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Results for “Thermal analysis”

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PubMed1998

Thermal analysis of bones from ovariectomized rats.

Thermal analyses [thermogravimetry (TG) and differential thermal analysis (DTA)], X-ray diffraction, and infrared absorption analysis of bones from ovariectomized rats were carried out. The rats were divided into five groups: sham operated (Sham); ovariectomized (OVX); OVX given traditional Chinese (Kampo) medicine, Unkei-to; OVX given 17 beta-estradiol; and OVX given the estradiol vehicle, respectively. The activation energy (delta E), a kinetic parameter from TG data of OVX rats, increased by 57% from that in Sham rats. The administration of Unkei-to and 17 beta-estradiol to OVX rats clearly restored the delta E to the levels of Sham rats, while the vehicle for 17 beta-estradiol had no effect. DTA data from thermal analyses of rats from the Sham, OVX, and OVX given various compounds were almost the same except for OVX rats given 17 beta-estradiol. The X-ray diffraction pattern and infrared absorption spectrum of bone powders from Sham rats were not different from those of OVX rats or others. These results strongly suggest that kinetic parameter, delta E calculated from TG data, may be a useful method for assessing both experimentally induced osteoporosis and drug effects on it.

Animals↗

PubMed1999

An investigation into the use of micro-thermal analysis for the solid state characterisation of an HPMC tablet formulation.

The use of micro-thermal analysis (microTA) as a novel means of differentiating between components in a model tablet formulation is described. This technique involves a modification of atomic force microscopy (AFM) such that the standard AFM tip is replaced with a Wollaston wire, thereby allowing the probe to act as a thermistor and temperature probe. Consequently it is possible to map not only the topology but also the thermal conductivity of the sample. Furthermore, it is possible to apply a heating signal to the material and thereby to perform thermal analysis on highly localised regions of the sample. Compacts were prepared comprising ibuprofen, HPMC E4M prem and 1:1 mixes of the two components and analysed using a microTA micro-thermal analyser. The surface topology and conductivity images of the three systems are reported. In addition, the ability of the technique to perform thermal analysis on highly specific regions of the sample is described. The method was able to differentiate between the components of the sample on the basis of micro-thermomechanical experiments. The implications of the use of the technique for the study of pharmaceutical tablets is discussed.

Differential Thermal Analysis↗

PubMed2000

Discrimination of polymorphic forms of a drug product by localized thermal analysis.

In chemical processing, it is important to distinguish between and identify polymorphic forms. We demonstrate the novel use of scanning thermal microscopy (SThM) and localized thermal analysis to distinguish and identify polymorphic forms of the drug cimetidine. These forms cannot be resolved by classical bulk thermal analysis. SThM reveals a sample consisting of a 50 : 50 mixture of the polymorphs contains regions of different thermal conductivity, corresponding to the different polymorphs. Localized thermal analysis of small volumes of pure polymorphic samples (approximately 50 microm3) shows that the origin of the thermal conductivity contrast lies, at least in part, with the presence of a surface water layer on the more hydrophilic polymorph.

Chemistry, Pharmaceutical↗

PubMedDate not supplied

Freeze-drying of protein pharmaceuticals--the application of thermal analysis.

This review describes the range of thermal analysis techniques that may be used to investigate the key thermal properties of formulations to be freeze-dried and the resultant products. The use of these allows development of cost-effective processing while maintaining optimum product quality.

Calorimetry↗

PubMed2005

Characterisation of Ca- and Al-pectate gels by thermal analysis and FT-IR spectroscopy.

Thermal analysis (TG-DTA) and FT-IR spectroscopy have been performed on calcium-pectate membranes to investigate their structure and the consequent variation caused by aluminium sorption. Calcium-polygalacturonate (Ca-PG) membranes, model systems of the soil-root interface, were exposed to aluminium solutions at different concentrations (25-800 microM). Three different pHs (3.50, 4.00 and 4.50) were chosen to study the influence of different aluminium species, such as [Al(H2O)6]3+, [Al(OH)(H2O)5]2+ and [Al(OH)2(H2O)(4)]+, on the structure of the Ca-PG membrane. The DTA profiles and FT-IR spectra showed how aluminium sorption induces structural modifications leading to a reorganisation of the chain aggregates and a weakening of the structure. Higher pH, that is, 4.00 and 4.50, and thus hydrolytic aluminium species and related higher calcium content maintain a more regular structure than at pH 3.50. At pH 3.50, both the effect of [Al(H2O)6]3+ and a major calcium release had a greater impact and thus induced a greater weakening of the structure.

Aluminum↗

PubMed2000

Studies on the number of contacts between ibuprofen and ethenzamide using thermal analysis.

We studied a method of estimating the number of contacts in a solid dosage form using thermal analysis. Ibuprofen (IB) and Ethenzamide (ET) were used as model actives. IB and ET were granulated and sieved with each other. We prepared mixtures of IB and ET using different diameter granules. The number of contacts between the samples was calculated by the expression method of Ouchiyama and Tanaka. By thermal analysis, we measured the quantity of endotherm up to 60-63 degrees C from 56 degrees C. The quantity of endotherm up to 61 degrees C from 56 degrees C was in good proportion to the number of contacts calculated by the expression.

Algorithms↗

PubMed2003

Thermal analysis of the antiretroviral zidovudine (AZT) and evaluation of the compatibility with excipients used in solid dosage forms.

Modern thermal analysis techniques are frequently used because of their ability to provide detailed information about both the physical and the energetic properties of a substance. In the present work, the thermal decomposition of zidovudine (AZT) was studied using differential scanning calorimetry (DSC) and thermogravimetry/derivative thermogravimetry (TG/DTG). Thermal analysis was supplemented using elemental analysis (C, H, and N), infrared (IR) spectroscopy, and X-ray powder diffraction to characterize the solid intermediates products. Volatile products of the thermal decomposition of AZT were studied by a system composed of the TG/DTA coupled gas chromatography/mass spectrometry (GC/MS). The physical-chemical properties and compatibilities of several commonly used pharmaceutical excipients with AZT were evaluated using thermal methods. The results showed that the product originated from the first thermal decomposition stage corresponds to the cleavage followed by elimination of the azide group and consequent formation of thymine. The second event corresponds to thermal decomposition of thymine. TG/DTA-GC/MS system identified thymine's decomposition products as furan and 2-furanmethanol like volatile species. Comparison of the thermoanalytical profiles of the mixtures with individual compounds did not give any evidence of interactions.

Antiviral Agents↗

PubMedDate not supplied

Hybrid finite element-finite difference method for thermal analysis of blood vessels.

A hybrid finite-difference/finite-element technique for the thermal analysis of blood vessels embedded in perfused tissue has been developed and evaluated. This method provides efficient and accurate solutions to the conjugated heat transfer problem of convection by blood coupled to conduction in the tissue. The technique uses a previously developed 3D automatic meshing method for creating a finite element mesh in the tissue surrounding the vessels, coupled iteratively with a 1-D marching finite difference method for the interior of the vessels. This hybrid technique retains the flexibility and ease of automated finite-element meshing techniques for modelling the complex geometry of blood vessels and irregularly shaped tissues, and speeds the solution time by using a simple finite-difference method to calculate the bulk mean temperatures within all blood vessels. The use of the 1D finite-difference technique in the blood vessels also eliminates the large computer memory requirements needed to accurately solve large vessel network problems when fine FE meshes are used in the interior of vessels. The accuracy of the hybrid technique has been verified against previously verified numerical solutions. In summary, the hybrid technique combines the accuracy and flexibility found in automated finite-element techniques, with the speed and reduction of computational memory requirements associated with the 1D finite-difference technique, something which has not been done before. This method, thus, has the potential to provide accurate, flexible and relatively fast solutions for the thermal analysis of coupled perfusion/blood vessel problems, and large vessel network problems.

Biomedical Engineering↗

PubMed2006

[Study of FTIR spectra and thermal analysis of polyurethane].

The thermal behavior of polyester-polyurethane and polyether-polyurethane in air atmosphere was investigated by using FTIR analysis in the temperature range from 20 to 400 degrees C. The thermal degradation behaviors of polyester-polyurethane and polyether-polyurethane in different atmospheres were investigated by using thermogravimetry analysis (TG) in the temperature range from 20 to 700 degrees C. The FTIR results together with the TG investigations showed that polyester-polyurethane has two degradation steps in air, but polyether-polyurethane has only one degradation step. The thermal analysis results also showed that the onset degradation temperature of polyether-polyurethane is lower than that of polyester-polyurethane, suggesting that the thermal stability of polyester-polyurethane is higher than polyether-polyurethane, and the onset degradation temperature of polyurethane in air is lower than that in nitrogen, suggesting that the presence of oxygen affects significantly the break of the polymeric chains.

English Abstract↗

PubMed1998

Electroperturbation of human stratum corneum fine structure by high voltage pulses: a freeze-fracture electron microscopy and differential thermal analysis study.

Application of high voltage pulses (HVP) to the skin has been shown to promote the transdermal drug delivery by a mechanism involving skin electroporation. The aim of this study was to detect potential changes in lipid phase and ultrastructure induced in human stratum corneum by various HVP protocols, using differential thermal analysis and freeze-fracture electron microscopy. Due to the time involved between the moment the electric field is switched off and the analysis, only "secondary" phenomena rather than primary events could be observed. A decrease in enthalpies for the phase transitions observed at 70 degrees C and 85 degrees C was detected by differential thermal analysis after HVP treatment. No changes in transition temperature could be seen. The freeze-fracture electron microscopy study revealed a dramatic perturbation of the lamellar ordering of the intercellular lipid after application of HVP. Most of the planes displayed rough surfaces. The lipid lamellae exhibited rounded off steps or a vanished stepwise order. There was no evidence for perturbation of the corneocytes content. In conclusion, the freeze-fracture electron microscopy and differential thermal analysis studies suggest that HVP application induces a general perturbation of the stratum corneum lipid ultrastructure.

Electric Stimulation↗

PubMed1997

Dynamic mechanical thermal analysis of maxillofacial elastomers.

STATEMENT OF PROBLEM: Maxillofacial prosthetic materials should simulate the oral tissues as much as possible and therefore have a similar flexibility and resilience. In light of the oral tissues constantly moving, the dynamic deformation properties of maxillofacial materials would seem the most relevant. PURPOSE: In this study, dynamic mechanical thermal analysis was used to evaluate the deformation properties of five silicone rubber materials used to construct facial prostheses. The technique involves the application of a sinusoidally oscillating stress to a material and analyzes how the material elastically or viscoelastically responds to the stress. The dynamic mechanical thermal analysis can operate at a fixed frequency or range of frequencies over a specific temperature range and also isothermally as a function of time. RESULTS: Cosmesil and A-2186 materials were the most resilient materials and Silbione had the greater energy absorption capacity, which was particularly noticeable at the higher frequencies. Silbione also had a lower shear modulus (G'), which indicated it was more flexible than the other materials. CONCLUSION: The dynamic mechanical thermal analysis proved to be a rapid, reliable, and convenient method for the determination of viscoelastic properties of maxillofacial materials.

Analysis of Variance↗

PubMed2002

Complexity of intercalation of hydrazine into kaolinite--a controlled rate thermal analysis and DRIFT spectroscopic study.

Controlled rate thermal analysis (CRTA) allows the separation of adsorbed and intercalated hydrazine. CRTA displays the presence of three different types of hydrogen-bonded hydrazine in the intercalation complex: (a) The first is adsorbed loosely bonded on the kaolinite structure fully expanded by hydrazine-hydrate and liberated between approx 50 and 70 degrees C (b) The second intercalated hydrazine is lost between approx 70 and 85 degrees C. (c) The third type of intercalated-hydrazine molecule is lost in the 85-130 degrees C range. CRTA at 70 degrees C enables the removal of hydrazine-water and results in the partial collapse of the hydrazine-intercalated kaolinite structure to form a hydrazine-intercalated kaolinite. Removal of the adsorbed hydrazine enables the DRIFT spectra of the hydrazine-intercalated complex without any adsorbed hydrazine to be obtained. A band at 3626 cm(-1) attributed to the inner surface hydroxyls of kaolinite hydrogen bonded to hydrazine is observed. The intercalation of hydrazine-hydrate into kaolinite is complex and results from the different types of surface interactions of the hydrazine with the kaolinite surfaces.

Journal Article↗

PubMedDate not supplied

Cultures and thermal analysis of the marine microalga Tetraselmis suecica Kylin (Butch).

In this paper, the growth of the marine microalga Tetraselmis suecica was investigated using thermogravimetry (TG) and differential thermal analysis (DTA) to determine suitable diets for larval and juvenile development in aquaculture systems. Microalgae were maintained in synthetic sea water (19@1000 salinity, 18 degrees C constant temperature) and the algal growth was evaluated by cell abundance. Exponential, stationary and senescence cells were analyzed by TG and DTA. The results of thermal analysis pointed out marked differences between exponential, stationary and senescence phases and showed that exponentially growing microalgae could represent a suitable food in aquaculture systems.

Differential Thermal Analysis↗

PubMed2006

Thermal analysis in the evaluation of sediment pollution.

Characterization of organic matter in four sediments in the infuence area of wastewater discharges was carried out by both chemical and thermal analysis in order to assess their pollution level. Oxidisable organic carbon and organic matter were calculated by the standard methodology in laboratory. Thermogravimetry (TG), between 50 and 900 degrees C, was simultaneously performed in oxidizing conditions on ground sediments samples after three different pretreatments. Linear regression adjust of thermal analysis results versus chemical parameters provides the better Pearson's coefficients, leading to the best coefficients for weight loss in 250-400 degree C temperature range versus oxidisable organic carbon and organic matter at 360 degrees C, respectively. These results demonstrated the utility of thermoanalysis technique for the evaluation of the organic matter content of fresh sediments.

Differential Thermal Analysis↗

PubMed2026

Thermal analysis techniques for microplastic mass quantification: Methodological challenges and standardization needs.

Microplastics (MPs, 1 μm-5 mm) and nanoplastics (NPs, <1 μm) are ubiquitous contaminants requiring standardized quantification methods. This systematic review evaluates thermal analysis techniques for mass-based MP detection, including pyrolysis-gas chromatography-mass spectrometry (Py-GC-MS), thermogravimetry-MS (TGA-MS), thermal extraction desorption-GC-MS (TED-GC-MS), and differential scanning calorimetry (DSC). Database searches (Web of Science, from inception to December 1, 2025) following PRISMA guidelines identified studies across seven environmental matrices (water, soil/sediment, atmosphere, biota, human tissues). We identify critical standardization gaps: inconsistent marker ion selection, unvalidated conversion factors for tire and road wear particles (TRWPs), and the absence of certified reference materials for complex matrices. Py-GC-MS demonstrates versatility but suffers from lipid interference in biological samples; TED-GC-MS offers superior sensitivity (sample capacity ∼200× Py-GC-MS) but lacks real-time chromatographic monitoring. To advance data comparability, we propose: (i) harmonized ion selection hierarchies based on specificity-sensitivity balance, (ii) matrix-specific TRWP quantification protocols, and (iii) inter-laboratory validation using environmental reference materials. This review provides a methodological roadmap for standardizing thermal analysis in MP research.

Humans↗

PubMed2002

Dynamic mechanical thermal analysis studies of polymer films prepared from aqueous dispersion.

Dynamic Mechanical Thermal Analysis of cast and sprayed films of an aqueous dispersion of polymethyl methacrylate (Eudragit NE30D) and mixtures with an aqueous dispersion of ethylcellulose (Aquacoat ECD-30) has been undertaken. Such analysis allows the identification of glass transition temperatures and the degree of miscibility of the polymers. It was found that the two polymers formed as cast or sprayed films were not miscible but had an optimal composition of 30% of the ethylcellulose dispersion in the polymethyl methacrylate dispersion.

Acrylates↗

PubMed1977

[Differential thermal analysis of the organic fraction of bone].

Thermal decomposition analysis of Bovine femur bone has been carried out by means of a Micro Differential Thermal Analyser. The analysis of both thermograms and amino acid compositions has revealed the complexity of collagen degradation mechanisms.

Amino Acids↗

PubMed1991

Ibuprofen-loaded ethylcellulose microspheres: analysis of the matrix structure by thermal analysis.

The determination of the drug dispersion state in microspheres prepared by the solvent evaporation method is essential to foresee the stability of the particles and the drug release behavior. The present work deals with ibuprofen-loaded ethylcellulose microspheres, that are characterized by a lower drug melting point than the polymer glass transition temperature. Although annealing experiments were not possible, the study has evidenced the presence of a metastable molecular dispersion for intermediate loadings, coexisting with a solid solution and a crystalline dispersion of the drug in the polymer matrix. In addition, differential scanning calorimetry helped to distinguish between surface and inner ibuprofen crystals, which interact differently with the polymer matrix and therefore have different melting points.

Calorimetry, Differential Scanning↗