Thermal characterization of lignocellulosic residue from different sugarcanes

Bagasse samples from four different sugarcane were directly collected as the residues of milling in a processing plant. The samples were dried at 105 °C, compressed to small granules and then their TG/DTA and DSC curves in synthetic air were recorded. Similar thermogravimetric curves were obtained for the different samples and they exhibited four mass loss steps. However, the analysis of the exotherm DSC peaks showed that the oxidation of the organic matter resulted different enthalpy values (ΔH/kJ g⁻¹).     

Synthesis,characterization and tg-dsc study of lanthanide trifluoroacetate-2-azacyclononanone compounds

The synthesis, characterization and tg-dsc study of Ln(tfa)₃?·?3aza where Ln?=?La, Pr, Nd, Sm, Eu, Gd, Tb and Er, tfa?=?trifluoroacetate and aza?=?2-azacyclononanone are reported. The obtained X-ray powder diffraction patterns show that the compounds are divided in two isomorphous groups: La, Pr, Nd and Eu, Sm, Gd, Tb and Er. For all compounds, the thermodegradation under nitrogen gave the respective oxifluorides (LnOF) as the final product. The melting temperature intervals are 105–110°C, 100–112°C, 90–95°C, 79–101°C, 65–70°C, 75–90°C, 64–76°C and 50–65°C for the La, Pr, Nd, Sm, Eu, Gd, Tb and Er compounds, respectively, and it is verified that the lanthanide contraction induces a weaker intermolecular interaction between adjacent molecules in the solid state.     

Identification of gamma-irradiated Chinese herbs by thermoluminescence analysis

The feasibility of thermoluminescence (TL) to differentiate irradiated Chinese medicinal herbs from non-irradiated was investigated. Thirty different dried Chinese herbs were tested, including root, flower, ramulus, rhizome, cortex, and whole plant samples. Irradiation of Chinese herbs was associated with strong TL peaks at ~150–250 °C, while TL curves of non-irradiated herbs had very low intensities above 250 °C, which was also confirmed by the TL ratio (non-irradiated, TL₁/TL₂ < 0.1). The ability to determine the irradiation dose by the TL method was influenced by the amount and types of minerals in the samples. All levels of irradiation doses could be detected when between 0.1 and 1.0 kGy, except for three herbs at 0.1 kGy dose. Different blends with small quantities (0.1–10 %) of irradiated herbs were also tested in this study. Samples with powder mixtures containing 1 % irradiated components could be differentiated (TL₁/TL₂ > 0.1) except for sterculia lychnophora, semen cassia, flos inulae, and anemone root. TL ratios of some herbs indicated irradiation (TL₁/TL₂ > 0.1) even if the irradiated components were as low as 0.1 %. Thus we demonstrated that TL analysis had excellent sensitivity and reliability for the identification of irradiated Chinese herbs.     

Thermal analysis of the rice and by-products

The thermogravimetry (TG) is a technique used in the quality control of foods. In this work the moisture and ash contents in the rice and by-products (bran and husk), the thermal stability and the gelatinization process by conventional, thermogravimetric and calorimetric methods were studied. The moisture and ash contents obtained by TG and conventional methods did not present significant differences. The rice presented higher starch content, while the bran presented higher protein content. The thermogravimetric data presented the following thermal stability order: rice>bran>husk. The calorimetric curves indicated the gelatinization of the starch. The kinetic parameters were compatible. This revised version was published online in August 2006 with corrections to the Cover Date.     

Kinetic study of pyrolysis of waste water treatment plant sludge

Activated sewage sludge samples obtained from two different waste water treatment plants were investigated by thermogravimetric analysis. Due to a very high content of water in the sludge samples, these had to be dried at 160°C in an electrical oven in order to remove all adsorbed water. To ensure pyrolysis conditions, nitrogen atmosphere was applied. The pyrolysis decomposition process was carried out in the temperature range from ambient temperature to 900°C at three different heating rates: 2 K min⁻¹, 5 K min⁻¹, 10 K min⁻¹. TGA and DTG curves of the decomposition processes were obtained. Temperature of onset decomposition, final temperature of decomposition, maximum decomposition rate, and decomposition temperature were determined by thermogravimetric analysis for both sludge samples used. The main decomposition process takes place at temperatures in the range from 230°C to 500°C. Above this temperature, there are only small changes in the mass loss which are often attributed to the decomposition of carbonates present in the sewage sludge samples. To determine the apparent kinetic parameters such as the activation energy and the preexponential factor, the so called Friedman isoconversional method was used. Because of the requirements of this method, initial and final parts of the decomposition process, where crossings of the decomposition lines occurred, were cut off. Obtained dependencies of the apparent activation energies and preexponential factors as a function of conversion were used backwards to calculate the modeled decomposition process of sewage sludge and the experimental data were in good accordance with the data obtained by simulation.     

Grafting onto Wool. IX. Graft Copolymerization of Vinyl Monomers by Use of Vanadium Oxyacetylacetonate as Initiator

Methyl methacrylate (MMA), acrylic acid (AAc), and vinyl acetate (VAc) were graft copolymerized onto Himachali wool in an aqueous medium by using vanadium oxyacetyl acetonate as initiator. Graft copolymerization was studied at 45, 55, 65, and 75°C for various reaction periods. The percentage of grafting was determined as functions of concentration of monomers, concentration of initiator, time, and temperature. The maximum percentage of grafting with each monomer occurred at 55°. Several grafting experiments were carried out in the presence of various additives which include HNO3, DMSO, and pyridine. Nitric acid was found to promote grafting of MMA. All these additives had adverse effects on grafting of VAc and AAc. MMA, VAc, and AAc were found to differ in reactivity toward grafting and followed the order MMA > AAc > VAc.     

Physicochemical Properties and Storage Stability of Microencapsulated DHA-Rich Oil with Different Wall Materials

This study aimed to evaluate the physicochemical properties and storage stability of microencapsulated DHA-rich oil spray dried with different wall materials: model 1 (modified starch, gum arabic, and maltodextrin), model 2 (soy protein isolate, gum arabic, and maltodextrin), and model 3 (casein, glucose, and lactose). The results indicated that model 3 exhibited the highest microencapsulation efficiency (98.66 %) and emulsion stability (>99 %), with a moisture content and mean particle size of 1.663 % and 14.173 μm, respectively. Differential scanning calorimetry analysis indicated that the Tm of DHA-rich oil microcapsules was high, suggesting that the entire structure of the microcapsules remained stable during thermal processing. A thermogravimetric analysis curve showed that the product lost 5 % of its weight at 172 °C and the wall material started to degrade at 236 °C. The peroxide value of microencapsulated DHA-rich oil remained at one ninth after accelerated oxidation at 45 °C for 8 weeks to that of the unencapsulated DHA-rich oil, thus revealing the promising oxidation stability of DHA-rich oil in microcapsules.     

Characterization and performance of immobilized amylase and cellulase

The performance of cellulase and amylase immobilized on siliceous supports was investigated. Enzyme uptake onto the support depended on the enzyme source and immobilization conditions. For amylase, the uptake ranged between 20 and 60%, and for cellulase, 7–10%. Immobilized amylase performance was assessed by batch kinetics in 100–300 g/L of corn flour at 65°C. Depending on the substrate and enzyme loading, between 40 and 60% starch conversion was obtained. Immobilized amylase was more stable than soluble amylase. Enzyme samples were preincubated in a water bath at various temperatures, then tested for activity. At 105°C, soluble amylase lost ∼55% of its activity, compared with ∼30% loss for immobilized amylase. The performance of immobilized cellulase was evaluated from batch kinetics in 10 g/L of substrate (shredded wastepaper) at 55°C. Significant hydrolysis of the wastepaper was also observed, indicating that immobilization does not preclude access to and hydrolysis of insoluble cellulose.     

Thermoluminescence analyses of irradiated dried sea foods using different methods of mineral separation

This research was conducted to find the most suitable parameters to separate minerals from irradiated dried shrimps and mussels (0 and 5 kGy) for thermoluminescence analysis using density separation and modified acid hydrolysis (at 50 °C with continuous agitation) methods. Nonirradiated samples gave TL glow curve of low intensity with peak after 300 °C except dried mussel sample, which gave false positive result. This problem was absent in minerals separated by acid hydrolysis. TL ratios of all nonirradiated samples were <0.1 irrespective of method used for mineral separation. Minerals separated from irradiated samples by density separation showed very high intensity of TL glow peak before 200 °C, where results from irradiated dried shrimp samples were better because of good availability of minerals. The minerals separated from irradiated samples by acid hydrolysis showed slightly low TL intensity and glow curve peak was found at about 200 °C. However, acid hydrolysis method was less laborious and required less sample weight as compared to density separation method. TL ratios of all irradiated samples were >0.1 confirming the quality of minerals on TL discs.     

Interaction of the general volatile anesthetic Enflurane with bacteriorhodopsin-DPPC proteoliposomes

Thermal decomposition of dried crystalline powder obtained from titanium(IV) bis(acetylacetonate) diisopropoxide (75% solution in 2-propanol) (1) was monitored by simultaneous TG/DTA, EGA-FTIR and EGA-MS measurements and the results were compared with those of amorphous powder obtained by gelling of acetylacetonate-modified titanium(IV) tetra-isopropoxide at molar ratio of 1:2 in boiling 2-methoxyethanol (2). Thermal degradation of 1 in the temperature range of 25–700°C consists of 5 steps with a total mass loss of 62.5%. EGA by FTIR and MS revealed the release of H₂O below 120°C; followed by an intensive evolution of acetylacetone around 245°C. The release of acetone and acetic acid occurs up to 270°C and that of CO and CO₂ up to 530°C.     

Study of catalytic action of micro-particles and synthesized nanoparticles of CuS on cellulose pyrolysis

The catalytic action of copper sulfide (CuS) micro-particles and as-synthesized nanoparticles was studied on cellulose pyrolysis. The market procured CuS powder was used as micro-particles without any treatment. The CuS nanoparticles were synthesized at ambient temperature by simple wet chemical technique. Before using the micro-particles and nanoparticles for catalytic study, they were comprehensively characterized. The thermal analysis including catalytic properties of both the micro-particles and nanoparticles of CuS on cellulose pyrolysis was studied employing thermogravimetric (TG), differential thermogravimetric, and differential thermal analysis techniques. Prior to the study as catalyst in cellulose pyrolysis, the CuS micro- and nanoparticles were characterized by thermal analysis in inert atmosphere. The TG curves showed two steps and five steps decomposition having total mass loss of 29 and 42 % in case of CuS micro- and as-synthesized nanoparticles, respectively. The catalytic study in cellulose pyrolysis showed that the decomposition commences at temperature 295 °C for pure cellulose, 270 °C for cellulose mixed with 3 % CuS micro-particles and 205 °C for cellulose mixed with 3 % CuS nanoparticles. It clearly showed that the decomposition starting temperature decreased by 65 °C in case of cellulose mixed with CuS nanoparticles compared to cellulose mixed with CuS micro-particles. Thus, CuS nanoparticles act as better catalyst then CuS micro-particles in cellulose pyrolysis. The obtained results are deliberated in details.     

Synthesis of high specific surface area YSZ (ZrO<Subscript>2</Subscript>–8Y<Subscript>2</Subscript>O<Subscript>3</Subscript>) nanocrystalline powder by modified polymerized complex method

In this study high specific surface area yttria-stabilized zirconia (ZrO₂–8Y₂O₃) nanocrystalline powder have been synthesized through “modified polymerized complex (MPC) method”. Zirconium chloride, yttrium nitrate, citric acid and ethylene glycol were polymerized at 80 °C to produce a gel-like mass in which metallic ions were uniformly distributed. During the thermal treatment of dried gel, nanocrystalline YSZ powder was formed. Thermal reactions and phase formation of dried gel were investigated through thermal analysis (DTA/TG) and X-ray diffraction (XRD) analysis, respectively. Chemical bonding and thermal decomposition behavior of dried gel was investigated by FTIR analysis. During decomposition, the nature of the bonding between carboxylate groups and the cations changed from unidentate to bridging at 370 °C and carbonate species were detected at 470 °C. Morphology of powder calcined at 650 °C was analyzed by scanning electron microscope (SEM). YSZ powder with high specific surface area was prepared successfully by this method.     

Crystal forms of a capsaicin derivative analgesic DA-5018

DA-5018 is a new capsaicin derivative and has analgesic effect. The objective of this work was to investigate the existence of polymorphs and pseudopolymorphs of DA-5018 and the transformation of crystal forms. Eight crystal forms of DA-5018 have been isolated by recrystallization and characterized by powder X-ray diffractometry (PXRD), differential scanning calorimetry (DSC), and thermogravimetric analysis (TG). The PXRD and DSC patterns of the eight crystal forms were different respectively. In the dissolution studies in simulated intestinal fluid at 37±0.5°C, the solubility of Form 2 was the highest. And the solubility in water decreased in rank order: Form 2>Form 3>Form 1>Form 5>Form 7>Form 4>Form 6>Form 8. Eight crystal forms were shown to have a good physical stability at room temperature for 60 days.     

Evaluation of solid and submerged fermentations for the production of cyclodextrin glycosyltransferase by Paenibacillus campinasensis H69-3 and characterization of crude enzyme

Cyclodextrin glycosyltransferase (CGTase) is an enzyme that produces cyclodextrins from starch by an intramolecular transglycosylation reaction. Cyclodextrins have been shown to have a number of applications in the food, cosmetic, pharmaceutical, and chemical industries. In the current study, the production of CGTase by Paenibacillus campinasensis strain H69-3 was examined in submerged and solid-state fermentations. P. campinasensis strain H69-3 was isolated from the soil, which grows at 45°C, and is a Gramvariable bacterium. Different substrate sources such as wheat bran, soybean bran, soybean extract, cassava solid residue, cassava starch, corn starch, and other combinations were used in the enzyme production. CGTase activity was highest in submerged fermentations with the greatest production observed at 48–72 h. The physical and chemical properties of CGTase were determined from the crude enzyme produced from submerged fermentations. The optimum temperature was found to be 70–75°C, and the activity was stable at 55°C for 1 h. The enzyme displayed two optimum pH values, 5.5 and 9.0 and was found to be stable between a pH of 4.5 and 11.0.     

High density polyethylene/hydrogenated oligo(cyclopentadiene) blends: Tensile stress-strain behavior

The influence of hydrogenated olio(cyclopentadiene) (HOCP) on tensile mechanical properties of its blends with high density polyethylene (HDPE) has been studied at 20, 80, and 100°C. The nominal stress-strain curves performed at 20°C indicate an increase of the modulus and a conspicuous decrease of the ultimate properties increasing the HOCP content in the blend. Blends with HOCP content > 20%-wt are found to be very fragile at 20°C. These behaviors have been related to the presence of the HOCP-rich phase that has the glass transition at about 55°C. At 20°C the HOCP oligomers act as a hardener for the HDPE. The nominal stress-strain curves performed at 80 and 100°C show a strong decrease of the modulus (compared to the value at 20°C), plastic deformation for all the blends tested, and rupture of HDPE and blend samples at the beginning of the cold-drawing. Moreover, the modulus and the ultimate parameters are found to decrease with the composition. The behaviors at 80 and 100°C have been related to several factors: the higher mobility of HDPE molecules at these temperatures compared to that at 20°C; the HOCP-rich phase that is at temperatures higher than its glass transition, and so it acts as a plasticizer for the HDPE; and the decreases of crystallinity and number of entanglements when the HOCP is added to the HDPE component. ©1995 John Wiley & Sons, Inc.     

The effect of different types of carbon blacks on the rheological and thermal properties of acrylonitrile butadiene rubber

The influence of two types of carbon black filler N330 and N990 (primary particle size 46 nm and >230 nm) on elastomeric composites based on acrylonitrile-butadiene rubber (NBR) have been investigated. The activation energy (E _a) were determined from two high temperature rheokinetic curves (T ₁ = 180 °C and T ₂ = 190 °C). For tensile testing, the compounds with different content of carbon black were vulcanized in a hydraulic press at 150 °C. The stress-strain experiments were performed before and after ageing the specimens in an air-circulating oven at 100 °C for 168 h. The thermal degradation and thermal stability of carbon black filled NBR rubber was investigated by thermogravimetric analysis in a flowing nitrogen atmosphere at a heating rate of 10 °C/min.     

Analytical comparison between unprepared and calcined magnetitum (Cishi)

The phases, chemical composition, surface appearance, crystal size, specific surface and thermal behavior of the unprepared and calcined forms of the mineral Magnetitum (Cishi), used as Chinese traditional medicine, were characterized by using X-ray powder diffraction, scan electron microscopy, inductively coupled plasma-atomic emission spectometry (ICP) and thermogravimetric (TG). The results indicated that after calcination the main phase Fe₃O₄ of the calcined Magnetitum (Duan Cishi) remained, while the Fe₂O₃ phase disappeared. The contents of the harmful chemical elements Cd and Pb were obviously reduced, while the crystal size increased from 24.5 to 35.7 nm and surface loosened. There were different TG curves for unprepared and calcined Magnetitum (Cishi) samples on heating. The former showed two weight-losing steps (at 367.9–422.1°C and 568.8–594.1°C), and the latter only one. These results might serve as a base for quality evaluation of Magnetitum (Cishi). Translated from Chinese Journal of Applied Chemistry, 2005, 22(11) (in Chinese)     

Effect of post-synthetic processing conditions on structural variations and applications of bacterial cellulose

Physicochemical properties of materials can be amended by altering their physical structure through different processing conditions. The present study was conducted to investigate the post-synthesis structural variations and physico-mechanical properties of bacterial cellulose (BC) sheets prepared using different drying methods. Wet BC sheets of the same origin were freeze dried (BC-FD), dried at room temperature (25 °C) (BC-DRT), and dried at elevated temperature (50 °C) (BC-DHT). FE-SEM micrographs revealed that BC-DRT and BC-DHT had a more tightly packed and compact structure than the loosely held fibrils of BC-FD. XRD analysis revealed the relative crystallinity of the BC sample to be 64.60, 59.16, and 47.20 % for BC-DHT, BC-DRT and BC-FD, respectively. The water holding capacity (WHC) of the BC-FD was higher than that of the other two samples. Four consecutive drying and rewetting cycles demonstrated that the WHC of all samples decreased with each cycle. The WHC of BC-DRT and BC-DHT was reduced to almost 0 after the first drying cycle, but the BC-FD samples were able to regain some of their WHC. The tensile strength and elongation modulus were in the order of BC-DHT > BC-DRT > BC-FD. Overall, the results of this study revealed that the post-synthetic processing conditions had a strong effect on the structure and physico-mechanical properties of BC.     

Molecular weight distributions in radiation-induced polymerization. VI. γ-ray-induced polymerization of “dry” styrene in the solid state

The γ-ray-initiated polymerization of styrene in the solid state has been studied over the temperature range ?35°C to ?55°C for samples exhaustively purified and dried to remove residual water (“dry” samples). Comparison with kinetic results previously reported for dry samples in the liquid state indicates a sharp decrease in the rate of polymerization resulting from the liquid to solid state transition. The molecular weight distributions for in-source polymerization at ?35°C and ?40°C are bimodal in nature, and the appearance of a third peak is noticeable at ?47°C and ?55°C. In the case of postpolymerization at ?35°C the molecular weight distribution is bimodal as in the case of in-source samples. In the former case, however, the high molecular weight peak is predominant whereas the low molecular weight peak predominates in the latter. These results have been tentatively attributed to the postulated coexistence of two distinct propagating species which are radical and cationic in nature.     

Determination of Selenium and Tin in Human Brain by Graphite Furnace Atomic Absorption Spectrometry

 A method is reported for measuring Se and Sn in human brain tissue. The patients from whom the samples were taken had no diseases in their central nervous system. Microwave energy was applied to digest the brain samples. The digested samples were analyzed without dilution by transversely heated graphite atomizer for atomic absorption spectrometry with longitudinal Zeeman background correction. The dependence of integrated absorbance on various chemical modifiers has been examined. The most appropriate technique proved to be 5 μl sample injection using 20 μg prereduced palladium-nitrate for Se determination, and 20 μl sample injection applying 10 μg palladium-nitrate + 3 μg magnesium-nitrate for the measurements of Sn. The optimal temperature program was found to be 1200 °C pyrolysis and 2100 °C atomisation temperature for Se and 1500 °C pyrolysis and 2300 °C atomisation temperature for Sn. Accuracy of the applied techniques was tested by the analysis of standard reference materials. The precision was ±5% for Se and ±10% for Sn. The range of recovery values was 85–95% for Se and 95–105% for Sn. The mean Se concentrations in the investigated brain parts ranged from 200 to 700 ng/g, while the Sn concentrations were between 20 and 300 ng/g dry weight. Received October 3, 2000. Revision February 1, 2001.