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Journal of Thermal Analysis and Calorimetry
Authors: Ticiano do Nascimento, Irinaldo Basílio Júnior, Rui Macêdo, Elisana Moura, Camila Dornelas, Vanderson Bernardo, Vânia Rocha, and Csaba Nóvak

Abstract  

This article characterizes the stability of indinavir sulfate using different analytical techniques of quality control to evaluate important steps in the manufacturing process of indinavir, specifically involving storage and compression. Indinavir A, B, and C were obtained from different suppliers and submitted to DSC, Karl Fisher, NIR, XRPD analyses and dissolution assay. DSC curves of indinavir presented endothermic peaks of fusion at 149–150 °C for indinavir A and B (form I) and 139–143 °C for indinavir C (form II). When indinavir A and B were submitted to high Relative Humidity (RH) pseudo-polymorphic form II was formed. Indinavir C converted into an amorphous substance when submitted to compression. Near infrared and Karl Fisher assays detected high values of water for indinavir C in relation to indinavir A and B. X-ray powder diffraction of indinavir B and C showed displacement of 0.05–0.10 θ in the peaks and higher angle of diffraction in relation to indinavir A. Amorphous indinavir C demonstrated a higher intrinsic dissolution rate than indinavir A and B. Indinavir form I should be monitored during the pharmaceutical process to avoid its conversion to indinavir form II or an amorphous substance which can alter the dissolution rate.

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Acta Chromatographica
Authors: M. Pacenti, S. Dugheri, R. Gagliano-Candela, G. Strisciullo, E. Franchi, F. Degli Esposti, N. Perchiazzi, P. Boccalon, G. Arcangeli, and V. Cupelli

Summary

2-Chloroacetophenone (CA) is widely used as tear gas by law-enforcement agents, and by civilians for personal protection. Crimes involving robbery and rape using tear gas sprays have recently increased. Experimental and in-field evaluations have been performed to validate use of solid-phase microextraction (SPME) with a porous fiber for sampling and analysis of CA in air before analysis by fast gas chromatography-mass spectrometry equipped with a new device called a multi-fiber system. CA vapor was generated by use of a syringe pump in a dynamic system in which temperature, relative humidity, and air velocity were monitored. The theoretical sampling rate for time-weighted average and rapid-SPME were, furthermore, estimated by use of the Fuller-Schettler-Giddings diffusion coefficient and the theory of heat transfer, respectively, and were in accordance with experimental values. Concentrations of CA were analyzed in a military store containing tear gas canisters, to evaluate the risk. The results obtained in this field study showed values ranging from 0.206 to 2.46 mg m−3.

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Abstract  

The system of sulfoaluminate ferrite belite (SAFB) clinkers premixed with Portland cement (PC) in mass ratio 85:15 in combination with hydroxypropylmethyl cellulose (HPMC) or polyphosphates(poly-P) was used for the syntheses of Macro-Defect-Free (MDF) materials. The subsequent moisture treatment and thermal stability of these MDF materials were investigated. The effect of individual humidity upon the evolution of mass is more intensive than the effects of composition of MDF materials or duration of the original MDF material synthesis. Detailed values of mass changes at 100% relative humidity (RH) and under ambient conditions are strongly affected by the nature of polymer used. A significant improvement of moisture resistance of MDF materials is achieved when the materials are dried after 24 h of finishing the pressure application. In the inter-phase section of MDF material samples, the content ofC-(A,F)-S hydraulic phases, mainly tetracalcium aluminate ferrite monosulphatehydrate (AFm) decomposing by 250°C and CaCO3 decomposing at 600–700°C increase after the moisture attack, while cross-links in AFm-like section with typical thermoanalytical traces in temperature region 250–550°C remain intact.

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Abstract

These days, the investigations of the physical properties of the insulating materials are very important. In this paper we report the measured water uptaking capabilities of a thermal insulating paint. They can be found in liquid phase, but we measured dried solid samples. The thin thermal insulators (insulator coatings) are starting to spread on the market of the building materials. The proper understanding of sorption behavior of the materials is important from the applied building technology point of view. Moisture sorption and desorption measurements were carried out on two samples with different geometry by using climatic chamber method. After drying the samples at 90 °C for one hour in the Venticell 111 type drying equipment they were wetted with a Climacell 111 type climate chamber, where the relative humidity (RH) was varied from 25% to 90% at 293 K for 2 hours. The samples were wetted for 2 and 4 hours as well. Sorption and desorption as well as kinetic curves are presented in this paper.

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The biology of Sesamia inferens (Walker) was studied at 25±1 °C and 70±5 per cent relative humidity on PMH 1 maize hybrid. The incubation period was 6.82±0.05 days. There were six larval instars and the larval development was completed in 29.95±0.16 days. The duration of instars I-VI was 4.17±0.09, 3.60±0.08, 4.47±0.02, 4.40±0.03, 6.18±0.06 and 7.13±0.05 days, respectively. The pre-pupal period was 2.83±0.02 days. The male and female pupa had duration of 8.05±0.12 days and 10.33±0.16 days, respectively. The adult emergence was 93.02±0.01 per cent, with a sex ratio of 1:1.05. The males had shorter longevity of 3.92±0.23 days, while females had 5.05±0.28 days. The pre-oviposition, oviposition and post-oviposition period was 1.11±0.10, 2.96±0.19 and 0.79±0.10 days, respectively. The fecundity was 211.92 ±11.92 eggs with 53.69±10.78 eggs per cluster. The egg hatchability was 92.19±0.01 per cent. The total life cycle was completed in 47.65±0.24 days (Male) and 49.93±0.21 days (female). The observations on the biology will help in developing efficient strategies to manage S. inferens on maize in the north western plains of India.

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Abstract  

The reactivity of MgO obtained from calcination of magnesium carbonate at different temperatures has been investigated by means of hydration in a constant relative humidity environment at 40°C for periods up to 24 days. Natural magnesite and AR grade basic MgCO3 calcined in the range of 500–1000°C was characterised in terms of surface area, crystallite size, morphology, and hydration rate. It was found that the hydration rate is dependent on the surface area and crystallite size where temperature was the main variable affecting them. The most reactive MgO was produced at the lowest calcination temperature with the highest surface area and the smallest crystallite size. The basic MgO specimens showed higher degree of hydration compared to the natural MgO specimens due to the smaller surface area and larger crystallite size. The low MgO content of the starting natural magnesite is also attributable to the lower reactivity. This preliminary study serves as a mean to investigate potential utilisation of reactive MgO as a supplementary cementitious material in eco-friendly cements.

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The effect of sprouting of onions on total phenolic content, antioxidant activity, and anthocyanin profile of freeze dried powders produced from Indian onion cultivars was examined. Sprouting was carried out at an average light intensity of 64 Lumen, average relative humidity of 80.2%, and average temperature of 15.22 °C for three weeks. Two way analyses of data revealed significant (P<0.05) effect of sprouting and cultivar on functional composition of freeze dried powders. In all sprouted powder samples, there were significant (P<0.05) enhancements in total phenolic content, total flavonoid content, vitamin C content, antioxidant activity, and colour due to increase in anthocyanin contents. The anthocyanin profile depicted an increase in total anthocyanin concentration in powders developed from all four cultivars with the highest increase in powder from PRO-6 (23.87–27.15 mg kg−1), followed by Punjab Naroya (9.97–12.92 mg kg−1), commercial (7.15–8.43 mg kg−1), and Punjab White cultivar (3.45–4.09 mg kg−1).

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Abstract  

MDF cements using the blends of sulfoaluminate ferrite belite (SAFB) clinkers and ordinary Portland cement (OPC) in mass ratio 85:15 with Al2O3, and starch, polyphosphate (poly-P) or butylacrylate/acrylonitrile were subjected to moist atmospheres (ambient, 52 and 100% relative humidity (RH)) to investigate their moisture resistance. Their chemical, thermal, electron microscopic and magnetic properties were also studied before and after moisture attack. Butylacrylate/acrylonitrile (BA/AN) copolymer was found to be the most suitable for MDF cement synthesis since the sample containing BA/AN showed the best moisture resistant. There are significant differences in scanning electron microscopy (SEM) of MDF cements before and after moisture attack and with different polymers. New data on the paramagnetic nonhysteresis magnetization curves for all the samples are observed. The MDF cements synthesized from SAFB clinker with dissolved poly-P give the best signal/noise (S/N) ratio. Three main temperature regions on TG curves of both series of MDF cements are observed. In the inter-phase section of MDF cements, the content of classical cement hydrates decomposing by 250C is increased. Combustion of organic material took place by 550C. In the temperature range 550-800C, the decomposition of CaCO3 occurs.

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Journal of Thermal Analysis and Calorimetry
Authors: D. Giron, Ch. Goldbronn, M. Mutz, S. Pfeffer, Ph. Piechon, and Ph. Schwab

Abstract  

Manufacturing processes may involve the presence of water in the crystallization of the drug substance or in manufacturing or in the composition of the drug product through excipients. Dehydration steps may occur in drying, milling, mixing and tabletting processes. Furthermore, drug substances and drug products are submitted to different temperatures and relative humidities, due to various climatic conditions giving rise to unexpected hydration or dehydration aging phenomena. Therefore the manufacture and the characterization of hydrates is part of the study of the physical properties of drug substances. Several hydrates and even polymorphic forms thereof can be encountered. Upon dehydration crystal hydrates may retain more or less their original crystal structure, they can lose crystallinity and give anamorphous phase, they can transform to crystalline less hydrated forms or to crystalline anhydrous forms. The proper understanding of the complex polyphasic systemhydrates–polymorphs–amorphous state needs several analytical methods. The use of techniques such as DSC-TG, TG-MS, sorption-desorption isotherms, sub-ambient experiments, X-ray diffraction combined with temperature or moisture changes as well as crystal structure and crystal modelling in addition to solubilities and dissolution experiments make interpretation and quantitation easier as demonstrated with some typical examples.

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Abstract  

The chemical stability of a propellant and its influence on the ballistic properties during aging is a subject of interest. The effect of aging on ballistic properties, viz., ignition delay, burning rate, and heat of combustion for an aluminised ammonium perchlorate–hydroxyl-terminated polybutadiene (AP/HTPB) composite propellant during accelerated aging were investigated. Samples of composite propellants were aged at 60 and 70 °C at relative humidity of 50% in a climatic chamber. The propellant samples were tested with pressurized nitrogen gas environment for ignition delay measurement. Test results indicate that aging does not have any appreciable effect on ignition delay. The change in ignition delay time is less than 3% within the scatter of the data. Experiment results indicate that burn rate do affect with pressure but aging does not have much effect on burn rate. It was also observed that the burning rate at low pressures did not undergo significant changes during the aging period. The most significant of all the ballistic properties of this propellant is the burning rate exponent which increased by about 10% during the aging period.

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