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Changes in the water content of aluminium sulphate hydrate were investigated gravimetrically at room temperature in air with different relative humidities. The samples conditioned in this way were characterized by thermoanalytical (TG, DTG, DSC) and X-ray diffraction measurements. Industrial aluminium sulphate hydrate obtained by freezing the melt has a partly crystalline structure. After grinding, this material crystallizes during storage. This process requires a humid atmosphere; increasing relative humidity brings about more intensive crystallization.

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Abstract  

The stability of Supersulphated Cement (SSC) is investigated at 95°C when subjected to relative humidities of 100, 53 and 11% of water vapour. Previously [1] investigations at 25, 50, 75°C under the same conditions of humidity reported the stability of ettringite, one of the initial hydration products. At 95°C, decomposition of ettringite, is found at all humidities and is rapid at 100% relative humidity. The hydration products of cement pastes at a water cement ratio of 0.27 were determined by thermogravimetry (TG) and X-ray diffraction (XRD). The formation of the hydragarnet, plazolite is recorded during the decomposition/dehydration process enhanced by possible carbonation. Rehydration studies on the products after storage for up to 9 months were carried out using distilled water and the samples tested for ettringite content. It is concluded that ettringite in SSC is inherently unstable at 95°C.

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The interaction between samples of metallic zinc and water vapour was studied gravimetrically, both in the absence and in the presence of oxygen. The experimental total mass gain vs. time curves exhibited two plateaus, whose heights increased with, elevations both of relative humidity and of temperature. The amount of product retained on the surface after desorption was also determined as a function of time. The product was identified as hydrated zinc oxide. In the runs conducted without oxygen, the retained product curves displayed a time delay with respect to the total mass gain curves. In the presence of oxygen, however, there was practically only one chronogravimetric curve. This behaviour is interpreted on the basis of a common mechanism involving the formation of an intermediate precursor oxide, which is more readily formed in the presence of oxygen than in its absence. A set of mathematical equations was derived, from which the rate constants for both processes were obtained. The second step was ascribed to a further weak adsorption of water.

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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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7Be activity concentrations were measured in the lower atmosphere at Thessaloniki, Northern Greece (40°38′N, 22°58′E) over the year 2009, a year of a particular minimum of solar activity. The mean annual activity concentration of 7Be at that year was 6.01 mBq m−3. The variability of 7Be surface concentrations related to the solar cycle appeared to be deviated about 40% between the maximum and the minimum values. A positive correlation (R = 0.97) was revealed between the activity concentrations of 7Be and the temperature, confirming that the increased rates of vertical transport within the troposphere, especially during the warmer months, resulted in carrying down to the surface layer air masses enriched in 7Be. Relatively high values of 7Be activity concentrations were observed by increasing of the tropopause height. A negative correlation (R = −0.65) between the 7Be activity concentrations and the relative humidity was due to the condensation process in the lower atmosphere which resulted in increased aerosol particle sizes with higher scavenging rates of aerosols and low activity concentrations of 7Be in the atmosphere. Influence of precipitation on the changes of 7Be activity concentrations was also observed.

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Journal of Thermal Analysis and Calorimetry
Authors: E.T. Stepkowska, J. Perez-Rodriguez, M. Aviles, M. Jimenez de Haro, and M. Sayagues

Abstract  

Specific surface, S, of CSH-gel particles of disordered layered structure, was studied by water sorption/retention in two cement pastes differing in strength, i.e. C-33 (weaker) and C-43 (stronger), w/c=0.4. Hydration time in liquid phase was t h=1 and 6 months, followed by hydration in water vapour either on increasing stepwise the relative humidity, RH=0.5→0.95→1.0 (WS) or on its lowering in an inverse order (WR). Specific surface was estimated from evaporable (sorbed) water content, EV (110C), assuming a bi- and three-molecular sorbed water layer at RH=0.5 or 0.95, respectively (WS). On WR it was three- and three- to four-molecular (50 to 75%), respectively, causing a hysteresis of sorption isotherm. At RH=0.5 the S increased with cement strength from 146 m2 g-1 (C-33, 1 m) to 166 m2 g-1 (C-43, 1 m) and with hydration time to 163 (C-33, 6 m) and to 204 m2 g-1 (C-43, 6 m). At RH=1.0 (and 0.95), higher S-value were measured but these differences were smaller: S amounted to 190-200 m2 g-1 in C-33 (1 and 6 m) and 198-210 m2 g-1 in C-43 (1 and 6 m). Thus no collapse occurred on air drying of paste C-43 (6 m).

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Abstract  

The CISORP Water Sorption Analyser has been used to characterise a selection of solid samples at relative humidities from 0 to 100% and at ambient pressure. The analysis reveals many interesting features about the samples and shows the scope of the equipment. Hysteresis due to porosity and differences in the physical properties of similar chemical samples show up clearly in isotherm curves. Kinetic curves reveal features such as the level of stability of dehydrated food products, changes in the hydration states of salts, and the effect of adding powdered excipient on the water sorption behaviour of a pharmaceutical compound. Kinetic curves were also used to compare the water sorption behaviour of two types of wood found inside a pine cone, and to determine equilibrium moisture sorption by calculation. It was shown that many samples take up moisture irreversibly under the experimental conditions such as amorphous sucrose and other freeze-dried samples, as well as unstable crystalline forms of compounds. Wet samples such as soaked brick and archaeological wood from a well dry out irreversibly even at 100% RH. Recording isotherms at different temperatures allows the calculation of enthalpies of water sorption. If these are compared with the enthalpy of water condensation the two processes can be compared quantitatively.

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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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The purpose of this study was to conduct a thermal analysis of the hydrolysis and degradation behavior of biodegradable polymers and bio-composites at 50°C and 90% relative humidity (RH). With increasing hydrolysis time, the thermal stability and degradation temperature of polybutylene succinate (PBS) slightly decreased. The glass transition temperature (T g) and melting temperature (T m) of PBS and the anti-hydrolysis agent treated PBS did not vary significantly with increasing hydrolysis time, whereas those of the trimethylolpropane triacrylate (TMPTA)-treated PBS slightly increased. With increasing hydrolysis time, the storage modulus (E’) values of the bio-composites decreased, whereas those of the TMPTA treated bio-composites slightly increased. Also, the tan values of the anti-hydrolysis agent and TMPTA treated PBS-BF bio-composites were slightly lower than those of the non-treated bio-composites, due to the reduction in their degree of hydrolysis. The tanδmax peak temperature (T g) of the anti-hydrolysis agent treated bio-composites was not significantly changed, whereas that of the TMPTA treated bio-composites was increased.

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Abstract  

Aerosol particles smaller than 1.8 m were size-fractionated with micro-orifice impactors at two urban sites near Washington, DC, and analyzed for 44 elements including, As, Se, Sb, and Zn, i.e., elements strongly associated with coal combustion, incineration, and regionally transported secondary aerosol, by Instrumental Neutron Activation. Size distribution parameters were determined nonparametrically and with a least-squares peak-fitting method using impactor calibration data. Geometric and fitted mass mean aerodynamic diameters typically differed by <10% and increased continuously with increasing relative humidity (RH) in the range 56 to 79%, but along different curves for samples influenced by local and distant sources. The geometric mass mean diameters for samples influenced by winds from the direction of local sources were uniformly smaller than those influenced by westerly winds bearing aerosol from distant, regional, sources. At 60% RH, gmmads were As, 0.30±0.03 and 0.46±0.04; Se, 0.33±0.06 and 0.54±0.04; Sb, 0.39±0.03 and 0.53±0.04; and Zn, 0.39±0.06 and 0.53±0.08; respectively.

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