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.)

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

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.

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

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

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

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.

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

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.

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.

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)

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.

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.

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.

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

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

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)

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)

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.

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