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Abstract  

Parent and mixed ligand complexes of cobalt and copper with antipyrine derivatives of 1,2-ethanediamine or piperazine and with 2-aminobenzothiazole (TAB) were synthesized and their thermal behaviour was investigated. The complexes contain N,N′-bis(4-antipyrylmethyl)-piperazine (BAMP) or N,N′-tetra(4-antipyrylmethyl)-1,2-diaminoethane (TAMEN) or/and TAB as ligand, and Cl, ClO4 or SCN. The complexes decompose with the evolution of heat. The decomposition route depends on the presence of ClO4 . If the ClO4 is not coordinated, it oxidizes the TAB and BAMP or TAMEN and the decomposition is explosive.

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Abstract  

The thermal behaviour of the mixed-ligand complexes of cobalt(II) and copper(I) ions with antipyrine derivatives of 1,2-ethanediamine or piperazine (BAMP and TAMEN), with water and with 2-mercapto-benzothiazole (Hmbt) was investigated. The complexes contain 2-mercaptobenzothiazole (Hmbt, in the case of cobalt(II) ion) or dimercaptobenzothiazine (mbt–mbt, in the case of copper(I) ion) molecules as ligands and perchlorate (ClO4 ) or thiocyanate (SCN – ) ion as counterion. By heating, water and ligands release the solid phase at lower temperature. At higher temperatures process of different organic reactions of ligands (e.g. polymerization, polycondensation) could be suggested to interpret the relative high final mass values.

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Journal of Thermal Analysis and Calorimetry
Authors: H. El-Boraey, F. El-Saied, and S. Aly

Abstract  

UO2(VI), Sn(IV), Th(IV) and Li(I) complexes of 4-azomalononitrile antipyrine (L) have been isolated and characterized based on IR spectra, 1H NMR, elemental analyses, molar conductance and thermal analysis (DTA/TG). The study revealed that the ligand behaves as a neutral bidentate one and coordination takes place via the carbonyl atom of pyrazolone ring >C=O and the azomethine nitrogen >C=N. The thermal stability of the metal complexes were investigated by thermogravimetry (TG), differential thermal analysis (DTA) techniques and infrared spectra, and correlated to their structure. The thermal study revealed that Th(IV) complexes show lower thermal stability than both UO2(VI) and Sn(IV) complexes.

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Abstract

Aim: To evaluate endogenous toxic substrates and liver monooxygenase function in cardiosurgical patients with multiple organ dysfunction syndrome (MODS). Methods: 45 patients with MODS and 34 patients with an uneventful postoperative period were studied. The endogenous substrates were quantified with blood middle molecules (MM). Liver monooxygenase function was evaluated with antipyrine (AP) pharmacokinetics. Results: On the first postoperative day, MODS patients were characterized by high concentration of toxic substrates (MM: +43.8%) and a significant decrease in liver monooxygenase function (AP clearance: −44%), while controls patients had a mild increase in endogenous substrates and a slight depression in monooxygenase function. On the 3rd–4th postoperative day, in the main group, endogenous substrates increased (MM: +53.1%), while in the control group toxic substrates decreased (MM: +6.9%). In both groups, an increase in liver monooxygenase function was noticed. Major differences were observed on the 10th–12th postoperative day. In the main group, toxic substrates remained elevated (MM: +37.5%) and monooxygenase function was depressed (AP clearance: −45.4%), while in the control group endogenous substrates and monooxygenase function were equal to the baseline. The correlation analysis showed a negative relationship between AP pharmacokinetics and endogenous substrates. Conclusion: Slowdown in liver microsomal oxidation is one of the main reasons for the accumulation of endogenous toxic substrates in MODS cardiac patients.

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Summary Thermally carbonised mesoporous silicon microparticles were produced and loaded with two active pharmaceutical ingredients, ibuprofen and antipyrine. By combining the results measured with TG and DSC, reliable estimations for the degrees of the drug loads were obtained. To distinguish the drug adsorbed on the surfaces of the microparticles from that absorbed into the pores, the principle of thermoporometry on the DSC measurements was employed. According to the principle, the drug held in the capillaries of porous material has a depressed melting temperature because of the higher pressure of the drug in cavities with a curved interface. On the other hand, the drug located on the external surface of the microparticles exhibits the normal melting of bulk drug. The loading degrees obtained with the thermoanalytical methods (31 and 26 mass& for ibuprofen and antipyrine, respectively) were comparable with the results obtained with helium pycnometry (the corresponding values were 33 and 28 mass&). Nitrogen sorption studies were not reliable for quantitative determinations due to the inability of nitrogen to penetrate in all pores, which might be blocked by the drug on the surface of the microparticles.

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Abstract  

Parent and mixed ligand complexes of cobalt(II) and copper(II) ions with N,N'-bis- (4-antipyrylmethyl)piperazine or N,N'-tetra(4-antipyryl-methyl)-1,2-diaminoethane or/and imidazole as ligand and ClO4 - or SCN- as counterion were synthesised and their thermal behaviour was investigated.

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Journal of Thermal Analysis and Calorimetry
Authors: Viorel Sasca, Elena Mosoarca, Livia Avram, Ramona Tudose, and Otilia Costisor

Abstract  

The thermal decomposition of Mannich base N,N′-tetra(4-antipyrylmethyl)-1,2-diaminoethane (TAMEN), and its Ni(II), binuclear complex, Ni2(TAMEN)Cl4, in air and in nitrogen atmosphere, were investigated. X-ray powder diffractometry, infrared spectroscopy and simultaneous thermogravimetry-differential thermal analysis (TG-DTA), have been used to characterize and to study the thermal behavior of these compounds. The results provided information concerning the stoichiometry, crystallinity, thermal stability and decomposition mechanism of the compound.

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Summary  

Thorium was extracted quantitatively with the neutral ligand 1-phenyl-2,3-dimethyl-5-pyrazolone (Apy) in the presence of perchlorate (ClO4 -) and di/trichloroacetates (DCA/TCA) at pH 2.5 into an organic solvent. Optimization of experimental parameters like pH, equilibration time, solvents, reactant concentrations, best suited conditions for back extraction, interference due to the presence of different anions and cations and effect of metal ion concentration were studied. The composition of the complexes has been established using log-log plots and are represented as [Th(Apy)2(ClO4)4], [Th(Apy)2(TCA)4], [Th(Apy)(H2O)(DCA)4]. The respective conditional stability constants of the effectively extracted complexes have also been calculated as 9.4±0.03 and 10.4±0.04, respectively . The method has been extended for the separation of thorium from a number of cations in binary and multicomponent mixtures. The method is simple, rapid, selective and has a good reproducibility (±0.5%).

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Abstract  

This project investigated the interaction between poly-L-lactic acid (PLLA) and several therapeutic agents. Low percentage crystallinity PLLA (melt-pressed, molded and drawn) was studied. X-ray diffraction (XRD) and differential scanning calorimetry (DSC) were used to characterize the crystallinity and thermal properties in a thermal cycling process. Repeatable melting and crystallization events were observed. The thermal properties of a drug-polymer combination using PLLA and an acidic, basic, neutral and zwitterionic material were investigated. A sufficient quantity of the drug must be present in the polymer to be observed thermally. Release of atropine sulfate from a PLLA tablet showed a two-phase process.

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Abstract  

Thorium(IV) reacts with 1-(2-thiazolylazo)-2-naphthol (TAN) in the presence of antipyrine to form a sparingly soluble red-coloured chelate, soluble in 36% methanol (v/v). Complexation takes place instantaneously at pH 2.4–2.8, maintained by glycine buffer. Antipyrine is found to enhance sensitivity of the complex, which is stable for 19 hours. The 12 complex exhibits maximum absorbance at 555 nm, obyes Beer's law in the concentration range from 0.32 to 6.56 g of thorium(IV) per ml, has a molar absorptivity of 3.14·104 dm3/mol–1·cm–1 and a Sandel sensitivity of 7.4 ng·cm–2. The formation constant (log K) is found to be 8.62 and 8.45. Interference of 57 anions and cations in the determination of thorium(IV) has been studied. From ten repeated determinations, the coefficient of variation was found to be ±0.98%. The method was successfully applied for determination of thorium content in a sample of monazite.

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