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Query: EC:4.1.2.42 (DTA)
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The quaternary mixed anion of rare earth with 2,3-dimethoxylbenzoic acid and 1,10-phenanthroline has been synthesized from the water-ethanol solution. Elemental analysis shows that the complexes general formula is RE(2,3-DMOBA)2NO3Phen (RE = La, Nd, Eu, Dy). The complexes are characterized by IR, UV, TG-DTA analysis. Nu2 + nu5, nu2 + nu6 of NO3- are observed in 1772 and 1737 cm(-1) in IR spectra of complexes, it shows that NO3- group is in a bridging-chelating mode in which two O atoms chelate to RE3+ ions. UV spectra of ligand and complexes are different, it shows that ligand 2,3-dimethoxylbenzoate and 1,10-phenanthroline coordinate to RE3+ ions. Visible absorption spectra of Nd(2,3-DMOBA)2NO3Phen show that hypersensitive transition of neodymium.
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PMID:[Synthesis and characterization of mixed ligand complexes rare earth with 2,3-dimethoxylbenzoic acid and 1,10-phenanthroline]. 1576 90

The title ternary complex La(C5O3H3)3 x C12H8N2 x H2O was synthesized by reaction of lanthanum nitrate with alpha-furoic acid (C5O3H4) and 1,10-phenanthroline (C12H8N2) as ligand in the alcohol solvent. The composition of the complex was determined by element analysis. Its structure and properties were characterized by IR, 1H NMR, UV and TG-DTA. IR, 1H NMR, UV spectra showed that the ligand alpha-furoic acid coordinate to the center ion La (III) with the deprotonized form, and 1, 10-10phenanthroline with the bidentate form using its two N atoms. The TG-DTA analysis exhibited that the complex is stable in the range of room temperature and undergo the disassociation of water and oxygenized decomposition of the organic ligands in order with the rising of temperature, and the final oxide obtained is La2O3. The quantitative analysis of TG-DTA was coincided with the structural composition of the title complex.
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PMID:[Synthesis and characterization of complex La(C5O3H3)3 x C12H8N2 x H2O]. 1582 7

Cobalt(II) complexes of reduced glutathione (GSH) of general composition Na[Co(L)(X)].nH2O (where H2L = GSH; X = Cl-, NO3-, NCS-, CH3CO2-, HCO2-, ClO4- and n = 0-4) have been synthesized and characterised by elemental analyses, vibrational spectra, electronic spectra, magnetic susceptibility measurements, thermal studies and molecular modeling studies. Electronic spectra indicate planar geometry for all the complexes. Infrared spectra indicate the presence of H2O molecules (except perchlorate complex) in the complexes that has been supported by TG/DTA. The room temperature magnetic moment values for all complexes lie in the range of 2.60-2.80 BM range indicating departure from spin only values due to second order Zeeman effect. Thermal decomposition of all the complexes proceeds via first order kinetics. The Na[Co(L)(Cl)].2H2O complex has the minimum activation energy and Na[Co(L)(CH3CO2)].3H2O has the maximum activation energy. The molecular modeling calculation for energy minimization optimizes geometry of the metal complexes.
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PMID:Cobalt(II) complexes of biologically active glutathione: spectroscopic and molecular modeling studies. 1634 45

Paramolybdate-LDHs with MgAl or ZnAl cations within the layers have been prepared by the ion-exchange method from hydrotalcites with different interlayer anions (OH-, NO3(-), and terephthalate). The samples and the oxides obtained after their calcination were characterized by element chemical analysis, PXRD, FT-Raman spectroscopy, thermal analysis (TG/DTA), N2 adsorption at -196 degrees C, and SEM. The results show that layered solids with hydrotalcite-type structure were obtained in which the interlayer space is occupied by heptamolybdate with a small amount of MoO4(2-) units formed through hydrolysis of the polyanion; both oxomolybdenum species undergo a progressive distortion of the octahedral units from 50 degrees C but are roughly stable up to 250 degrees C as a consequence of the interaction between the polyanion and the brucite-like layers. This distortion is responsible for the observed decrease in the height of the gallery for samples heated in the temperature range, 50-250 degrees C, with respect to the original samples. Rehydration of the calcined solids allows recovering of their original structures and the initial values for the gallery heights. Calcination between 300 and 400 degrees C gives rise to a collapse of the layered structure, and amorphous phases are formed, in which molybdenum is both octahedrally and tetrahedrally coordinated. Crystalline magnesium and zinc molybdates (MgMoO4 and ZnMoO4) are formed at 450 and 600 degrees C, respectively. All solids have some microporosity, which decreases with increasing the calcination temperature.
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PMID:Structural and texture evolution with temperature of layered double hydroxides intercalated with paramolybdate anions. 1644 Nov 36

Highly ordered silver sulfide nanorods conjugated with the Bovine Serum Albumin (BSA) protein have been successfully achieved at ambient temperature. Such a process is very simple and controllable, directly using silver nitrate and thioacetamide (TAA) as the reactants in the aqueous solution of BSA. The products have been characterized by XRD, HRTEM-SAED, SEM-EDS, TG-DTA, FT-IR, and CD spectroscopy. The results of the research show that the as-prepared Ag2S nanorods are monodispersed with sizes about 40 nm in diameter and 220 nm in length, and exhibit a high degree of crystallinity and good photoluminescence. Furthermore, an interesting mechanism is discussed for the formation of the Ag2S nanorods.
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PMID:Fabrication of protein-conjugated silver sulfide nanorods in the bovine serum albumin solution. 1672 64

A new ligand, N,N'-di(pyridine N-oxide-2-yl)pyridine-2,6-dicarboxamide (LH2) and its several lanthanide (III) complexes (La, Eu, Gd, Tb, Y) were synthesized and characterized in detail based on elemental analysis, conductivity measurements, IR, 1H NMR, MS (FAB) and UV spectra and TG-DTA studies. The results indicated that the composition of these binary complexes is [Ln(LH2)(NO3)2.H2O]NO3.nH2O (n=0-1); while the ligand has a good planar structure with strong hydrogen bonds. The fluorescence spectra exhibits that the Tb (III) complex and the Eu (III) complex display characteristic metal-centered fluorescence in solid state while ligand fluorescence is completely quenched. However, the Tb (III) complex displays more effective luminescence than the Eu (III) complex, which is attributed to especial effectivity in transferring energy from the lowest triplet energy level of the ligands (T) onto the excited state (5D4) of Tb (III) than that (5D1) of Eu (III).
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PMID:Synthesis, characterization and luminescence property of N,N'-di(pyridine N-oxide-2-yl)pyridine-2,6-dicarboxamide and corresponding lanthanide (III) complexes. 1683 6

Simultaneous uptake of Ni2+, NH4+, and PO4(3-) by amorphous CaO-Al2O3-SiO2 (C-A-S) compounds was investigated using batch and column methods. Fifteen different C-A-S samples with systematically varied chemical compositions were prepared by coprecipitation from ethanol-water solutions containing Ca(NO3)2.4H2O, Al(NO3)3.9H2O, and Si(OC2H5)4, using NH4OH as the precipitating agent. The resulting precipitates were dried and heated at various temperatures to produce the C-A-S samples, which were then characterized by XRD, FTIR, solid state MAS NMR, DTA-TG, and N2 adsorption. All the C-A-S samples prepared at 600-900 degrees C were amorphous, apart from the CaO-rich samples. Simultaneous uptake of Ni2+, NH4+, and PO4(3-) was determined by a batch method using a solution with an initial concentration of 2 mM. In these experiments, the uptake abilities of the C-A-S samples for Ni2+ and PO4(3-) were high, but were relatively low for NH4+. The uptake abilities for Ni2+ and PO4(3-) increased but that for NH4+ decreased as the silica content in the C-A-S decreased, suggesting that similar uptake mechanisms (ion substitution and/or precipitation) are operating for Ni2+ and PO4(3-), but the uptake mechanism for NH4+ is different (physical adsorption). The column experiments indicate that the order of uptake ability of C-A-S for the three ions is NH4+ << PO4(3-) < Ni2+. Although the silica content of the C-A-S does not have the expected influence on the uptake of these three ions, for NH4+ it plays an important role in the formation of the amorphous phase and also in the suppression of Ca2+ and/or Al3+ release from the C-A-S during the uptake experiments. The optimum uptake properties of the C-A-S can thus be controlled by adjusting the chemical compositions and heating conditions under which the samples are prepared.
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PMID:Simultaneous uptake of Ni2+, NH4+ and PO4(3-) by amorphous CaO-Al2O3-SiO2 compounds. 1706 11

A novel cetyltrimethyl ammonium silver bromide (CTASB) complex has been prepared simply through the reaction of silver nitrate with cetyltrimethyl ammonium bromide (CTAB) in aqueous solution at room temperature by controlling the concentration of CTAB and the molar ratio of CTAB to silver nitrate in the reaction solution, in which halogen in CTAB is used as surfactant counterion. The structure and thermal behavior of cetyltrimethyl ammonium silver bromide have been investigated by using X-ray diffraction (XRD), infrared spectroscopy (IR), X-ray photoelectron spectroscopy (XPS), UV/vis spectroscopy, thermal analysis (TG-DTA), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). The results show that the complex possesses a metastable layered structure. Upon heating the CTASB aqueous dispersion to above 80 degrees C, the structure change of the complex took place and CTAB-capped nanosized silver bromide particles further formed.
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PMID:A novel cetyltrimethyl ammonium silver bromide complex and silver bromide nanoparticles obtained by the surfactant counterion. 1718 88

The binuclear complex of Schiff base C14H12NO3K(KHL) derived from 2-hydroxy-l-naphthaldehyde and beta-alanine with lanthanide nitrate was synthesized and characterized by elemental analysis, IR, UV, TG-DTA, and molar conductance analysis. The composition of the complex was [La2(L)2 (NO3)2] x 2C2H5OH. The interaction of the complex and DNA was studied by fluorescence spectrum. The result indicates that the La(III) complex could cause a sharp decrease in the fluorescence intensity of EB-DNA system, and the complex could partly sustain the place of EB.
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PMID:[Synthesis and characterization of La(III) binuclear complex with 2-hydroxy-l-naphthaldehyde-beta-alanine and its interaction with DNA]. 1736 27

The hydration of tricalcium silicate (C(3)S) in the presence of heavy metal is very important to cement-based solidification/stabilisation (s/s) of waste. In this work, tricalcium silicate pastes and aqueous suspensions doped with nitrate salts of Zn(2+), Pb(2+), Cu(2+) and Cr(3+) were examined at different ages by X-ray powder diffraction (XRD), thermal analysis (DTA/TG) and (29)Si solid-state magic angle spinning/nuclear magnetic resonance (MAS/NMR). It was found that heavy metal doping accelerated C(3)S hydration, even though Zn(2+) doping exhibited a severe retardation effect at an early period of time of C(3)S hydration. Heavy metals retarded the precipitation of portlandite due to the reduction of pH resulted from the hydrolysis of heavy metal ions during C(3)S hydration. The contents of portlandite in the control, Cr(3+)-doped, Cu(2+)-doped, Pb(2+)-doped and Zn(2+)-doped C(3)S pastes aged 28 days were 16.7, 5.5, 5.5, 5.5, and <0.7%, respectively. Heavy metals co-precipitated with calcium as double hydroxides such as (Ca(2)Cr(OH)(7).3H(2)O, Ca(2)(OH)(4)4Cu(OH)(2).2H(2)O and CaZn(2)(OH)(6).2H(2)O). These compounds were identified as crystalline phases in heavy metal doping C(3)S suspensions and amorphous phases in heavy metal doping C(3)S pastes. (29)Si NMR data confirmed that heavy metals promoted the polymerisation of C-S-H gel in 1-year-old of C(3)S pastes. The average numbers of Si in C-S-H gel for the Zn(2+)-doped, Cu(2+)-doped, Cr(3+)-doped, control, and Pb(2+)-doped C(3)S pastes were 5.86, 5.11, 3.66, 3.62, and 3.52. And the corresponding Ca/Si ratios were 1.36, 1.41, 1.56, 1.57 and 1.56, respectively. This study also revealed that the presence of heavy metal facilitated the formation of calcium carbonate during C(3)S hydration process in the presence of carbon dioxide.
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PMID:Characterisation of products of tricalcium silicate hydration in the presence of heavy metals. 1741 62


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