberg, Magdalena; Svirkova, Anastasiya; Grasl, Christian; Liska, Robert; Bergmeister, Helga; Marchetti-Deschmann, Martina

    2015-09-07

    Cardiovascular diseases present amongst the highest mortality risks in Western civilization and are frequently caused by arteriosclerotic vessel failure. Coronary artery and peripheral vessel reconstruction necessitates the use of small diameter systems that are mechanically stress-resistant and biocompatible. Expanded polytetrafluorethylene (ePTFE) is amongst the materials used most frequently for non-degradable and bio-degradable vessel reconstruction procedures, with thermoplastic polyurethanes (TPU) representing a promising substitute. The present study describes and compares the biological adsorption and diffusion occurring with both materials following implantation in rat models. Gel electrophoresis and thin-layer chromatography, combined with mass spectrometry and mass spectrometry imaging, were utilized to identify the adsorbed lipids and proteins. The results were compared with the analytes present in native aorta tissue. It was revealed that both polymers were severely affected by biological adsorption after 10 min in vivo. Proteins associated with cell growth and migration were identified, especially on the luminal graft surface, while lipids were found to be located on both the luminal and abluminal surfaces. Lipid adsorption and cholesterol diffusion were found to be correlated with the polymer modifications identified on degradable thermoplastic urethane graft samples, with the latter revealing extensive cholesterol adsorption. The present study demonstrates an interaction between biological matter and both graft materials, and provides insights into polymer changes, in particular, those observed with thermoplastic urethanes already after 10 min in vivo exposure. ePTFE demonstrated minor polymer modifications, whereas several different polymer signals were observed for TPU, all were co-localized with biological signals.

  13. Polymeric matrix membrane sensors for stability-indicating potentiometric determination of oxybutynin hydrochloride and flavoxate hydrochloride urogenital system drugs.

    Science.gov (United States)

    Heba, Mohamed; Ramadan, Nesrin; El-Laithy, Moustafa

    2008-01-01

    Four polyvinyl chloride (PVC) matrix membrane electrodes responsive to 2 drugs affecting the urogenital system--oxybutynin hydrochloride (OX) and flavoxate hydrochloride (FX)--were developed, described, and characterized. A precipitation-based technique with tungstophosphate (TP) and ammonium reineckate (R) anions as electroactive materials in a PVC matrix with an OX cation was used for electrode 1 and 2 fabrication, respectively. Electrode 3 and 4 fabrication was based on use of the precipitation technique of FX cation with tetrakis (4-chlorophenyl) borate and R anions as electroactive materials. Fast and stable Nernstian responses in the range 1 x 10(-2)-1 x 10(-6) M for the 2 drugs over the pH range 5-8 revealed the performance characteristics of these electrodes, which were evaluated according to International Union of Pure and Applied Chemistry recommendations. The method was applied to FX and OX in their pharmaceutical formulations and in human plasma samples. The 4 proposed sensors were found to be specific for the drugs in the presence of up to 60% of their degradation products. Validation of the method according to the quality assurance standards showed suitability of the proposed electrodes for use in the quality control assessment of these drugs. The recoveries for determination of the drugs by the 4 proposed selective electrodes were 99.5 +/- 0.5, 100.0 +/- 0.4, 99.9 +/- 0.4, and 100.1 +/- 0.4% for sensors 1-4, respectively. Statistical comparison between the results obtained by this method and the official method of the drugs was done, and no significant difference found.

  14. Spectrometric techniques 3

    CERN Document Server

    Vanasse, George A

    2013-01-01

    Spectrometric Techniques, Volume III presents the applications of spectrometric techniques to atmospheric and space studies. This book reviews the spectral data processing and analysis techniques that are of broad applicability.Organized into five chapters, this volume begins with an overview of the instrumentation used for obtaining field data. This text then reviews the contribution that space-borne spectroscopy in the thermal IR has made to the understanding of the planets. Other chapters consider the instruments that have recorded the planetary emission spectra. This book discusses as well

  15. Marine gamma spectrometric survey

    International Nuclear Information System (INIS)

    Kostoglodov, V.V.

    1979-01-01

    Presented are theoretical problems physical and geochemical prerequisites and possibilities of practical application of the method of continuous submarine gamma-spectrometric survey and radiometric survey destined for rapid study of the surface layer of marine sediments. Shown is high efficiency and advantages of this method in comparison with traditional and widely spread in marine geology methods of bottom sediments investigation

  16. Analysis of mathematical modelling on potentiometric biosensors.

    Science.gov (United States)

    Mehala, N; Rajendran, L

    2014-01-01

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

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

    Science.gov (United States)

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

    1980-06-01

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

  18. Spectrometric techniques 2

    CERN Document Server

    Vanasse, George A

    2013-01-01

    Spectrometric Techniques, Volume II provides information pertinent to vacuum ultraviolet techniques to complete the demonstration of the diversity of methods available to the spectroscopist interested in the ultraviolet visible and infrared spectral regions. This book discusses the specific aspects of the technique of Fourier transform spectroscopy.Organized into five chapters, this volume begins with an overview of the large number of systematic effects in the recording of an interferogram. This text then examines the design approach for a Fourier transform spectrometer with focus on optics.

  19. Potentiometric assay for acid and alkaline phosphatase

    International Nuclear Information System (INIS)

    Koncki, Robert; Ogonczyk, Dominika; Glab, Stanislaw

    2005-01-01

    Simple potentiometric kinetic assay for evaluation of acid and alkaline phosphatase activity has been developed. Enzymatically catalyzed hydrolysis of monofluorophosphate, the simplest inorganic compound containing P-F bond, has been investigated as the basis of the assays. Fluoride ions formed in the course of the hydrolysis of this specific substrate have been detected using conventional fluoride ion-selective electrode based on membrane made of lanthanum fluoride. The key analytical parameters necessary for sensitive and selective detection of both enzymes have been assessed. Maximal sensitivity of the assays was observed at monofluorophosphate concentration near 10 -3 M. Maximal sensitivity of acid phosphatase assay was found at pH 6.0, but pH of 4.8 is recommended to eliminate effects from alkaline phosphatase. Optimal pH for alkaline phosphatase assay is 9.0. The utility of the developed substrate-sensor system for determination of acid and alkaline phosphatase activity in human serum has been demonstrated

  20. A mass spectrometric system for analyzing thermal desorption spectra of ion-implanted argon and cesium in tungsten. Ph.D. Thesis

    Science.gov (United States)

    Wood, G. M., Jr.

    1974-01-01

    A mass spectrometric system for determining the characteristics of materials used in instrumental development and aerospace applications was developed. The desorption spectra of cesium that was ion-implanted into polycrystalline tungsten and the effects on the spectra of bombardment of the tungsten by low energy (70 eV) electrons were investigated. Work function changes were measured by the retarding potential diode method. Flash desorption characteristics were observed and gas-reaction mechanisms of the surface of heated metal filaments were studied. Desorption spectra were measured by linearly increasing the sample temperature at a selected rate, the temperature cycling being generated from a ramp-driven dc power supply, with the mass spectrometer tuned to a mass number of interest. Results of the study indicate an anomolous desorption mechanism following an electron bombardment of the sample surface. The enhanced spectra are a function of the post-bombardment time and energy and are suggestive of an increased concentration of cesium atoms, up to 10 or more angstroms below the surface.

  1. ALPHA SPECTROMETRIC EVALUATION OF SRM-995 AS A POTENTIAL URANIUM/THORIUM DOUBLE TRACER SYSTEM FOR AGE-DATING URANIUM MATERIALS

    Energy Technology Data Exchange (ETDEWEB)

    Beals, D.

    2011-12-06

    Uranium-233 (t{sub 1/2} {approx} 1.59E5 years) is an artificial, fissile isotope of uranium that has significant importance in nuclear forensics. The isotope provides a unique signature in determining the origin and provenance of uranium-bearing materials and is valuable as a mass spectrometric tracer. Alpha spectrometry was employed in the critical evaluation of a {sup 233}U standard reference material (SRM-995) as a dual tracer system based on the in-growth of {sup 229}Th (t{sub 1/2} {approx} 7.34E3 years) for {approx}35 years following radiochemical purification. Preliminary investigations focused on the isotopic analysis of standards and unmodified fractions of SRM-995; all samples were separated and purified using a multi-column anion-exchange scheme. The {sup 229}Th/{sup 233}U atom ratio for SRM-995 was found to be 1.598E-4 ({+-} 4.50%) using recovery-corrected radiochemical methods. Using the Bateman equations and relevant half-lives, this ratio reflects a material that was purified {approx} 36.8 years prior to this analysis. The calculated age is discussed in contrast with both the date of certification and the recorded date of last purification.

  2. Regional potentiometric-surface map of the Great Basin carbonate and alluvial aquifer system in Snake Valley and surrounding areas, Juab, Millard, and Beaver Counties, Utah, and White Pine and Lincoln Counties, Nevada

    Science.gov (United States)

    Gardner, Philip M.; Masbruch, Melissa D.; Plume, Russell W.; Buto, Susan G.

    2011-01-01

    Water-level measurements from 190 wells were used to develop a potentiometric-surface map of the east-central portion of the regional Great Basin carbonate and alluvial aquifer system in and around Snake Valley, eastern Nevada and western Utah. The map area covers approximately 9,000 square miles in Juab, Millard, and Beaver Counties, Utah, and White Pine and Lincoln Counties, Nevada. Recent (2007-2010) drilling by the Utah Geological Survey and U.S. Geological Survey has provided new data for areas where water-level measurements were previously unavailable. New water-level data were used to refine mapping of the pathways of intrabasin and interbasin groundwater flow. At 20 of these locations, nested observation wells provide vertical hydraulic gradient data and information related to the degree of connection between basin-fill aquifers and consolidated-rock aquifers. Multiple-year water-level hydrographs are also presented for 32 wells to illustrate the aquifer system's response to interannual climate variations and well withdrawals.

  3. glycylvaline and imidazoles: An aqueous potentiometric and ...

    Indian Academy of Sciences (India)

    Unknown

    s.d. Fine Chem.) were used as received. All other chemicals used were of reagent grade. Solutions were prepared using double distilled water. 2.2 Potentiometric measurements. Values of pH were determined with a Systronics pH meter, ...

  4. Potentiometric Study of Trismethioninato Complexes of some ...

    African Journals Online (AJOL)

    Potentiometric study of methionine complexes of chromium, manganese, iron, cobalt and nickel was carried out in aqueous media by titrating with standard sodium hydroxide solution. The values of the stepwise and overall stability constant were obtained by new computational method, 'ORIGIN 50'. The values of the ...

  5. Potentiometric Study of Trismethioninato Complexes of some ...

    African Journals Online (AJOL)

    Chemical Society, 92: 4210 - 4222. Na'aliya, J. (2008). Potentiometric studies of some essential metal amino acid complexes. PhD thesis, Department of pure and Industrial. Chemistry, Bayero University, Kano. (Unpublished). Satya, P., Tuli, G.D., Basu, S.K. and Madan, R.D.. (2006). Advanced Inorganic Chemistry Vol. I S.

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

    Energy Technology Data Exchange (ETDEWEB)

    Liang, Jintao [School of Life and Environmental Sciences, Guilin University of Electronic Technology, Guilin, Guangxi 541004 (China); Guangxi Experiment Center of Information Sciences, Guilin University of Electronic Technology, Guilin, Guangxi 541004 (China); Guan, Mingyuan; Huang, Guoyin; Qiu, Hengming; Chen, Zhengcheng [School of Life and Environmental Sciences, Guilin University of Electronic Technology, Guilin, Guangxi 541004 (China); Li, Guiyin, E-mail: liguiyin01@163.com [School of Life and Environmental Sciences, Guilin University of Electronic Technology, Guilin, Guangxi 541004 (China); Guangxi Experiment Center of Information Sciences, Guilin University of Electronic Technology, Guilin, Guangxi 541004 (China); Huang, Yong, E-mail: huangyong503@126.com [School of Life and Environmental Sciences, Guilin University of Electronic Technology, Guilin, Guangxi 541004 (China); Guangxi Experiment Center of Information Sciences, Guilin University of Electronic Technology, Guilin, Guangxi 541004 (China)

    2016-06-01

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

  7. Utilizing the Inherent Electrolysis in a Chip-Based Nanoelectrospray Emitter System to Facilitate Selective Ionization and Mass Spectrometric Analysis of Metallo Alkylporphyrins

    Energy Technology Data Exchange (ETDEWEB)

    Van Berkel, Gary J [ORNL; Kertesz, Vilmos [ORNL

    2012-01-01

    A commercially available chip-based infusion nanoelectrospray ionization system was used to ionize metallo alkylporphyrins for mass spectrometric detection and structure elucidation by mass spectrometry. Different ionic forms of model compounds (nickel (II), vanadyl (II), copper (II) and cobalt (II) octaethylporphyrin) were created by using two different types of conductive pipette tips supplied with the device. These pipette tips provide the conductive contact to solution at which the electrolysis process inherent to electrospray takes places in the device. The original unmodified, bare carbon-impregnated plastic pipette tips, were exploited to intentionally electrochemically oxidize (ionize) the porphyrins to form molecular radical cations for detection. Use of modified pipette tips, with a surface coating devised to inhibit analyte mass transport to the surface, was shown to limit the ionic species observed in the mass spectra of these porphyrins largely, but not exclusively, to the protonated molecule. Under the conditions of these experiments, the effective upper potential limit for oxidation with the uncoated pipette tip was 1.1 V or less and the coated pipette tips effectively prevented the oxidation of analytes with redox potentials greater than about 0.25 V. Product ion spectra of either molecular ionic species could be used to determine the alkyl chain length on the porphyrin macrocycle. The utility of this electrochemical ionization approach for the analysis of naturally occurring samples was demonstrated using nickel geoporphyrin fractions isolated from Gilsonite bitumen. Acquiring neutral loss spectra as a means to improve the specificity of detection in these complex natural samples was also illustrated.

  8. Potentiometric and spectrometric study: Copper(II), nickel(II) and ...

    Indian Academy of Sciences (India)

    Abstract. Equilibrium and solution structural study of mixed-metal–mixed-ligand complexes of Cu(II), Ni(II) and Zn(II) with L-cysteine, L-threonine and imidazole are conducted in aqueous solution by potentiometry and spectrophotometry. Stability constants of the binary, ternary and quaternary complexes are determined at ...

  9. Outdoor spectrometric measurement of gamma source activities

    International Nuclear Information System (INIS)

    Cespirova, I.

    2003-01-01

    Two methods for outdoor activity measurements are described. The one is the in situ measurement method which is based on a proportionality between the flux density of non-dispersed photons of the given energy at the detector site and the specific activity of the relevant radionuclide in soil. The other method, for the monitoring of large areas, uses the spectrometric IRIS system (Integrated Radiation Information System), located on a helicopter for aerial monitoring or in a car for terrestrial measurement. (P.A.)

  10. Mass spectrometric study of thermodynamic properties in the Gd2O3-Y2O3system at high temperatures.

    Science.gov (United States)

    Kablov, Eugene N; Stolyarova, Valentina L; Lopatin, Sergey I; Vorozhtcov, Viktor A; Karachevtsev, Fedor N; Folomeikin, Yuriy I

    2017-03-30

    The Gd 2 O 3 -Y 2 O 3 system possesses a number of practical applications, one of the most important of them being production of casting molds for gas turbine engine blades. The components of this system are often added to zirconia or hafnia to obtain high-temperature ceramics which are used for the development of thermal barrier coatings. However, Gd 2 O 3 and Y 2 O 3 are more volatile than zirconia or hafnia and may vaporize selectively during synthesis or usage of high-temperature materials which may lead to changes in their physicochemical properties. Therefore, information on the vaporization processes and thermodynamic properties of the Gd 2 O 3 -Y 2 O 3 system is of great importance. High-temperature Knudsen effusion mass spectrometry was used to study the vaporization processes and to determine the thermodynamic properties of the Gd 2 O 3 -Y 2 O 3 system. Measurements were performed with a MS-1301 mass spectrometer. Vaporization was carried out using a tungsten twin effusion cell containing the sample under study and pure Gd 2 O 3 as a reference substance. Electron ionization at an energy of 25 eV was employed. At the temperature of 2630 K, GdO, YO and O vapor species were identified over the samples in the Gd 2 O 3 -Y 2 O 3 system. The Gd 2 O 3 and Y 2 O 3 activities and the vaporization rates of samples as functions of composition in the Gd 2 O 3 -Y 2 O 3 system were derived from the partial pressures of the vapor species mentioned. Using these data the Gibbs energy of mixing and excess Gibbs energy of the hexagonal solid solution in this system were calculated at 2630 K. The thermodynamic properties of the Gd 2 O 3 -Y 2 O 3 system, such as the activities of components and the excess Gibbs energy, obtained in the present study using Knudsen mass spectrometry at 2630 K, demonstrated significant negative deviations from ideal behavior. The vaporization rates of the samples were found to decrease as the Y 2 O 3 content increased. Copyright © 2016 John

  11. New medical imaging systems exploiting the energy dispersive X-ray diffraction with spectrometric CdZnTe based detector

    International Nuclear Information System (INIS)

    Barbes, Damien

    2016-01-01

    This thesis studies the interest of measuring the coherent scattering of X-rays for breast diagnosis imaging. Nowadays, most of X-ray-based medical imaging techniques use the information of X-rays attenuation through the tissues. It is the case for mammography, the most common breast imaging modality. The recent emergence of energy resolved detectors (based on semiconductors in particular) allows to consider using another phenomenon: the coherent X-ray scattering. Measurement of diffracted spectra can provide new information related to the molecular structure of the examined tissues, in order to improve their characterization and therefore improve the final diagnosis. Two modalities are considered: the breast cancer detection in vivo, following a suspicious mammography result, or biopsy analysis. The coherent scattering measurement system developed during this thesis work uses energy-resolved CdZnTe-based detectors, these detectors combining performances (energy resolution, sensitivity, spatial resolution, and compactness) promising for clinical application. This system is also based on the detector pixelation, which allows to provide an imaging modality capable of characterizing analyzed materials or tissues in one direction without any translation or rotation. A complete study of the measurement system is proposed in this thesis, structured in three main parts: modeling and simulation of the system, development of the processing of the data measured by the detector in order to image and characterize the analyzed sample and finally, designing of a new and more complex experimental setup based on a whole detector and multi-slit collimation system. An experimental validation is proposed for each of these three parts. (author) [fr

  12. Development of a portable mass spectrometric system for determination of isotopic composition of solid uranium samples using fluorine volatilization

    Science.gov (United States)

    Loge, G.

    1994-09-01

    Using hardware and materials supplied by LANL, a prototype quadrupole mass spectrometer system designed for portable field analysis of isotopic composition of solid uranium samples was assembled and tested. The system contained the capability for fluorine volatilization of solid uranium samples with gas introduction, which was successfully tested and demonstrated using 100 mg samples of U3O8. Determination of precision and accuracy for measuring isotopic composition was performed using isotopic standards. Use with soil samples containing uranium were also attempted. Silicates in the soil forming SiF4 were found to be a kinetic bottleneck to the formation of UF6. This could be avoided by performing some sort of chemical separation as a pre-treatment step, which was demonstrated using nitric acid.

  13. Automated on-line liquid-liquid extraction system for temporal mass spectrometric analysis of dynamic samples.

    Science.gov (United States)

    Hsieh, Kai-Ta; Liu, Pei-Han; Urban, Pawel L

    2015-09-24

    Most real samples cannot directly be infused to mass spectrometers because they could contaminate delicate parts of ion source and guides, or cause ion suppression. Conventional sample preparation procedures limit temporal resolution of analysis. We have developed an automated liquid-liquid extraction system that enables unsupervised repetitive treatment of dynamic samples and instantaneous analysis by mass spectrometry (MS). It incorporates inexpensive open-source microcontroller boards (Arduino and Netduino) to guide the extraction and analysis process. Duration of every extraction cycle is 17 min. The system enables monitoring of dynamic processes over many hours. The extracts are automatically transferred to the ion source incorporating a Venturi pump. Operation of the device has been characterized (repeatability, RSD = 15%, n = 20; concentration range for ibuprofen, 0.053-2.000 mM; LOD for ibuprofen, ∼0.005 mM; including extraction and detection). To exemplify its usefulness in real-world applications, we implemented this device in chemical profiling of pharmaceutical formulation dissolution process. Temporal dissolution profiles of commercial ibuprofen and acetaminophen tablets were recorded during 10 h. The extraction-MS datasets were fitted with exponential functions to characterize the rates of release of the main and auxiliary ingredients (e.g. ibuprofen, k = 0.43 ± 0.01 h(-1)). The electronic control unit of this system interacts with the operator via touch screen, internet, voice, and short text messages sent to the mobile phone, which is helpful when launching long-term (e.g. overnight) measurements. Due to these interactive features, the platform brings the concept of the Internet-of-Things (IoT) to the chemistry laboratory environment. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. Spectrometric electronic equipment for a 90-channel cherenkov mass spectrometer

    International Nuclear Information System (INIS)

    Astvatsaturov, R.G.; Basiladze, S.G.; Ivanov, V.I.

    1978-01-01

    Detecting spectrometric electronic equipment of a 90-channel cherenkov γ-spectrometer operating on-line with HP2116B type computer is described. The equipment contains linear amplifiers, analog memory blocks, a linear summator, discriminators, and a coincidence circuit. Three computer-controlled systems are used for checking the characteristics of the spectrometric electronic equipment, photomultipliers, and also for energy calibrations of the detectors. The long-term stability of the equipment has been measured with the aid of the checkup systems. It is established that the average instability of the pedestal magnitudes for all the channels is less than 10%, while the instability of the transmission coefficients is not worse than 0.5% for 5 days. The average nonlinearity over all the channels is 0.6%. The resolution time of the spectrometric equipment is 180 nsec

  15. Potentiometric perchlorate determination at nanomolar concentrations in vegetables.

    Science.gov (United States)

    Leoterio, Dilmo M S; Paim, Ana Paula S; Belian, Mônica F; Galembeck, André; Lavorante, André F; Pinto, Edgar; Amorim, Célia G; Araújo, Alberto N; Montenegro, Maria C B S M

    2017-07-15

    In this work, an expeditious method based on the multi-commutated flow-analysis concept with potentiometric detection is proposed to perform determinations of the emergent contaminant perchlorate in vegetable matrices down to nanomolar concentration. To accomplish the task, a tubular shaped potentiometric sensor selective to perchlorate ion was constructed with a PVC membrane containing 12mmol/kg of the polyamine bisnaphthalimidopropyl-4,4'-diaminodiphenylmethane and 2-nitrophenyl phenyl ether 68% (w/w) as plasticizer casted on a conductive epoxy resin. Under optimal flow conditions, the sensor responded linearly in the concentration range of 6.3×10 -7 -1.0×10 -3 mol/L perchlorate. In order to extend the determinations to lower concentrations (4.6(±1.3)×10 -10 mol/L perchlorate), a column packed with 70mg of sodium 2,5,8,11,14-pentaoxa-1-silacyclotetradecane-polymer was coupled to the flow-system thus enabling prior pre-concentration of the perchlorate. The proposed procedure provides a simpler alternative for the determination of perchlorate in foods, nowadays only allowed by sophisticated and expensive equipment and laborious methods. Copyright © 2017 Elsevier Ltd. All rights reserved.

  16. A computer controlled potentiometric titrator for quantitative determination of uranium

    International Nuclear Information System (INIS)

    Verdingh, V.; Michiels, A.

    1988-01-01

    The modified Davies and Gray methods is frequently used for the potentiometric titration of uranium. It is based upon the reduction of U(VI) to U(IV) with a reductant (e.g. Fe ++ ) followed by a selective oxidation of the excess of reductant and subsequent titration of U(IV) with potassium dichromate (K 2 Cr 2 O 7 ). Interference from other elements is low, but the method is rather cumbersome due to the number of reactants to be added before the titration is started. The timing of these additions also plays a role. In order to render the titration less dependent on human factors and with the aim of reaching high reproducibility, a computer controlled system has been designed and set-up. Reagents are added by five computer controlled burettes. A program allows the choice of volumes and waiting times, and commands the start of the final titration which is followed by the microprocessor of the automatic potentiometric titrator. In this way a routine uranium titration can be completed in about twelve minutes. Reproducibilities of the order of ±15% are achievable in routine operation. For high precision work, the titrator is used as an end-point detector. Titrant is added manually by mass, so as to react with > 99% of the uranium. The residual uranium is then titrated automatically by colume with diluted titrant. The precision can be improved by a factor of approximately ten. (orig.)

  17. Conductometry, spectrophotometry and mass spectrometric ...

    African Journals Online (AJOL)

    ... versus the mole ratio of [AZT]/[M2+], Job's method of continuous variation and mole ratio method showed the stoichiometry to be 1:1 (M2+:AZT) for both the cations. The metal ion-AZT complexes formed through the nitrogen of the azide group were further ascertained by liquid chromatography-mass spectrometric analysis.

  18. NZG 201 portable spectrometric unit

    International Nuclear Information System (INIS)

    Jursa, P.; Novakova, O.; Slezak, V.

    The NZG 201 spectrometric unit is a portable single-channel processing unit supplied from the mains or a battery which allows the qualitative and quantitative measurement of different types of ionizing radiation when connected to a suitable detection unit. The circuit layout and the choice of control elements makes the spectrometric unit suitable for use with scintillation detector units. The spectrometric unit consists of a pulse amplifier, an amplitude pulse analyzer, a pulse counter, a pulse rate counter with an output for a recorder, a high voltage source and a low voltage source. The block diagram is given. All circuits are modular and are mounted on PCB's. The apparatus is built in a steel cabinet with a raised edge which protects the control elements. The linear pulse amplifier has a maximum gain of 1024, the pulse counter has a maximum capacity of 10 6 -1 imp and time resolution better than 0.5 μs. The temperature interval at which the apparatus is operational is 0 to 45 degC, its weight is 12.5 kg and dimensions 36x280x310 mm, energy range O.025 to 2.5 MeV, for 137 Cs the energy resolution is 8 to 10%. The spectrometric unit NZG 2O1 may, with regard to its parameters, number and range of control elements, be used as a universal measuring unit. (J.P.)

  19. Comparison of the precision and accuracy of digital versus analogue gamma-ray spectrometric systems used in INAA for evaluation of homogeneity and certification of reference materials of the IAEA

    International Nuclear Information System (INIS)

    Makarewicz, M.; Burns, K.

    2000-01-01

    Performance of three commercial gamma-ray spectrometric systems was evaluated for precision and accuracy prior to use in characterization of reference materials. Two of the systems were based on fast processing of the analogue signal from the amplifier (EGG Ortec model 672) using a loss free counting module (Canberra model LFC 599) interfaced to one of two analog-to-digital converters (Canberra models 8713 or 8715). The third system was based on a digital signal processor (Canberra model DSP 9660). Performance of the systems was tested over a range of count rates up to a maximum of 70,000 counts per second (dead time up to 90%) using 60 Co and 137 Cs sources. Best resolution was achieved with an analogue system with ADC 8713. The analytical results obtained with the digital system show the lowest and well-quantified uncertainty. (author)

  20. Changes in the potentiometric-surface altitude of the confined aquifer, Wood River Valley aquifer system, south-central Idaho, October 2006 to October 2012.

    Data.gov (United States)

    Department of the Interior — Water levels in 93 wells completed in the Wood River Valley aquifer system were measured during October 22–24, 2012; these wells are part of a network established...

  1. A nonlinear electrostatic potential change in the T-system of skeletal muscle detected under passive recording conditions using potentiometric dyes.

    Science.gov (United States)

    Heiny, J A; Jong, D S

    1990-01-01

    Voltage-sensing dyes were used to examine the electrical behavior of the T-system under passive recording conditions similar to those commonly used to detect charge movement. These conditions are designed to eliminate all ionic currents and render the T-system potential linear with respect to the command potential applied at the surface membrane. However, we found an unexpected nonlinearity in the relationship between the dye signal from the T-system and the applied clamp potential. An additional voltage- and time-dependent optical signal appears over the same depolarizing range of potentials where change movement and mechanical activation occur. This nonlinearity is not associated with unblocked ionic currents and cannot be attributed to lack of voltage clamp control of the T-system, which appears to be good under these conditions. We propose that a local electrostatic potential change occurs in the T-system upon depolarization. An electrostatic potential would not be expected to extend beyond molecular distances of the membrane and therefore would be sensed by a charged dye in the membrane but not by the voltage clamp, which responds solely to the potential of the bulk solution. Results obtained with different dyes suggest that the location of the phenomena giving rise to the extra absorbance change is either intramembrane or at the inner surface of the T-system membrane.

  2. Potentiometric studies of Nickel (II) and copper (II) acetyl acetonato ...

    African Journals Online (AJOL)

    Potentiometric studies of Nickel (II) and copper (II) acetyl acetonato complexes. HN Aliyu, A Mustapha. Abstract. The dissociation constant pKa of acetylacetone has been determined potentiometrically. The pKa value obtained is 9.40, indicating a weak acid. The stability constants of the complex compounds formed from the ...

  3. Hydrogeology, groundwater levels, and generalized potentiometric-surface map of the Green River Basin lower Tertiary aquifer system, 2010–14, in the northern Green River structural basin

    Science.gov (United States)

    Bartos, Timothy T.; Hallberg, Laura L.; Eddy-Miller, Cheryl

    2015-07-14

    In cooperation with the Bureau of Land Management, groundwater levels in wells located in the northern Green River Basin in Wyoming, an area of ongoing energy development, were measured by the U.S. Geological Survey from 2010 to 2014. The wells were completed in the uppermost aquifers of the Green River Basin lower Tertiary aquifer system, which is a complex regional aquifer system that provides water to most wells in the area. Except for near perennial streams, groundwater-level altitudes in most aquifers generally decreased with increasing depth, indicating a general downward potential for groundwater movement in the study area. Drilled depth of the wells was observed as a useful indicator of depth to groundwater such that deeper wells typically had a greater depth to groundwater. Comparison of a subset of wells included in this study that had historical groundwater levels that were measured during the 1960s and 1970s and again between 2012 and 2014 indicated that, overall, most of the wells showed a net decline in groundwater levels.

  4. Scanning electrochemical microscopy determination of hydrogen flux at liquid|liquid interface with potentiometric probe

    OpenAIRE

    Jedraszko, Justyna; Nogala, Wojciech; Adamiak, Wojciech; Girault, Hubert H.; Opallo, Marcin

    2014-01-01

    Scanning electrochemical microscopy potentiometric determination of local hydrogen concentration and its flux next to the liquid|liquid interface was demonstrated. This method is based on the shift of open circuit potential of Pt-based reversible hydrogen electrode. The detection system was verified with a system generating hydrogen under galvanostatic conditions. Then, it was applied to aqueous|1,2-dichloroethane interface where hydrogen is produced with decamethylferrocene as electron donor.

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

    International Nuclear Information System (INIS)

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

    1994-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1994-12-01

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

  7. Spectrometric mixture analysis: An unexpected wrinkle

    Indian Academy of Sciences (India)

    The spectrometric analysis of a mixture of two chemically and spectroscopically similar compounds is illustrated for the simultaneous spectrometric determination of caffeine and theobromine, the primary stimulants in coffee and tea, based on their ultraviolet absorbances. Their analysis indicates that such measurements ...

  8. Development and application of potentiometric stripping analysis

    Directory of Open Access Journals (Sweden)

    Babincev Ljiljana M.

    2017-01-01

    Full Text Available This paper focuses on the voltammetric determination of lead, cadmium and zinc in water. Two ways of determining were investigated: individually and all three metals simultaneously. The experiments were performed using the Potentiometric Stripping Analysis (PSA. Determination of metals in real samples was preceded by preliminary tests. Preliminary investigations were performed in order to determine the optimal conditions of measurement. It was concluded that the process of determining was for most part influenced by: pH, time of metals extraction, stirring rate of the solution and the thickness of the mercury layer on the working electrode. The smallest concentrations of metals which can be determined using this method are: for lead 22.48 μg dm-3, for cadmium 16.23 μg dm-3 and for zinc 18.75 μg dm-3. The obtained results deviated from the actual 1.12% for lead, 1.91% for cadmium and 1.81% for zinc. All tests (individually and simultaneously were conducted from model solution with concentration as follows: 44.96 μg dm-3 for lead, 32.47 μg dm-3 for cadmium and 37.50 μg dm-3 for zinc. The results of individual measurements deviated by 1.02% lead, 1.90% for cadmium and 1.89% for zinc. Simultaneously the contents were lower than real for: -4.58% for lead, cadmium for -1.91% and -1.89% for zinc. For the conditions determined, except for lead, deviations did not exceed ±2% . This indicates that Potentiometric Stripping Analysis is a good way of individual and simultaneous determination of lead, cadmium and zinc and for determination of their concentrations in water (river and groundwater.

  9. Spectrometric assembly for portable installations

    International Nuclear Information System (INIS)

    Kluger, A.; Popescu, C.

    1997-01-01

    The components of the portable spectrometric assembly are: - the detecting probe with Na I(Tl) crystal and air-tight case of industrial type; - a microcomputer; - a unit of analogical processing of the signal from the detecting probe; - a single-channel analyzer with adjustable threshold; - commands and display module; - a source of high voltage; - an electrical supply battery. The device uses the method of gamma photons detection in energetic windows. Through theoretical and experimental studies carried out during the prototype development phase, the superiority of this method has been proved as compared with the installations which make use of the classical principle of photon integral detection. The achieved prototype has a basic program enabling the setting of all working parameters (measuring time, discriminating thresholds, discriminators operating conditions, etc.). Through the included interface RS232 it is possible to transmit the data to a more powerful computer in order to continually process the results. The spectrometric assembly, realized on the basis of micro-computers, can be used in a wide range of applications: measurement of thickness and erosion of walls and tubes, measurement of level in closed containers, of soil density, etc. The adjustment for specific application is performed only through a program modification. (authors)

  10. Potentiometric Titration Method for Quantitative Determination of Hydrogen Peroxide

    National Research Council Canada - National Science Library

    Bessette, Russell R

    2005-01-01

    An electrochemical potentiometric titration method that entails titration of a known volume of a catholyte containing an unknown amount of hydrogen peroxide in a titration cell having two electrodes...

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

    Science.gov (United States)

    Flowers, Paul A.

    1997-07-01

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

  12. New triiodomercurate-modified carbon paste electrode for the potentiometric determination of mercury

    Energy Technology Data Exchange (ETDEWEB)

    Abbas, M.N.; Mostafa, G.A.E

    2003-02-22

    A new tetrazolium-triiodomercurate-modified carbon paste electrode has been described for the sensitive and selective determination of mercury. The electrode shows a stable, near-Nernstian response for 1x10{sup -3} to 6x10{sup -6} M [HgI{sub 3}]{sup -} at 25 deg. C over the pH range of 4.0-9.0, with an anionic slope of 55.5{+-}0.4 mV. The lower detection limit is 4x10{sup -6} M with a fast response time of 30-50 s. Selectivity coefficients of a number of interfering anions and iodo complexes of some metal ions have been estimated. The interference from many of the investigated ions is negligible. The determination of 1-200 {mu}g/ml of mercury in aqueous solutions shows an average recovery of 98.5% and a mean relative standard deviation of 1.6% at 50.0 {mu}g/ml. The direct determination of mercury in spiked wastewater, metal amalgams and dental alloy gave results that compare favorably with those obtained by the cold vapor atomic absorption spectrometric method. Potentiometric titration of mercury and phenylmercury acetate with standard potassium iodide has been monitored using the developed triiodomercurate-carbon paste electrode (CPE) as an end point indicator electrode.

  13. Mass spectrometric detection of radiocarbon for dating applications

    OpenAIRE

    Synal Hans-Arno

    2013-01-01

    Radiocarbon is still the most important nuclide measured by accelerator mass spectrometry (AMS). The related capabilities for dating and tracer studies are eminent not only in archaeology but also drive important applications in the earth and environmental sciences as well as in biomedical research. So far standard mass spectrometric systems have not been capable of radiocarbon dating because of interfering molecular isobars which however can be completely eliminated in charge changing proces...

  14. Electrolyte system strategies for anionic isotachophoresis with electrospray-ionization mass-spectrometric detection. 2. Isotachophoresis in moving-boundary systems

    Czech Academy of Sciences Publication Activity Database

    Gebauer, Petr; Malá, Zdeňka; Boček, Petr

    2013-01-01

    Roč. 34, č. 24 (2013), s. 3245-3251 ISSN 0173-0835 R&D Project s: GA ČR(CZ) GA13-05762S Institutional support: RVO:68081715 Keywords : electrolyte systems * ESI-MS detection * isotachophoresis * moving-boundary electrophoresis Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.161, year: 2013

  15. Potentiometric Membrane Sensors for Levamisole Determination

    Directory of Open Access Journals (Sweden)

    Natalia Zubenya

    2016-11-01

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

  16. Potentiometric Determination of Fluoride Concentration in Beers.

    Science.gov (United States)

    Jaudenes, Juan Ramón; Hardisson, Arturo; Paz, Soraya; Rubio, Carmen; Gutiérrez, Angel José; Burgos, Antonio; Revert, Consuelo

    2018-01-01

    Beer is a widely consumed drink throughout the world, and because its manufacture involves the use of water, beer can be, in some cases, a source of fluorides. For this reason, the objective of this study was to determine the concentration of fluorides in 50 samples of beers from different sources sold in two different types of container (aluminum can and glass bottle). The possible significant differences between the different types of packaging and the intake of fluoride from the consumption of these beers were evaluated. The concentration of fluoride in beers has been determined using the potentiometric method of fluoride determination by standard addition. The concentration of fluoride ranged between 0.06 and 1.77 mg/L. In general, the concentration was below 1 mg/L, except for three beer samples from Ireland and the USA, whose concentration was over 1.5 mg/L. No significant differences were found between the types of packaging. The contribution of fluoride to the diet from beer consumption is not high (<27%); however, it is necessary to warn consumers whenever they are in areas of high concentrations of fluoride in the water supply.

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

    International Nuclear Information System (INIS)

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

    1999-01-01

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

  18. Standard test methods for chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade plutonium nitrate solutions

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2010-01-01

    1.1 These test methods cover procedures for the chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade plutonium nitrate solutions to determine compliance with specifications. 1.2 The analytical procedures appear in the following order: Sections Plutonium by Controlled-Potential Coulometry Plutonium by Amperometric Titration with Iron(II) Plutonium by Diode Array Spectrophotometry Free Acid by Titration in an Oxalate Solution 8 to 15 Free Acid by Iodate Precipitation-Potentiometric Titration Test Method 16 to 22 Uranium by Arsenazo I Spectrophotometric Test Method 23 to 33 Thorium by Thorin Spectrophotometric Test Method 34 to 42 Iron by 1,10-Phenanthroline Spectrophotometric Test Method 43 to 50 Impurities by ICP-AES Chloride by Thiocyanate Spectrophotometric Test Method 51 to 58 Fluoride by Distillation-Spectrophotometric Test Method 59 to 66 Sulfate by Barium Sulfate Turbidimetric Test Method 67 to 74 Isotopic Composition by Mass Spectrom...

  19. Potentiometric Determination of Free Chloride in Cement Paste – an ...

    African Journals Online (AJOL)

    NICO

    Corrosion of rebar in concrete is commonly associated with, and to a large degree influenced by, the free chloride concentration in the pore water. The amount of chloride in concrete is important because chloride can promote corrosion of steel reinforcement when moisture and oxygen are present. A potentiometric ...

  20. POTENTIOMETRIC STUDIES OF NICKEL (II) AND COPPER (II ...

    African Journals Online (AJOL)

    DR. AMINU

    2005) potentiometric studies on manganese (II) and cobalt (II) acetylacetonate complexes, where the two metal complexes have been found to show high formation constant of 9.52 x 1013 and 7.89 x 1013 for the Mn(II) and Co(II) complexes, respectively. In that paper we reported that when exposed to air, the coordination ...

  1. Improving the limits of detection in potentiometric sensors

    NARCIS (Netherlands)

    Bent, Van Der J.F.; Puik, E.C.N.; Tong, H.D.; Rijn, Van C.J.M.

    2015-01-01

    Potentiometric sensors will generally suffer from unwanted responses as a result to changing temperatures by generating an electromotive force. Typically, this voltage drift has a non-linear character and therefore it is difficult to compensate using linear algorithms implemented in the analogue

  2. Potentiometric study of polyaniline film synthesized with various ...

    Indian Academy of Sciences (India)

    Unknown

    The pH was adjusted by adding nitric acid and/or sodium hydroxide and measured by calibrated. pH meter. The electrochemical polymerization of aniline was carried out by potentiometric method in one compartment electro- chemical cell. Platinum was used as a counter electrode. (cathode) and another ITO glass was ...

  3. Potentiometric Determination of Free Chloride in Cement Paste – an ...

    African Journals Online (AJOL)

    NICO

    analysis,10 X-ray fluorescence (XRF),11 and ion chromatography.12. The use of ion selective electrode (ISE) is limited to field determi- nations due to perceptions that it is less accurate and is depend- ent upon the ionic strength and composition of the solution. It is also reported that direct potentiometric readings are known ...

  4. Potentiometric study of polyaniline film synthesized with various ...

    Indian Academy of Sciences (India)

    The potentiometric study of polyaniline (PANI) film synthesized with dopants viz. polyvinyl sulfonic acid (PVS), -toluene sulfonic acid (TS), dodecyl benzene sulfonic acid (DBS) and composite-dopants viz. PVS–TS and PVS–DBS, has been carried out. The synthesized PANI films were characterized by electrochemical ...

  5. Virtual Instrument for an Automated Potentiometric e-Tongue Employing the SIA Technique

    Directory of Open Access Journals (Sweden)

    Manuel del Valle

    2005-12-01

    Full Text Available In this work we report the design, construction, and applications of an electronictongue (abbreviated e-tongue based on an array of potentiometric sensors employing theSequential Injection Analysis technique (SIA operated as a Virtual Instrument implementedin LabVIEW6.1TM. The system can use transient and stationary responses as the measuredinput information for e-tongues. The new concepts applied, lead to different advantages tobe obtained, such as complete automation, easy handling, saving time, reliability andmodularity.

  6. Simultaneous determination of potassium and nitrate ions in mouthwashes using sequential injection analysis with potentiometric detection.

    Science.gov (United States)

    Zárate, N; Irazu, E; Araújo, A N; Montenegro, M C B S M; Pérez-Olmos, R

    2008-06-01

    Two methods for the determination of potassium nitrate in mouthwashes, used against dentin hypersensitivity, have been simultaneously implemented in an sequence injection analysis (SIA) system. In addition to in-line dilution of the samples, the equipment simultaneously detected potassium and nitrate using two tubular potentiometric detectors, selective to each ion, providing a real-time assessment of the quality of the results. Both determinations were shown to be precise and accurate and the obtained results do not statistically differ from those furnished by applying the AES and HPLC reference methods.

  7. Vaporization and thermodynamics of ceramics based on the La2O3-Y2O3-HfO2system studied by the high temperature mass spectrometric method.

    Science.gov (United States)

    Kablov, Eugene N; Stolyarova, Valentina L; Vorozhtcov, Viktor A; Lopatin, Sergey I; Fabrichnaya, Olga В; Ilatovskaya, Mariia O; Karachevtsev, Fedor N

    2018-02-27

    Materials based on the La 2 O 3 -Y 2 O 3 -HfO 2 system are promising for the production of highly refractory ceramics, e.g., thermal barrier coatings and molds for casting of elements of gas turbine engines. When these ceramics are synthesized or used at high temperatures, selective vaporization of components may take place, resulting in changes in the physicochemical The verties of the materials. Consequently, development of materials based on the La 2 O 3 -Y 2 O 3 -HfO 2 system requires information on vaporization in this system as well as on its thermodynamics, without which prediction and modeling of their physicochemical properties are impossible. Vaporization processes and thermodynamic properties in the La 2 O 3 -Y 2 O 3 -HfO 2 system were studied by the high temperature Knudsen effusion mass spectrometric method using a MS-1301 mass spectrometer. Electron ionization of vapor species was employed at an ionization energy of 25 eV. The samples under study and reference substances were vaporized from a tungsten twin effusion cell. At 2337 K the main vapor species over samples in the La 2 O 3 -Y 2 O 3 -HfO 2 system were shown to be LaO, YO and O. The partial pressures of the vapor species mentioned and the La 2 O 3 and Y 2 O 3 activities in the samples were obtained at 2337 K. The Gibbs energies of mixing and excess Gibbs energies were found in the solid solution of this system. Vaporization of ceramics based on the La 2 O 3 -Y 2 O 3 -HfO 2 system at 2337 K led to selective transition of La 2 O 3 and Y 2 O 3 to the gaseous phase, with the La 2 O 3 vaporization rate being higher than that of Y 2 O 3 . The directions of composition changes of samples due to their vaporization at 2337 K were determined. In the solid solution of this system negative deviations from ideal behavior were found. The ability to estimate the excess Gibbs energies in the solid solution of the La 2 O 3 -Y 2 O 3 -HfO 2 system by the Kohler method was shown. This article is protected by

  8. Array of potentiometric sensors for simultaneous determination of copper, silver, and cadmium ions in complex mixtures

    International Nuclear Information System (INIS)

    Shirmardi-Dezaki, Abbas; Shamsipur, Mojtaba; Akhond, Morteza; Sharghi, Hashem; Doroodmand, Mohammad Mahdi

    2012-01-01

    Graphical abstract: - Abstract: A programmed switching system combined with an array of potentiometric sensors consisting of seven potentiometric sensors (i.e., ion-selective or cross-selective electrodes) was connected directly to a pH/potentiometer and a computer (PC) to sequentially acquire the potential corresponding to water sample mixtures. The acquired potentials were recorded and saved on the PC and were used as input variables for an artificial neural network to simultaneously yield the concentrations of Cd 2+ , Cu 2+ , and Ag + in simple and complex mixtures. A feed-forward, back propagation network with a Levenburg–Maquart algorithm was employed to optimize the network parameters. Certain characteristics of each of the seven ion-selective electrodes, including selectivity coefficients, calibration curves, and response times, were also studied. A five-second delay time was used when recording the potentials of the electrodes using the switching system. The array system was also optimized for the selection of the ion-selective electrodes. A four-electrode array system was found to be the best choice for the prediction of Cd 2+ , Ag + and Cu 2+ ion concentration, but application of all seven ion-selective electrodes was necessary for prediction of these primary ions in samples containing a combination of zinc and nickel ions as interfering ions.

  9. High-temperature mass spectrometric study of the vaporization processes and thermodynamic properties of samples in the Bi2O3-P2O5-SiO2system.

    Science.gov (United States)

    Vorozhtcov, Viktor A; Stolyarova, Valentina L; Lopatin, Sergey I; Shugurov, Sergey M; Shilov, Andrey L; Sapega, Vladimir F

    2017-01-15

    The Bi 2 O 3 -P 2 O 5 -SiO 2 system possesses a number of valuable properties that may be of use for various practical applications, both for obtaining new materials, e.g. optical fibers, and for replacing systems based on toxic lead silicate. Information on vaporization processes and thermodynamic properties obtained in the present study will be useful for the development of synthetic methods and approaches for modeling the thermodynamic properties of materials based on this system. High-temperature Knudsen effusion mass spectrometry was used to study the vaporization processes and to determine the thermodynamic properties of the components in the Bi 2 O 3 -P 2 O 5 -SiO 2 system. Measurements were performed with a MS-1301 magnetic sector mass spectrometer. Vaporization was carried out using an iridium-plated molybdenum twin effusion cell containing the sample under study and pure bismuth(III) oxide as a reference substance. Electron ionization at an energy of 30 eV was employed in the study. At a temperature of 950 K, Bi and O 2 were found to be the main vapor species over the samples studied. The Bi 2 O 3 activity as a function of composition in the Bi 2 O 3 -P 2 O 5 -SiO 2 system was derived from the obtained Bi partial pressures. The excess Gibbs energy of the system studied was calculated at 950 K and 1273 K. The possibility of using the Kohler method for the calculation of thermodynamic properties in the Bi 2 O 3 -P 2 O 5 -SiO 2 system was illustrated. The excess Gibbs energy of the Bi 2 O 3 -P 2 O 5 -SiO 2 system obtained in the present study using the Knudsen mass spectrometric method at 950 K and 1273 K demonstrated significant negative deviations from ideal behavior. The excess Gibbs energy values calculated by the Kohler method were shown to be in good agreement with those obtained from experimental data. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  10. Liquid chromatographic-mass spectrometric method for ...

    African Journals Online (AJOL)

    spectrometric (LC-MS/MS) method for the quantitative determination of two dermatological drugs,. Lamisil® (terbinafine) and Proscar® (finasteride), in split tablet dosage form. Methods: Thirty tablets each of the 2 studied medications were randomly selected. Tablets were weighed and divided into 3 groups. Ten tablets of ...

  11. Spectrometric mixture analysis: An unexpected wrinkle

    Indian Academy of Sciences (India)

    Administrator

    Dedicated to the memory of the late Professor S K Rangarajan. Spectrometric mixture analysis: An unexpected wrinkle. †. ROBERT DE LEVIE. Chemistry Department ..... For a quick visual check of the mixture spectra, we plotted the absorbances of those solutions that have a constant value of c + t, such as (0, 180), (90,.

  12. High-temperature mass spectrometric study and modeling of thermodynamic properties of binary glass-forming systems containing Bi2O3.

    Science.gov (United States)

    Stolyarova, V L; Shilov, A L; Lopatin, S I; Shugurov, S M

    2014-04-15

    Binary glass-forming systems containing bismuth(III) oxide, especially the Bi2O3-SiO2 system, are of great importance in modern materials science: preparation of thin films, fiber optics, potential solar converters, and radiation shields in nuclear physics. Information on vaporization processes and thermodynamic properties obtained in the present study and the results of modeling of this system will be useful for optimization of the synthesis and applications of Bi2O3-containing materials at high temperatures. High-temperature Knudsen effusion mass spectrometry was used to study the vaporization processes and to determine the partial pressures of components of the Bi2O3-SiO2 system. Measurements were performed with a MS-1301 mass spectrometer. Vaporization was carried out using two iridium-plated molybdenum effusion cells containing the sample under study and pure bismuth(III) oxide (reference substance). Modeling of the thermodynamic properties and structure of glasses and melts in the Bi2O3-SiO2 and Bi2O3-B2O3 systems was performed using a modified approach based on the generalized lattice theory of associated solutions (GLTAS). At a temperature of 1000 K, Bi and O2 were found to be the main vapor species over the samples studied. The Bi2O3 activity as a function of composition of the Bi2O3-SiO2 system was obtained from the measured partial pressures of the vapor species. The thermodynamic properties of mixing from oxides in this system were calculated. The advantages of GLTAS for modeling of glasses and melts in the binary systems containing Bi2O3 were demonstrated. The thermodynamic functions of mixing in glasses and melts of the Bi2O3-SiO2 system determined at 1000 K in the present study, as well as in the Bi2O3-B2O3 system, demonstrated negative deviations from ideality. Modeling of the obtained experimental data using GLTAS allowed a correlation to be found between the thermodynamic properties and the relative number of bonds of various types formed in

  13. High-temperature mass spectrometric study of the vaporization processes and thermodynamic properties in the Gd2O3-Y2O3-HfO2system.

    Science.gov (United States)

    Kablov, Eugene N; Stolyarova, Valentina L; Lopatin, Sergey I; Vorozhtcov, Viktor A; Karachevtsev, Fedor N; Folomeikin, Yuriy I

    2017-07-15

    The refractory properties of the Gd 2 O 3 -Y 2 O 3 -HfO 2 system are considered promising for the production of many high-temperature materials, e.g., thermal barrier coatings and casting molds for gas turbine engine blades. At high temperatures, components of the Gd 2 O 3 -Y 2 O 3 -HfO 2 system may vaporize selectively and this may significantly change the physicochemical properties of the materials. Therefore, information on vaporization processes and thermodynamic properties of the Gd 2 O 3 -Y 2 O 3 -HfO 2 system is of great importance. The vaporization processes and thermodynamic properties of the Gd 2 O 3 -Y 2 O 3 -HfO 2 system were studied using high-temperature Knudsen effusion mass spectrometry with a MS-1301 mass spectrometer. Vaporization was carried out using a tungsten twin effusion cell containing the samples under study and pure Gd 2 O 3 as a reference substance. Electron ionization at an energy of 25 eV was employed in the present study. It was shown that at a temperature of 2500 K the vapor over the samples in the Gd 2 O 3 -Y 2 O 3 -HfO 2 system consisted of the GdO, YO and O vapor species. The Gd 2 O 3 and Y 2 O 3 activities in the samples in the Gd 2 O 3 -Y 2 O 3 -HfO 2 system as well as their vaporization rates were derived from the partial pressures of the vapor species. Using these data the HfO 2 activities, the Gibbs energy of mixing and the excess Gibbs energy in this system were calculated at 2500 K. The thermodynamic properties of the Gd 2 O 3 -Y 2 O 3 -HfO 2 system, i.e., the component activities in the samples and the excess Gibbs energy, obtained in the present study at 2500 K, exhibited negative deviations from ideal behavior. The concentration dependence of excess Gibbs energy of the Gd 2 O 3 -Y 2 O 3 -HfO 2 system was approximated with an empirical equation. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

  14. Development of a portable mass spectrometric system for determination of isotopic composition of solid uranium samples using fluorine volatilization. Final report

    International Nuclear Information System (INIS)

    Loge, G.

    1994-01-01

    Using hardware and materials supplied by LANL, a prototype quadrupole mass spectrometer system designed for portable field analysis of isotopic composition of solid uranium samples was assembled and tested. The system contained the capability for fluorine volatilization of solid uranium samples with gas introduction, which was successfully tested and demonstrated using 100 mg samples of U 3 O 8 . Determination of precision and accuracy for measuring isotopic composition was performed using isotopic standards. Use with soil samples containing uranium were also attempted. Silicates in the soil forming SiF 4 were found to be a kinetic bottleneck to the formation of UF 6 . This could be avoided by performing some sort of chemical separation as a pre-treatment step, which was demonstrated using nitric acid

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

    Science.gov (United States)

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

    2015-06-02

    Potentiometric sensing utilizing textile-based micro-volume sampling was applied and evaluated for the determination of clinically (Na(+), K(+), Cl(-)) and environmentally (Cd(2+), Pb(2+) and pH) relevant analytes. In this technological design, calibration solutions and samples were absorbed into textiles while the potentiometric cells (ion-selective electrodes and reference electrode) were pressed against the textile. Once the liquid, by wicking action, reached the place where the potentiometric cell was pressed onto the textile, hence closing the electric circuit, the potentiometric response was obtained. Cotton, polyamide, polyester and their blends with elastane were applied for micro-volume sampling. The textiles were found to influence the determination of pH in environmental samples with pH close to neutral and Pb(2+) at low analyte concentrations. On the other hand, textile-based micro-volume sampling was successfully applied in measurements of Na(+) using solid-contact sodium-selective electrodes utilizing all the investigated textiles for sampling. It was found that in order to extend the application of textile-based sampling toward environmental analysis of ions it will be necessary to tailor the physio-chemical properties of the textile materials. In general, textile-based sampling opens new possibilities for direct chemical analysis of small-volume samples and provide a simple and low-cost method to screen various textiles for their effects on samples to identify which textiles are the most suitable for on-body sensing. Copyright © 2015 Elsevier B.V. All rights reserved.

  16. Potentiometric and coulometric titration of 2-thiobarbituric acid.

    Science.gov (United States)

    Ciesielski, W; Kowalska, J; Zakrzewski, R

    1995-05-01

    A new method for the determination of 2-thiobarbituric acid, using its reaction with iodine in an alkaline medium is presented. In the volumetric titration with potentiometric end-point detection, the determinability range is 10-400 micromol (1.4-58 mg). In coulometric titration using the biamperometric end-point detection, 0.1-20 micromol (1.4 x 10(-2)-2.9 mg) of 2-thiobarbituric acid was successfully determined.

  17. Mass spectrometric detection of radiocarbon for dating applications

    Energy Technology Data Exchange (ETDEWEB)

    Synal, H.-A., E-mail: synal@phys.ethz.ch [ETH Zurich, Laboratory of Ion Beam Physics, Building HPK, 8093 Zurich (Switzerland); Schulze-Koenig, T.; Seiler, M.; Suter, M.; Wacker, L. [ETH Zurich, Laboratory of Ion Beam Physics, Building HPK, 8093 Zurich (Switzerland)

    2013-01-15

    Radiocarbon is still the most important nuclide measured by accelerator mass spectrometry (AMS). The related capabilities for dating and tracer studies are eminent not only in archaeology but also drive important applications in the earth and environmental sciences as well as in biomedical research. So far, standard mass spectrometric systems have not been capable of radiocarbon dating because of interfering molecular isobars which, however, can be completely eliminated in charge changing processes at high ion beam energies (MeV) [1,2]. Here, we present a novel type mass spectrometry system for radiocarbon analyses. Radiocarbon dating was performed using 45 keV {sup 14}C ions from the ion source and a molecule dissociation unit kept at ground potential. This proof-of-principle experiment demonstrates for the first time the feasibility of mass spectrometric radiocarbon dating without an accelerator. The results obtained will be the basis of an optimized design for a radiocarbon dating instrument comparable in size, complexity and cost to standard mass spectrometers.

  18. Mass spectrometric detection of radiocarbon for dating applications

    International Nuclear Information System (INIS)

    Synal, H.-A.; Schulze-König, T.; Seiler, M.; Suter, M.; Wacker, L.

    2013-01-01

    Radiocarbon is still the most important nuclide measured by accelerator mass spectrometry (AMS). The related capabilities for dating and tracer studies are eminent not only in archaeology but also drive important applications in the earth and environmental sciences as well as in biomedical research. So far, standard mass spectrometric systems have not been capable of radiocarbon dating because of interfering molecular isobars which, however, can be completely eliminated in charge changing processes at high ion beam energies (MeV) [1,2]. Here, we present a novel type mass spectrometry system for radiocarbon analyses. Radiocarbon dating was performed using 45 keV 14 C ions from the ion source and a molecule dissociation unit kept at ground potential. This proof-of-principle experiment demonstrates for the first time the feasibility of mass spectrometric radiocarbon dating without an accelerator. The results obtained will be the basis of an optimized design for a radiocarbon dating instrument comparable in size, complexity and cost to standard mass spectrometers.

  19. Mass spectrometric detection of radiocarbon for dating applications

    Science.gov (United States)

    Synal, H.-A.; Schulze-König, T.; Seiler, M.; Suter, M.; Wacker, L.

    2013-01-01

    Radiocarbon is still the most important nuclide measured by accelerator mass spectrometry (AMS). The related capabilities for dating and tracer studies are eminent not only in archaeology but also drive important applications in the earth and environmental sciences as well as in biomedical research. So far, standard mass spectrometric systems have not been capable of radiocarbon dating because of interfering molecular isobars which, however, can be completely eliminated in charge changing processes at high ion beam energies (MeV) [1,2]. Here, we present a novel type mass spectrometry system for radiocarbon analyses. Radiocarbon dating was performed using 45 keV 14C ions from the ion source and a molecule dissociation unit kept at ground potential. This proof-of-principle experiment demonstrates for the first time the feasibility of mass spectrometric radiocarbon dating without an accelerator. The results obtained will be the basis of an optimized design for a radiocarbon dating instrument comparable in size, complexity and cost to standard mass spectrometers.

  20. Potentiometric-surface map, 1993, Yucca Mountain and vicinity, Nevada

    International Nuclear Information System (INIS)

    Tucci, P.; Burkhardt, D.J.

    1995-01-01

    The revised potentiometric surface map here, using mainly 1993 average water levels, updates earlier maps of this area. Water levels are contoured with 20-m intervals, with additional 0.5-m contours in the small-gradient area SE of Yucca Mountain. Water levels range from 728 m above sea level SE of Yucca to 1,034 m above sea level north of Yucca. Potentiometric levels in the deeper parts of the volcanic rock aquifer range from 730 to 785 m above sea level. The potentiometric surface can be divided into 3 regions: A small gradient area E and SE of Yucca, a moderate-gradient area on the west side of Yucca, and a large-gradient area to the N-NE of Yucca. Water levels from wells at Yucca were examined for yearly trends (1986-93) using linear least-squares regression. Of the 22 wells, three had significant positive trends. The trend in well UE-25 WT-3 may be influenced by monitoring equipment problems. Tends in USW WT-7 and USW WTS-10 are similar; both are located near a fault west of Yucca; however another well near that fault exhibited no significant trend

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

    Science.gov (United States)

    Kamel, Ayman H

    2015-11-01

    A new potentiometric transducer for selective recognition of azide is characterized and developed. The PVC plasticized based sensor incorporates Mn(II) [2-formylquinoline thiosemicarbazone] complex in the presence of tri dodecyl methyl ammonium chloride (TDMAC) as a lipophilic cationic additive. The sensor displayed a near-Nernstian response for azide over 1.0×10(-2)-1.0×10(-5) mol L(-1), with an anionic slope of -55.8±0.6 mV decade(-1) and lower limit of detection 0.34 µg mL(-1). The sensor was pH independent in the range 5.5-9 and presented good selectivity features towards several inorganic anions, and it is easily used in a flow injection system and compared with a tubular detector. The intrinsic characteristics of the detector in a low dispersion manifold were determined and compared with data obtained under a hydrodynamic mode of operation. This simple and inexpensive automation, with a good potentiometric detector, enabled the analysis of ~33 samples h(-1) without requiring pre-treatment procedures. The proposed method is also applied to the analysis of trace levels of azide in primer mixtures. Significantly improved accuracy, precision, response time, stability and selectivity were offered by these simple and cost-effective potentiometric sensor compared with other standard techniques. The method has the requisite accuracy, sensitivity and precision to determine azide ions. Copyright © 2015 Elsevier B.V. All rights reserved.

  2. Fabrication of SO/sub 2/preparation system and calibration of PINSTECH sulfur standard for /sup 34/S/sup 32/S mass spectrometric analysis

    International Nuclear Information System (INIS)

    Sajjad, M.I.; Latif, Z.; Ali, M.; Qureshi, R.M.; Tasneem, M.A.; Khan, I.H.; Ahmed, M.; Ahmed, I.

    1994-05-01

    This report describes the fabrication and standardization of operation procedures of a SO/sub 2/ preparation system used for the extraction of sulfur dioxide gas from sulfur minerals (aqueous sulfate, elemental sulfur, and sulfides) for sulfur isotope ratio measurements on a gas source mass spectrometer for hydrological, geological and environmental applications. SO/sub 2/ preparation procedure as described by Fumitaka Yanagisawa and Hitoshi Sakai (1983) is adopted with some modifications. A chemically pure BaSO/sub 4/ powder is chosen as PINSTECH Sulfur Standard PSS-I for routine laboratory /sup 34/S analysis. PSS-1 is calibrated against the International Atomic Energy Agency (IAEA) standard Cannon Diablo Troilite (CDT) using the NBS-127 sulfur standard Sigma /sup 34/S values of PSS-1 as analyzed at PINSTECH and Institute fur Hydorlogie, Munich are found to be 14.58 +-0.07 % CDT (n=6) and 14.59+-0.15% CDT (n=2) respectively. NBS-127 is BaSO/sub 4/ powder from the National Bureau of Standards, USA and has been calibrated against CDT. Interlaboratory comparison of various standards is also documented. Using this system, the reproducibility of sulfur isotope ratio measurements is better than +-0.2 % (n=10). (author)

  3. On the Origin of Microheterogeneity : A Mass Spectrometric Study of Dimethyl Sulfoxide-Water Binary Mixture

    NARCIS (Netherlands)

    Shin, Dong Nam; Wijnen, Jan W.; Engberts, Jan B.F.N.; Wakisaka, Akihiro

    2001-01-01

    We have studied the microscopic solvent structure of dimethyl sulfoxide-water mixtures and its influence on the solvation structure of solute from a clustering point of View, by means of a specially designed mass spectrometric system. It was observed that the propensity to the cluster formation is

  4. Determination of evaporation coefficients of melt components of B2O3-GeO2 system by mass-spectrometric method

    International Nuclear Information System (INIS)

    Stolyarova, V.L.; Ambrok, A.G.; Nikolaev, E.N.; Semenov, G.A.

    1977-01-01

    Determined are the evaporation coefficients of the components of a glass-like system constituting boron oxide and germanium dioxide. Measurements were performed from the platinum channel and platinum effusion chamber of a low-temperature evaporator. Evaporation from the platinum channel was assumed to take place from an open surface in accord with Lengmuir, and that from the platinum chamber in accord with Knudsen. The evaporation coefficient was calculated on the basis of the Motzfeldt equation. In boron germanate glasses, the evaporation coefficient of germanium dioxide was shown to differ from the evaporation coefficient of pure germanium dioxide. Within the margin of error involved in the calculations, the evaporation coefficient of boron oxide coincides with the evaporation coefficient of pure boron oxide

  5. On-line sequential injection dispersive liquid-liquid microextraction system for flame atomic absorption spectrometric determination of copper and lead in water samples.

    Science.gov (United States)

    Anthemidis, Aristidis N; Ioannou, Kallirroy-Ioanna G

    2009-06-30

    A simple, sensitive and powerful on-line sequential injection (SI) dispersive liquid-liquid microextraction (DLLME) system was developed as an alternative approach for on-line metal preconcentration and separation, using extraction solvent at microlitre volume. The potentials of this novel schema, coupled to flame atomic absorption spectrometry (FAAS), were demonstrated for trace copper and lead determination in water samples. The stream of methanol (disperser solvent) containing 2.0% (v/v) xylene (extraction solvent) and 0.3% (m/v) ammonium diethyldithiophosphate (chelating agent) was merged on-line with the stream of sample (aqueous phase), resulting a cloudy mixture, which was consisted of fine droplets of the extraction solvent dispersed entirely into the aqueous phase. By this continuous process, metal chelating complexes were formed and extracted into the fine droplets of the extraction solvent. The hydrophobic droplets of organic phase were retained into a microcolumn packed with PTFE-turnings. A portion of 300 microL isobutylmethylketone was used for quantitative elution of the analytes, which transported directly to the nebulizer of FAAS. All the critical parameters of the system such as type of extraction solvent, flow-rate of disperser and sample, extraction time as well as the chemical parameters were studied. Under the optimum conditions the enhancement factor for copper and lead was 560 and 265, respectively. For copper, the detection limit and the precision (R.S.D.) were 0.04 microg L(-1) and 2.1% at 2.0 microg L(-1) Cu(II), respectively, while for lead were 0.54 microg L(-1) and 1.9% at 30.0 microg L(-1) Pb(II), respectively. The developed method was evaluated by analyzing certified reference material and applied successfully to the analysis of environmental water samples.

  6. Towards absolute quantification of allergenic proteins in food--lysozyme in wine as a model system for metrologically traceable mass spectrometric methods and certified reference materials.

    Science.gov (United States)

    Cryar, Adam; Pritchard, Caroline; Burkitt, William; Walker, Michael; O'Connor, Gavin; Burns, Duncan Thorburn; Quaglia, Milena

    2013-01-01

    Current routine food allergen quantification methods, which are based on immunochemistry, offer high sensitivity but can suffer from issues of specificity and significant variability of results. MS approaches have been developed, but currently lack metrological traceability. A feasibility study on the application of metrologically traceable MS-based reference procedures was undertaken. A proof of concept involving proteolytic digestion and isotope dilution MS for quantification of protein allergens in a food matrix was undertaken using lysozyme in wine as a model system. A concentration of lysozyme in wine of 0.95 +/- 0.03 microg/g was calculated based on the concentrations of two peptides, confirming that this type of analysis is viable at allergenically meaningful concentrations. The challenges associated with this promising method were explored; these included peptide stability, chemical modification, enzymatic digestion, and sample cleanup. The method is suitable for the production of allergen in food certified reference materials, which together with the achieved understanding of the effects of sample preparation and of the matrix on the final results, will assist in addressing the bias of the techniques routinely used and improve measurement confidence. Confirmation of the feasibility of MS methods for absolute quantification of an allergenic protein in a food matrix with results traceable to the International System of Units is a step towards meaningful comparison of results for allergen proteins among laboratories. This approach will also underpin risk assessment and risk management of allergens in the food industry, and regulatory compliance of the use of thresholds or action levels when adopted.

  7. Processing of gamma-ray spectrometric logs

    International Nuclear Information System (INIS)

    Umiastowski, K.; Dumesnil, P.

    1984-10-01

    CEA (Commissariat a l'Energie Atomique) has developped a gamma-ray spectrometric tool, containing an analog-to-digital converter. This new tool permits to perform very precise uranium logs (natural gamma-ray spectrometry), neutron activation logs and litho-density logs (gamma-gamma spectrometric logs). Specific processing methods were developped to treate the particular problems of down-hole gamma-ray spectrometry. Extraction of the characteristic gamma-ray peak, even if they are superposed on the background radiation of very high intensity, is possible. This processing methode enables also to obtain geological informations contained in the continuous background of the spectrum. Computer programs are written in high level language for SIRIUS (VICTOR) and APOLLO computers. Exemples of uranium and neutron activation logs treatment are presented [fr

  8. Spectrometric characteristics of polystyrene scintillation films

    CERN Document Server

    Astvatsaturov, A R; Gavalyan, V B; Gavalyan, V G

    1999-01-01

    The spectrometric characteristics of five types of polystyrene scintillation films with thicknesses of 10, 30, 50 and 80 mu m and of analogous 250 mu m thick plates irradiated with sup 2 sup 3 sup 9 Pu, sup 2 sup 3 sup 8 Pu and sup 2 sup 2 sup 6 Ra sources of alpha-particles have been studied. The prospects of utilization of scintillation films as radiators for detection of heavy charged particles and measurement of their energy was experimentally shown.

  9. Development of on-line single-drop micro-extraction sequential injection system for electrothermal atomic absorption spectrometric determination of trace metals

    International Nuclear Information System (INIS)

    Anthemidis, Aristidis N.; Adam, Ibrahim S.I.

    2009-01-01

    A novel automatic sequential injection (SI) single-drop micro-extraction (SDME) system is proposed as versatile approach for on-line metal preconcentration and/or separation. Coupled to electrothermal atomic absorption spectrometry (ETAAS) the potentials of this SI scheme are demonstrated for trace cadmium determination in water samples. A non-charged complex of cadmium with ammonium diethyldithiophosphate (DDPA) was produced and extracted on-line into a 60 μL micro-drop of di-isobutyl ketone (DIBK). The extraction procedure was performed into a newly designed flow-through extraction cell coupled on a sequential injection manifold. As the complex Cd(II)-DDPA flowed continuously around the micro-droplet, the analyte was extracting into the solvent micro-drop. All the critical parameters were optimized and offered good performance characteristics and high preconcentration ratios. For 600 s micro-extraction time, the enhancement factor was 10 and the sampling frequency was 6 h -1 . The detection limit was 0.01 μg L -1 and the precision (RSD at 0.1 μg L -1 of cadmium) was 3.9%. The proposed method was evaluated by analyzing certified reference material

  10. Potentiometric Electrodes in Ocean Monitoring: Past, Present, and Future

    Science.gov (United States)

    Zirino, A.; Kounaves, S. P.; Kirsanov, D.; Martin Hernandez-Ayon, J. M.

    2016-02-01

    It was not until the early 1970's that glass electrodes would be routinely deployed on CTD's and that a moving vessel could obtain oceanographically meaningful horizontal pH profiles by simply pumping seawater into a cell on deck containing an electrode array. pH electrodes in seawater streams improved with continued use. This effect was attributed to the fact that the glass membrane slowly dissolved in the flowing seawater stream, thereby preventing fouling. This effect was also observed for the pressed crystal Cu2+ ISE. In summary, ISE's that are to provide continuously accurate ocean measurements need to be both physically robust and ablative to minimize fouling. Four types of ISE membranes qualify for continuous field use: membranes based on silicate glasses, membranes based on chalcogenide glasses, polycrystalline membranes typically based on pressed mixtures of metal sulfides and PVC-based membranes doped with ionophores for selectivity, and available for a wide variety of ionic and even non-ionic species. The PVC membrane ISE have been made sufficiently robust to changes in temperature and pressure that they have been used to make measurements on the surface of Mars. The last 20 years have seen the development of the "electronic tongue" or ET. The ET is a multisensory system that consists of an array of cross-sensitive chemical sensors (typically potentiometric, but without sharp selectivity) and appropriate chemometric tools for data processing to extract information about analytes in a sample. ET produces a "spectrum-like" response that can be analyzed to yield both quantitative and qualitative information not only of the specific analytes but also of the organic matrix that binds to ions in seawater. This information may lead to an enhanced understanding of microbial/chemical activity from surface to deep sea vents. Electrodes "bundled" into very small packages, and the recent progress in microelectronics and microfluidics indicate that intelligent sensor

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

  12. Open-Source Low-Cost Wireless Potentiometric Instrument for pH Determination Experiments

    Science.gov (United States)

    Jin, Hao; Qin, Yiheng; Pan, Si; Alam, Arif U.; Dong, Shurong; Ghosh, Raja; Deen, M. Jamal

    2018-01-01

    pH determination is an essential experiment in many chemistry laboratories. It requires a potentiometric instrument with extremely low input bias current to accurately measure the voltage between a pH sensing electrode and a reference electrode. In this technology report, we propose an open-source potentiometric instrument for pH determination…

  13. Potentiometric determination of hexavalent uranium in uranium silicide samples

    International Nuclear Information System (INIS)

    Arlegui, Oscar

    1999-01-01

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

  14. Plutonium potentiometric analysis after reduction by copper (I)

    International Nuclear Information System (INIS)

    Anon.

    Plutonium determination in solutions containing fission products and an important amount of uranium (ratio U/Pu = 7), suitable for a mass of plutonium between 5 to 30 mg, by reduction of plutonium to the valency state III with an excess of copper (I) in hydrochloric acid saturated with aluminium chloride and sulfamic acid; molybdemum (VI) and uranium (VI) are not reduced. Copper (I) in excess is titrated potentiometrically with potassium dichromate. Addition of sulfuric-phosphoric acid and oxidation of plutonium to the valency state IV by potassium dichromate by potentiometry. The mass of plutonium is obtained from the volume of dichromate used [fr

  15. Redox behaviour of molybdenum in aqueous medium : a potentiometric study

    International Nuclear Information System (INIS)

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

    1975-01-01

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

  16. Determination of milligram amounts of neptunium by potentiometric titration

    International Nuclear Information System (INIS)

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

    1981-01-01

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

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

    International Nuclear Information System (INIS)

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

    1981-09-01

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

  18. Potentiometric and coulometric titration of 6-propyl-2-thiouracil.

    Science.gov (United States)

    Ciesielski, W; Zakrzewski, R

    1997-05-01

    A method for the determination of 6-propyl-2-thiouracil involving its reaction with iodine in an alkaline medium is presented. In volumetric titration with potentiometric end-point detection, the range of determination is 125-500 mumol (21-85 mg). In coulometric titration using biamperometric end-point detection, 0.5-5.0 mumol (0.085-0.85 mg) of 6-propyl-2-thiouracil was successfully determined. The RSD in all applied techniques was < 1%. The methods developed were applied to the determination of 6-propyl-2-thiouracil in tablets.

  19. Mass spectrometric examinations of Hungarian triassic dolomites

    International Nuclear Information System (INIS)

    Vitalis, Gy.; Kada I-ne

    1982-01-01

    A limited number of mass spectrometric investigations (viz.:57) of representative rock types were applied both in the research work of geology and the mining for the industry of building materials of Hungary. Tabulated results covering all rock types and all stratigraphic levels of the Hungarian Triassic are given. Sr, Mn, Ti and Cr trace elements had the highest occurrence and Zn, Y or Pb, Ba, V or Cu, depending on the genetical type of the rock studied, has relatively higher concentrations as well. The results of the examinations of Hungarian Triassic dolomites were discussed according to genetical types, all represented by a small level of trace elements. (Sz.J.)

  20. Standard test methods for chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade mixed oxides ((U, Pu)O2)

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2010-01-01

    1.1 These test methods cover procedures for the chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade mixed oxides, (U, Pu)O2, powders and pellets to determine compliance with specifications. 1.2 The analytical procedures appear in the following order: Sections Uranium in the Presence of Pu by Potentiometric Titration Plutonium by Controlled-Potential Coulometry Plutonium by Amperometric Titration with Iron (II) Nitrogen by Distillation Spectrophotometry Using Nessler Reagent 7 to 14 Carbon (Total) by Direct Combustion-Thermal Conductivity 15 to 26 Total Chlorine and Fluorine by Pyrohydrolysis 27 to 34 Sulfur by Distillation-Spectrophotometry 35 to 43 Moisture by the Coulometric, Electrolytic Moisture Analyzer 44 to 51 Isotopic Composition by Mass Spectrometry Rare Earths by Copper Spark Spectroscopy 52 to 59 Trace Impurities by Carrier Distillation Spectroscopy 60 to 69 Impurities by Spark-Source Mass Spectrography 70 to 76 Total Gas in Reactor-Grade Mixed Dioxide P...

  1. Evaluation of mass spectrometric techniques for characterization of engineered proteins

    DEFF Research Database (Denmark)

    Roepstorff, P; Schram, K H; Andersen, Jens S.

    1995-01-01

    Mass spectrometric characterization of engineered proteins has been examined using bovine recombinant Acyl-CoA-Binding Protein (rACBP), [15N]-labeled rACBP, and a number of sequence variants of ACBP produced by site-directed mutagenesis. The mass spectrometric techniques include ESIMS and MALDIMS...

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

    International Nuclear Information System (INIS)

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

    1984-01-01

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

  3. Advances in Mass Spectrometric Tools for Probing Neuropeptides

    Science.gov (United States)

    Buchberger, Amanda; Yu, Qing; Li, Lingjun

    2015-07-01

    Neuropeptides are important mediators in the functionality of the brain and other neurological organs. Because neuropeptides exist in a wide range of concentrations, appropriate characterization methods are needed to provide dynamic, chemical, and spatial information. Mass spectrometry and compatible tools have been a popular choice in analyzing neuropeptides. There have been several advances and challenges, both of which are the focus of this review. Discussions range from sample collection to bioinformatic tools, although avenues such as quantitation and imaging are included. Further development of the presented methods for neuropeptidomic mass spectrometric analysis is inevitable, which will lead to a further understanding of the complex interplay of neuropeptides and other signaling molecules in the nervous system.

  4. Potentiometric titration and equivalent weight of humic acid

    Science.gov (United States)

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

    1960-01-01

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

  5. Semi-automated potentiometric titration method for uranium characterization

    Energy Technology Data Exchange (ETDEWEB)

    Cristiano, B.F.G., E-mail: barbara@ird.gov.br [Comissao Nacional de Energia Nuclear (CNEN), Instituto de Radioprotecao e Dosimetria (IRD), Avenida Salvador Allende s/n Recreio dos Bandeirantes, PO Box 37750, Rio de Janeiro, 22780-160 RJ (Brazil); Delgado, J.U.; Silva, J.W.S. da; Barros, P.D. de; Araujo, R.M.S. de [Comissao Nacional de Energia Nuclear (CNEN), Instituto de Radioprotecao e Dosimetria (IRD), Avenida Salvador Allende s/n Recreio dos Bandeirantes, PO Box 37750, Rio de Janeiro, 22780-160 RJ (Brazil); Lopes, R.T. [Programa de Engenharia Nuclear (PEN/COPPE), Universidade Federal do Rio de Janeiro (UFRJ), Ilha do Fundao, PO Box 68509, Rio de Janeiro, 21945-970 RJ (Brazil)

    2012-07-15

    The manual version of the potentiometric titration method has been used for certification and characterization of uranium compounds. In order to reduce the analysis time and the influence of the analyst, a semi-automatic version of the method was developed in the Brazilian Nuclear Energy Commission. The method was applied with traceability assured by using a potassium dichromate primary standard. The combined standard uncertainty in determining the total concentration of uranium was around 0.01%, which is suitable for uranium characterization. - Highlights: Black-Right-Pointing-Pointer We developed a semi-automatic version of potentiometric titration method. Black-Right-Pointing-Pointer The method is used for certification and characterization of uranium compounds. Black-Right-Pointing-Pointer The traceability of the method was assured by a K{sub 2}Cr{sub 2}O{sub 7} primary standard. Black-Right-Pointing-Pointer The results of U{sub 3}O{sub 8} reference material analyzed was consistent with certified value. Black-Right-Pointing-Pointer The uncertainty obtained, near 0.01%, is useful for characterization purposes.

  6. A Urea Potentiometric Biosensor Based on a Thiophene Copolymer

    Directory of Open Access Journals (Sweden)

    Cheng-Yuan (Kevin Lai

    2017-03-01

    Full Text Available A potentiometric enzyme biosensor is a convenient detector for quantification of urea concentrations in industrial processes, or for monitoring patients with diabetes, kidney damage or liver malfunction. In this work, poly(3-hexylthiophene-co-3-thiopheneacetic acid (P(3HT-co-3TAA was chemically synthesized, characterized and spin-coated onto conductive indium tin oxide (ITO glass electrodes. Urease (Urs was covalently attached to the smooth surface of this copolymer via carbodiimide coupling. The electrochemical behavior and stability of the modified Urs/P(3HT-co-3TAA/ITO glass electrode were investigated by cyclic voltammetry, and the bound enzyme activity was confirmed by spectrophotometry. Potentiometric response studies indicated that this electrode could determine the concentration of urea in aqueous solutions, with a quasi-Nernstian response up to about 5 mM. No attempt was made to optimize the response speed; full equilibration occurred after 10 min, but the half-time for response was typically <1 min.

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

    Energy Technology Data Exchange (ETDEWEB)

    1986-07-01

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

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

    International Nuclear Information System (INIS)

    1986-07-01

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

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

    International Nuclear Information System (INIS)

    Tasleem, S.; Ishrat, B.

    2008-01-01

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

  10. Potentiometric titration of free acid in uranium solutions

    Energy Technology Data Exchange (ETDEWEB)

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

    1998-02-01

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

  11. Limitations of potentiometric oxygen sensors operating at low oxygen levels

    DEFF Research Database (Denmark)

    Lund, Anders; Jacobsen, Torben; Hansen, Karin Vels

    2011-01-01

    The electrochemical processes that limit the range of oxygen partial pressures in which potentiometric oxygen sensors can be used, were analysed using a theoretical and an experimental approach. Electrochemical impedance spectroscopy was performed on porous Pt/yttria stabilised zirconia (YSZ......) electrodes between 10−6 and 0.2 bar and at temperatures between 500 and 950 °C. The flow of oxide ions and electron holes through a sensor cell, with a YSZ electrolyte, were calculated under similar conditions. The oxygen permeation of the sensor cell was insignificant at an oxygen partial pressure of 10......−6 bar for an inlet flow rate higher than 2 L h−1 between 600 and 800 °C. The polarisation resistance measured between 10−6 and 10−4 bar was found to be inversely proportional to the oxygen partial pressure, nearly temperature independent and inversely proportional to the inlet gas flow rate, which shows...

  12. An accurate potentiometric titration of 5-25 mg uranium

    International Nuclear Information System (INIS)

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

    1976-01-01

    A potentiometric titration of 5 to 25 mg uranium is described. Sulphamic and phosphoric acid are added to the sample (volume 1 ml), U VI is reduced to U IV by Fe 2+ and the excess of Fe 2+ is oxidized by a mixture of nitric acid, sulphamic acid and ammonium molybdate; vanadyl sulphate is added to ensure a sharp end-point of the titration. The resultant U IV is titrated automatically with 0.02500N potassiumdichromate using a platinum indicator electrode. The automatic titration is performed both with a commercial titrator (Mettler) and with an R.C.N. titrator which waits after each addition until the equilibrium is reached. Using the Mettler titrator an accuracy of 0.05% relative was reached. The R.C.N. setpoint titrator gave results with an accuracy of 0.04% relative at the 20-mg U level. Each titration takes 5 to 7 min. (author)

  13. CHEMICALLY MODIFIED FIELD-EFFECT TRANSISTORS - POTENTIOMETRIC AG+ SELECTIVITY OF PVC MEMBRANES BASED ON MACROCYCLIC THIOETHERS

    NARCIS (Netherlands)

    BRZOZKA, Z; COBBEN, PLHM; REINHOUDT, DN; EDEMA, JJH; KELLOGG, RM

    1993-01-01

    A chemically modified field-effect transistor (CHEMFET) with satisfactory Ag+ selectivity is described. The potentiometric Ag+ selectivities of CHEMFETs with plasticized PVC membranes based on macrocyclic thioethers have been determined. All the macrocyclic thioethers tested showed silver response

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

  15. Energy dispersive X-Ray fluorescence spectrometric study of ...

    African Journals Online (AJOL)

    Energy dispersive X-Ray fluorescence spectrometric study of compositional differences in trace elements in dried Moringa oleifera leaves grown in two different agro-ecological locations in Ebonyi State, Nigeria.

  16. Improved Performance of the Potentiometric Biosensor for the Determination of Creatinine

    DEFF Research Database (Denmark)

    Andersen, Jens Enevold Thaulov; Rasmussen, Claus/Dallerup; Zachau-Christiansen, Birgit

    2007-01-01

    The development of potentiometric biosensors for the determination of creatinine is attractive because it is a frequently analysed species in clinical chemistry. Contemporary methods of analysing creatinine engage chemicals harmful to the environment and generate large volumes of waste disposals....... By introducing a membrane-based potentiometric biosensor with immobilised creatinine deaminase, the measurements can be performed by miniaturised portable devices that are easy to handle and allow rapid analysis at a minimum consumption of chemicals. Thus, the enzymatic creatinine biosensors was revisited...

  17. Potentiometric titration of zinc and cadmium in electrolytes of in galvanic baths

    International Nuclear Information System (INIS)

    Kosyuga, E.A.; Kalugin, A.A.; Gur'ev, I.A.

    1979-01-01

    The method of potentiometric titration of zinc and cadmium by complexone 3 in electrolytes of galvanic baths using sulphide - silver electrode for determining the finite point of titration is suggested. Copper (2) ions are proposed as indicator ions. The potentiometric determination should be performed at pH=10. The method is verified on model electrolyte solutions and on the electrolyte solutions of operating baths.The technique can be used for automatic control. The time for analysis is 10 minutes

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

    Science.gov (United States)

    Price, Randi; Wan, Ping

    2010-01-01

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

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

    International Nuclear Information System (INIS)

    1984-03-01

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

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

    International Nuclear Information System (INIS)

    Nery, Emilia Witkowska; Kubota, Lauro T.

    2016-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Nery, Emilia Witkowska, E-mail: ewitkowskanery@ichf.edu.pl [Department of Analytical Chemistry, Institute of Chemistry – UNICAMP, P.O. Box 6154, 13084-971 Campinas, SP (Brazil); National Institute of Science and Technology in Bioanalytics, Institute of Chemistry – UNICAMP, P.O. Box 6154, Campinas (Brazil); Kubota, Lauro T. [Department of Analytical Chemistry, Institute of Chemistry – UNICAMP, P.O. Box 6154, 13084-971 Campinas, SP (Brazil); National Institute of Science and Technology in Bioanalytics, Institute of Chemistry – UNICAMP, P.O. Box 6154, Campinas (Brazil)

    2016-04-28

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

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

    Science.gov (United States)

    Nery, Emilia Witkowska; Kubota, Lauro T

    2016-04-28

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

  3. Status of mass spectrometric radiocarbon detection at ETHZ

    Energy Technology Data Exchange (ETDEWEB)

    Seiler, Martin; Maxeiner, Sascha; Wacker, Lukas; Synal, Hans-Arno

    2015-10-15

    A prototype of a mass spectrometric radiocarbon detection instrument without accelerator stage was built for the first time and set into operation at ETH Zurich. The system is designed as an experimental platform to optimize performance of {sup 14}C detection at low ion energies and to study the most relevant processes that may limit system performance. The optimized stripper unit incorporates differential pumping to maintain a low gas outflow and a revised tube design to better match the phase space volume of the ion beam at low energies. The system is fully operational and has demonstrated true radiocarbon dating capabilities. The overall beam transmission through the stripper tube is about 40% for the 1{sup +} charge state. Radiocarbon analyses with an overall precision of 0.6% were obtained on a single sample under regular measurement conditions. By analyzing multiple targets of the same sample material an uncertainty level of 0.3% has been reached. The background level corresponds to a radiocarbon age of 40,000 years.

  4. Stepwise injection potentiometric determination of caffeine in saliva using single-drop microextraction combined with solvent exchange.

    Science.gov (United States)

    Timofeeva, I; Medinskaia, K; Nikolaeva, L; Kirsanov, D; Bulatov, A

    2016-04-01

    A flow potentiometric method for determination of caffeine in saliva is suggested. This task is important for non-invasive assessment of drug metabolizing system activity in hepatocytes. In the current study, stepwise injection analysis (SWIA) was successfully combined with single-drop liquid microextraction (SDLME) and solvent exchange procedure. The method is based on the caffeine SDLME with subsequent solvent evaporation and dissolution of analyte in sulfuric acid followed by potentiometric detection using poly(vinyl chloride) membrane electrode containing potassium tetrakis[3,5-bis(trifluoromethyl)phenyl]borate as electroactive component. SDLME was employed for elimination of interfering matrix effects of saliva and caffeine metabolites such as theophylline, theobromine and paraxanthine. A linear range of 10(-5)-10(-2)M was established for caffeine with detection limit at 6 × 10(-6)M. The sample throughput was 6 samples h(-1). The proposed method was successfully applied to the determination of caffeine in saliva and the analytical results agreed well with the results obtained with reference HPLC method. Copyright © 2016 Elsevier B.V. All rights reserved.

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

  6. Mass Spectrometric C-14 Detection Techniques: Progress Report

    Science.gov (United States)

    Synal, H.

    2013-12-01

    Accelerator Mass Spectrometry (AMS) has been established as the best-suited radiocarbon detection technique. In the past years, significant progress with AMS instrumentation has been made resulting in a boom of new AMS facilities around the World. Today, carbon only AMS systems predominantly utilize 1+ charge state and molecule destruction in multiple ion gas collisions in stripper gas cell. This has made possible a significant simplification of the instruments, a reduction of ion energies and related to this less required space of the installations. However, state-of-the-art AMS instruments have still not reached a development stage where they can be regarded as table-top systems. In this respect, more development is needed to further advance the applicability of radiocarbon not only in the traditional fields of dating but also in biomedical research and new fields in Earth and environmental sciences. In a the proof-of-principle experiment the feasibility of radiocarbon detection over the entire range of dating applications was demonstrated using a pure mass spectrometer and ion energies below 50 keV. Now an experimental platform has been completed to test performance and to explore operation and measurement conditions of pure mass spectrometric radiocarbon detection. This contribution will overview the physical principles, which make this development possible and discuss key parameters of the instrumental design and performance of such an instrument.

  7. Potentiometric polymeric membrane electrodes for mercury detection using calixarene ionophores.

    Science.gov (United States)

    Tyagi, Sonika; Agarwal, Himanshu; Ikram, Saiqa

    2010-01-01

    It is here established that potentiometric polymeric membrane electrodes based on electrically neutral ionophores are a useful analytical tool for the detection of heavy metal ions from environmental and industrial waste water. PVC based membrane containing p-tert-butyl-calix[4]arenethioether derivative as active material along with sodiumtetraphenylborate (NaTPB) as solvent mediator and dibutylphthalate as a plasticizer in the ratio 45:9:460:310 (w/w%) (I:NaTPB:DBP:PVC) exhibits good properties with a Nernstian response of 29.50+/-1.0 mV per decade of activity and a working concentration range of 7.2 x 10(-8)-1.0 x 10(-1) M. The electrode gave more stable potential readings when used around pH 2.5-6.8 and exhibits fast response time of 14 s. The sensors were found to work satisfactorily in partially non-aqueous media up to 40% (v/v) content of acetone, methanol or ethanol and could be used over a period of 7-9 months. Excellent selectivity for Hg(2+) ions is indicated by match potential method and fixed interference method. The sensors could be used successfully in the estimation of mercury in different sample.

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

    International Nuclear Information System (INIS)

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

    1990-01-01

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

  9. Numerical bias estimation for mass spectrometric mass isotopomer analysis.

    Science.gov (United States)

    Yang, Tae Hoon; Bolten, Christoph J; Coppi, Maddalena V; Sun, Jun; Heinzle, Elmar

    2009-05-15

    Mass spectrometric (MS) isotopomer analysis has become a standard tool for investigating biological systems using stable isotopes. In particular, metabolic flux analysis uses mass isotopomers of metabolic products typically formed from (13)C-labeled substrates to quantitate intracellular pathway fluxes. In the current work, we describe a model-driven method of numerical bias estimation regarding MS isotopomer analysis. Correct bias estimation is crucial for measuring statistical qualities of measurements and obtaining reliable fluxes. The model we developed for bias estimation corrects a priori unknown systematic errors unique for each individual mass isotopomer peak. For validation, we carried out both computational simulations and experimental measurements. From stochastic simulations, it was observed that carbon mass isotopomer distributions and measurement noise can be determined much more precisely only if signals are corrected for possible systematic errors. By removing the estimated background signals, the residuals resulting from experimental measurement and model expectation became consistent with normality, experimental variability was reduced, and data consistency was improved. The method is useful for obtaining systematic error-free data from (13)C tracer experiments and can also be extended to other stable isotopes. As a result, the reliability of metabolic fluxes that are typically computed from mass isotopomer measurements is increased.

  10. Mass Spectrometric Immunoassays in Characterization of Clinically Significant Proteoforms

    Directory of Open Access Journals (Sweden)

    Olgica Trenchevska

    2016-03-01

    Full Text Available Proteins can exist as multiple proteoforms in vivo, as a result of alternative splicing and single-nucleotide polymorphisms (SNPs, as well as posttranslational processing. To address their clinical significance in a context of diagnostic information, proteoforms require a more in-depth analysis. Mass spectrometric immunoassays (MSIA have been devised for studying structural diversity in human proteins. MSIA enables protein profiling in a simple and high-throughput manner, by combining the selectivity of targeted immunoassays, with the specificity of mass spectrometric detection. MSIA has been used for qualitative and quantitative analysis of single and multiple proteoforms, distinguishing between normal fluctuations and changes related to clinical conditions. This mini review offers an overview of the development and application of mass spectrometric immunoassays for clinical and population proteomics studies. Provided are examples of some recent developments, and also discussed are the trends and challenges in mass spectrometry-based immunoassays for the next-phase of clinical applications.

  11. Electrolyte system strategies for anionic isotachophoresis with electrosprayionization mass-spectrometric detection. 3. The ITP spacer technique in moving-boundary systems and configurations with two self-maintained ITP subsystems

    Czech Academy of Sciences Publication Activity Database

    Gebauer, Petr; Malá, Zdeňka; Boček, Petr

    2014-01-01

    Roč. 35, č. 5 (2014), s. 746-754 ISSN 0173-0835 R&D Project s: GA ČR(CZ) GA13-05762S Keywords : electrolyte systems * ESI-MS detection * moving-boundary electrophoresis * spacers * ITP Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.028, year: 2014

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

    Energy Technology Data Exchange (ETDEWEB)

    Engmann, J.; Blanch, H.W.; Prausnitz, J.M. [Univ. of California, Berkeley, CA (United States). Dept. of Chemical Engineering]|[Lawrence Berkeley National Lab., CA (United States). Chemical Sciences Div.

    1997-03-01

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

  13. Determining a Solubility Product Constant by Potentiometric Titration to Increase Students' Conceptual Understanding of Potentiometry and Titrations

    Science.gov (United States)

    Grabowski, Lauren E.; Goode, Scott R.

    2017-01-01

    Potentiometric titrations are widely taught in first-year undergraduate courses to connect electrochemistry, stoichiometry, and equilibria and to reinforce acid-base titrations. Students perform a potentiometric titration that is then analyzed to determine analyte concentrations and the solubility product constant of the solid species.

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

    Directory of Open Access Journals (Sweden)

    A. HAKAN AKTAŞ

    2008-01-01

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

  15. Biocompatible Poly(catecholamine)-Film Electrode for Potentiometric Cell Sensing.

    Science.gov (United States)

    Kajisa, Taira; Yanagimoto, Yoshiyuki; Saito, Akiko; Sakata, Toshiya

    2018-02-23

    Surface-coated poly(catecholamine) (pCA) films have attracted attention as biomaterial interfaces owing to their biocompatible and physicochemical characteristics. In this paper, we report that pCA-film-coated electrodes are useful for potentiometric biosensing devices. Four different types of pCA film, l-dopa, dopamine, norepinephrine, and epinephrine, with thicknesses in the range of 7-27 nm were electropolymerized by oxidation on Au electrodes by using cyclic voltammetry. By using the pCA-film electrodes, the pH responsivities were found to be 39.3-47.7 mV/pH within the pH range of 1.68 to 10.01 on the basis of the equilibrium reaction with hydrogen ions and the functional groups of the pCAs. The pCA films suppressed nonspecific signals generated by other ions (Na + , K + , Ca 2+ ) and proteins such as albumin. Thus, the pCA-film electrodes can be used in pH-sensitive and pH-selective biosensors. HeLa cells were cultivated on the surface of the pCA-film electrodes to monitor cellular activities. The surface potential of the pCA-film electrodes changed markedly because of cellular activity; therefore, the change in the hydrogen ion concentration around the cell/pCA-film interface could be monitored in real time. This was caused by carbon dioxide or lactic acid that is generated by cellular respiration and dissolves in the culture medium, resulting in the change of hydrogen concentration. pCA-film electrodes are suitable for use in biocompatible and pH-responsive biosensors, enabling the more selective detection of biological phenomena.

  16. Potentiometric sensor for Betahistine determination in pharmaceuticals, urine and blood serum

    OpenAIRE

    Ensafi,Ali A.; Doozandeh,Fatemeh; Allafchian,Ali R.

    2010-01-01

    The construction, evaluation and analytical application of a new potentiometric sensor for the determination of betahistine are described. The membrane electrode acts based on betahistine-tetraphenylborate ion-exchangers as electroactive material. This electrode has a linear dynamic range between 1.0 x 10-6-1.0 x 10-1 mol L-1 betahistine with a Nernstian slope of (29.74 ± 1.47) mV decade-1 and a detection limit of 5.8 x 10-7 mol L-1. The potentiometric response is independent of the pH of the...

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

    Science.gov (United States)

    Y Lmaz, Demet; Karaku, Emine

    2011-12-01

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

  18. pH-based Detection of Phenylalnine by Potentiometric and Colorimetric Methods

    Directory of Open Access Journals (Sweden)

    Elżbieta Remiszewska

    2006-04-01

    Full Text Available In this paper, methods of sample preparation for potentiometric measurement ofphenylalanine are presented. Basing on the spectrophotometric measurements ofphenylalanine, the concentrations of reagents of the enzymatic reaction (10 mM L-Phe,0,4 mM NAD+ , 2U L-PheDH were determined. Then, the absorption spectrum of thereaction product, NADH, was monitored (maximum peak at 340 nm. The results obtainedby the spectrophotometric method were compared with the results obtained by thecolourimetry, using pH indicators. The above-mentioned two methods will be used asreferences for potentiometric measurements of phenylalanine concentration.

  19. pH-based Detection of Phenylalnine by Potentiometric and Colorimetric Methods

    Science.gov (United States)

    Pijanowska, Dorota G.; Remiszewska, El żbieta

    2006-01-01

    In this paper, methods of sample preparation for potentiometric measurement of phenylalanine are presented. Basing on the spectrophotometric measurements of phenylalanine, the concentrations of reagents of the enzymatic reaction (10 mM L-Phe, 0,4 mM NAD+, 2U L-PheDH) were determined. Then, the absorption spectrum of the reaction product, NADH, was monitored (maximum peak at 340 nm). The results obtained by the spectrophotometric method were compared with the results obtained by the colourimetry, using pH indicators. The above-mentioned two methods will be used as references for potentiometric measurements of phenylalanine concentration.

  20. Use of 3-(4-hydroxyphenyl)propionic acid as electron donating compound in a potentiometric aflatoxin M1-immunosensor

    International Nuclear Information System (INIS)

    Rameil, Steffen; Schubert, Peter; Grundmann, Peter; Dietrich, Richard; Maertlbauer, Erwin

    2010-01-01

    We developed a potentiometric aflatoxin M 1 -immunosensor which utilizes 3-(4-hydroxyphenyl)propionic acid (p-HPPA) as electron donating compound for horseradish peroxidase (HRP; EC 1.11.1.7). The assay system consists of a polypyrrole-surface-working electrode coated with a polyclonal anti-M 1 antibody (pAb-AFM 1 ), a Ag/AgCl reference electrode and a HRP-aflatoxin B 1 conjugate (HRP-AFB 1 conjugate). To optimize the potentiometric measuring system p-HPPA as well as related compounds serving as electron donating compounds were compared. Also the influence of different buffer systems, varying pH and substrate concentrations on signal intensity was investigated. Our results suggest that reaction conditions that favor the formation of Pummerer's type ketones lead to an increase in signal intensity rather than formation of fluorescent dye. Comparison with commercial ready-to-use HRP electron donating compounds such as 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) diammonium salt (ABTS), o-phenylenediamine (OPD) or 3,3',5,5'-tetramethylbenzidine (TMB) showed that only 34%, 77% and 49% of the signal intensity of p-HPPA were reached, respectively. The optimized assay had a detection limit of 40 pg mL -1 and allowed detection of 500 pg mL -1 (FDA action limit) aflatoxin M 1 (AFM 1 ) in pasteurized milk and UHT-milk containing 0.3-3.8% fat within 10 min without any sample treatment. The working range was between 250 and 2000 pg mL -1 AFM 1 .

  1. Potentiometric, UV and 1H NMR study on the interaction of Cu2+ with ampicillin and amoxicillin in aqueous solution.

    Science.gov (United States)

    Cardiano, Paola; Crea, Francesco; Foti, Claudia; Giuffrè, Ottavia; Sammartano, Silvio

    2017-05-01

    A potentiometric, UV and 1 H NMR study on Cu 2+ -ampicillin [(2S,5R,6R)-6-([(2R)-2-amino-2-phenylacetyl]amino)-3,3-dimethyl-7-oxo-4-thia-1-azabicyclo[3.2.0]heptane-2-carboxylic acid] and -amoxicillin [(2S,5R,6R)-6-{[(2R)-2-amino-2-(4-hydroxyphenyl)-acetyl]amino}-3,3-dimethyl-7-oxo-4-thia-1-azabicyclo[3.2.0]heptane-24-carboxylic acid] systems in NaCl aqueous solution at I=0.15molL -1 and t=25°C is reported. On the basis of potentiometric results two speciation models were proposed for each system. It was found that spectrophotometric and 1 H NMR measurements are essential for selecting the most reliable speciation models. They included ML, MLOH and ML(OH) 2 species in both systems and, only for Cu 2+ -ampicillin, also MLH species. The stability constants obtained by UV and 1 H NMR titrations were comparable to the ones calculated by potentiometry. The sequestering ability of the ligands under study towards Cu 2+ by pL 0.5 empiric parameter (ligand concentration required to sequester 50% of the metal cation present in traces) at several pH values was calculated as well. For ampicillin and amoxicillin, pL 0.5 =7.19 and 6.67, respectively, at physiological pH, I=0.15molL -1 and t=25°C were obtained. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. Experimental characterization of the Clear-PEM scanner spectrometric performance

    Science.gov (United States)

    Bugalho, R.; Carriço, B.; Ferreira, C. S.; Frade, M.; Ferreira, M.; Moura, R.; Ortigão, C.; Pinheiro, J. F.; Rodrigues, P.; Rolo, I.; Silva, J. C.; Trindade, A.; Varela, J.

    2009-10-01

    In the framework of the Clear-PEM project for the construction of a high-resolution and high-specificity scanner for breast cancer imaging, a Positron Emission Mammography tomograph has been developed and installed at the Instituto Português de Oncologia do Porto hospital. The Clear-PEM scanner is mainly composed by two planar detector heads attached to a robotic arm, trigger/data acquisition electronics system and computing servers. The detector heads hold crystal matrices built from 2 × 2 × 20 mm3 LYSO:Ce crystals readout by Hamamatsu S8550 APD arrays. The APDs are optically coupled to both ends of the 6144 crystals in order to extract the DOI information for each detected event. Each one of 12288 APD's pixels is read and controlled by Application Specific Integrated Circuits water-cooled by an external cooling unit. The Clear-PEM frontend boards innovative design results in a unprecedented integration of the crystal matrices, APDs and ASICs, making Clear-PEM the PET scanner with the highest number of APD pixels ever integrated so far. In this paper, the scanner's main technical characteristics, calibration strategies and the first spectrometric performance evaluation in a clinical environment are presented. The first commissioning results show 99.7% active channels, which, after calibration, have inter-pixel and absolute gain distributions with dispersions of, respectively, 12.2% and 15.3%, demonstrating that despite the large number of channels, the system is uniform. The mean energy resolution at 511 keV is of 15.9%, with a 8.8% dispersion, and the mean CDOI-1 is 5.9%/mm, with a 7.8% dispersion. The coincidence time resolution, at 511 keV, for a energy window between 400 and 600 keV, is 5.2 ns FWHM.

  3. Experimental characterization of the Clear-PEM scanner spectrometric performance

    Energy Technology Data Exchange (ETDEWEB)

    Bugalho, R; Carrico, B; Ferreira, C S; Frade, M; Ferreira, M; Moura, R; Ortigao, C; Pinheiro, J F; Rodrigues, P; Rolo, I; Silva, J C; Trindade, A; Varela, J [Laboratorio de Instrumentacao e Fisica Experimental de Particulas (LIP), Av. Elias Garcia 14-1, 1000-149 Lisboa (Portugal)], E-mail: frade@lip.pt

    2009-10-15

    In the framework of the Clear-PEM project for the construction of a high-resolution and high-specificity scanner for breast cancer imaging, a Positron Emission Mammography tomograph has been developed and installed at the Instituto Portugues de Oncologia do Porto hospital. The Clear-PEM scanner is mainly composed by two planar detector heads attached to a robotic arm, trigger/data acquisition electronics system and computing servers. The detector heads hold crystal matrices built from 2 x 2 x 20 mm{sup 3} LYSO:Ce crystals readout by Hamamatsu S8550 APD arrays. The APDs are optically coupled to both ends of the 6144 crystals in order to extract the DOI information for each detected event. Each one of 12288 APD's pixels is read and controlled by Application Specific Integrated Circuits water-cooled by an external cooling unit. The Clear-PEM frontend boards innovative design results in a unprecedented integration of the crystal matrices, APDs and ASICs, making Clear-PEM the PET scanner with the highest number of APD pixels ever integrated so far. In this paper, the scanner's main technical characteristics, calibration strategies and the first spectrometric performance evaluation in a clinical environment are presented. The first commissioning results show 99.7% active channels, which, after calibration, have inter-pixel and absolute gain distributions with dispersions of, respectively, 12.2% and 15.3%, demonstrating that despite the large number of channels, the system is uniform. The mean energy resolution at 511 keV is of 15.9%, with a 8.8% dispersion, and the mean C{sub DOI}{sup -1} is 5.9%/mm, with a 7.8% dispersion. The coincidence time resolution, at 511 keV, for a energy window between 400 and 600 keV, is 5.2 ns FWHM.

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

    Science.gov (United States)

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

    2013-07-15

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

  5. Preparation and spectrometric identification of amide derivatives with antimalaric

    International Nuclear Information System (INIS)

    Ferreira, E.J.

    1987-01-01

    The structures of polymeric compounds using spectrometric analysis of infrared, ultraviolet and protonic magnetic resonance and 13 C nuclear magnetic resonance are studied. Some structural models are used such as antimalaric-sulfones and pyrimidinic derivatives, and non-polymeric derivatives of active compounds. A comparative analysis on structures less complexes is shown. (M.J.C.). Spectrums 186 p [pt

  6. Spectrometric determination of ammonium-nitrogen with quinol in ...

    African Journals Online (AJOL)

    Quinol is proposed as a reagent for the spectrometric determination of ammonium-nitrogen (NH4+-N) in aqueous medium. Quinol forms a pink complex with ammonium salt in aqueous medium. Hydrogen peroxide is needed for colour accentuation. The quinol/ammonium charge transfer complex has absorption maximum ...

  7. Partial least squares−near infrared spectrometric determination of ...

    African Journals Online (AJOL)

    Partial least squares−near infrared spectrometric determination of ethanol in distilled alcoholic beverages. ... Derivative, mean centering and subtracting minimum value were used as data treatment techniques for noise reduction and baseline correction. Mean centering has given the best partial least squares model with ...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-07-01

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

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

    International Nuclear Information System (INIS)

    Saefurohman, Asep; Buchari,; Noviandri, Indra; Syoni

    2014-01-01

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

  10. potentiometric studies of the complexes formed by copper (ii) and zinc

    African Journals Online (AJOL)

    MBI

    proline, threonine and asparagines were determined by potentiometric titration in aqueous solution. The values of the constants were found using ORIGIN 50 program computational ... have polar uncharged groups. The constants obtained will help in the understanding of the function and efficiency of copper and zinc in.

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

  12. BIOSENSOR FOR DIRECT DETERMINATION OF ORGANOPHOSPHATE NERVE AGENTS. 1. POTENTIOMETRIC ENZYME ELECTRODE. (R823663)

    Science.gov (United States)

    A potentiometric enzyme electrode for the direct measurement of organophosphate (OP)nerve agents was developed. The basic element of this enzyme electrode was a pH electrodemodified with an immobilized organophosphorus hydrolase (OPH) layer formed by cross-linkingOPH ...

  13. Computer analysis of potentiometric data of complexes formation in the solution

    Science.gov (United States)

    Jastrzab, Renata; Kaczmarek, Małgorzata T.; Tylkowski, Bartosz; Odani, Akira

    2018-02-01

    The determination of equilibrium constants is an important process for many branches of chemistry. In this review we provide the readers with a discussion on computer methods which have been applied for elaboration of potentiometric experimental data generated during complexes formation in solution. The review describes both: general basis of modeling tools and examples of the use of calculated stability constants.

  14. Lead in Hair and in Red Wine by Potentiometric Stripping Analysis: The University Students' Design.

    Science.gov (United States)

    Josephsen, Jens

    1985-01-01

    A new program for training upper secondary school chemistry teachers (SE 537 693) depends heavily on student project work. A project in which lead in hair and in red wine was examined by potentiometric stripping analysis is described and evaluated. (JN)

  15. Reversible potentiometric oxygen sensors based on polymeric and metallic film electrodes.

    Science.gov (United States)

    Yim, H S; Meyerhoff, M E

    1992-09-01

    Various materials and sensor configurations that exhibit reversible potentiometric responses to the partial pressure of oxygen at room temperature in neutral pH solution are examined. In one arrangement, platinum electrodes are coated with plasticized poly(vinyl chloride) films doped with a cobalt(II) tetraethylene pentamine complex. For such sensors, potentiometric oxygen response is attributed to a mixed potential originating from the underlying platinum electrode surface as well as a change in redox potential of the Co(II)-tetren-doped film as the complex binds oxygen reversibly. The response due to the platinum surface is prolonged by the presence of the Co(II)-tetren/PVC film. Alternately, thin films of metallic copper, electrochemically deposited on platinum and/or sputtered or vapor deposited on a single crystal silicon substrate, may be used for reversible oxygen sensing. The long-term reversibility and potentiometric stability of such copper film-based sensors is enhanced (up to 1 month) by preventing the formation of cuprous oxide on the surfaces via the application of an external nonpolarizing cathodic current through the working electrode or by specifically using sputtered copper films that have [100] preferred crystal structures as determined by X-ray diffraction. The implications of these findings in relation to fabricating analytically useful potentiometric oxygen sensors are discussed.

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

    Science.gov (United States)

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

    2008-01-21

    The 'formal' hydrolysis ratio (h = C(OH-)added/C(Al)total) of hydrolysed aluminium-ions is an important parameter required for the exhaustive and quantitative speciation-fractionation of aluminium in aqueous solutions. This paper describes a potentiometric method for determination of the formal hydrolysis ratio based on an automated alkaline titration procedure. The method uses the point of precipitation of aluminium hydroxide as a reference (h = 3.0) in order to calculate the initial formal hydrolysis ratio of hydrolysed aluminium-ion solutions. Several solutions of pure hydrolytic species including aluminium monomers (AlCl3), Al13 polynuclear cluster ([Al13O4(OH)24(H2O)12]7+), Al30 polynuclear cluster ([Al30O8(OH)56(H2O)26]18+) and a suspension of nanoparticulate aluminium hydroxide have been used as 'reference standards' to validate the proposed potentiometric method. Other important variables in the potentiometric determination of the hydrolysis ratio have also been optimised including the concentration of aluminium and the type and strength of alkali (Trizma-base, NH3, NaHCO3, Na2CO3 and KOH). The results of the potentiometric analysis have been cross-verified by quantitative 27Al solution nuclear magnetic resonance (27Al NMR) measurements. The 'formal' hydrolysis ratio of a commercial basic aluminium chloride has been measured as an example of a practical application of the developed technique.

  17. Combined Voltammetric-Potentiometric Sensor with the Silver Solid Amalgam Link for Electroanalytical Measurements

    Czech Academy of Sciences Publication Activity Database

    Josypčuk, Bohdan; Novotný, Ladislav

    2002-01-01

    Roč. 14, č. 24 (2002), s. 1739-1741 ISSN 1040-0397 R&D Projects: GA ČR GV204/97/K084 Institutional research plan: CEZ:AV0Z4040901 Keywords : combined voltammetric-potentiometric sensors * solid amalgam Subject RIV: CG - Electrochemistry Impact factor: 1.783, year: 2002

  18. Potentiometric pH Measurements of Acidity Are Approximations, Some More Useful than Others

    Science.gov (United States)

    de Levie, Robert

    2010-01-01

    A recent article by McCarty and Vitz "demonstrating that it is not true that pH = -log[H+]" is examined critically. Then, the focus shifts to underlying problems with the IUPAC definition of pH. It is shown how the potentiometric method can provide "estimates" of both the IUPAC-defined hydrogen activity "and" the hydrogen ion concentration, using…

  19. Synthesis of H2SO4 doped polyaniline film by potentiometric method

    Indian Academy of Sciences (India)

    Unknown

    Synthesis of H2SO4 doped polyaniline film by potentiometric method. P D GAIKWAD, D J SHIRALE, V K GADE, ... transition from insulator to semiconductor when doped with oxidizing or reducing agent (Kobayashi et ... protonation (doping) and many other physical–chemical properties are connected to the presence of ...

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

    International Nuclear Information System (INIS)

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

    1990-09-01

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

  1. Potentiometric response and mechanism of anionic recognition of heterocalixarene-based ion selective electrodes

    Energy Technology Data Exchange (ETDEWEB)

    Shishkanova, T.V. [Department of Analytical Chemistry, Institute of Chemical Technology, Technicka 5, 166 28 Prague 6 (Czech Republic)]. E-mail: tatiana.shishkanova@vscht.cz; Sykora, D. [Department of Analytical Chemistry, Institute of Chemical Technology, Technicka 5, 166 28 Prague 6 (Czech Republic); Sessler, J.L. [Department of Chemistry and Biochemistry, Institute for Cellular and Molecular Biology, University of Texas, Austin, TX 78712-0615 (United States); Kral, V. [Department of Analytical Chemistry, Institute of Chemical Technology, Technicka 5, 166 28 Prague 6 (Czech Republic)

    2007-03-28

    The ion selective electrode (ISE)-based potentiometric approach is shown to be an effective means of characterizing the anion recognition sites in the molecular receptor calix[2]pyridino[2]pyrrole (CPP). In particular, potentiometric pH-measurements involving the use of experimental PVC-membranes based on CPP revealed the existence of both mono- and diprotonated forms of the receptor under readily accessible conditions. Based on these analyses, apparent surface protonation constants for this heterocalixarene were found to lie between 8.5-8.9 (pK {sub B1}) and 3.3-3.8 (pK {sub B2}). CPP was found to interact with targeted anionic analytes based on both coulombic and hydrogen bond interactions, as inferred from varying the kinds of ionic sites present within the membrane phase. Potentiometric selectivity studies revealed that CPP preferred 'Y-shaped' anions (e.g. acetate, lactate, benzoate) over spherical anions (e.g. fluoride and chloride), fluoride over chloride within the set of spherical anions, and the ortho-isomer over the corresponding meta- and para-isomers in the case of hydroxybenzoate (salicylate and congeners). In the context of this study, the advantages of potentiometric determinations of acetylsalicylic acid using optimized PVC-membranes based on CPP relative to more conventional PVC-membrane ISEs based on traditional anion exchanger were also demonstrated.

  2. Application Of A Potentiometric Electronic Tongue For The Determination Of Free SO2 And Other Analytical Parameters In White Wines From New Zealand

    Science.gov (United States)

    Mednova, Olga; Kirsanov, Dmitry; Rudnitskaya, Alisa; Kilmartin, Paul; Legin, Andrey

    2009-05-01

    The present study deals with a potentiometric electronic tongue (ET) multisensor system applied for the simultaneous determination of several chemical parameters for white wines produced in New Zealand. Methods in use for wine quality control are often expensive and require considerable time and skilled operation. The ET approach usually offers a simple and fast measurement protocol and allows automation for on-line analysis under industrial conditions. The ET device developed in this research is capable of quantifying the free and total SO2 content, total acids and some polyphenolic compounds in white wines with acceptable analytical errors.

  3. Potentiometric-level monitoring program, Mississippi and Louisiana: Annual status report for fiscal year 1985

    International Nuclear Information System (INIS)

    1986-10-01

    Potentiometric-level data presented in this report were collected at 82 wells in Mississippi and Louisiana from October 1984 through September 1985. These wells are located near Richton and Cypress Creek Domes in Mississippi and Vacherie dome in Louisiana. Three wells were reinstated to the program during this period. Two previously destroyed wells were deleted from the program. Protective barriers were installed around 26 shallow borings in Mississippi. Cursory analysis of the data in Mississippi indicated minimal, if any, change in potentiometric level during the past year in the Citronelle, Hattiesburg, Cockfield, Sparta, and Wilcox Formations. A slight decline, on the order of 0.3 meter (1 foot), occurred during the past year in well MCCG-1, which is screened in the caprock of Cypress Creek Dome. The potentiometric level in well MRIG-9, in the caprock of Richton Dome, stabilized during fiscal year 1985 following 5 years of increase. The Catahoula Formation experienced a continuing decline of about 0.3 meter/year (1 foot/year). Well MH-5C, screened in the Cook Mountain Formation, showed a continuing, long-term, upward trend on the order of 1.5 meters (4.9 feet) during the past year. The potentiometric level of well MH-8C, screened in the Cook Mountain Formation, stabilized during fiscal year 1985, following 5 years of large annual increases. Wells screened in the Austin Formation in Louisiana showed a downward trend of 0.3 to 1 meter (1 to 3.3 feet) during fiscal year 1985. Other formations in Louisiana generally showed no change in potentiometric level

  4. 40 CFR 86.107-96 - Sampling and analytical systems; evaporative emissions.

    Science.gov (United States)

    2010-07-01

    ... tuned to provide a smooth temperature pattern that has a minimum of overshoot, hunting, and instability... chart potentiometric recorder, by use of an on-line computer system or other suitable means. In any case... space, nor to the liquid-vapor interface. (e) Temperature recording system. A strip chart potentiometric...

  5. 40 CFR 86.1207-96 - Sampling and analytical systems; evaporative emissions.

    Science.gov (United States)

    2010-07-01

    ... tuned to provide a smooth temperature pattern that has a minimum of overshoot, hunting, and instability... test, as described in § 86.1233. The recording may be taken by means of a strip chart potentiometric... system. A strip chart potentiometric recorder, an on-line computer system, or other suitable means shall...

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

    Science.gov (United States)

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

    2006-11-01

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

  7. Mass spectrometric identification of an azobenzene derivative produced by smectite-catalyzed conversion of 3-amino-4-hydroxyphenylarsonic acid.

    Science.gov (United States)

    Wershaw, R L; Rutherford, D W; Rostad, C E; Garbarino, J R; Ferrer, Imma; Kennedy, K R; Momplaisir, Georges-Marie; Grange, Andrew

    2003-05-01

    The compound 3-amino-4-hydroxyphenylarsonic acid (3-amino-HPAA) reacts with smectite to form a soluble azobenzene arsonic acid compound. This reaction is of particular interest because it provides a possible mechanism for the formation of a new type of arsenic compound in natural water systems. 3-Amino-HPAA is a degradation product excreted by chickens that are fed rations amended with roxarsone. Roxarsone is used to control coccidial intestinal parasites in most of the broiler chickens grown in the United States. The structure of the azobenzene arsonic acid compound was first inferred from negative-ion and positive-ion low-resolution mass-spectrometric analyses of the supernatant of the smectite suspension. Elemental composition of the parent ion determined by high-resolution positive-ion mass spectrometric measurements was consistent with the proposed structure of the azobenzene arsonic acid compound.

  8. Mass spectrometric identification of an azobenzene derivative produced by smectite-catalyzed conversion of 3-amino-4-hydroxyphenylarsonic acid

    Science.gov (United States)

    Wershaw, R. L.; Rutherford, D.W.; Rostad, C.E.; Garbarino, J.R.; Ferrer, I.; Kennedy, K.R.; Momplaisir, G.-M.; Grange, A.

    2003-01-01

    The compound 3-amino-4-hydroxyphenylarsonic acid (3-amino-HPAA) reacts with smectite to form a soluble azobenzene arsonic acid compound. This reaction is of particular interest because it provides a possible mechanism for the formation of a new type of arsenic compound in natural water systems. 3-Amino-HPAA is a degradation product excreted by chickens that are fed rations amended with roxarsone. Roxarsone is used to control coccidial intestinal parasites in most of the broiler chickens grown in the United States. The structure of the azobenzene arsonic acid compound was first inferred from negative-ion and positive-ion low-resolution mass-spectrometric analyses of the supernatant of the smectite suspension. Elemental composition of the parent ion determined by high-resolution positive-ion mass spectrometric measurements was consistent with the proposed structure of the azobenzene arsonic acid compound. Published by Elsevier Science B.V.

  9. Potentiometric Sensor for Real-Time Monitoring of Multivalent Ion Concentrations in Molten Salt

    Energy Technology Data Exchange (ETDEWEB)

    Peter A. Zink; Jan-Fong Jue; Brenda E. Serrano; Guy L. Fredrickson; Ben F. Cowan; Steven D. Herrmann; Shelly X. Li

    2010-07-01

    Electrorefining of spent metallic nuclear fuel in high temperature molten salt systems is a core technology in pyroprocessing, which in turn plays a critical role in the development of advanced fuel cycle technologies. In electrorefining, spent nuclear fuel is treated electrochemically in order to effect separations between uranium, noble metals, and active metals, which include the transuranics. The accumulation of active metals in a lithium chloride-potassium chloride (LiCl-KCl) eutectic molten salt electrolyte occurs at the expense of the UCl3-oxidant concentration in the electrolyte, which must be periodically replenished. Our interests lie with the accumulation of active metals in the molten salt electrolyte. The real-time monitoring of actinide concentrations in the molten salt electrolyte is highly desirable for controlling electrochemical operations and assuring materials control and accountancy. However, real-time monitoring is not possible with current methods for sampling and chemical analysis. A new solid-state electrochemical sensor is being developed for real-time monitoring of actinide ion concentrations in a molten salt electrorefiner. The ultimate function of the sensor is to monitor plutonium concentrations during electrorefining operations, but in this work gadolinium was employed as a surrogate material for plutonium. In a parametric study, polycrystalline sodium beta double-prime alumina (Na-ß?-alumina) discs and tubes were subject to vapor-phase exchange with gadolinium ions (Gd3+) using a gadolinium chloride salt (GdCl3) as a precursor to produce gadolinium beta double-prime alumina (Gd-ß?-alumina) samples. Electrochemical impedance spectroscopy and microstructural analysis were performed on the ion-exchanged discs to determine the relationship between ion exchange and Gd3+ ion conductivity. The ion-exchanged tubes were configured as potentiometric sensors in order to monitor real-time Gd3+ ion concentrations in mixtures of gadolinium

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

    Science.gov (United States)

    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. Complexação da tetraciclina, da oxitetraciclina e da clortetraciclina com o catião cobre (II. Estudo potenciométrico Tetracycline, oxytetracycline and chlortetracycline complexation with copper (II. Potentiometric study

    Directory of Open Access Journals (Sweden)

    Cristina M. C. M. Couto

    2000-08-01

    Full Text Available Stability constants of complexes formed by copper (II with three different tetracyclines (tetracycline, oxytetracycline and chlortetracycline have been determined potentiometrically with an automatic system in aqueous medium at 25,0 ± 0,2 ºC and I = 0,1 mol L-1 NaNO3. The protonation constants of the three tetracyclines were also determined under the same conditions. The distribution of the complexes was then simulated at therapeutic levels of the drugs.

  12. Potentiometric surface of the Upper Floridan aquifer in Florida and parts of Georgia, South Carolina, and Alabama, May – June 2010

    Science.gov (United States)

    Kinnaman, Sandra L.; Dixon, Joann F.

    2011-01-01

    The Floridan aquifer system covers nearly 100,000 square miles in the southeastern United States throughout Florida and in parts of Georgia, South Carolina, and Alabama, and is one of the most productive aquifers in the world (Miller, 1990). This sequence of carbonate rocks is hydraulically connected and is over 300 feet thick in south Florida and thins toward the north. Typically, this sequence is subdivided into the Upper Floridan aquifer, the middle confining unit, and the Lower Floridan aquifer. The majority of freshwater is contained in the Upper Floridan aquifer and is used for water supply (Miller, 1986). The Lower Floridan aquifer contains fresh to brackish water in northeastern Florida and Georgia, while in south Florida it is saline. The potentiometric surface of the Upper Floridan aquifer in May–June 2010 shown on this map was constructed as part of the U.S. Geological Survey Floridan Aquifer System Groundwater Availability Study (U.S. Geological Survey database, 2011). Previous synoptic measurements and regional potentiometric maps of the Upper Floridan aquifer were prepared for May 1980 (Johnston and others, 1981) and May 1985 (Bush and others, 1986) as part of the Floridan Regional Aquifer System Analysis.

  13. Mass spectrometric analysis of nanogram levels of ruthenium

    International Nuclear Information System (INIS)

    Delmore, J.E.

    1979-01-01

    Previous investigations have demonstrated the possibility of using ruthenium originating from the spontaneous fission of 238 U for geochronological purposes. Because the abundance of ruthenium is low in geologic specimens and isotopic data are required, an indepth study of the production of steady mass spectrometer ion beams from nanogram amounts of ruthenium was undertaken. The results of this continuing mass spectrometric investigation are presented with some illustrative data

  14. Enzyme-based Colorimetric and Potentiometric Biosensor for Detecting Pb (II Ions in Milk

    Directory of Open Access Journals (Sweden)

    Hardeep Kaur

    2014-08-01

    Full Text Available The aim of the present work was to study a simple colorimetric and potentiometric biosensor based on urease inhibition by Pb (II ions for its estimation in milk samples. Urease immobilized on nylon membrane by hydrosol gel method was used as the biocomponent to demonstrate the metal effect on the enzyme activity using phenol red as the pH indicator. A lower limit detection of 38.6µm was achieved in the milk and the enzyme membranes were stable for more than two months at 4ºC. In potentiometric approach, response of an ion selective electrode (ISE to changing ammonium ion concentration as a consequence of urease inhibition by Pb (II ions was explored to achieve a detection limit of 9.66 µm. Lead specificity was attained by means of masking agents 1,10 - phenanthroline and sodium potassium tartarate. Validation of the developed biosensors was carried out with spiked milk samples.

  15. Potentiometric Surface of the Magothy Aquifer in Southern Maryland, September 2009

    Science.gov (United States)

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

    2010-01-01

    This report presents a map showing the potentiometric surface of the Magothy aquifer in the Magothy Formation of Late Cretaceous age in Southern Maryland during September 2009. The map is based on water-level measurements in 66 wells. The highest measured water level was 85 feet above sea level near the northern boundary and outcrop area of the aquifer in the north-central part of Anne Arundel County. The potentiometric surface declined towards the south. Local hydraulic gradients were directed toward the center of a cone of depression in the Waldorf area that developed in response to pumping. Measured groundwater levels were as low as 71 feet below sea level in the Waldorf area. The map also shows well yield in gallons per day for 2008 at wells or well fields.

  16. Potentiometric Surface of the Magothy Aquifer in Southern Maryland, September 2007

    Science.gov (United States)

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

    2009-01-01

    This report presents a map showing the potentiometric surface of the Magothy aquifer in the Magothy Formation of Late Cretaceous age in Southern Maryland during September 2007. The map is based on water-level measurements in 69 wells. The highest measured water level was 85 feet above sea level near the northern boundary and outcrop area of the aquifer in the north-central part of Anne Arundel County. The potentiometric surface declined towards the south. Local gradients were directed toward the center of a cone of depression in the Waldorf area that developed in response to pumping. Measured ground-water levels were as low as 90 feet below sea level in the Waldorf area.

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

    Science.gov (United States)

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

    2002-09-01

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

  18. Potentiometric determination of nitrate in products used for the treatment of dentinal hypersensitivity.

    Science.gov (United States)

    Pérez-Olmos, R; Bezares, P; Pérez, J

    2000-02-01

    In this paper, a rapid, simple and inexpensive potentiometric method for the determination of the potassium nitrate contained in different dentinal desensitizer products is described. The nitrate-selective electrode, using a tetraoctylammonium salt as sensor, was constructed without an internal filling solution. The ionic strength of the sample solutions was fixed by means of a 0.33 mol 1(-1) K2SO4 solution and direct potentiometry was used as the analytical technique of measurement. Precision and accuracy of the method developed were adequate since the mean of the relative standard deviations was 1.2% and the average percentage of spike recoveries was 100.9%. Eleven samples of toothpastes, gels and mouthwashes were analyzed by the proposed potentiometric method and the quality of the results was compared by means of linear regression analysis with those obtained by high-performance liquid chromatography (HPLC), adopted as the reference technique. Satisfactory agreement was observed.

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

    International Nuclear Information System (INIS)

    Ozeroglu, C.; Karahan, M.

    2011-01-01

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

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

    International Nuclear Information System (INIS)

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

    1965-01-01

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

  1. Discrimination of olive oil by cultivar, geographical origin and quality using potentiometric electronic tongue fingerprints

    OpenAIRE

    Souayah, Fatma; Rodrigues, Nuno; Veloso, Ana C. A.; Dias, Luís G.; Pereira, José A.; Oueslati, Souheib; Peres, António M.

    2017-01-01

    Legal regulations are set for protecting claims regarding olive oil geographical denomination. When meteorological or agroecological factors similarly affect different regions, the origin identification is a challenging task. This study demonstrated the use of a potentiometric electronic tongue coupled with linear discriminant analysis to discriminate the geographical origin of monovarietal Tunisian olive oil produced from local cv Chemlali (Kairouan, Sidi Bouzid or Sfax regions) and cv Sahli...

  2. Potentiometric pKa Determination of Piroxicam and Tenoxicam in Acetonitrile-Water Binary Mixtures

    OpenAIRE

    Çubuk Demiralay, Ebru; Yılmaz, Hülya

    2012-01-01

    Abstract: Ionization constant (pKa) is one among the parameter to be estimated with accuracy, irrespective of solubility constraints. In the present study, acid-base behaviour of the piroxicam and tenoxicam was studied. By using the potentiometric method, pKa values of piroxicam and tenoxicam have been determined in different percentage of acetonitrile-water binary mixtures (acetonitrile content between 30 and 45% in volume). Aqueous pKa values of these compounds were calculated by mole fract...

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

    International Nuclear Information System (INIS)

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

    1980-01-01

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

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

    International Nuclear Information System (INIS)

    Baumann, E.W.

    1976-11-01

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

  5. pH-based Detection of Phenylalnine by Potentiometric and Colorimetric Methods

    OpenAIRE

    Pijanowska, Dorota G.; Remiszewska, El ?bieta

    2006-01-01

    In this paper, methods of sample preparation for potentiometric measurement of phenylalanine are presented. Basing on the spectrophotometric measurements of phenylalanine, the concentrations of reagents of the enzymatic reaction (10 mM L-Phe, 0,4 mM NAD+, 2U L-PheDH) were determined. Then, the absorption spectrum of the reaction product, NADH, was monitored (maximum peak at 340 nm). The results obtained by the spectrophotometric method were compared with the results obtained by the colourimet...

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

    Directory of Open Access Journals (Sweden)

    ZORAN V. LAUSEVIC

    2001-03-01

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

  7. Screen-printed sensor for batch and flow injection potentiometric chromium(VI) monitoring

    Energy Technology Data Exchange (ETDEWEB)

    Sanchez-Moreno, Raul A.; Gismera, M.J.; Sevilla, M.T.; Procopio, Jesus R. [Facultad de Ciencias, Universidad Autonoma de Madrid, Departamento de Quimica Analitica y Analisis Instrumental, Madrid (Spain)

    2010-05-15

    A disposable screen-printed electrode was designed and evaluated for direct detection of chromium(VI) in batch and flow analysis. The carbon screen-printed electrode was modified with a graphite-epoxy composite. The optimal graphite-epoxy matrix contains 37.5% graphite powder, 12.5% diphenylcarbohydrazide, a selective compound for chromium(VI), and 50% epoxy resin. The principal analytical parameters of the potentiometric response in batch and flow analysis were optimized and calculated. The screen-printed sensor exhibits a response time of 20 {+-} 1 s. In flow analysis, the analytical frequency of sampling is 70 injections per hour using 0.1 M NaNO{sub 3} solution at pH 3 as the carrier, a flow rate of 2.5 mL.min{sup -1}, and an injection sample volume of 0.50 mL. The sensor shows potentiometric responses that are very selective for chromium(VI) ions and optimal detection limits in both static mode (2.1 x 10{sup -7} M) and online analysis (9.4 x 10{sup -7} M). The disposable potentiometric sensor was employed to determine toxicity levels of chromium(VI) in mineral, tap, and river waters by flow-injection potentiometry and batch potentiometry. Chromium(VI) determination was also carried out with successful results in leachates from municipal solid waste landfills. (orig.)

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

    Directory of Open Access Journals (Sweden)

    Siavash Riahi

    2008-03-01

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

  9. Solid-contact potentiometric sensor for ascorbic acid based on cobalt phthalocyanine nanoparticles as ionophore.

    Science.gov (United States)

    Wang, Kun; Xu, Jing-Juan; Tang, Kai-Shi; Chen, Hong-Yuan

    2005-10-15

    A novel solid-contact potentiometric sensor for ascorbic acid based on cobalt phthalocyanine nanoparticles (NanoCoPc) as ionophore was fabricated without any need of auxiliary materials (such as membrane matrix, plasticizer, and other additives). The electrode was prepared by simple drop-coating NanoCoPc colloid on the surface of a glassy carbon electrode. A smooth, bright and blue thin film was strongly attached on the surface of the glassy carbon electrode. The electrode showed high selectivity for ascorbic acid, as compared with many common anions. The influences of the amount of NanoCoPc at the electrode surface and pH on the response characteristics of the electrode were investigated. To overcome the instability of the formal potential of the coated wire electrode, a novel electrochemical pretreatment method was proposed for the potentiometric sensor based on redox mechanism. This resulting sensor demonstrates potentiometric response over a wide linear range of ascorbic acid concentration (5.5 x 10(-7) to 5.5 x 10(-2)M) with a fast response (determination of practical samples.

  10. Stripping potentiometric analysis: application to determination of metallic cations in presence of uranium

    International Nuclear Information System (INIS)

    Pereira-Ramos, J.P.; Chivot, J.; Sarantopoulos, F.; Godard, R.

    1984-01-01

    Potentiometric stripping analysis consists of a potentiostatic deposition step of trace elements and a subsequent stripping step. The trace metals are simultaneously reduced at a rotating electrode, the working electrode being a mercury film coated glassy carbon electrode; the amalgamated metals are then re-oxidized with an oxidizing agent. The analytical signal of this method is the time required for complete re-oxidation. Influence of different parameters on the analytical signal is studied by using mercury (II) ions as oxidizing agent in 5.10 -4 M H 2 SO 4 aqueous solution. Here, we point out the main characteristics of the potentiometric stripping analysis under the same experimental conditions. The reproductibility ranges are comprised between 0.5% to 1.5% and the detection limit for cadmium (II) is estimated to be 2.10 -10 M with a plating time of 300 seconds. Small quantities, as 10 -7 M Cd 2+ , Pb 2+ and Zn 2+ are simultaneously determined in presence of U (VI) ions (UO 2 2+ ) with an accuracy of 0.5% for Cd 2+ and Zn 2+ , and 4.5% for Pb 2+ . Compared to well-known electrochemical techniques, potentiometric stripping analysis appears to be a performing method for trace analysis in a wide range of media: this method permits the analysis of elements in presence of species more concentrated and being able to oxidize the trace elements [fr

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

    Directory of Open Access Journals (Sweden)

    Abdelatty Mohamed Radalla

    2015-06-01

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

  12. Determination of trace metal ions via on-line separation and preconcentration by means of chelating Sepharose beads in a sequential injection lab-on-valve (SI-LOV) system coupled to electrothermal atomic absorption spectrometric detection

    DEFF Research Database (Denmark)

    Long, Xiangbao; Hansen, Elo Harald; Miró, Manuel

    2005-01-01

    The analytical performance of an on-line sequential injection lab-on-valve (SI-LOV) system using chelating Sepharose beads as sorbent material for the determination of ultra trace levels of Cd(II), Pb(II) and Ni(II) by electrothermal atomic absorption spectrometry (ETAAS) is described and discussed...

  13. Antioxidant activity and physico-chemical parameters for the differentiation of honey using a potentiometric electronic tongue.

    Science.gov (United States)

    Juan-Borrás, Marisol; Soto, Juan; Gil-Sánchez, Luis; Pascual-Maté, Ana; Escriche, Isabel

    2017-05-01

    This work evaluates the capacity of a potentiometric electronic tongue to differentiate between types of honey (orange blossom, rosemary, thyme, sunflower, winter savory and honeydew honey) according to their antioxidant level. The classical procedures used to evaluate the antioxidant potential of honey are inappropriate for in situ monitoring on reception of batches of raw honey in the packaging industry. They are also destructive, time-consuming and very tedious, requiring highly expert analysts and specialised equipment. The electronic tongue system made with Ag, Ni, Co, Cu and Au was able to not only differentiate between types of honey but also to predict their total antioxidant capacity. The discrimination ability of the system was proved by means of a fuzzy ARTMAP type ANN, with 100% classification success. A prediction multiple linear regression model showed that the best correlation coefficient was for antioxidant activity (0.9666), then for electrical conductivity (0.8959) and to a lesser extent for a w , moisture and colour. The proposed measurement system could be a quick, easy option for the honey packaging sector to provide continuous in-line information about a characteristic as important as the antioxidant level. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

  14. Reconstruction of neutron spectra using neural networks starting from the Bonner spheres spectrometric system; Reconstruccion de espectros de neutrones usando redes neuronales a partir del sistema espectrometrico de esferas de Bonner

    Energy Technology Data Exchange (ETDEWEB)

    Ortiz R, J.M.; Martinez B, M.R.; Arteaga A, T.; Vega C, H.R.; Hernandez D, V.M.; Manzanares A, E. [Universidad Autonoma de Zacatecas, A.P. 336, 98000 Zacatecas (Mexico)

    2005-07-01

    The artificial neural networks (RN) have been used successfully to solve a wide variety of problems. However to determine an appropriate set of values of the structural parameters and of learning of these, it continues being even a difficult task. Contrary to previous works, here a set of neural networks is designed to reconstruct neutron spectra starting from the counting rates coming from the detectors of the Bonner spheres system, using a systematic and experimental strategy for the robust design of multilayer neural networks of the feed forward type of inverse propagation. The robust design is formulated as a design problem of Taguchi parameters. It was selected a set of 53 neutron spectra, compiled by the International Atomic Energy Agency, the counting rates were calculated that would take place in a Bonner spheres system, the set was arranged according to the wave form of those spectra. With these data and applying the Taguchi methodology to determine the best parameters of the network topology, it was trained and it proved the same one with the spectra. (Author)

  15. Determination of uranium enrichment by using gamma-spectrometric methods

    International Nuclear Information System (INIS)

    Kutnyj, D.V.; Telegin, Yu.N.; Odejchuk, N.P.; Mikhailov, V.A.; Tovkanets, V.E.

    2009-01-01

    By using commercial analysis programs MGAU (LLNL, USA) and FRAM (LANL, USA) the summary error of gamma-spectrometric uranium enrichment measurements was investigated. Uranium samples with enrichments of 0,71; 4,46 and 20,1 % were measured. The coaxial high purity germanium detector (type GC) and the planar germanium detector (type LEGe) were used as gamma-radiation detectors. It was shown that experimental equipment and mathematical software available in NSC KIPT allow us to measure uranium enrichment by nondestructive method with accuracy of not worse than 2%.

  16. Photometric and emission-spectrometric determination of boron in steels

    International Nuclear Information System (INIS)

    Thierig, D.

    1982-01-01

    A method for the photometric determination of boron in unalloyed and alloyed steels is described, in which Curcumine is used as reagent. A separation of boron is not necessary. Limit of detection: 0.0003% B. The decomposition of boron nitride in the steel is achieved by heating the whole sample in fuming sulphuric acid/phosphoric acid. For the emission spectrometric investigation of solid steel samples and for the spectrochemical analysis of solutions with plasma excitation working parameters are given and possibilities of interferences are demonstrated. (orig.) [de

  17. Challenges and recent advances in mass spectrometric imaging of neurotransmitters

    Science.gov (United States)

    Gemperline, Erin; Chen, Bingming; Li, Lingjun

    2014-01-01

    Mass spectrometric imaging (MSI) is a powerful tool that grants the ability to investigate a broad mass range of molecules, from small molecules to large proteins, by creating detailed distribution maps of selected compounds. To date, MSI has demonstrated its versatility in the study of neurotransmitters and neuropeptides of different classes toward investigation of neurobiological functions and diseases. These studies have provided significant insight in neurobiology over the years and current technical advances are facilitating further improvements in this field. neurotransmitters, focusing specifically on the challenges and recent Herein, we advances of MSI of neurotransmitters. PMID:24568355

  18. Gamma spectrometric analyses of environmental samples at PINSTECH

    International Nuclear Information System (INIS)

    Faruq, M.U.; Parveen, N.; Ahmed, B.; Aziz, A.

    1979-01-01

    Gamma spectrometric analyses of air and other environmental samples from PINSTECH were carried out. Air particulate samples were analyzed by a Ge(Li) detector on a computer-based multichannel analyzer. Other environmental samples were analyzed by a Na(T1) scintillation detector spectrometer and a multichannel analyzer with manual analysis. Concentration of radionuclides in the media was determined and the sources of their production were identified. Age of the fall out was estimated from the ratios of the fission products. (authors)

  19. Detection of organic materials by spectrometric radiography method

    CERN Document Server

    Naydenov, S V; Onyshchenko, G.M.; Lecoq, P.; Smith, C.

    2008-01-01

    In this paper we report a spectrometric approach to dual-energy digital radiography that has been developed and applied to identify specific organic substances and discern small differences in their effective atomic number. An experimental setup has been designed, and a theoretical description proposed based on the experimental results obtained. The proposed method is based on application of special reference samples made of materials with different effective atomic number and thickness, parameters known to affect X-ray attenuation in the low-energy range. The results obtained can be used in the development of a new generation of multi-energy customs or medical X-ray scanners.

  20. Photometric and emission-spectrometric determination of boron in steels

    Energy Technology Data Exchange (ETDEWEB)

    Thierig, D.

    1982-01-01

    A method for the photometric determination of boron in unalloyed and alloyed steels is described, in which Curcumine is used as reagent. A separation of boron is not necessary. Limit of detection: 0.0003% B. The decomposition of boron nitride in the steel is achieved by heating the whole sample in fuming sulphuric acid/phosphoric acid. For the emission spectrometric investigation of solid steel samples and for the spectrochemical analysis of solutions with plasma excitation working parameters are given and possibilities of interferences are demonstrated.

  1. Determination of Mass Spectrometric Sensitivity of Different Metalloporphyrin Esters Relative to Porphyrin Ester

    DEFF Research Database (Denmark)

    Larsen, Elfinn; Egsgaard, Helge; Møller, J.

    1977-01-01

    Quantitative determination of metalloporphyrin contamination in preparations of biologically important porphyrins was achieved mass spectrometrically by application of the integrated ion current technique. For this purpose, the relative molecular ion sensitivities of the contaminating metal...... of calibration samples, including complex formation and the mass spectrometric methodology, is described and discussed....

  2. Decoupling optical and potentiometric band gaps in pi-conjugated materials.

    Science.gov (United States)

    Susumu, Kimihiro; Therien, Michael J

    2002-07-24

    Syntheses, optical spectroscopy, potentiometric studies, and electronic structural calculations are reported for two classes of conjugated (porphinato)metal oligomers that feature a meso-to-meso ethyne-bridged linkage topology. One set of these systems, bis[(5,5'-10,20-bis[3,5-bis(3,3-dimethyl-1-butyloxy)phenyl]porphinato)zinc(II)]ethyne (DD), 5,15-bis[[5'-10',20'-bis[3,5-di(3,3-dimethyl-1-butyloxy)phenyl]porphinato)zinc(II)]ethynyl]-10,20-bis[3,5-di(9-methoxy-1,4,7-trioxanonyl)phenyl]porphinato)zinc(II) (DDD), and 5,15-bis[[15' '-(5'-10',20'-bis[3,5-bis(3,3-dimethyl-1-butyloxy)phenyl]porphinato)zinc(II)]-[(5' '-10' ',20' '-bis[3,5-di(9-methoxy-1,4,7-trioxanonyl)phenyl]porphinato)zinc(II)]ethyne]ethynyl]-10,20-bis[3,5-di(9-methoxy-1,4,7-trioxanonyl)phenyl]porphinato)zinc(II) (DDDDD), constitute highly soluble analogues of previously studied examples of this structural motif having simple 10,20-diaryl substituents, while a corresponding set of conjugated oligomers, [(5-10,20-bis[3,5-bis(3,3-dimethyl-1-butyloxy)phenyl]porphinato)zinc(II)]-[(5'-15'-ethynyl-10',20'-bis[10,20-bis(heptafluoropropyl)porphinato)zinc(II)]ethyne (DA), 5,15-bis[[5'-10',20'-bis[3,5-di(3,3-dimethyl-1-butyloxy)phenyl]porphinato)zinc(II)]ethynyl]-10,20-bis(heptafluoropropyl)porphinato]zinc(II) (DAD), and 5,15-bis[[15' '-(5'-10',20'-bis[3,5-bis(3,3-dimethyl-1-butyloxy)phenyl]porphinato)zinc(II)]-[(5' '-(10' ',20' '-bis(heptafluoropropyl)porphinato)zinc(II)]ethyne]ethynyl]-10,20-bis[3,5-di(9-methoxy-1,4,7-trioxanonyl)phenyl]porphinato)zinc(II) (DADAD), features alternating electron-rich and electron-poor (porphinato)zinc(II) units. Electrooptic and computational data for these species demonstrate that it is possible to engineer conjugated oligomeric structures that possess highly delocalized singlet (S1) excited states yet manifest apparent one-electron oxidation and reduction potentials (E1/20/+ and E1/2-/0 values) that are essentially invariant with respect to those elucidated for their

  3. Potentiometric Sensor for Real-Time Monitoring of Multivalent Ion Concentrations in Molten Salt

    International Nuclear Information System (INIS)

    Zink, Peter A.; Jue, Jan-Fong; Serrano, Brenda E.; Fredrickson, Guy L.; Cowan, Ben F.; Herrmann, Steven D.; Li, Shelly X.

    2010-01-01

    Electrorefining of spent metallic nuclear fuel in high temperature molten salt systems is a core technology in pyroprocessing, which in turn plays a critical role in the development of advanced fuel cycle technologies. In electrorefining, spent nuclear fuel is treated electrochemically in order to effect separations between uranium, noble metals, and active metals, which include the transuranics. The accumulation of active metals in a lithium chloride-potassium chloride (LiCl-KCl) eutectic molten salt electrolyte occurs at the expense of the UCl3-oxidant concentration in the electrolyte, which must be periodically replenished. Our interests lie with the accumulation of active metals in the molten salt electrolyte. The real-time monitoring of actinide concentrations in the molten salt electrolyte is highly desirable for controlling electrochemical operations and assuring materials control and accountancy. However, real-time monitoring is not possible with current methods for sampling and chemical analysis. A new solid-state electrochemical sensor is being developed for real-time monitoring of actinide ion concentrations in a molten salt electrorefiner. The ultimate function of the sensor is to monitor plutonium concentrations during electrorefining operations, but in this work gadolinium was employed as a surrogate material for plutonium. In a parametric study, polycrystalline sodium beta double-prime alumina (Na-β(double p rime)-alumina) discs and tubes were subject to vapor-phase exchange with gadolinium ions (Gd3+) using a gadolinium chloride salt (GdCl3) as a precursor to produce gadolinium beta double-prime alumina (Gd-β(double p rime)-alumina) samples. Electrochemical impedance spectroscopy and microstructural analysis were performed on the ion-exchanged discs to determine the relationship between ion exchange and Gd3+ ion conductivity. The ion-exchanged tubes were configured as potentiometric sensors in order to monitor real-time Gd3+ ion concentrations in

  4. The use of emulsions for the determination of methylmercury and inorganic mercury in fish-eggs oil by cold vapor generation in a flow injection system with atomic absorption spectrometric detection.

    Science.gov (United States)

    Burguera, J L; Quintana, I A; Salager, J L; Burguera, M; Rondón, C; Carrero, P; Anton de Salager, R; Petit de Peña, Y

    1999-04-01

    An on-line time based injection system used in conjunction with cold vapor generation atomic absorption spectrometry and microwave-aided oxidation with potassium persulfate has been developed for the determination of the different mercury species in fish-eggs oil samples. A three-phase surfactant-oil-water emulsion produced an advantageous flow when a peristaltic pump was used to introduce the highly viscous sample into the system. The optimum proportion of the oil-water mixture ratio was 2:3 v/v with a Tween 20 surfactant concentration in the emulsion of 0.008% v/v. Inorganic mercury was determined after reduction with sodium borohydride while total mercury was determined after an oxidation step with persulfate prior to the reduction step to elemental mercury with the same reducing agent. The difference between total and inorganic mercury determined the organomercury content in samples. A linear calibration graph was obtained in the range 0.1-20 micrograms l-1 of Hg2+ by injecting 0.7 ml of samples. The detection limits based on 3 sigma of the blank signals were 0.11 and 0.12 microgram l-1 for total and inorganic mercury, respectively. The relative standard deviation of ten independent measurements were 2.8 and 2.2% for 10 micrograms l-1 and 8.8 and 9.0% for 0.1 microgram l-1 amounts of total and inorganic mercury, respectively. The recoveries of 0.3, 0.6 and 8 micrograms l-1 of inorganic and organic mercury added to fish-eggs oil samples ranged from 93.0 to 94.8% and from 100 to 106%, respectively. Good agreement with those values obtained for total mercury content in real samples by electrothermal atomic absorption spectrometry was also obtained, differences between mean values were catfish-eggs oil samples from the northwestern coast of Venezuela were measured; while the organic mercury lay in the range 2.0 and 3.3 micrograms l-1, inorganic mercury was not detected.

  5. Potentiometric determination of acetylsalicylic acid by sequential injection analysis (SIA) using a tubular salicylate-selective electrode.

    Science.gov (United States)

    Paseková, H; Sales, M G; Montenegro, M C; Araújo, A N; Polásek, M

    2001-03-01

    This paper deals with the development of an automated procedure for formulation assays and dissolution tests based on a sequential injection analysis (SIA) system involving an ion-selective electrode as sensing device. Construction of a tubular salicylate (Sal) selective electrode suitable for potentiometric determination of acetylsalicylic acid (Asa) in pharmaceutical formulations is described. The flow-through electrode is formed by a PVC membrane containing 29.2% (w/w) PVC, 5.8% (w/w) tetraoctylammonium salicylate (ionic sensor), 58.5% o-nitrophenyloctylether (plasticizer) and 6.5% (w/w) p-tert-octylphenol (stabilising additive which increases electrode selectivity). The calibration range is 0.05--10 mM Sal, the limit of detection (LOD) is 0.05 mM Sal, the slope is 56.0 mV per decade at 22 degrees C. The R.S.D. is 0.20% (15 readings) when determining 2.5 mM Sal in standard solution. The electrode is used for sensing Asa after its on-line chemical hydrolysis to Sal in a SIA system. The sampling rate is 6 h(-1) but for the dissolution tests the frequency is increased to 20 h(-1). The SIA set-up is employed for the assay of Asa in plain tablets, composed tablets and effervescent tablets and for performing dissolution tests of normal and sustained release tablets. Results obtained by this technique compare well with those required by the US Pharmacopoeia XXIV.

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

  7. Mass spectrometric analysis of monolayer protected nanoparticles

    Science.gov (United States)

    Zhu, Zhengjiang

    Monolayer protected nanoparticles (NPs) include an inorganic core and a monolayer of organic ligands. The wide variety of core materials and the tunable surface monolayers make NPs promising materials for numerous applications. Concerns related to unforeseen human health and environmental impacts of NPs have also been raised. In this thesis, new analytical methods based on mass spectrometry are developed to understand the fate, transport, and biodistributions of NPs in the complex biological systems. A laser desorption/ionization mass spectrometry (LDI-MS) method has been developed to characterize the monolayers on NP surface. LDI-MS allows multiple NPs taken up by cells to be measured and quantified in a multiplexed fashion. The correlations between surface properties of NPs and cellular uptake have also been explored. LDI-MS is further coupled with inductively coupled plasma mass spectrometry (ICP-MS) to quantitatively measure monolayer stability of gold NPs (AuNPs) and quantum dots (QDs), respectively, in live cells. This label-free approach allows correlating monolayer structure and particle size with NP stability in various cellular environments. Finally, uptake, distribution, accumulation, and excretion of NPs in higher order organisms, such as fish and plants, have been investigated to understand the environmental impact of nanomaterials. The results indicate that surface chemistry is a primary determinant. NPs with hydrophilic surfaces are substantially less toxic and present a lower degree of bioaccumulation, making these nanomaterials attractive for sustainable nanotechnology.

  8. Separation Techniques for Uranium and Plutonium at Trace Levels for the Thermal Ionization Mass Spectrometric Determination

    Energy Technology Data Exchange (ETDEWEB)

    Suh, M. Y.; Han, S. H.; Kim, J. G.; Park, Y. J.; Kim, W. H

    2005-12-15

    This report describes the state of the art and the progress of the chemical separation and purification techniques required for the thermal ionization mass spectrometric determination of uranium and plutonium in environmental samples at trace or ultratrace levels. Various techniques, such as precipitation, solvent extraction, extraction chromatography, and ion exchange chromatography, for separation of uranium and plutonium were evaluated. Sample preparation methods and dissolution techniques for environmental samples were also discussed. Especially, both extraction chromatographic and anion exchange chromatographic procedures for uranium and plutonium in environmental samples, such as soil, sediment, plant, seawater, urine, and bone ash were reviewed in detail in order to propose some suitable methods for the separation and purification of uranium and plutonium from the safeguards environmental or swipe samples. A survey of the IAEA strengthened safeguards system, the clean room facility of IAEA's NWAL(Network of Analytical Laboratories), and the analytical techniques for safeguards environmental samples was also discussed here.

  9. Separation Techniques for Uranium and Plutonium at Trace Levels for the Thermal Ionization Mass Spectrometric Determination

    International Nuclear Information System (INIS)

    Suh, M. Y.; Han, S. H.; Kim, J. G.; Park, Y. J.; Kim, W. H.

    2005-12-01

    This report describes the state of the art and the progress of the chemical separation and purification techniques required for the thermal ionization mass spectrometric determination of uranium and plutonium in environmental samples at trace or ultratrace levels. Various techniques, such as precipitation, solvent extraction, extraction chromatography, and ion exchange chromatography, for separation of uranium and plutonium were evaluated. Sample preparation methods and dissolution techniques for environmental samples were also discussed. Especially, both extraction chromatographic and anion exchange chromatographic procedures for uranium and plutonium in environmental samples, such as soil, sediment, plant, seawater, urine, and bone ash were reviewed in detail in order to propose some suitable methods for the separation and purification of uranium and plutonium from the safeguards environmental or swipe samples. A survey of the IAEA strengthened safeguards system, the clean room facility of IAEA's NWAL(Network of Analytical Laboratories), and the analytical techniques for safeguards environmental samples was also discussed here

  10. Tandem mass spectrometric studies of lanthanum-α-hydroxycarboxylate complexes

    International Nuclear Information System (INIS)

    Kumar, Pranaw; Telmore, V.M.; Jaison, P.G.; Sadhu, Biswajit; Sundararajan, Mahesh

    2017-01-01

    The complexation of lanthanides with hydroxycarboxylic acids is important to understand its separation behavior on liquid chromatography. Electrospray ionization mass spectrometry (ESI-MS) being the soft ionization technique is known for studying the speciation and stoichiometry of metal ligand species. The gentle ionization process of this technique is well suited for transferring the species from solution to gas phase with the retention of stoichiometry. The use of tandem mass spectrometric application has been utilized for studying the path of dissociation. The possible pathways of fragmentation and its geometry have been explained by using the density functional theory (OFT) in the gas phase. Present work describes integrated DFT and tandem mass spectrometric studies of La with α-hydroxyisobutyric acid (HIBA) along with their dissociation studies. In this study, unusual elimination of -CO with the loss of m/z 28 from the complex was observed. This fragmentation resulted the conversion of HIBA into acetone in the fragmented product. The possible fragmentation pathways with the energetic were identified

  11. Spectrometric properties and radiation damage of BGO crystals

    Science.gov (United States)

    Kim, Gen C.; Gasanov, Eldar M.

    1997-07-01

    Spectrometric properties, such as light output, energy resolution BGO crystals before and after (superscript 60)Co gamma-ray (dose 10(superscript 4) - 10(superscript 6) R) and neutron irradiation (fluence 10(superscript 14) cm(superscript -2)) are investigated. Condition for degradation of spectrometric properties and their recovering after irradiation are studied. The energy spectrum of the photons emitted from BGO crystals irradiated with neutron fluence contains the long living background peak which is caused by self-irradiation with radioactive isotopes produced in the crystals. The defect production was studied in crystals under the high dose gamma-irradiation with (superscript 60)Co isotope. It was found that after doses above 10(superscript 8) R the color center at 365 nm and doses higher than 10(superscript 9) R a wide absorption band in the region of 300 - 350 nm occur. Comparison of these results with those of reactor irradiation has shown that under the high dose gamma-irradiation the structure defect production takes place.

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

    Directory of Open Access Journals (Sweden)

    Clausius Duque Gonçalves Reis

    2010-04-01

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

  13. Potentiometric investigation of acid dissociation and anionic homoconjugation equilibria of substituted phenols in dimethyl sulfoxide[Substituted phenols; Acid-base equilibria; Dimethyl sulfoxide (DMSO); Potentiometry

    Energy Technology Data Exchange (ETDEWEB)

    Czaja, Malgorzata; Kozak, Anna; Makowski, Mariusz; Chmurzynski, Lech. E-mail: lech@chemik.chem.univ.gda.pl

    2003-10-01

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

  14. Self-assembly of SiO2 nanoparticles for the potentiometric detection of neurotransmitter acetylcholine and its inhibitor.

    Science.gov (United States)

    Arruda, Izabela G; Guimarães, Francisco E G; Ramos, Romildo J; Vieira, Nirton C S

    2014-09-01

    The detection and quantification of neurotransmitter acetylcholine (ACh) are relevant because modifications in the ACh levels constitute a threat to human health. The biological regulator of this neurotransmitter is acetylcholinesterase (AChE), an enzyme that catalyzes the hydrolysis of ACh to choline and acetic acid. However, its activity is inhibited in the presence of organophosphate and carbamate pesticides, compromising the degradation of the neurotransmitter. There has been a growing interest in faster and more sensitive detection systems that include new methods and materials for the determination of the ACh concentration. This paper proposes a potentiometric biosensor for the detection of neurotransmitter ACh and its inhibitors, specifically organophosphate pesticide methamidophos. The biosensor is based on a self-assembled platform formed by poly(allylamine) hydrochloride (PAH) and silicon dioxide nanoparticles (SiO2-Np) that contains the immobilized enzyme AChE. First, the responses of the biosensor were investigated for different concentrations of ACh in buffer solutions. After quantifying ACh, the inhibition of AChE in the presence of methamidophos was determined, enabling the quantification of methamidophos expressed as the percentage of enzyme inhibition. The potential advantages of this biosensor include simplicity in building the electrode, possible production on an industrial scale, limited need for qualified personnel to operate the device and low processing cost.

  15. Incorporating β-Cyclodextrin with ZnO Nanorods: A Potentiometric Strategy for Selectivity and Detection of Dopamine

    Directory of Open Access Journals (Sweden)

    Sami Elhag

    2014-01-01

    Full Text Available We describe a chemical sensor based on a simple synthesis of zinc oxide nanorods (ZNRs for the detection of dopamine molecules by a potentiometric approach. The polar nature of dopamine leads to a change of surface charges on the ZNR surface via metal ligand bond formation which results in a measurable electrical signal. ZNRs were grown on a gold-coated glass substrate by a low temperature aqueous chemical growth (ACG method. Polymeric membranes incorporating β-cyclodextrin (β-CD and potassium tetrakis (4-chlorophenyl borate was immobilized on the ZNR surface. The fabricated electrodes were characterized by X-ray diffraction (XRD and scanning electron microscopy (SEM techniques. The grown ZNRs were well aligned and exhibited good crystal quality. The present sensor system displays a stable potential response for the detection of dopamine in 10−2 mol·L−1 acetic acid/sodium acetate buffer solution at pH 5.45 within a wide concentration range of 1 × 10−6 M–1 × 10−1 M, with sensitivity of 49 mV/decade. The electrode shows a good response time (less than 10 s and excellent repeatability. This finding can contribute to routine analysis in laboratories studying the neuropharmacology of catecholamines. Moreover, the metal-ligand bonds can be further exploited to detect DA receptors, and for bio-imaging applications.

  16. Conventional and planar chip sensors for potentiometric assay of uric acid in biological fluids using flow injection analysis.

    Science.gov (United States)

    Kamel, Ayman H

    2007-10-18

    The potentiometric response properties of several PVC-based membrane sensors using phthalocyanine complexes of cobalt(II) (CoPC) and Fe(II) (FePC) as anion carriers, towards uric acid were constructed and characterized. The sensors demonstrated fast near-Nernstian response for uric acid over the concentration ranges 9.1 x 10(-6) to 9.1 x 10(-2) and 3.1 x 10(-5) to 3.1 x 10(-2)M with detection limits 0.67 and 2.85 microg mL(-1) over pH 6.5-8 for CoPC and FePC based membrane sensors plasticized with o-NPOE and 1% TDMAC, respectively. A novel solid-state planar chip urate sensor was developed, characterized according to IUPAC recommendations, easily used in a single channel wall-jet flow injection system and compared with a tubular detector. The intrinsic characteristics of the detectors in a low dispersion manifold were determined and compared with data obtained under hydrodynamic mode of operation. Validation of the assay methods with the proposed sensors by measuring the lower limit, range, accuracy, precision, repeatability and between-day-variability revealed good performance characteristics confirming applicability for continuous determination of uric acid. The sensors were used for determining urate in biological fluids at an input rate of 50 samples per hour. The results compare favorably with data obtained by the standard spectrophotometry.

  17. CMP(O) tripodands: synthesis, potentiometric studies and extractions

    NARCIS (Netherlands)

    Reinoso garcia, M.M.; Janczewski, D.J.; Reinhoudt, David; Verboom, Willem; Malinowska, Elzbieta; Pietrzak, Mariusz; Hill, Clement; Baca, Jiri; Gruner, Bohumir; Selucky, Pavel; Gruttner, Cordula

    2006-01-01

    Ligand systems containing three carbamoylmethylphosphonate (CMP) or -phosphine oxide (CMPO) moieties attached to a tripodal platform have been synthesized for metal complexation and subsequent extraction from HNO3 solutions. The incorporation into ion selective electrodes (ISE) and picrate

  18. Knudsen cell mass spectrometric study of the Cs2IOH(g) molecule thermodynamics

    International Nuclear Information System (INIS)

    Roki, F-Z.; Ohnet, M-N.; Fillet, S.; Chatillon, C.; Nuta, I.

    2013-01-01

    Highlights: • The pronounced ionic character leads to only dissociative ionization processes. • Ions formed are same as those coming from pure dimmers. • De-convolution of the ions origin needs accurate thermodynamic values for the pure gas phase. • Mass spectrometric interpretation has to be performed gradually and as a function of suitable condensed compositions. • Thermal functions have to be fully estimated. -- Abstract: The gas phase of the CsI + CsOH system is analyzed by high temperature Knudsen cell mass spectrometry in order to confirm the existence of the Cs 2 IOH(g) complex molecule. The mass spectrometric analysis is quite complex since such molecules undergo dissociative ionization into fragment ions that mix with the same ions from dimers of the pure compounds in the same vapor phase. Varying the chemical conditions for vaporization by using different CsI + CsOH mixture contents showed that the ionization of the Cs 2 IOH(g) molecule led to five different fragment ions, Cs 2 OH + , Cs 2 I + , Cs + , CsOH + and CsI + . This complex ionization pattern was studied in relation with previous assessed values for the vaporization of CsOH and CsI pure compounds in which monomer and dimer molecules are predominant. The equilibrium constant for the reaction CsI(g) + CsOH(g) = Cs 2 IOH(g) was determined and, after modeling the structure of the Cs 2 IOH molecule, the enthalpy of formation was determined using the third law of thermodynamics, as follows: Δ f H°(Cs 2 IOH, g, 298.15 K) = −578 ± 14.7 kJ · mole −1

  19. Energy-resolved X-ray imaging: Material decomposition methods adapted for spectrometric detectors

    International Nuclear Information System (INIS)

    Potop, Alexandra-Iulia

    2014-01-01

    Scintillator based integrating detectors are used in conventional X-ray imaging systems. The new generation of energy-resolved semiconductor radiation detectors, based on CdTe/CdZnTe, allows counting the number of photons incident on the detector and measure their energy. The LDET laboratory developed pixelated spectrometric detectors for X-ray imaging, associated with a fast readout circuit, which allows working with high fluxes and while maintaining a good energy resolution. With this thesis, we bring our contribution to data processing acquired in radiographic and tomographic modes for material components quantification. Osteodensitometry was chosen as a medical application. Radiographic data was acquired by simulation with a detector which presents imperfections as charge sharing and pile-up. The methods chosen for data processing are based on a material decomposition approach. Basis material decomposition models the linear attenuation coefficient of a material as a linear combination of the attenuations of two basis materials based on the energy related information acquired in each energy bin. Two approaches based on a calibration step were adapted for our application. The first is the polynomial approach used for standard dual energy acquisitions, which was applied for two and three energies acquired with the energy-resolved detector. We searched the optimal configuration of bins. We evaluated the limits of the polynomial approach with a study on the number of channels. To go further and take benefit of the elevated number of bins acquired with the detectors developed in our laboratory, a statistical approach implemented in our laboratory was adapted for the material decomposition method for quantifying mineral content in bone. The two approaches were compared using figures of merit as bias and noise over the lengths of the materials traversed by X-rays. An experimental radiographic validation of the two approaches was done in our laboratory with a

  20. New amperometric and potentiometric immunosensors based on gold nanoparticles/tris(2,2'-bipyridyl)cobalt(III) multilayer films for hepatitis B surface antigen determinations.

    Science.gov (United States)

    Tang, Dianping; Yuan, Ruo; Chai, Yaqin; Fu, Yingzi; Dai, Jianyuan; Liu, Yan; Zhong, Xia

    2005-10-15

    Two generic, fast, sensitive and novel electrochemical immunosensors have been developed. Initially, a layer of plasma-polymerized Nafion film (PPF) was deposited on the platinum electrode surface, then positively charged tris(2,2'-bipyridyl)cobalt(III) (Co(bpy)(3)(3+)) and negatively charged gold nanoparticles were assembled on the PPF-modified Pt electrode by layer-by-layer technique. Finally, hepatitis B surface antibody (HBsAb) was electrostatically adsorbed on the gold nanoparticles surface. Electrochemical behavior of the {Au/Co(bpy)(3)(3+)}(n) multilayer film-modified electrodes was studied. Cyclic voltammetry, electrochemical impedance spectroscopy (EIS) were adopted to monitor the regular growth of the multilayer films. The performance and factors influencing the performance of the resulting immunosensors were studied in detail. The multilayer film-modified immunosensor was used for hepatitis B surface antigen (HBsAg) determination via the amperometric and potentiometric immunosensor systems, and both systems provided the same linear ranges from 0.05 to 4.5 microg/mL with different detection limits for the amperometric system 0.005 microg/mL and for the potentiometric system 0.015 microg/mL. The immunosensors were used to analyse HBsAg in human serum samples. Analytical results of clinical samples show that the developed immunoassay is comparable with the enzyme-linked immunosorbent assays (ELISAs) method, implying a promising alternative approach for detecting HBsAg in the clinical diagnosis. In addition, the multilayer films also showed better stability for 1 month at least.

  1. Fusion of Potentiometric & Voltammetric Electronic Tongue for Classification of Black Tea Taste based on Theaflavins (TF) Content

    Science.gov (United States)

    Bhattacharyya, Nabarun; Legin, Andrey; Papieva, Irina; Sarkar, Subrata; Kirsanov, Dmitry; Kartsova, Anna; Ghosh, Arunangshu; Bandyopadhyay, Rajib

    2011-09-01

    Black tea is an extensively consumed beverage worldwide with an expanding market. The final quality of black tea depends upon number of chemical compounds present in the tea. Out of these compounds, theaflavins (TF), which is responsible for astringency in black tea, plays an important role in determining the final taste of the finished black tea. The present paper reports our effort to correlate the theaflavins contents with the voltammetric and potentiometric electronic tongue (e-tongue) data. Noble metal-based electrode array has been used for collecting data though voltammetric electronic tongue where as liquid filled membrane based electrodes have been used for potentiometric electronic tongue. Black tea samples with tea taster score and biochemical results have been collected from Tea Research Association, Tocklai, India for the analysis purpose. In this paper, voltammetric and potentiometric e-tongue responses are combined to demonstrate improvement of cluster formation among tea samples with different ranges of TF values.

  2. Cobalt(II) salophen-modified carbon-paste electrode for potentiometric and voltammetric determination of cysteine.

    Science.gov (United States)

    Amini, Mohammad K; Khorasani, Jafar H; Khaloo, Shokooh S; Tangestaninejad, Shahram

    2003-09-01

    A chemically modified electrode constructed by incorporating N,N(')-bis(salicylidene)-1,2-phenylenediaminocobalt(II) into carbon-paste matrix was used as a sensitive electrochemical sensor for detection of cysteine. The resulting electrode exhibits catalytic properties for the electrooxidation of cysteine and lowers the overpotential for the oxidation of this compound. The faster rate of electron transfer results in a near-Nernstian behavior of the modified electrode and makes it a suitable potentiometric and voltammetric sensor for the fast and easy determination of cysteine. A linear response in concentration range from approximately 2 microM to 0.01 M was obtained with a detection limit of 1 microM for the potentiometric detection of cysteine. The modified electrode was also used for the amperometric and differential pulse voltammetric determination of cysteine and the results were compared with those of the potentiometric method.

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

    Energy Technology Data Exchange (ETDEWEB)

    Cubuk, Osman [Department of Chemistry, Faculty of Arts and Sciences, Erzincan University, 24100 Erzincan (Turkey); Caglar, Bulent, E-mail: bcaglar55@gmail.com [Department of Chemistry, Faculty of Arts and Sciences, Erzincan University, 24100 Erzincan (Turkey); Topcu, Cihan; Coldur, Fatih; Sarp, Gokhan [Department of Chemistry, Faculty of Arts and Sciences, Erzincan University, 24100 Erzincan (Turkey); Tabak, Ahmet [Department of Chemistry, Faculty of Arts and Sciences, Recep Tayyip Erdoğan University, 53100 Rize (Turkey); Sahin, Erdal [Department of Chemistry, Faculty of Arts and Sciences, Erzincan University, 24100 Erzincan (Turkey)

    2015-05-30

    Graphical abstract: - Highlights: • Surfactant cations intercalated with different molecular arrangements into smectite layers. • The electrophoretic mobility values indicate that excess surfactant loadings also create positive charges on the organosmectites surfaces. • A novel potentiometric SCN{sup −} selective electrode was fabricated based on modified smectite. - Abstract: Organosmectites were prepared by the intercalation of hexadecyltrimethylammonium cations at various ratios into interlayer of Unye smectite. Structural, thermal, morphological and textural properties of the synthesized organosmectites were characterized. Afterwards, a novel potentiometric PVC-membrane thiocyanate selective electrode was prepared based on the obtained hexadecyltrimethylammonium modified smectites as electroactive material. The basal spacing values of organosmectites were observed in the range of 15.61 and 35.50 Å. Powder X-ray diffraction data show that the surfactant cations penetrated into the smectite layers with different molecular arrangements. Modification of smectite with hexadecyltrimethylammonium led to appreciable decreases in the intensities of the FTIR bands at 3402 and 1635 cm{sup −1} and the new characteristic vibrational bands at 2927, 2850, 1472 and 722 cm{sup −1} originating from the surfactant molecules appeared. The thermal analysis data showed that the decomposition of surfactant species occurred in the temperature range of 170–720 °C and the amount of dehydrated water gradually decreased with the increase in surfactant amount. The intercalation of surfactant species within the gallery spacing led gradually to smaller surface areas. In addition, the electrophoretic mobility values indicate that excess surfactant loadings also generate positive charges on the organosmectite surfaces. The most convenient membrane composition resulting in the best potentiometric performance was investigated. The optimum membrane composition was determined to

  4. Analysis of Lead and Zinc by Mercury-Free Potentiometric Stripping Analysis

    DEFF Research Database (Denmark)

    Andersen, Jens Enevold Thaulov

    1997-01-01

    A method is presented for trace-element analysis of lead and zinc by potentiometric stripping analysis (PSA) where both the glassy-carbon working electrode and the electrolyte are free of mercury. Analysis of zinc requires an activation procedure of the glassy-carbon electrode. The activation...... is performed by pre-concentrating zinc on glassy carbon at -1400 mV(SCE) in a mercury-free electrolyte containing 0.1 M HCl and 2 ppm Zn2+, followed by stripping at approx. -1050 mV. A linear relationship between stripping peak areas, recorded in the derivative mode, and concentration was found...

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

    International Nuclear Information System (INIS)

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

    1995-01-01

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

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

    International Nuclear Information System (INIS)

    Verdingh, V.; Le Duigou, Y.

    1991-01-01

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

  7. Integrated potentiometric detector for use in chip-based flow cells

    Science.gov (United States)

    Tantra; Manz

    2000-07-01

    A new kind of potentiometric chip sensor for ion-selective electrodes (ISE) based on a solvent polymeric membrane is described. The chip sensor is designed to trap the organic cocktail inside the chip and to permit sample solution to flow past the membrane. The design allows the sensor to overcome technical problems of ruggedness and would therefore be ideal for industrial processes. The sensor performance for a Ba2+-ISE membrane based on a Vogtle ionophore showed electrochemical behavior similar to that observed in conventional electrodes and microelectrode arrangements.

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

    African Journals Online (AJOL)

    The voltage or current cannot be sensed with digital systems. To perform the transformation of a voltage or current level into a digital value an analog-to-digital converter. (ADC) is used [13]. When interfacing an analog signal from the instrument to the ADC we have to consider the input range of the device. If the input is too ...

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

    Science.gov (United States)

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

    2009-01-01

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

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

    Science.gov (United States)

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

    2009-01-01

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

  11. The Difference Between the Potentiometric Surfaces of the Magothy Aquifer in Southern Maryland, September 1975 and September 2009

    Science.gov (United States)

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

    2010-01-01

    This report presents a map showing the change in the potentiometric surface of the Magothy aquifer in the Magothy Formation of Late Cretaceous age in Southern Maryland between September 1975 and September 2009. The map, based on water level differences obtained from 48 wells, shows that during the 34-year period, the potentiometric surface had little change at the outcrop area, which is in the northernmost part of the study area, but declined 75 feet at Waldorf. Waldorf is located near the southwesternmost part of the study area, and approaches the downdip boundary of the aquifer. The map also shows well yield in gallons per day for 2008 at wells or well fields.

  12. Potentiometric maps and ground-water-level data for the industrial area, northwest of Delaware City, Delaware

    Science.gov (United States)

    Donnelly, Colleen A.; Hinaman, Kurt C.

    1996-01-01

    Potentiometric maps of the water-table aquifer in the spring and fall of 1993 in the industrial area northwest of Delaware City, Delaware, are presented. The maps are based on continuously recorded ground-water-level data collected at eight wells screened in the water-table aquifer from October 15, 1993 through November 8, 1994. These data are presented on a 33" by 44" plate. The U.S. Army Corps of Engineers collected the synoptic water-level data used to construct contours of the potentiometric surface in the water-table aquifer. The U.S. Geological Survey collected the continuously recorded ground- water-level data.

  13. Cobalt phthalocyanine as a novel molecular recognition reagent for batch and flow injection potentiometric and spectrophotometric determination of anionic surfactants

    OpenAIRE

    El-Nemma, Eman M.; Badawi, Nahla M.; Hassan, Saad S. M.

    2008-01-01

    Cobalt(II) phthalocyanine [Co(II)Pc] is used as both an ionophore and chromogen for batch and flow injection potentiometric and spectrophotometric determination of anionic surfactants (SDS), respectively. The potentiometric technique involves preparation of a polymeric membrane sensor by dispersing [Co(II)Pc] in a plasticized PVC membrane. Under batch mode of operation, the sensor displays a near-Nernstian slope of −56.5 mV decade−1, wide response linear range of 7.8 × 10−4 to 8.0 × 10−7 mol ...

  14. Use of 3-(4-hydroxyphenyl)propionic acid as electron donating compound in a potentiometric aflatoxin M{sub 1}-immunosensor

    Energy Technology Data Exchange (ETDEWEB)

    Rameil, Steffen, E-mail: s.rameil@r-biopharm.de [R-Biopharm AG, An der neuen Bergstrasse 17, 64297 Darmstadt (Germany); Schubert, Peter, E-mail: p.schubert@r-biopharm.de [R-Biopharm AG, An der neuen Bergstrasse 17, 64297 Darmstadt (Germany); Grundmann, Peter, E-mail: peter.grundmann@jennewein-biotech.de [R-Biopharm AG, An der neuen Bergstrasse 17, 64297 Darmstadt (Germany); Dietrich, Richard, E-mail: R.Dietrich@mh.vetmed.uni-muenchen.de [Department of Veterinary Sciences, University of Munich, Schoenleutner Str 8, 85764 Oberschleissheim (Germany); Maertlbauer, Erwin, E-mail: E.Maertlbauer@mh.vetmed.uni-muenchen.de [Department of Veterinary Sciences, University of Munich, Schoenleutner Str 8, 85764 Oberschleissheim (Germany)

    2010-02-19

    We developed a potentiometric aflatoxin M{sub 1}-immunosensor which utilizes 3-(4-hydroxyphenyl)propionic acid (p-HPPA) as electron donating compound for horseradish peroxidase (HRP; EC 1.11.1.7). The assay system consists of a polypyrrole-surface-working electrode coated with a polyclonal anti-M{sub 1} antibody (pAb-AFM{sub 1}), a Ag/AgCl reference electrode and a HRP-aflatoxin B{sub 1} conjugate (HRP-AFB{sub 1} conjugate). To optimize the potentiometric measuring system p-HPPA as well as related compounds serving as electron donating compounds were compared. Also the influence of different buffer systems, varying pH and substrate concentrations on signal intensity was investigated. Our results suggest that reaction conditions that favor the formation of Pummerer's type ketones lead to an increase in signal intensity rather than formation of fluorescent dye. Comparison with commercial ready-to-use HRP electron donating compounds such as 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) diammonium salt (ABTS), o-phenylenediamine (OPD) or 3,3',5,5'-tetramethylbenzidine (TMB) showed that only 34%, 77% and 49% of the signal intensity of p-HPPA were reached, respectively. The optimized assay had a detection limit of 40 pg mL{sup -1} and allowed detection of 500 pg mL{sup -1} (FDA action limit) aflatoxin M{sub 1} (AFM{sub 1}) in pasteurized milk and UHT-milk containing 0.3-3.8% fat within 10 min without any sample treatment. The working range was between 250 and 2000 pg mL{sup -1} AFM{sub 1}.

  15. 5th colloquium on atomic spectrometric trace analysis

    International Nuclear Information System (INIS)

    Welz, B.

    1989-01-01

    This book deals with apparatus, use-oriented and theoretical aspects of trace analysis and spectroscopy. General articles are concerned with the analysis of environmentally relevant samples; a comparison of modern spectroscopic techniques, the coupling of hydride production, chromatography and spectrometry; chemical modifiers for graphite tube furnace atomic absorption spectroscopy (AAS), and possible applications of flow injection to atomic spectrometric trace analysis - one of the outstanding subjects of the colloquium. About one quarter of the 85 contributions deals with new techniques including flow injection. Other priority subjects are the theory and application of graphite tube furnace AAS, and a comparison between different dissolution methods and direct solid analysis. Medicine and toxicology, analysis of biological materials and environmentally relevant samples are in the foreground of use-oriented papers. (orig./BBR) [de

  16. Mass spectrometric methods for trace analysis of metals

    International Nuclear Information System (INIS)

    Bahr, U.; Schulten, H.R.

    1981-01-01

    A brief outline is given of the principles of mass spectrometry (MS) and the fundamentals of qualitative and quantitative mass spectrometric analysis emphasizing recent developments and results. Classical methods of the analysis of solids, i.e. spark-source MS and thermal ionization MS, as well as recent methods of metal analysis are described. Focal points in this survey of recently developed techniques include secondary ion MS, laser probe MS, plasma ion source MS, gas discharge MS and field desorption MS. Here, a more detailed description is given and the merits of these emerging methods are discussed more explicitly. In particular, the results of the field desorption techniques in elemental analyses are reviewed and critically evaluated

  17. Correlation between Electrical Properties and Potentiometric Response of CS-Clay Nanocomposite Membranes

    Directory of Open Access Journals (Sweden)

    M. Oviedo Mendoza

    2015-01-01

    Full Text Available The aim of this work is to study the relationship between electrical, structure, and potentiometric response to nitrate anions using Ion Selective Electrodes (ISE. These ISE are based on chitosan-montmorillonite nanocomposite membranes with different content of montmorillonite. Membrane properties have been studied using SEM, FTIR, and impedance spectroscopy measurements. With the advent of impedance spectroscopy one is allowed to obtain the DC conductivity dependence on montmorillonite concentration and the percolation threshold. Additionally, the potentiometric response to nitrate anions of ISE based on chitosan-clay nanocomposite has been investigated. It is shown that the properties and performance of these membrane electrodes depend upon the clay wt% and that the best sensitivity to nitrate ions (with detection limit 7 × 10−5 M is obtained near the percolation concentration ca. 8 ± 2.5 wt% of clay. This observation is traceable to higher clay content (higher agglomeration that tends to decrease the intercalation and absorption of the number of chitosan chains in the interlayer space of montmorillonite.

  18. Potentiometric Surface of the Lower Patapsco Aquifer in Southern Maryland, September 2007

    Science.gov (United States)

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

    2009-01-01

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

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

    Science.gov (United States)

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

    2010-01-01

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

  20. Potentiometric surface of the Upper Patapsco aquifer in southern Maryland, September 2009

    Science.gov (United States)

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

    2010-01-01

    This report presents a map showing the potentiometric surface of the upper Patapsco aquifer in the Patapsco Formation of Early Cretaceous age in Southern Maryland during September 2009. The map is based on water-level measurements in 65 wells. The highest measured water level was 118 feet above sea level near the northern boundary and outcrop area of the aquifer in northern Anne Arundel County. From this area, the potentiometric surface declined to the south toward a well field in the Annapolis-Arnold area, and from all directions toward three additional cones of depression. These cones are located in the Waldorf-La Plata area, Chalk Point, and the Leonardtown-Lexington Park area. The lowest measured groundwater levels were 26 feet below sea level at Annapolis, 108 feet below sea level south of Waldorf, 60 feet below sea level at Chalk Point, and 83 feet below sea level at Leonardtown. The map also shows well yield in gallons per day for 2008 at wells or well fields.

  1. Potentiometric Surface of the Upper Patapsco Aquifer in Southern Maryland, September 2007

    Science.gov (United States)

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

    2009-01-01

    This report presents a map showing the potentiometric surface of the upper Patapsco aquifer in the Patapsco Formation of Early Cretaceous age in Southern Maryland during September 2007. The map is based on water-level measurements in 50 wells. The highest measured water level was 120 feet above sea level near the northern boundary and outcrop area of the aquifer in northern Anne Arundel County. From this area, the potentiometric surface declined to the south toward a well field in the Annapolis-Arnold area, and from all directions toward four cones of depression. These cones are located in the Waldorf-La Plata area, Chalk Point-Prince Frederick area, Swan Point subdivision in southern Charles County, and the Lexington Park-St. Inigoes area. The lowest measured ground-water level was 44 feet below sea level at Arnold, 106 feet below sea level south of Waldorf, 54 feet below sea level at Swan Point, 59 feet below sea level at Chalk Point, and 58 feet below sea level at Lexington Park.

  2. Potentiometric and spectrofluorimetric studies on complexation of tenoxicam with some metal ions.

    Science.gov (United States)

    Mohamed, Horria A; Wadood, Hanaa M A; Farghaly, Othman A

    2002-06-01

    The interaction of tenoxicam with six metal ions, viz. Fe(III), Bi(III), Sb(III), Cr(III), Cd(II) and Al(III) was studied using potentiometric and fluorimetric methods. In the potentiometric method the ionization constant of the ligand and stability constants of the complexes formed have been tabulated at 25+/-0.1 degrees C, ionic strength of NaNO3 in 50% (v/v) aqueous acetonitrile solution was 0.05 mol x dm(-3). Complexes of 1:1 and/or 1:2 and/or 1:3 metal to ligand ratios are formed. The fluorescence of tenoxicam in the presence and absence of the metal ions was studied. The drug can be determined fluorimetrically in 0.5 M HNO3 at an emission wavelength of 450 nm (excitation at 350 nm). The linear range is 0.040-0.2 microg/ml in the absence of Al(III) and 0.016-0.1 microg/ml in the presence of Al(III). Tenoxicam was determined by the proposed method in tablet, suppository and injection. The recovery percent ranged from 98.16 to 102.22%. The effect of 2-aminopyridine on the recovery of tenoxicam was also investigated.

  3. Potentiometric stripping analysis of Cadmium and Lead in superficial waters

    International Nuclear Information System (INIS)

    Arias, Juan Miguel; Marciales Castiblanco, Clara

    2003-01-01

    This paper contains the implementation and validation of an analytical method for determining cadmium and lead in surface waters. This is a valuable tool for the description of actual conditions and qualitative and quantitative control of dangerous heavy metals discharge in water bodies. Test were run for selecting stripping potentiometry conditions that as indicated by results were: sample oxidant concentration 36.4 μg/L Hg 2+ stirring frequency 2400 rpm, electrolysis time 80 s., electrolysis potential -950 mV and pH of 2.0. Interference of Cu 2+ and Fe 2+ showed that copper concentrations larger than 150 μg/L and 500 μg/L negatively influence the analytical response for Cadmium and lead respectively; [Fe 3+ ] larger than 60 μg/L and 400 μg/L cause variations in cadmium and lead read content respectively. Linear concentration range for cadmium lies between 5 and 250 μg/L; for lead range goes from 10 to 250 μg/L. Precision expressed as repeatability for both system and method, exhibit good reproducibility with variation coefficients below 6%. Accuracy, assessed from recuperation, is strongly influenced by concentration level therefore standard addition is recommended for lead and cadmium quantification. Analysis performed on surface waters from Colombian Magdalena and Cauca rivers pointed lead and cadmium contents below detection limits

  4. Mass spectrometric imaging of red fluorescent protein in breast tumor xenografts

    NARCIS (Netherlands)

    Chughtai, K.; Jiang, L.; Post, H.; Winnard Jr., P.T.; Greenwood, T.R.; Raman, V.; Bhujwalla, Z.V.; Heeren, R.M.A.; Glunde, K.

    2013-01-01

    Abstract. Mass spectrometric imaging (MSI) in combination with electrospray mass spectrometry (ESI-MS) is a powerful technique for visualization and identification of a variety of different biomolecules directly from thin tissue sections. As commonly used tools for molecular reporting,

  5. Enrichment/isolation of phosphorylated peptides on hafnium oxide prior to mass spectrometric analysis.

    Science.gov (United States)

    Rivera, José G; Choi, Yong Seok; Vujcic, Stefan; Wood, Troy D; Colón, Luis A

    2009-01-01

    Hafnium oxide (hafnia) exhibits unique enrichment properties towards phosphorylated peptides that are complementary to those of titanium oxide (titania) and zirconium oxide (zirconia) for use with mass spectrometric analysis in the field of proteomics.

  6. An efficient ab initio DFT and PCM assessment of the potentiometric selectivity of a salophen type Schiff base.

    Science.gov (United States)

    Demir, Serkan; Yilmaz, Hakan; Dilimulati, Maowulidan; Andaç, Müberra

    2014-06-01

    As a neutral carrier component for the preparation of a potentiometric membrane sensor, the affinity and selectivity of the salophen type Schiff base ligand obtained by 1:2 condensation of 2.3-diaminopyridine with salicylaldehyde toward a series of common cations has been fully examined by DFT/B3LYP and integral equation formalism polarizable continum model (IEF-PCM or only given with PCM as default input in the computations) in combination with the experimental data. Both the potentiometric measurements and DFT calculations have exhibited that the ionophore shows appreciable selectivity for Cu(2+) ion over other cations. Four different approaches where the last three are the modified version of each other have been evaluated and compared with potentiometric data. Based upon the results of comparison among the approaches suggested to verify the selective behavior of ionophore toward Cu(2+), PCM implemented approach having a whole computational groundwork has given well-matched results with the observed data and with the method augmented with experimental hydration energies. The foremost interferences were detected by determining potentiometric selectivity coefficients for each metal ion relative to Cu(2+) and compared to the results obtained by the DFT calculations.

  7. Review of procedures involving separation and preconcentration for the determination of cadmium using spectrometric techniques

    International Nuclear Information System (INIS)

    Ferreira, Sergio L.C.; Andrade, Jailson B. de; Korn, Maria das Gracas A.; Pereira, Madson de G.; Lemos, Valfredo A.; Santos, Walter N.L. dos; Rodrigues, Frederico de Medeiros; Souza, Anderson S.; Ferreira, Hadla S.; Silva, Erik G.P. da

    2007-01-01

    Spectrometric techniques for the analysis of trace cadmium have developed rapidly due to the increasing need for accurate measurements at extremely low levels of this element in diverse matrices. This review covers separation and preconcentration procedures, such as electrochemical deposition, precipitation, coprecipitation, solid phase extraction, liquid-liquid extraction (LLE) and cloud point extraction (CPE), and consider the features of the their application with several spectrometric techniques

  8. A gas/liquid chromatographic-mass spectrometric method for the rapid screening of 250 pesticides in aqueous matrices

    Energy Technology Data Exchange (ETDEWEB)

    Chandramouli, B.; Harvan, D.; Brittain, S.; Hass, R. [Eno River Labs, LLC. Durham, NC (United States)

    2004-09-15

    Pesticide residues in food present a potentially serious and significant cause for concern. Many pesticides have been associated with significant health effects to the nervous and endocrine systems and some have been deemed carcinogenic. There are many well-established techniques for pesticide analysis. However, commercial pesticide methods have traditionally only been available for specific pesticide families, such as chlorinated pesticides or herbicides, and at detection limits ranging from 0.05 ppb to 1 ppm in aqueous matrices. Techniques that can quickly screen for the presence/absence of pesticide residues in food matrices are critical in ensuring the safety of food and water. This paper outlines a combined Gas Chromatographic-High Resolution Mass Spectrometric (GC-HRMS) and Liquid Chromatographic Tandem Mass Spectrometric (LC-MS/MS) screening assay for 250 pesticides that was developed for use in water, and soda samples at screening levels ranging from 0.1-5 ppb. The pesticides selected have been identified by the European Union as being of concern and the target of possible legislation. The list encompasses a variety of pesticide classes and compound groupings.

  9. Use of information visualization methods eliminating cross talk in multiple sensing units investigated for a light-addressable potentiometric sensor.

    Science.gov (United States)

    Siqueira, José R; Maki, Rafael M; Paulovich, Fernando V; Werner, Carl F; Poghossian, Arshak; de Oliveira, Maria C F; Zucolotto, Valtencir; Oliveira, Osvaldo N; Schöning, Michael J

    2010-01-01

    The integration of nanostructured films containing biomolecules and silicon-based technologies is a promising direction for reaching miniaturized biosensors that exhibit high sensitivity and selectivity. A challenge, however, is to avoid cross talk among sensing units in an array with multiple sensors located on a small area. In this letter, we describe an array of 16 sensing units of a light-addressable potentiometric sensor (LAPS), which was made with layer-by-layer (LbL) films of a poly(amidomine) dendrimer (PAMAM) and single-walled carbon nanotubes (SWNTs), coated with a layer of the enzyme penicillinase. A visual inspection of the data from constant-current measurements with liquid samples containing distinct concentrations of penicillin, glucose, or a buffer indicated a possible cross talk between units that contained penicillinase and those that did not. With the use of multidimensional data projection techniques, normally employed in information visualization methods, we managed to distinguish the results from the modified LAPS, even in cases where the units were adjacent to each other. Furthermore, the plots generated with the interactive document map (IDMAP) projection technique enabled the distinction of the different concentrations of penicillin, from 5 mmol L(-1) down to 0.5 mmol L(-1). Data visualization also confirmed the enhanced performance of the sensing units containing carbon nanotubes, consistent with the analysis of results for LAPS sensors. The use of visual analytics, as with projection methods, may be essential to handle a large amount of data generated in multiple sensor arrays to achieve high performance in miniaturized systems.

  10. Enantioanalysis of S-deprenyl using enantioselective, potentiometric membrane electrodes based on C60 derivatives

    International Nuclear Information System (INIS)

    Stefan-van Staden, Raluca-Ioana

    2010-01-01

    Enantioselective, potentiometric membrane electrodes based on (1,2-methanofullerene C 60 )-61-carboxylic acid, diethyl (1,2-methanofullerene C 60 )-61-61-dicarboxylate and tert-butyl (1,2-methanofullerene C 60 )-61-carboxylic acid were proposed for the enantioanalysis of S-deprenyl in pharmaceutical compounds. Molecular modeling calculations were performed to prove the reliability of the proposed electrodes. The different characteristics involved in this analysis were explained, namely (i) the stability of each molecule using total energy, hardness and dipole moment, and (ii) the explanation of the mechanism of interaction using intermolecular forces (moderate hydrogen bond interactions), atomic charges and electrostatic potential. Electronic structures as well as molecular interaction have been investigated using Hartree-Fock theory, 3-21G(*) basis set. Stability and feasibility of all the generated structures were supported by their respective energy minima and fundamental frequencies.

  11. Open ISEmeter: An open hardware high-impedance interface for potentiometric detection

    International Nuclear Information System (INIS)

    Salvador, C.; Carbajo, J.; Mozo, J. D.; Mesa, M. S.; Durán, E.; Alvarez, J. L.

    2016-01-01

    In this work, a new open hardware interface based on Arduino to read electromotive force (emf) from potentiometric detectors is presented. The interface has been fully designed with the open code philosophy and all documentation will be accessible on web. The paper describes a comprehensive project including the electronic design, the firmware loaded on Arduino, and the Java-coded graphical user interface to load data in a computer (PC or Mac) for processing. The prototype was tested by measuring the calibration curve of a detector. As detection element, an active poly(vinyl chloride)-based membrane was used, doped with cetyltrimethylammonium dodecylsulphate (CTA + -DS − ). The experimental measures of emf indicate Nernstian behaviour with the CTA + content of test solutions, as it was described in the literature, proving the validity of the developed prototype. A comparative analysis of performance was made by using the same chemical detector but changing the measurement instrumentation.

  12. Open ISEmeter: An open hardware high-impedance interface for potentiometric detection

    Energy Technology Data Exchange (ETDEWEB)

    Salvador, C.; Carbajo, J.; Mozo, J. D., E-mail: jdaniel.mozo@diq.uhu.es [Applied Electrochemistry Laboratory, Faculty of Experimental Sciences, University of Huelva, Av. 3 de Marzo s/n., 21007 Huelva (Spain); Mesa, M. S.; Durán, E. [Department of Electronics Engineering, Computers and Automatic, ETSI, University of Huelva, Campus de La Rabida, 21810 Huelva (Spain); Alvarez, J. L. [Department of Information Technologies, ETSI, University of Huelva, Campus de La Rabida, 21810 Huelva (Spain)

    2016-05-15

    In this work, a new open hardware interface based on Arduino to read electromotive force (emf) from potentiometric detectors is presented. The interface has been fully designed with the open code philosophy and all documentation will be accessible on web. The paper describes a comprehensive project including the electronic design, the firmware loaded on Arduino, and the Java-coded graphical user interface to load data in a computer (PC or Mac) for processing. The prototype was tested by measuring the calibration curve of a detector. As detection element, an active poly(vinyl chloride)-based membrane was used, doped with cetyltrimethylammonium dodecylsulphate (CTA{sup +}-DS{sup −}). The experimental measures of emf indicate Nernstian behaviour with the CTA{sup +} content of test solutions, as it was described in the literature, proving the validity of the developed prototype. A comparative analysis of performance was made by using the same chemical detector but changing the measurement instrumentation.

  13. Potentiometric stripping analysis of lead and cadmium leaching from dental prosthetic materials and teeth

    Directory of Open Access Journals (Sweden)

    GORAN M. NIKOLIC

    2004-07-01

    Full Text Available Potentiometric stipping analysis (PSA was applied for the determination of lead and cadmium leaching from dental prosthetic materials and teeth. The soluble lead content in finished dental implants was found to be much lower than that of the individual components used for their preparation. Cadmium was not detected in dental implants and materials under the defined conditions. The soluble lead and cadmium content of teeth was slightly lower than the lead and cadmium content in whole teeth (w/w reported by other researchers, except in the case of a tooth with removed amalgam filling. The results of this work suggest that PSA may be a good method for lead and cadmium leaching studies for investigation of the biocompatibility of dental prosthetic materials.

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

    Directory of Open Access Journals (Sweden)

    MARIA PLENICEANY

    2005-02-01

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

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

    International Nuclear Information System (INIS)

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

    1985-01-01

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

  16. Functionalization of PVC membrane with ss oligonucleotides for a potentiometric biosensor.

    Science.gov (United States)

    Shishkanova, T V; Volf, R; Krondak, M; Král, V

    2007-05-15

    A novel application of a single stranded (ss) oligonucleotide as an active component of polymeric membrane in an ion-selective electrode (ISE) is described. The original oligonucleotides, oligo(dA)(15), modified by cholesterol, triphenylmethyl and hexadecyl derivatives, were immobilized into poly(vinyl chloride) (PVC) membrane using extraction protocol. In parallel, the adsorption protocol was used to immobilize unmodified oligo(dA)(15) on the PVC membrane based on tridodecylmethyammonium chloride (TDDMA(+)Cl(-)). Immobilization of ss oligonucleotide probe through spacer was more effective for the potentiometric detection of the hybridization between complementary oligonucleotides. It was found that cholesterol-oligo(dA)(15) modified membranes were sensitive toward complementary oligo(dT)(15) in the concentration range 2-80 nM at pH 7. An explanation for the detection mechanism is proposed.

  17. Potentiometric titration of Co(II) in presence of Co(III).

    Science.gov (United States)

    Norkus, E

    1998-12-01

    A potentiometric titration for cobalt(II) determination in the presence of Co(III) based on the oxidation of Co(II) with Na(2)CrO(4) in ethylenediamine medium and back-titration of the oxidant excess with (NH(4))(2)Fe(SO(4))(2) in acid medium is described. The titration is monitored with a Pt indicator electrode and carried out until the greatest jump of potential from one drop of titrant appears. A RSD smaller than 1.5% has been obtained for 50-300 mumol Co(II). The method proposed was applied in the analysis of a new type electroless copper plating solutions containing Co(II)-ethylenediamine complex compounds as reducing agents. Cu(II), Co(III) and Cr(III) do not interfere in the determination of Co(II).

  18. A poly(pyrrole-Cobalt(IIdeuteroporphyrin electrode for the potentiometric determination of nitrite

    Directory of Open Access Journals (Sweden)

    Michael Wedel

    2003-07-01

    Full Text Available The electrochemical properties of a new Co(II deuteroporphyrin substituted by two electropolymerizable pyrrole groups has been investigated in organic solvent. This functionalization has allowed the preparation of the first example of a cobalt deuteroporphyrin film by oxidative electropolymerization. The resulting conducting polypyrrole film exhibits the regular electroactivity of cobalt deuteroporphyrin. Compared to conventional cobalt porphyrin electrochemistry, the replacement of porphyrin macrocycle by deuteroporphyrin ring results in markedly more negative potential values for the metalcentered oxidation and reduction processes. The influence of NO2- as axial ligand on the reductive behavior of the electropolymerized cobalt (II deuteroporphyrin is examined. The recognition properties of the film illustrated by the potentiometric shift of the Co(II/(I reduction were exploited for the determination of NO2- in the concentration range 2 10-6- 2.5 10-4 M.

  19. Potentiometric studies on mixed-ligand chelates of uranyl ion with carboxylic acid phenolic acids

    International Nuclear Information System (INIS)

    Bandiwadekar, S.P.; Chavar, A.M.

    1988-01-01

    Mixed ligand complexes of UO 2 2+ with bidentate carboxylic and phenolic acids have been studied potentiometrically at 30 ± 0.1degC and μ=0.2M (NaClO 4 ). 1:1 and 1:2 complexes of UO 2 2+ with phthalic acid (PTHA), maleic acid (MAE), malonic acid (MAL), quinolinic acid (QA), 5-sulphosalicylic acid (5-SSA), salicylic acid (SA), and only 1:1 complexes in the case of mandelic acid (MAD) have been detected. The formation of 1:1:1 mixed ligand complexes has been inferred from simultaneous equilibria in the present study. The values of ΔlogK, Ksub(DAL), Ksub(2LA) or Ksub(2AL) for the ternary complexes have been calculated. The stabilities of mixed ligand complexes depend on the size of the chelate ring and the stabilities of the binary complexes. (author). 15 refs

  20. Carbon paste and PVC electrodes for the flow injection potentiometric determination of dextromethorphan.

    Science.gov (United States)

    Khaled, Elmorsy; Hassan, H N A; Mohamed, Gehad G; Seleim, A A

    2010-04-15

    The construction and performance characteristics of dextromethorphan (DXM) carbon paste (CPEs) and polyvinyl chloride (PVC) electrodes are described. Different modes for electrode modification, including incorporation of ion pairs (IPs), ion pairing agent or soaking the plain electrode in IPs suspension, have been used. Matrices compositions were optimized referring to the effect of modifier and plasticizer. The fabricated electrodes work satisfactorily in the concentration range from 10(-5) to 10(-2) mol L(-1) with fast response time (1.6s) and long operational lifetime (2 months). The developed electrodes have been successfully applied for the potentiometric determination of DXM in pharmaceutical formulation under batch and flow injection analysis (FIA) conditions. Under FIA conditions, the proposed electrodes allow the analysis of 90 samples h(-1) and offer the advantage of simplicity, accuracy and automation feasibility. The solubility products of various DXM-IPs were determined conductometrically. (c) 2010 Elsevier B.V. All rights reserved.

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

    International Nuclear Information System (INIS)

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

    1996-01-01

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

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

    International Nuclear Information System (INIS)

    Mainka, E.; Coerdt, W.

    1978-10-01

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

  3. Potentiometric determination of uranium in simulated Purex Process solutions by acidiometry

    International Nuclear Information System (INIS)

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

    1983-01-01

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

  4. Direct Potentiometric Determination of Penicillamine in Real Samples by Using Copper ISE

    Directory of Open Access Journals (Sweden)

    Tina Vukušić

    2015-12-01

    Full Text Available Direct potentiometric method for determination of penicillamine in pharmaceuticals by using commercial copper ISE is described. Proposed method is very inexpensive, simple and reasonably fast method for determination of Pen in acetic buffer, pH = 4 without pretreatment of pharmaceuticals. Determination is based on the reaction between Pen and Cu2+ from electrode membrane. Described method has linear response range for Pen from 2×10−6 to 1×10−2 mol L−1 with limit of detection of 1.1×10−6 mol L−1. Found concentrations of Pen are in very good agreement with declared ones with standard deviation values in range 4.00−4.50 %.

  5. Paper-based potentiometric pH sensor using carbon electrode drawn by pencil

    Science.gov (United States)

    Kawahara, Ryotaro; Sahatiya, Parikshit; Badhulika, Sushmee; Uno, Shigeyasu

    2018-04-01

    A flexible and disposable paper-based pH sensor fabricated with a pencil-drawn working electrode and a Ag/AgCl paste reference electrode is demonstrated for the first time to show pH response by the potentiometric principle. The sensor substrate is made of chromatography paper with a wax-printed hydrophobic area, and various types of carbon pencils are tested as working electrodes. The pH sensitivities of the electrodes drawn by carbon pencils with different hardnesses range from 16.5 to 26.9 mV/pH. The proposed sensor is expected to be more robust against shape change in electrodes on a flexible substrate than other types of chemiresistive/amperometric pH sensors.

  6. Radio spectrometric survey of un-surveyed areas in Syria

    International Nuclear Information System (INIS)

    Aissa, M.; Al-Hent, R; Jubeli, Y.

    2002-11-01

    The values and distribution of the radioelements e U, e Th, % K and Ur units in the surface geological formations of the west and south sectors of Syrian region, were estimated using carbone gamma ray spectrometric survey. The radiometric maps were prepared, as well as, many geological profiles, cross sections studied in different locations and geochemical samples were analyzed by laboratory gamma ray spectrometry and by x-ray diffractometry, the results of the all sets were compared. In general, the survey shows, low radioelement concentrations in the area, especially on basic rocks (Jabal Al-arab, Hawran) south Syria, and on ultra basic rocks (ophiolitic complex) north-west Syria, but there are some separate anomalous spots were connected with phosphate rocks, detected on cretaceous and Palaeogene age. Some times we noticed high radioelement concentrations haloes associated with fractured zones were already arise from secondary uranium mineralization, as a result of solutions movement through fissures in carbonatic and/or chalk like limestone rocks. finally, the obtained concentrations, represent a background values which has no significant importance for uranium exploration point of view. (author)

  7. Determination of iodine to compliment mass spectrometric measurements

    International Nuclear Information System (INIS)

    Hohorst, F.A.

    1994-11-01

    The dose of iodine-129 to facility personnel and the general public as a result of past, present, and future activities at DOE sites is of continuing interest, WINCO received about 160 samples annually in a variety of natural matrices, including snow, milk, thyroid tissue, and sagebrush, in which iodine-129 is determined in order to evaluate this dose, Currently, total iodine and the isotopic ratio of iodine-127 to iodine-129 are determined by mass spectrometry. These two measurements determine the concentration of iodine-129 in each sample, These measurements require at least 16 h of mass spectrometer operator time for each sample. A variety of methods are available which concentrate and determine small quantities of iodine. Although useful, these approaches would increase both time and cost. The objective of this effort was to determine total iodine by an alternative method in order to decrease the load on mass spectrometry by 25 to 50%. The preparation of each sample for mass spectrometric analysis involves a common step--collection of iodide on an ion exchange bed. This was the focal point of the effort since the results would be applicable to all samples

  8. Study of natural diamond detector spectrometric properties under neutron irradiation

    CERN Document Server

    Alekseyev, A B; Kaschuck, Y; Krasilnikov, A; Portnov, D; Tugarinov, S

    2002-01-01

    Natural diamond detector (NDD) performance was studied up to a neutron fluence of 10 sup 1 sup 5 neutron/cm sup 2. The variations of the NDD spectrometric response to incident alpha-particles from sup 2 sup 4 sup 1 Am source after exposure to fast neutron fluences up to 3x10 sup 1 sup 6 n/cm sup 2 were examined. No significant variations up to the level of 10 sup 1 sup 4 n/cm sup 2 were observed. Degradation of charge collection efficiency at higher fluences is reported. No remarkable increase of the NDD leakage current and count rate change had been observed up to a neutron fluence of 3x10 sup 1 sup 6 n/cm sup 2. The charge collection efficiency variations of neutron irradiated diamond spectrometer were studied ex situ under gamma-rays, beta-radiation and visible light excitation. Charge collection efficiency restoration up to 75% level and the NDD performance stabilization by extrinsic low-intensity visible light (550 nm

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

    Directory of Open Access Journals (Sweden)

    Jokić Anja B.

    2013-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Kasra Saeedfar

    2013-12-01

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

  11. Spectrophotometric and potentiometric determination of piroxicam and tenoxicam in pharmaceutical preparations.

    Science.gov (United States)

    El-Ries, Mohamed A; Mohamed, Gehad; Khalil, Shaeban; El-Shall, Manal

    2003-01-01

    Two simple and accurate methods are described for the determination of piroxicam and tenoxicam in their pharmaceutical preparations. The spectrophotometric method involves the oxidation of these drugs with potassium iodate in acid medium with the liberation of iodine and subsequent extraction with cyclohexane followed by measuring the absorbance at lambda=522 nm. Beer's law is obeyed in the concentration range of 0.05-1.1 and 0.05-0.6 mg x ml(-1) for piroxicam and tenoxicam, respectively. The apparent molar absorptivities of the resulting coloured products are found to be 2.7 x 10(3) and 2.5 x 10(3) l mol(-1) x cm(-1), whereas Sandell sensitivities are 0.012 and 0.013 g x cm(-2) for piroxicam and tenoxicam, respectively. The potentiometric method involves the direct titration of both drugs with N-bromosuccinimide in acid medium and the end point is determined potentiometrically using platinum indicator electrode. Piroxicam and tenoxicam can be determined quantitatively in the concentration range of 0.33-3.37 and 0.33-4.08 mg x ml(-1) for tenoxicam and piroxicam, respectively. The standard deviation and relative standard deviation values are found to be ranged from 0.05-0.07 and 0.37-0.98% and 0.025-0.078 and 0.25-1.2% for tenoxicam and piroxicam, respectively. The two methods are accurate within +/-1.0%. Optimum conditions affecting both methods are studied. The proposed methods are applied for the determination of the drugs in pure form and in commercial pharmaceutical preparations.

  12. Synthesis, spectral, thermal, potentiometric and antimicrobial studies of transition metal complexes of tridentate ligand

    Directory of Open Access Journals (Sweden)

    Sarika M. Jadhav

    2014-01-01

    Full Text Available A series of metal complexes of Cu(II, Ni(II, Co(II, Fe(III and Mn(II have been synthesized with newly synthesized biologically active tridentate ligand. The ligand was synthesized by condensation of dehydroacetic acid (3-acetyl-6-methyl-(2H pyran-2,4(3H-dione or DHA, o-phenylene diamine and fluoro benzaldehyde and characterized by elemental analysis, molar conductivity, magnetic susceptibility, thermal analysis, X-ray diffraction, IR, 1H-NMR, UV–Vis spectroscopy and mass spectra. From the analytical data, the stoichiometry of the complexes was found to be 1:2 (metal:ligand with octahedral geometry. The molar conductance values suggest the non-electrolyte nature of metal complexes. The IR spectral data suggest that the ligand behaves as a dibasic tridentate ligand with ONN donor atoms sequence towards central metal ion. Thermal behaviour (TG/DTA and kinetic parameters calculated by the Coats–Redfern and Horowitz–Metzger method suggest more ordered activated state in complex formation. To investigate the relationship between stability constants of metal complexes and antimicrobial activity, the dissociation constants of Schiff bases and stability constants of their binary metal complexes have been determined potentiometrically in THF–water (60:40% solution at 25 ± 1 °C and at 0.1 M NaClO4 ionic strength. The potentiometric study suggests 1:1 and 1:2 complexation. Antibacterial and antifungal activities in vitro were performed against Staphylococcus aureus, Escherichia coli and Aspergillus niger, Trichoderma, respectively. The stability constants of the metal complexes were calculated by the Irving–Rosotti method. A relation between the stability constant and antimicrobial activity of complexes has been discussed. It is observed that the activity enhances upon complexation and the order of antifungal activity is in accordance with stability order of metal ions.

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

    Science.gov (United States)

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

    2014-12-01

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

  14. Potentiometric determination of trace amounts of volatile thiols in natural gas

    International Nuclear Information System (INIS)

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

    1986-01-01

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

  15. Acidity constants of sparingly water-soluble drugs from potentiometric determinations in aqueous dimethyl sulfoxide.

    Science.gov (United States)

    Fini, A; De Maria, P; Guarnieri, A; Varoli, L

    1987-01-01

    A brief analysis of the acid-base equilibria in pure organic solvents and/or in their aqueous mixtures is reported with the aim of determining dissociation constants of acidic drugs that are sparingly soluble in water. Among aqueous organic mixtures, aqueous Me2SO (80% w/w) presents properties particularly suitable for acid-base studies, and thermodynamically meaningful acidity constants can be obtained by a potentiometric technique, provided that the glass electrode is properly calibrated. Thermodynamic acidity constants of more than 100 acids have been potentiometrically determined at 25 degrees C in this mixed solvent, and the selected series of acids has been divided into four classes according to the nature of the acidic group (COOH, OH, SH) and the structure of the acid (aliphatic, aromatic, heterocyclic). A linear relationship between the experimental pKa values in water and pKa values in aqueous Me2SO (80% w/w) has been found within the single classes and a group of equations has been derived (the asterisk denotes pKa values in which infinite dilution in the mixed solvent is taken as a standard state). For the carboxylic acid class, the following "common" equation has been found: pKa(H2O) = -0.80 + 0.67 pKa (Me2SO; 80% w/w). As an application, pKa values in water are reported for a representative number of sparingly soluble acids. These values have been calculated by means of the "common" equation, using pKa values experimentally determined in aqueous Me2SO (80% w/w). The calculated values are in good agreement with those expected from the acid structures.

  16. Vapor generation – atomic spectrometric techniques. Expanding frontiers through specific-species preconcentration. A review

    Energy Technology Data Exchange (ETDEWEB)

    Gil, Raúl A.; Pacheco, Pablo H.; Cerutti, Soledad [Área de Química Analítica, Facultad de Química Bioquímica y Farmacia, Universidad Nacional de San Luis, Ciudad de San Luis 5700 (Argentina); Instituto de Química de San Luis, INQUISAL, Centro Científico-Tecnológico de San Luis (CCT-San Luis), Consejo Nacional de Investigaciones Científicas y Universidad Nacional de San Luis, Ciudad de San Luis 5700 (Argentina); Martinez, Luis D., E-mail: ldm@unsl.edu.ar [Área de Química Analítica, Facultad de Química Bioquímica y Farmacia, Universidad Nacional de San Luis, Ciudad de San Luis 5700 (Argentina); Instituto de Química de San Luis, INQUISAL, Centro Científico-Tecnológico de San Luis (CCT-San Luis), Consejo Nacional de Investigaciones Científicas y Universidad Nacional de San Luis, Ciudad de San Luis 5700 (Argentina)

    2015-05-22

    This article reviews 120 articles found in SCOPUS and specific Journal cites corresponding to the terms ‘preconcentration’; ‘speciation’; ‘vapor generation techniques’ and ‘atomic spectrometry techniques’ in the last 5 years. - Highlights: • Recent advances in vapor generation and atomic spectrometry were reviewed. • Species-specific preconcentration strategies after and before VG were discussed. • New preconcentration and speciation analysis were evaluated within this framework. - Abstract: We review recent progress in preconcentration strategies associated to vapor generation techniques coupled to atomic spectrometric (VGT-AS) for specific chemical species detection. This discussion focuses on the central role of different preconcentration approaches, both before and after VG process. The former was based on the classical solid phase and liquid–liquid extraction procedures which, aided by automation and miniaturization strategies, have strengthened the role of VGT-AS in several research fields including environmental, clinical, and others. We then examine some of the new vapor trapping strategies (atom-trapping, hydride trapping, cryotrapping) that entail improvements in selectivity through interference elimination, but also they allow reaching ultra-low detection limits for a large number of chemical species generated in conventional VG systems, including complete separation of several species of the same element. This review covers more than 100 bibliographic references from 2009 up to date, found in SCOPUS database and in individual searches in specific journals. We finally conclude by giving some outlook on future directions of this field.

  17. Vapor generation – atomic spectrometric techniques. Expanding frontiers through specific-species preconcentration. A review

    International Nuclear Information System (INIS)

    Gil, Raúl A.; Pacheco, Pablo H.; Cerutti, Soledad; Martinez, Luis D.

    2015-01-01

    This article reviews 120 articles found in SCOPUS and specific Journal cites corresponding to the terms ‘preconcentration’; ‘speciation’; ‘vapor generation techniques’ and ‘atomic spectrometry techniques’ in the last 5 years. - Highlights: • Recent advances in vapor generation and atomic spectrometry were reviewed. • Species-specific preconcentration strategies after and before VG were discussed. • New preconcentration and speciation analysis were evaluated within this framework. - Abstract: We review recent progress in preconcentration strategies associated to vapor generation techniques coupled to atomic spectrometric (VGT-AS) for specific chemical species detection. This discussion focuses on the central role of different preconcentration approaches, both before and after VG process. The former was based on the classical solid phase and liquid–liquid extraction procedures which, aided by automation and miniaturization strategies, have strengthened the role of VGT-AS in several research fields including environmental, clinical, and others. We then examine some of the new vapor trapping strategies (atom-trapping, hydride trapping, cryotrapping) that entail improvements in selectivity through interference elimination, but also they allow reaching ultra-low detection limits for a large number of chemical species generated in conventional VG systems, including complete separation of several species of the same element. This review covers more than 100 bibliographic references from 2009 up to date, found in SCOPUS database and in individual searches in specific journals. We finally conclude by giving some outlook on future directions of this field

  18. Mass spectrometric study of rhamnolipid biosurfactants and their interactions with cell membrane phospholipids

    Directory of Open Access Journals (Sweden)

    Pashynska V. A.

    2009-12-01

    Full Text Available Aim. To examine the formation of supramolecular complexes of biogenous rhamnolipids with membrane phospholipids that is considered as a molecular mechanism of the biosurfactants antimicrobial action. Method. In the present work rhamnolipid biosurfactant samples produced by Pseudomonas sp. PS-17 strain have been investigated by electrospray ionization mass spectrometry for the first time. Results. As a result of the study, characteristic mass spectra of the rhamnolipid samples were obtained, that can be used as reference spectra for mass spectrometric identification of the compounds in any biological or industrial samples. At the next stage of the experiments the pair systems, containing the biosurfactants and a membrane phospholipid dipalmitoylphosphatidylcholine, have been tested. The cationized noncovalent complexes of the rhamnolipids with the phospholipid were observed in the spectra. Conclusions. The results obtained testify to the consideration that rhamnolipids (similar to other membranotropic agents can form stable supramolecular complexes with membrane phospholipids that are able to evoke the biosurfactants antimicrobial action. A great potential of electrospray ionization mass spectrometry for the biosurfactants identification and study has been demonstrated in the work.

  19. Mass spectrometric characterization of the sarcoplasmic reticulum from rabbit skeletal muscle by on-membrane digestion.

    Science.gov (United States)

    Staunton, Lisa; Ohlendieck, Kay

    2012-03-01

    The sarcoplasmic reticulum from skeletal muscle constitutes an elaborate membrane system that contains a considerable number of integral and very large proteins that exist in highly complex supramolecular clusters. Conventional proteomics using two-dimensional gel electrophoresis greatly underestimates the presence of these proteins. Here, we have applied one-dimensional gradient gels and on-membrane digestion to overcome this technical problem. Mass spectrometric analysis has determined the presence of 31 distinct protein species in the sarcoplasmic reticulum, including key Ca2+-handling proteins such as the ryanodine receptor, Ca2+-ATPase, calsequestrin and sarcalumenin. Immunoblotting confirmed the relative position of these Ca2+-regulatory elements in analytical gel replicas. Interestingly, aldolase and phosphofructokinase were found to be present in the purified sarcoplasmic reticulum, supporting the idea of a close physical coupling between the glycolytic pathway and the energy-dependent sarcoplasmic reticulum. Hence, on-membrane digestion is highly suitable as the method of choice for studying integral and high-molecular-mass proteins in proteomic studies.

  20. Sequence-specific capture of protein-DNA complexes for mass spectrometric protein identification.

    Directory of Open Access Journals (Sweden)

    Cheng-Hsien Wu

    Full Text Available The regulation of gene transcription is fundamental to the existence of complex multicellular organisms such as humans. Although it is widely recognized that much of gene regulation is controlled by gene-specific protein-DNA interactions, there presently exists little in the way of tools to identify proteins that interact with the genome at locations of interest. We have developed a novel strategy to address this problem, which we refer to as GENECAPP, for Global ExoNuclease-based Enrichment of Chromatin-Associated Proteins for Proteomics. In this approach, formaldehyde cross-linking is employed to covalently link DNA to its associated proteins; subsequent fragmentation of the DNA, followed by exonuclease digestion, produces a single-stranded region of the DNA that enables sequence-specific hybridization capture of the protein-DNA complex on a solid support. Mass spectrometric (MS analysis of the captured proteins is then used for their identification and/or quantification. We show here the development and optimization of GENECAPP for an in vitro model system, comprised of the murine insulin-like growth factor-binding protein 1 (IGFBP1 promoter region and FoxO1, a member of the forkhead rhabdomyosarcoma (FoxO subfamily of transcription factors, which binds specifically to the IGFBP1 promoter. This novel strategy provides a powerful tool for studies of protein-DNA and protein-protein interactions.

  1. Quantitation of dissolved gas content in emulsions and in blood using mass spectrometric detection

    Science.gov (United States)

    Grimley, Everett; Turner, Nicole; Newell, Clayton; Simpkins, Cuthbert; Rodriguez, Juan

    2011-01-01

    Quantitation of dissolved gases in blood or in other biological media is essential for understanding the dynamics of metabolic processes. Current detection techniques, while enabling rapid and convenient assessment of dissolved gases, provide only direct information on the partial pressure of gases dissolved in the aqueous fraction of the fluid. The more relevant quantity known as gas content, which refers to the total amount of the gas in all fractions of the sample, can be inferred from those partial pressures, but only indirectly through mathematical modeling. Here we describe a simple mass spectrometric technique for rapid and direct quantitation of gas content for a wide range of gases. The technique is based on a mass spectrometer detector that continuously monitors gases that are rapidly extracted from samples injected into a purge vessel. The accuracy and sample processing speed of the system is demonstrated with experiments that reproduce within minutes literature values for the solubility of various gases in water. The capability of the technique is further demonstrated through accurate determination of O2 content in a lipid emulsion and in whole blood, using as little as 20 μL of sample. The approach to gas content quantitation described here should greatly expand the range of animals and conditions that may be used in studies of metabolic gas exchange, and facilitate the development of artificial oxygen carriers and resuscitation fluids. PMID:21497566

  2. Analysis of Endocrine Disrupting Pesticides by Capillary GC with Mass Spectrometric Detection

    Directory of Open Access Journals (Sweden)

    Svetlana Hrouzková

    2012-09-01

    Full Text Available Endocrine disrupting chemicals, among them many pesticides, alter the normal functioning of the endocrine system of both wildlife and humans at very low concentration levels. Therefore, the importance of method development for their analysis in food and the environment is increasing. This also covers contributions in the field of ultra-trace analysis of multicomponent mixtures of organic pollutants in complex matrices. With this fact conventional capillary gas chromatography (CGC and fast CGC with mass spectrometric detection (MS has acquired a real importance in the analysis of endocrine disrupting pesticide (EDP residues. This paper provides an overview of GC methods, including sample preparation steps, for analysis of EDPs in a variety of matrices at ultra-trace concentration levels. Emphasis is put on separation method, mode of MS detection and ionization and obtained limits of detection and quantification. Analysis time is one of the most important aspects that should be considered in the choice of analytical methods for routine analysis. Therefore, the benefits of developed fast GC methods are important.

  3. Atomic absorption spectrometric determination of mineral elements in mammalian bones

    International Nuclear Information System (INIS)

    Udoh, Anthony P.

    2000-01-01

    The phosphorus content of the major bones of male and female selected mammals was determined using the yellow vanadomolybdate colorimetric method. For each animal, the bone with the highest phosphorus content was used as pilot sample. Varying concentrations of strontium were added to solutions of the ashed pilot samples to minimize phosphorus interference in the determination of calcium and magnesium using flame atomic absorption spectrophotometry operated on the air-acetylene mode. At least 6,000 ppm (0.6%) of strontium was required to give optimum results for calcium. The amount of magnesium obtained from the analysis was not affected by the addition of strontium. With the incorporation of strontium in the sample solution, all elements of interest can be determined in the same sample solution. Based on this, a procedure is proposed for the determination of calcium and other elements in bones. Average recoveries of spiked calcium and magnesium were 97.85% and 98.16%, respectively at the 95% confidence level. The coefficients of variation obtained for replicate determinations using one of the samples were 0.00% for calcium, lead and sodium, 2.93% for magnesium, 3.27% for iron and 3.92% for zinc at the concentration levels found in that sample. Results from the proposed procedure compared well with those from classical chemical methods at the 95% confidence level. It is evident that calcium phosphorus, magnesium and sodium which are the most abundant elements in the bones are distributed in varying amounts both in the different types of bones and different animal species, although the general trend is Ca > P > Na > Mg for each bone considered. The calcium - phosphorus ratio is generally 3:1. The work set out to propose an atomic absorption spectrometric method for the multi-element analysis of mammalian bones with a single sample preparation and to study the distribution pattern of these elements in the bones. (Author)

  4. Spectrometric assessment of thyroid depth within the radioiodine test

    International Nuclear Information System (INIS)

    Rink, T.; Bormuth, F.-J.; Schroth, H.-J.; Braun, S.; Zimny, M.

    2005-01-01

    Aim of this study is the validation of a simple method for evaluating the depth of the target volume within the radioiodine test by analyzing the emitted iodine-131 energy spectrum. Patients, methods: In a total of 250 patients (102 with a solitary autonomous nodule, 66 with multifocal autonomy, 29 with disseminated autonomy, 46 with Graves' disease, 6 for reducing goiter volume and 1 with only partly resectable papillary tyhroid carcinoma), simultaneous uptake measurements in the Compton scatter (210±110 keV) and photopeak (364-45/+55 keV) windows were performed over one minute 24 hours after application of the 3 MBq test dose, with subsequent calculation of the respective count ratios. Measurements with a water-filled plastic neck phantom were carried out to perceive the relationship between these quotients and the average source depth and to get a calibration curve for calculating the depth of the target volume in the 250 patients for comparison with the sonographic reference data. Another calibration curve was obtained by evaluating the results of 125 randomly selected patient measurements to calculate the source depth in the other half of the group. Results: The phantom measurements revealed a highly significant correlation (r=0,99) between the count ratios and the source depth. Using these calibration data, a good relationship (r=0,81, average deviation 6 mm corresponding to 22%) between the spectrometric and the sonographic depths was obtained. When using the calibration curve resulting from the 125 patient measurements, the average deviation in the other half of the group was only 3 mm (12%). There was no difference between the disease groups. Conclusion: The described method allows an easy to use depth correction of the uptake measurements providing good results. (orig.)

  5. Mass spectrometric characterization of methylaluminoxane-activated metallocene complexes.

    Science.gov (United States)

    Trefz, Tyler K; Henderson, Matthew A; Linnolahti, Mikko; Collins, Scott; McIndoe, J Scott

    2015-02-09

    Electrospray-ionization mass spectrometric studies of poly(methylaluminoxane) (MAO) in the presence of [Cp2 ZrMe2 ], [Cp2 ZrMe(Cl)], and [Cp2 ZrCl2 ] in fluorobenzene (PhF) solution are reported. The results demonstrate that alkylation and ionization are separate events that occur at competitive rates in a polar solvent. Furthermore, there are significant differences in ion-pair speciation that result from the use of metallocene dichloride complexes in comparison to alkylated precursors at otherwise identical Al/Zr ratios. Finally, the counter anions that form are dependent on the choice of precursor and Al/Zr ratio; halogenated aluminoxane anions [(MeAlO)x (Me3 Al)y-z (Me2 AlCl)z Me](-) (z=1, 2, 3…︁) are observed using metal chloride complexes and under some conditions may predominate over their non-halogenated precursors [(MeAlO)x (Me3 Al)y Me](-) . Specifically, this halogenation process appears selective for the anions that form in comparison to the neutral components of MAO. Only at very high Al/Zr ratios is the same "native" anion distribution observed when using [Cp2 ZrCl2 ] when compared with [Cp2 ZrMe2 ]. Together, the results suggest that the need for a large excess of MAO when using metallocene dichloride complexes is a reflection of competitive alkylation vs. ionization, the persistence of unreactive, homodinuclear ion pairs in the case of [Cp2 ZrCl2 ], as well as a change in ion pairing resulting from modification of the anions formed at lower Al/Zr ratios. Models for neutral precursors and anions are examined computationally. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. The difference between the potentiometric surfaces of the Upper Patapsco aquifer in southern Maryland, September 1990 and September 2009

    Science.gov (United States)

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

    2010-01-01

    This report presents a map showing the change in the potentiometric surface of the upper Patapsco aquifer in the Patapsco Formation of Early Cretaceous age in Southern Maryland between September 1990 and September 2009. The map, based on water level differences obtained from 33 wells, shows that during the 19-year period, the change in the potentiometric surface ranged from zero at the edge of the outcrop area in northern Anne Arundel County to a decline of 20 feet at Broad Creek, 16 feet near Arnold, 32 feet at Waldorf, 37 feet at the Chalk Point power plant, and 43 feet at Lexington Park. The map also shows well yield in gallons per day for 2008 at wells or well fields.

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

    Science.gov (United States)

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

    2010-01-01

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

  8. The difference between the potentiometric surfaces of the lower Patapsco aquifer in southern Maryland, September 1990 and September 2007

    Science.gov (United States)

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

    2009-01-01

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

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-08-15

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

  11. Influence of morphology and topography on potentiometric response of magnesium and calcium sensitive PEDOT films doped with adenosine triphosphate (ATP)

    International Nuclear Information System (INIS)

    Paczosa-Bator, B.; Peltonen, J.; Bobacka, J.; Lewenstam, A.

    2006-01-01

    Poly(3,4-ethylenedioxythiophene) (PEDOT) films doped with adenosine triphosphate (ATP) are used to study the biologically relevant competitive magnesium and calcium ion-exchange at ATP membrane sites. It is shown, by atomic force microscopy (AFM) and scanning electron microscopy (SEM), that the surface topography and morphology of the PEDOT-ATP films determines the quality of their potentiometric response. More smooth and less rough films result in better potentiometric characteristics, particularly in a faster response. The topography/morphology of the PEDOT-ATP films is influenced by conditions during electrodeposition (electrochemical method of deposition, pH, concentration of electrolytes) and post-deposition soaking (including net-time of soaking), as evidenced by X-ray photoelectron spectroscopy (XPS) and energy dispersive analysis of X-rays (EDAX)

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

    Directory of Open Access Journals (Sweden)

    MARIAN ISVORANU

    2006-12-01

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

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

    OpenAIRE

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

    2014-01-01

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

  14. A cell-based potentiometric biosensor using the fungus Lentinus sajor-caju for permethrin determination in treated wood.

    Science.gov (United States)

    Arip, Mohamad Nasir Mat; Heng, Lee Yook; Ahmad, Musa; Ujang, Salmiah

    2013-11-15

    The characteristics of a potentiometric biosensor for the determination of permethrin in treated wood based on immobilised cells of the fungus Lentinus sajor-caju on a potentiometric transducer are reported this paper. The potentiometric biosensor was prepared by immobilisation of the fungus in alginate gel deposited on a pH-sensitive transducer employing a photocurable acrylic matrix. The biosensor gave a good response in detecting permethrin over the range of 1.0-100.0 µM. The slope of the calibration curve was 56.10 mV/decade with detection limit of 1.00 µM. The relative standard deviation for the sensor reproducibility was 4.86%. The response time of the sensor was 5 min at optimum pH 8.0 with 1.00 mg/electrode of fungus L. sajor-caju. The permethrin biosensor performance was compared with the conventional method for permethrin analysis using high performance liquid chromatography (HPLC), and the analytical results agreed well with the HPLC method (at 95% confidence limit). There was no interference from commonly used organophosphorus pesticides such as diazinon, parathion, paraoxon, and methyl parathion. © 2013 Elsevier B.V. All rights reserved.

  15. Spectrometric methods for the determination of chlorine in crude oil and petroleum derivatives — A review

    International Nuclear Information System (INIS)

    Doyle, Adriana; Saavedra, Alvaro; Tristão, Maria Luiza B.; Mendes, Luiz A.N.; Aucélio, Ricardo Q.

    2013-01-01

    Chlorine determination in crude oil is made in order to guarantee that the oil does not contain levels of this element that might cause damages in the oil processing equipment. In petroleum products, the determination of chlorine is made, for instance, to evaluate if there are proper concentrations of organochloride compounds, which are used as additives. Such determinations are currently performed following official guidelines from the ASTM International and from the United States Environmental Protection Agency as well as protocols indicated by the Universal Oil Products. X-ray fluorescence spectroscopy plays an important role in many of these official methods. In contrast, other spectrometric methods based on optical and mass detection are plagued by limitations related to both the fundamental characteristics of non-metals and to the complex sample matrices, which reflects in the small number of articles devoted to these applications. In this review, the current status of the spectrometric methods, especially the role played by X-ray fluorescence spectrometry, is evaluated in terms of the determination of chlorine in crude oil and petroleum derivatives. Comparison of the performance of the methods, limitations and potential new approaches to ensure proper spectrometric determinations of chlorine is indicated. - Highlights: • Critical evaluation of spectrometric methods for chlorine in petroleum products. • Reviews on element determination in petroleum have not address the case of chlorine. • Peculiarities of the spectrometric determination of Cl in petroleum are discussed. • The spectrometric approaches are detailed and compared to the official methods. • New trends in chlorine determination in petroleum products are indicated

  16. Spectrometric methods for the determination of chlorine in crude oil and petroleum derivatives — A review

    Energy Technology Data Exchange (ETDEWEB)

    Doyle, Adriana [Department of Chemistry, Pontifical Catholic University of Rio de Janeiro, Rua Marquês de São Vicente 225, Gávea, Rio de Janeiro, RJ 22451-900 (Brazil); Saavedra, Alvaro; Tristão, Maria Luiza B.; Mendes, Luiz A.N. [Leopoldo Américo Miguez de Mello Research Center — Petrobras (CENPES), Cidade Universitária, Quadra 7, Ilha do Fundão, Rio de Janeiro 21949-900 (Brazil); Aucélio, Ricardo Q., E-mail: aucelior@puc-rio.br [Department of Chemistry, Pontifical Catholic University of Rio de Janeiro, Rua Marquês de São Vicente 225, Gávea, Rio de Janeiro, RJ 22451-900 (Brazil)

    2013-08-01

    Chlorine determination in crude oil is made in order to guarantee that the oil does not contain levels of this element that might cause damages in the oil processing equipment. In petroleum products, the determination of chlorine is made, for instance, to evaluate if there are proper concentrations of organochloride compounds, which are used as additives. Such determinations are currently performed following official guidelines from the ASTM International and from the United States Environmental Protection Agency as well as protocols indicated by the Universal Oil Products. X-ray fluorescence spectroscopy plays an important role in many of these official methods. In contrast, other spectrometric methods based on optical and mass detection are plagued by limitations related to both the fundamental characteristics of non-metals and to the complex sample matrices, which reflects in the small number of articles devoted to these applications. In this review, the current status of the spectrometric methods, especially the role played by X-ray fluorescence spectrometry, is evaluated in terms of the determination of chlorine in crude oil and petroleum derivatives. Comparison of the performance of the methods, limitations and potential new approaches to ensure proper spectrometric determinations of chlorine is indicated. - Highlights: • Critical evaluation of spectrometric methods for chlorine in petroleum products. • Reviews on element determination in petroleum have not address the case of chlorine. • Peculiarities of the spectrometric determination of Cl in petroleum are discussed. • The spectrometric approaches are detailed and compared to the official methods. • New trends in chlorine determination in petroleum products are indicated.

  17. Secondary Ion Mass Spectrometric Image Depth Profiling for Three-Dimensional Elemental Analysis.

    Science.gov (United States)

    1981-10-01

    69-74. 18. Hofker, W.K.; et al. Rad. Eff. 1973, 17, 83-90. 19. Lindhard , J .; Scharff, M.; Schiott, H.E. Mat. Fys. Medd. Dan . Vid. Selsk. 1963, 33, 1...7A-A1OS 092 CORNELL UNIV ITHACA NY DEPT OF CHEMISTRY F/9 7/4 SCONARY ION MASS SPECTROMETRIC MAGE DEPTH PROFILING FOR THKf-ETC LW OCT SI A . J PATKIN...SECONDARY ION MASS SPECTROMETRIC IMAGE DEPTH PROFILING FOR THREE-DIMENSIONAL ELEMENTAL ANALYSIS by Adam J . Patkin and George H. Morrison Prepared for

  18. Enrichment and separation of mono- and multiply phosphorylated peptides using sequential elution from IMAC prior to mass spectrometric analysis

    DEFF Research Database (Denmark)

    Thingholm, Tine E; Jensen, Ole N; Larsen, Martin R

    2009-01-01

    Phospho-proteomics relies on methods for efficient purification and sequencing of phosphopeptides from highly complex biological systems using low amounts of starting material. Current methods for phosphopeptide enrichment, e.g., immobilized metal affinity chromatography and titanium dioxide...... multiply phosphorylated peptides using sequential elution from immobilized metal affinity chromatography is described. The two separate phosphopeptide fractions are subsequently analyzed by mass spectrometric methods optimized for mono-phosphorylated and multiply phosphorylated peptides, respectively...... chromatography, provide varying degrees of selectivity and specificity for phosphopeptide enrichment. Furthermore, the number of multiply phosphorylated peptides that are identified in most published studies is rather low. Here the protocol for a new strategy that separates mono-phosphorylated pep-tides from...

  19. New Potentiometric Wireless Chloride Sensors Provide High Resolution Information on Chemical Transport Processes in Streams

    Directory of Open Access Journals (Sweden)

    Keith Smettem

    2017-07-01

    Full Text Available Quantifying the travel times, pathways, and dispersion of solutes moving through stream environments is critical for understanding the biogeochemical cycling processes that control ecosystem functioning. Validation of stream solute transport and exchange process models requires data obtained from in-stream measurement of chemical concentration changes through time. This can be expensive and time consuming, leading to a need for cheap distributed sensor arrays that respond instantly and record chemical transport at points of interest on timescales of seconds. To meet this need we apply new, low-cost (in the order of a euro per sensor potentiometric chloride sensors used in a distributed array to obtain data with high spatial and temporal resolution. The application here is to monitoring in-stream hydrodynamic transport and dispersive mixing of an injected chemical, in this case NaCl. We present data obtained from the distributed sensor array under baseflow conditions for stream reaches in Luxembourg and Western Australia. The reaches were selected to provide a range of increasingly complex in-channel flow patterns. Mid-channel sensor results are comparable to data obtained from more expensive electrical conductivity meters, but simultaneous acquisition of tracer data at several positions across the channel allows far greater spatial resolution of hydrodynamic mixing processes and identification of chemical ‘dead zones’ in the study reaches.

  20. Fe (III - Galactomannan Solid and Aqueous Complexes: Potentiometric, EPR Spectroscopy and Thermal Data

    Directory of Open Access Journals (Sweden)

    Mercê Ana L. R.

    2001-01-01

    Full Text Available Galactomannans can be employed in food industries to modify the final rheological properties of the products. Since they are not absorbed by the living organisms they can also be used in dietary foods. The equilibria involving the interactions of Fe(III and galactomannans and arabinogalactan of several leguminous plants were characterized by potentiometric titrations and EPR spectroscopy. The log of the equilibrium constants for the formation of ML species, where M is the metal ion and L is the monomeric unit of the biopolymers, were 15.4, 14.1 and 18.5, for the galactomannans of C. fastuosa, L. leucocephala and S. macranthera, respectively. Log K values for protonated species (MHL were 3.1, 3.3, and were not detected for the galactomannan of S. macranthera. The log K values for the formation of ML2 were 14.1, 13.3 and 15.2, respectively. Early formation of insoluble products in the equilibrium with arabinogalactan and Fe(III prevented acquisition of reliable data. The solid complexes assays showed a great dipolar interaction between two Fe(III ions in the inner structure of the biopolymer which increased as the degree of substitution of the galactomannan decreased, and also showed the resulting thermal stability. The complexes impart a new possibility of providing essential metal ions in dietary foods since decomplexation of the complexes can occur at different pH values existing in the human body.

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

    Directory of Open Access Journals (Sweden)

    Eugenia Fagadar-Cosma

    2010-09-01

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

  2. Determination of the activity coefficient of neodymium in liquid aluminium by potentiometric methods

    Energy Technology Data Exchange (ETDEWEB)

    De Cordoba, G. [HLW/DFN/DE, CIEMAT, Avda. Complutense 22, Madrid 28040 (Spain)], E-mail: g.cordoba@ciemat.es; Laplace, A.; Conocar, O.; Lacquement, J. [DEN/DRCP/SCPS/LPP, CEA, Site de Marcoule. Bat. 399, BP 17171, 30207 Bagnols sur Ceze (France); Caravaca, C. [HLW/DFN/DE, CIEMAT, Avda. Complutense 22, Madrid 28040 (Spain)

    2008-12-30

    The activity coefficient of neodymium in liquid aluminium phase has been determined potentiometrically in the temperature range of 973-1073 K. To the author's knowledge, no data on this parameter has been published yet. Three different electrochemical methods have been tested: the cyclic voltammetry technique, the coulometric additions method and the direct use of an Al-Nd alloy. In addition, an experimental set-up has been designed which allows working with small amounts of solvent (30 g). The molten eutectic mixture CaCl{sub 2}-NaCl (52-48 mol%) has been selected as the electrolyte. From the results obtained, the variation of the activity coefficient of Nd in Al(l) as a function of the temperature can be expressed as follows: log {gamma}{sub Nd(Al)} = 9.81 - 17134/T(K), in the range 973-1073 K. It has been found a good agreement between the activity coefficient values obtained from the different methods tested. Hence, it can be stated that either of the techniques used allows determining reliable values for the activity coefficient.

  3. Fabrication of newspaper-based potentiometric platforms for flexible and disposable ion sensors.

    Science.gov (United States)

    Yoon, Jo Hee; Kim, Kyung Hoon; Bae, Nam Ho; Sim, Gap Seop; Oh, Yong-Jun; Lee, Seok Jae; Lee, Tae Jae; Lee, Kyoung G; Choi, Bong Gill

    2017-12-15

    Paper-based materials have attracted a great deal of attention in sensor applications because they are readily available, biodegradable, inexpensive, and mechanically flexible. Although paper-based sensors have been developed, but important obstacles remian, which include the retention of chemical and mechanical stabilities when paper is wetted. Herein, we develop a simple and scalable process for fabrication of newspaper-based platforms by coating of parylene C and patterning of metal layers. As-prepared parylene C-coated newspaper (PC-paper) provides low-cost, disposable, and mechanically and chemically stable electrochemical platforms for the development of potentiometric ion sensors for the detection of electrolyte cations, such as, H + and K + . The pH and K + sensors produced show near ideal Nernstian sensitivity, good repeatability, good ion selectivity, and low potential drift. These disposable, flexible ion sensors based on PC-paper platforms could provide new opportunities for the development of point-of-care testing sensors, for diagnostics, healthcare, and environment testing. Copyright © 2017 Elsevier Inc. All rights reserved.

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

    Directory of Open Access Journals (Sweden)

    Džudović Radmila M.

    2010-01-01

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

  5. Indicator electrodes from d-elements for application in different types of potentiometric analytical methods

    Directory of Open Access Journals (Sweden)

    Z. Kunasheva

    2012-05-01

    Full Text Available The article covers the use of metal electrodes from titanium, tungsten, molybdenum as indicator electrodes at potentiometric method of analysis. The condition of measuring operation in dependence on pH, ionic strength of solutions is described in the article. Electrode potential of testing electrodes are measured in the interval of concentration of salts from 0,1∙10-1 mole/l till 0,1∙10-6 mole/l. The results of testing of electrical-analytical description of metal electrodes made of d-elements, in particular, titanium, tungsten, molybdenum in solutions of cations of some metals and anions were mentioned. As ions of metal cations Cu2+, Cd2+, Zn2+, Pb2+ and anions Cl-, I-, F- were chosen.It is identified that titanic electrode has different response to ions of copper (II, zinc and cadmium. However, dependence of electrode potential on concentration of ions of metal is rectilinear, that is vequired of indicator electrodes in the direct potential metrics.  

  6. A Potentiometric Formaldehyde Biosensor Based on Immobilization of Alcohol Oxidase on Acryloxysuccinimide-modified Acrylic Microspheres

    Directory of Open Access Journals (Sweden)

    Lee Yook Heng

    2010-11-01

    Full Text Available A new alcohol oxidase (AOX enzyme-based formaldehyde biosensor based on acrylic microspheres has been developed. Hydrophobic poly(n-butyl acrylate-N-acryloxy-succinimide [poly(nBA-NAS] microspheres, an enzyme immobilization matrix, was synthesized using photopolymerization in an emulsion form. AOX-poly(nBA-NAS microspheres were deposited on a pH transducer made from a layer of photocured and self-plasticized polyacrylate membrane with an entrapped pH ionophore coated on a Ag/AgCl screen printed electrode (SPE. Oxidation of formaldehyde by the immobilized AOX resulted in the production of protons, which can be determined via the pH transducer. Effects of buffer concentrations, pH and different amount of immobilization matrix towards the biosensor’s analytical performance were investigated. The formaldehyde biosensor exhibited a dynamic linear response range to formaldehyde from 0.3–316.2 mM and a sensitivity of 59.41 ± 0.66 mV/decade (R2 = 0.9776, n = 3. The lower detection limit of the biosensor was 0.3 mM, while reproducibility and repeatability were 3.16% RSD (relative standard deviation and 1.11% RSD, respectively (n = 3. The use of acrylic microspheres in the potentiometric formaldehyde biosensor improved the biosensor’s performance in terms of response time, linear response range and long term stability when compared with thick film immobilization methods.

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

    Science.gov (United States)

    Qiang, Zhimin; Adams, Craig

    2004-07-01

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

  8. Graphene oxide modified light addressable potentiometric sensor and its application for ssDNA monitoring.

    Science.gov (United States)

    Jia, Yunfang; Yin, Xue-Bo; Zhang, Jia; Zhou, Shuang; Song, Meng; Xing, Ke-Li

    2012-12-21

    A light addressable potentiometric sensor (LAPS) is a kind of silicon based semiconductor sensor, and surface modification is a fundamental problem for its application in biological fields. Graphene oxide (GO) based biochemically activated LAPS were proposed, called GO-LAPS. The GO-LAPS were applied to monitoring single strand DNA (ssDNA) probe immobilization and its hybridization with complementary ssDNA molecules of different chain lengths (30, 21 and 14 base pairs, respectively). It was discovered that the curves of LAPS' currents versus analyte concentrations for ssDNA probe binding and the target ssDNA hybridization were different. Explanations were proposed based on the semiconductor's surface-electric-field-effect and the electrical properties of ssDNA molecule. Moreover, comparisons between GO-LAPS and LAPS without GO modification were carried out. Enhanced response currents of GO-LAPS were reported experimentally and analyzed theoretically based on X-ray photoelectron spectroscopy (XPS) of GO-LAPS. The limitation of target ssDNA monitoring was 1 pM to 10 nM, which suggested that this LAPS based platform could be developed as a sensitive means for short chain ssDNA detection.

  9. Novel PVC-membrane electrode for flow injection potentiometric determination of Biperiden in pharmaceutical preparations.

    Science.gov (United States)

    Khaled, Elmorsy; El-Sabbagh, Inas A; El-Kholy, N G; Ghahni, E Y Abdel

    2011-12-15

    The construction and performance characteristics of Biperiden (BP) polyvinyl chloride (PVC) electrodes are described. Different methods for electrode fabrication are tested including; incorporation of BP-ion pairs (BP-IPs), incorporation of ion pairing agents, or soaking the plain electrode in BP-ion pairs suspension solution. Electrode matrices were optimized referring to the effect of modifier content and nature, plasticizer and the method of modification. The proposed electrodes work satisfactorily in the BP concentration range from 10(-5) to 10(-2)mol L(-1), with fast response time (7s) and adequate operational lifetime (28 days). The electrode potential is pH independent within the range 2.0-7.0, with good selectivity towards BP in presence of various interfering species. The developed electrodes have been applied for potentiometric determination of BP in pharmaceutical formulation under batch and flow injection analysis (FIA) conditions. FIA offers the advantages of accuracy and automation feasibility with high sampling frequency. The dissolution profile for Akineton tablets (2mg BP/tablet) was studied using the proposed electrode in comparison with the official methods. Copyright © 2011 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2010-01-01

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

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

    Science.gov (United States)

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

    2015-08-12

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

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

    Science.gov (United States)

    Black, Stuart; Ferrell, Jack R

    2017-02-07

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

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

    Science.gov (United States)

    Skic, Kamil; Boguta, Patrycja; Sokołowska, Zofia

    2016-07-01

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

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

    Science.gov (United States)

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

    2013-05-01

    Tartrazine dye Na(3)TZ in foodstuff products was determined by a new modified carbon paste electrode, encoded sensor A, and a coated silver wire electrode, encoded sensor B, based on tartrazine TZ- cetryltrimethyl ammoniumbromide CTAB as a chemical modifier TZ-CTA. The electrodes exhibit the following characteristics listed respectively: a Nernstian slope of 17.9±0.5 and 19.4±0.2 mV/decade for tartrazine ion over a wide concentration range from 4.3×10(-7) to 1.0×10(-2) and 1.1×10(-7) to 1.0×10(-2) M. The lower detection limits: 3.2×10(-7) and 5.5×10(-8) M. Short response time (5-8 s) over the pH range 3.8-7.7 and 4.2-8.1. The proposed sensors display significantly high selectivity for TZ ion over a wide variety of sugars, some anions, common organic, inorganic compounds and additives. The developed electrodes were applied to the potentiometric determination of tartrazine ion in different kinds of foodstuffs: solid jelly (strawberry and custard) powder samples and soft drink (orange) samples with satisfactory results. Copyright © 2012 Elsevier Ltd. All rights reserved.

  15. Novel LTCC-potentiometric microfluidic device for biparametric analysis of organic compounds carrying plastic antibodies as ionophores: application to sulfamethoxazole and trimethoprim.

    Science.gov (United States)

    Almeida, S A A; Arasa, E; Puyol, M; Martinez-Cisneros, C S; Alonso-Chamarro, J; Montenegro, M C B S M; Sales, M G F

    2011-12-15

    Monitoring organic environmental contaminants is of crucial importance to ensure public health. This requires simple, portable and robust devices to carry out on-site analysis. For this purpose, a low-temperature co-fired ceramics (LTCC) microfluidic potentiometric device (LTCC/μPOT) was developed for the first time for an organic compound: sulfamethoxazole (SMX). Sensory materials relied on newly designed plastic antibodies. Sol-gel, self-assembling monolayer and molecular-imprinting techniques were merged for this purpose. Silica beads were amine-modified and linked to SMX via glutaraldehyde modification. Condensation polymerization was conducted around SMX to fill the vacant spaces. SMX was removed after, leaving behind imprinted sites of complementary shape. The obtained particles were used as ionophores in plasticized PVC membranes. The most suitable membrane composition was selected in steady-state assays. Its suitability to flow analysis was verified in flow-injection studies with regular tubular electrodes. The LTCC/μPOT device integrated a bidimensional mixer, an embedded reference electrode based on Ag/AgCl and an Ag-based contact screen-printed under a micromachined cavity of 600 μm depth. The sensing membranes were deposited over this contact and acted as indicating electrodes. Under optimum conditions, the SMX sensor displayed slopes of about -58.7 mV/decade in a range from 12.7 to 250 μg/mL, providing a detection limit of 3.85 μg/mL and a sampling throughput of 36 samples/h with a reagent consumption of 3.3 mL per sample. The system was adjusted later to multiple analyte detection by including a second potentiometric cell on the LTCC/μPOT device. No additional reference electrode was required. This concept was applied to Trimethoprim (TMP), always administered concomitantly with sulphonamide drugs, and tested in fish-farming waters. The biparametric microanalyzer displayed Nernstian behaviour, with average slopes -54.7 (SMX) and +57.8 (TMP) m

  16. Ground gamma-ray spectrometric studies of El-Sahu area, southwestern Sinai, Egypt

    Science.gov (United States)

    Abdrabboh, Ahmad M.

    2017-12-01

    Based on the previous airborne gamma-ray spectrometric study carried out in southwestern Sinai area, El Sahu area was selected for detail ground gamma-ray spectrometric survey. This area is considered as a good target for radioactive mineral exploration. The study area is exposed in a Paleozoic basin covered by different rocks (ranging from Precambrian to Quaternary). The ground gamma-ray spectrometric survey has been conducted along the study area through random survey. The resultant gamma-ray spectrometric maps show different levels of radioactivity over the studied area, which reflect contrasting radioelement contents for the exposed various rock types. The studied area possesses total count ranging from 2.6 to 326 Ur, 0.1 to 2.8% K, 1.7 to 316 ppm eU and 0.9 to 47.5 ppm eTh. The highest uranium concentrations are located in the northern and southern parts of El Sahu area. They are mainly associated with Um Bogma Formation occurrences. Uranium ratio maps (eU/K and eU/eTh) as well as ternary maps show sharp increase of eU content over both potassium and thorium contents associated with the ENE and NNW trends in Um Bogma Formation, indicating an increase in the U-potentiality than the surrounding rocks. This indicates that the mineralization in the study area may be structurally-controlled.

  17. Structure elucidation of metabolite x17299 by interpretation of mass spectrometric data.

    Science.gov (United States)

    Zhang, Qibo; Ford, Lisa A; Evans, Anne M; Toal, Douglas R

    2017-01-01

    A major bottleneck in metabolomic studies is metabolite identification from accurate mass spectrometric data. Metabolite x17299 was identified in plasma as an unknown in a metabolomic study using a compound-centric approach where the associated ion features of the compound were used to determine the true molecular mass. The aim of this work is to elucidate the chemical structure of x17299, a new compound by de novo interpretation of mass spectrometric data. An Orbitrap Elite mass spectrometer was used for acquisition of mass spectra up to MS 4 at high resolution. Synthetic standards of N,N,N -trimethyl-l-alanyl-l-proline betaine (l,l-TMAP), a diastereomer, and an enantiomer were chemically prepared. The planar structure of x17299 was successfully proposed by de novo mechanistic interpretation of mass spectrometric data without any laborious purification and nuclear magnetic resonance spectroscopic analysis. The proposed structure was verified by deuterium exchanged mass spectrometric analysis and confirmed by comparison to a synthetic standard. Relative configuration of x17299 was determined by direct chromatographic comparison to a pair of synthetic diastereomers. Absolute configuration was assigned after derivatization of x17299 with a chiral auxiliary group followed by its chromatographic comparison to a pair of synthetic standards. The chemical structure of metabolite x17299 was determined to be l,l-TMAP.

  18. Malevolent use of radioactive materials: An international exercise in the analysis of gamma-spectrometric data

    DEFF Research Database (Denmark)

    Dowdall, M.; Andersson, Kasper Grann; Palsson, S.E.

    2010-01-01

    with isotopes and activities that present significant challenges with respect to identification and quantification using gamma ray spectrometry. The MALRAD international exercise was designed to provide a practice opportunity for authorities and laboratories to work with synthetic gamma-spectrometric data...

  19. Mass spectrometric identification of isocyanate-induced modifications of keratins in human skin

    NARCIS (Netherlands)

    Hulst, A.G.; Verstappen, D.R.W.; Riet-van Oeveren, D. van der; Vermeulen, N.P.E.; Noort, D.

    2015-01-01

    In the current paper we show that exposure of human callus to isocyanates leads to covalent modifications within keratin proteins. Mass spectrometric analyses of pronase digests of keratin isolated from exposed callus show that both mono- and di-adducts (for di-isocyanates) are predominantly formed

  20. Quantitative MALDI tandem mass spectrometric imaging of cocaine from brain tissue with a deuterated internal standard.

    NARCIS (Netherlands)

    Pirman, D.A.; Reich, R.F.; Kiss, A.; Heeren, R.M.A.; Yost, R.A.

    2013-01-01

    Mass spectrometric imaging (MSI) is an analytical technique used to determine the distribution of individual analytes within a given sample. A wide array of analytes and samples can be investigated by MSI, including drug distribution in rats, lipid analysis from brain tissue, protein differentiation

  1. Verification of exposure to organophosphates: Generic mass spectrometric method for detection of human butyrylcholinesterase adducts

    NARCIS (Netherlands)

    Noort, D.; Fidder, A.; Schans, M.J. van der; Hulst, A.G.

    2006-01-01

    We present a generic mass spectrometric method to verify exposure to organophosphates, based on the chemical conversion of the phosphylated peptides obtained after pepsin digestion of human butyrylcholinesterase (HuBuChE) to a common precursor peptide. After exposure of plasma to various

  2. Retrospective detection of exposure to organophosphorus anti-cholinesterases: Mass spectrometric analysis of phosphylated human butyrylcholinesterase

    NARCIS (Netherlands)

    Fidder, A.; Hulst, A.G.; Noort, D.; Ruiter, R. de; Schans, M.J. van der; Benschop, H.P.; Langenberg, J.P.

    2002-01-01

    In this paper a novel and general procedure is presented for detection of organophosphate-inhibited human butyrylcholinesterase (HuBuChE), which is based on electrospray tandem mass spectrometric analysis of phosphylated nonapeptides obtained after pepsin digestion of the enzyme. The utility of this

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

    Science.gov (United States)

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

    2016-01-01

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

  4. Polarographic and potentiometric studies on some binary and ternary complex systems of dioxouranium(VI)

    International Nuclear Information System (INIS)

    Janarthanam, M.; Sivasankar, B.; Rengaraj, K.; Nair, M.S.

    1995-01-01

    The relative coordinating abilities of donor sites in the potentially tridentate ligands viz., asparagine, glutamine, aspartic acid and glutamic acid towards uranyl ion have been investigated by polarographic and pH-metric techniques. The metal ion forms 1:2 complexes under polarographic conditions. However, only 1:1 complex is observed under pH-metric conditions, where 1:2 complexes do not proceed due to extensive hydrolysis of the metal ion. The relative variations of ΔE 1/2 with pH and ligand concentration supported by conductometric titration data indicate that the primary amino groups in the amino acids are not involved in coordination with uranyl ion. Further, the amide groups in asparagine and glutamine also do not participate in coordination thus rendering these ligands unidentate. In aspartic and glutamic acid complexes, seven- and eight- membered chelate rings are formed involving two terminal carboxyl groups. The mixed ligand complex equilibria of uranyl ion involving aspartic acid/glutamic acid as primary ligands (A) and maleic acid, malonic acid, succinic acid and lactic acid as secondary ligands (B) have also been studied by computer based numerical evaluation of pH titration data. The concentration profiles have indicated the favorability of the formation of ternary complexes in general as reflected in the Δlog K values. (author). 10 refs., 1 fig., 1 tab

  5. Comparison Between Potentiometric and Stripping Voltammetric Detection of Trace Metals: Measurements of Cadmium and Lead in the Presence of Thalium, Indium, and Tin.

    Science.gov (United States)

    Chumbimuni-Torres, Karin Y; Calvo-Marzal, Percy; Wang, Joseph

    2009-08-12

    Recent advances in ion-selective electrodes have pushed the detection limits of direct potentiometry to the nanomolar concentration range. Here we present a direct comparison of the sensitivity and selectivity of potentiometric and stripping-voltammetric measurements of cadmium and lead. While both techniques offer a similar sensitivity, the potentiometric method offers higher selectivity in the presence of excess of metal ions (e.g., thallium, tin) that commonly interfere in the stripping-voltammetric operation. Because of the complementary nature of the potentiometric and stripping-voltammetric methods, it is recommended that these techniques will be selected based on the specific analytical problem or used in parallel to provide additional analytical information.

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

    Science.gov (United States)

    Papanastasiou, G; Ziogas, I

    1995-06-01

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

  7. Potentiometric Sensors Based on Surface Molecular Imprinting: Detection of Cancer Biomarkers and Viruses

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Y.; Zhang, Z; Jain, V; Yi, J; Mueller, S; Sokolov, J; Liu, Z; Levon, K; Rigas, B; Rafailovich, M

    2010-01-01

    The continuing discovery of cancer biomarkers necessitates improved methods for their detection. Molecular imprinting using artificial materials provides an alternative to the detection of a wide range of substances. We applied surface molecular imprinting using self-assembled monolayers to design sensing elements for the detection of cancer biomarkers and other proteins. These elements consist of a gold-coated silicon chip onto which hydroxyl-terminated alkanethiol molecules and template biomolecule are co-adsorbed, where the thiol molecules are chemically bound to the metal substrate and self-assembled into highly ordered monolayers, the biomolecules can be removed, creating the foot-print cavities in the monolayer matrix for this kind of template molecules. Re-adsorption of the biomolecules to the sensing chip changes its potential, which can be measured potentiometrically. We applied this method to the detection of carcinoembryonic antigen (CEA) in both solutions of purified CEA and in the culture medium of a CEA-producing human colon cancer cell line. The CEA assay, validated also against a standard immunoassay, was both sensitive (detection range 2.5-250 ng/mL) and specific (no cross-reactivity with hemoglobin; no response by a non-imprinted sensor). Similar results were obtained for human amylase. In addition, we detected virions of poliovirus in a specific manner (no cross-reactivity to adenovirus, no response by a non-imprinted sensor). Our findings demonstrate the application of the principles of molecular imprinting to the development of a new method for the detection of protein cancer biomarkers and to protein-based macromolecular structures such as the capsid of a virion. This approach has the potential of generating a general assay methodology that could be highly sensitive, specific, simple and likely inexpensive.

  8. Potentiometric sensing of iodide using polymeric membranes of microwave stabilized β-AgI

    International Nuclear Information System (INIS)

    James, Dhanya; Rao, T. Prasada

    2012-01-01

    Highlights: ► Stable β-phase was obtained by post MW irradiation of AgI precipitate. ► Constructed ISEby dispersing stable β-AgI crystals in polyvinyl chloride. ► Designed iodide ISE exhibited wide linear range and fast response. ► Highly selective with selectivity factors less than 10 −6 . ► Successfully applied to natural waters, table salt and human urine samples. - Abstract: A polymer based heterogeneous ion selective electrode (ISE) membrane was fabricated for the potentiometric sensing of iodide. The sensing element used for the preparation of the ISE membrane was microwave stabilized β-AgI. Because microwave energy was found to be beneficial for causing hysteresis at the phase transition temperature of AgI, an attempt has been made to prepare stable and conductive β-AgI crystals by post microwave irradiation under high pressure. A conventionally precipitated AgI based ISE was also fabricated for comparative studies. The β-AgI based ISE could respond to a wide range of iodide concentrations (1 × 10 −8 to 1 M) within 60 s with a detection limit of 10 nM. The ISE gave stable response to iodide ions in a pH range of 2.0–8.0 and was highly selective in the presence of various interfering ions. The performance of the proposed iodide ISE in the analysis of natural and seawater samples was encouraging, and the determination of iodide in table salt and human urine samples was explained using the developed sensor.

  9. Potentiometric determination of moxifloxacin in some pharmaceutical formulation using PVC membrane sensors.

    Science.gov (United States)

    Hefnawy, Mohammed M; Homoda, Atef M; Abounassif, Mohammed A; Alanazi, Amer M; Al-Majed, Abdulrahaman; Mostafa, Gamal A

    2014-01-01

    The construction and electrochemical response characteristics of Poly (vinyl chloride) membrane sensors for moxifloxacin HCl (MOX) are described. The sensing membranes incorporate ion association complexes of moxifloxacin cation and sodium tetraphenyl borate (NaTPB) (sensor 1), phosphomolybdic acid (PMA) (sensor 2) or phosphotungstic acid (PTA) (sensor 3) as electroactive materials. The sensors display a fast, stable and near-Nernstian response over a relative wide moxifloxacin concentration range (1 × 10(-2) - 4.0 × 10(-6), 1 × 10(-2) - 5.0 × 10(-6), 1 × 10(-2) - 5.0 × 10(-6) M), with detection limits of 3 × 10(-6), 4 × 10(-6) and 4.0 × 10(-6) M for sensor 1, 2 and 3, respectively over a pH range of 6.0 - 9.0. The sensors show good discrimination of moxifloxacin from several inorganic and organic compounds. The direct determination of 400 μg/ml of moxifloxacin show an average recovery of 98.5, 99.1 and 98.6% and a mean relative standard deviation of 1.8, 1.6 and 1.8% for sensors 1, 2 and 3 respectively. The proposed sensors have been applied for direct determination of moxifloxacin in some pharmaceutical preparations. The results obtained by determination of moxifloxacin in tablets using the proposed sensors are comparable favorably with those obtained using the US Pharmacopeia method. The sensors have been used as indicator electrodes for potentiometric titration of moxifloxacin.

  10. Silver ion recognition using potentiometric sensor based on recently synthesized isoquinoline-1,3-dione derivatives

    Directory of Open Access Journals (Sweden)

    AJAR KAMAL

    2012-08-01

    Full Text Available The four derivatives of isoquinoline-1,3-dione based on β-lactum (I-IV, have been explored as neutral ionophores for preparing poly(vinylchloride based polymeric membrane electrodes (PME selective to silver(I ions. The addition of sodium tetraphenylborate (NaTPB and dioctylsebacate (DOS as a plasticizer was found to improve the performance of ion selective electrodes. The best performance was obtained with PME-1 based on ionophore I having composition: ionophore (9.2 mg, PVC (100.1 mg, DOS (201.1 mg and NaTPB (1.5 mg in 5 mL tetrahydrofuran. The electrode response was linear with Nernstian slope of 58.44 mV/decade in the concentration range of 1.0 x 10-1 M to 5.0 x 10-6 M and detection limit of 5.83 x 10-6 M. It performs satisfactorily over wide pH range of 1.0-5.5. The proposed sensor can be used over a period of more than three months without any significant drift in potential and shows good selectivity to silver(I ion over a number of cations especially with no interference of mercury(II ions. Sharp end point was obtained when the sensor was used as an indicator electrode for the potentiometric titration of silver(I ions with chloride ions and therefore this electrode (PME-1 could be used for quantitative determination of silver(I ion in synthetic water, silver foil and dental amalgam samples.

  11. Novel biomimetic composite material for potentiometric screening of acetylcholine, a neurotransmitter in Alzheimer's disease.

    Science.gov (United States)

    Sacramento, Ana S; Moreira, Felismina T C; Guerreiro, Joana L; Tavares, Ana P; Sales, M Goreti F

    2017-10-01

    This work describes a novel approach to produce an antibody-like biomimetic material. It includes preparing composite imprinted material never presented before, with highly conductive support nanostructures and assembling a high conductivity polymeric layer at low temperature. Overall, such highly conductive material may enhance the final features of electrically-based devices. Acetylcholine (ACh) was selected as target analyte, a neurotransmitter of importance in Alzheimer's disease. Potentiometric transduction was preferred, allowing quick responses and future adaptation to point-of-care requirements. The biomimetic material was obtained by bulk polymerization, where ACh was placed in a composite matrix of multiwalled carbon nanotubes (MWCNTs) and aniline (ANI). Subsequent polymerization, initiated by radical species, yielded a polymeric structure of polyaniline (PANI) acting as physical support of the composite. A non-imprinted material (NIM) having only PANI/MWCNT (without ACh) has been prepared for comparison of the biomimetic-imprinted material (BIM). RAMAN and Fourier Transform Infrared spectroscopy (FTIR), Transmission Electron microscopy (TEM), and Scanning Electron microscope (SEM) analysis characterized the structures of the materials. The ability of this biomaterial to rebind ACh was confirmed by including it as electroactive compound in a PVC/plasticizer mixture. The membranes with imprinted material and anionic additive presented the best analytical characteristics, with a sensitivity of 83.86mV decade -1 and limit of detection (LOD) of 3.45×10 -5 mol/L in HEPES buffer pH4.0. Good selectivity was observed against creatinine, creatine, glucose, cysteine and urea. The electrodes were also applied on synthetic serum samples and seemed a reliable tool for screening ACh in synthetic serum samples. The overall performance showed fast response, reusability, simplicity and low price. Copyright © 2017 Elsevier B.V. All rights reserved.

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

    International Nuclear Information System (INIS)

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

    1985-01-01

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

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

    International Nuclear Information System (INIS)

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

    1978-01-01

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

  14. Acid base characterization of the surface of mixed species of algae Spirulin by potentiometric titration and discrete site distribution model

    OpenAIRE

    Lima, Elizabete C. de; Masini, Jorge C.

    1999-01-01

    Acid base properties of mixed species of the microalgae Spirulina were studied by potentiometric titration in medium of 0.01 and 0.10 mols L-1 NaNO3 at 25.0±0.10 C using modified Gran functions or nonlinear regression techniques for data fitting. The discrete site distribution model was used, permitting the characterization of five classes of ionizable sites in both ionic media. This fact suggests that the chemical heterogeneity of the ionizable sites on the cell surface plays a major role on...

  15. iMS2Flux – a high–throughput processing tool for stable isotope labeled mass spectrometric data used for metabolic flux analysis

    Directory of Open Access Journals (Sweden)

    Poskar C Hart

    2012-11-01

    Full Text Available Abstract Background Metabolic flux analysis has become an established method in systems biology and functional genomics. The most common approach for determining intracellular metabolic fluxes is to utilize mass spectrometry in combination with stable isotope labeling experiments. However, before the mass spectrometric data can be used it has to be corrected for biases caused by naturally occurring stable isotopes, by the analytical technique(s employed, or by the biological sample itself. Finally the MS data and the labeling information it contains have to be assembled into a data format usable by flux analysis software (of which several dedicated packages exist. Currently the processing of mass spectrometric data is time-consuming and error-prone requiring peak by peak cut-and-paste analysis and manual curation. In order to facilitate high-throughput metabolic flux analysis, the automation of multiple steps in the analytical workflow is necessary. Results Here we describe iMS2Flux, software developed to automate, standardize and connect the data flow between mass spectrometric measurements and flux analysis programs. This tool streamlines the transfer of data from extraction via correction tools to 13C-Flux software by processing MS data from stable isotope labeling experiments. It allows the correction of large and heterogeneous MS datasets for the presence of naturally occurring stable isotopes, initial biomass and several mass spectrometry effects. Before and after data correction, several checks can be performed to ensure accurate data. The corrected data may be returned in a variety of formats including those used by metabolic flux analysis software such as 13CFLUX, OpenFLUX and 13CFLUX2. Conclusion iMS2Flux is a versatile, easy to use tool for the automated processing of mass spectrometric data containing isotope labeling information. It represents the core framework for a standardized workflow and data processing. Due to its flexibility

  16. Standard test methods for chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade plutonium metal

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2004-01-01

    1.1 These test methods cover procedures for the chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade plutonium metal to determine compliance with specifications.

  17. Silver ion imprinted polymer nanobeads based on a aza-thioether crown containing a 1,10-phenanthroline subunit for solid phase extraction and for voltammetric and potentiometric silver sensors

    Energy Technology Data Exchange (ETDEWEB)

    Shamsipur, Mojtaba, E-mail: mshamsipur@yahoo.com [Department of Chemistry, Razi University, Kermanshah (Iran, Islamic Republic of); Hashemi, Beshare; Dehdashtian, Sara; Mohammadi, Moslem; Gholivand, Mohammad Bagher [Department of Chemistry, Razi University, Kermanshah (Iran, Islamic Republic of); Garau, Alessandra; Lippolis, Vito [Dipartimento di Scienze Chimiche e Geologiche, Universita' degli Studi di Cagliari, S.S. 554 Bivio per Sestu, 09042 Monserrato, CA (Italy)

    2014-12-10

    Highlights: • Preparation of Ag{sup +} imprinted polymeric nanobeads via precipitation polymerization. • Use of a mixed aza-thioether crown containing a 1,10-phenanthroline subunit a selective host for Ag{sup +} ion. • Highly selective, sensitive and fast recognition of traces of Ag{sup +} ions. • Use of the prepared Ag{sup +}-IIP for preparation of an Ag{sup +}-voltammetric sensor with LOD of 9.0 × 10{sup −10} M. • Use of the prepared Ag{sup +}-IIP for preparation of Ag{sup +}-ISEs with LOD of 1.2 × 10{sup −9} M 9.0 × 10{sup −10} M. - Abstract: A new nano-sized silver(I) ion-imprinted polymer (IIP) was prepared via precipitation copolymerization using ethyleneglycol dimethacrylate, as a cross-linking agent in the presence of Ag{sup +} and an aza-thioether crown containing a 1,10-phenanthroline subunit as a highly selective complexing agent. The imprint silver(I) ion was removed from the polymeric matrix using a 1.0 M HNO{sub 3} solution. The resulting powder material was characterized using IR spectroscopy and scanning electron microscopy. The SEM micrographs showed colloidal nanoparticles of about 52 nm and 75 nm in diameter and slightly irregular in shape for leached and unleached IIPs, respectively. The optimal pH for quantitative enrichment was 6.0 and maximum sorbent capacity of the prepared IIP for Ag{sup +} was 18.08 μmol g{sup −1}. The relative standard deviation and limit of detection (LOD = 3S{sub b}/m) for flame atomic absorption spectrometric determination of silver(I) ion, after its selective extraction by the prepared IIP nanobeads, were evaluated as 2.42% and 2.2 × 10{sup −8} M, respectively. The new Ag{sup +}-IIP was also applied as a suitable sensing element to the preparation of highly selective and sensitive voltammetric and potentiometric sensors for ultra trace detection of silver(I) ion in water samples, with limits of detection of 9.0 × 10{sup −10} and 1.2 × 10{sup −9} M, respectively.

  18. High-efficient method for spectrometric data real time processing with increased resolution of a measuring channel

    International Nuclear Information System (INIS)

    Ashkinaze, S.I.; Voronov, V.A.; Nechaev, Yu.I.

    1988-01-01

    Solution of reduction problem as a mean to increase spectrometric tract resolution when it is realized using the digit-by-digit modified method and special strategy, significantly reducing the time of processing, is considered. The results presented confirm that the complex measurement tract plus microcomputer is equivalent to the use of the tract with a higher resolution, and the use of the digit-by-digit modified method permits to process spectrometric information in real time scale

  19. Novel atomic absorption spectrometric and rapid spectrophotometric methods for the quantitation of paracetamol in saliva: application to pharmacokinetic studies.

    Science.gov (United States)

    Issa, M M; Nejem, R M; El-Abadla, N S; Al-Kholy, M; Saleh, Akila A

    2008-01-01

    A novel atomic absorption spectrometric method and two highly sensitive spectrophotometric methods were developed for the determination of paracetamol. These techniques based on the oxidation of paracetamol by iron (III) (method I); oxidation of p-aminophenol after the hydrolysis of paracetamol (method II). Iron (II) then reacts with potassium ferricyanide to form Prussian blue color with a maximum absorbance at 700 nm. The atomic absorption method was accomplished by extracting the excess iron (III) in method II and aspirates the aqueous layer into air-acetylene flame to measure the absorbance of iron (II) at 302.1 nm. The reactions have been spectrometrically evaluated to attain optimum experimental conditions. Linear responses were exhibited over the ranges 1.0-10, 0.2-2.0 and 0.1-1.0 mug/ml for method I, method II and atomic absorption spectrometric method, respectively. A high sensitivity is recorded for the proposed methods I and II and atomic absorption spectrometric method value indicate: 0.05, 0.022 and 0.012 mug/ml, respectively. The limit of quantitation of paracetamol by method II and atomic absorption spectrometric method were 0.20 and 0.10 mug/ml. Method II and the atomic absorption spectrometric method were applied to demonstrate a pharmacokinetic study by means of salivary samples in normal volunteers who received 1.0 g paracetamol. Intra and inter-day precision did not exceed 6.9%.

  20. Potentiometric determination of Nickel (II ion using 2-hydroxy-1-naphthylidene-N-cyanoacetohydrazone as electroactive material

    Directory of Open Access Journals (Sweden)

    Harish Kumar Sharma

    2014-01-01

    Full Text Available A potentiometric Nickel sensor was prepared using 2-hydroxy-1-naphthylidene-N-cyanoacetohydrazone as electro-active material and epoxy resin as a binding material. A membrane composed of 40% Schiff's base and 60% epoxy resin exhibited the best performance. The membrane showed excellent response in the concentration range of 0.15 ppm to 0.1 mol L- 1 Ni+2 ions with non-Nernstian slope of 22.0 mV/decade, had a rapid response time (less than 10 s, and can be used for three months without any considerable loss of potential. The sensor was useful within the pH range of 1.3 to 9.6, and was able to discriminate between Ni2+ and a large number of alkaline earth and transition metal ions. The practical utility of the sensor has been demonstrated by using it successfully as an indicator electrode in the potentiometric titration of Ni2+ with EDTA and oxalic acid.

  1. Miniaturized ionophore-based potentiometric sensors for the flow-injection determination of metformin in pharmaceutical formulations and biological fluids.

    Science.gov (United States)

    Khaled, Elmorsy; Kamel, Manal S; Hassan, Hassan N; Abd El-Alim, Sameh H; Aboul-Enein, Hassan Y

    2012-12-07

    Miniaturized potentiometric sensors based on β-cyclodextrins (β-CDs) are described for determination of metformin (Mf) in pharmaceutical preparations and biological fluids. Electrode matrix compositions are optimized on the basis of the nature and content of sensing ionophore, ionic sites and plasticizers. Coated wire electrodes (CWEs) modified with heptakis(2,3,6-tri-O-methyl)-β-CD, sodium tetrakis(4-fluorophenyl)borate (NaTFPB) and 2-fluorophenyl 2-nitrophenyl ether (f-NPE), work satisfactorily in the concentration range from 10(-6) to 10(-1) mol L(-1) with Nernstian compliance (55.7 ± 0.4 mV per decade activity) and a detection limit of 8 × 10(-7) mol L(-1). Incorporation of β-CD as a molecular recognition element improved the electrode sensitivity and selectivity due to encapsulation of Mf into the β-CD cavity (host-guest interaction). The developed electrodes have been successfully applied for the potentiometric determination of Mf under batch and flow injection analysis (FIA). FIA allows analysis of 90 samples per h offering the advantages of simplicity, accuracy and automation feasibility. The dissolution profile for metformin pharmaceutical samples (Cidophage®) was monitored using the proposed electrode in comparison with the official spectrophotometric methods. Characterization of the formed Mf-β-CD inclusion complexes is discussed in detail.

  2. Potentiometric RuO2-Ta2O5 pH sensors fabricated using thick film and LTCC technologies.

    Science.gov (United States)

    Manjakkal, Libu; Zaraska, Krzysztof; Cvejin, Katarina; Kulawik, Jan; Szwagierczak, Dorota

    2016-01-15

    The paper reports on the preparation, properties and application of potentiometric pH sensors with thick film RuO2-Ta2O5 sensing electrode and Ag/AgCl/KCl reference electrode screen printed on an alumina substrate. Furthermore, it presents fabrication procedure and characterization of a new miniaturized pH sensor on LTCC (low temperature cofired ceramics) substrate, destined for wireless monitoring. The crystal structure, phase and elemental composition, and microstructure of the films were investigated by X-ray diffractometry, Raman spectroscopy, scanning electron microscopy and energy dispersive spectroscopy. Potentiometric characterization was performed in a wide pH range of 2-12 for different storage conditions and pH loops. The advantages of the proposed thick film pH sensors are: (a) low cost and easy fabrication, (b) excellent sensitivity close to the Nernstian response (56mV/pH) in the wide pH range, (c) fast response, (d) long lifetime, (e) good reproducibility, (f) low hysteresis and drift effects, and (g) low cross-sensitivity towards Li(+), Na(+) and K(+) as interfering ions. The applicability of the sensors for pH measurement of river, tap and distilled water, and some drinks was also tested. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. A novel potentiometric biosensor for determination of L-lysine in commercial pharmaceutical L-lysine tablet and capsule.

    Science.gov (United States)

    Yarar, Saniye; Karakuş, Emine

    2016-01-01

    The construction of an L-lysine biosensor on ammonium-selective poly(vinylchloride) (PVC) membrane electrode is described in this study. The construction procedure occurs in two stages: (I) the preparation of ammonium-selective poly(vinylchloride) (PVC) membrane electrode and (II) the chemical immobilization of lysine oxidase on this ammonium-selective electrode by using glutaraldehyde. The ammonium ions produced after enzymatic reaction were determined potentiometrically. The sensitivity of the lysine biosensor against ammonium ions and lysine were studied. The response time, linear working range, reproducibility and life time of the biosensor were also determined. The interfering effect of other amino acids on the biosensor performance was also studied and potentiometric selectivity coefficients were calculated. Although the biosensor responded mainly against tyrosine, a lot of amino acids and ascorbic acid that can be present in some real samples did not show any important interference. Additionally, lysine assay in commercial pharmaceutical lysine tablets and capsules was also successfully carried out. The results were in good agreement with previously reported values.

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

    Science.gov (United States)

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

    2013-01-01

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

  5. Standard test methods for chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade boron carbide

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2004-01-01

    1.1 These test methods cover procedures for the chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade boron carbide powder and pellets to determine compliance with specifications. 1.2 The analytical procedures appear in the following order: Sections Total Carbon by Combustion and Gravimetry 7-17 Total Boron by Titrimetry 18-28 Isotopic Composition by Mass Spectrometry 29-38 Chloride and Fluoride Separation by Pyrohydrolysis 39-45 Chloride by Constant-Current Coulometry 46-54 Fluoride by Ion-Selective Electrode 55-63 Water by Constant-Voltage Coulometry 64-72 Impurities by Spectrochemical Analysis 73-81 Soluble Boron by Titrimetry 82-95 Soluble Carbon by a Manometric Measurement 96-105 Metallic Impurities by a Direct Reader Spectrometric Method 106-114

  6. [Determination of trace cobalt in human urine by graphite furnace atomic absorption spectrometr].

    Science.gov (United States)

    Zhong, L X; Ding, B M; Jiang, D; Liu, D Y; Yu, B; Zhu, B L; Ding, L

    2016-05-20

    To establish a method to determine cobalt in human urine by graphite furnace atomic absorption spectrometry. Urine with 2% nitric acid diluted two-fold, to quantify the curve, graphite furnace atomic absorption spectrometric detection. Co was linear within 2.5~40.0 ng/ml with r>0.999. Spike experiment showed that Co received good recovery rate, which was 90.8%~94.8%. Intra-assay precisions were 3.2%~5.1% for Co, inter-assay precisions were 4.4%~5.2% for Co. The method by using graphite furnace atomic absorption spectrometr to determine urine Co was fast, accurate and with low matrix effect. It could meet the requirement in GBZ/T 210.5-2008.

  7. Mass-spectrometric source for producing ions of bioorganic thermally unstable products

    International Nuclear Information System (INIS)

    Malakhov, K.V.; Pyatakin, A.N.; Tikhonov, V.M.; Turkina, M.Ya.

    1987-01-01

    A mass-spectrometric ion source of high-molecular compounds based on secondary emission of ions of the studied substance in liquid matrix (glycerol) under the effect of 5 keV Cs + primary ion beam is described. The current of the primary beam is 1 mA, the current of the secondary beam at the inlet of the multiplier makes up 10 -11 -10 -16 A

  8. Gamma-spectrometric examination of hot particles emitted during the Chernobyl accident

    International Nuclear Information System (INIS)

    Balashazy, I.; Szabadine-Szende, G.; Loerinc, M.; Zombori, P.

    1987-05-01

    Ge(Li) gamma-spectrometric examination of hot particles prepared from air filtered dust of Budapest air after the Chernobyl accident is presented. The method of separating hot particles is described and their concentration in the air is determined. The radioactive isotope composition of hot particles is discussed and compared with that of dust samples. Finally, the inhalation probability and radiation burden of hot particles are evaluated. (author)

  9. Mass-spectrometric investigation of thermal dissociation of alkaline earth metal monophosphates

    International Nuclear Information System (INIS)

    Lopatin, S.I.; Semenov, G.A.

    1989-01-01

    By the Knudsen effusion method with mass-spectrometric analysis of vapour phase, processes of thermal dissociation of Mg, Ca, Sr and Ba monophosphates have been studied. It is shown that vapour composition over alkaline-earth metal monophoshates depends on the compsition of condensed phase and volatility of alkaline-earth metal oxides. Dependences of partial pressures of vapour components on the temperature and duration of the experiment are given

  10. Heterogeneous nuclear ribonucleoproteins C1/C2 identified as autoantigens by biochemical and mass spectrometric methods

    DEFF Research Database (Denmark)

    Heegaard, N H; Larsen, Martin Røssel; Muncrief, T

    2000-01-01

    The antigenic specificity of an unusual antinuclear antibody pattern in three patient sera was identified after separating HeLa-cell nuclear extracts by two-dimensional (2D) gel electrophoresis and localizing the antigens by immunoblotting with patient serum. Protein spots were excised from the 2......-separation methods and mass-spectrometric peptide mapping in combination with database searches are powerful tools in the identification of novel autoantigen specificities....

  11. Aspects of optical fibers and spectrometric sensors in chemical process and industrial environments

    International Nuclear Information System (INIS)

    Boisde, G.; Perez, J.J.

    1988-01-01

    For on-line control, the two alternatives of automatic sample transfer and in situ remote analysis are discussed. New concepts are emerging from the possibilities offered by optical fibers. Absorption in the visible, UV and IR, fluorescence and Raman spectrometric techniques are examined. The state of the art of optodes and devices in chemical process control are given, with some examples of applications in nuclear plants

  12. Mass-spectrometric investigation of rare earth acetylacetonates dipivaloylmethanates and their adducts

    International Nuclear Information System (INIS)

    Gavrishzhuk, E.M.; Dzyubenko, N.G.; Martynenko, L.I.

    1985-01-01

    Peculiarities of fragmentation of molecular ions of rare earth acetylacetonates and dipivaloylmethanates under mass-spectrometric investigation of these compounds as well as their adducts with o-phenanthroline, α,α'-dipyridyl, triphenylphosphine oxide are considered in the given review. Similar data for identical derivants of some transitions metals are presented. Data on potentials of appearance and dissociation energy of basic ions in mass-spectra of the studied β-diketonates are analyzed

  13. Construction and performance characterization of ion-selective electrodes for potentiometric determination of pseudoephedrine hydrochloride applying batch and flow injection analysis techniques.

    Science.gov (United States)

    Zayed, Sayed I M; Issa, Yousry M; Hussein, Ahmed

    2006-01-01

    New pseudoephedrine selective electrodes have been constructed of the conventional polymer membrane type by incorporation of pseudoephedrine-phosphotungstate (PE-PT) or pseudoephedrine-silicotungstate (PE-SiT) ion-associates in a poly vinyl chloride (PVC) membrane plasticized with dibutyl phthalate (DBP). The electrodes were fully characterized in terms of the membrane composition, temperature, and pH. The electrodes exhibited mean slopes of calibration graphs of 57.09 and 56.10 mV concentration decade(-1) of PECl at 25 degrees C for (PE-PT) and (PE-SiT) electrodes, respectively. The electrodes showed fast, stable, and near-Nernstian response over the concentration ranges 6.31 x 10(-6)-1.00 x 10(-2) and 5.00 x 10(-5)-1.00x10(-2) M in the case of PE-PT applying batch and flow injection (FI) analysis, respectively, and 1.00 x 10(-5)-1.00 x 10(-2) and 5.00 x 10(-5)-1.00x10(-2) M in the case of PE-SiT for batch and FI analysis system, respectively. Detection limit was 5.01x 10(-6) M for PE-PT electrode and 6.31x10(-6) M for PE-SiT electrode. The electrodes were successfully applied for the potentiometric determination of pseudoephedrine hydrochloride (PECl) in pharmaceutical preparations with mean recovery 101.13 +/- 0.85% and 100.77+0.79% in case of PE-PT applying batch and flow injection systems, respectively, and 100.75+0.85% and 100.79 +/- 0.77% in case of PE-SiT for batch and flow injection systems, respectively. The electrodes exhibited good selectivity for PECl with respect to a large number of inorganic cations, sugars and amino acids.

  14. Potentiometric Surface in the Sparta-Memphis Aquifer of the Mississippi Embayment, Spring 2007

    Science.gov (United States)

    Schrader, T.P.

    2008-01-01

    -Memphis aquifer in the Mississippi embayment was about 540 million gallons per day (Mgal/d). Water use from the Sparta-Memphis aquifer was about 170 Mgal/d in Arkansas, about 68 Mgal/d in Louisiana, about 97 Mgal/d in Mississippi, and about 205 Mgal/d in Tennessee. The author acknowledges, with great appreciation, the efforts of the personnel in the U.S. Geological Survey Water Science Centers of Arkansas, Kentucky, Louisiana, Mississippi, Missouri, and Tennessee, and the Mississippi Department of Environmental Quality Office of Land and Water Resources that participated in the planning, water-level measurement, data evaluation, and review of the potentiometric-surface map. Without the contribution of data and the technical assistance of their staffs, this report would not have been completed.

  15. [MALDI-TOF mass-spectrometric analysis in the accelerated identification of the Vibrio genus microorganisms].

    Science.gov (United States)

    Afanasev, M V; Mironova, L V; Basov, E A; Ostyak, A S; Kulikalova, E S; Urbanovich, L Ya; Balahonov, S V

    2014-01-01

    The goal of this work was to develop methodological approaches to identification of the Vibrio genus representatives using the MALDI-TOF mass-spectrometric analysis technologies. The aspects of the biological safety in sample preparations for mass-spectrometric analysis were studied, reference spectra of six typical V. cholerae strains were developed. Identification of 55 strains, representatives of the Vibrio genus, including 45 V. cholerae strains with different epidemic importance, was performed using the MALDI Biotyper 3.0 basis comprising V. cholerae reference spectra. The possibility of reliable definition of the tested strain taxonomic belonging to the species level was demonstrated. Thus, the results completely corresponded to the data of classical microbiological identification. Stability and reproducibility of the offered research method was experimentally shown. The results allow identification of the Vibrio genus representatives to be implemented with the use of the mass-spectrometric analysis as an effective method that defines a species belonging of the basic Vibrio genus representatives in the shortest-terms.

  16. Spectrometric aerial survey as a new tool for geological survey and mining prospecting

    International Nuclear Information System (INIS)

    Cambon, R.

    1997-01-01

    Airborne survey for radioactive minerals started around 1945. The limited sensitivity of the tools used, the difficulties found for the topographic and training effect corrections, made difficult the evaluation of the results. The technical progresses realized in the recent past years in electronic and computer sciences allowed to overcome these difficulties and gave to the method all its potentialities. With the aerial spectrometric survey, a new step was made, because this method can be used for other topics than radioactive prospection such as geological survey and mining prospection for metallic and industrial minerals. The spectrometric method is based on the possibility to measure photopeak energies (gamma radiation) emitted by radioactive minerals and discriminate between them those emitted by U238, TI 208 and K40 respectively daughter products of uranium, thorium and potassium. For airborne survey, one consider that measuring instruments will allow to pick-up 80% of the radioactive emission concerning the first 15 to 30 centimetres of ground (1 metre maximum). The use of this method for geological and mineral exploration is based on the assumption that different rock types or ore bearing rock types are composed of certain amounts of rock forming minerals which comprise specific quantities of radioactive elements such as potassium, uranium and thorium (cf: Gabelman 77). To be able to evaluate the results of the spectrometric survey it will be necessary to know roughly the behaviour of the different radioactive elements through a complete geological cycle. (author)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-07-01

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

  18. Potentiometric determination of stability constants of cyanoacetato complexes of cobalt(II), nickel(II), copper(II), zinc(II), cadmium(II) and lead(II).

    Science.gov (United States)

    Matusinović, T; Filipović, I

    1981-03-01

    Stability constants of cyanoacetato complexes of cobalt(II), nickel(II), copper(II), zinc(II), cadmium(II) and lead(II) were determined potentiometrically at 25.0 +/- 0.1 degrees and ionic strength 2M (sodium perchlorate). The stability constants were evaluated by a weighted least-squares method.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-07-01

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

  20. Rapid in situ gamma spectrometric determination of fallout radioactivity in the environment. Progress report

    International Nuclear Information System (INIS)

    Zombori, Peter

    1995-01-01

    The main aim of the present CRP is to identify the existing analytical methods and develop new ones, if possible, which provide rapid, reliable, and detailed information on the radioactive contamination of the environment after a major nuclear accident. Gamma spectrometry has long been regarded as one of the most applicable radioanalytical techniques but its use for environmental studies requires some further considerations. There are two possible approaches to measure environmental radioactivity: (a) taking samples of the different environmental media and measuring them in a laboratory or (b) taking the spectrometer to the place of interest and making in situ measurements. In the former case sampling is a crucial factor hindering the rapid analysis while the latter case is not always reliable due to the problems and uncertainties of the measurement interpretation. The application of in situ gamma spectrometry for the determination of environmental radioactivity has become increasingly attractive since the advent of the high resolution semiconductor gamma detectors, especially, more recently, portable high purity Ge diodes (HpGe). The applicability of this technique was very well proved after the Chernobyl reactor accident when in situ spectrometry played an important role in the rapid evaluation of the fall-out situation. Our measurements provided information on the amount and composition of the radioactive contamination of the ground surface already in the first hours. These measurements enabled us to predict the time variation of the environmental radioactivity after the stabilization of the situation. The portability of the system was an important factor in performing a rapid and efficient survey in different parts of the country. A serious disadvantage of this method is, however, that it requires some knowledge about the radionuclide distribution in the soil, which is normally determined by tedious and time consuming sample analysis of the different soil

  1. Potentiometric-level monitoring program, Mississippi and Louisiana: Annual status report for fiscal year 1985. [Richton and Cypress Creek Domes, M5 and Vacherie Dome, LA

    Energy Technology Data Exchange (ETDEWEB)

    1986-10-01

    Potentiometric-level data presented in this report were collected at 82 wells in Mississippi and Louisiana from October 1984 through September 1985. These wells are located near Richton and Cypress Creek Domes in Mississippi and Vacherie dome in Louisiana. Three wells were reinstated to the program during this period. Two previously destroyed wells were deleted from the program. Protective barriers were installed around 26 shallow borings in Mississippi. Cursory analysis of the data in Mississippi indicated minimal, if any, change in potentiometric level during the past year in the Citronelle, Hattiesburg, Cockfield, Sparta, and Wilcox Formations. A slight decline, on the order of 0.3 meter (1 foot), occurred during the past year in well MCCG-1, which is screened in the caprock of Cypress Creek Dome. The potentiometric level in well MRIG-9, in the caprock of Richton Dome, stabilized during fiscal year 1985 following 5 years of increase. The Catahoula Formation experienced a continuing decline of about 0.3 meter/year (1 foot/year). Well MH-5C, screened in the Cook Mountain Formation, showed a continuing, long-term, upward trend on the order of 1.5 meters (4.9 feet) during the past year. The potentiometric level of well MH-8C, screened in the Cook Mountain Formation, stabilized during fiscal year 1985, following 5 years of large annual increases. Wells screened in the Austin Formation in Louisiana showed a downward trend of 0.3 to 1 meter (1 to 3.3 feet) during fiscal year 1985. Other formations in Louisiana generally showed no change in potentiometric level.

  2. Cobalt phthalocyanine as a novel molecular recognition reagent for batch and flow injection potentiometric and spectrophotometric determination of anionic surfactants.

    Science.gov (United States)

    El-Nemma, Eman M; Badawi, Nahla M; Hassan, Saad S M

    2009-05-15

    Cobalt(II) phthalocyanine [Co(II)Pc] is used as both an ionophore and chromogen for batch and flow injection potentiometric and spectrophotometric determination of anionic surfactants (SDS), respectively. The potentiometric technique involves preparation of a polymeric membrane sensor by dispersing [Co(II)Pc] in a plasticized PVC membrane. Under batch mode of operation, the sensor displays a near-Nernstian slope of -56.5 mV decade(-1), wide response linear range of 7.8 x 10(-4) to 8.0 x 10(-7)mol L(-1), lower detection limit of 2.5 x 10(-7)mol L(-1) and exhibits high selectivity for anionic surfactants in the presence of many common ions. Under hydrodynamic mode of operation (FIA), the slope of the calibration plot, limit of detection, and working linear range are -51.1 mV decade(-1), 5.6 x 10(-7) and 1.0 x 10(-3) to 1.0 x 10(-6)mol L(-1), respectively. The spectrophotometric method is based on the use of [Co(II)Pc] solution in dimethylsulfoxide (DMSO) as a chromogenic reagent. The maximum absorption of the reagent at 658 nm linearly decreases with the increase of anionic surfactant over the concentration range 2-30 microg mL(-1). The lower limit of detection is 1 microg mL(-1) and high concentrations of many interfering ions are tolerated. Flow injection spectrophotometric measurements are carried out by injection of the surfactant test solution in a stream of the reagent in DMSO. The sample throughput, working range and lower detection limit are 25-30 samples h(-1), 4-60 and 2 microg mL(-1), respectively. The potentiometric and spectrophotometric techniques are applied to the batch and flow injection measurements of anionic surfactants in some commercial detergent products. The results agree fairly well with data obtained using the standard methylene blue spectrophotometric method.

  3. Fabrication of a multilayer film electrode containing porphyrin and its application as a potentiometric sensor of iodide ion.

    Science.gov (United States)

    Sun, C; Zhao, J; Xu, H; Sun, Y; Zhang, X; Shen, J

    1998-05-01

    A novel iodide ion-selective electrode has been produced based on a molecular deposition technique in which water-soluble porphyrin was alternatively deposited with water-soluble polypyrrole on a 2-aminoethanethiol modified silver electrode. The potentiometric response is independent of pH of the solution between pH 1 and 7, while it is dependent on the nature of the medium. The electrode has a linear dynamic range between 1.6x10(-6) and 0.1 M with a Nernstian slope of 59 mV/decade and a detection limit of 1.0x10(-6) M in acetate buffer (0.1 M, pH 4.6). The electrode has the advantages of low resistance, short conditioning time and fast response.

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

    International Nuclear Information System (INIS)

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

    1990-01-01

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

  5. Spectrophotometric and potentiometric studies of oxidation of Mo(III) by Mo(VI) in phosphoric acid medium

    International Nuclear Information System (INIS)

    Kumar, Arvind; Verma, G.S.P.

    1975-01-01

    Oxidation of Mo(III) (green) by Mo(VI) in an inert atmosphere and in orthophosphoric acid medium at various acid concentrations is reported. Potentiometric and spectrophotometric data suggest that oxidation of Mo(III) proceeds to Mo(V) through a binuclear species Mo(III) Mo(IV) absorbing at 400 nm. The formation of this species is facilitated at high acid concentrations. It is further found that quantitative conversion of Mo(III) into Mo(V) takes place at fairly high acid concentrations. In high phosphoric acid concentrations, solution of Mo(III) has been found to be oxidized to Mo(VI) by air and hence this can be used as a good oxygen absorber. (author)

  6. Potentiometric in Situ Monitoring of Anions in the Synthesis of Copper and Silver Nanoparticles Using the Polyol Process.

    Science.gov (United States)

    Carey, Jesse L; Whitcomb, David R; Chen, Suyue; Penn, R Lee; Bühlmann, Philippe

    2015-12-22

    Potentiometric sensors, such as polymeric membrane, ion-selective electrodes (ISEs), have been used in the past to monitor a variety of chemical processes. However, the use of these sensors has traditionally been limited to aqueous solutions and moderate temperatures. Here we present an ISE with a high-capacity ion-exchange sensing membrane for measurements of nitrate and nitrite in the organic solvent propylene glycol at 150 °C. It is capable of continuously measuring under these conditions for over 180 h. We demonstrate the usefulness of this sensor by in situ monitoring of anion concentrations during the synthesis of copper and silver nanoparticles in propylene glycol using the polyol method. Ion chromatography and a colorimetric method were used to independently confirm anion concentrations measured in situ. In doing so, it was shown that in this reaction the co-ion nitrate is reduced to nitrite.

  7. Sequential potentiometric complexometric redox determination of iron(III) and cobalt(II) with application to alloys.

    Science.gov (United States)

    Rao, B V; Gopinath, R

    1989-08-01

    A simple potentiometric method is presented for successive determination of iron(III) and cobalt(II) by complexometric titration of the iron(III) with EDTA at pH 2 and 40 degrees , followed by redox titration of the cobalt(II) complex with 1,10-phenanthroline or 2,2'-bipyridyl at pH 4-5 and 40 degrees , with gold(III). There is no interference in either determination from common metal ions other than copper(II), which severely affects the cobalt determination but can be removed by electrolysis. The method has been successfully applied to determination of iron and cobalt in Kovar and Alnico magnet alloys.

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

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

    DEFF Research Database (Denmark)

    Olsen, Gunnar; Ulstrup, Jens; Chi, Qijin

    2016-01-01

    We report the design and synthesis of newly functionalized graphene hybrid material that can be used for selective membrane-free potentiometric detection of alkali metal ions, represented by potassium ions. Reduced graphene oxide (RGO) functionalized covalently by 18-crown[6] ether with a dense...... surface coverage is achieved by the introduction of a flexible linking molecule. The resulting hybrid composite is highly stable and is capable of detecting potassium ions down to micromolar ranges with a selectivity over other cations (including Ca2+, Li+, Na+, NH4+) at concentrations up to 25 m......M. This material can be combined further with disposable chips, demonstrating its promise as an effective ion-selective sensing component for practical applications....

  10. Mass Spectrometric Analyses Reveal a Central Role for Ubiquitylation in Remodeling the Arabidopsis Proteome during Photomorphogenesis.

    Science.gov (United States)

    Aguilar-Hernández, Victor; Kim, Do-Young; Stankey, Robert J; Scalf, Mark; Smith, Lloyd M; Vierstra, Richard D

    2017-06-05

    The switch from skotomorphogenesis to photomorphogenesis is a key developmental transition in the life of seed plants. While much of the underpinning proteome remodeling is driven by light-induced changes in gene expression, the proteolytic removal of specific proteins by the ubiquitin-26S proteasome system is also likely paramount. Through mass spectrometric analysis of ubiquitylated proteins affinity-purified from etiolated Arabidopsis seedlings before and after red-light irradiation, we identified a number of influential proteins whose ubiquitylation status is modified during this switch. We observed a substantial enrichment for proteins involved in auxin, abscisic acid, ethylene, and brassinosteroid signaling, peroxisome function, disease resistance, protein phosphorylation and light perception, including the phytochrome (Phy) A and phototropin photoreceptors. Soon after red-light treatment, PhyA becomes the dominant ubiquitylated species, with ubiquitin attachment sites mapped to six lysines. A PhyA mutant protected from ubiquitin addition at these sites is substantially more stable in planta upon photoconversion to Pfr and is hyperactive in driving photomorphogenesis. However, light still stimulates ubiquitylation and degradation of this mutant, implying that other attachment sites and/or proteolytic pathways exist. Collectively, we expand the catalog of ubiquitylation targets in Arabidopsis and show that this post-translational modification is central to the rewiring of plants for photoautotrophic growth. Copyright © 2017 The Author. Published by Elsevier Inc. All rights reserved.

  11. Abortion after deliberate Arthrotec® addition to food. Mass spectrometric detection of diclofenac, misoprostol acid, and their urinary metabolites.

    Science.gov (United States)

    Watzer, Bernhard; Lusthof, Klaas J; Schweer, Horst

    2015-07-01

    Arthrotec(®) (AT) is a combination of diclofenac, a nonsteroidal anti-inflammatory drug (NSAID), and misoprostol (MP), a synthetic analogue of prostaglandin E1 (PGE1). MP is a lipophilic methyl ester prodrug. It is readily metabolized to the biologically active misoprostol acid (MPA). During the last few years, medical studies exhibited MP to be an excellent abortive. In this paper, we describe a rare criminal case of MP abortion, initiated by the expectant father. After the abortion, samples of vomit and urine were collected. Systemic exposure to MP is difficult to prove, because both MP and the active metabolite MPA are hardly excreted in urine. Therefore, in addition to routine toxicological analysis, we used slightly modified, well-established liquid and gas chromatographic/tandem mass spectrometric (LC/MS/MS and GC/MS/MS) methods, for the direct and the indirect detection of MPA and its metabolites. In this case, we were able to demonstrate the presence of the major MP metabolites 2,3-dinor-MPA and 2,3,4,5-tetranor-MPA in the urine of the victim. We also detected paracetamol, 3-methoxyparacetamol and diclofenac-glucuronide in the urine. In the vomit of the victim, we detected diclofenac and MPA. These results, combined with the criminal investigations, showed that the accused had mixed MP into the food of his pregnant girlfriend. Finally, these investigations contributed to a confession of the accused.

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

    Directory of Open Access Journals (Sweden)

    Chenyi Wang

    2008-12-01

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

  13. Gamma Spectrometric Determination of U, Th, K and Some Geochemical Applications

    International Nuclear Information System (INIS)

    Dodona, A.; Tashko, A.

    2001-01-01

    The application of 'in situ' gamma-spectrometric method (''infinite'' environment), made possible the simultanious determination of U, Th and K. 4 channel gamma-spectrometric analyser with NaI(TI) scintilation counter crystal detector (103 cm 3 φ=50x50mm) was used to determin U, Th(more than 1-2 ppm) and K (more than 1%) in laboratory conditions. The detector was inserted into a lead camera and calibrated for measurement geometry with vessel of ''Marineli'' type of a 17o cm 3 volume. The study of main factors, which influence in the gamma spectrometric measurements, (the technical, physical, geometrical and time parameters) has been carried out. International standards of U, Th, K and internal monitoring standard samples are used for the calibration. External analytical control has been realized by other radiometric and chemical methods. The detection limits ( 1 ppm Th, 2ppm U and 1% K) and the relative errors (17-20% for 1-10 ppm U, Th and 10-15% for more than 10 ppm U, Th and more than 1% K) guarantee a quantitative analysis that may be used successfully in the geochemical studies. Some geochemical applications, based on the content of Th, U and Th/U ratio in rocks samples that we have we have analyzed with this method, are shown in this paper. U, Th and their ratio are used as trace elements to indicate the differences between the acidic magmatic rocks of Albania (Th/U ratio=2-6 and>10). The bimodal character of Th/U scattering in ignimbrides and monzonites (Korabi zone) shows that in addition to the ''normal'' rocks, there are also some ones enriched with Th, So, the differential analysis of Th, U, and K may be used as geochemical exploration criteria for the radioactive and non-radioactive mineralization, such as REE (Rare Earth Elements), phospghorites, bauxites, placers etc. (authors)

  14. Mass-spectrometric exploration of proteome structure and function

    DEFF Research Database (Denmark)

    Aebersold, Ruedi; Mann, Matthias

    2016-01-01

    Numerous biological processes are concurrently and coordinately active in every living cell. Each of them encompasses synthetic, catalytic and regulatory functions that are, almost always, carried out by proteins organized further into higher-order structures and networks. For decades......, the structures and functions of selected proteins have been studied using biochemical and biophysical methods. However, the properties and behaviour of the proteome as an integrated system have largely remained elusive. Powerful mass-spectrometry-based technologies now provide unprecedented insights...... into the composition, structure, function and control of the proteome, shedding light on complex biological processes and phenotypes....

  15. Chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade plutonium nitrate solutions

    International Nuclear Information System (INIS)

    Anon.

    1981-01-01

    These analytical procedures are designed to show whether a given material meets the purchaser's specifications as to plutonium content, effective fissile content, and impurity content. The following procedures are described in detail: plutonium by controlled-potential coulometry; plutonium by amperometric titration with iron(II); free acid by titration in an oxalate solution; free acid by iodate precipitation-potentiometric titration method; uranium by Arsenazo I spectrophotometric method; thorium by thorin spectrophotometric method; iron by 1,10-phenanthroline spectrophotometric method; chloride by thiocyanate spectrophotometric method; fluoride by distillation-spectrophotometric method; sulfate by barium sulfate turbidimetric method; isotopic composition by mass spectrometry; americium-241 by extraction and gamma counting; americium-241 by gamma counting; gamma-emitting fission products, uranium, and thorium by gamma-ray spectroscopy; rare earths by copper spark spectrochemical method; tungsten, niobium (columbium), and tantalum by spectrochemical method; simple preparation by spectrographic analysis for general impurities

  16. Radiometric and Spectrometric Calibrations, and Distance Noise Measurement of ToF Cameras

    Science.gov (United States)

    Erz, Michael; Jähne, Bernd

    This paper proposes to extend the EMVA 1288 standard to characterize the properties and noise of image sensors for ToF cameras. The concepts for radiometric and spectrometric sensitivities were extended for intensity images recorded by lock-in pixels. The characterization of the distance information was performed by describing the phase shift analogous to intensities. Results of sensitivity and noise measurements are presented for two ToF cameras: PMDTec CamCube and MESA Imaging SR3101. Both cameras had no intrinsic filter, so the quantum efficiency could be measured from UV to IR. The noise in the phase measurement could be related to the noise in the intensity.

  17. Gas chromatographic-mass spectrometric determination of levodropropizine plasma levels in healthy volunteers.

    Science.gov (United States)

    Zaratin, P; De Angelis, L; Cattabeni, F

    1988-08-01

    A gas chromatographic-mass spectrometric method for the qualitative and quantitative analysis of levodropropizine (S(-)-3-(4-phenyl-piperazin-1-yl)-propane-1,2-diol, DF 526) in plasma is described. The method proved to be highly selective and sensitive. Drug concentrations as low as 5 ng/ml could be measured. Levodropropizine plasma levels were measured in 6 healthy volunteers after administration of an acute 60 mg dose. Peak concentrations were reached between 40 and 60 min and measurable amounts of drug were present till 8 h after administration.

  18. A spectrometric approach in radiography for detection of materials by their effective atomic number

    CERN Document Server

    Ryzhikov, V D; Onyshchenko, G M; Lecoq, P; Smith, C F

    2009-01-01

    In this paper we report a spectrometric approach to dual-energy digital radiography that has been developed and applied to identify specific organic substances and discern small differences in their effective atomic number. An experimental setup has been designed, and a theoretical description proposed based on the experimental results obtained. The proposed method is based on the application of special reference samples made of materials with different effective atomic number and thickness parameters known to affect X-ray attenuation in the low-energy range. The results obtained can be used in the development of a new generation of multi-energy customs or medical X-ray scanners.

  19. The application study on the prospecting for gold by car-borne gamma-ray spectrometric method in northern Hebei and other areas

    International Nuclear Information System (INIS)

    Ma Zhongxiang; Liu Tengyao; Zhang Peng; Lu Shili; Zhai Yugui; Ma Yanfang

    1995-01-01

    The prospecting method for gold by car-borne gamma-ray spectrometric survey is a new geophysical and geochemical technique in the search for concealed gold deposits which can be used to effectively predict the regional gold metallogenetic potential area. The method of car-borne gamma-ray spectrometric survey was adopted and 63416 data at gamma-ray spectrometric measuring sites from rock masses (or strata) in northern Hebei and other areas (49100 km 2 ) are obtained. On the basis of the size of geological bodies, the sliding filtering technique was applied to process the gamma-ray spectrometric data from regional geological bodies and maps showing the parameter distribution characteristics were plotted (11 sheets). In accordance with the thorough on the distribution characteristics of gamma-ray spectrometric parameters that reflect the regional geological environment of gold metallogenesis, a set of gamma-ray spectrometric combination parameters in correlation with regional gold metallogenesis has been established and the characteristic information of gamma-ray spectrometric parameters has been extracted. Combined with geological information, the gold metallogenetic geological environment in the working area was studied, and two potential areas were predicted. After verification, gold mineralization was encountered in some areas. The study results show that the car-borne gamma-ray spectrometric method used for regional gold prospecting is a rapid, economical and effective one

  20. Single-stage mass spectrometric analyses of resin bead samples

    Energy Technology Data Exchange (ETDEWEB)

    Smith, D. H.; Walker, R. L.; Bertram, L. K.; Carter, J. A.

    1978-10-01

    Plutonium and uranium from dissolver solutions loaded on resin beads can be analyzed on single-stage mass spectrometers with little or no degradation of results provided proper care is exercised with regard to sample handling techniques. Additionally, storage of samples on resin beads is feasible for periods at least as long as six months provided the beads are not exposed to residual HNO/sub 3/ and air; it is probable that beads will retain their integrity much longer than six months when stored under collodion, but as yet no data to support this contention have been collected. Conventional or commercial mass spectrometers can readily be adapted to the resin bead technique by installing a pulse-counting detection system. The cost of such conversion will vary depending on whether or not a data acquisition system will be needed. A reasonable estimate is that the cost will be in the neighborhood of $15,000; this figure includes the price of a multi-channel analyzer to serve as a temporary data storage device, but does not include the cost of a computer. It does not appear that it will be practicable to switch easily back and forth between pulse-counting and current integration modes unless the instrument is provided with a movable Faraday cup. Using the same multiplier in both modes would undoubtedly degrade its performance in each. The requirements of low background counting rates and high gain for pulse counting, and of relatively high signal handling capacity in current integration are mutually incompatible if demanded of the same multiplier.

  1. Recent developments in atomic spectrometric methods as tools for the analysis of advanced materials with the example of advanced ceramics

    International Nuclear Information System (INIS)

    Broekaert, J.A.C.

    1995-01-01

    Atomic spectrometric methods are based on the emission, absorption and fluorescence processes and using radiation in the UV and VIS region. These methods are suitable for the direct analysis of solids. The first type of methodology is extremely attractive for routine analysis. Atomic spectrometric methods are relative methods and characterized with independent methods and these are widely available in the analytical laboratories. For solution analysis inductively coupled plasma (ICP) sources became available. For electrically non-conducting samples such as ceramics are discussed as laser ablation in combination with various types of spectrometry. (A.B.)

  2. Assessment of predictive indices for glioblastomas radiation therapy: comparison of perfusion MRI and spectrometric imagery by magnetic resonance

    International Nuclear Information System (INIS)

    Lemoine, J.M.; Laprie, A.; Moyal Cohen-Jonathan, E.; Ken, S.; Lemoine, J.M.; Laprie, A.; Franceries, X.; Lotterie, J.A.; Celsis, P.; Lubrano, V.; Berry, I.; Ken, S.; Lemoine, J.M.; Franceries, X.; Lotterie, J.A.; Berry, I.; Lubrano, V.

    2010-01-01

    The authors report the comparison of several imagery modalities: anatomic imagery (T1-weighted MRI after gadolinium injection and T2-weighted MRI), metabolic imagery (spectrometric imagery by magnetic resonance) and functional imagery (perfusion MRI). This comparison has been performed within the frame of a prospective clinic test associating a radiosensitizer concomitant with a radiation therapy of glioblastomas. It appears that the integration of data of spectrometric imagery by magnetic resonance and of perfusion MRI is a promising method to overcome the resistance of glioblastomas. Short communication

  3. Mass spectrometric identification of proteins that interact through specific domains of the poly(A) binding protein

    DEFF Research Database (Denmark)

    Richardson, Roy; Denis, Clyde L; Zhang, Chongxu

    2012-01-01

    Poly(A) binding protein (PAB1) is involved in a number of RNA metabolic functions in eukaryotic cells and correspondingly is suggested to associate with a number of proteins. We have used mass spectrometric analysis to identify 55 non-ribosomal proteins that specifically interact with PAB1 from...... Saccharomyces cerevisiae. Because many of these factors may associate only indirectly with PAB1 by being components of the PAB1-mRNP structure, we additionally conducted mass spectrometric analyses on seven metabolically defined PAB1 deletion derivatives to delimit the interactions between these proteins...

  4. Vis-NIR spectrometric determination of Brix and sucrose in sugar production samples using kernel partial least squares with interval selection based on the successive projections algorithm.

    Science.gov (United States)

    de Almeida, Valber Elias; de Araújo Gomes, Adriano; de Sousa Fernandes, David Douglas; Goicoechea, Héctor Casimiro; Galvão, Roberto Kawakami Harrop; Araújo, Mario Cesar Ugulino

    2018-05-01

    This paper proposes a new variable selection method for nonlinear multivariate calibration, combining the Successive Projections Algorithm for interval selection (iSPA) with the Kernel Partial Least Squares (Kernel-PLS) modelling technique. The proposed iSPA-Kernel-PLS algorithm is employed in a case study involving a Vis-NIR spectrometric dataset with complex nonlinear features. The analytical problem consists of determining Brix and sucrose content in samples from a sugar production system, on the basis of transflectance spectra. As compared to full-spectrum Kernel-PLS, the iSPA-Kernel-PLS models involve a smaller number of variables and display statistically significant superiority in terms of accuracy and/or bias in the predictions. Published by Elsevier B.V.

  5. A Caenorhabditis elegans Mass Spectrometric Resource for Neuropeptidomics

    Science.gov (United States)

    Van Bael, Sven; Zels, Sven; Boonen, Kurt; Beets, Isabel; Schoofs, Liliane; Temmerman, Liesbet

    2018-01-01

    Neuropeptides are important signaling molecules used by nervous systems to mediate and fine-tune neuronal communication. They can function as neurotransmitters or neuromodulators in neural circuits, or they can be released as neurohormones to target distant cells and tissues. Neuropeptides are typically cleaved from larger precursor proteins by the action of proteases and can be the subject of post-translational modifications. The short, mature neuropeptide sequences often entail the only evolutionarily reasonably conserved regions in these precursor proteins. Therefore, it is particularly challenging to predict all putative bioactive peptides through in silico mining of neuropeptide precursor sequences. Peptidomics is an approach that allows de novo characterization of peptides extracted from body fluids, cells, tissues, organs, or whole-body preparations. Mass spectrometry, often combined with on-line liquid chromatography, is a hallmark technique used in peptidomics research. Here, we used an acidified methanol extraction procedure and a quadrupole-Orbitrap LC-MS/MS pipeline to analyze the neuropeptidome of Caenorhabditis elegans. We identified an unprecedented number of 203 mature neuropeptides from C. elegans whole-body extracts, including 35 peptides from known, hypothetical, as well as from completely novel neuropeptide precursor proteins that have not been predicted in silico. This set of biochemically verified peptide sequences provides the most elaborate C. elegans reference neurpeptidome so far. To exploit this resource to the fullest, we make our in-house database of known and predicted neuropeptides available to the community as a valuable resource. We are providing these collective data to help the community progress, amongst others, by supporting future differential and/or functional studies.

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

    Science.gov (United States)

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

    2016-08-07

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

  7. Determination of plutonium-241 half-life by mass spectrometric measurement

    International Nuclear Information System (INIS)

    Hiyama, Takashi; Wada, Yukio; Onishi, Koichi

    1982-01-01

    Much data for Pu-241 half-life have been reported, but these values range from 13.8 years to 15.1 years depending on investigators. In order to define the half-life of Pu-241, the half-life was calculated by analyzing the mass spectrometry data obtained in the author's laboratory over the past six years on Plutonium Isotopic Standard Reference Materials prepared at the National Bureau of Standards (NBS). The sample used for this work consisted of SRM-947 and SRM-948 prepared at NBS. Before mass spectrometric analysis, the plutonium aliquot was separated from its Am-241 daughter by anion exchange chromatography, since Am-241 is not distinguished from Pu-241 in the mass spectrometer. 241 Pu/ 239 Pu and 241 Pu/ 240 Pu ratios were calculated from the values of mass spectrometric measurement. From the relation of log N to time, the half-life of Pu-241 was determined, based on the slope using a least squares fit. The half-life of Pu-241 was estimated to be 14.29+-0.15 years. (Yoshitake, I.)

  8. Fully Automated Spectrometric Protocols for Determination of Antioxidant Activity: Advantages and Disadvantages

    Directory of Open Access Journals (Sweden)

    Marketa Ryvolova

    2010-11-01

    Full Text Available The aim of this study was to describe behaviour, kinetics, time courses and limitations of the six different fully automated spectrometric methods - DPPH, TEAC, FRAP, DMPD, Free Radicals and Blue CrO5. Absorption curves were measured and absorbance maxima were found. All methods were calibrated using the standard compounds Trolox® and/or gallic acid. Calibration curves were determined (relative standard deviation was within the range from 1.5 to 2.5 %. The obtained characteristics were compared and discussed. Moreover, the data obtained were applied to optimize and to automate all mentioned protocols. Automatic analyzer allowed us to analyse simultaneously larger set of samples, to decrease the measurement time, to eliminate the errors and to provide data of higher quality in comparison to manual analysis. The total time of analysis for one sample was decreased to 10 min for all six methods. In contrary, the total time of manual spectrometric determination was approximately 120 min. The obtained data provided good correlations between studied methods (R = 0.97 – 0.99.

  9. Assessment of current mass spectrometric workflows for the quantification of low abundant proteins and phosphorylation sites

    Directory of Open Access Journals (Sweden)

    Manuel Bauer

    2015-12-01

    Full Text Available The data described here provide a systematic performance evaluation of popular data-dependent (DDA and independent (DIA mass spectrometric (MS workflows currently used in quantitative proteomics. We assessed the limits of identification, quantification and detection for each method by analyzing a dilution series of 20 unmodified and 10 phosphorylated synthetic heavy labeled reference peptides, respectively, covering six orders of magnitude in peptide concentration with and without a complex human cell digest background. We found that all methods performed very similarly in the absence of background proteins, however, when analyzing whole cell lysates, targeted methods were at least 5–10 times more sensitive than directed or DDA methods. In particular, higher stage fragmentation (MS3 of the neutral loss peak using a linear ion trap increased dynamic quantification range of some phosphopeptides up to 100-fold. We illustrate the power of this targeted MS3 approach for phosphopeptide monitoring by successfully quantifying 9 phosphorylation sites of the kinetochore and spindle assembly checkpoint component Mad1 over different cell cycle states from non-enriched pull-down samples. The data are associated to the research article ‘Evaluation of data-dependent and data-independent mass spectrometric workflows for sensitive quantification of proteins and phosphorylation sites׳ (Bauer et al., 2014 [1]. The mass spectrometry and the analysis dataset have been deposited to the ProteomeXchange Consortium (http://proteomecentral.proteomexchange.org via the PRIDE partner repository with the dataset identifier PXD000964.

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

    OpenAIRE

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

    2016-01-01

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

  11. Determination of cilnidipine, a new calcium antagonist, in human plasma using high performance liquid chromatography with tandem mass spectrometric detection.

    Science.gov (United States)

    Zhang, Xianhua; Zhai, Suodi; Zhao, Rongsheng; Ouyang, Jin; Li, Xiaoguang; Baeyens, Willy R G

    2007-09-26

    A rapid, sensitive and reliable high performance liquid chromatographic method coupled with tandem mass spectrometry (HPLC-MS/MS) has been developed and validated for the determination of cilnidipine, a relatively new calcium antagonist, in human plasma. The reversed-phase chromatographic system was interfaced with a TurboIonSpray (TIS) source. Nimodipine was employed as the internal standard (IS). Sample extracts following protein precipitation were injected into the HPLC-MS/MS system. The analyte and IS were eluted isocratically on a C18 column, with a mobile phase consisting of CH(3)OH and NH(4)Ac (96:4, v/v). The ions were detected by a triple quadrupole mass spectrometric detector in the negative mode. Quantification was performed using multiple reaction monitoring (MRM) of the transitions m/z 491.2-->122.1 and m/z 417.1-->122.1 for cilnidipine and for the IS, respectively. The analysis time for each run was 3.0 min. The calibration curve fitted well over the concentration range of 0.1-10 ngmL(-1), with the regression equation Y=(0.103+/-0.002)X+(0.014+/-0.003) (n=5), r=0.9994. The intra-day and inter-day R.S.D.% were less than 12.51% at all concentration levels within the calibration range. The recoveries were between 92.71% and 97.64%. The long-term stability and freeze-thaw stability were satisfying at each level. The present method provides a modern, rapid and robust tool for pharmacokinetic studies of cilnidipine.

  12. An Attempt to automate the lithological classification of rocks using geological, gamma-spectrometric and satellite image datasets

    International Nuclear Information System (INIS)

    Fouad, M. K.; Mielik, M. L.; Gharieb, A. N.

    2004-01-01

    The present study aims essentially at proving that the application of the integrated airborne gamma spectrometric and satellite image data is capable of refining the mapped surface geology, and identification of anomalous zones of radioelement content that could provide favorable exploration targets for radioactive mineralizations.The application of the appropriate statistical technique to correlate between satellite image data and gamma-spectrometric data is of great significance in this respect. Experience shows that Landsat T M data in 7 spectral bands are successfully used in such studies rather than MSS. Multivariate statistical analysis techniques are applied to airborne spectrometric and different spectral Landsat T M data. Reduction of the data from n-dimensionality, both qualitatively as color composite image, and quantitatively, as principal component analysis, is performed using some statistical control parameters. This technique shows distinct efficiency in defining areas where different lit ho facies occur. An area located at the north of the Eastern Desert of Egypt, north of Hurgada town, was chosen to test the proposed technique of integrated interpretation of data of different physical nature. The reduced data are represented and interpreted both qualitatively and quantitatively. The advantages and limitations of applying such technique to the different airborne spectrometric, and Landsat T M data are identified. (authors)

  13. Identifying tissue-specific signal variation in MALDI mass spectrometric imaging by use of an internal standard

    NARCIS (Netherlands)

    Pirman, D.A.; Kiss, A.; Heeren, R.M.A.; Yost, R.A.

    2013-01-01

    Generating analyte-specific distribution maps of compounds in a tissue sample by matrix-assisted laser desorption/ionization (MALDI) mass spectrometric imaging (MSI) has become a useful tool in numerous areas across the biological sciences. Direct analysis of the tissue sample provides MS images of

  14. Differentiation of whole grain and refined wheat (T. aestivum) flour using a fuzzy mass spectrometric fingerprinting and chemometric approaches

    Science.gov (United States)

    A fuzzy mass spectrometric (MS) fingerprinting method combined with chemometric analysis was established to provide rapid discrimination between whole grain and refined wheat flour. Twenty one samples, including thirteen samples from three cultivars and eight from local grocery store, were studied....

  15. Mass spectrometric confirmation criterion for product-ion spectra generated in flow-injection analysis. Environmental application

    NARCIS (Netherlands)

    Geerdink, R.B.; Niessen, W.M.A.; Brinkman, U.A.T.

    2001-01-01

    The suitability of a confirmation criterion recently recommended in the Netherlands for gas chromatography with mass spectrometric detection (GC-MS), was evaluated for flow-injection analysis (FIA) with atmospheric pressure chemical ionisation MS-MS detection. The main feature of the criterion is

  16. Method and apparatus for enhanced sequencing of complex molecules using surface-induced dissociation in conjunction with mass spectrometric analysis

    Science.gov (United States)

    Laskin, Julia [Richland, WA; Futrell, Jean H [Richland, WA

    2008-04-29

    The invention relates to a method and apparatus for enhanced sequencing of complex molecules using surface-induced dissociation (SID) in conjunction with mass spectrometric analysis. Results demonstrate formation of a wide distribution of structure-specific fragments having wide sequence coverage useful for sequencing and identifying the complex molecules.

  17. Liquid chromatography-tandem mass spectrometric assay for the nucleoside reverse transcriptase inhibitor emtricitabine in human plasma

    NARCIS (Netherlands)

    Sparidans, Rolf W.; Prins, Jan M.; Schellens, Jan H. M.; Beijnen, Jos H.

    2007-01-01

    A liquid chromatography-tandem mass spectrometric assay for the determination of the antiretroviral nucleoside emtricitabine in human plasma was developed and validated using a simple sample pre-treatment procedure. After addition of 5'-deoxy-5-fluorocytidine as the internal standard and protein

  18. Determination of isotope fractionation effect using a double spike (242Pu+240Pu) during the mass spectrometric analysis of plutonium

    International Nuclear Information System (INIS)

    Chitambar, S.A.; Parab, A.R.; Khodade, P.S.; Jain, H.C.

    1986-01-01

    Isotope fractionation effect during the mass spectrometric analysis of plutonium has been investigated using a double spike ( 242 Pu+ 240 Pu) and the determination of concentration of plutonium in dissolver solution of irradiated fuel is reported. (author). 6 refs., 2 tables

  19. Water-Table and Potentiometric-Surface Altitudes in the Upper Glacial, Magothy, and Lloyd Aquifers beneath Long Island, New York, March-April 2006

    Science.gov (United States)

    Monti, Jack; Busciolano, Ronald J.

    2009-01-01

    The U.S. Geological Survey (USGS), in cooperation with State and local agencies, systematically collects ground-water data at varying measurement frequencies to monitor the hydrologic situation on Long Island, New York. Each year during March and April, the USGS conducts a synoptic survey of hydrologic conditions to define the spatial distribution of the water table and potentiometric surfaces within the three main water-bearing units underlying Long Island - the upper glacial, Magothy, and Lloyd aquifers. These data and the maps constructed from them are commonly used in studies of Long Island's hydrology, and by water managers and suppliers for aquifer management and planning purposes. Water-level measurements made in 502 wells across Long Island during March-April 2006, were used to prepare the maps in this report. Measurements were made by the wetted-tape method to the nearest hundredth of a foot. Water-table and potentiometric-surface altitudes in these aquifers were contoured using these measurements. The water-table contours were interpreted using water-level data collected from 341 wells screened in the upper glacial aquifer and (or) shallow Magothy aquifer; the Magothy aquifer's potentiometric-surface contours were interpreted from measurements at 102 wells screened in the middle to deep Magothy aquifer and (or) contiguous and hydraulically connected Jameco aquifer; and the Lloyd aquifer's potentiometric-surface contours were interpreted from measurements at 59 wells screened in the Lloyd aquifer or contiguous and hydraulically connected North Shore aquifer. Many of the supply wells are in continuous operation and, therefore, were turned off for a minimum of 24 hours before measurements were made so that the water levels in the wells could recover to the level of the potentiometric head in the surrounding aquifer. Full recovery time at some of these supply wells can exceed 24 hours; therefore, water levels measured at these wells are assumed to be less

  20. Comparative Analysis of Volatile Defensive Secretions of Three Species of Pyrrhocoridae (Insecta: Heteroptera by Gas Chromatography-Mass Spectrometric Method.

    Directory of Open Access Journals (Sweden)

    Jan Krajicek

    Full Text Available The true bugs (Hemiptera: Heteroptera have evolved a system of well-developed scent glands that produce diverse and frequently strongly odorous compounds that act mainly as chemical protection against predators. A new method of non-lethal sampling with subsequent separation using gas chromatography with mass spectrometric detection was proposed for analysis of these volatile defensive secretions. Separation was performed on Rtx-200 column containing fluorinated polysiloxane stationary phase. Various mechanical irritation methods (ultrasonics, shaking, pressing bugs with plunger of syringe were tested for secretion sampling with a special focus on non-lethal irritation. The preconcentration step was performed by sorption on solid phase microextraction (SPME fibers with different polarity. For optimization of sampling procedure, Pyrrhocoris apterus was selected. The entire multi-parameter optimization procedure of secretion sampling was performed using response surface methodology. The irritation of bugs by pressing them with a plunger of syringe was shown to be the most suitable. The developed method was applied to analysis of secretions produced by adult males and females of Pyrrhocoris apterus, Pyrrhocoris tibialis and Scantius aegyptius (all Heteroptera: Pyrrhocoridae. The chemical composition of secretion, particularly that of alcohols, aldehydes and esters, is species-specific in all three pyrrhocorid species studied. The sexual dimorphism in occurrence of particular compounds is largely limited to alcohols and suggests their epigamic intraspecific function. The phenetic overall similarities in composition of secretion do not reflect either relationship of species or similarities in antipredatory color pattern. The similarities of secretions may be linked with antipredatory strategies. The proposed method requires only a few individuals which remain alive after the procedure. Thus secretions of a number of species including even the rare

  1. A microchip electrophoresis-mass spectrometric platform for fast separation and identification of enantiomers employing the partial filling technique

    Science.gov (United States)

    Li, Xiangtang; Xiao, Dan; Ou, Xiao-Ming; McCullumn, Cassandra; Liu, Yi-Ming

    2013-01-01

    A microchip electrophoresis-mass spectrometric (MCE-MS) method was developed for fast chiral analysis. The proposed MCE-MS platform deployed a glass /PDMS hybrid microchip with an easy-to-fabricate monolithic nanoelectrospray emitter. Enantiomeric MCE separation was achieved by means of the partial filling technique. A novel chip design with an arm channel connecting to the middle of the MCE separation channel for delivering the chiral selector was tested and proven valid. Enantiomeric separation of 3.4-dihydroxyphenylalanine (DOPA), glutamic acid (Glu), and serine (Ser), the selected test compounds, were achieved within 130 s with resolution values (Rs) of 2.4, 1.1, and 1.0, respectively. The proposed chiral MCE-MS assay was sensitive and had detection limits of 43 nM for L-DOPA and 47 nM for D-DOPA. The analytical platform was well suited for studies of stereochemical preference in living cells because it integrated cell culture, sample injection, chiral separation, and MS detection into a single platform. Metabolism of DOPA in human SH-SY5Y neuronal cells was studied as a model system. On-chip incubation of SH-SY5Y cells with racemic DOPA was carried out, and the incubation solution was injected and in-line assayed at time intervals. It was found that L-DOPA concentration decreased gradually as incubation time increased while the concentration of coexisting D-DOPA remained constant. The results firmly indicated that SH-SY5Y cells metabolized L-DOPA effectively while left D-DOPA intact. PMID:24354006

  2. Spectrometric characterization of effluent organic matter of a sequencing batch reactor operated at three sludge retention times.

    Science.gov (United States)

    Esparza-Soto, M; Núñez-Hernández, S; Fall, C

    2011-12-01

    Effluent organic matter (EfOM) from activated sludge systems is composed primarily of influent refractory compounds, residual degradable substrate, intermediate products and soluble microbial products (SMPs). Depending on operational conditions (hydraulic and sludge retention time (SRT)), the quantity and quality of EfOM significantly changes. The main objective of this research was to quantify and characterize the EfOM of a lab-scale activated sludge sequencing batch reactor (SBR), which was operated at three SRTs and fed glucose, an easily biodegradable substrate. EfOM was followed with two direct-quantification methods (chemical oxygen demand (COD) and dissolved organic carbon (DOC)), three spectrometric methods (ultraviolet absorbance at 254 nm (UVA(254)), excitation-emission matrix (EEM) fluorescence and parallel factor analysis (PARAFAC)) and three organic matter (OM) indices (specific UVA(254) (SUVA), SUVA-COD, COD/DOC ratio). The significant increment of UVA(254) and OM indices after treatment indicated an accumulation of refractory high-molecular-weight humic-like compounds in the EfOM, which demonstrated that EfOM was composed mainly by SMPs and not glucose. On the other hand, as the SRT increased, the amount of EfOM decreased, but SUVA, SUVA-COD and fluorescence intensity increased; these trends indicated the accumulation of SMPs of increased molecular weight and aromaticity. Increasing SRT in the SBRs reduced the amount of EfOM, but increased its aromaticity and reactivity. Visual analysis of EfOM EEMs showed two protein- and one humic-like peak, which were attributed to SMPs generated within the SBRs. PARAFAC determined that a two-component model best represented EfOM EEMs. The two-components from PARAFAC were mathematically correlated to the visually identified protein- and humic-like SMPs peaks. Copyright © 2011 Elsevier Ltd. All rights reserved.

  3. Potentiometric Sensor for Gadolinium(III Ion Based on Zirconium(IV Tungstophosphate as an Electroactive Material

    Directory of Open Access Journals (Sweden)

    Harish K. Sharma

    2009-01-01

    Full Text Available A new inorganic ion exchanger has been synthesized namely Zirconium(IV tungstophosphate [ZrWP]. The synthesized exchanger was characterized using ion exchange capacity and distribution coefficient (Kd. For further studies, exchanger with 0.35 meq/g ion-exchange capacity was selected. Electrochemical studies were carried out on the ion exchange membranes using epoxy resin as a binder. In case of ZrWP, the membrane having the composition; Zirconium(IV tugstophosphate (40% and epoxy resin (60% exhibits best performance. The membrane works well over a wide range of concentration from 1×10-5 to 1×10-1 M of Gd(III ion with an over- Nernstian slope of 30 mv/ decade. The response time of the sensor is 15 seconds. For this membrane, effect of internal solution has been studied and the electrode was successfully used in partially non-aqueous media too. Fixed interference method and matched potential method has been used for determining selectivity coefficient with respect to alkali, alkaline earth, some transition and rare earth metal ions that are normally present along with Gd(III in its ores. The electrode can be used in the pH range 4.0-10.0 for 10-1 M and 3.0-7.0 for 10-2 M concentration of target ion. These sensors have been used as indicator electrodes in the potentiometric titration of Gd(III ion against EDTA and oxalic acid.

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

    Science.gov (United States)

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

    2016-05-01

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

  5. A Novel Potentiometric Sensor for Determination of Neurotoxin β-N-Oxalyl-L-α, β-Diaminopropionic Acid

    Directory of Open Access Journals (Sweden)

    Omer Isildak

    2014-01-01

    Full Text Available A novel potentiometric sensor based on ionophore (Cd(NH2CH2CH2OCH2CH2OCH2CH2NH2Ag3(CN5 for the determination of β-N-oxalyl-l-α, β-diaminopropionic acid (ODAP is developed. The ODAP-selective membrane sensor demonstrates high sensitivity and short response time. The detection limit of the ODAP-selective membrane sensor is about 2×10-6 mol L-1 and the response time is shorter than 6 s. The linear dynamic range of the ODAP-selective membrane sensor is between ODAP concentrations of 1.0×10-2 and 1×10-6 mol L-1. The ODAP-selective membrane sensor exhibits good operational stability for at least one week in dry conditions at 4–6°C. It has a reproducible and stable response during continuous work for at least 10 h with a relative standard deviation of 0.28% (n = 18.

  6. Enantioselective Potentiometric Membrane Electrodes Based on Antibiotics for the Determination of L- and D-Glyceric Acids

    Directory of Open Access Journals (Sweden)

    Raluca-Ioana Stefan-van Staden

    2011-01-01

    Full Text Available Glyceric acid (GA is a human metabolite existing in L- and D-configurations, which are considered the markers for the diseases L- and D-glyceric aciduria/academia, respectively. Enantioselective, potentiometric membrane electrodes based on carbon paste modified with antibiotics as chiral selectors, vancomycin, and teicoplanin were designed for the assay of L- and D-GA, respectively, in the concentration ranges of 10−9–10−7 and 10−4–10−2 moL/L with very low detection limits (1.5 × 10−10 moL/L for L-GA and 1.6 × 10−4  moL/L for D-GA, resp.. The surface of the electrodes can be regenerated simply by polishing in order to obtain a fresh surface ready to be used in a new assay. The proposed electrodes can be successfully applied for the enantioanalysis of L- and D-glyceric acids in serum samples.

  7. A fast response oxygen sensor based upon a fully-sealed zirconia pump-gauge operated in the potentiometric mode

    Science.gov (United States)

    Benammar, M.; Maskell, W. C.

    1992-06-01

    An instrument for fast and continuous measurement of oxygen partial pressure not requiring a reference gas was constructed around a sealed zirconia oxygen pump-gauge sensor operated in the ac mode. By appropriate signal processing of the gauge EMF, the mean oxygen partial pressure within the sensor was determined and maintained constant via a feedback loop. Potentiometric measurement of the oxygen partial pressure in the sample gas was made relative to this controlled internal reference. The response time of the instrument for a step change in oxygen partial pressure from 1 to 10 kPa was only 65 ms. ned" OutputMedium="All"> 1 3 Proceedings of the 29th International Conference on the Applications of the Mössbauer Effect (ICAME 2007) held in Kanpur, India, 14-19 October 2007, PART IV/VII 30 2008 11 19 2008 11 18 2008 7 2008 Springer Science+Business Media B.V. 2008 9803 10.1007/s10751-008-9803-9 1 On the phenomena occurring at the interface between iron and iron–platinum thin films 1 7 2008 9 17 2008 10 10 Springer Science+Business Media B.V.

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

    Science.gov (United States)

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

    2013-03-01

    In this research, we report a new Ho(3+)-PVC membrane electrode based on N-(4,5-dimethyl-2-(picolinamido)phenyl)picolinamide (H(2)Me(2)bpb) as a suitable ion carrier. Poly vinylchloride (PVC)-based membrane composed of H(2)Me(2)bpb with oleic acid (OA) as anionic additives, and o-nitrophenyloctyl ether (NPOE) as plasticized solvent mediator. The sensor exhibits a Nernstian slope of 20.1 ± 0.2 mV decade(-1) over the concentration range of 1.0 × 10(-6) to 1.0 × 1(-2) mol L(-1), and a detection limit of 5.0 × 10(-7) mol L(-1) of Ho(3+) ions. The potentiometric response of the sensor is independent of the solution pH in the range of 3.5-9.4. It has a very short response time, in the whole concentration range (<10s), and can be used for at least eight weeks. The proposed electrode shows a good selectivity towards Ho(3+) ions over a wide variety of cations, including alkali, alkaline earth, transition and heavy metal ions. To assess its analytical applicability the proposed Ho(3+) sensor was successfully applied as an indicator electrode in the titration of Ho(3+) ion solutions in certified reference materials, alloy samples and for the determination of the fluoride ion in two mouthwash preparations. Copyright © 2012 Elsevier B.V. All rights reserved.

  9. A metallic cobalt electrode for the indirect potentiometric determination of calcium and magnesium in natural waters using flow injection analysis.

    Science.gov (United States)

    Chen, Z; Adams, M A

    1998-11-01

    A flow injection analysis of Ca(2+) and Mg(2+) using indirect potentiometric detection in natural waters is proposed, where Ca(2+) or Mg(2+) are injected into a buffer carrier containing phosphate, resulting in the formation of Ca(3)(PO(4))(2) or Mg(3)(PO(4))(2). The consequent reduction in free phosphate in the carrier solution is detected using a metallic cobalt wire electrode. Indirect electrode response was used and the experimental conditions affecting electrode response were optimized. Responses were linear in the concentration range 5x10(-4) to 5x10(-3) M with a detection limit of 1x10(-5) M in 20 mM phosphate buffer at pH 8.0. The relative standard derivation at 1 mM of Ca(2+) and Mg(2+) were 3.9 and 3.7% (n=10), respectively. EGTA and 8-hydroxyquinoline were used as the masking agents for Ca(2+) and Mg(2+), respectively. Concentrations of Ca(2+) and Mg(2+) in natural waters were successfully determined by the proposed method.

  10. A novel cobalt(II)-selective potentiometric sensor based on p-(4-n-butylphenylazo)calix[4]arene.

    Science.gov (United States)

    Kumar, Pankaj; Shim, Yoon-Bo

    2009-01-15

    A new poly(vinyl chloride)-based membranes containing p-(4-n-butylphenylazo)calix[4]arene (I) as an electroactive material along with sodiumtetraphenylborate (NaTPB), and dibutyl(butyl)phosphonate in the ratio 10:100:1:200 (I:DBBP:NaTPB:PVC) (w/w) was used to fabricate a new cobalt(II)-selective sensor. It exhibited a working concentration range of 9.2 x 10(-6) to 1.0 x 10(-1)M, with a Nernstian slope of 29.0+/-1.0 mV/decade of activity and the response time of 25s. This sensor shows the detection limit of 4.0 x 10(-6)M. Its potential response remains unaffected of pH in the range, 4.0-7.2, and the cell assembly can be used successfully in partially non-aqueous medium (up to 10%, v/v) without significant change in the slope of working concentration range. The sensor has a lifetime of about 3 months and exhibits excellent selectivity over a number of mono-, bi-, and tri-valent cations including alkali, alkaline earth metal, heavy and transition metal ions. It can be used as an indicator electrode for the end point determination in the potentiometric titration of cobalt ions against ethylenediaminetetraacetic acid (EDTA) as well as for the determination of cobalt ion concentration in real samples.

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

    Science.gov (United States)

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

    2017-12-01

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

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

  13. Spectrometric gamma radiation of shale cores applied to sweet spot discrimination in Eastern Pomerania, Poland

    Science.gov (United States)

    Skupio, Rafal; de Alemar Barberes, Gabriel

    2017-12-01

    This paper describes the application and calculation of hydrocarbon anomalies in two different boreholes located in Eastern Pomerania (northern Poland). Spectrometric data from borehole geophysical probe (borehole 1) and portable gamma logger (borehole 2) were used to analyze shale formations. The results from borehole 1 presented a statistically significant, moderate correlation between calculated hydrocarbon anomalies and hydrocarbon saturation data obtained from well log interpretation. Borehole 2 has been analyzed focusing on the gamma radiation of the core samples, and the positive results of borehole 1. Hydrocarbon anomalies calculated from spectral gamma radiation are reliable indicators of sweet spots, based solely on a cursory evaluation of core measurements. These preliminary information acquired from gamma-ray measurements could help increase sampling precision of further geochemical analysis.

  14. New fortran computer programs to acquire and process isotopic mass spectrometric data

    Energy Technology Data Exchange (ETDEWEB)

    Smith, D.H.

    1979-09-01

    This report describes in some detail the operation of newly written programs that acquire and process isotopic mass spectrometric data. Both functional and overall design aspects are addressed. The three basic program units - file manipulation, data acquisition, and data processing - are discussed in turn. Step-by-step instructions are included where appropriate, and each subsection is described in enough detail to give a clear picture of its function. Organization of the file structure, which is central to the entire concept, is extensively discussed with the help of numerous tables. Appendices contain flow charts and definitions of variables to help a programmer unfamiliar with the programs to alter them with a minimum of lost time. 12 figures, 17 tables.

  15. Mass spectrometric imaging of flavonoid glycosides and biflavonoids in Ginkgo biloba L.

    Science.gov (United States)

    Beck, Sebastian; Stengel, Julia

    2016-10-01

    Ginkgo biloba L. is known to be rich in flavonoids and flavonoid glycosides. However, the distribution within specific plant organs (e.g. within leaves) is not known. By using HPLC-MS and MS/MS we have identified a number of previously known G. biloba flavonoid glycosides and biflavonoids from leaves. Namely, kaempferol, quercetin, isorhamnetin, myricetin, laricitrin/mearnsetin and apigenin glycosides were identified. Furthermore, biflavonoids like ginkgetin/isoginkgetin were also detected. The application of MALDI mass spectrometric imaging, enabled the compilation of concentration profiles of flavonoid glycosides and biflavonoids in G. biloba L. leaves. Both, flavonoid glycosides and biflavonoids show a distinct distribution in leaf thin sections of G. biloba L. Copyright © 2016 Elsevier Ltd. All rights reserved.

  16. Quantitative Mass Spectrometric Analysis and Post-Extraction Stability Assessment of the Euglenoid Toxin Euglenophycin

    Directory of Open Access Journals (Sweden)

    Paul V. Zimba

    2013-09-01

    Full Text Available Euglenophycin is a recently discovered toxin produced by at least one species of euglenoid algae. The toxin has been responsible for several fish mortality events. To facilitate the identification and monitoring of euglenophycin in freshwater ponds, we have developed a specific mass spectrometric method for the identification and quantitation of euglenophycin. The post-extraction stability of the toxin was assessed under various conditions. Euglenophycin was most stable at room temperature. At 8 °C there was a small, but statistically significant, loss in toxin after one day. These methods and knowledge of the toxin’s stability will facilitate identification of the toxin as a causative agent in fish kills and determination of the toxin’s distribution in the organs of exposed fish.

  17. Mass Spectrometric Calibration of Controlled Fluoroform Leak Rate Devices Technique and Uncertainty Analysis

    CERN Document Server

    Balsley, S D; Laduca, C A

    2003-01-01

    Controlled leak rate devices of fluoroform on the order of 10 sup - sup 8 atm centre dot cc sec sup - sup 1 at 25 C are used to calibrate QC-1 War Reserve neutron tube exhaust stations for leak detection sensitivity. Close-out calibration of these tritium-contaminated devices is provided by the Gas Dynamics and Mass Spectrometry Laboratory, Organization 14406, which is a tritium analytical facility. The mass spectrometric technique used for the measurement is discussed, as is the first principals calculation (pressure, volume, temperature and time). The uncertainty of the measurement is largely driven by contributing factors in the determination of P, V and T. The expanded uncertainty of the leak rate measurement is shown to be 4.42%, with a coverage factor of 3 (k=3).

  18. MASS SPECTROMETRIC ANALYSIS FOR THE IDENTIFICATION OF THUNNUS GENUS FOUR SPECIES

    Directory of Open Access Journals (Sweden)

    T. Pepe

    2011-01-01

    Full Text Available An accurate identification of similar fish species is necessary to prevent illegal substitution and is imposed by labeling regulations in UE countries (1. The genus Thunnus comprises many species of different quality and commercial value. The increasing trade of fish preparations of the species included in this genus and the consequent loss of the external anatomical and morphological features enables fraudulent substitutions. This study reports data relating to the proteomic analysis of four tuna species (T. thynnus, T. alalunga, T. albacares, T. obesus. Sarcoplasmic proteins were studied by mono and two dimensional electrophoresis. The most significant proteins for the characterization of the species were analyzed by mass spectrometric techniques. As reported in a previous study (2, an accurate identification of the species seems possible, owing to the polymorphism displayed by the species of the Thunnus genus.

  19. Terverticillate Penicillia studied by direct electrospray mass spectrometric profiling of crude extracts: I. Chemosystematics

    DEFF Research Database (Denmark)

    Smedsgaard, Jørn; Frisvad, Jens Christian

    1997-01-01

    A chemosystematic study of 339 isolates from all known terverticillate Penicillium taxa was performed using electrospray mass spectrometric analysis of extractable metabolites. The mass profiles were made by injecting crude plug extracts made from cultures grown on Czapek Yeast Autolysate agar (CYA......) and Yeast Extract Sucrose agar (YES) directly into the electrospray source of the mass spectrometer. A data matrix was made from each substrate by transferring the complete centroid mass spectrum from 200 to 700 amu as 501 variables to individual columns. No attempt was made to identify ions in the mass...... dominated by a single intense ion together, whereas logarithmized data revealed finer detail but with a shorter distance between clusters. The overall results showed that substantial taxonomic information can be extracted from mass profiles even when the identity of ions is unknown. ions corresponding...

  20. Standard test methods for chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of uranium hexafluoride

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2011-01-01

    1.1 These test methods cover procedures for subsampling and for chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of uranium hexafluoride UF6. Most of these test methods are in routine use to determine conformance to UF6 specifications in the Enrichment and Conversion Facilities. 1.2 The analytical procedures in this document appear in the following order: Note 1—Subcommittee C26.05 will confer with C26.02 concerning the renumbered section in Test Methods C761 to determine how concerns with renumbering these sections, as analytical methods are replaced with stand-alone analytical methods, are best addressed in subsequent publications. Sections Subsampling of Uranium Hexafluoride 7 - 10 Gravimetric Determination of Uranium 11 - 19 Titrimetric Determination of Uranium 20 Preparation of High-Purity U3O 8 21 Isotopic Analysis 22 Isotopic Analysis by Double-Standard Mass-Spectrometer Method 23 - 29 Determination of Hydrocarbons, Chlorocarbons, and Partially Substitut...

  1. Mass spectrometric identification of proteins and characterization of their post-translational modifications in proteome analysis

    DEFF Research Database (Denmark)

    Roepstorff, P; Larsen, Martin Røssel

    2001-01-01

    for more than 425.000 protein sequences. However, the cellular functions are determined by the set of proteins expressed in the cell--the proteome. Two-dimensional gel electrophoresis, mass spectrometry and bioinformatics have become important tools in correlating the proteome with the genome. The current......High-throughput DNA sequencing has resulted in increasing input in protein sequence databases. Today more than 20 genomes have been sequenced and many more will be completed in the near future, including the largest of them all, the human genome. Presently, sequence databases contain entries...... dominant strategies for identification of proteins from gels based on peptide mass spectrometric fingerprinting and partial sequencing by mass spectrometry are described. After identification of the proteins the next challenge in proteome analysis is characterization of their post...

  2. Electron ionization mass spectrometric analysis of air- and moisture-sensitive organometallic compounds.

    Science.gov (United States)

    Penafiel, Johanne; Hesketh, Amelia V; Granot, Ori; Scott McIndoe, J

    2016-10-04

    Electron ionization (EI) is a reliable mass spectrometric method for the analysis of the vast majority of thermally stable and volatile compounds. In direct EI-MS, the sample is placed into the probe and introduced to the source. For air- and moisture-sensitive organometallic complexes, the sample introduction step is critical. A small quantity must be briefly exposed to the atmosphere, during which time decomposition can occur. Here we present a simple tool that allows convenient analysis of air- and moisture-sensitive organometallic species by direct probe methods: a small purge-able glove chamber affixed to the front end of the mass spectrometer. Using the upgraded mass spectrometer, we successfully characterized a series of air- and moisture-sensitive organometallic complexes, ranging from mildly to very air-sensitive.

  3. Sr isotope geochemistry of East Alpine mineral deposits and mass spectrometric analyses of fluid inclusions

    International Nuclear Information System (INIS)

    Grum, W.

    1995-05-01

    Strontium isotope geochemistry and deformational history of selected carbonate-hosted deposits from different tectonic positions in the Eastern Alps were studied. In this context an equipment has been constructed to analyze the composition of volatile components of fluid inclusions (FI). Based on the results of Sr-isotopic investigations two groups of deposits are discriminated: Deposits formed by formation waters and/or metamorphogenic fluids: Tux (magnesite, scheelite), Otterzug (barite), Lassing (magnesite), Rabenwald (talc), Laussa and Mooseck (fluorite). The mineralizing fluids are derived from different sedimentary rock series and therefore 87 Sr/ 86 Sr-ratios vary between 0.707 and 0.719. Deposits situated along fault zones: Lassing (talc), Gasteiner Tal (Silberpfennig area; gold), Schlaining (stibnite) and Waldenstein (specularite). Sr isotope ratios of the mineralizing fluids from Lassing, Waldenstein and Schlaining ranges from 0.7112 to 0.7127 and are therefore thought to have scavenged the East Alpine crystalline. The mineralizing solutions of the Gasteiner Tal deposit may either have equilibrated with low radiogenic sedimentary or with (ultra-)basic rocks. A cracking chamber has been constructed in order to open FI by cracking for mass spectrometric analysis of volatile components. Gases are analysed using a quadrupole mass spectrometer. The desorption of gas from metal and sample surfaces during cracking can be neglected. The amount of gas released from the mineral lattices was studied. With that fast method ore bearing from barren host rocks have been distinguished by different composition of the FI at the Brixlegg barite mineralization (Eastern Alps). Within the Galway fluorite deposit (Ireland) different fluids were involved and mass spectrometric analysis were carried out to characterize these different fluids and to identify their origin. (author)

  4. GNU polyxmass: a software framework for mass spectrometric simulations of linear (bio-polymeric analytes

    Directory of Open Access Journals (Sweden)

    Rusconi Filippo

    2006-04-01

    Full Text Available Abstract Background Nowadays, a variety of (bio-polymers can be analyzed by mass spectrometry. The detailed interpretation of the spectra requires a huge number of "hypothesis cycles", comprising the following three actions 1 put forth a structural hypothesis, 2 test it, 3 (invalidate it. This time-consuming and painstaking data scrutiny is alleviated by using specialized software tools. However, all the software tools available to date are polymer chemistry-specific. This imposes a heavy overhead to researchers who do mass spectrometry on a variety of (bio-polymers, as each polymer type will require a different software tool to perform data simulations and analyses. We developed a software to address the lack of an integrated software framework able to deal with different polymer chemistries. Results The GNU polyxmass software framework performs common (bio-chemical simulations–along with simultaneous mass spectrometric calculations–for any kind of linear bio-polymeric analyte (DNA, RNA, saccharides or proteins. The framework is organized into three modules, all accessible from one single binary program. The modules let the user to 1 define brand new polymer chemistries, 2 perform quick mass calculations using a desktop calculator paradigm, 3 graphically edit polymer sequences and perform (bio-chemical/mass spectrometric simulations. Any aspect of the mass calculations, polymer chemistry reactions or graphical polymer sequence editing is configurable. Conclusion The scientist who uses mass spectrometry to characterize (bio-polymeric analytes of different chemistries is provided with a single software framework for his data prediction/analysis needs, whatever the polymer chemistry being involved.

  5. Increased Protein Structural Resolution from Diethylpyrocarbonate-based Covalent Labeling and Mass Spectrometric Detection

    Science.gov (United States)

    Zhou, Yuping; Vachet, Richard W.

    2012-04-01

    Covalent labeling and mass spectrometry are seeing increased use together as a way to obtain insight into the 3-dimensional structure of proteins and protein complexes. Several amino acid specific (e.g., diethylpyrocarbonate) and non-specific (e.g., hydroxyl radicals) labeling reagents are available for this purpose. Diethylpyrocarbonate (DEPC) is a promising labeling reagent because it can potentially probe up to 30% of the residues in the average protein and gives only one reaction product, thereby facilitating mass spectrometric analysis. It was recently reported, though, that DEPC modifications are labile for some amino acids. Here, we show that label loss is more significant and widespread than previously thought, especially for Ser, Thr, Tyr, and His residues, when relatively long protein digestion times are used. Such label loss ultimately decreases the amount of protein structural information that is obtainable with this reagent. We find, however, that the number of DEPC modified residues and, thus, protein structural information, can be significantly increased by decreasing the time between the covalent labeling reaction and the mass spectrometric analysis. This is most effectively accomplished using short (e.g., 2 h) proteolytic digestions with enzymes such as immobilized chymotrypsin or Glu-C rather than using methods (e.g., microwave or ultrasonic irradiation) that accelerate proteolysis in other ways. Using short digestion times, we show that the percentage of solvent accessible residues that can be modified by DEPC increases from 44% to 67% for cytochrome c, 35% to 81% for myoglobin, and 76% to 95% for β-2-microglobulin. In effect, these increased numbers of modified residues improve the protein structural resolution available from this covalent labeling method. Compared with typical overnight digestion conditions, the short digestion times decrease the average distance between modified residues from 11 to 7 Å for myoglobin, 13 to 10 Å for

  6. Reply to "On Vaporization of liquid Pb-Li eutectic alloy from 1000 K to 1200 K- A high temperature mass spectrometric study"

    Science.gov (United States)

    Jain, Uttam; Mukherjee, Abhishek

    2018-03-01

    This communication is in response to a letter to editor commenting on the authors' earlier paper "Vaporization of liquid Pb-Li eutectic alloy from 1000 K to 1200 K - A high temperature mass spectrometric study".

  7. Partial vapor-phase hydrolysis of peptide bonds: A method for mass spectrometric determination of O-glycosylated sites in glycopeptides

    DEFF Research Database (Denmark)

    Mirgorodskaya, E; Hassan, H; Wandall, H H

    1999-01-01

    In this study we present a method for determination of O-glycosylation sites in glycopeptides, based on partial vapor-phase acid hydrolysis in combination with mass spectrometric analysis. Pentafluoropropionic acid and hydrochloric acid were used for the hydrolysis of glycosylated peptides....... The reaction conditions were optimized for efficient polypeptide backbone cleavages with minimal cleavage of glycosidic bonds. The glycosylated residues were identified by mass spectrometric analysis of the hydrolytic cleavage products. Although glycosidic bonds are partially cleaved under acid hydrolysis...

  8. A potentiometric and spectrophotometric study on acid-base equilibria in ethanol-aqueous solution of acetazolamide and related compounds.

    Science.gov (United States)

    Chufán, E E; Suvire, F D; Enriz, R D; Pedregosa, J C

    1999-07-12

    Acid-base equilibria in ethanol-aqueous solution of 5-acetamido-1,3,4-thiadiazole-2-sulfonamide (acetazolamide, H(2)acm), 5-tertbutyloxycarbonylamido-1,3,4-thiadiazole-2-sulfonamide (B-H(2)ats), 5-amino-1,3,4-thiadiazole-2-sulfonamide (Hats) and 5-amino-1,3,4-thiadiazole-2-thiol (Hatm) at 25 degrees C, 0.15 mol dm(-3) ionic strength (NaNO(3)), have been investigated by potentiometry and UV spectrophotometry. The ionization constants were calculated with SUPERQUAD program from potentiometric measurements and by a method according to Edsall et al. using the mole fractions determined by complementary tri-stimulus colorimetry (CTS). The constants obtained by potentiometry were: B-H(2)ats, pk(a(1))=7.33(3) and pk(a(2))=9.27(1); Hats, pk(a(1))=2.51(3) and pk(a(2))=8.49(1); Hatm, pk(a(1))=1.92(1) and pk(a(2))=6.81(1); whereas the constants determined by spectrophotometry were: H(2)acm, pk(a(1))=7.78(1) and pk(a(2))=9.57(2); B-H(2)ats, pk(a(1))=7.71(2) and pk(a(2))=9.61(2); Hats, pk(a(1))=2.19(3) and pk(a(2))=8.61(2); Hatm, pk(a(2))=6.90(2). Theoretical calculations using MO semiempirical and ab-initio RHF/6-31G* computations for the compounds were also performed. It was possible to clarify the preferred deprotonation mechanism of acetazolamide and B-H(2)ats in which the first deprotonation takes place at the carbonamido group.

  9. Tripodal (N-alkylated) CMP(O) and malonamide ligands: synthesis, extraction of metal ions, and potentiometric studies

    International Nuclear Information System (INIS)

    Janczewski, D.; Reinhoudt, D.N.; Verboom, W.; Malinowska, E.; Pietrzak, M.; Hill, C.; Allignol, C.

    2007-01-01

    Tripodal ligands build on the C-pivot (9b-e, 13b-d, and 17a-d) and tri-alkyl-benzene platforms (10a,b, 11, 12, 14a,b, and 18a,b) bearing (N-alkylated) carbamoyl-methyl-phosphine oxide (CMPO), carbamoyl-methyl-phosphonate (CMP), and malonamide moieties were synthesized. Extraction studies with Am 3+ and Eu 3+ show that in general there is a positive influence of the N-alkyl substituents in C-pivot CMP(O) ligands on the D(distribution) coefficients. The tri-alkyl-benzene CMPO ligands 10a,b, 11, and 12 have considerably larger D coefficients than the corresponding C-pivot analogues 9a-e, although hardly having any selectivity, while N-alkylation gives rise to smaller D coefficients. Although less effective the extraction behavior of the C-pivot CMP analogues 13b-d shows more or less the same trend as the corresponding CMPO ligands 9b-e upon substitution of the carboxamide N-atom with different alkyl chains. The different malonamide ligands 17a-d and 18a,b are bad extractants, while N-alkylation makes them even worse. Potentiometric studies of CMP(O) and malonamide ligands in polymeric membranes on Pb 2+ , Cu 2+ , Ca 2+ , Mg 2+ , Na + , and K + salts revealed that N-alkyl substituents increase the stability constants of ion-ionophore complexes compared to unsubstituted ligands. In polymeric membrane electrodes the ligands induce a selectivity pattern that differs significantly from the so-called Hofmeister series, giving the highest selectivity coefficients for UO 2 2+ among all examined cations (Pb 2+ , Cu 2+ , Ca 2+ , Mg 2+ , Na + , K + ). (authors)

  10. Real-time potentiometric sensor; an innovative tool for monitoring hydrolysis of chemo/bio-degradable drugs in pharmaceutical sciences.

    Science.gov (United States)

    Ma'mun, Ahmed; Abd El-Rahman, Mohamed K; Abd El-Kawy, Mohamed

    2018-05-30

    In recent years, the whole field of ion-selective electrodes(ISEs) in pharmaceutical sciences has expanded far beyond its original roots. The diverse range of opportunities offered by ISEs was broadly used in a number of pharmaceutical applications, with topics presented ranging from bioanalysis of drugs and metabolites, to protein binding studies, green analytical chemistry, impurity profiling, and drug dissolution in biorelevant media. Inspired from these advances and with the aim of extending the functional capabilities of ISEs, the primary focus of the present paper is the utilization of ISE as a tool in personalized medicine. Given the opportunity to explore biological events in real-time (such as drug metabolism) could be central to personalized medicine. (ATR) is a chemo-degradable and bio-degradable pharmaceutically active drug. Laudanosine (LDS) is the major degradation product and metabolite of ATR and is potentially toxic and reported to possess epileptogenic activity which increases the risk of convulsive effects. In this work, ATR have been subjected to both chemical and biological hydrolysis, and the course of the reactions is monitored by means of a ISE. In this study, we have designed an efficient real-time tracking strategy which substantially resolve the challenges of the ATR chemical and biological degradation kinetics. By utilizing a potentiometric sensor, tracking of ATR chemical and biological degradation kinetics can be performed in a very short time with excellent accuracy. The LOD was calculated to be 0.23 μmol L -1 , the potential drift was investigated over a period of 60 min and the value was 0.25 mV h -1 . Real serum samples for measurement the rate of in vitro metabolism of ATR was performed. Furthermore, a full description of the fabricated screen-printed sensor was presented. Copyright © 2018 Elsevier B.V. All rights reserved.

  11. Scanning electrochemical microscopy: using the potentiometric mode of SECM to study the mixed potential arising from two independent redox processes.

    Science.gov (United States)

    Serrapede, Mara; Denuault, Guy; Sosna, Maciej; Pesce, Giovanni Luca; Ball, Richard J

    2013-09-03

    This study demonstrates how the potentiometric mode of the scanning electrochemical microscope (SECM) can be used to sensitively probe and alter the mixed potential due to two independent redox processes provided that the transport of one of the species involved is controlled by diffusion. This is illustrated with the discharge of hydrogen from nanostructured Pd hydride films deposited on the SECM tip. In deareated buffered solutions the open circuit potential of the PdH in equilibrium between its β and α phases (OCP(β→α)) does not depend on the tip-substrate distance while in aerated conditions it is found to be controlled by hindered diffusion of oxygen. Chronopotentiometric and amperometric measurements at several tip-substrate distances reveal how the flux of oxygen toward the Pd hydride film determines its potential. Linear sweep voltammetry shows that the polarization resistance increases when the tip approaches an inert substrate. The SECM methodology also demonstrates how dissolved oxygen affects the rate of hydrogen extraction from the Pd lattice. Over a wide potential window, the highly reactive nanostructure promotes the reduction of oxygen which rapidly discharges hydrogen from the PdH. The flux of oxygen toward the tip can be adjusted via hindered diffusion. Approaching the substrate decreases the flux of oxygen, lengthens the hydrogen discharge, and shifts OCP(β→α) negatively. The results are consistent with a mixed potential due to the rate of oxygen reduction balancing that of the hydride oxidation. The methodology is generic and applicable to other mixed potential processes in corrosion or catalysis.

  12. Synthesis, spectroscopic identification, thermal, potentiometric and antibacterial activity studies of 4-amino-5-mercapto-S-triazole Schiff's base complexes

    Science.gov (United States)

    Alaghaz, Abdel-Nasser M. A.; Zayed, Mohamed E.; Alharbi, Suliman A.; Ammar, Reda A. A.; Chinnathambi, Arunachalam

    2015-05-01

    Complexes of manganese(II), cobalt(II), nickel(II), copper(II) and zinc(II) of general composition [M(L)2] have been synthesized [L = 4-pyridin-2-yl-methylene amino-4H-1,2,4-triazole-3-thiol]. The elemental analyses, molar conductance, spectral (IR, UV-Vis, 1H NMR, mass), magnetic moment and thermal measurements studies of the compounds led to the conclusion that the ligand acts as a tridentate manner (SNN). The molar conductance of the metal complexes in fresh solution of DMSO lies in the range of 8.34-10.46 Ω-1 cm2 mol-1 indicating their non-electrolytic behavior. On the basis of analytical and spectroscopic techniques, octahedral geometry of the complexes was proposed. The Schiff base acts as tridentate ligand coordinated through deprotonated thiolic sulfur, azomethine nitrogen and pyridine nitrogen atoms. The ligand field parameters were calculated for Co(II), Ni(II) and Cu(II) complexes and their values were found in the range reported for a octahedral structure. The data show that the complexes have composition of ML2 type. The activation of thermodynamic parameters are calculated using Coast-Redfern, Horowitz-Metzger (HM), Piloyan-Novikova (PN) and Broido's equations. Protonation constants of Schiff base and stability constants of their binary metal complexes have been determined potentiometrically in 50% DMSO-water media at 25 °C and ionic strength 0.10 M potassium nitrate. Both the Schiff's base ligand and its complexes have been screened for antibacterial activities.

  13. All-solid-state potentiometric sensors for ascorbic acid by using a screen-printed compatible solid contact

    International Nuclear Information System (INIS)

    Veltsistas, Panayotis G.; Prodromidis, Mamas I.; Efstathiou, Constantinos

    2004-01-01

    The development of all-solid-state potentiometric ion selective electrodes for monitoring of ascorbic acid, by using a screen-printed compatible solid contact is described. The applied methodology is based on the use of PVC membrane modified with some firstly-tested ionophores (triphenyltin(IV)chloride, triphenyltin(IV)hydroxide and palmitoyl-L-ascorbic acid) and a novel one synthesized in our laboratory (dibutyltin(IV) diascorbate). Synthesis protocol and some preliminary identification studies are given. A conductive graphite-based polymer thick film ink was used as an internal solid contact between the graphite electrode and the PVC membrane. The presence and the nature of the solid contact (plain or doped with lanthanum 2,6-dichlorophenolindophenol (DCPI)) seem to enhance the analytical performance of the electrodes in terms of sensitivity, dynamic range, and response time. The analytical performance of the constructed electrodes was evaluated with potentiometry, constant-current chronopotentiometry and electrochemical impedance spectroscopy (EIS). The interference effect of various compounds was also tested. The potential response of the optimized Ph 3 SnCl-based electrode was linear against ascorbic acid concentration range 0.005-5.0 mM. The applicability of the proposed sensors in real samples was also tested. The detection limit was 0.002 mM ascorbic acid (50 mM phosphate, pH 5 in 50 mM KCl). The slope of the electrodes was super-Nernstian and pH dependent, indicating a mechanism involving a combination of charge transfer and ion exchange processes. Fabrication of screen-printed ascorbate ISEs has also been demonstrated

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

    International Nuclear Information System (INIS)

    Campiglio, A.

    1985-01-01

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

  15. Antibody Biomimetic Material Made of Pyrrole for CA 15-3 and Its Application as Sensing Material in Ion-Selective Electrodes for Potentiometric Detection

    Directory of Open Access Journals (Sweden)

    Alexandra R. T. Santos

    2018-01-01

    Full Text Available This work reports a very simple approach for creating a synthetic antibody against any protein of interest and its application in potentiometric transduction. The selected protein was Breast Cancer Antigen (CA 15-3, which is implicated in breast cancer disease and used to follow-up breast cancer patients during treatment. The new material with antibody-like properties was obtained by molecular-imprinting technology, prepared by electropolymerizing pyrrol (Py, 5.0 × 10−3 mol/L around Breast Cancer Antigen (CA 15-3 (100 U/mL on a fluorine doped tin oxide (FTO conductive glass support. Cyclic voltammetry was employed for this purpose. All solutions were prepared in 4-(2-Hydroxyethyl-1-piperazineethanesulfonic acid (HEPES buffer, of pH 6.5. The biomarker was removed from the imprinted sites by chemical action of ethanol. The biomimetic material was then included in poly vinyl chloride (PVC plasticized membranes to act as potentiometric ionophore, having or not a lipophilic ionic additive added. The corresponding selective electrodes were evaluated by calibration curves (in buffer and in synthetic serum and by selectivity testing. The best analytical performance was obtained by selective electrodes including the plastic antibody and no lipophilic additive. The average limits of detection were 1.07 U/mL of CA 15-3, with a linear response from 1.44 to 13.2 U/mL and a cationic slope of 44.5 mV/decade. Overall, the lipophilic additives yielded no advantage to the overall potentiometric performance. The application of the MIP-based electrodes to the analysis of spiked synthetic serum showed precise and accurate results.

  16. Optimization of the thickness of a conducting polymer, polyaniline, deposited on the surface of poly(vinyl chloride) membranes: a new way to improve their potentiometric response.

    Science.gov (United States)

    Shishkanova, T V; Matejka, P; Král, V; Sedenková, I; Trchová, M; Stejskal, J

    2008-08-29

    Repeated depositions of polyaniline (PANI) have been used to control the thickness of the polymeric film deposited on poly(vinyl chloride) (PVC) membrane surface. The oxidation of aniline was carried out in a dispersion mode, i.e. in the presence of poly(N-vinylpyrrolidone) (PVP). Two kinds of PVC were used for this purpose: a non-plasticized PVC for the study of PANI deposition and PVC, plasticized with nitrophenyl octyl ether (NPOE), as a prototype of a liquid membrane electrode. The results of UV-visible and FTIR spectroscopies and electron microscopy showed that (1) the film thickness increased by about equal increments of approximately 40 nm after each polymerization, and (2) the interface with PVC was constituted by PANI film and adhering PANI-PVP colloidal particles. The various thicknesses of the deposited PANI films affected the potentiometric response of the NPOE/PVC membrane with and without an anion-exchanger. The potentiometric anionic response was observed with a minimal thickness of PANI film on the blank NPOE/PVC membrane. Sensitivity of the PANI film to pH occurred only with a blank NPOE/PVC membrane coated with a thick polymeric film, while it was strongly suppressed by the presence of a lipophilic anion-exchanger, tridodecylmethylammonium chloride (TDDMACl), in the membrane, regardless of the thickness of the polymer film. The thickness of the PANI film did not affect the anionic selectivity pattern of TDDMACl-based membranes to any great extent, but its presence improved and stabilized their potentiometric characteristics (sensitivity, linear-response range).

  17. Label-free Detection of Microcystin-LR in Waters Using Real-Time Potentiometric Biosensors Based on Single-Walled Carbon Nanotubes Imprinted Polymers

    OpenAIRE

    Queirós, Raquel B.; Noronha, João P. C.; Marques, P.V.S.; Sales, M. Goreti F.

    2012-01-01

    Microcystin-LR (MC-LR) is a dangerous toxin found in environmental waters, quantified by high performance liquid chromatography and/or enzyme-linked immunosorbent assays. Quick, low cost and on-site analysis is thus required to ensure human safety and wide screening programs. This work proposes label-free potentiometric sensors made of solid-contact electrodes coated with a surface imprinted polymer on the surface of Multi-Walled Carbon NanoTubes (CNTs) incorporated in a polyvinyl chloride me...

  18. Simultaneous determination of trace-levels of alloying zinc and copper by semi-mercury-free potentiometric stripping analysis with chemometric data treatment

    DEFF Research Database (Denmark)

    Andersen, Jens Enevold Thaulov; Hansen, Elo Harald

    1998-01-01

    Assays of copper and zinc in brass samples were performed by Semi-Mercury Free Potentiometric Stripping Analysis (S-MF PSA) using a thin-film mercury covered glassy-carbon working electrode and dissolved oxygen as oxidizing agent during the stripping step. The stripping peak transients were resol...... by factors in the range 2.104 - 5.105 which resulted in quantification of the copper and of zinc contents comparable to the specified values within 10%. On the basis of the chemometric treatment, an empirical expression is deduced relating the stripping time to the recorded potential....

  19. Potentiometric study of rhenium (V) complex formation with 4-methyl-1.2.4-triazol thiol-5 in the medium of 7 mol/l HBr

    International Nuclear Information System (INIS)

    Amindzhanov, A.A.; Safarmamadov, S.M.

    1992-01-01

    Present article is devoted to potentiometric study of rhenium (V) complex formation with 4-methyl-1.2.4-triazol thiol-5 in the medium of 7 mol/l HBr. The function of formation of oxo bromine-4-methyl-1.2.4-triazol thiol complexes of rhenium (V) in the medium of 5 mol/l HBr at 273 K temperature was determined. The function of formation of oxo bromine-4-methyl-1.2.4-triazol thiol complexes of rhenium (V) in the medium of 5 mol/l HBr at 298 K temperature was determined as well.

  20. Comparison of accelerator mass spectrometric measurement with liquid scintillation counting measurement for the determination of 14C in environmental samples

    International Nuclear Information System (INIS)

    Yasuike, Kaeko; Yamada, Yoshimune; Amano, Hikaru

    2010-01-01

    The concentrations of organically-bound 14 C in tree-ring cellulose of a Japanese Black Pine grown in Shika-machi (37.0 deg. N, 136.8 deg. E) and those of a Japanese Cedar grown in Kanazawa (36.5 deg. N, 136.7 deg. E), Japan, were analyzed for the ring-years from 1989 to 1998 by the accelerator mass spectrometric measurement. The results were compared with those of the same samples analyzed by the liquid scintillation counting measurement to determine the reliability of liquid scintillation counting measurement. An important result of this study is that the sensitivity and reproducibility of accelerator mass spectrometric measurement was almost equal to that of liquid scintillation counting measurement.

  1. Standard test methods for chemical and mass spectrometric analysis of nuclear-grade gadolinium oxide (Gd2O3) powder

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2006-01-01

    1.1 These test methods cover procedures for the chemical and mass spectrometric analysis of nuclear-grade gadolinium oxide powders to determine compliance with specifications. 1.2 The analytical procedures appear in the following order: Sections Carbon by Direct CombustionThermal Conductivity C1408 Test Method for Carbon (Total) in Uranium Oxide Powders and Pellets By Direct Combustion-Infrared Detection Method Total Chlorine and Fluorine by Pyrohydrolysis Ion Selective Electrode C1502 Test Method for Determination of Total Chlorine and Fluorine in Uranium Dioxide and Gadolinium Oxide Loss of Weight on Ignition 7-13 Sulfur by CombustionIodometric Titration Impurity Elements by a Spark-Source Mass Spectrographic C761 Test Methods for Chemical, Mass Spectrometric, Spectrochemical,Nuclear, and Radiochemical Analysis of Uranium Hexafluoride C1287 Test Method for Determination of Impurities In Uranium Dioxide By Inductively Coupled Plasma Mass Spectrometry Gadolinium Content in Gadolinium Oxid...

  2. Study of the spectrometric performances of monolithic CdZnTe / CdTe gamma ray detectors

    International Nuclear Information System (INIS)

    Gros d'Aillon, E.

    2005-11-01

    Pixelated monolithic CdTe/CdZnTe semiconductor gamma ray detectors are brought to replace scintillation detectors for medical applications, notably for single photon emission computed tomography (SPECT). In addition to compactness, they present better spectrometric performances: energy resolution, detection efficiency, and spatial resolution. Moreover, the photons depth of interaction in the crystal can be measured. This work aimed in studying experimentally and by simulation the correlations between anodes pitch, material physic properties (resistivity and electron transport properties), and detectors spectrometric performances. We have compared several methods of measuring the photon interaction depth, and have obtained an energy resolution ranging from 1.7% to 7% at 122 keV, according to material, for 5 mm thick detectors. Charge sharing between adjacent anodes has been studied and a measured data processing is proposed. (author)

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

    OpenAIRE

    Abu Ghalwa, Nasser

    2012-01-01

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

  4. Topic model-based mass spectrometric data analysis in cancer biomarker discovery studies.

    Science.gov (United States)

    Wang, Minkun; Tsai, Tsung-Heng; Di Poto, Cristina; Ferrarini, Alessia; Yu, Guoqiang; Ressom, Habtom W

    2016-08-18

    A fundamental challenge in quantitation of biomolecules for cancer biomarker discovery is owing to the heterogeneous nature of human biospecimens. Although this issue has been a subject of discussion in cancer genomic studies, it has not yet been rigorously investigated in mass spectrometry based proteomic and metabolomic studies. Purification of mass spectometric data is highly desired prior to subsequent analysis, e.g., quantitative comparison of the abundance of biomolecules in biological samples. We investigated topic models to computationally analyze mass spectrometric data considering both integrated peak intensities and scan-level features, i.e., extracted ion chromatograms (EICs). Probabilistic generative models enable flexible representation in data structure and infer sample-specific pure resources. Scan-level modeling helps alleviate information loss during data preprocessing. We evaluated the capability of the proposed models in capturing mixture proportions of contaminants and cancer profiles on LC-MS based serum proteomic and GC-MS based tissue metabolomic datasets acquired from patients with hepatocellular carcinoma (HCC) and liver cirrhosis as well as synthetic data we generated based on the serum proteomic data. The results we obtained by analysis of the synthetic data demonstrated that both intensity-level and scan-level purification models can accurately infer the mixture proportions and the underlying true cancerous sources with small average error ratios (data, we found more proteins and metabolites with significant changes between HCC cases and cirrhotic controls. Candidate biomarkers selected after purification yielded biologically meaningful pathway analysis results and improved disease discrimination power in terms of the area under ROC curve compared to the results found prior to purification. We investigated topic model-based inference methods to computationally address the heterogeneity issue in samples analyzed by LC/GC-MS. We observed

  5. Mass spectrometric characterization of the selective androgen receptor modulator (SARM) YK-11 for doping control purposes.

    Science.gov (United States)

    Thevis, Mario; Piper, Thomas; Dib, Josef; Lagojda, Andreas; Kühne, Dirk; Packschies, Lars; Geyer, Hans; Schänzer, Wilhelm

    2017-07-30

    Selective androgen receptor modulators (SARMs) represent an emerging class of therapeutics targeting inter alia conditions referred to as cachexia and sarcopenia. Due to their anabolic properties, the use of SARMs is prohibited in sports as regulated by the World Anti-Doping Agency (WADA), and doping control laboratories test for these anabolic agents in blood and urine. In order to accomplish and maintain comprehensive test methods, the characterization of new drug candidates is critical for efficient sports drug testing. Hence, in the present study the mass spectrometric properties of the SARM YK-11 were investigated. YK-11 was synthesized according to literature data and three different stable-isotope-labeled analogs were prepared to support the mass spectrometric studies. Using high-resolution/high-accuracy mass spectrometry following electrospray ionization as well as electron ionization, the dissociation pathways of YK-11 were investigated, and characteristic features of its (product ion) mass spectra were elucidated. These studies were flanked by density functional theory (DFT) computation providing information on proton affinities of selected functional groups of the analyte. The steroidal SARM YK-11 was found to readily protonate under ESI conditions followed by substantial in-source dissociation processes eliminating methanol, acetic acid methyl ester, and/or ketene. DFT computation yielded energetically favored structures of the protonated species resulting from the aforementioned elimination processes particularly following protonation of the steroidal D-ring substituent. Underlying dissociation pathways were suggested, supported by stable-isotope labeling of the analyte, and diagnostic product ions for the steroidal nucleus and the D-ring substituent were identified. Further, trimethylsilylated YK-11 and its deuterated analogs were subjected to electron ionization high-resolution/high-accuracy mass spectrometry, complementing the dataset characterizing

  6. High performance liquid chromatographic-mass spectrometric assay for the quantitation of BMS-204352 in dog K(3)EDTA plasma.

    Science.gov (United States)

    Yao, Ming; Mantha, Subbarao; Shah, Vinod R; Vachharajani, Nimish N; Arnold, Mark E; Pursley, Janice M; Srinivas, Nuggehally R

    2002-05-01

    A high performance liquid chromatographic-mass spectrometric (LC/MS) assay was developed and validated for the determination of BMS-204352 in dog K(3)EDTA plasma. A 0.5 mL aliquot of control plasma was spiked with BMS-204352 and internal standard (IS) and buffered with 1 mL of 5 mM ammonium acetate. The mixture was then extracted with 3 mL of toluene. After separation and evaporation of the organic phase to dryness using nitrogen at 40 degrees C, the residue was reconstituted in the mobile phase and 25 microL of the sample were injected onto a Hypersil C(18) column (2 x 50 mm; 3 microm) at a flow rate of 0.5 mL/min. The mobile phase was consisted of two solvent mixtures (A and B). Solvent A was composed of 5 mM ammonium acetate and 0.1% triethylamine in 75:25 v/v water:methanol, pH adjusted to 5.5 with glacial acetic acid, and solvent B was 5 mM ammonium acetate in methanol. A linear gradient system was used to elute the analytes. The mass spectrometer was programmed to admit the de-protonated molecules at m/z 352.7 (IS) and m/z 357.9 (BMS-204352). Standard curves of BMS-204352 were linear (r(2) > or = 0.998) over the concentration range of 0.5-1000 ng/mL. The mean predicted quality control (QC) concentrations deviated less than 5.1% from the corresponding nominal values (ie 4, 80, 400 and 2000 ng/mL); the within- and between-assay precision of the assay were within 5.5% relative standard deviation. Stability of BMS-204352 was confirmed after at least three freeze/thaw cycles and BMS-204532 was stable in dog plasma when stored frozen at or below -20 degrees C for at least 16 weeks in spiked QC samples and for at least 4 1/2 weeks for in vivo study samples. BMS-204352 and IS were stable in the injection solvent at room temperature for at least 24 h. The assay was applied to delineate the pharmacokinetic disposition of BMS-204352 in dogs following a single intravenous dose administration. In conclusion, the assay is accurate, precise, specific, sensitive and

  7. A spectrometrical method to measure the deuterium content in 2H-enriched water

    International Nuclear Information System (INIS)

    Dumke, I.

    1980-04-01

    A test method and spectrometer has been developed for emission-spectrometrical measurement of the deuterium content in water enriched with deuterium. The water sample is melted into a previously evacuated glas tube and a gas discharge is excited in vapour over the cooled sample to adjust to a low vapour pressure with high frequency. The intensities of the H(α) and D(α) lines appearing in the spectrum determine the D-content. Both lines were resolved by a Fabry-Perot interferometer and geometrically separated fed to two photodetectors. The remaining spectrum is filtered off. Following electronic calculation of the signals, the measured value is indicated which has to be corrected by a standard curve. The relative measuring accuracy is about +-1% for enrichments of over 1% D and less than +-5% in the region of 0.3-1% D. The detection limit is about 0.03% D (sample amount: 50 μl, average of 5 samples). (orig./HP) [de

  8. Determination of ractopamine in pig hair using liquid chromatography with tandem mass spectrometric detection.

    Science.gov (United States)

    Wu, Junlin; Liu, Xiaoyun; Peng, Yunping

    2014-01-01

    A quantitative analytical procedure for the determination of ractopamine in pig hair has been developed and validated. The hair samples were washed and incubated at 75°C with isoxuprine and hair extraction buffer. The drug present was quantified using mixed solid-phase extraction and liquid chromatography with tandem mass spectrometric detection. The limit of quantization (LOQ) was 10pg/mg and the intra-day precision at 25pg/mg and 750pg/mg was 0.49% and 2.8% respectively. Inter-day precision was 0.88% and 3.52% at the same concentrations. The hair extraction percentage recovery at 25pg/mg and 50ng/mL was 99.47% and 103.83% respectively. The extraction percentage recovery at 25pg/mg and 50ng/mg was 93.52% and 100.26% respectively. Our results showed that ractopamine residues persist in hair in 24days of withdrawal and also showed the possibility to test ractopamine from pig hair samples. Copyright © 2014 Elsevier Inc. All rights reserved.

  9. Synoptic view of the different domains of application of airborne radiometric and spectrometric surveys in egypt

    International Nuclear Information System (INIS)

    Fouad, K.M.

    1998-01-01

    Airborne radiometric survey has been applied for more than three decades in egypt. Experience gained from the acquired data over different geological environments has revealed the importance of this geophysical tool in: 1. disclosure of anomalies of potential uranium deposits, 2. geological mapping, 3. environmental monitoring of natural radiometric background around nuclear facilities, as well as the detection of nuclear fallout resulting from local or foreign nuclear activities. The advent of recording of the discriminated gamma ray energies in the airborne 256-channel spectrometer has eventually resulted in the quantitative detection of uranium, thorium, and potassium and their elemental ratios in the rocks. This has greatly widened the scope of geophysical and geochemical application. When this type is coupled with airborne magnetometry, the geological and structural configuration is appreciably revealed in three dimensions. The important role played by the statistical method of analysis is also shown. Case histories from the eastern desert, and sinai peninsula, are exhibited to help manifest the wide variety of applications of radiometric and spectrometric surveys

  10. Precise timing of the last interglacial period from mass spectrometric determination of thorium-230 in corals

    Science.gov (United States)

    Chen, J. H.; Wasserburg, G. J.; Ku, T.-L.; Edwards, R. Lawrence

    1987-01-01

    The development of mass spectrometric techniques for determination of Th-230 abundance has made it possible to reduce analytical errors in (U-238)-(U-234)-(Th-230) dating of corals even with very small samples. Samples of 6 x 10 to the 8th atoms of Th-230 can be measured to an accuracy of + or - 3 percent (2sigma), and 3 x 10 to the 10th atoms of Th-230 can be measured to an accuracy of + or - 0.2 percent. The time range over which useful age data on corals can be obtained now ranges from about 50 to about 500,000 years. For young corals, this approach may be preferable to C-14 dating. The precision with which the age of a coral can now be determined should make it possible to critically test the Milankovitch hypothesis concerning Pleistocene climate fluctuations. Analyses of a number of corals that grew during the last interglacial period yield ages of 122,000 to 130,000 years. The ages coincide with, or slightly post-date, the summer solar insolation high at 65 deg N latitude which occurred 128,000 years ago. This supports the idea that changes in Pleistocene climate can be the result of variations in the distribution of solar insolation caused by changes in the geometry of the earth's orbit and rotation axis.

  11. Determination of platinum originated from antitumoral drugs in human urine by atomic absorption spectrometric methods.

    Science.gov (United States)

    da Costa, Anilton Coelho; Vieira, Mariana Antunes; Luna, Aderval Severino; de Campos, Reinaldo Calixto

    2010-10-15

    Cisplatin and carboplatin are the most common platinum-based drugs used in cancer treatment. Pharmacokinetic investigations, the evaluation of the body burden during the treatment, as well as baseline levels of platinum in humans have attracted great interest. Thus, accurate analytical methods for fast and easy Pt monitoring in clinical samples become necessary. In the present study atomic absorption spectrometric methods for the determination of platinum in the forms of cisplatin and carboplatin in human urine were investigated. Platinum, in these different forms, could be determined in urine, after simple sample dilution. Regarding electrothermal atomic absorption spectrometry, the optimum parameters were defined by a central composite design optimization. Multiplicative matrix effects were overcome by using a mixture of HCl and NaCl as modifier. The limit of detection (LOD) was 0.004 mgL(-1) of platinum in the original sample. For the analysis of more concentrated samples, high resolution continuous source flame atomic absorption spectrometry was also investigated. Flame conditions were optimized by a multivariate D-optimal design, using as response the sum of the analyte addition calibration slopes and their standard deviations. Matrix matched external calibration with PtCl(2) calibration solutions, was possible, and the LOD was 0.06 mgL(-1) in the original sample. The results obtained by the proposed procedures were also in good agreement with those obtained by an independent comparative procedure. Copyright © 2010 Elsevier B.V. All rights reserved.

  12. Targeted selected reaction monitoring mass spectrometric immunoassay for insulin-like growth factor 1.

    Directory of Open Access Journals (Sweden)

    Eric E Niederkofler

    Full Text Available Insulin-like growth factor 1 (IGF1 is an important biomarker of human growth disorders that is routinely analyzed in clinical laboratories. Mass spectrometry-based workflows offer a viable alternative to standard IGF1 immunoassays, which utilize various pre-analytical preparation strategies. In this work we developed an assay that incorporates a novel sample preparation method for dissociating IGF1 from its binding proteins. The workflow also includes an immunoaffinity step using antibody-derivatized pipette tips, followed by elution, trypsin digestion, and LC-MS/MS separation and detection of the signature peptides in a selected reaction monitoring (SRM mode. The resulting quantitative mass spectrometric immunoassay (MSIA exhibited good linearity in the range of 1 to 1,500 ng/mL IGF1, intra- and inter-assay precision with CVs of less than 10%, and lowest limits of detection of 1 ng/mL. The linearity and recovery characteristics of the assay were also established, and the new method compared to a commercially available immunoassay using a large cohort of human serum samples. The IGF1 SRM MSIA is well suited for use in clinical laboratories.

  13. Mass-spectrometric investigation of complex sulfates of hafnium and ammonium

    International Nuclear Information System (INIS)

    Motov, D.L.; Sozinova, Yu.P.; Korobejnikov, L.S.

    1981-01-01

    In the 100-600 deg temperature range by means of mass-spectrometric investigation a thermal decomposition of complex sulphates of hafnium and ammonium: basic (NI 4 ) 2 Hf 2 O 3 (SO 4 ) 2 x2h 2 o(I), (NH 4 ) 2 Hf 2 O(SO 4 ) 4 x2H 2 O (2) and neutral (NH 4 ) 2 Hf(SO 4 ) 3 x2H 2 O (3), (NH 4 ) 4 xHf(SO 4 ) 4 x4H 2 O (4) is studied. It has been found that the coordinated water is more strongly bound in basic salts as compared with the neutral ones. As to water removal 1 is hydroxo-, 2 - oxocompound, in 3 water bonds are equivalent, in 4 -crystallohydrate water is removed in two stages. It is shown that the NH 4 and SO 4 bond strength decreases from basic to neutral salts. In investigated compounds the NH 4 - and SO 4 groups are more strongly bound than in ammonium sulphate that confirms the complex character of double hafnium ammonium sulfates [ru

  14. A Spectrometric Method for Hydrogen Peroxide Concentration Measurement with a Reusable and Cost-Efficient Sensor

    Directory of Open Access Journals (Sweden)

    Cheng-Chih Hsu

    2015-10-01

    Full Text Available In this study we developed a low cost sensor for measuring the concentration of hydrogen peroxide (H2O2 in liquids utilizing a spectrometric method. The sensor was tested using various concentrations of a peroxidase enzyme immobilized on a glass substrate. H2O2 can be catalyzed by peroxidase and converted into water and oxygen. The reagent 4-amino-phenazone takes up oxygen together with phenol to form a colored product that has absorption peaks at 510 nm and 450 nm. The transmission intensity is strongly related to the hydrogen peroxide concentration, so can be used for quantitative analysis. The measurement range for hydrogen peroxide is from 5 × 10−5% to 1 × 10−3% (0.5 ppm to 10 ppm and the results show high linearity. This device can achieve a sensitivity and resolution of 41,400 (photon count/% and 3.49 × 10−5% (0.35 ppm, respectively. The response time of the sensor is less than 3 min and the sensor can be reused for 10 applications with similar performance.

  15. Isolation and characterization of related substances in alogliptin benzoate by LC-QTOF mass spectrometric techniques.

    Science.gov (United States)

    Lu, Yuting; Yang, Danyi; Li, Zhiyu; Hang, Taijun; Song, Min

    2016-09-05

    A highly specific and efficient LC-QTOF mass spectrometric method was developed for the separation and characterization of process related substances and the major degradation products in alogliptin benzoate and its tablets. The separation was performed on Phenomenex Gemini-NX C18 column (250mm×4.6mm, 5μm) using 0.2% formic acid-0.2% ammonium acetate in water as mobile phase A, acetonitrile and methanol (60:40, v/v) as mobile phase B in linear gradient elution mode. Forced degradation studies were also conducted under ICH prescribed stress conditions. Alogliptin benzoate and its tablets were tending to degrade under acid, alkaline, oxidative and thermal stresses, while relatively stable to photolytic stress. A total of seven related substances were detected and characterized through liquid chromatography-high resolution QTOF mass spectrometry techniques, including process related substances and degradation products, and two of them were further synthesized and characterized by NMR spectroscopy. Based on the related substances elucidation and the plausible formation mechanisms, efficient approaches were proposed to reduce or eliminate related substances, and in consequence the quality of alogliptin benzoate and its tablets have been promoted obviously. Therefore, the impurity profiles obtained are critical to the quality control and manufacturing processes optimization and monitoring of alogliptin benzoate and its tablets. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Mass spectrometric investigation of neutral and charged constituents in saturated vapor over PrI3

    International Nuclear Information System (INIS)

    Motalov, V.B.; Vorobiev, D.E.; Kudin, L.S.; Markus, T.

    2009-01-01

    The Knudsen effusion mass spectrometric technique was used to study vapor species over praseodymium triiodide. The monomer, PrI 3 , and dimer, Pr 2 I 6 , molecules and the negative ions, PrI 4 - and Pr 2 I 7 - , were observed in saturated vapor in the temperature range from 856 K to 1048 K. The partial vapor pressures of neutral constituents were determined and the enthalpies of sublimation obtained using the second and the third laws of thermodynamics (Δ s H deg. (298.15 K) = 291 ± 4 kJ mol -1 for PrI 3 , and Δ s H deg. (298.15 K) = 400 ± 30 kJ mol -1 for Pr 2 I 6 ). The equilibrium constants for various ion molecular reactions were measured and the enthalpies of reactions obtained. The enthalpies of formation, Δ f H deg. (298.15 K) kJ mol -1 , of gaseous molecules and ions were calculated and are as follows: -374 ± 6 (PrI 3 ), -929 ± 30 (Pr 2 I 6 ), -867 ± 30 (PrI 4 - ), -1432 ± 50 (Pr 2 I 7 - )

  17. Quantum dots assisted laser desorption/ionization mass spectrometric detection of carbohydrates: qualitative and quantitative analysis.

    Science.gov (United States)

    Bibi, Aisha; Ju, Huangxian

    2016-04-01

    A quantum dots (QDs) assisted laser desorption/ionization mass spectrometric (QDA-LDI-MS) strategy was proposed for qualitative and quantitative analysis of a series of carbohydrates. The adsorption of carbohydrates on the modified surface of different QDs as the matrices depended mainly on the formation of hydrogen bonding, which led to higher MS intensity than those with conventional organic matrix. The effects of QDs concentration and sample preparation method were explored for improving the selective ionization process and the detection sensitivity. The proposed approach offered a new dimension to the application of QDs as matrices for MALDI-MS research of carbohydrates. It could be used for quantitative measurement of glucose concentration in human serum with good performance. The QDs served as a matrix showed the advantages of low background, higher sensitivity, convenient sample preparation and excellent stability under vacuum. The QDs assisted LDI-MS approach has promising application to the analysis of carbohydrates in complex biological samples. Copyright © 2016 John Wiley & Sons, Ltd.

  18. Mass Spectrometric Characterization of Benzoxazinoid Glycosides from Rhizopus-Elicited Wheat (Triticum aestivum) Seedlings.

    Science.gov (United States)

    de Bruijn, Wouter J C; Vincken, Jean-Paul; Duran, Katharina; Gruppen, Harry

    2016-08-17

    Benzoxazinoids function as defense compounds and have been suggested to possess health-promoting effects. In this work, the mass spectrometric behavior of benzoxazinoids from the classes benzoxazin-3-ones (with subclasses lactams, hydroxamic acids, and methyl derivatives) and benzoxazolinones was studied. Wheat seeds were germinated with simultaneous elicitation by Rhizopus. The seedling extract was screened for the presence of benzoxazinoid (glycosides) using reversed-phase ultra-high-performance liquid chromatography with photodiode array detection coupled in line to multiple-stage mass spectrometry (RP-UHPLC-PDA-MS(n)). Benzoxazin-3-ones from the different subclasses showed distinctly different ionization and fragmentation behaviors. These features were incorporated into a newly proposed decision guideline to aid the classification of benzoxazinoids. Glycosides of the methyl derivative 2-hydroxy-4-methoxy-1,4-benzoxazin-3-one were tentatively identified for the first time in wheat. We conclude that wheat seedlings germinated with simultaneous fungal elicitation contain a diverse array of benzoxazinoids, mainly constituted by benzoxazin-3-one glycosides.

  19. Mass Spectrometric and Spectrofluorometric Studies of the Interaction of Aristolochic Acids with Proteins

    Science.gov (United States)

    Li, Weiwei; Hu, Qin; Chan, Wan

    2015-10-01

    Aristolochic acid (AA) is a potent carcinogen and nephrotoxin and is associated with the development of “Chinese herb nephropathy” and Balkan endemic nephropathy. Despite decades of research, the specific mechanism of the observed nephrotoxicity has remained elusive and the potential effects on proteins due to the observed toxicity of AA are not well-understood. To better understand the pharmacotoxicological features of AA, we investigated the non-covalent interactions of AA with proteins. The protein-binding properties of AA with bovine serum albumin (BSA) and lysozyme were characterized using spectrofluorometric and mass spectrometric (MS) techniques. Moreover, the protein-AA complexes were clearly identified by high-resolution MS analyses. To the best of our knowledge, this is the first direct evidence of non-covalently bound protein-AA complexes. An analysis of the spectrofluorometric data by a modified Stern-Volmer plot model also revealed that both aristolochic acid I (AAI) and aristolochic acid II (AAII) were bound to BSA and lysozyme in 1:1 stoichiometries. A significantly stronger protein binding property was observed in AAII than in AAI as evidenced by the spectrofluorometric and MS analyses, which may explain the observed higher mutagenicity of AAII.

  20. [Spectrometric characteristics and underlying mechanisms of protective effects of selenium on Spirulina platensis against oxidative stress].

    Science.gov (United States)

    Wu, Hua-lian; Chen, Tian-feng; Yin, Xi; Zheng, Wen-jie

    2012-03-01

    To investigate the possibility and the underlying mechanisms of sodium selenite as antagonist for oxidative stress, the authors examined the effects of pretreatment with selenium on the growth, morphology, spectrometric characteristics and content of reactive oxygen species (ROS) in Spirulina platensis (S. platensis) exposed to H2O2 stress for 24 h in the present study. The results showed that H2O2 induced obvious inhibition of growth and serious morphological damage. The intensity of absorbance peak at 440 nm increased, whereas the peaks at 620 and 680 nm decreased after exposed to H2O2. The emission and excitation spectrum of S. platensis decreased dramatically after H2O2 treatment, and the emission peak from phycocyanin exhibited blue-shift from 660 to 650 nm. The results of FTIR analysis showed that the positions of transmission peaks had no shift, but the relative intensity of characteristic bands from protein and polypeptides including amide I and amide II decreased. Furthermore, the intracellular ROS generation in S. platensis increased significantly in response to H2O2 treatment. In contrast, pretreatments of the cells with selenium for 24 h significantly prevented the H2O2-induced oxidative damages in a dose-dependent manner. Taken together, our results indicate that pretreatments with selenium could prevent ROS overproduction in S. platensis and improve its antioxidant ability. Moreover, selenium could also reduce the effects of free radicals on energy harvest and energy transfer in S. platensis that play vital roles in its photosynthesis.