Search results for "Calorimetry"
showing 10 items of 504 documents
The comparison of seven different methods to quantify the amorphous content of spray dried lactose
2006
The purpose of this work was to verify the usefulness, advantages and disadvantages of seven methods that are widely used to detect, and quantify the amorphous contents in pharmaceutical solids. Here, StepScan DSC, a type of modulated temperature calorimetry method, was applied for the first time to quantify amorphicity. The comparison of the analytical methods was undertaken with real (non-artificial) test samples, i.e. spray-dried lactose samples with various degrees of crystallinity. In these samples, it was essential that the amorphous and the crystalline portions are not present as separate particles, which is the case when physical (artificial) mixtures of totally amorphous and totall…
Effects of Ethanol to Water Ratio in Feed Solution on the Crystallinity of Spray-Dried Lactose
2002
In the present study, the effects of ethanol to water ratio in feed solution on the physical properties of spray-dried alpha-lactose monohydrate were evaluated. Crystallinity of the spray-dried lactose was determined by isothermal microcalorimetry (IMC) and by differential scanning calorimetry (DSC). Water content of the spray-dried lactose was determined by thermogravimetric analysis and the surface area was evaluated by Brunauer, Emmett, and Teller (BET) method. The crystallinity of spray-dried lactose varied from 0% to 100%, depending on the ratio of ethanol to water in the feed solution. Lactose spray dried from pure ethanol was 100% crystalline and contained hydrate water. Lactose spra…
Hydrophobic effects in the stabilisation of copper(I) by the macrocyclic ligands 16,17,19,20-tetramethyl-2,6,9,13-tetraaza[14]paracyclophane and 14,1…
1996
Abstract The interaction of Cu 2+ with the para -azacychlophanes 16,17,19,20-tetramethyl-2,6,9,13-tetraazal[14]paracyclophane (L1) and 14,15,17,18-tetramethyl-2,5,8,11-tetraaza[12]paracyclophane (L2) has been studied by potentiometry, and direct microcalorimetry at 298.1±0.1 K in 0.15 mol dm −3 NaClO 4 . The stability constants (log K CuLi = 13.35(3), log K CuL2 = 9.32(4)) and the thermodynamic parameters ( ΔH ° CuL1 = −47.3(8) kJ mol −1 , ΔH ° CuL2 = 20.9(8) kJ mol −1 ) evidence that not all four nitrogen atoms in the ligands are involved in the coordination to the metal centre. These results, particulary in the case of L1, are similar to those reported for the analogous cyclophanes contai…
Binding of Short Alkyl Chain Surfactants to the (Ethylene oxide)13−(Propylene oxide)30−(Ethylene oxide)13and (Ethylene oxide)75−(Propylene oxide)30−(…
2002
The enthalpy of transfer (ΔHt) of neutral copolymers, at a fixed and low concentration ca. 10-3 mol kg-1, from water to the aqueous surfactant solutions as a function of the surfactant concentration (fSmS) was determined at 25 °C. The surfactants studied are sodium octanoate, sodium decanoate, N-octylpyridinium chloride (OPC), and N,N-dimethyloctylamine-N-oxide (ODAO). The copolymers are (ethylene oxide)13−(propylene oxide)30−(ethylene oxide)13 (L64) and (ethylene oxide)75−(propylene oxide)30−(ethylene oxide)75 (F68). The two copolymers show different hydrophilic−hydrophobic ratios, the larger being for F68. As a general feature, the shape of the ΔHt vs fSmS curve depends on the nature of t…
Myoglobin on Silica: A Case Study of the Impact of Adsorption on Protein Structure and Dynamics
2013
International audience; If protein structure and function changes upon adsorption are well documented, modification of adsorbed protein dynamics remains a blind spot, despite its importance in biological processes. The adsorption of metmyoglobin on a silica surface was studied by isotherm measurements, microcalorimetry, circular dichroïsm, and UV-visible spectroscopy to determine the thermodynamic parameters of protein adsorption and consequent structure modifications. The mean square displacement and the vibrational densities of states of the adsorbed protein were measured by elastic and inelastic neutron scattering experiments. A decrease of protein flexibility and depletion in low freque…
Miscibility and properties of linear poly(l-lactide)/branched poly(l-lactide) copolyester blends
2006
Abstract Polymer blends consisting of linear poly( l -lactide) (PLLA) and different proportions of dendritic PLLA-based copolyesters ( hb -PLLA) characterized by different degrees of branching (DB) were obtained in melt. The solid-state properties of poly( l -lactide)s and their blends were investigated by differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA), atomic force microscopy (AFM) and stress–strain measurements. DSC and DMA methods proved miscibility of PLLA/ hb -PLLA blends for the studied composition range. AFM indicated that no phase separation occurs in PLLA/ hb -PLLA blends and that PLLA and hb -PLLA cocrystallize in one single lamellae type. The mechanica…
Comparison of two melting range analysis methods with lactitol monohydrate
2001
Abstract In pharmacopoeia, the melting point is determined by a standard method with a melting point instrument. The melting point can also be determined with differential scanning calorimetry (DSC). In this study, the standard method and DSC method are compared for determining the melting range of lactitol monohydrate. The effect of initial temperature, grinding, and drying on the melting range of different lactitol monohydrate samples was studied by a melting point instrument. The melting point and melting enthalpy of the stable form of lactitol monohydrate was identified by DSC. The statistical analysis of the results is based on a t-test. All studied variables had a small effect on the …
New amphiphilic terphenyl liquid crystals for the preparation of highly ordered ultrathin films
1991
Four new amphiphilic liquid crystals have been synthesized, in which terphenyl was used as the mesogenic unit. In order to enable the formation of Langmuir Monolayers at the air/water-interface, the molecules were equipped with slightly polar headgroups such as esters or a carboxylic acid group. All compounds can be transferred onto solid substrates. In addition, it is possible to prepare freely suspended films of at least one compound in the temperature range of the smectic phases. The phases of the different states, bulk, monolayer, freely suspended film, and Langmuir-Blodgett multilayers have been investigated by means of monolayer isotherms, optical textures, differential scanning calor…
Small Angle Neutron Scattering, X-ray Diffraction, Differential Scanning Calorimetry, and Thermogravimetry Studies to Characterize the Properties of …
2009
Nanocomposites based on laponite RD and (ethylene oxide)98(propylene oxide)67(ethylene oxide)98 (F127)triblock copolymer or poly(ethylene) glycol 2000 (PEG2000) were prepared by using the melting method. Small-angle neutron scattering and the X-ray diffraction experiments provided insights into the organization of the laponite RD dispersed in the macromolecular matrix over a wide length scale. SANS data analysis by means of a fractal law evidenced the formation of clusters of laponite RD at long correlation distance. The single laponite RD particles and the lamellar structure of F127 were described in the shorter length scale. Finally, the crystalline structure of the macromolecule was obse…
Hypothalamic CB1 cannabinoid receptors regulate energy balance in mice.
2012
Cannabinoid type 1 (CB(1)) receptor activation is generally considered a powerful orexigenic signal and inhibition of the endocannabinoid system is beneficial for the treatment of obesity and related metabolic diseases. The hypothalamus plays a critical role in regulating energy balance by modulating both food intake and energy expenditure. Although CB(1) receptor signaling has been implicated in the modulation of both these mechanisms, a complete understanding of its role in the hypothalamus is still lacking. Here we combined a genetic approach with the use of adeno-associated viral vectors to delete the CB(1) receptor gene in the adult mouse hypothalamus and assessed the impact of such ma…