Thermogravimetric Analysis of Carbonate Aggregate, HR-336, 1994

Research has shown that one of the major contributing factors in early joint deterioration of portland cement concrete (PCC) pavement is the quality of the coarse aggregate. Conventional physical and freeze/thaw tests are slow and not satisfactory in evaluating aggregate quality. In the last ten years the Iowa DOT has been evaluating X-ray analysis and other new technologies to predict aggregate durability in PCC pavement. The objective of this research is to evaluate thermogravimetric analysis (TGA) of carbonate aggregate. The TGA testing has been conducted with a TA 2950 Thermogravimetric Analyzer. The equipment is controlled by an IBM compatible computer. A "TA Hi-RES" (trademark) software package allows for rapid testing while retaining high resolution. The carbon dioxide is driven off the dolomite fraction between 705 deg C and 745 deg C and off the calcite fraction between 905 deg C and 940 deg C. The graphical plot of the temperature and weight loss using the same sample size and test procedure demonstrates that the test is very accurate and repeatable. A substantial number of both dolomites and limestones (calcites) have been subjected to TGA testing. The slopes of the weight loss plot prior to the dolomite and calcite transitions does correlate with field performance. The noncarbonate fraction, which correlates to the acid insolubles, can be determined by TGA for most calcites and some dolomites. TGA has provided information that can be used to help predict the quality of carbonate aggregate.

Thermogravimetric analysis of water release from wheat flour and wheat bran suspensions

Bran is hygroscopic and competes actively for water with other key components in baked cereal products like starch and gluten. Thermogravimetric analysis (TGA) of flour–water mixtures enriched with bran at different incorporation levels was performed to characterise the release of compartmentalised water. TGA investigations showed that the presence of bran increased compartmentalised water, with the measurement of an increase of total water loss from 58.30 ± 1.93% for flour only systems to 71.80 ± 0.37% in formulations comprising 25% w/w bran. Deconvolution of TGA profiles showed an alteration of the distribution of free and bound water, and its interaction with starch and gluten, within the formulations. TGA profiles showed that water release from bran-enriched flour is a prolonged event with respect to the release from non-enriched flour, which suggests the possibility that bran may interrupt the normal characteristic processes of texture formation that occur in non-enriched products.

Thermo-gravimetric analysis (TGA) after different exposures of high density polyethylene (HDPE) and poly vinyl chloride (PVC) geomembranes

This paper presents the results of thermogravimetric analysis (TGA) tests in PVC (1.0; 2.0 mm) and HDPE (0.8; 2.5 mm) geomembranes exposed to weathering and leachate after 30 months. The aim of this paper is the comparison of fresh and exposed samples to assess the degradation process concerning the total loss of mass of geomembranes. The exposure was conducted in accordance with the recommendations of ASTM standards. The TGA tests were carried out according to ASTM D6370 and E2105. Results show, for instance, that for PVC geomembrane the largest reductions of plasticizers occurred for samples exposed to weathering. The loss of plasticizers after the exposure contributed to the decrease of deformation and consequent increase in stiffness. TGA tests shows to be a valuable tool to control the quality of the materials. © 2012 ejge.

Kinetic study of the pyrolysis of miscanthus and its acid hydrolysis residue by thermogravimetric analysis

The kinetic parameters of the pyrolysis of miscanthus and its acid hydrolysis residue (AHR) were determined using thermogravimetric analysis (TGA). The AHR was produced at the University of Limerick by treating miscanthus with 5 wt.% sulphuric acid at 175 °C as representative of a lignocellulosic acid hydrolysis product. For the TGA experiments, 3 to 6 g of sample, milled and sieved to a particle size below 250 μm, were placed in the TGA ceramic crucible. The experiments were carried out under non-isothermal conditions heating the samples from 50 to 900 °C at heating rates of 2.5, 5, 10, 17 and 25 °C/min. The activation energy (EA) of the decomposition process was determined from the TGA data by differential analysis (Friedman) and three isoconversional methods of integral analysis (Kissinger–Akahira–Sunose, Ozawa–Flynn–Wall, Vyazovkin). The activation energy ranged from 129 to 156 kJ/mol for miscanthus and from 200 to 376 kJ/mol for AHR increasing with increasing conversion. The reaction model was selected using the non-linear least squares method and the pre-exponential factor was calculated from the Arrhenius approximation. The results showed that the best fitting reaction model was the third order reaction for both feedstocks. The pre-exponential factor was in the range of 5.6 × 1010 to 3.9 × 10+ 13 min− 1 for miscanthus and 2.1 × 1016 to 7.7 × 1025 min− 1 for AHR.

Thermogravimetric analysis of the pyrolysis of several materials used in the preparation of commercial cigarettes

Comunicación presentada en forma de póster en el "12th Mediterranean Congress of Chemical Engineering", Barcelona (Spain), November 15-18, 2011

Thermogravimetric analysis of carbon deposition over Ni/gamma-Al2O3 catalysts in carbon dioxide reforming of methane

Carbon formation on Ni/gamma-Al2O3 catalysts and its kinetics during methane reforming with carbon dioxide was studied in the temperature range of 500-700 degrees C using a thermogravimetric analysis technique. The activation energies of methane cracking, carbon gasification in CO2, as well as carbon deposition in CO2-CH4 reforming were obtained. The results show that the activation energy for carbon gasification is larger than that of carbon formation in methane cracking and that the activation energy of coking in CO2-CH4 reforming is also larger than that of methane decomposition to carbon. The dependencies of coking rate on partial pressures of CH4 and CO2 indicate that methane decomposition is the main route for carbon deposition. A mechanism and kinetic model for carbon deposition is proposed.

A thermogravimetric analysis of the combustion of a Brazilian mineral coal

Knowledge of coal combustion kinetics is crucial for burner design. This work aims to contribute on this issue by determining the kinetics of a particular Brazilian bituminous coal. Non-isothermal thermogravimetry was applied for determining both the pre-exponential factor and the activation energy. Coal samples of 10 mg and 775 mm mean size were used in synthetic air atmospheres (21 % O2). Heating rates from 10 to 50 ºC/min were applied until the temperature reached 850 ºC, which was kept constant until burnout. The activation energy for the primary and the secondary combustion resulted, respectively, in 135.1 kJ/mol and 85.1 kJ/mol.

Influence of experimental factors on results of thermogravimetric analysis

Thermogravimetric results are influenced by a series of experimental factors, such as furnace heating rate and atmosphere, velocity of carrier gas, sample mass, etc. In this work a practical evaluation of these parameters are showed for calcium oxalate, with teaching objectives, considering that undergraduate text books discuss but do not show experimental details for these cases.

Evaluation of Decomposition Kinetics of Poly (Ether-Ether-Ketone) by Thermogravimetric Analysis

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Use of high-resolution thermogravimetric analysis (HRTG) technique in spent FCC catalyst/Portland cement pastes

Thermogravimetric analysis is one of the most common instrumental techniques used for the characterization of pastes, mortars and concretes based on both calcium hydroxide and Portland cement. Important information about pozzolanic materials can be assessed concerning calcium hydroxide consumption and the formation of new hydrated products. Nevertheless, in some cases, problems associated with the overlapped decomposition processes for hydrates make the analysis of obtained data difficult. In this paper, the use of high-resolution thermogravimetric analysis, a powerful technique that allows separating decomposition processes in analysis of hydrated binders, was performed for spent FCC catalyst-Portland cement pastes. These pastes were monitored for 1, 4, 8 h and 1, 2, 3, 7 and 28 curing days. In order to study the influence of the pozzolanic material (spent FCC catalyst), Portland cement replacements of 5, 15 and 30 % by mass were carried out. The presence of spent FCC catalyst in blended pastes modified the amount and the nature of the formed hydrates, mainly ettringite and stratlingite.

XRD, AFM, IR and TGA study of nanostructured hydroxyapatite

In this work, the synthetic hydroxyapatite (HAP) was studied using different preparation routes to decrease the crystal size and to study the temperature effect on the HAP nano-sized hydroxyapatite crystallization. X-ray diffraction (XRD) analysis indicated that all samples were composed by crystalline and amorphous phases . The sample with greater quantity of amorphous phase (40% of total mass) was studied. The nano-sized hydroxyapatite powder was heated and studied at 300, 500, 700, 900 and 1150 °C. All samples were characterized by XRD and their XRD patterns refined using the Rietveld method. The crystallites presented an anisotropic form, being larger in the [001] direction. It was observed that the crystallite size increased continuously with the heating temperature and the eccentricity of the ellipsoidal shape changed from 2.75 at 300 °C to 1.94, 1.43, 1.04 and 1.00 respectively at 500, 700, 900 and 1150 °C. In order to better characterize the morphology of the HAP the samples were also examined using atomic force microscopy (AFM), infrared spectrometry (IR) and thermogravimetric analysis (TGA).

Investigating the role of cholesterol in the formation of non-ionic surfactant based bilayer vesicles:thermal analysis and molecular dynamics

The aim of this research was to investigate the molecular interactions occurring in the formulation of non-ionic surfactant based vesicles composed monopalmitoyl glycerol (MPG), cholesterol (Chol) and dicetyl phosphate (DCP). In the formulation of these vesicles, the thermodynamic attributes and surfactant interactions based on molecular dynamics, Langmuir monolayer studies, differential scanning calorimetry (DSC), hot stage microscopy and thermogravimetric analysis (TGA) were investigated. Initially the melting points of the components individually, and combined at a 5:4:1 MPG:Chol:DCP weight ratio, were investigated; the results show that lower (90 C) than previously reported (120-140 C) temperatures could be adopted to produce molten surfactants for the production of niosomes. This was advantageous for surfactant stability; whilst TGA studies show that the individual components were stable to above 200 C, the 5:4:1 MPG:Chol:DCP mixture show ∼2% surfactant degradation at 140 C, compared to 0.01% was measured at 90 C. Niosomes formed at this lower temperature offered comparable characteristics to vesicles prepared using higher temperatures commonly reported in literature. In the formation of niosome vesicles, cholesterol also played a key role. Langmuir monolayer studies demonstrated that intercalation of cholesterol in the monolayer did not occur in the MPG:Chol:DCP (5:4:1 weight ratio) mixture. This suggests cholesterol may support bilayer assembly, with molecular simulation studies also demonstrating that vesicles cannot be built without the addition of cholesterol, with higher concentrations of cholesterol (5:4:1 vs 5:2:1, MPG:Chol:DCP) decreasing the time required for niosome assembly. © 2013 Elsevier B.V.

Heat treatment of a direct composite resin: influence on flexural strength

The purpose of this study was to evaluate the flexural strength of a direct composite, for indirect application, that received heat treatment, with or without investment. One indirect composite was used for comparison. For determination of the heat treatment temperature, thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) were performed, considering the initial weight loss temperature and glass transition temperature (Tg). Then, after photoactivation (600 mW/cm² - 40 s), the specimens (10 x 2 x 2 mm) were heat-treated following these conditions: 170ºC for 5, 10 or 15 min, embedded or not embedded in investment. Flexural strength was assessed as a means to evaluate the influence of different heat treatment periods and investment embedding on mechanical properties. The data were analyzed by ANOVA and Tukey's test (α = 0.05). TGA showed an initial weight loss temperature of 180ºC and DSC showed a Tg value of 157°C. Heat treatment was conducted in an oven (Flli Manfredi, Italy), after 37°C storage for 48 h. Flexural strength was evaluated after 120 h at 37°C storage. The results showed that different periods and investment embedding presented similar statistical values. Nevertheless, the direct composite resin with treatments presented higher values (178.7 MPa) compared to the indirect composite resin (146.0 MPa) and the same direct composite submitted to photoactivation only (151.7 MPa). Within the limitations of this study, it could be concluded that the heat treatment increased the flexural strength of the direct composite studied, leading to higher mechanical strength compared to the indirect composite.