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Sample records for complexometry

  1. New data on masking reagents in complexometry

    International Nuclear Information System (INIS)

    Yurist, I.M.; Talmud, M.M.; Zajtsev, P.M.

    1985-01-01

    Recent literature data on employing inorganic and organic oxygen-, nitrogen- and sulfur-containing substances as masking reagents (MR) in complexonometry of alkali earths, rare earths and transition elements are reviewed for the period of 1971-1983. Effectiveness of any type of MR is shown to be dependent on the electron configuration of a cation being masked. Sr, La, Th, V(6), Zr, Hf, V(5), Nb(5), Ta(5), Mo(6), W(6) a.o. are masked by oxygen-containing ligands. Zn, Cd, Fe(2, 3), Co(2, 3), Ni, etc. are masked by nitrogen- and sulfur-bearing ligands. Thiocompounds mask mainly In, Tl(3), Sn(2), Pb, Bi

  2. Determination of aluminium in iron ores and ferroalloys by complexometry

    International Nuclear Information System (INIS)

    Tikhonov, V.N.; Grigorovich, L.F.

    1977-01-01

    The present method is based on fusing iron ore samples and ferroalloys with NaOH, leaching of the alloy in water, and complexometric estimation of aluminium in the filtrate by back titration of excess EDTA with a CuSO 4 solution in the presence of a glycine-thymol blue tracer, using NaF to increase selectivity. The final titration point is fixed by means of a photoelectrical titrator. Fifty-fold amounts of Cu(2), Mg, Zn, In, Pb, Fe(3) and Ni, twenty-five-fold amounts of Ca, Sr and Cd, ten-fold amounts of Co, five-fold amounts of Hg(2), Bi and Mo(6), two-fold amounts of Mn, and equal amounts of Ga, Tl(3), Zr, V(5) and W(6) do not impede determination. Determination is impeded by metals that form strong fluoride complexes with Sc, Y, rare-earth elements, Ti(4), Sn(2) and V(4), even when those metals are contained in equal amounts; it is also impeded by equal amounts of Cr(3). The selectivity of the given method has been compared with that of methods involving titration with a solution constituting zinc chloride with xylenol orange and with a solution comprising copper chloride and sulphur chrome-azurol in the presence of cytil trimethyl ammonium. The method is more selective. A hexamethylenetetramine buffer solution has been used to obtain an optimum (pH 6) medium. The above procedure is employed to assay standard ferroboron samles of iron ore

  3. Interference of Lithium in Measuring Magnesium by Complexometry: Discussions of the Mechanism

    Directory of Open Access Journals (Sweden)

    Jie Gao

    2013-01-01

    Full Text Available There is usually a large concentration of magnesium in the brine of salt lakes and as a consequence it is difficult to measure Mg2+ accurately with the complexometric titration by ethylenediaminetetraacetic acid disodium salt (EDTA because of the large levels of Li+ also coexisting in brine samples. In this study, a relationship between the relative error related to the number of drops of the indicator and the NMR spectra of anhydrous ethanol and n-butanol, with or without LiCl, was analyzed and compared. It was then possible to suggest a mechanism to explain the interference of Li+ when measuring Mg2+ and to control the interference in the alcohol mixture because Li+ can then complex with the alcohols and mainly form a complex with n-butanol.

  4. Determinación de Ca y Mg en extracto de saturación de suelos

    OpenAIRE

    Abadía Bayona, Anunciación; Millán Martín, Esmeralda; Abadía Bayona, Javier

    1981-01-01

    [EN] Complexometry and atomic spectrometry were used to determine calcium and magnesium values in saturation extracts from calcareous soils. The results show that for calcium both methods can be indistinctly used, while for magnesium complexomtry gives higher values than atomic absorption spectrometry.

  5. Abstracts of the 1. Brazilian Meeting on Analytical Chemistry

    International Nuclear Information System (INIS)

    Curtius, A.J.

    1982-01-01

    Abstracts from experimental studies on analytical chemistry are presented. Several techniques have been used, such as: neutron activation analysis, potentiometry, optical emission spectroscopy, alpha and gamma spectroscopy, atomic absorption spectrophotometry, radiometric analysis, fission track detection, complexometry and others. Samples analysed are of various kinds: environmental materials (soil, water, air), rocks, coal, lanthanide complexes, polycarbonates and synthetic quartz. (C.L.B.) [pt

  6. Mineralogical study of Brazilian fly ashes; origin, characteristics and quality

    International Nuclear Information System (INIS)

    Kihara, Y.

    1984-01-01

    Thirty-one fly ash samples from the five main Brazilian coal-powered thermoelectric plants were subjected to gravimetric chemical analysis, complexometry, flame photometry, X-ray diffractometry, thermodifferential and thermogravimetric analysis, transmitted and reflected light microscopy, electron microprobe analysis and transmited and scanning electron microscopy. (Author) [pt

  7. Thermal decomposition of lanthanides (III) and yttrium (III) solid complexes from ethyl ene diamine tetraacetic acid

    International Nuclear Information System (INIS)

    Mercadante, A.

    1991-01-01

    Solid state compounds of lanthanides (III) and yttrium derived from ethyl ene diamine tetraacetic acid were prepared from respective basic carbonates, that were neutralized with EDTA stoichiometry quantities. Complexometry with EDTA, thermogravimetry (TG), differential thermal analysis (DTA) and X-ray diffraction have been used in the study of these compounds. The results of complexometry with EDTA as well as TG and DTA curves bed to the stoichiometry of these compounds the following general formula is obeyed: H[Ln(EDTA]. n H 2 O. X-ray powder patterns of these compounds permitted to establish two isomorphous series. The DTA ant TG curves allowed us to study the dehydration process, the thermal stability and thermal decomposition of these compounds. (C.G.C.)

  8. Studies on preparation of some alkaloid complexes and solvent extraction

    Energy Technology Data Exchange (ETDEWEB)

    Mohamed, A A

    1990-12-31

    Describes the various methods available in the literature for the determination of different classes of alkaloids spectrochemical (e.g.spectrophotometry and colorimetry, fluorimetry and phosphorimetry, nephelometry and reiractometry), electrochemical (e.g. polarography, amperometry, conductometry, coulometry and potentiometry), volumetric (e.q. acid-base, iodometry , bromimetry , oxidimetry, complexometry and precipitation ) and miscellaneous methods (e.g.gasliquid chromatography, gravimetry, thermometry and rediometry ) has been discussed. 31 tabs; 29 figs; 402 refs.

  9. Studies on preparation of some alkaloid complexes and solvent extraction

    International Nuclear Information System (INIS)

    Mohamed, A.A.

    1989-01-01

    Describes the various methods available in the literature for the determination of different classes of alkaloids spectrochemical (e.g.spectrophotometry and colorimetry, fluorimetry and phosphorimetry, nephelometry and reiractometry), electrochemical (e.g. polarography, amperometry, conductometry, coulometry and potentiometry), volumetric (e.q. acid-base, iodometry , bromimetry , oxidimetry, complexometry and precipitation ) and miscellaneous methods (e.g.gasliquid chromatography, gravimetry, thermometry and rediometry ) has been discussed

  10. Preparation, characterization and thermal behaviour study of 4-dimethyl amino benzal pyruvate of lanthanides (III) and yttrium (III) in solid state

    International Nuclear Information System (INIS)

    Miyano, M.H.

    1990-01-01

    Solid state compounds involving Ln and DMBP, where Ln trivalent lanthanides (except promethium) and yttrium; DMBP 4-dimethyl amino benzylidene pyruvate, were prepared by addition of ligand to the corresponding metal ions chlorides, both in aqueous solution. The precipitates were washed with distilled water and dried at 40 0 C in a forced circulation oven. Complexometry with EDTA, thermogravimetry (TG), differential thermal analysis (DTA), infra-red absorption and X-ray diffraction have been used in the study of these compounds. (author)

  11. Analytical chemistry

    Energy Technology Data Exchange (ETDEWEB)

    Chae, Myeong Hu; Lee, Hu Jun; Kim, Ha Seok

    1989-02-15

    This book give explanations on analytical chemistry with ten chapters, which deal with development of analytical chemistry, the theory of error with definition and classification, sample and treatment gravimetry on general process of gravimetry in aqueous solution and non-aqueous solution, precipitation titration about precipitation reaction and types, complexometry with summary and complex compound, oxidation-reduction equilibrium on electrode potential and potentiometric titration, solvent extraction and chromatograph and experiment with basic operation for chemical experiment.

  12. Analytical chemistry

    International Nuclear Information System (INIS)

    Chae, Myeong Hu; Lee, Hu Jun; Kim, Ha Seok

    1989-02-01

    This book give explanations on analytical chemistry with ten chapters, which deal with development of analytical chemistry, the theory of error with definition and classification, sample and treatment gravimetry on general process of gravimetry in aqueous solution and non-aqueous solution, precipitation titration about precipitation reaction and types, complexometry with summary and complex compound, oxidation-reduction equilibrium on electrode potential and potentiometric titration, solvent extraction and chromatograph and experiment with basic operation for chemical experiment.

  13. Analytical control of HTSC chemical composition of Y-Ba-Cu-O system

    International Nuclear Information System (INIS)

    Rojzenblat, E.M.; Kuchkina, E.D.; Bondarenko, S.K.; Ivanova, K.P.; Prisedskij, V.V.

    1989-01-01

    Methods for determining the cation composition and oxygen nonstoichiometry of YBa 2 Cu 3 O 6+δ superconductors are developed. Barium is determined in the form of BaSO 4 by the gravimetric method. Yttrium is determined using complexometry at pH=5.5 with a xylenol orange indicator in the presence of unithiol. Copper is determined using iodometry. Depending on conditions of analysis, it provides to determine both the total copper content in the sample and its oxygen nonstoichiometry. The method for determining the composition and structure of the studied ceramics according to the analysis of gas evolution from specimens during their dissolution in acids is described. The method of X-ray fluorescence analysis of ceramics cation composition is developed as well

  14. Determination of Sc and Th in ScI3-NaI-ThI4 sample

    International Nuclear Information System (INIS)

    Yuan Hui; Yang Zhihong

    1999-01-01

    Determination of Sc and Th in ScI 3 -NaI-ThI 4 sample is studied by X-ray fluorescence and complexometry. The effect of working condition of Sc on X-ray fluorescence spectrometer and different sample-making method on the determination of Sc and Th are studied experimentally. The X-ray fluorescence analysis of determination of Sc and Th is developed by polyester film sample-making technique, the measuring precision of Sc and Th is better than 4%. The effect of acidity and temperature on the determining end point of titration is obvious. The results of different complexometric methods are compared. The precision of Sc and Th is less than 2% by comlexometry, it is fit for the routine analysis of ScI 3 -NaI-ThI 4 sample

  15. Thermal and spectroscopic study to investigate p-aminobenzoic acid, sodium p-aminobenzoate and its compounds with some lighter trivalent lanthanides

    International Nuclear Information System (INIS)

    Teixeira, J.A.; Nunes, W.D.G.; Colman, T.A.D.; Nascimento, A.L.C.S do; Caires, F.J.; Campos, F.X.; Gálico, D.A.; Ionashiro, M.

    2016-01-01

    Highlights: • The p-aminobenzoic acid melts followed partial evaporation. • The stoichiometry of compounds was established by TG, EA and complexometry. • The TG–DTA curves provided previously unreported information about thermal behavior. - Abstract: The characterization, thermal stability and thermal decomposition of some lighter trivalent lanthanide p-aminobenzoates, Ln(C 7 H 6 NO 2 ) 3 ·H 2 O (Ln = La, Ce, Pr, Nd, Sm), as well as the thermal behavior and spectroscopic study of p-aminobenzoic acid C 7 H 7 NO 2 and its sodium salt were investigated. The following methods were utilized: simultaneous thermogravimetry and differential thermal analysis (TG–DTA) in dynamic dry air and nitrogen atmospheres; differential scanning calorimetry (DSC); middle (MIR) and near (NIR) infrared region spectroscopy; evolved gas analysis (EGA); elemental analysis; complexometry; X-ray diffraction (XRD); and diffuse reflectance spectroscopy (DR) in the ultraviolet and visible regions. All the compounds were obtained monohydrated and the thermal decomposition occurred in two, three or four steps in an air atmosphere, and three or four steps in N 2 atmosphere. In both atmospheres (air and N 2 ) the final residues were CeO 2 , Pr 6 O 11 , Ln 2 O 3 (Ln = La, Nd, Sm). The results also provided information concerning the coordination mode and thermal behavior, as well as the identification of the gaseous products which evolved during the thermal decomposition of these compounds. The DR and NIR spectra provided information about the ligand absorption bands and the f–f transitions of the Nd 3+ , Pr 3+ and Sm 3+ ions.

  16. Thermal and spectroscopic study to investigate p-aminobenzoic acid, sodium p-aminobenzoate and its compounds with some lighter trivalent lanthanides

    Energy Technology Data Exchange (ETDEWEB)

    Teixeira, J.A.; Nunes, W.D.G.; Colman, T.A.D.; Nascimento, A.L.C.S do [Instituto de Química, UNESP—Universidade Estadual Paulista, Campus Araraquara, Departamento de Química Analítica, Araraquara 14801-970, SP (Brazil); Caires, F.J. [Faculdade de Ciências, UNESP—Universidade Estadual Paulista, Campus Bauru, Departamento de Química, Bauru 17033-260, SP (Brazil); Campos, F.X. [Instituto de Química, UNESP—Universidade Estadual Paulista, Campus Araraquara, Departamento de Química Analítica, Araraquara 14801-970, SP (Brazil); Instituto Federal de Educação, Ciência e Tecnologia de Mato Grosso, Primavera do Leste 78850-000, MT (Brazil); Gálico, D.A. [Instituto de Química, UNICAMP—Universidade Estadual de Campinas, Campinas 13083-970, SP (Brazil); Ionashiro, M., E-mail: massaoi@yahoo.com.br [Instituto de Química, UNESP—Universidade Estadual Paulista, Campus Araraquara, Departamento de Química Analítica, Araraquara 14801-970, SP (Brazil)

    2016-01-20

    Highlights: • The p-aminobenzoic acid melts followed partial evaporation. • The stoichiometry of compounds was established by TG, EA and complexometry. • The TG–DTA curves provided previously unreported information about thermal behavior. - Abstract: The characterization, thermal stability and thermal decomposition of some lighter trivalent lanthanide p-aminobenzoates, Ln(C{sub 7}H{sub 6}NO{sub 2}){sub 3}·H{sub 2}O (Ln = La, Ce, Pr, Nd, Sm), as well as the thermal behavior and spectroscopic study of p-aminobenzoic acid C{sub 7}H{sub 7}NO{sub 2} and its sodium salt were investigated. The following methods were utilized: simultaneous thermogravimetry and differential thermal analysis (TG–DTA) in dynamic dry air and nitrogen atmospheres; differential scanning calorimetry (DSC); middle (MIR) and near (NIR) infrared region spectroscopy; evolved gas analysis (EGA); elemental analysis; complexometry; X-ray diffraction (XRD); and diffuse reflectance spectroscopy (DR) in the ultraviolet and visible regions. All the compounds were obtained monohydrated and the thermal decomposition occurred in two, three or four steps in an air atmosphere, and three or four steps in N{sub 2} atmosphere. In both atmospheres (air and N{sub 2}) the final residues were CeO{sub 2}, Pr{sub 6}O{sub 11}, Ln{sub 2}O{sub 3} (Ln = La, Nd, Sm). The results also provided information concerning the coordination mode and thermal behavior, as well as the identification of the gaseous products which evolved during the thermal decomposition of these compounds. The DR and NIR spectra provided information about the ligand absorption bands and the f–f transitions of the Nd{sup 3+}, Pr{sup 3+} and Sm{sup 3+} ions.

  17. Thermal behaviour of nicotinic acid, sodium nicotinate and its compounds with some bivalent transition metal ions

    Energy Technology Data Exchange (ETDEWEB)

    Nascimento, A.L.C.S. do; Caires, F.J., E-mail: caires.flavio@yahoo.com.br; Gomes, D.J.C.; Gigante, A.C.; Ionashiro, M.

    2014-01-10

    Graphical abstract: - Highlights: • The transition metal ion nicotinates were synthesized. • The TG–DTA curves provided previously unreported information about thermal behaviour. • The gaseous products released were detected by TG–DSC coupled to FTIR. - Abstract: Solid-state M(L){sub 2}·nH{sub 2}O compounds, where M stands for bivalent transition metals (Mn, Fe, Co, Ni, Cu and Zn), L is nicotinate and n = 0–4.5, have been synthesized. Characterization and thermal behaviour of these compounds were investigated employing elemental analysis based on the mass losses observed in the TG–DTA curves, complexometry, X-ray diffractometry, infrared spectroscopy (FTIR), simultaneous thermogravimetric and differential thermal analysis (TG–DTA) and TG–DSC coupled to FTIR. The thermal behaviour of nicotinic acid and its sodium salt was also investigated. For the hydrated transition metal compounds, the dehydration and thermal decomposition of the anhydrous compounds occur in a single step. For the sodium nicotinate, the final residue up to 765 °C is sodium carbonate and for the transition metal nicotinates, the final residues are Mn{sub 3}O{sub 4}, Fe{sub 2}O{sub 3}, Co{sub 3}O{sub 4}, NiO, CuO and ZnO. The results also provided information concerning the thermal stability, thermal decomposition and identification of the gaseous products evolved during the thermal decomposition of the compounds.

  18. Simultaneous complexometric determination of bismuth and indium in thermoelectronic material (Bisub(1-x)Insub(x))/sub 2/Te/sub 3/

    Energy Technology Data Exchange (ETDEWEB)

    Danzaki, Yuetsu; Shoji, Tsutomu; Sase, Masahiko; Takeyama, Shuro [Tohoku Univ., Sendai (Japan). Research Inst. for Iron, Steel and Other Metals

    1983-08-01

    A sample of 0.1 g was dissolved in 5 ml of conc. HNO/sub 3/ and diluted to about 100 ml with water. To the sample solution 20 % KOH solution was added so as to make 2 % KOH alkaline solution. The solution was boiled for about 5 min and cooled in running water. The coagulated precipitate was filtered and washed with 1 % KOH solution. The precipitate on the filter paper was dissolved in 15 ml of hot HNO/sub 3/ (1 + 1), and washed with warm HNO/sub 3/ (2 + 100). After the filtrate was evaporated to about 2 ml and diluted to about 10 ml with water, 20 ml of 0.02 M EDTA was added and diluted to about 100 ml. The pH of the solution was adjusted to 5--5.5 with hexamethylenetetramine. The excess of EDTA was back-titrated with 0.01 M Pb(NO/sub 3/)/sub 2/ in the presence of MTBas an indicater, and total amounts of Bi and In were determined. To the same solution, 1 g of ascorbic acid was added, and pH was adjusted to 10 with ammoniacal water. After (1--2) min, the liberated EDTA was titrated with 0.01 M MnCl/sub 2/, and the amount of Bi was determined. The results obtained with complexometry were compared with those of BiOCl gravimetry for Bi and atomic absorption for In.

  19. Rare earths: preparation of spectro chemically pure standards, study of their carbonates and synthesis of a new compound series - the peroxy carbonates; Terras-raras: obtencao de padroes espectroquimicos, estudo dos carbonatos e sintese dos peroxicarbonatos. Uma nova serie de compostos

    Energy Technology Data Exchange (ETDEWEB)

    Queiroz, Carlos Alberto da Silva

    1996-05-01

    In this work the following studies are concerned: I) preparation of lanthanum, cerium, praseodymium, neodymium and samarium oxides for use as spectro chemically pure standards; II) behavior of the rare earth (La, Ce, Pr, Nd, Sm) carbonates soluble in ammonium carbonate and mixture of ammonium carbonate/ammonium hydroxide, and III) synthesis and characterization of rare earth peroxy carbonates - a new series of compounds. Data for the synthesis and characterization of the rare earths peroxy carbonates described for the first time in this work are presented and discussed. With the aid of thermal analysis (TG-DTG) the thermal stability and the stoichiometric composition for new compounds were established and a mechanism of thermal decomposition was proposed. The peroxy carbonate was prepared by the addition of hydrogen peroxyde to the complexed soluble rare earths carbonates. These studies included also the determinations of active oxygen, the total rare earth oxide by gravimetry and complexometry and the C, H and N contents by microanalysis. The new compounds were also investigated by infrared spectroscopy. (author)

  20. Rare earths: preparation of spectro chemically pure standards, study of their carbonates and synthesis of a new compound series - the peroxy carbonates

    International Nuclear Information System (INIS)

    Queiroz, Carlos Alberto da Silva

    1996-05-01

    In this work the following studies are concerned: I) preparation of lanthanum, cerium, praseodymium, neodymium and samarium oxides for use as spectro chemically pure standards; II) behavior of the rare earth (La, Ce, Pr, Nd, Sm) carbonates soluble in ammonium carbonate and mixture of ammonium carbonate/ammonium hydroxide, and III) synthesis and characterization of rare earth peroxy carbonates - a new series of compounds. Data for the synthesis and characterization of the rare earths peroxy carbonates described for the first time in this work are presented and discussed. With the aid of thermal analysis (TG-DTG) the thermal stability and the stoichiometric composition for new compounds were established and a mechanism of thermal decomposition was proposed. The peroxy carbonate was prepared by the addition of hydrogen peroxyde to the complexed soluble rare earths carbonates. These studies included also the determinations of active oxygen, the total rare earth oxide by gravimetry and complexometry and the C, H and N contents by microanalysis. The new compounds were also investigated by infrared spectroscopy. (author)

  1. Thermal and spectroscopic studies on solid ibuprofen complexes of lighter trivalent lanthanides

    Energy Technology Data Exchange (ETDEWEB)

    Gálico, D.A.; Holanda, B.B.C.; Guerra, R.B.; Legendre, A.O.; Rinaldo, D. [UNESP – Univ Estadual Paulista, Faculdade de Ciências, Departamento de Química, São Paulo CEP 17033-260 (Brazil); Treu-Filho, O. [UNESP – Univ Estadual Paulista, Instituto de Química, São Paulo CEP 14800-900 (Brazil); Bannach, G., E-mail: gilbert@fc.unesp.br [UNESP – Univ Estadual Paulista, Faculdade de Ciências, Departamento de Química, São Paulo CEP 17033-260 (Brazil)

    2014-01-10

    Highlights: • Lighter trivalent lanthanide complexes of ibuprofen have been synthesized. • The TG-FTIR allowed the identification of propane as the gas evolved during the thermal decomposition of the neodymium compound. • The thermal analysis provided information about the composition, dehydration, thermal behavior and thermal decomposition of the samples. • The theoretical and experimental spectroscopic studies suggest that the carboxylate group of ibuprofen is coordinated to the metals by a bidentate bond. - Abstract: Solid-state compounds of general formula Ln(L){sub 3}, in which L is ibuprofen and Ln stands for trivalent La, Ce, Pr, Nd, Sm and Eu, have been synthesized. Simultaneous thermogravimetry and differential thermal analysis (TG-DTA), X-ray powder diffractometry (DRX), complexometry, Fourier-transformed infrared spectroscopy (FTIR) and thermogravimetry coupled to Fourier-transformed infrared spectroscopy (TG-FTIR) were used to characterize these compounds. The results provided information concerning the chemical composition, dehydration, coordination modes of the ligands, crystallinity of the samples, thermal behavior and thermal decomposition of the compounds. The theoretical and experimental spectroscopic studies suggest that ibuprofen coordinates through the carboxylate group as a chelating ligand.

  2. Simultaneous complexometric determination of bismuth and indium in thermoelectronic material (Bisub(1-x)Insub(x))2Te3

    International Nuclear Information System (INIS)

    Danzaki, Yuetsu; Shoji, Tsutomu; Sase, Masahiko; Takeyama, Shuro

    1983-01-01

    A sample of 0.1 g was dissolved in 5 ml of conc. HNO 3 and diluted to about 100 ml with water. To the sample solution 20 % KOH solution was added so as to make 2 % KOH alkaline solution. The solution was boiled for about 5 min and cooled in running water. The coagulated precipitate was filtered and washed with 1 % KOH solution. The precipitate on the filter paper was dissolved in 15 ml of hot HNO 3 (1 + 1), and washed with warm HNO 3 (2 + 100). After the filtrate was evaporated to about 2 ml and diluted to about 10 ml with water, 20 ml of 0.02 M EDTA was added and diluted to about 100 ml. The pH of the solution was adjusted to 5--5.5 with hexamethylenetetramine. The ex cess of EDTA was back-titrated with 0.01 M Pb(NO 3 ) 2 in the presence of MTBas an indicater, and total amounts of Bi and In were determined. To the same solution, 1 g of ascorbic acid was added, and pH was adjusted to 10 with ammoniacal water. After (1--2) min, the liberated EDTA was titrated with 0.01 M MnCl 2 , and the amount of Bi was determined. The results obtained with complexometry were compared with those of BiOCl gravimetry for Bi and atomic absorption for In. (author)

  3. Thermal behaviour of nicotinic acid, sodium nicotinate and its compounds with some bivalent transition metal ions

    International Nuclear Information System (INIS)

    Nascimento, A.L.C.S. do; Caires, F.J.; Gomes, D.J.C.; Gigante, A.C.; Ionashiro, M.

    2014-01-01

    Graphical abstract: - Highlights: • The transition metal ion nicotinates were synthesized. • The TG–DTA curves provided previously unreported information about thermal behaviour. • The gaseous products released were detected by TG–DSC coupled to FTIR. - Abstract: Solid-state M(L) 2 ·nH 2 O compounds, where M stands for bivalent transition metals (Mn, Fe, Co, Ni, Cu and Zn), L is nicotinate and n = 0–4.5, have been synthesized. Characterization and thermal behaviour of these compounds were investigated employing elemental analysis based on the mass losses observed in the TG–DTA curves, complexometry, X-ray diffractometry, infrared spectroscopy (FTIR), simultaneous thermogravimetric and differential thermal analysis (TG–DTA) and TG–DSC coupled to FTIR. The thermal behaviour of nicotinic acid and its sodium salt was also investigated. For the hydrated transition metal compounds, the dehydration and thermal decomposition of the anhydrous compounds occur in a single step. For the sodium nicotinate, the final residue up to 765 °C is sodium carbonate and for the transition metal nicotinates, the final residues are Mn 3 O 4 , Fe 2 O 3 , Co 3 O 4 , NiO, CuO and ZnO. The results also provided information concerning the thermal stability, thermal decomposition and identification of the gaseous products evolved during the thermal decomposition of the compounds

  4. Selective Lanthanides Sequestration Based on a Self-Assembled Organo-silica

    Energy Technology Data Exchange (ETDEWEB)

    Ahmad, M.; Reye, C.; Corriu, R.J. P. [Univ Montpellier, Inst Charles Gerhardt Montpellier, UMR 5253, Chim Mol and Org Solide, F-34095 Montpellier 5 (France); Besson, E. [ICSM Site Marcoule, UMR 5257, Inst Chim Separat Marcoule, F-30207 Bagnols Sur Ceze (France); Van der Lee, Arie [Univ Montpellier, Inst Europeen Membranes, UMR 5635, CNRS, F-34095 Montpellier 5 (France); Besson, E.; Chollet, H. [CEA Valduc, Dept Traitement Mat Nucl, F-21120 Is Sur Tille (France); Guilard, R. [Univ Bourgogne, Inst Chim Mol, CNRS, ICMUB, UMR 5260, F-21078 Dijon (France)

    2010-07-01

    In this paper, we investigate the cation-exchange properties of a self-assembled hybrid material towards trivalent ions, lanthanides (La{sup 3+}, Eu{sup 3+}, Gd{sup 3+}, Yb{sup 3+}) and Fe{sup 3+}. The bis-zwitterionic lamellar material was prepared by sol-gel process from only 3-aminopropyltriethoxysilane (APTES), succinic anhydride, and ethylenediamine. In ethanol heated under reflux, the exchange ethylenediammonium versus Ln{sup 3+} proved to be complete by complexometry measurements and elemental analyses, one Cl{sup -} ion per one Ln(III) remaining as expected for charge balance. In aqueous solution at 20 degrees C, the material was found to be selective towards lanthanide in spite of the similarity of their ionic radii. The cation uptake depends on the nature of the salt, the difference between two lanthanides reaching up to 20% in some cases. Finally, ion-exchange reaction with FeCl{sub 3} was chosen as a probe to get more information on the material after incorporation of trivalent ions. Based on Moessbauer spectroscopic investigations on the resulting material in conjunction with the XRD analysis of materials containing trivalent ions, a structural model was proposed to describe the incorporation of trivalent ions by exchange reaction within the original zwitterionic material. (authors)

  5. Thermal and spectroscopic studies on solid ibuprofen complexes of lighter trivalent lanthanides

    International Nuclear Information System (INIS)

    Gálico, D.A.; Holanda, B.B.C.; Guerra, R.B.; Legendre, A.O.; Rinaldo, D.; Treu-Filho, O.; Bannach, G.

    2014-01-01

    Highlights: • Lighter trivalent lanthanide complexes of ibuprofen have been synthesized. • The TG-FTIR allowed the identification of propane as the gas evolved during the thermal decomposition of the neodymium compound. • The thermal analysis provided information about the composition, dehydration, thermal behavior and thermal decomposition of the samples. • The theoretical and experimental spectroscopic studies suggest that the carboxylate group of ibuprofen is coordinated to the metals by a bidentate bond. - Abstract: Solid-state compounds of general formula Ln(L) 3 , in which L is ibuprofen and Ln stands for trivalent La, Ce, Pr, Nd, Sm and Eu, have been synthesized. Simultaneous thermogravimetry and differential thermal analysis (TG-DTA), X-ray powder diffractometry (DRX), complexometry, Fourier-transformed infrared spectroscopy (FTIR) and thermogravimetry coupled to Fourier-transformed infrared spectroscopy (TG-FTIR) were used to characterize these compounds. The results provided information concerning the chemical composition, dehydration, coordination modes of the ligands, crystallinity of the samples, thermal behavior and thermal decomposition of the compounds. The theoretical and experimental spectroscopic studies suggest that ibuprofen coordinates through the carboxylate group as a chelating ligand

  6. Quality control methods of strontium chloride 89SrCl2, radiopharmaceutical for palliative treatment of bone metastases

    International Nuclear Information System (INIS)

    Deptula, C.Z.; Kempisty, T.; Markiewicz, A.; Mikolajczak, R.; Stefancyk, S.; Terlikowska, T.; Zulczyk, W.

    1997-01-01

    Strontium chloride, 89 SrCI 2 , a radiopharmaceutical used for palliative therapy of bone metastases from breast and prostate cancer is produced by irradiation in a nuclear reactor. The analytical quality control procedures are established to confirm the radionuclidic purity of the preparation, its chemical composition and specific activity. Chemical concentration of strontium in the product is determined by complexometry with arsenazo III and chlorides assay by potentiometric titration with silver nitrate. The contamination with chemical impurities is determined by DC graphite spark spectrography. The specific activity and isotonicity of the solution are corrected by addition of natural SrCI 2 and NaCI. 90 Sr is produced in the 89 Sr(n,γ) 90 Sr reaction contributes to impurities. It decays to 90 Y and the activity of 90 Sr can be calculated from the activity of 90 Y. The extraction chromatography on nonionic acrylic ester polymer coated with organic solutions of selective features (Spec resins for Eichrom) is applied for separation of radionuclides. The extraction chromatography system consisting of two columns: strontium selective resin and rare earth elements selective resin was used for separation of 90 Y from 90 Sr in the 89 SrCI 2 solution. The 90 Y and 90 Sr carrier-free solutions used as tracers helped for determination of extraction conditions and efficiency. The concentration of 90 Sr determined in the analysed solution is at the level of 2.10 -4 % which conforms with the data calculated from irradiation parameters. The obtained product, strontium chloride 89 SrCI 2 for injection, forms a sterile and isotonic water solution (pH - 4-7) with specific activity of 89 Sr in the range from 3.5 to 6.3. MBq/mg and radioactive concentration of 37.5 MBq/ml. The radionuclidic purity of the obtained preparations is at the level of 99.9% with respect to 89 Sr

  7. Analytical methodology for the study of decontamination factors in mixer-settlers

    International Nuclear Information System (INIS)

    Alzabet, Horacio; Crubellati, Ricardo; Di Santo, Norberto; Eppis, Maria; Gonzalez, Guillermo; Bof, Elba; Devida, Claudio

    1987-01-01

    Due to the complexity of the samples, the choice of the analytical methodology to be applied at a radiochemical laboratory, for the evaluation of different separation steps if of a great importance. It is necessary to know the performance of mixer-settlers in two extreme situations: efficiency limit determined by fluid dynamic factors and separation factor determined by physicochemical variables. The element used to determine the efficiency limit was magnesium, due to its low distribution coefficient in tri-n-butyl phosphate (TBP). Zirconium, being one of the principal fission product, is partially extracted and was used to study the influence of chemical conditions. Atomic absorption spectrometry was selected for the determination of micro quantities of magnesium, and complexometry for macro quantities of this element. It was necessary to separate uranium using extraction chromatography with Kel F-TBP columns. Concentration range was 0.1 - 1 mg/L and 7 - 70 g/L respectively. Zirconium was determined by spectrophotometry with xylenol orange. For organic samples, it was necessary to reextract the analyte with fluoride, to evaporate with sulfuric acid and to complex the excess of fluoride with aluminum. Uranium determinations, required for mass balance, were carried out by spectrophotometry and potentiometry depending upon concentration. Because of the presence of zirconium, two methods were developed for uranium determination using liquid-liquid extraction in the presence of complexing agents. In one case, TBP was used as extractant, dibenzoylmethane as chromogenic reagent and EDTA as complexing agent. For very low quantities of uranium, tri-octyl phosphine oxide (TOPO) was the extractant, 2-(2-thiazolylazo)-5-diethylaminophenol (TAAP) the chromogenic reagent, and (1-2-cyclohexylenedinitrilo) tetraacetic acid (CDTA) the complexing agent. (Author)

  8. Extraction studies of actinides by diamylbutyl phosphonate

    International Nuclear Information System (INIS)

    Brahmananda Rao, C.V.S.; Jayalakshmi, S.; Subramaniam, S.; Sabharwal, K.N.; Sivaraman, N.; Vasudeva Rao, P.R.

    2014-01-01

    The extraction ability of a monodentate organophosphorus extractant depends on the basicity of the phosphoryl oxygen atom and the nature of the substituents attached to the phosphorus atom. The basicity on the phosphoryl oxygen in the neutral organophosphorus extractant series increases in the order, phosphates 1 H, 13 C and 31 P NMR spectra. Extraction of U(VI) by 1.1 M DABP/n-dodecane as a function of nitric acid was studied using 233 U tracer. Th(IV) extraction behaviour as a function of nitric acid was studied using Arsenazo-III as chromogenic agent. 5 mL of the 1.1 M DABP solution in the diluent (n-dodecane) was equilibrated with 5mL of saturated thorium nitrate in an equilibration tube using a magnetic stirring bar. The organic and aqueous phases were analysed by complexometry using DTPA as titrant and xylenol orange as indicator. The LOC values were determined as a function of nitric acid concentration. The extraction of U(VI) and Th(IV) by 1.1M DABP along with TBP in n-dodecane at 303 K as a function of equilibrium nitric acid concentration are shown. The DABP shows higher distribution ratios for U(VI) and Th(IV) in the entire range of nitric acid concentrations studied compared to TBP. The steep rise in the distribution ratio is attributed to the higher basicity of phosphoryl group in phosphonates compared to the less basic nature of phosphates. The third phase formation of thorium as function of nitric acid concentration with 1.1 M DABP at 303 K are given. The LOC values for DABP system were higher throughout the nitric acid concentration compared to the TBP system. (author)

  9. A Nanostructured Lipid System as a Strategy to Improve the in Vitro Antibacterial Activity of Copper(II Complexes

    Directory of Open Access Journals (Sweden)

    Patricia B. da Silva

    2015-12-01

    Full Text Available The aim of this study was to construct a nanostructured lipid system as a strategy to improve the in vitro antibacterial activity of copper(II complexes. New compounds with the general formulae [CuX2(INH2]·nH2O (X = Cl− and n = 1 (1; X = NCS− and n = 5 (2; X = NCO− and n = 4 (3; INH = isoniazid, a drug widely used to treat tuberculosis derived from the reaction between the copper(II chloride and isoniazid in the presence or absence of pseudohalide ions (NCS− or NCO− were synthesized and characterized by infrared spectrometry, electronic absorption spectroscopy, electron paramagnetic resonance (EPR spectroscopy, elemental analysis, melting points and complexometry with 2,2′,2′′,2′′′-(Ethane-1,2-diyldinitrilotetraacetic acid (EDTA. The characterization techniques allowed us to confirm the formation of the copper(II complexes. The Cu(II complexes were loaded into microemulsion (MEs composed of 10% phase oil (cholesterol, 10% surfactant [soy oleate and Brij® 58 (1:2] and 80% aqueous phase (phosphate buffer pH = 7.4 prepared by sonication. The Cu(II complex-loaded MEs displayed sizes ranging from 158.0 ± 1.060 to 212.6 ± 1.539 nm, whereas the polydispersity index (PDI ranged from 0.218 ± 0.007 to 0.284 ± 0.034. The antibacterial activity of the free compounds and those that were loaded into the MEs against Staphylococcus aureus ATCC® 25923 and Escherichia coli ATCC® 25922, as evaluated by a microdilution technique, and the cytotoxicity index (IC50 against the Vero cell line (ATCC® CCL-81TM were used to calculate the selectivity index (SI. Among the free compounds, only compound 2 (MIC 500 μg/mL showed activity for S. aureus. After loading the compounds into the MEs, the antibacterial activity of compounds 1, 2 and 3 was significantly increased against E. coli (MIC’s 125, 125 and 500 μg/mL, respectively and S. aureus (MICs 250, 500 and 125 μg/mL, respectively. The loaded compounds were less toxic against the Vero