Synthesis, characterization and thermal studies on solid 3-methoxybenzoate of some bivalent transition metal ions

Solid-state M-3-MeO-Bz compounds, where M stands for bivalent Mn, Co, Ni, Cu and Zn and 3-MeO-Bz is 3-methoxybenzoate, have been synthesized. Simultaneous thermogravimetry and differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), X-ray powder diffractometry, infrared spectroscopy, and chemical analysis were used to characterize and to study the thermal behaviour of these compounds. The results led to information about the composition, dehydration, thermal stability and thermal decomposition of the isolated compounds.

Synthesis, characterization and thermal behaviour of solid-state compounds of 2-methoxybenzoate with some bivalent transition metal ions

Solid-state M-2-MeO-Bz compounds, where M stands for bivalent Mn, Co, Ni, Cu and Zn and 2-MeO-Bz is 2-methoxybenzoate, have been synthesized. Simultaneous thermogravimetry-differential thermal analysis (TG-DTA), thermogravimetry, derivative thermogravimetry (TG/DTG), differential scanning calorimetry (DSC), X-ray powder diffractometry, infrared spectroscopy and complexometry were used to characterize and to study the thermal behaviour of these compounds. The results led to have information about the composition, dehydration, thermal stability and thermal decomposition of the isolated compounds.

Synthesis, characterization and thermal behaviour of solid-state compounds of 4-methoxybenzoate with lanthanum (III) and trivalent lighter lanthanides

Solid-state M-4-MeO-Bz compounds, where M stands for trivalent La, Ce, Pr, Nd and Sm and 4-MeO-Bz is 4-methoxybenzoate, have been synthesized. Simultaneous thermogravimetry and differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), X-ray powder diffractometry, infrared spectroscopy and complexometry were used to characterize and to study the thermal behaviour of these compounds. The results led to information about the composition, dehydration, polymorphic transformation, ligand's denticity, thermal behaviour and thermal decomposition of the isolated compounds.

Synthesis, characterization and thermal studies on solid state 3-methoxybenzoate of lighter trivalent lanthanides

Solid-state Ln -3-MeO-Bz compounds, where Ln stands for lighter trivalent lanthanides (La Sm) and 3-methoxybenzoate, have been synthesized. Thermogravimetry (TG), differential scanning calorimetry (DSC), X-ray powder diffractometry, infrared spectroscopy, and complexometry were used to characterize and to study the thermal behaviour of these compounds. The results led to information concerning the composition, dehydration, polymorphic transformation, thermal behaviour and thermal decomposition of the synthesized compounds.

Synthesis, characterization and thermal behaviour on solid pyruvates of light trivalent lanthanides

Solid State Ln-L compounds, where Ln stands for light trivalent lanthanides (La - Gd) and L is pyruvate, have been synthesized. Thermogravimetry and derivative thermogravimetry (TG/DTG), differential scanning calorimetry (DSC), X-Ray powder diffractometry, infrared spectroscopy, elemental analysis, and complexometry were used to characterize and to study the thermal behaviour of these compounds. The results led to information about the composition, dehydration, ligand denticity, thermal behaviour and thermal decomposition of the isolated compounds.

Synthesis and characterization of activated carbon fibers from Kevlar

Kevlar [poly (p-phenilylene terephtalamide)], was used as a precursor in the preparation of activated carbon fibers. For this intention, physical and chemical activations were carried out. Activated fibers were physically prepared from the carbonization of the Kevlar and its later activation with CO2 and steam of water, by the other hand; the chemically activated fibers were obtained by means of the impregnation of the material with phosphoric acid and their later carbonization. Different conditions were used and preliminary analyses of the precursor were taken into account (TGA-DTA / IR). The resulting fibers were characterized by N2 (77K) adsorption, infrared spectroscopy, SEM, and immersion calorimetry. Yields and Burn off were also evaluated. The results shows that if you want to synthesize activated carbon fibers from Kevlar strong conditions respect to the commonly used such as water steam, high phosphoric acid concentrations and methods of impregnation are the ones who allows the development of optimal surface areas and pore volumes.

Thermal behavior of corn starch granules modified by acid treatment at 30 and 50°C

Unprocessed native starches are structurally too weak and functionally too restricted for application in today's advanced food technologies. Processing is necessary to engender a range of functionality. Naturals or natives starches can be modified by using several methods physical, chemical, enzymatic or combined, according industrial purposes. In this work, native corn starch was hydrolyzed by hydrochloric acid solution and investigated by using thermoanalytical techniques (thermogravimetry - TG, differential thermal analysis - DTA and differential scanning calorimetry - DSC), as well as optical microscopy and X-ray diffractometry. After acid treatment at 30 and 50°C, a decrease of gelatinization enthalpy (ΔHgel) was verified. Optical microscopy and X-ray diffractometry allowed us to verify the granules contorn and rugosity typical of cereal starches.

Synthesis and characterization of solid 2-methoxycinnamylidenepyruvic acid

The 2-methoxycinnamylidenepyruvic acid (2-MeO-HCP) was synthesized and characterized for nuclear magnetic resonance (¹H and 13C NMR), mass spectrometry (MS), Infrared spectroscopy (FTIR) and differential scanning calorimetry (DSC). The application of DSC for purity determination is well documented in literature and is used in the analysis of pure organic compounds. The molecular geometry and vibrational frequencies of 2-MeO-HCP have been calculated.

Thermoanalytical study and characterization of native starches of Paraná pine seeds (Araucaria angustiofolia, Bert O. Ktze) and European chestnut seeds (Castanea sativa, Mill)

Starch is the most important carbohydrate storage in plants. It is a raw material with diverse botanical origins, and is used by the food, paper, chemical, pharmaceutical, textile and other industries. In this work, native starches of Paraná pine seeds (pinhão) (Araucária angustiofolia, Bert O. Ktze) and european chestnut seeds (Castanea sativa, Mill) were studied by thermoanalytical techniques: thermo-gravimetry (TG), differential thermal analysis (DTA) and differential scanning calorimetry (DSC), as well as X-ray powder patterns diffractometry. Apparent and total amylose content was also determined.

Synthesis, characterization and thermal behaviour on solid pyruvates of some bivalent metal ions

Solid state M-L compounds, were M stands for bivalent Mn, Fe, Co, Ni, Cu, Zn and L is pyruvate, have been synthesized. Thermogravimetry and derivative thermogravimetry (TG/DTG), differential scanning calorimetry (DSC), X-Ray powder diffractometry, infrared spectroscopy, elemental analysis, and complexometry were used to characterize and to study the thermal behaviour of these compounds. The results led to information about the composition, dehydration, ligand denticity, and thermal decomposition of the isolated compounds.

Thermal stability and thermal decomposition of sucralose

Several papers have been described on the thermal stability of the sweetener, C12H19Cl3O8 (Sucralose). Nevertheless no study using thermoanalytical techniques was found in the literature. Simultaneous thermogravimetry and differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC) and infrared spectroscopy, have been used to study the thermal stability and thermal decomposition of sweetener.

Synthesis, characterization and thermal behaviour of solid 2-methoxycinnamylidenepyruvate of some bivalent metal ions in CO2 and N2 atmospheres

Solid State M-2-MeO-CP compounds, where M stands for bivalent metals (Mn, Fe, Co, Ni, Cu and Zn) and 2-MeO-CP is 2-methoxycinnamylidenepyruvate, were synthesized. Simultaneous thermogravimetry and differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), elemental analysis and complexometry were used to establish the stoichiometry and to study the thermal behaviour of these compounds in CO2 and N2 atmospheres. The results were consistent with the general formula: M(L)2∙H2O. In both atmospheres (CO2, N2) the thermal decomposition occurs in consecutive steps which are characteristic of each compound. For CO2 atmosphere the final residues were: Mn3O4, Fe3O4, Co3O4, NiO, Cu2O and ZnO, while under N2 atmosphere the thermal decomposition is still observed at 1000 º C.

Synthesis, characterization and thermal behaviour of heavy trivalent lanthanide malonates

Solid-state Ln-L compounds, where Ln stands for heavy trivalent lanthanides (Tb-Lu) and L is malonate, have been synthesized. Simultaneous thermogravimetry and differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), X-ray powder diffractometry, infrared spectroscopy, TG-FTIR system, elemental analysis and complexometry were used to characterize and to study the thermal behaviour of these compounds. The dehydration of the compounds begins at 303 K and the anhydrous compounds are stable up to 548 K. The results also provided information concerning the ligand's denticity, thermal behaviour and identification of some gaseous products evolved during the thermal decomposition of these compounds.

Characterization of ß-trypsin at acid pH by differential scanning calorimetry

Trypsin is a serino-protease with a polypeptide chain of 223 amino acid residues and contains six disulfide bridges. It is a globular protein with a predominance of antiparallel ß-sheet and helix in its secondary structure and has two domains with similar structures. We assessed the stability of ß-trypsin in the acid pH range using microcalorimetric (differential scanning calorimetry) techniques. Protein concentrations varied in the range of 0.05 to 2.30 mg/ml. Buffer solutions of 50.0 mM ß-alanine and 20.0 mM CaCl2 at different pH values (from 2.0 to 4.2) and concentrations of sorbitol (1.0 and 2.0 M), urea (0.5 M) or guanidinium hydrochloride (0.5 and 1.0 M) were used. The data suggest that we are studying the same conformational transition of the protein in all experimental situations using pH, sorbitol, urea and guanidinium hydrochloride as perturbing agents. The observed van't Hoff ratios (deltaHcal/deltaHvH) of 1.0 to 0.5 in the pH range of 3.2 to 4.2 suggest protein aggregation. In contrast, deltaHcal/deltaHvH ratios equal to one in the pH range of 2.0 to 3.2 suggest that the protein unfolds as a monomer. At pH 3.00, ß-trypsin unfolded with Tm = 54ºC and deltaH = 101.8 kcal/mol, and the change in heat capacity between the native and unfolded forms of the protein (deltaCp) was estimated to be 2.50 ± 0.07 kcal mol-1 K-1. The stability of ß-trypsin calculated at 298 K was deltaG D = 5.7 kcal/mol at pH 3.00 and deltaG D = 15.2 kcal/mol at pH 7.00, values in the range expected for a small globular protein.

Comparison of the homeostasis model assessment and quantitative insulin sensitivity check index with data from forearm metabolic studies for the in vivo assessment of insulin sensitivity

The present study was designed to compare the homeostasis model assessment (HOMA) and quantitative insulin sensitivity check index (QUICKI) with data from forearm metabolic studies of healthy individuals and of subjects in various pathological states. Fifty-five healthy individuals and 112 patients in various pathological states, including type 2 diabetes mellitus, essential hypertension and others, were studied after an overnight fast and for 3 h after ingestion of 75 g of glucose, by HOMA, QUICKI and the forearm technique to estimate muscle uptake of glucose combined with indirect calorimetry (oxidative and non-oxidative glucose metabolism). The patients showed increased HOMA (1.88 ± 0.14 vs 1.13 ± 0.10 pmol/l x mmol/l) and insulin/glucose (I/G) index (1.058.9 ± 340.9 vs 518.6 ± 70.7 pmol/l x (mg/100 ml forearm)-1), and decreased QUICKI (0.36 ± 0.004 vs 0.39 ± 0.006 (µU/ml + mg/dl)-1) compared with the healthy individuals. Analysis of the data for the group as a whole (patients and healthy individuals) showed that the estimate of insulin resistance by HOMA was correlated with data obtained in the forearm metabolic studies (glucose uptake: r = -0.16, P = 0.04; non-oxidative glucose metabolism: r = -0.20. P = 0.01, and I/G index: r = 0.17, P = 0.03). The comparison of QUICKI with data of the forearm metabolic studies showed significant correlation between QUICKI and non-oxidative glucose metabolism (r = 0.17, P = 0.03) or I/G index (r = -0.37, P < 0.0001). The HOMA and QUICKI are good estimates of insulin sensitivity as data derived from forearm metabolic studies involving direct measurements of insulin action on muscle glucose metabolism.