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AN678 - Pyrolysis study of lignocellulosic biomass and its components by DSC

Wood, straw, sugarcane bagasse and coconut shell are examples of lignocellulosic biomass. This category of biomass is mainly composed of cellulose, hemicelluloses and lignin. Small quantities of mineral materials are added to these polymers. The proportion of each component can vary considerably according to the type of biomass.

AN677 - Evolution of CO2 released during pyrolysis of lignocellulosic biomass and its components

Biomass is a renewable source of energy if it is produced in a protected environment, allowing its constant production. The renewable characters present an interest to reduce CO2 emissions. Indeed, when biomass is burnt, it releases CO2 but this one was previously captured in the atmosphere by photosynthesis. Thus, carbon balance is theoretically neutral during one cycle of production-consumption (Figure 2). The thermogravimetry-FTIR coupling is proposed to study the CO2 release from lignocellulosic biomass.

AN676 - Cellulose pyrolysis investigation by thermogravimetry coupled with FTIR spectrometry

Cellulose is a polysaccharide (Figure 1) consisting of a linear chain of several hundred to over ten thousand b(1->4) linked D-glucose units. Cellulose, located in the cytoplasmic membrane of plant cells, is the principal component and therefore the most abundant matter in the nature. According to the Broido-Shafizadeh model [1] (Figure 2), during cellulose pyrolysis, there is a formation of an activated cellulose with a lower polymerization degree. The thermal degradation of this activated cellulose produce in one hand, volatiles and in other hand, char and gases. Proportions of each pyrolysis product depend of experimental conditions (heating rate, sample mass, gas flow...)

AN675 - Biomass pyrolysis: study of parameters determining the charcoal yield by thermogravimetry

Pyrolysis of biomass products three kinds of components: charcoal, gases and bio-oil. The proportion of each energy product depends on experimental parameters. In order to study the influence of these parameters under the charcoal yield, the reaction of pyrolysis of biomass is simulated by thermogravimetry. In this application, three parameters are studied: the mass of sample introduced in the reactor, the heating rate and the sample size

AN674 - Gas adsorption on catalysts and adsorbents using a quartz tube reactor on a Calvet type DSC

The investigation of gas adsorption on catalysts and more generally solid adsorbents requires a very good interaction between the reactive gas and the powder. The Calvet-type DSC offers the main advantage to work with an open tube detection. This configuration allows the adaptation of different types of experimental crucibles, especially with the possibility of introduction of various types of gas under normal or high pressure. The quartz tube reactor is one option for the applications on catalysts, and more generally for all the adsorption investigations. It makes possible the simulation of the use of a plug-flow fixed bed reactor in heterogeneous catalysis.

AN673 - CO2 capture on aminated solid sorbents by thermogravimetry

The leading contender for post-combustion carbon dioxide capture from coal-fired power plants is the use of amine solvents. Despite the advantages of solvent scrubbing, there are several disadvantages, especially the thermal efficiency losses due to the energy needed to regenerate the solvent by driving off the captured CO2. The use of solid sorbents impregnated with different amine solutions provides a new technological approach for CO2 capture with the absorption capacity of amines and the easy handling of solids without corrosion drawback. Thermogravimetry is very well adapted to investigate the adsorption and desorption performances of the samples and define the CO2 capture capacity of the corresponding aminated solid sorbents

AN672 - Chemical Looping Combustion by Thermogravimetry

Chemical Looping Combustion (CLC) or also called oxy-combustion is a process that was developed in 1994 by the laboratory of Professor Ishida (Japan) for the CO2 capture. It is a new method of oxidizing fuels without the direct use of either air or oxygen. The interest of such a combustion is to have a more efficient process for burning fuels (natural gas, coal) with a production of CO2 for sequestration. In order to improve the fuel combustion, more oxygen is brought to the system through metal oxides. So the metal oxide is used as an oxygen carrier to facilitate the fuel combustion and is permanently regenerated and reoxidised. Thermogravimetry is very well adapted to measure the oxygen transfer capacity (OTC) of the metal oxide sample.

AN671 - Polymorphic behavior of cocoa butter.Influence on chocolate tempering conditions

Cocoa butter is one of the main constituents of chocolate. It is composed of triglycerides (TG) formed mainly of Stearic, Palmitic and Oleic acids. Due to their nodal structure, TG can crystallize under different forms, leading to a polymorphic behavior. Six different polymorphic forms of cocoa butter are reported in literature [1,2], noted from I to VI, by order of stability (VI is the thermodynamically stable form).

AN670 - Heat capacity determination of low density insulation materials by calorimetry

Maintaining acceptable temperatures in buildings (by heating and cooling) uses a large proportion of global energy consumption, leading to a high R&D interest in more efficient insulation materials. Among others, aerogels are interesting low density, low conductivity materials in which the liquid component of the gel has been replaced with a gas. Cp of such an insulation material is a key parameter that describes its aptitude to accumulate heat. As large amounts of sample are needed for such a Cp determination, the C80 calorimeter is perfectly adapted for the measurement.

AN669 - Melting and Crystallization of Phase Change Materials (PCM) by MicroDSC

A phase change material (PCM) is a substance with a high heat of fusion that through melting and solidifying at a certain temperature, is capable of storing and releasing large amounts of energy (see fig 1). Among other energy savings related applications, PCM are used to design more efficient insulation systems. Indeed, these substances can be encapsulated in building materials such as bricks, or other wall, flooring, roofing, and ceiling materials. By successive melting and crystallization, they can damp the day / night outside temperature variations and allow maintaining acceptable indoor temperatures

AN668 - Effect of pressure on the glass transition temperature Tg of an elastomer sample by HP-MicroDSC

When an elastomer is cooled below its glass transition temperature (Tg), it loses its elasticity and becomes brittle. For elastomer O-rings, that are used for sealing purpose, Tg thus corresponds to a lower limit of use. Problems arise when they are used in high pressures systems, as their Tg may be shifted to higher temperatures. The HP-MicroDSC technique is used to investigate the Tg dependence to the pressure

AN667 - CO2 adsorption on basolite C300 studied by coupled volumetry-microDSC

Metal-organic frameworks (MOFs) offer an advantage over classical other porous materials (activated carbon, zeolithes) because their properties can be tailored due to the vast available hoices of metal clusters and organic linkers. Nowadays these structure are foreseen to multiple applications in gas adsorption, like hydrogen storage, selective adsorption of CO2 against CH4, CO2 against H2. The Cu-BTC is chosen as a example of Metal Organic Framework that is available commercially of the demonstration of adsorption studied by Sievert's technique and heat flow calorimetry.

AN666 - Cyclic oxidation of metallic alloys by symmetrical TGA

Metallic alloys are frequently subjected to combined environmental attack and mechanical stresses during their actual service life. Their resistance to this complex loading relies partly on their ability to form a protective oxide scale, i.e. an oxide layer with low growth kinetics and high adherence to the alloy. The nature and kinetics of the growth of the oxide layer is ,most of the time, studied using isothermal laboratory tests. When testing the resistance to oxidation of high-temperature materials, the cyclic-oxidation test is used as a reference because it integrates isothermal oxidation kinetics, oxide-scale adherence, mechanical stresses, metallic alloy and oxide creep and the evolution of these properties with time, for conditions close to the actual conditions of use. Such a cyclic test is run with the symmetrical TAG thermobalance

AN665 - Differential Reaction Calorimetry (DRC) for CO2 capture in amine solutions

The Differential Reaction Calorimeter is a very convenient calorimetri tool to investigate quickly and simply the potential of amine solutions for CO2 capture and help in the development of new technologies in the field of Carbon Capture and Storage

AN663 - Coupled manometric-calorimetric measurements on Mg-based materials for H2 storage

in recent years, increased efforts are under way to develop materials with reversible H2 storage properties meeting the targets for on-board applications fixed by the US Department of Energy. At this respect, it is fundamental to evaluate with accuracy both the thermodynamic and the kinetics sorption properties of the candidate materials. On the analytical point of view, the coupling between a manometric technique (PCTPro) and a calorimetric technique (Sensys DSC) is very interesting as both the absorbed/desorbed volume of hydrogen together with the corresponding enthalpy is measured on the same sample.

AN662 - Characterization of a polyimide by DSC

Polyimides are polymers known for their outstanding thermal stability. Indeed, they are well adapted for very tough conditions such as in aerospace, in insulating material or in protective clothing. In the industry, the verification of the resistance of a polyimide requires the knowledge of its thermal profile that is easily obtained with the DSC method.

AN661 - Characterization of PEN (PolyEthylene Naphtalate) by DSC

PolyEthylene Naphtalate (PEN) is a polyester which has the property to be a particularly good oxygen barrier. Hence, it is well adapted to protect compounds susceptible to oxidation. In the industry, to obtain the best properties of the polymer, the thermal handling as to be thoroughly controlled. The DSC test is very useful to determine its thermal profile

AN660 - Characterization of PTFE (Teflon) by DSC

PolyTetraFluoroEthylene, more commonly known under the name of Teflon®, is essentially used for its non-stick properties. In addition, because of its chemical stability and electrical insulation properties, it can be employed in many domains. In order to make the best of its abilities, it is essential to understand the thermal profile of PTFE using the DSC technique.

AN659 - Characterization of glass transitions of different polymers (PVC, PS, SAN, PEEK and PES) by DSC

Glass transition is the transformation of a solid or liquid polymer into a vitreous state. This state is characterized by a modification of the polymer physical properties such as viscosity, thermal expansion or heat capacity. The glass transition temperature (Tg) is easily determined by DSC. The ISO1135762 standard describes the experimental Tg determination for polymers

AN658 - Melting of different polymers (PTFE, Nylon6, PP, PE-LLD, PE-MD) by DSC

When the polymer's melting temperature is reached, the crystals begin to fall apart. The chains come out of their ordered arrangements, and begin to move around freely. So the knowledge of the melting point of a polymer is one of the basic information for its use. This temperature depends most of all on the type of polymer but also on its crystal forms, including plasticizers or other additives. The melting point of a polymer is easily determined by DSC and measured at the top of the endothermic peak. The dedicated ISO11357-3 standard describes such a melting determination. In this note are given the melting curve of different types of polymers

AN657 - Shrinkage temperature of bovine pericardium tissue for bioprosthetic heart valve application by MicroDSC

Bovine pericardium, a fibrous tissue enclosing the heart of a cow, is commonly used for heart valve replacement. It possesses excellent hemodynamic properties (the ability to move blood) but lacks the same long-term durability of mechanical valves. Glutaraldehyde stabilizes the collagen structure and increases its durability. The stabilizing effects of cross-linking agents such as glutaraldehyde can be assessed by measuring the shrinkage induced by denaturation of tropocollagen of the tissue. So denaturation temperature (DT) coinciding with a temperature at which the collagen shrinks can be used as a measure of the "shrinkage temperature"(ST). The goal of this study is to measure the ST change, which reflects the stabilizing effect of glutaraldehyde, and to find correlations with the mechanical testing results.

AN656 - Melting of different types of chocolates by DSC

Chocolate is mainly composed of cocoa butter, cocoa paste and sugars. Moreover, the composition could differ from one type of chocolate to another. The dark chocolate contains solid cocoa, cocoa butter and sugar. In the milk chocolate, powder milk is added. In the white chocolate, there is no solid cocoa. Then, the thermal profile is an essential information for the industry to improve the quality and properties of their products, like for example the ability to be solid at room temperature and soft in the mouth.

AN655 - Denaturation of albumin by MicroDSC

Albumins are major proteins which are found in many food products such as egg white, milk or meat. These proteins are able to coagulate under the influence of the temperature. This thermal property is commonly used in food processes, such as in sugar refining to clarify the solutions or as emulsifying and gelling agents.

AN654 - CO2 adsorption into coal measured by PCTPro-E&E

In addition with the research for alternatives to reduce the use of hydrocarbon, every realistic future scenario confirms the continuous use of fossil fuel and thus the release of carbon dioxide (CO2) in the atmosphere. Therefore high research effort is needed to find ways to efficiently store CO2. Unminable coal bed are foreseen as potential solution for a sustainable storage. This application note shows the results of CO2 adsorption on two coal samples using the volumetric technique

AN653 - Methane adsorption into coal measured by PCTPro-E&E

Coalbed methane is an important source of energy in many countries. In contrast to a conventional gas reservoir, methane is stored by adsorption into pores of the coal. In underground coal mining, it presents a serious safety risk and is one of the leading causes of coal mine accidents. Thus characterization of methane uptake is essential to development of new technologies to harness energy while mitigating environmental and underground mining risks. This application note shows the results of methane adsorption into a coal sample at room temperature and up to 150 bar.

AN652 - Metabolism of mealworms monitored by microdsc

Mealworms are the larva of the mealworm beetle. The mealworm beetles go through four life-stages: egg, larva, pupa, and adult. Mealworms are food for other animals and are sold at pet tores to feed pet reptiles and birds. Worms like other living organisms generate heat when they move and consume nutrients. These result in heat flow measured by a calorimeter.

AN651 - Phase change of lipids under high pressures with HP-microDSC

Copepods are a group of crustaceans found in the sea and nearly every freshwater habitat. They are the smallest, but most abundant living species in the oceans. The way in which these animals survive the very low temperatures in the Antarctic ocean is probably linked with their lipids (or wax esters). High pressure ?DSC allows measuring the thermal properties of these lipids under different pressures, and more particularly their phase change properties.

AN650 - Methane adsorption into zeolite 13X with PCTPro-E&E

The Pressure Swing Adsorption (PSA) has become an alternative to expensive methods of CO2 sequestration in clean fuel burning technologies. The ability of zeolites to selectively adsorb molecules is exploited in methane gas separation and purification. Knowledge about methane and CO2 sorption properties of zeolites (adsorption capacity, pressure regimes and kinetics) is essential to the design of advanced materials capable of capturing methane and CO2 in industrial settings. Among zeolites, 13X is known for its relatively high methane and CO2 capacity. This application note reports on precision measurements of methane adsorption into zeolite 13X over a temperature range 0-50 °C

AN649 - Combined calorimetric and sorption measurements on Mg-based hydride with small sample mass

The thermodynamic stability of hydrides is a key to applications in hydrogen storage. As shown in AN622, it is possible to quantify both the heat of formation of the hydride and its hydrogen sorption capacity using a combined calorimetric and sorption technique. In this example, the sample is small and the HP cell of the Sensys is used for such a coupling with the PCTPro-2000.

AN648 - Larger Adsorption Capacity of CO2 compared with H2 in MOF's demonstrated with PCTPro-E&E

Atomistic simulations have shown MOFs to be an excellent material for high-pressure selective adsorption of CO2 over H2. The PCTPro E&E allows for facile adsorption measurements of these two sorbates in MOFs, leading the community in this new and important application. As a showcase example, data for two MOFs are presented showing selectivity for CO2 at pressures up to 50 bar.

AN647 - CO2 adsorption into zeolite 13X with PCTPro-E&E

CO2 Absorption studies on a zeolite 13X at different tempratures.

AN646 - Decomposition of NH3BH3 studied by coupling Calorimetry, Sievert's method and Mass Spectrometry

Study of the thermal decompostion of ammonia borane with an innovative combination of Sievert's technique, calorimetry and mass spectrometry.

AN645 - Crystallization of palm oil by DSC

Classically, crude palm oil has to undergo processes to improve its qualities before being proposed on the market. In a first step, an absorption bleaching is performed to produce refined palm oil. This latter is constituted by a liquid phase and a solid phase which could be separated by a fractionation process. This process is based on the crystallization temperature of each phase, that is why, the thermal profile of palm oil should be clearly established. It will be shown that DSC 131 is an equipment perfectly adapted to characterize palm oil in terms of crystallization and quality control.

AN644 - Fish oil (omega-3 fatty acid) oxidation by DSC

Fish oil is a product extracted from several species of fish, like herring, sardines or mackerels. It is frequently used as a supplement which provides omega-3 fatty acids, well known to regulate cholesterol in the body. For that use, fish oil is usually marketed under the form of softgels for an easier absorption. The determination of fish oil oxidation is very important to understand its mechanisms in the body

AN643 - Influence of pressure on wax precipitation in crude oil with HP-MicroDSC

The presence of paraffin hydrocarbons (C18 - C36) and naphthenic hydrocarbons (C30 - C60) in crude oil, diesels and biodiesels is known to cause wax precipitation at low temperature. Solidified waxes thickens the oil and allow to clog fuel filters and injectors in engines (in the case of diesels or biodiesels) and can cause flow assurance related problems as bad as full pipeline blockage (in the case of crude oil). The prevention of precipitation requires a detailed characterization of the crude oil. On top of its simplicity and fast response, Differential Scanning Calorimetry (DSC) technique has the advantage of allowing operations at the high pressures that can be met in engines or pipelines.

AN642 - Determination of melting peaks of sugar solutions by DSC

The melting point of a sugar solution is an important characteristic in the syrup and ice cream manufacturing processes. It depends on the concentration of sugar in the solution following the phase diagram of sucrose in water

AN641 - Characterization of a polymorphous powder by DSC

The characterization of crystal polymorphisms in drugs is an important point for the pharmaceutical industry. This importance is justified by the fact that the properties of a drug depends a lot on its polymorphic forms. One of the DSC important issue is the qualification of polymorphs and the determination of their stabilities.

AN640 - Thermal stability of therapeutic proteins with MicroDSC3

Antibodies are gamma globulin proteins that are found in blood or other bodily fluids of vertebrates, and are used by the immune system to identify and neutralize foreign objects, such as bacteria and viruses. Antibodies can either neutralize targets directly by, for example, binding to an infection-leading part of a pathogen, or recognize an antigen and tag it for attack by other parts of the immune system. DSC allow to test and understand thermally induced unfolding of immunoglobulin

AN637 - Adsorption and desorption of CO2 on hydrophilic amine polymer in humid atmosphere using the TGDSC technique

Solid sorbents, such as hydrophilic amine polymers, are known to have a large capacity of CO2 adsorption with a full regeneration after heating. To investigate such a process, the TG-DSC technique, combined with the relative humidity generator Wetsys, is the ideal tool

AN636 - Application of thermogravimetric analysis to the evaluation of aminated solid sorbents for CO2 capture

The enhancement of a specific adsorption capacity may be carried out by promoting chemisorption through impregnation with chemicals that react reversibly with CO2, such as amines

AN635 - Enthalpy and solubility data of CO2 in water and NaCl(aq) at conditions of interest for geological sequestration

The data on solubility of weak electrolyte gases like carbon dioxide and hydrogen sulphide in geological brines are therefore of direct interest for processes developed, namely by the petroleum industry, for storage of the acid gases

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AN634 - Adsorption and desorption of CO2 on active coal

With the TG-DSC experiment, it is possible to determine the corresponding enthalpies of adsorption or desorption versus the amount of CO2 adsorbed or desorbed on the sample

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AN633 - CO2 sorption on activated carbon in presence of water

Volumetric technique and in particular the PCTPro-2000 are well suited to characterize any type of CO2 sorption on solid media. Its wide ranges of temperature and pressure permit to access to a large number of applications in carbon capture and sequestration.

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AN632 - Hydrogen uptake measurement on MOF-177 in order to establish a benchmark for hydrogen adsorption.

Use of PCTPro for the determination of PCT isotherms for Metal Organic Frameworks (MOF's)

AN631 - Measurement of PCT isotherms on sodium alanate with different level of Ti-doping

Use of PCTPro for the determination of PCT isotherms for alanates

AN630 - PCT isotherms of Mg-Ni-Cu mixtures prepared by reactive mechanical grinding

Use of PCTPro for the determination of PCT isotherms for metallic hydrides

AN628 - Temperature programmed desorption on amide- hydride mixture

Use of PCTPro as a TPD technique for metallic hydrides

AN627 - Measure of the heat of adsorption of hydrogen in microporous high-surface-area materials

Use of PCTPro with the Microdoser attachment for measuring adsorption of hydrogen on microporous materials

AN624 - CO2 sorption measurement of materials used infood packaging

Precise determination of CO2 gas sorption properties of the well known packaging material, polyethylene terephthalate (PET) with the PCTPro-2000

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AN623 - Combined mass spectrometry and sorption measurements on mixed Alanate-Amide hydrogen storage materials

Combination of PCTPro and mass spectrometry for investigation of hydrogen storage

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AN622 - Combined calorimetry and hydrogen sorption measurements on LaNi5

Combination of C80 and PCTPro to investigate the hydrogen sorption on metallic hydride

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AN620 - Study of the Setting of a Cement by µDSC3

Presents the setting of a cement in microDSC3

AN618 - Characterization of CTAB-based w/o microemulsions

Presents the characterization of CTAB-based w/o microemulsions

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AN617 - Micellisation of aqueous block copolymer solution in presence of propofol

Presents the micellisation of aqueous block copolymer solution in presence of propofol

AN616 - Transition behavior of hydrophobically modified N-isopropylacrylamide copolymer solution

Presents Transition behavior of hydrophobically modified N-isopropylacrylamide copolymer solution

AN615 - Denaturation and aggregation of IgG immunoglobulin with MicroDSC3

Presents the denaturation and aggregation of immunoglobulin

AN614 - TG-DSC + FTIR of tobacco

Presents the decomposition of tobacco with analysis of evolving gases

AN613 - Analysis of wood and paper

Presents the decomposition of paper

AN611 - Adsorption and desorption of CO2 on a catalyst

Presents the adsorption and the sedorption of CO2 on a catalyst

AN610 - Determination of quartz content in inorganic material

Presents a method to determine the quartz content in an inorganic material

AN609 - Decomposition of an organic compound

Presents the decomposition of an organic compound

AN608 - Martensitic transitions in a TiNi shape memory alloy

Presents the transitons observed during the austenite to martensite transitions

AN607 - Oxidative Induction Time (OIT) of polyolefines

Presents the oxidation of different polyolefines

AN606 - Melting of polyethylene

Presents the melting of different polyethylenes

AN605 - Curing of an epoxy resin

Shows the curing of an epoxy resin and the Tg is determined during the first heating

AN585 - TG FTIR analysis of a carbon fiber

Carbon fiber is most notably used to reinforce composite materials, particularly the class of materials known as carbon fiber or graphite reinforced polymers. A common method of making carbon filaments is the oxidation and thermal pyrolysis of polyacrilonitrile (PAN). The interest of the TG + FTIR is to quantify the non pyrolyzed material and to identify the substances remained with the final carbon fiber.

AN584 - Sintering of a WC + Co pellet

Sintering is a process for making objects from powder, increasing the adhesion between particles as they are heated. It is used with ceramic powders and in powder metallurgy. Sintering is related to diffusion. Tungsten carbide is generally prepared from a powder containing WC and Cobalt as a bind.

AN578 - Oxidation of a metallic plate at 1100°C during 100 hours under O2

oxidation of a metallic plate

AN577 - Study of the reactivity and stability of organic azides by C80 coupled with gas analysis

decomposition of azides

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AN576 - DSC analysis of a phase change materials at very slow scan rate

The variation of enthalpy of a phase change material is determined by DSC at a very slow scan rate (0,05K/min = 3K/h) in order to approach, as well as possible, the real condition of use of material.

AN575 - DSC analysis of a plaster containing phase change materials

The variation of enthalpy of a plaster containing phase change materials is determined by DSC.

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AN559 - A calorimetric study of steroid-liposome interactions

High sensitivity differential scanning calorimetry was employed to investigate the interaction between dimyristoylphosphatidylcholine (DMPC) liposomal bilayers and the model steroid beclometasone dipropionate (BDP).

AN558 - Oxidation behavior of the 9%Cr steel P91

The oxidation behavior of the 9%Cr steel P91 was studied by thermogravimetry in model N2-O2-H2O gas mixtures at 650°C

AN557 - Enthalpy of solution of CO2 in aqueous solutions of 2-amino-2-methyl-1-propanol (AMP)

A flow calorimetric technique was used to measure the heat of absorption of CO2 in aqueous solutions of AMP.

AN555 - Absorption of humidity of a lyophilized pharmaceutical sample

The purpose of this test is to determine the absorption of humidity of a lyophilized pharmaceutical sample by TG-DSC.

AN554 - Study of the distribution of the size of water droplets in an emulsion

Presents the determination of the droplet size of an emulsion by DSC.

AN553 - Analysis of cement samples by thermogravimetry coupled with FTIR spectrometry

The aim of these analysis is to identify the evolve gas from a cement sample by thermogravimetry coupled with FTIR spectrometry.

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AN552 - Hydrogen absorption-desorption in CeNi2

Thermal effects of hydrogen absorption-desorption in CeNi2 were studied by calorimetry.

AN551 - Hydration of hydratable alumina

The objective of this work is to determine, by thermogravimetry, the difference in the hydration products between the mixtures of hydratable alumina with reactive magnesia and those of hydratable alumina with deadburnt or fused magnesite powder.

AN550 - Characterization of H-Titanate nanotubes

H-titanate nanotubes are synthesized from Na-titanate nanotubes and then they are analyzed by thermogravimetry.

AN549 - Analysis of municipal waste residues with and without flue gas cleaning system

The aim of this paper is to study by TG-DSC a residue originate from a municipal solid waste incinerator (MSWI) after installing a wet flue gas cleaning system.

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AN548 - Carbonation of bottom ash

Simultaneous TG/DSC was used before and after a complete carbonation of bottom ash in order to investigate calcite formation resulting from accelerated carbonation.

AN547 - Determination of CO2 hydrate dissociation enthalpy by multi-cycle DSC

Measurements of the CO2 hydrate dissociation enthalpy were performed by DSC.

AN546 - Oxygen stoichiometry of LaGa0.65Mg0.15Ni0.20O(3-d)

Oxygen stoichiometry of LaGa0.65Mg0.15Ni0.20O(3-d) was estimated by TGA

AN545 - Adsorption and desorption of H2 at 20 bar at 400°C on an Mg alloy

DSC was used to study the adsorption and desorption of hydrogen on an Mg alloy when the pressure is increased to 20 bar and the temperature stabilized at 400°C.

AN544 - PEG/C12E6 phase diagram obtained by DSC

The aim of this study is to determine the phase diagram of PEG (polyethylene glycol) / C12E6 (n-dodecyl hexaoxyethylene glycol monoether) water solution.

AN543 - Oxidation behavior of alumina deposit on austenitic stainless steel

TGA was used to study the oxidation behavior and its improvement thanks to the alumina deposit on austenitic stainless steel.

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AN542 - A study of the adsorption of thiophenic sulfur compounds using flow calorimetry

The adsorption of refractory benzothiophenic type S compounds present in diesel was studied using a liquid phase flow calorimetry technique with hexadecane as a solvent and zeolites as sorbents.

AN541 - Study of oxidation behavior of y-AlON-TiN by thermogravimetry

In order to study the effect of TiN on AlON oxidation properties, AlON-TiN composites plates have been analyzed by thermogravimetry in the temperature range 1100-1500°C.

AN540 - Follow-up of the BaTiO3 formation by TG-DTA

The formation of barium titanate powder by solid-state reaction and oxalate coprecipitation route is investigated by TG-DTA

AN539 - Sintering shrinkage of WC-Co materials with bimodal grain size distributions

Experiments were carried out in a TMA to explore the influence of wide grain size distribution on sintering shrinkage of WC-Co materials.

AN538 - Enthalpies of mixing of a lead-free soldering : Ag-Pd

Enthalpies of mixing of the lead-free soldering Ag-Pd were measured by the drop calorimetric method

AN537 - Linear thermal expansion of (Pu0.25,Zr0.25)N pellets

In order to predict the in pile behaviour of nitride fuels, the thermophysical properties of plutonium-zirconium nitride (0-25at.% Pu), in particular the density, were measured on pellets.

AN536 - Crystallization behaviour of the metallic glass Fe75Si9B16

DSC measurements were used to investigate the transformation from the amorphous to the crystalline state during heating of Fe75Si9B16

AN535 - Pyrolysis of waste tyres

Thermogravimetric method was used to obtain previous information about the thermal decomposition process of the tyre material. Then, the gas generated during the pyrolysis was analyzed by gas chromatography.

AN534 - Analysis of sewage sludges by thermogravimetry

The aim of this paper is to predict the behavior of sewage sludges, the principal waste produced by a sewage treatment plant, in combustion or pyrolysis by thermogravimetric analysis and determine, from that, the parameter PII/(PI+PII).

AN533 - Effect of sonication time on the phase transition of DODAB vesicles

DSC technique is used as a systematic method of investigation of the influence of sonication time on the phase transition of DODAB vesicles

AN532 - Temperature memory effect in CuAlNi and CuZnAl shape memory alloys

DSC was used to determine the temperature memory effect in CuAlNi and CuZnAl shape memory alloys

AN531 - Incomplete transformation of a TiNi shape memory alloys

DSC was used to bring out the incomplete transformation of a TiNi shape memory alloy during an incomplete cycle on heating and cooling

AN530 - Detection of Low Level (0.3%) of Amorphous Phase in lactose thanks to Thermally Stimulated Current Technique (TSC)

TSC technique is particularly suited for detection of low levels of amorphicity in crystalline structure. Example given here is the lactose, a classical excipient used in the pharmaceutical domain. We have chosen this molecule as a model to demonstrate the sensitivity of our TSC II

AN529 - Measure of reactivity of asphalt-salt mixtures by calorimetry

The reactivity of asphalt-salt mixtures (ASMs) was measured by using a heat flux calorimeter (C80) and then, the C80 data was used to calculate the SADT (self-accelerating decomposition temperature) of simulated ASMs.

AN528 - Hazard evaluation of self-decomposition materials by the combination of pressure and heat flux measurements

The use of C80 heat flux calorimeter with a very low scanning rate provides an easy approach to identify and determine the intrinsic characteristics of an unstable substance associated with the exothermic decomposition in a closed vessel

AN527 - Oxidation behavior of Single-Walled Carbon Nanotubes (SWCNTs)

TGA was used as a tool to measure the SWCNTs content, the amounts of nontubular carbon impurities and the metal content in SWCNTs samples

AN526 - Hydration process of calcium phosphate cement

Presents the hydration process of calcium phosphate cement by calorimetry

AN525 - Study of ribosome's core deprived of proteins

The DSC approach was used to investigate ribosome's cores deprived of proteins as a consequence of LiCl treatment.

AN524 - Structural studies of E. coli ribosomes : 70S ribosomes and 50S subunits

Presents the transitions observed in 70S ribosomes and 50S subunits of E. coli.

AN523 - Thermochemical activities during the silicon nitride and carbon interaction

Study by thermoanalytical techniques the interaction and the reaction between silicon nitride and carbon

AN522 - The influence of wood aqueous extractives on the hydration kinetics of plaster

Presents the influence of wood aqueous extractives on the hydration of plaster by calorimetry

AN521 - Adsorption of CO2 on a drug during its transport in dry ice

When a drug is transport or store in dry ice, the carbon dioxide can be adsorbed on the drug. In order to simulate these conditions, the sample is studied at -70°C under CO2 in a thermobalance. The mass variation brings out the adsorption.

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AN520 - Testing Ceramics

testing thermal conductivity on ceramics

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AN517 - Storage of hydrogen: hydriding of Ti-Mg-Ni mechanically alloyed

Presents hydrogen absorption on an alloyed mixtures of Ti-Mg-Ni by DSC

AN516 - Sintering of Silicon Carbide (SiC)

Presents the sintering of Silicon Carbide (SiC)

AN515 - Phase transition of a solution of amphiphilic polymer

Present the phase transition of a solution of amphiphilic polymer studied by microDSC

AN514 - Use of isothermal Microcalorimetry to evaluate stability of Ascorbic Acid

Several factors could modify the stability of Ascorbic Acid, the aim of this study is to test the impact of hydrogen peroxide on its decomposition thanks to microcalorimetric technique.

AN512 - Decomposition of nitrocellulose + nitroglycerine with kinetic study by C80 + AKTS

Presents the decomposition of nitrocellulose at different heating rates by calorimetry

AN502 - Detection of low Levels of Amorphous Phase in Crystalline Pharmaceutical materials by Thermally Stimulated Current

TSC technique is here used as a quantitative method, indeed it has been possible to quantify low level of amorphous phase (1%) in a crystalline pharmaceutical compound.

AN501 - Oxidation behavior of Ti3AlC2 powders in flowing air

the oxidation behaviour of Ti3AlC2 powders has been investigated in air by means of simultaneous TGA-DSC, XRD, Raman spectra, SEM, EDS and BET specific surface measurement to understand the intrinsic oxidation behaviour of this newly developed ternary compound.

AN500 - Improving the oxidation resistance of Ti3SiC2 by forming a Ti3Si0,9Al0,1C2 solid solution

Ti3Si(Al)C2 solid solutions with different Al contents were prepared by substituting a small amount of Si with Al. The results demonstrated that the substitution of Si with 10 at % of Al dramatically improved the oxidation resistance and eliminated TiC. The oxidation behavior of the Ti3Si0,9Al0,1C2 solid solution in air was then investigated at 1000-1350 °C. The oxide layers were dense, adher ent and resistant to thermal cycling.

AN397 - Direct Calorimetric Measurement of Enthalpies of Phase Transitions at 2000°C-2400°C in Yttria and Zirconia

High-temperature differential thermal analysis provided data on phase transitions in zirconia and yttria. The tetragonal form of ZrO2 transforms to the cubic fluorite structure at 2311±15°C with an enthalpy of 3.4±2 kJ/mol. Cubic C-type Y2O3 transforms, probably to the fluorite structure, at 2308±15°C with ?H=47.7±3.0 kJ/mol. This high-temperature polymorph melts at 2382±15°C with an enthalpy of fusion of 35.6±3.0 kJ/mol.

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AN396 - Study of a Thermite Reaction: Fe2O3 + 2 Al --> Al2O3 + 2 Fe

A thermite reaction (a type of aluminothermic reaction) is one in which aluminium metal is oxidized by an oxide of another metal, most commonly iron oxide. Although the reactants are stable at room temperature, when they are exposed to sufficient heat to ignite, they burn with an extremely intense exothermic reaction. Thermite contains its own supply of oxygen, and does not require any external source (such as air). Consequently, it cannot be smothered and may ignite in any environment (it will burn perfectly well underwater, for example), given sufficient initial heat. Such a reaction can be successfully be studied by drop calorimetry and its heat measured.

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AN395 - Thermochemistry of Water Adsorption on Hafnia and Zirconia Surfaces

Novel setup for gas adsorption microcalorimetry, unique to UC Davis Thermochemistry Facility, employs Micromeritics ASAP 2020 as dosing system and Setaram Calvet-DSC111 operated in isoperibol mode as calorimetric detector for heat of adsorption.

AN391 - Behaviour of a Drug under Controlled Humidity

Presents the analysis of the behaviour of a drug under controlled humidity : it is done with C80 calorimeter connected to a wetsys

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AN390 - TSC/DSC : Sensitivity Comparison on the Tg Determination for a Poly(amide)

Presents a comparison of the determination of the Tg of a polyamide by both DSC and TSC methods

AN389 - Study of collagen

Presents the study of collagen by TSC

AN388 - Determination of crystalline.amorphous phase

Presents the determination of cristalline / amorpous drug by TSC method

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AN387 - Purity determination by DSC

Presents the method of purity determination by DSC using the Van t'Hoff relation. Application to different samples of phenacetin

AN386 - Cp of Nickel in continuous mode between 50°C and 450°C

Presents the determination of Cp of nickel between 50°C and 450°C

AN385 - Cp of Hastelloy in step mode between -50°C and 200°C

Presents the determination of Cp of hastelloy between -50°C and 200°C

AN384 - Heat of wetting of carbon with water at 20°C

Presents the wetting of carbon by water on using an ampoule mixing vessel

AN383 - Heat of wetting of TiO2 with water at 30°C

Presents the wetting of TiO2 by water on using an ampoule mixing vessel

AN380 - Study of a process in off normal conditions : synthesis and decomposition of a diazo compound using the C80 safety vessel.

Before carrying out chemical processes in pilot or production plants, they are subject to a thorough risk analysis. As a part of the risk analysis related to a chemical process, thermochemical data are needed to assess the thermal risks. The heat of the reaction, the energy released in case of triggering the decomposition reaction, the amount of gas released during a runaway, etc are current questions during a risk analysis in a the chemical industry. The Swiss Institute of Safety and Security in Basle has designed in collaboration with Setaram a new Mini-Reactor adapted to the study of chemical reactions in order to determine rapidly the data required for a first screening of the thermal risks.

AN379 - Synthesis of 2, 3, 6-trimethyl, 4-nitrosophenol

Presents the synthesis of 2, 3, 6-trimethyl, 4-nitrosophenol with DRC

AN378 - Reduction of an Intermediate of Azithromycin

Presents the reduction of an Intermediate of Azithromycin

AN377 - Study of a process in normal conditions : esterification of propanoic acid by 2-butanol

Presents the esterification of propanoic anhydride by 2-butanol

AN376 - Hydrolysis of acetic anhydride at 10°C, 25°C and 40°C

Presents the hydrolysis of acetic anhydride at 10°C, 25°C and 40°C

AN375 - Self discharge of lithium batteries

Presents the calorimetric curve obtained during the self discharge of a lithium battery

AN374 - TG of epoxy resin with Labsys DSC

Presents the DSC curve obtained with LabsysDSC showing the Tg of an epoxy resin

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AN373 - Expansion of a steel between ambient and 1400°C

Presents the expansion of steel up to 1400°C : shows a phase transition

AN372 - Heat capacity of a steel betwwen 50°C and 1550°C (liquid state)

Presents the heat capacity of steel in the solid and liquid phases

AN370 - Expansion of a graphite sample (Ø=18 mm; h=50 mm)

Presents the measures of expansion of graphite

AN369 - Oxidation of a steel during temperature cycling

Presents the oxidation of a piece of steel when temperature is cycled between 500°C and 1100°C

AN368 - Oxidation of a steel at 1000°C

Presents the oxidation of a piece of steel studied at 1000°C

AN367 - Analysis of plaster with high volume TG

Presents the TG analysis on a large sample (13 g) of sample

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AN366 - Crystallization and melting of mandelic acid in the cooling and heating modes

Presents the melting and cristallisation of mandelic acid with DRC in the scanning mode

AN364 - Reaction of hydrogen peroxide on an amine in water emulsion

Presents the reaction of synthesis of hydrogen peroxide on an amine in water emulsion with DRC

AN363 - Synthesis of polyepichlorhydrin

Presents the reaction of synthesis of epichlorhydrin with DRC

AN362 - Study of process in normal conditions by DRC Evolution : nitration of chlorobenzene

Presents the reaction of nitration of chlorobenzene with DRC

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AN361 - Melting of butters and margarine by DSC

Butters and margarines are mainly composed of droplets of water (about a concentration of 16%) in a fatty matrix. The proportions of these components induce the thermal characteristics of the final product. In the industry, determination of their thermal profiles is essential to control their properties in term of "easy-to-spread" and good thermal stability, especially at room temperature. The DSC technique is the ideal tool for such investigations

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AN360 - Sintering of a steel powder under vacuum

Presents the sintering of steel powder when heated under vacuum

AN354 - Flexure of epoxy printed circuit boards

Printed circuit (PC) boards are composed of several conducting layers intercalated with epoxy resin prepreg layers. These different layers are pressed together and then heated until reticulation. After reticulation, the thermal expansion coefficient of the PC board is lowered, which prevents metallic wires soldered on it from being broken. In flexure mode, the sample is supported by two parallel edges ; a load is applied on an edge-ended probe which comes to rest in the middle of the sample.

AN352 - Controlled sintering rate of hydroxyapatite (2)

During a test with controlled sintering rate, the heating rate is no more constant but decreases if the sintering rate becomes higher than the preset value. The enlargement of the previous temperature curve shows the temperature profile required to obtain a sintering process at a rate which never exceeds the preset value.

AN351 - Controlled sintering rate of hydroxyapatite (1)

The densification which occurs during the sintering process allows to obtain chemically, thermally and mechanically stable materials. However, the properties of the materials can be still improved by maintaining a constant and not too fast rate of shrinkage during the sintering (see application sheet AN350). With a specific software package it is possible to simulate a sintering process at a constant rate of shrinkage, the temperature scanning rate being controlled simultaneously.

AN350 - Sintering of hydroxyapatite

Hydroxyapatite, a derivative of a calcium phosphate mineral, is the main inorganic component of vertebrate bone and tooth tissue. Sintered hydroxyapatite ceramics should have medical applications as bone fillers or artificial tooth roots.

AN349 - Sintering of carboniferous shale

Shales are very fine-grained varieties of sedimentary rocks composed of clay, quartz, mica and other minerals. Sintered carboniferous shales can be used as building materials.

AN348 - Sintering of refractory clay

Refractory clays contain only small amounts of fluxing impurities but high amounts of silica, alumina and water and therefore capable of withstanding high temperatures. A refractory clay is considered as a fire-clay if its melting point exceeds 1600°C.

AN347 - Thermomechanical behavior of Ni-based superalloy

For numerous industrial applications, metallic alloys need to have a high resistance to oxidation and corrosion and good mechanical properties, especially between 700 and 1000°C. Among them, Nickel-based superalloys are often used with additive elements such as Chromium to resist oxidation and Molybdenum, Titanium and Niobium to reinforce the initial metallic matrix.

AN346 - Expansion of carbon powder

With the SetsysTMA, it is possible to study the thermomechanical behavior of powder samples. The powder is contained in a crucible, the height and external diameter of which are respectively 20 mm and 10 mm. A flat-ended probe, with a diameter end of 7 mm, is brought into contact with the sample within the crucible.

AN345 - Characterization of glass

The Setsys 92, equipped with a furnace composed of a metal heating coil surrounding an inner silica tube, allows experiments to be carried out up to 1200°C. Thus, glasses can be characterized by different parameters such as : the glass transition temperature, the softening point, the true and average coefficients of thermal expansion ?.

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AN344 - Correlation between TMA and DSC data of PET

Glass transition, softening, crystallization, melting are events which cause a change in the characteristic properties of a compound like its heat capacity or its thermal expansion coefficient. These changes can be observed by both DSC and TMA measurements.

AN343 - Glass transition and thermal expansion coefficient of epoxy resin

The epoxy resins are thermoset polymers often used in the elaboration of composite materials for aircraft industry. The resulting composite compounds have good mechanical properties and can be utilized up to 150°C to 200°C.

AN342 - Glass transition of butadiene-styrene copolymer

The SetsysTMA equiped with a cryostat allows thermomechanical measurements to be carried out at very low temperature (down to -150°C), like the determination of the glass transition temperature of polymeric materials. The glass transition temperature can be defined as the temperature at which a material loses its glass-like rigid properties and becomes more flexible in nature like rubber. This event is accompanied by a student increase of the thermal expansion coefficient of the material.

AN338 - Metabolism of ladybird (Coccinella septempunctata L)

Direct calorimetry is a method which consists in monitoring the heat production of living organisms : it gives direct information about their aerobic and anaerobic metabolism.

AN336 - Thermal behaviour of an antibiotic

The knowledge of the behavior of pharmaceutics has a certain importance as it can give information about an eventual decomposition process. For the certification of drug stability certain tests are generally required : a calorimetric experiment will enable the analysis of a substance required for prescribed conditions.

AN334 - Propellant stability

A propellant is generally a mixture of two substances which decompose strongly after ignition. But also in storage conditions this mixture can react very slowly and this process must be surveyed. It is accomplished by carrying out isothermal experiments with less than one gram of sample at different temperatures (50°C, 60°C, 70°C, 80°C for example). The lost time between two experiments is only 1000s ? 17 min. (see application sheet TN335).

AN333 - Stability of a fertilizer

A fertilizer is generally a medium, which can supply to plant roots elements like N, P, K, Mg, S, Ca.. They are provided under a mixture of NH4NO3, phosphates, P2O5, K2O, MgO, SO3.. When they are stored these mixtures can age. A calorimetric experiment carried out at a fixed temperature can give information about the fertilizer behavior at this temperature.

AN332 - Thermal stability of sulphur

Sulfur is a base compound for the processing of rubber through the vulcanisation process. During this process a fine powdered ?-sulfur is incorporated into the crude rubber then heated. When heated, ?-sulfur will transform into ?-sulfur but this transformation must be avoided for a good vulcanisation because the ?-sulfur aggregates and then creates heterogeneity inside the vulcanized compound. It must be pointed out that the process has been monitored only on using a very slow scanning of 2 K.h-1. All the attempts at higher scanning rate were not successful : it demonstrates that only a very sensitive instrument can be used and that a conventional DSC will not be sensitive enough.

AN331 - Phase transitions in a liquid crystal

With a normal DSC, experiments are generally carried out at a high scanning rate (5 K.min-1). In these conditions the determination of solid-mesophase or mesophase-isotropic liquid transitions can be performed easily. Bus as far as the mesophase-mesophase transitions analysis is concerned, much smaller scanning rate are required (a few K.h-1 or less). The main drawback is that in these conditions CONVENTIONNAL DSC IS NOT SENSITIVE ENOUGH. For these reasons micro-DSC, A VERY SENSITIVE DSC IS OF GREAT INTEREST. The capability of the micro-DSC of scanning the temperature upwards and downwards is also essential as it can provide information about the reversibility of the different transitions. This facility is especially important with the MONOTROPIC crystals which present mesophases only in the cooling mode.

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AN330 - Phase transition of DPPC

DPPC or DIPALMITOYL PHOSPHATIDYLCHOLINE is one of the main constituents of cell membranes. Its dispersion in water presents two endotherms : at low temperature a gel / gel transition involving a molecular packing rearrangement between two gel-state forms, and a gel / liquid crystalline phase transition, involving the melting of the hydrocarbon chains.

AN329 - Melting and gelation of kappa carrageenan by MicroDSC

Carrageenans are extracted from red algae and used in food processing for their gelation properties. This polysaccharide shows an order-disorder transition when heat-treated. The kappa-carrageenan, obtained under aggregating conditions in the presence of K+ ion, shows a single molecular process when heated and cooled. The kappa-carrageenan forms rigid, thermally reversible, high strength gels e.g. dessert gels, petfood gels, air freshener gels. The MicroDSC technique is well adapted to investigate the formation and the melting of such gels

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AN328 - Denaturation of an insulin solution

Insulin is the hormone which reduces the blood sugar concentration. It is synthesized by the pancreas. A disturbance in the synthesis leads to diabetes. Thus diabetic people need periodic injection of insulin. This insulin is now synthesized by genetic engineering. Insulin tends to denature and aggregate when it is in injection ready solution. It is of great interest to get information about these processes, as they must be avoided in practice.

AN327 - Stability of human growth hormone

hGH (or somatotropin) is synthesized in the anterior pituitary (hypophysis). A malfunction of the pituitary gland can lead to pituitary dwarfism. As treatment a hGH solution can be injected. An experiment in the temperature scanning mode will provide information about the thermal stability of the hormone : the processes of denaturation and aggregation can then be investigated.

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AN326 - Unfolding transition of ribunuclease A

The micro-DSC provides information on the enthalpy, temperature and heat capacity changes that accompany conformational transitions of biological molecules in solution.

AN325 - Helix-coil transition of plasmid DNA

The helix-coil transition of DNA is often called the "fine structure of DNA melting". The DSC method is so sensitive that it can detect small structural changes, even those due to cleavage of plasmid DNA with different restriction enzymes and the deletions of small portions of the DNA. Therefore, detailed DSC studies of the helix-coil transition, one of the most important physical properties related to such gene functions as replication, recombination, and transcription, are useful for further understanding of the structure of DNA.

AN324 - Thermal stability of a protease

Protease is a peculiar type of enzyme : its "mission" is to degrade other proteins. It is incorporated into washing powder : it is then the agent which will clean linen stained with blood, eggs,.. As it is to be used in a washing process it is important to know up to what temperature it can withstand denaturation

AN322 - Denaturation of a collagen solution

Collagen is the principal structural protein found in mammalian tissues, such as skin, bone, cartilage, cardiovascular tissue.. Generally extracted from bovine tissue, collagen is used for clinical applications such as hemostatic sponge, wound-dressing material, suture, nerve repair.

AN316 - Analysis of forsterite

This compound is found in large quantity in the earth's crust and corresponds to Mg2SiO4 formula where magmas are originated from. With TAG, it is determined that the decomposition of forsterite begins at around 1780°C.

AN315 - Thermal control of carbon fibers

Carbon and graphite fibers are the only ceramic materials made by one chemical element. Their properties are well known : low expansion coefficient, good resistance to thermal shocks, excellent chemical resistance, use at very high temperatures, easy to use, high thermal conductivity.

AN314 - Supercooling of a monocrystal

The neodymium doped LaMgAl11O19 compounds are used in LASER manufacturing. These compounds melt at high temperatures (around 1900°C). As crystal elaboration is carried out from a melted state bath, temperature must be well known. From a crystal nucleous soaked in the bath, a very slow stretching is carried out. The knowledge of the crystallization as well as possible supercooling must be determinate.

AN313 - Liquid - solid phase diagram

Liquid-solid phase diagrams can be calculated using thermal analysis techniques. In the field of very high temperatures, mixing of ceramics with a high melting point can be investigated. Like alloys, mixtures of ceramics have almost the same applications but at higher temperatures. For example, in some new motors cars, ceramics are introduced to protect the hot zones in the cylinders.

AN312 - Silicon carbide

Silicon carbide have good properties (tensile strength, ..) for a large range of temperatures. These materials have transformations at high temperature, which can modify the mechanical properties.

AN311 - Stability of uranium oxide at 2000°C

UO2 powder used as nuclear fuel is mixed with gadolinium oxide (Gd2O3). Gadolinium oxide is a neutron collector. The normal working temperature of these elements is about 1600°C but we can measure the properties and behavior of these material in the case of a temperature raise up to 2000°C.

AN310 - Study of boron-titanium ceramics

Boride based ceramics also have high melting point. They have particularly interesting applications in reducing gases or under vacuum at very high temperature. Titanium boride (TiB2) is especially required due to its refractory properties, its hardness and its electrical characteristics. It is used as cutting tool and for aircraft noses as well.

AN309 - Melting of metallic carbides

Metallic carbides are known to resist changes at very high temperatures. They have excellent characteristics of chemical inertia and mechanical resistance. It is important to study the thermal behavior of such products for their applications.

AN303 - Cycle temperature up to 1750 °C

The temperature of the furnaces of the TAG is scanned by the controller. Scanning rates when heating or cooling can be set from 0.01 K.min-1 up to 99.99 K.min-1. Studying alloys requires a high temperature limit (1750°C) with accurate heating and cooling scanning rates in order to determinate melting and crystallization points and also the evolution of these points after several cycles.

AN302 - Decomposition of calcium oxalate

Inorganic compounds, like oxalate, have well known decomposition reactions. With the calcium oxalate, the following reactions occur when heating up to 900°C. CaC2O4, H2O --> CaC2O4 + H2O --> CaCO3 + CO --> CaO + CO2

AN301 - Gas desorption by thermogravimetry

Sensitive materials like "silicon plates" are prepared under controlled atmosphere. Gas adsorption depends on the pressure and gas nature. When heating, theses gas can be desorbed and quantified thanks to thermogravimetry. The TAG must be used in a symmetrical configuration, to get a very high sensitivity of less than 1 µg. To be sure of the results, three cycles of temperature must be run ; the difference between the third and the second runs gives balance stability and measurement reproducibility.

AN299 - Phase transitions in zirconium alloys

Alloys have transitions or phase transformations. These transformations can be detected only by DTA, so a good sensitivity and a controlled atmosphere are needed to avoid others effects (oxidation, nitridation, ..). When a transition occurs it corresponds to a variation of heat capacity which is detected by a change of baseline on the DTA curve. This transition also changes the properties of alloys.

AN298 - Hydrogenation of "dead" catalysts

Some catalysts can be regenerated. A quick thermal analysis is able to separate the different compounds absorbed when being used and choose the appropriate cycle of regeneration. Such products are expensive and regeneration has to be done in the best conditions. To provide products like sulfur which are reacting with platinum at low concentrations, a "protected probe" without exposed platinum can be utilized up to 1750°C.

AN297 - Decomposition of sulfate

This classical example shows dehydration of pentahydrate copper sulfate CuSO4, 5H2O with argon sweeping at a rate of 1 l/h. TGA and DTA curves are plotted without any digital correction. Note : levels, separating the successive mass losses, are clearly horizontal, especially at the beginning of the heating. The DTA curve is stable. Symmetrical configuration is especially efficient when the available sample mass is small or when the variations in the expected mass are low.

AN295 - Thermal strength of carbon fiber

Silicon carbide fibers are known for their tensile strength and also thermal behavior at high temperature. It is used as fiber in composite materials. SiC fibers are analyzed in oxidizing atmosphere, they are heated up to 1500°C during 10 hours under air flow, to simulate, for example, an entry into the earth's atmosphere of a space shuttle. Mechanical properties can also be evaluated after this test.

AN294 - Kinetic reaction : carbon hydrogenation

A reaction can be studied with thermogravimetric method to determinate kinetic parameters. For one temperature, the derivative of the mass loss (DTG), usually constant, gives the speed of the reaction, the total mass loss, and the conversion rate. The active gas option is used to introduce hydrogen into the furnaces and to get a rapid atmosphere change. As platinum becomes brittle at high temperatures, under hydrogen, tungsten-rhenium thermocouples and tungsten crucibles are utilized.

AN293 - Quantity determination of water in powder milk

Milk powders have different composition for various utilization from baby milk to diet milk, but all include water, under the form of humidity or bound with other constituents. By thermogravimetric analysis, these two kinds of water can be separated. Stale milks and climate conditions modify these concentrations, and this analysis makes it possible to control these evolutions.

AN286 - Enzymatic reaction : amylase + maltose

The µDSCIII can be used at two levels for checking enzymes : defining the temperature limit of use of the enzyme (see application note AN285), and also for simulating an enzymatic reaction. Mixing vessels, consisting in two inlet tubes and one outlet tube, are available. In the example the reaction between a fungal gluco-amylase solution and a maltose solution is investigated, giving a transformation of the sugar.

AN285 - Thermal denaturation of an enzyme (fungal gluco-amylase)

Enzymes are specific catalysts of biochemical reactions. They are usually proteins which are denatured by temperature. A temperature scan gives a knowledge of the enzyme stability and thus of its working temperature range. For example, fungal gluco-amylase is used in the fermentation industry for enzymatic reaction (see application note AN286). The Micro DSCIII enables the thermal stability of the enzyme and the optimum temperature for its use to be determined.

AN283 - Thermal denaturation of animal proteins

Differential scanning calorimetry analysis can field information on the composition of multi-component systems, frequently encountered in foods, such as muscles. Muscle is a complex system consisting of different classes of proteins (myofibrillar, sarcoplasmic, collagenous). The DSC thermogram of the whole muscle shows the contribution of the proteins by their denaturation and enables identification of the main protein components (actin, myosin, sarcoplasmic proteins). Variations in this " fingerprint " of the muscles can be observed on the thermograms due to differences in the structure of proteins, different amounts of protein components, the state of the muscle. The µDSCIII is especially adapted for this type of analysis.

AN282 - Detection of a-lactose in whey powder

Dry milk and whey powder contain amorphous lactose. But the storage of these products under high relative humidity induces lactose crystallization (a-lactose monohydrate). This produces a dense powder, which becomes unusable for consumption. The DSC technique enables the a-phase to be detected by measuring the dehydration of the a-lactose monohydrate. This is a very easy and useful test for checking of whey powder and dried milk.

AN281 - Freezing of an extract of liquid coffee

For the frozen products, the DSC method can provide four different characteristics : the temperature at the beginning of freezing (especially for the solutions), the amount of ice at given temperature (also for the solutions), the temperature at the beginning of melting, the detection of possible phenomena of recrystallization. The temperature at the beginning of freezing is especially interesting for the industrial operations of extract freezing. It also defines the temperatures range of freeze drying for which the completely frozen water is evaporated under vacuum. In the example, the temperature of freezing of an extract of liquid coffee is measured.

AN280 - Oxidation of edible oil under pressure

The main problem caused by lipid oxidation is the formation of volatile compounds, which smell. This limits the time of conservation of different foods. When food containing lipids is heated, the temperature increases the degree of oxidation. This is especially true for edible oils used for frying. The pressure of oxygen has also an important effect on the kinetics of the oxidation reaction. The high-pressure crucible with gas flow under pressure is used in the DSC121 to characterize the effect of oxygen pressure on the oxidation of peanut oil.

AN278 - Determination of the Solid Fat Index (SFI) of Chocolate by DSC

The melting curve of a fat is generally complex: for a given fat, there is not a melting point, but more a melting range. In processing fat, it is also interesting to know, for a given temperature, what is the amount of fat melted. The DSC technique is now widely used to determine solid-liquid ratios in fats, called the Solid Fat Index (SFI). This method is based on measuring the heat of fusion successively at different temperatures. By reference to the total melting heat, the fraction of fat melted is determined. This technique is faster than dilatometry, and give results comparable with NMR. DSC gives the possibility of tempering the fat at different temperatures prior to index determining.

AN277 - Characterization of palm oils at different temperature scanning rates by MicroDSC

Palm oil is mainly constituted of esters of glycerol and fatty acids named glycerides. The composition of glycerides in oil is an important characteristic to control its quality. This composition can be determined following the specific phase transitions between polymorphic forms and solid-liquid phases of the constituents. It is shown that MicroDSC VII Evo is an equipment perfectly designed to characterize palm oil in terms of research and quality control.

AN276 - Tripalmitine melting : influence of heat treatment

When measuring melting points of fats or oils, some anomalies can be detected due to supercooling, but mainly to the fact that solid triglycerides exist in different crystalline forms (polymorphism), each of them with a different melting point. The crystalline form depends on the rate of cooling or heating, on the storage conditions (time, temperature..) These crystalline forms have an influence on the functional properties of the fat : butter spreading, milky aspects of oils.. The DSC 121 is used to characterize the crystalline forms of tripalmitine.

AN275 - Melting and solidification of cheese

Cheese is the curd of milk, basically a gel of casein. It contains mainly water, fat and proteins, the ratio of which depends on the type of cheese. If the curd is heated up to melting, a cream of cheese is obtained. The DSC test can give information on the thermal processing of cheese, also about possible storage at low temperature (refrigerator). On the example, a sample of cheese cream is cooled, then heated to show the thermal transformations in the product.

AN274 - Melting of different sugars by DSC

Different types of sugars are present in food products (sucrose, fructose, maltose, saccharose..). Many of them are used in the food industry, as a powder or liquid. During food processing, they are heated, cooled, quenched according to different heat treatments. The DSC test is useful in this case to characterize the thermal behavior of the sugar when heated or cooled, to know if the sugar is in a crystalline or amorphous form according to the preparation. In the example the melting of three different sugars is measured.

AN273 - Melting of an edible oil after different processes

Fats are either liquid at room temperature (oils) or plastic (solid fats). Crude fat or oil undergoes a series of manufacturing processes before it is marketed. These include treatment with alkali to remove impurities, dehydration, hydrogenation, fractionation.. Depending on the treatment, the consistency of fat is different. The DSC method, by measuring the melting of the triglycerides contained in the fat, shows what is the effect of the manufacturing process on the crude fat.

AN263 - Liquid adsorption : an hydrocarbon (C32H66) and butanol (in heptane) on a powdered coal

The surface reactivity of powdered coal depends on the thermal treatment during its preparation. The characterization of the surface is done through the desorption of solvents with different structures. For such an investigation, a special flow cell (see application sheet TN262) is used. N-heptane is the carrier liquid, and butanol and C32H66 (both dissolved in n-heptane) are to be absorbed on the powdered coal, which has been heated under inert atmosphere at 260°C.

AN261 - Wetting and gelation : Potato starch in water

Starch is a vegetal polysaccharide from different origins (potato, maize,..). It is industrially used in many foodstuffs, especially in fast cooking products. When mixed with water at low temperature, wetting of starch occurs. When heated in water, a gel is formed. The temperature of gelation depends on the origin of starch. The mixing vessel with membrane is used to investigate the wetting and gelation of starch in water.

AN259 - Organic reaction : Formol + Butanal in Soda

The reaction between two organic liquids most often liberates a large amount of heat. In an industrial reactor, when the reaction takes place, large volumes of each component are involved. It is important to know what will be the heat evolved and the rate of reaction, in order to drive correctly the reactor. The calorimeter is well adapted for this type of simulation. As many reactions occur in alkaline medium, the mixing vessel with metallic membrane is indicated for these experiments, like the reaction between formol and butanal in soda.

AN257 - Hydration : calcium sulfates (plaster and anhydrite III) in water

Four forms of calcium sulfate are known : dihydrate : CaSO4, 2H20 (gypsum), hemihydrate : CaSO4, ½ H20 (plaster) and two anhydrites CaSO4 : natural and insoluble anhydrite and soluble anhydrite III (obtained by heating plaster up to 200°C). Plaster and anhydrite III, which are soluble in water, are used in the building industry, because of their setting properties. The reversal mixing vessel is particularly well adapted for the investigation of plaster setting. Water and plaster are initially separated in the vessel, then mixed.

AN256 - Dissolution : Potassium Chloride KCl in water

The dissolution test is a standard one for the mixing calorimetry. It is a way to check the calibration of the calorimeter. The dissolution of potassium chloride in water is used as a reference test. With the C80 calorimeter, the best results are obtained with the reversal mixing vessel.

AN255 - Neutralization : Edible oils by soda

Raw edible oils contain a certain amount of free fatty acids, which have to be neutralized before their use. In industrial plants, an excess of soda is added to neutralize the free acidity. The problem is the adjustment of the amount of soda to be added, knowing the oil acidity. The simulation of the operation is made in a calorimeter on different edible oils, using the reversal mixing vessel.

AN254 - Polymorphism detection : Active drugs (forms 1 and 2) in soda

The determination of drug polymorphism is an important problem for the pharmaceutical research. Depending on the polymorphic form present in a drug, its characteristics can be very different. The detection of the polymorphic forms is not easy. DSC has been used with some success, but cannot be used for all products (thermal stability limitation). As the polymorphic forms have different behaviors especially dissolution properties, the calorimetric test of dissolution is used to investigate their differentiation.

AN253 - Binding : carrageenan in mineral salts solutions

Carrageenan is a polysaccharide, largely used in the food industry especially for its gelation properties. In solution, the polysaccharide exhibits ion selectivity. A specific site binding is observed with certain ions in preference to others. The calorimetric test is used to measure the heat of binding of iota carrageenan with different ions from mineral salts.

AN251 - Dehydration : hydrated salts Ba(OH)2 - 8H2O and AlCl3 - 6H2O

The heats involved during dehydration processes of some mineral compounds can be used for energy storage as the heat of vaporization of water has a high value (? 42 kJ.mol-1). Hydrated salts are especially interesting for such applications. Calorimetry is the ideal method for testing the capacity of energy storage and for determining the range of temperature in which the transformation occurs. The gas circulation normal pressure vessel is used for such an investigation. Water vapor during dehydration is evacuated through the tube.

AN249 - Vapor adsorption : Benzene on a zeolite

Many solid porous compounds, especially zeolites, are well known for their adsorbing properties. In order to measure their adsorption capacity, a special experimental set-up has been designed for the C80 calorimeter. This device allows the characterization of the adsorption of vapor on a solid under reduced pressures. The liquid to be absorbed is initially frozen then kept at a well-defined temperature, determining a well-known vapor pressure. This vapor is absorbed on the solid, previously regenerated under vacuum. The solid is contained in a vacuum high-pressure vessel. An example of the use of such a device is given by the adsorption of benzene vapor on a zeolite.

AN248 - Decomposition under pressure : Coffee in argon (20 bars)

The knowledge of thermal stability of products to be transformed under heating is of the first importance. This is often the case in food industry where raw products are heated in reactors, e.g. coffee when roasted. It appears that during the roasting operation, large quantities of heat are liberated. In order to determine the risk of thermal hazard or spontaneous ignition of the product, a simulation is operated by calorimetry, using the vacuum high pressure vessel. This vessel enables a pressure of inert gas (20 bars) to be applied during the reaction, in order to simulate the real industrial conditions.

AN246 - Solubility : potassium and sodium chlorides in water

The standard high-pressure vessel is well adapted for the heating of solutions above 100°C. An interesting application is the detection of the limit of solubility of salt mixtures. The corresponding temperature is detected when the calorimetric signal changes abruptly, showing the end of the thermal effect of dissolution. In the example a mixture of potassium and sodium chlorides in water is investigated at different ratios.

AN245 - Decomposition of sodium borohydride NaBH4

In chemical industries, the determination of the thermal hazards or decomposition risk for organic products is one of the most important experimentation to be run before any transformation or storage of the products. The thermal methods give an interesting mean of experimentation and simulation for such a determination. The organic sample set in a closed standard high pressure vessel is heated quickly at a fixed temperature and the thermal behavior of the sample is observed by recording the calorimeter signal.

AN244 - Solid-solid reaction : Hydrated baryta + potassium nitrate

The storage of chemical heat consists in using the reversible endothermic and exothermic reactions of a chemical equilibrium. This is the case of the reaction between two solids materials : hydrated baryta and potassium nitrate : Ba(OH)2 - 8H20 + 2KNO3 <--> Ba(NO3)2 + 2KOH + 8H20. The calorimetric standard vessel enables the investigation of a large amount of mixture at low heating or cooling rates. In order to have a better homogeneity of the solid mixture during the reaction, the reversing mechanism of the calorimeter can be used to shake the mixture.

AN243 - Gelatinization of different starches in water by MicroDSC

Starch is a base product in foodstuffs, especially for rapid cooking. When the grains of starch are in the same time in presence of water and heated an effect of gelation occurs, for a well-defined temperature. This temperature depends on the origin of the starch.

AN240 - Heat capacity : coal

The heat capacity determination by the calorimetric method is well known and very easy to run. The sample is heated in the calorimeter, and the heat flow detected by the heatflux transducer is directly proportional to its heat capacity. In practice, two successive tests are necessary : one test with empty vessels on both sides (measure and reference), and a second test with the sample in the "measure" vessel, the "reference" vessel remaining empty. The experimental conditions must be strictly identical for both experimentation. The heat flow deviation between the two curves characterizes the variation of the sample heat capacity versus temperature.

AN239 - Transitions : Ammonium Nitrate

The temperature range of the C80 calorimeter is large enough to investigate some phase changes or transitions in materials. The experimentations are run on large amounts of sample, with low heating rates. That gives precise quantitative measures, and solves also the problem of sampling for some inhomogeneous materials. Using a standard vessel, a sample of ammonium nitrate is heated at 0.2K.min-1 for detecting different characteristic transitions.

AN238 - Melting : hydrated ferric chloride FeCl3 - 6 H20

The latent heat is the energy evolved by a material when it undergoes to a structure change. The effective storage of this heat requires the use of materials with large melting heat, which can be recovered during solidification. For latent heat storage below 130°C, hydrated salts are frequently used. Mostly they are tightly encapsulated in order to prevent evaporation or contamination of the material. A glass ampoule containing a large amount of FeCl3 - 6H2O is placed in a standard vessel, and the melting of the hydrated salt is easily investigated.

AN236 - Adsorption of CO2 on a molecular sieve

CO2 Catalyst catalysis barbon dioxide

AN234 - Determination of adsorbed and structure water in a catalyst

Thermogravimetry is frequently used in characterizing the natural or synthetic types of catalysts and zeolites, and especially in distinguishing the loss of adsorbed and structural (hydroxyl) water. For their use as adsorbents or catalysts, it is also important to know how the dehydration process occurs. An example of determination of adsorbed and structural water in a catalyst is shown hereunder.

AN233 - Adsorption of benzene on a zeolite

Isothermal calorimetry is well adapted to measure the adsorption capacity of zeolite for different compounds. The incremental vapor pressure method is used in the following example, showing the adsorption of benzene on a zeolite. The experimental adsorption device, described on application note TN231, allows running such an investigation.

AN232 - Adsorption of water vapor on a zeolite

Zeolites are hydrated silicates of aluminum, and either sodium or calcium or both, of the general formula Na2O-AI2O3-nSiO2.xH2O. They are well known for their adsorption and catalyst properties, used more and more for industrial applications. An example of adsorption of water vapor on a zeolite is given to show the possibilities of the experimental set-up described on application note TN231. The amount of adsorbed water depends on the type of zeolite, the temperature and the pressure of water vapor. The calorimetric test is very useful to measure the adsorption capacity of a zeolite and to compare the efficiency of different zeolites.

AN230 - Adsorption of oxygen on nickel oxide

The CALVET microcalorimeters are particularly well adapted for the determination of differential heats of adsorption of reactive gas on solid catalysts (see P.C. GRAVELLE, Catal.Rev.Sci,1977, 16(1), 37-110). A well-known volume of reactive gas is injected on the catalyst. The adsorbed volume is evaluated and the heat of adsorption measured. Then the curve of variation of the heat of adsorption versus the degree of surface coverage can be drawn.

AN229 - Adsorption of carbon monoxide on palladium catalyst

The platinum catalyst, described on the application note AN227, has relatively large amount of platinum. In order to give a limit of detection to the DSC-GC combination device, an experimentation has been run on a catalyst containing only 0.2 % Palladium (support : alumina), for the adsorption of carbon monoxide (10% in helium). The effect of metal dispersion on the support is also investigated for a catalyst containing 0.75% Palladium. Helium is used as a carrier gas. Catalysts have been initially preheated under H2 at 250°C, then desorbed under helium.

AN228 - Temperature programmed desorption of a platinum catalyst

After adsorption of a gas on a catalyst, it is interesting to know what type of adsorbed species have been formed. One mode of investigation is to desorb the catalyst by heating and record the desorption thermogram : that is the temperature programmed desorption. On the thermogram, peaks will appear corresponding to the different species formed during the gas adsorption. An example is given by the desorption of a platinum catalyst after hydrogen adsorption (see application note AN227).

AN227 - Adsorption of hydrogen on a platinum (6,3 %) catalyst

The use of the DSC-GC combination (see application note AN226) is illustrated by the investigation of hydrogen adsorption on a platinum catalyst, called Eurocat. The catalyst contains 6.26% platinum deposited on silica. Hydrogen is diluted to 5.4% in argon, and injected on the sample through an injection loop (0.5 ml), in the carrier gas (argon). Before adsorption investigation, the catalyst is initially pretreated in the DSC by heating under hydrogen up to 450°C, and held at this temperature during 2 hours. Then, the surface of catalyst is completely desorbed under a flow of argon, before cooling at the temperature of investigation.

AN226 - Gas adsorption and gas analysis (gas chromatography, mass spectrometry)

The combination of thermal analysis with evolved gas analysis is frequently used in order to characterize the exhausted gases of a reaction. Such a connection requires a continuous circulation of gas through the instrument, with an easy fitting of the EGA apparatus. The open structure of the Calvet DSC111 is particularly interesting for such a combination. The quantitative measurement of both heat evolved by a sample and the amount of gas emitted is made possible, giving a great interest for the better comprehension of the reactions occurring during the experiment. This is particularly powerful for gas-solid interactions, like adsorption in the catalysis field. Two types of combination are described : DSC-gas chromatography and DSC-mass spectrometry using the silica reactor (see application note TN225).

AN224 - Oxygen interaction with coal before combustion

The thermogram of coal combustion (application note AN214) shows two steps in the oxidation reaction. The first peak has been often associated with the combustion of volatiles. But when a coal is maintained under oxygen at 110°C in a thermobalance, a mass increase is detected, corresponding to an oxygen adsorption on coal. The result of this interaction is the modification of coal structure and the formation of complex compounds. The first peak detected by DSC seems to be associated to this coal transformation before the burning of fixed carbon.

AN223 - Proximate analysis of a coal

The proximate analysis, as described in application sheet AN222, allows classifying a coal and gives information for its industrial use. Coal is particularly classified according to its volatiles content : anthracite (8 to 18 %), semi-bituminous (18 to 26 %), bituminous (26 to 40 %), semi-bituminous (40 to 50 %). The thermogravimetric test allows giving a rapid result for a coal. All the operations heating and gas switching are automatically achieved by the controller associated with the thermoanalyzer.

AN222 - Proximate analysis of anthracite

Anthracite is a higher species of coal, which contains a low content of volatiles. A rapid characterization of anthracite is obtained by the proximate analysis. This industrial determination gives the contents of moisture, volatiles, fixed carbon and ash in the sample. The proximate analysis is easily achieved by thermogravimetry according to the following scheme : - Heating to 110°C and isothermal level during 5 minutes => moisture - Rapid heating to 950°C under inert gas and isothermal level during 10 minutes => volatiles - Switch from inert gas to oxygen at 950°C => fixed carbon - Test residue => ash

AN221 - Melting of coals ashes

Melting of ashes is of a high importance in the use of coal. According to the conditions of use, it can be interesting or forbidden. Melting of ashes depends on their chemical composition, and also the type of atmosphere in which melting occurs. A coal has rather fusible ashes when the melting point is about 1300°C. If melting does not occur below 1500°C, ashes are said refractory. Setsys DTA is used to characterize the melting of two ashes.

AN219 - Adsorption and desorption of an hydrocarbon (C32H66) and butanol (in n-heptane) on a powdered coal

The surface reactivity of powdered coal depends on the thermal treatment for its preparation. The characterization of the surface is done through the adsorption of solvents with different structures. For such an investigation, a special flow cell (see application note TN220) is used. n-heptane is the carrier liquid, and butanol and C32H66 (both dissolved in n-heptane) are to be adsorbed on the powdered coal, which has been heated under inert atmosphere at 260°C.

AN218 - Heat capacity of powdered coke

If the calorific value of coal is of first importance, the value of the enthalpy is also necessary to establish the heat balance of the system under study. By the isothermal drop method, the total heat necessary for heating the sample from a temperature T1 (generally ambient temperature) up to higher temperature T2, is measured. The method is used for measuring the enthalpy of a powdered coke (30-40 mesh) at different temperatures.

AN217 - Oxidation of bituminous shales with various oil contents

The interest of bituminous shales is growing, due to its organic part. But the cost of oil extraction from shale is a limitation. Some investigations are done in order to use the oil shale without treatment, as a fuel, like in cement industry. In this case, it is necessary to determine the range of temperature in which combustion of the organic part occurs, and also the heat evolved during combustion. The calorimetric test is well adapted to give those two experimental values. The CALVET HT1000 calorimeter is used for investigation of large samples at low scanning rates. Two bituminous shales with different oil contents are investigated.

AN216 - Comparison of bituminous and coal shales oxidation

The oil of bituminous shale, as described on application note AN217, burns in three different steps between 100°C and 500°C. Coal shale is often used as a fuel in cement industry. The same mass of sample is heated under oxygen in the CALVET HT1000 calorimeter. Oxygen is introduced in the crucible by means of a small tube plunging in the sample.

AN215 - Pyrolysis of a coal

According to the temperature of the test, different types of products are obtained during the pyrolysis of coal : gases, chars, condensable products (water, ammonia), benzols and coke as final product above 1000°C. The production of gases (hydrogen, methane, ethylene,..) begins at about 350°C. After this distillation, an intermediary coke is obtained at about 600°C. The formation of this compound and the production of gases is investigated by DSC, in an inert atmosphere.

AN214 - Combustion of coal

In the case of coal products, the calorific value is usually determined with bomb calorimeters. This type of method is accurate, but does not yield information on the combustion reaction. Differential Scanning Calorimetry allows another approach of the combustion investigation. The heat of combustion is measured, referring to a standard coal with a well known heat content (in this case coal 7 DE from DSM Holland).

AN213 - Combustion of coke with different sample masses

Coke is especially used in steel industry and in metallurgy. Its calorific content varies from 6500 to 7500 cal.g-1, and the combustion gives very few ashes. The combustion of coke can be investigated by DSC. But, as the sample masses are generally little, it is necessary to know what is the influence of the mass on the determination of the heat of combustion.

AN212 - Combustion of carboneous products

Coal is particularly characterized by its calorific value which essentially depends on its carbon and volatile contents. The combustion of coal occurs on a wide range of temperature (from 200°C up to 600°C). Coke, which is a high carbon content product, burns at higher temperature, with only a step of combustion. Carbon graphite is an ideal case of combustion, the reaction yielding only water and carbon dioxide.

AN208 - Thermal stability study by SENSYS DSC : influence of pressure on the thermal stability of azodicarbonamide

Azodicarbonamide formula is NH2 - CO - N = N - CO - NH2. The compound belongs to the family of azo dyes. Azodicarbonamide decomposes at about 200°C. But the decomposition phenomena largely depends on the pressure above the sample. Different tests are run in an open crucible, a sealed crucible and a controlled high pressure crucible, in order to show that the pressure on the sample has a great influence on the decomposition rate.

AN207 - Decomposition of nitrophenol : influence of internal pressure and cell volume

Ortho-nitrophenol is a hazardous solid used as an intermediate in organic synthesis. The thermal stability of the compound is investigated in different crucibles, with variable internal pressures. According to this pressure, the decomposition phenomena is very different.

AN206 - Decomposition of diethylenglycol -Na diluted in diethylenglycol

Diethylenglycol is largely used in organic chemistry due to its excellent solvent properties. The sodium derivative of diethylenglycol is an intermediate for organic synthesis. Diluted in diethylenglycol, diethylenglycol-Na has a relatively good thermal stability up to 250°C. Decomposition of DEG-Na at different concentrations in DEG is investigated in sealed crucibles. The pressure developped during decomposition is about 50 bars or more.

AN205 - Decomposition of a peroxide in solution in cyclohexane

Peroxides are known as very unstable materials : concentrated material may react explosively with combustible materials. The knowledge of the thermal stability of such a product must be well known before its use in organic reactions, or also storage. A sample of peroxide in solution in cyclohexane is investigated in a sealed crucible.

AN204 - Decomposition of azobisisobutyronitrile (ABIBN) in solution in di-N-butylphtalate

Investigation of azobisisobutyronitrile (ABIBN) in solution in di-N-butylphtalate is used as a reference test for the determination of kinetics parameters by the FREEMAN-CAROLL method. A single test is only needed to determine reaction order, reaction rate and activation energy.

AN203 - Decomposition of polyacrylonitrile

Polyacrylonitrile (CH2 - CH -)n is mainly transformed in synthetic fibers or l used for elaboration of different copolymers. CN Polyacrylonitrile is thermally stable for medium temperatures. Above 250°C, it undergoes a very strong decomposition. The kinetics parameters of the reaction are determined according to the FREEMAN-CAROLL method.

AN202 - Decomposition of paranitroacetanilide

Paranitroacetanilide (NO2 - C6H4- NH - CO - CH3) is obtained by nitration of acetanilide, in concentrated sulfuric acid solution. Hydrolysis of paranitroacetanilide is thermally stable up to 270°C. The kinetics parameters of the decomposition are determined according to the FREEMAN-CAROLL method.

AN201 - Decomposition of nitrocumene

Nitrocumene (NO2- C6H4 - CH - (CH3)2) is an organic liquid used in synthesis. This liquid is thermally stable at medium temperatures and begins to decompose at about 250°C. The kinetics parameters of the decomposition are determined according to the FREEMAN-CAROLL method.

AN200 - Decomposition of 2,4 - dinitrotoluene at various scanning rates

2,4-dinitrotoluene (CH3 - C6H3 - (NO2)2), obtained by nitration of toluene, is an intermediate for organic synthesis and especially used in mixtures of explosives. 2,4-dinitrotoluene has a dangerous fire hazard. The decomposition of this material is investigated at different scanning rates, and the kinetics parameters are determined according to OZAWA and KISSINGER methods.

AN199 - Comparison of the thermal stabilities of nitrocellulose, nitrocumene and nitrobenzene

Decomposition of various nitroorganic compounds is investigated in order to show the possibilities of the sealed high pressure crucible at different temperatures. The sealed crucible is well adapted for violent decomposition (nitrocellulose), decomposition at medium temperature (nitrocumene) or decomposition at high temperature (nitrobenzene).

AN198 - Hydration of cement (C3S) at different temperatures

The setting time of a cement has to be well known in order to determine its industrial applications Tricalcic silicate (C3S) is the active component of cements, giving a high resistance which obtained rapidly. A thermal investigation of C3S hydration by means of calorimetry allows us to determine the setting time and the kinetics of hydration, and also the influence of temperature on the parameters.

AN197 - Hydration of plaster at different temperatures

The influence of temperature on the hydration of plaster is well known to plasterers in view of the differences they observe between the behaviour of their material in winter and summer. Also it appears that, above a well defined temperature, the water-plaster mixture gives a paste which does not set for several hours. The calorimeter C80 is used for studying the influence of temperature on plaster setting.

AN196 - Hydration of two calcium sulfates (plasters and anhydrite III)

Four forms of calcium sulfate are known : dihydrate CaSO4, 2H2O (gypsum), hemihydrate CaSO4, ½ H2O (plaster) and two anhydrites CaSO4 : natural and insoluble anhydrite and soluble anhydrite III (obtained by heating plaster to 200°C) . Plaster and anhydrite III, which are soluble in water , are used in the building industry, because of their setting properties. Calorimetry is an interesting method for studying the setting of calcium sulfates.

AN195 - Heat content of crude Portland cement

The problem of power consumption is becoming increasingly important in many industries, particularly those which use high temperature furnaces. So it is important to be able to establish total or partial heat balances for any given system. The 1500°C calorimeter allows us to measure the heat which must be supplied to a system, for example to run clinkerisation of crude Portland cement. The sample, thermostated at ambient temperature, is dropped into the calorimeter which has been stabilized at 1430°C.

AN194 - Heating of crude in a (CO2 + H2O + N2) atmosphere

Crude cement is industrially heated in rotary kilns where the atmosphere is a gaseous mixture of carbon dioxide, water vapour and nitrogen. In order to simulate the heating of the cement in the kiln, the measurement is carried out in the high temperature Calvet calorimeter in the presence of a gaseous mixture containing 25% CO2 , 10% H2O vapour and 65% N2 (see calorimetric device below).

AN193 - Baking of crude Portland cement

After preparation of the raw materials (lime, clay, marl,..) in proportions dependent on the process selected, paste, powder or granules are introduced into the rotary kiln so that the mixture may be gradually heated to the clinkerisation temperature, that is to say to the temperature at which partial melting occurs, about 1450°C. Differential thermal analysis is used to simulate the conditions existing during cement manufacture and to characterize the phyzical and chemical processes which occur in the cement when it is heated to 1500°C.

AN192 - Dehydration of calcium sulfate CaSO4, 2H2O (gypsum)

Gypsum is used to prepare plaster products. Small amounts of gypsum are also contained in cements. Because of the characteristic nature of the gypsum peaks, the dehydration studies can be employed for the quantitative and qualitative determination of the components in any mixtures (dihydrate, hemihydrate). Dehydration of gypsum occurs in two stages : CaSO4, 2 H2O --> CaSO4, ½ H2O (plaster) --> CaSO4 (anhydrite)

AN191 - Heat capacity of crude cement and clinker

Heat capacity is a very important thermodynamic parameter, when determining the heat balance of a reaction. The specific heats of the different components, before and after the reaction, have to be known in order to define the correct heating of the system. The heat capacity of crude cement and clinker is measured according to the stepwise method. An increment of temperature is scanned, and the calorimetric peak, corresponding to the sample heated is integrated, as shown below.

AN190 - Thermal analysis of mineral salts used in the cement industry

Cement is obtained from the baking of mixture of clays and limestones in which silica is one of the main components. Mineral salts are numerous in the initial compound, and sometimes traces of nitrates. A controlled amount of gypsum can be added to the manufactured cement in order to retard its setting rate. The thermal behaviour of the three different salts (silica, nitrate, gypsum) is investigated by DSC .

AN187 - Isothermal stability of polybutadiene

Elastomers are often employed in severe conditions of use, particularly of temperature (joints, pipes, ..). Optimal conditions of use must be well defined in order to know when to make replacement. Isothermal thermogravimetry gives information on the resistance of elastomer to a given temperature and determines its decomposition kinetics. The investigation is run on cis-polybutadiene.

AN186 - Thermal stability of elastomer joints

Many elastomer are used in the manufacture of joints, due to their elastic properties, their good resistance to heat, oils, solvents.. Three different elastomer are investigated by thermogravimetry in order to compare their resistance to temperature : nitrile elastomer (Perbunan), fluorined elastomer (Viton) and silicon elastomer.

AN185 - Thermal Stability of various elastomers

Uses of natural rubber are numerous and well known (tires, pipes, shoes, ..). In some cases, synthetic rubbers are prefered due to their specific properties and their lower cost importance. Thermogravimetry allows to compare their resistance to temperature. The investigation is run on the following elastomers : natural rubber, butyl rubber, cis-polybutadien, polychloropren (Neoprene).

AN184 - Polymerization of polyurethan (polyol + polyisocyanate)

Reticulated polyurethan is obtained through the reaction of a glycol and a diisocyanate, according to the following reaction : X (O = C = N - R - N = C = O) + x (OH - R ' - OH) - --> X (O - C = NH .. R - HN - C = O) Il l O OR' The reaction is calorimetrically followed by using the mixing cell with a metallic menbrane (see description in C80 chapter).

AN183 - Heat capacity of elastomers

Elastomers show an important variation of their heat capacity near the glass transition. The knowledge of the heat capacity before and after transition is of a great utility for the uses and applications of the compounds. In DSC methods, heat capacity (Cp) is proportional to thermal power evolved when the sample is heated. Two runs are necessary in order to determine precisely Cp : the first one with empty cells (sample and reference), the second one using the same cells, with the sample. The difference between the two curves characterizes the heat capacity of the sample.

AN182 - Vulcanization of fine powdered rubber

Presents the vulcanization of rubber

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AN181 - Styrene - butadiene (7%) polymerization

The control of polymerization assumes the knowledge of the reaction rates. It is essential to know the quantities of heat which must be removed by the cooling systems to obtain maximum productivity. The isothermal calorimetric test gives the curve for the conversion of monomer into polymer versus time. Its analysis determines the kinetics of polymerization necessary for the previous previsions. An example is given for the polymerization of a mixture of styren and butadien (7%) at different temperatures (130,140,150°C).

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AN180 - Glass transition of various synthetic elastomers

Elastomers are frequently used for applications at low temperatures. Their point of brittleness or glass transition must be determined with precision in order to define the minimal temperature of use. The glass transition of an elastomer can be characterized by a variation of heat capacity, which makes thermal analysis a very useful method for detecting this phenomenon.

AN179 - H2O2 + FeCl3

Presents the determination of the heat of decomposition of H2O2 in presence of FeCl3

AN178 - Heat of reaction NaOH + HCl

Shows the neutralization of HCl solution by a NaOH solution

AN177 - Dissolution of KCl in water

Shows the dissolution of KCl in water

AN176 - Dissolution of NaCl in water

Shows the dissolution of NaCl in water

AN175 - Determination of the heat of reaction

Shows the determination of heat of reaction by DRC

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AN174 - Determination of Qdos

Shows the determination of Qdos by DRC

AN173 - Cp determination of product

Shows the determination of Cp by DRC

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AN172 - Calibration by Joule effect

Shows the calibration of DRC

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AN171 - Data processing

Shows the possibilities of DRC

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AN151 - Adsorption of n-butylamine on a zeolite

Shows the titration curve of a suspension of zeolite by a solution of n-butylamine

AN148 - Phase transitions and melting of iron

Shows the heating curve of iron : different phase transitions ansd melting are observed

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AN146 - Analysis of an emulsion of water in gas-oil

Presents the curve of melting and cristallization of water which is in a gas-oil water emulsion

AN145 - Crystallisation of paraffin in gas-oil

Presents the cristallization of paraffin which is in solution in gas-oil

AN144 - Determination of cristallinity of PET by DSC

PolyEthylene Terephtalate (PET) is a polyester widely employed in daily life (e.g. in water bottles, textile fibers, credit cards). The crystallinity is a very important characteristic because it is directly related to the properties of the polymer (e.g. toughness, clarity, stability). It is defined as the ratio between the crystalline and amorphous phases in the polymer. DSC is one of the main analytical techniques to determine the crystallinity ratio in a semicristalline polymer.

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AN143 - Oxidation Induction Time (OIT) of polyethylene by DSC

Oxidation induction time (OIT) is defined as the time that takes oxidation of a sample to occur under oxygen at a given temperature. Applied to polymers, this measurement enables the evaluation of its oxidative stability. As an example, the process of aging of water pipes submitted to chlorinated water could be forecasted by performing OIT analysis. The OIT measurement is defined in the ISO11357-6 standard.

AN142 - Tg of a solution prior to its freeze-drying

Freeze-drying of a solution consists in first cristallyzing it totally, then sublimating the formed ice on installing vacuum. In order to obtain a final product of good quality, it is necessary to install vacuum at a temperature lower than the glass temperature (Tg) of the frozen solution.

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AN139 - Self discharge of batteries

Presents the measurement of the energy dissipated during storage of a battery

AN138 - Formation of hydrocarbide gas hydrates

Presents the formation of hydrate of hydrocarbide on operating with BT215 at high pressure

AN135 - Analysis of kaolinite

Presents the different transformations during heating of kaolinite

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AN134 - Decomposition of calcium oxalate

Presents the decomposition of calcium oxalate

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AN133 - Proximate analysis of a coal

Presents the proximate analysis of a coal

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AN132 - Decomposition of a NBR rubber

Presents the decomposition of NBR rubber by thermogravimetry : enables to determine the content in oil+wax, elastomer, carbon black and ash

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AN119 - Phase diagram of Pb-Sn system

Explains how to determine a phase diagram from a melting curve of an alloy

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AN118 - Melting of Pb-Sn alloy

Presents the melting curve of a Pb-Sn alloy

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AN115 - Decomposition of DTBP (Di-Tert-Butyl Peroxide) + kinetic parameters

Presents the decomposition of ditertbutyl peroxide

AN114 - Degree of stalling of a bread

Presents the heating curve of a stalled bread

AN113 - Isothermal retrogradation of wheat flour at 4°C

Presents the retrogradation of a wheat flour suspension after gelatinization

AN112 - Gelatinization of wheat flour

Presents the gelatinization of a wheat flour suspension

AN111 - Crystallization of palm oil

Presents the cristallization of palm oil at avery low cooling rate (8 K/h)

AN110 - Denaturation and aggregation of ?-amylase

Presents the curve of denaturation + aggregation of a solution of amylase

AN109 - Denaturation of a lysozyme solution at 0,127%

Presents the curve of denaturation of a solution of lysozyme

AN108 - Thermal stability of interleukin-2

Presents the curve of denaturation + aggregation of a solution of interleukin

AN107 - Pore size distribution in polymer resins

Presents an example of determination of pore size distribution of a resin

AN104 - Thermophysical properties of the composite ceramic-salt system (SiO2/Na2SO4)

A composite ceramic-salt packed bed configuration is being developed for high-temperature thermal storage. The thermophysical properties of the more particular hybrid system SiO2/ Na2SO4 have been investigated in the range from room temperature above the melting point of the salt, 884°C. The Na 2SO4 fraction in the composite materials was varied between 20 and 50 %. The following properties were measured: specific enthalpy, coefficient of thermal expansion and thermal diffusivity.

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AN103 - Thermochemistry and structure of the liquid Na2O-GeO2 system

The main objective of the present investigation is the completion of the thermochemical data base for the Na2O- GeO2 system as well as the provision of systematic experimental data on the thermochemical behavior of oxide liquids.

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AN102 - Enthalpies of fusion and heat capacities for ice and tetrahydrofuran hydrate in the range 85 to 270 K

Clathrate hydrates are non-stoichiometric solid compounds in which individual " guest " atoms or molecules of suitable size and shape are held in the cavities provided by the hydrogen-bonded lattice of the " host " water molecules. Recent reports that large reserves of natural gas are present as clathrate hydrates in permafrost regions and beneath the oceans have generated interest in the study of their thermophysical properties such as heat capacity and thermal conductivity. An understanding of such properties will be required regardless of the production scheme used to recover natural gas from these deposits.

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AN101 - Heat of solubility of n-paraffines in supercritical CO2

Presents the set-up to determine the heat of solubility of n-paraffines by supercritical CO2

AN100 - Precise determination of low level sucrose amorphism by microcalorimetry

Amorphous sucrose is generally obtained by freeze-drying or by spray drying of sucrose solution. Due to an important mechanical friction and to quick cooling, a thin amorphous layer could be formed at the surface of the sucrose particles. By calorimetry method, it has been possible to evaluate low level amorphism of solid sucrose.

AN099 - Dehydration of CaSO4.2H2O with controlled DTG

Presents the decomposition of calcium sulfate at constant heating rate and constant DTG

AN098 - Dehydration of CuSO4.5H2O with controlled DTG

Presents the decomposition of copper sulfate at constant heating rate and constant DTG

AN097 - Decomposition of calcium oxalate with controlled DTG

Presents the decomposition of calcium oxalate at constant heating rate and constant DTG

AN093 - Zircona under water vapour up to 1700°C

Presents the reduction of zirconia when heated under wet helium at different levels of humidity

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AN090 - Calorimetric study of the acidity of Y-zeolites treated with silicon tetrachloride

The acidity of synthetic HY samples dealuminated with silicon tetrachloride vapour at various temperatures is investigated using microcalorimetry. The work covers sample preparation, characterization, and acidic properties. The differential heats of ammonia adsorption versus coverage and the acidity spectra are described. The catalytic performance is measured in the hydrogen transfer reaction.

AN089 - Heat of mixing of polymer alloys by heat of solution method

Direct measurement of the heat of mixing (interaction) of polymers is not feasible due to their high viscosity. The indirect approach described here is a heat of solution method, in which a Hess's Law cycle is used to determine the heat of mixing from the individual heats of solution of the alloy and its constituent polymers in a common solvent.

AN086 - Application of thermal analysis to the cement industry

Presents the method to determine the heta exchange during the clinkering reaction by drop method

AN085 - Mixed gels formed with konjac mannan and xanthan gum

Presents the curves of melting and gelification obtained on mixed konjac mannan and xanthan gum

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AN083 - Effect of KCl and NaCl on a thermal properties of gellan gum gels

Presents the influence of KCl or NaCl salts on the thermal properties of gellan gum gels

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AN082 - DSC study of melting and glass transition in gelatins

Heat capacity of crystalline and amorphous gelatins at different concentration have been here studied in a wide range of temperature

AN080 - Thermodynamic properties of strontium and barium feldspars

The molar heat capacities of two synthetic Sr and Ba compounds were measured by differential scanning calorimetry between 312 and 712 K. In addition, heat capacities were calculated from a model of the vibrational spectra using optical frequencies measured by IR spectroscopy.

AN079 - Heat production of frogs under normoxic and hypoxic conditions : a microcalorimetric study using a gas flow system

heat production of male frogs was measured in a microcalorimeter through which continuous flow of gas was passed in order to generate constant normoxic, hypoxic or anoxic conditions.

AN078 - Starch gelatinization in pasta cooking : differential flux calorimetry investigations

pasta cooking conditions were simulated in a differential flux calorimeter. The profile of the endothermic starch gelatinization peak was observed to directly describe the process according the first-order kinetics. Isothermal calorimetry provide much more reliable results than do other traditional approaches allowing here assessment of the gelatinization kinetics and simple thermodynamic treatment.

AN076 - Processing of yoghurt

Presents the growth of the batcteruia contained in yoghurt when more milk is provided

AN075 - Melting of steel

Presents the melting curve of steel

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AN074 - Thermal expansion of zirconia

Presents the expansion of cast iron : a sudden shrinkage is observed during a transition

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AN073 - Thermal expansion of cast iron

Presents the expansion of zirconia in the heating ans cooling modes : a rapid length variation is observed during the phase transitions

AN072 - Dissolution of Fe in Al at 1200°C

Presents the determination of the heat of dissolution of iron in aluminium on using the drop method

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AN071 - Crystallization of a lysozyme solution (13,4%) at 40°C

Presents the isothermal crystallization of a solution of lysozyme (13,4%)

AN070 - Decomposition of tyre

Presents the decomposition of tyre

AN069 - Decomposition of PVC

Presents the decomposition of PVC

AN068 - Transitions of cholesteryl myristate

Presents different transitions obtained in MBBA (liquid crystal)

AN067 - Transitions of M.B.B.A. (Metoxyde Benzymidene ButylAmine)

Presents different transitions obtained in cholesteryl myristate (liquid crystal)

AN066 - Thermal stability of a human growth hormone (hGH)

Presents the denaturation curve of human growth hormone

AN063 - Solid fat index (SFI) of suppository excipient

Presents the melting curve of the fatty fraction of a suppository

AN062 - Melting of suppository excipient

Presents the melting curve + Solid fat index of the fatty fraction of a suppository

AN059 - Glucoamylase - Maltose interaction

Presents the interaction of glucoamylase with a maltose solution

AN057 - Analysis of hydrochloride dihydrate salt

Presents the behaviour of hydrochloride dihydraye salt

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AN056 - Denaturation and unfolding of Ribonuclease A with MicroDSC3

Presents the denaturation of ribonuclease using the MicroDSC3

AN055 - Analysis of benzocaine

Presents the melting curve of benzocaine by DSC

AN053 - Thermal denaturation of a collagen solution with MicroDSC3

Presents the denaturation of several collagen solutions containing different hyaluronic acid concentrations

AN052 - Heat of solution of steroid in methanol

Presents the determination of the heat of dissolution of steroid in methanol

AN051 - Fermentation of yeast dough

Presents the DSC curve obtained when a yest dough grows

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AN049 - Growth of escherichia coli

Presents the DSC curve obtained during the growth of e.coli

AN039 - TMA of a polyester resin

Presents the expansion of a sample of polyester

AN037 - TMA of P.E.T.

Presents the expansion of a sample of PET

AN033 - Denaturation of soy solution

Presents the denaturation curve of egg white solution

AN031 - Denaturation of hen egg white solution

Presents the denaturation curve of soy solution

AN027 - Melting of Cu-Ti intermetallic compound

Presents the melting curve of an intermetallic CuTi

AN026 - Stability of SiC under O2

Presents the behaviour of SiC when hold at 1150°C under O2 during 1150°C

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AN024 - Melting and gelation of iota-kappa carrageenan by MicroDSC

Carrageenans are linear sulfated polysaccharides extracted from Red Algae and used in food processing for their gelation properties. Three types of carrageenan exist: iota, kappa and lambda. Gelation is only obtained with the kappa and iota forms. Iota carrageenan produces soft gels whereas the gels obtained with the kappa form are strong. The MicroDSC technique is well adapted to investigate the formation and the melting of such gels

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AN022 - Compatibility drug-excipient

Presents how to evaluate the compatibility between one drud and several excipients in order to select the best one

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AN021 - Gelification / melting of gelatine

Presents the melting / gelification curves observed during heating / cooling

AN020 - Dehydration of gypsum

Dehydration of gypsum presents two endothermic peaks : they make possible the quantification of gypsum and plaster

AN019 - TMA analysis of a polyethylene film

Presents the expansion of a sample of polyethylene : the Tg is determined : Tg is generally hardly determined by DSC but easily by TMA

AN018 - Decomposition of a supercritical NH4ClO4 solution

Presents the decomposition of a solution of ammonium perchlorate

AN016 - Loss of mechanical properties of polycarbonate

Presents the TMA curve of a polycarbonate sample : two shrinkages are observed : one due to TG one to the softening

AN015 - Decomposition of black powder

Presents he decomposition of black powder while heated

AN014 - Sintering of MoSi2

Presents the sintering of MoSi2 while heated

AN013 - Reduction of a steel at 1200°C

Presents the reduction of a plate of steel by hydrogene after previous oxidation

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AN012 - Oxidation of a steel at 500°C

Presents the oxidation of a plate of steel which is studied in the scanning mode under oxiding atmosphere

AN011 - Oxidation of a steel in the scanning mode

Presents the oxidation of a plate of steel which is studied in isotherm (500°C) under oxiding atmosphere

AN009 - Heat capacity of AgPO3

Presents the Cp of AgPO4

AN007 - Tg of polyurethane

Presents the expansion of a sample of polyurethane : the Tg is determined : Tg is generally hardly determined by DSC but easily by TMA

AN005 - Sintering of Al2O3 with control of the shrinking rate

Presents the shrinkage observed during the sintering of alumina powder while heated

AN004 - Long term setting of a mortar

Presents the setting of a mortar on a period of 4 days

AN003 - Expansion of copper

Presents the expansion of a sample of copper : coefficients of expansion are measured

AN002 - Melting of a polyester resin powder

Presents the melting of a polyester when heated : a shrinkage is observed

AN001 - Gelatinization of maize semolina (30%) in water

Presents the gelatinization of a suspension of maize in water by calorimetry

TN680 - MHTC96-Drop calorimetry-principles and applications

The MHTC 96 drop calorimetry is very convenient for the investigation og metals and alloys, for minerals and axodes, for any advanced material.

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TN679 - SETSYS Evolution - Working under corrosive atmospheres - Part 1 - TG mode

Solutions to work under corrosive or fluorine atmospheres

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TN664 - Boiling point measurement by DSC

The boiling point of a pure compound is one of the essential information necessary to know before any industrial implementation. Nevertheless, its determination needs very specific conditions to limit the influence of the atmosphere. Indeed, internal gas convection, vapor pressure in the crucible or kinetic of vaporization are important factors that play an important role in the measurement. To determine precisely the boiling point, those factors have to be optimized. The DSC technique can be used for such a measurement

TN638 - High Pressure Flow Mixing vessel for CO2 capture in amine solutions

The use of chemical sorbents is today one of the most popular absorption technique for the CO2 capture in post combustion processes. Flow mixing calorimetry is the ideal technique for measuring such enthalpies of adsorption. In order to work under pressure, a dedicated high pressure mixing vessel is adapted to be used on the Setaram C80 calorimeter

TN629 - Measurement of small hydrogen sorption quantities by the Sievert's method

With the recent advances in solid state research and the development of new synthesis paths, only small amounts of material are produced. To investigate the sorption properties of these small samples an accurate tool for measurement is required. The PCTPro-2000 can measure sample quantities down to mg's thank to its Microdoser attachment

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TN626 - Hydrogen storage measurements at liquid nitrogen temperature

Use of the PCTPro for measurements at very low temperature

TN625 - Direct Van't Hoff measurement

Kinetic determination using the PCTPro for hydrogen adsorption and desorption

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TN612 - Cp of a material with very low density : cork

Demonstrate the capability of SensysDSC to measure heat capacity even of material having a low density

TN556 - Critical point of water

TG-DSC was used to determine the critical point of water

TN519 - Testing through skins

testing through skins

TN518 - Testing vacuum insulation panels (VIPs)

The Mathis modified transient plane source technique offers the only method available today to test vacuum-sealed materials.

TN394 - Electric calibration of microDSCIII under different power levels

Calibration is essential for a calorimeter : the accurate determination of the calibration factor conditions the quality of the obtained results of energy. In a conventional DSC the heat transfer between the sample and the heat sink passes through the lower part of the crucible. In a Calvet type DSC such as DSC111, DSC121 and microDSC's, this heat transfer is done in all directions. These properties give to Calvet type DSC much better metrological properties such as the linearity of the output of a DSC to power dissipated in its heart.

TN371 - Melting of 0,15 mg of gold

Presents the melting curve of a small mass (0,15 mg) of gold

TN365 - Critical temperature and pressure of hexane

Presents the experiment of determination of critical temperature and pressure of hexane

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TN355 - Determination of thermal expansion coefficient

To assess the thermal expansion coefficient of a sample, the variation in length of this sample, ?L sample, has to be plotted against temperature T. With a non-differential system, the raw expansion curve obtained can be described by the following equation : ?L sample - ?L assembly + drift = f(T) ?L assembly is due to the expansion of the material making up the probe and the sample-holder tube which is not compensated for the length of the sample. The drift term is due to a temperature gradient between the sample-holder and the probe. With an adapted software it is possible to correct the raw data of the two above interfering terms and thus obtain the expansion curve of the sample.

TN353 - Shrinkage of fibers

The thermomechanical behavior of fibers or films can be highlighted by using a special device for traction studies. The sample is maintained between two clamps. The upper clamp is linked to the sample-holder tube whereas the lower clamp exhibits a hole in which the hooklike end of the probe is introduced.

TN341 - Thermomechanical analysis on wide temperature range

The SetsysTMA allows measuring variations in dimension of the sample when this sample is subjected to a temperature program under a non-oscillatory load. Dilatometric measurements under small loads can be carried out with SetsysTMA as well as stress-strain studies under various deformation modes (compression, penetration, traction, flexure) with appropriate probes. Depending on the temperature range, three versions are available.

TN340 - Heat of mixing : NaOH + HCl

On using the circulation mixing vessel it is possible to inject two different liquids continuously. Thus, the titration of an acid by a base is possible. On changing the flow-rates given by the two pumps the ratio HCI / NaOH is modified, but the total flow-rate is kept constant. For this application the micro-DSC must be used with a pair of circulation mixing vessel (S60/112014), the temperature prestabilizer (S60/26626) and two Peristaltic 2-channel pumps (2 times S60/29332)

TN337 - Baseline stability at constant temperature

Some experiments carried out at constant temperature consists of monitoring the calorimeter output over a long time period and measurements of minor thermal variations. To be sure that the measurement is significant it implies that the calorimetric output with an inert sample must be very stable. The curve shown below is the type of curve that could be expected on using the standard equipment without any special devices like main stabilizers, thermostated water circuit or air conditioners : it has been carried out in a normal room but under the following conditions : no heating system, closed shutter, no air stream in the room : the general rule is to avoid any rapid room temperature variation.

TN335 - Stabilisation at a set temperature

Some experiments require monitoring the thermal behavior of a substance at successively different temperatures (see sheet AN334 : Propellant stability). Some instruments available on the market have a water bath of 20-30 liters and for this reason are thermally very inert : after a modification of the set temperature they require about 24 hours to have a stable signal. The curve here under shows the calorimeter response after a set temperature modification.

TN321 - Calibration vessel (31/1527)

Connected to the Joule effect calibration device (S60/1429) this vessel consists of a resistor, which dissipates a constant heat power. The value of the power can be selected on the calibration device. Linked to a microcomputer the procedure of calibration is the automatic : it provides the calibration curve on the whole temperature range.

TN320 - Liquid heat capacity vessel (31/1531)

The accuracy of the measurement of the heat capacity of the liquid by calorimetric method depends on a correction term due to the vapor phase above the liquid. In order to overcome this difficulty, a special calorimetric vessel has been designed. The main feature is a tube welded to the experimental vessel. It is filled through one tube by means of a syringe, until the liquid comes out through a second tube. When the liquids is heated it expands freely in the tubes but the volume of the liquid in the vessel, located in the detection zone of the calorimeter remains constant. The determination of the heat capacity of this corresponding volume is achieved using the step heating mode. Notice : the heat capacity can also be measured by using the sealed vessel (S60/1528). The sample is then in the presence of its vapor pressure : it is suitable for solids but can sometimes also be used for liquids.

TN319 - Circulation mixing vessel (31/1530) : two inlet + one outlet

With this vessel it is possible simultaneously to introduce two liquids. They are injected by two peristaltic 2-channel pumps (S60/29332) or by gravity. The liquids enter first the temperature prestabilizer (S60/26626) through which they flow in a loop. In this zone the temperature of the liquid equilibrates to the temperature of the calorimeter. The two inlet liquids are then forced to be mixed through a mixer. The resulting heat is then monitored by the transducer. The mixture exits through the outlet tubing.

TN318 - Circulation vessel (31/1529) : one inlet + one outlet

With this vessels it is possible to introduce a liquid (or a gas). The liquid enters first the temperature prestabilizer (S60/26626) in which it flows in a loop. In this zone the temperature of the liquid equilibrates to the temperature of the calorimeter. The liquid then enters the lower part of the vessel. The liquid (gas) then exits via the outlet tubing. Generally a peristaltic pump is used (S60/29332).

TN317 - Sealed vessel (31/1528)

This liquid and gas tight vessel is used for any kind of investigation which requires the analysis of a liquid or a solid totally sealed off from the outside environment. For example even minute sample loss through evaporation is avoided. The seal is obtained by the elastomer 0-ring.

TN308 - Temperature calibration : melting of a standard

The DTA rod made of tungsten rhenium can be calibrated by a melting of a standard such as sapphire. At very high temperatures, only sapphire can be used because properties like melting point and enthalpy are well defined. The temperature given by thermocouples can be checked and the DTA signal calibrated.

TN307 - Sensitivity of the detector

The DTA transducer is made of tungsten and tungsten rhenium thermocouples to work up to 2400°C. It is less sensitive than a classical DTA rod made of platinum but small energy changes can be detected. Rhodium is a good example with a small enthalpy of melting of 50 cal/g.

TN306 - Very High Temperature (Up to 2400°C)

The alumina tube used up to 1750°C is removed to work up to 2400°C. The experiment is run directly in the graphite resistor under vacuum or inert gas (except nitrogen). The TGA-DTA probe used is made with a tungsten plate and four wires in W/Re for the measurement of the temperature of the sample and the DTA signal up to 2400°C.

TN305 - TGA - F.T.I.R COUPLING

Coupling a Fourrier Transformed Infrared Spectrometer makes it possible to identify evolved gas during a thermal analysis. All products of decomposition can be detected and compared with reference spectrums, except for metallic or monoatomic compounds. This powerful method has application in many fields ; polymers, inorganic materials, fiber..

TN304 - Evolved gas analysis by mass spectrometry

Thermogravimetry measures the mass loss or gain of the sample and DTA detects the corresponding thermal effects. But, these two methods do not identify the type of reaction or decomposition which measure the mechanism of the transformation. With a mass spectrometer linked to TAG, gases with a molar mass between 1 and 300 g are controlled with a high detection limit.

TN300 - Long term isothermal experiment

Mass loss of organic compounds are sometimes very long because they are enclosed in a mineral. For a long term experiment, it is important to have a good regulation of temperature and a controlled atmosphere, without leaks, in order to protect the sample from air exposure. Analyzed oil-bearing rock contains organic compounds ; evolved compounds should be a function of a temperature level similar to a distillation.

TN296 - Analysis in sealed crucibles

Some compounds have a high vapor pressure or evolved gas which are reactive with platinum or alumina. These materials can be analyzed in sealed crucibles (fig. 1) under vacuum or known atmosphere. The sensitivity of the DTA transducer is more than enough to detect thermal effects. Experiments were run with sulfides which are reactive to platinum at low concentrations.

TN292 - Quantitative analysis

The major advantage of the TGA-DTA rod is analysis on the same sample. Thermogravimetry and thermal analysis can be quantitative thanks to a calibration of this rod. Melting of metals gives a sensitivity of the rod at different temperatures and quantitative analysis can be run. The enthalpy of a thermal effect can be calculated when introducing the calibration of the rod into the computer during a data treatment.

TN291 - TG and DTA signals stability

The TAG provides the investigator with a symmetrical TGA-DTA system which means with two furnaces. Deviation on the thermogravimetric signal is equivalent to 1.5 mg at 1000°C with a monofurnace system. That is only due to the combined resulting form the buoyancy effect which vary with the density of the gas, combined with the driving force produced by flowing gases and other disturbing effects. These perturbations are physically compensated with a second furnace. Moreover, thanks to homogeneity in the furnaces, the DTA signal is stable.

TN272 - Standard, vacuum and gas circulation vessels (normal and high pressure) for the Calvet low temperature calorimeter

The Calvet Low Temperature calorimeter BT 2.15 is especially designed for calorimetric investigations from very low temperature (-196°C) up to medium temperature (200°C). The size of its experimental vessels is identical to the C80 one. In order to have compatible vessels on the C80 and the BT 2.15, identical vessel bodies are used for the standard, vacuum and gas circulation vessels (normal and high pressures). The length of the pipe connecting the vessel to the outside is different.

TN270 - Pressure evaluation during reaction

Many organic materials used in chemical reactions exhibit an hazardous behavior when heated. Their composition may produce a large amount of vapor and increase very highly the pressure in the reactor. So the pressure, especially its evolution during the reaction, has to be well known in order to design correctly the reactor and the safety devices to prevent any risk of explosion and destruction of the reactor. Chemical plants are especially interested in this pressure control during reaction or storage. SETARAM has designed a calorimetric high pressure vessel linked with a pressure gauge in order to evaluate in the same time the pressure evolved during the reaction and to follow the heat dissipated. Both data can be used to calculated the reactor dimensions and to evaluate the risk of decomposition.

TN269 - Mixing with mechanical stirring

In most organic reactions, the stirring of the mixture has to be maintained during the reaction for a good homogeneity of the mixture and for improving the efficiency of the reaction. In industrial reactors, large amounts of chemical products are continuously mixed by means of mechanical stirrers. It can be the reaction of two liquids giving a crystallized solid, or the mixing of a liquid and a solid giving another solid, or also reactions between solids. In all cases, stirring and sometimes strong stirring, is needed. SETARAM has designed a mixing vessel linked with a mechanical stirrer in order to simulate types of reactions and to evaluate what is the heat evolved during mixing and reaction. These data are helpful to design the reactor and its cooling system.

TN264 - Liquid heat capacity vessel

The accuracy of the heat capacity of a liquid by the calorimetric method depends on the corrective term due to the vapor phase above the liquid. In order to overcome this difficulty, a special calorimetric vessel has been designed. The main feature is a tube welded to the experimental vessel. Its filling is done through the tube by means of a syringe, until there is liquid in the tube. The top of the vessel is machined so that there is no vapor or bubble retained in the experimental vessel. When the liquid is heated the liquid expands freely in the tube, but the volume of liquid in the vessel, located in the direction zone of the calorimeter remains constant. The determination of the heat capacity of this corresponding volume is achieved using the step-heating mode.

TN262 - Liquid percolation vessel (normal and high pressure)

Many powdered compounds (catalysts, oxides, coals,..) are characterized by their surfaces. The measurement of physical or chemical interactions between any solute with the surface of powders characterizes their reactivity. Flow calorimetry is well-adapted method for such an investigation. The liquid percolation vessel enables the liquid to pass through the powder, deposited on a poral filter. The typical experimentation consists in using a first percolation of a carrier liquid in order to achieve the wetting of the powder. Then it is substituted by a solute and the adsorption heat of the solute on the powder is directly measured. After this process the solute is replaced by the carrier liquid and the adsorption heat is measured.

TN258 - Mixing vessel with membrane

For some types of mixing, the reversal mixing vessel (see application sheet TN252) is not adapted : incompatibility of mercury with the samples, mixing of viscous substances. It is replaced by the mixing vessel with membrane. A membrane separates the two chambers eliminating the use of mercury. Mixing is performed by piercing the membrane by a rod which also acts as a stirrer (manual stirring). In the case of viscous substances or formation of a solid during the reaction, a continuous stirring is obtained by adapting a driven motor on the rod. When possible the reversal mixing vessel is preferred to the mixing vessel with membrane. It gives a better precision (no connection with outside).

TN252 - Reversal mixing vessel

The two chambers of the reversal mixing vessel are separated by a tilting lid. The samples (liquid-liquid or liquid-solid) are separately introduced into the vessel outside of the calorimeter. In order to obtain a complete separation of the chambers, a mercury seal on the lid can be used. If the vapor pressures of the samples are low, the mercury seal is not required. After the introduction of the vessels into the calorimeter, the thermal equilibrium is to be achieved in order to have the two separated components at the same temperature. Then, mixing is performed by reversing the calorimeter. If the samples mix easily, only a few rotations of the calorimeter are necessary. In the case of difficult mixing, the reversing mechanism can be maintained during the whole test.

TN250 - Gas circulation vessels (normal and high pressures)

In the gas circulation vessels, the connection consists of two coaxial pipes, to enable the continuous and intermittent circulation of gas on the sample (liquid or solid). At the outlet of the vessel, the evolved gases carried by the sweeping gas can be analyzed on line through a gas analyzer. The gas circulation vessels are used with different types of carrier gas (inert, reductive, oxidative) at various pressures, depending on the model of vessel. Using an adapted gas circuit, different ways of experimentation are possible : use a simple carrier gas, or start an experiment with inert gas and switch for active gas in the second part of the experiment, or introduce an active gas in the carrier gas.

TN247 - Vacuum vessels (normal and high pressures)

The main feature of the vacuum vessels is the connection pipe between the container and outside. Vacuum in the container and also a static pressure of gas are obtained through the pipe. With this facility, different types of experiments are possible : purge the sample before applying a pressure of inert gas, work under vacuum or reduced pressure, work under static pressure of reactive gas (up to 100 bars).

TN237 - Standard vessels (normal and high pressures)

The standard vessels are simple tight containers to be used in the C80 calorimeter when the experiment requires no physical contact between outside and sample. Depending on the internal pressure in the container (gas evolved during heating) two models are available : the normal pressure vessel for investigations at medium temperature (220°C) and low pressure (5 bars) and the high pressure vessel for investigations at higher temperature (300°C) and high pressure (100 bars).

TN235 - Gas adsorption at low temperature under reduced pressure

Isothermal thermogravimetry is a very interesting method for the investigation of gas adsorption. An experimental thermogravimetric device is described, which allows running such tests at low temperature under reduced pressure, or with a linear programmation of the pressure. This is particularly well adapted for the determination of specific surface of compounds, and also to measure the capacity of gas adsorption of molecular sieves at low temperature.

TN231 - Device of adsorption of vapor under reduced pressure

Many solid porous compounds, especially zeolites, are well known for their adsorbing properties. In order to measure their adsorption capacity, a special experimental set-up has been designed for the C80 calorimeter. This device allows characterizing the adsorption of vapor on a solid under reduced pressures. The liquid to be adsorbed is initially frozen, then kept at a well-defined temperature, determining a well-known vapor pressure. This vapor is adsorbed on the solid, previously regenerated under vacuum.

TN225 - Silica reactor for gas adsorption

Gas adsorption investigation requires a good contact between the gas and the solid. A silica reactor has been designed for the Calvet DSC111 in which the reactive gas flows through the sample situated on a sintered glass. This particular cell design is especially interesting for the gas-solid reactions or also for the investigation of reactions occurring in a corrosive medium. The exhausted gases are easily analyzed at the outlet of the silica tube by means of a gas chromatograph or a mass spectrometer (see application note AN226).

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TN220 - Flow cell for liquid adsorption on powders

Applications of many powdered compounds (catalysts, oxydes, coals..) are dependent on their surfaces. The measurement of physical or chemical interactions between any solute with the surface of powders characterizes their reactivity. Flow calorimetry is a well adapted method for such investigation. A special flow cell is designed and allows the percolation of liquids through a powder. The solutes are introduced in a carrier liquid. Adsorption and desorption reactions can be investigated.

TN211 - Pressurization device for high pressure crucibles

For special applications (oxidation, reduction, decomposition), the pressure of reactive gas must be initially fixed in the experimental crucible. The described pressurization device is designed for the initial pressurization of the sealed high pressure crucibles with inert or reactive gases, after a previous degassing of the sample. The stainless steel crucibles are sealed under the pressure chosen on the control high pressure panel.

TN210 - Controlled high pressure crucibles

(polymerization, organic synthesis..).

TN188 - Mixing cell with metallic membrane

Mixing or reaction of two liquids, particularly when they are viscous

TN170 - What can you determine on using a DRC

Shows the possibilities of DRC

TN150 - Heat of mixing determination

Explains the different methods for the determination of heat of mixing and heat of interaction between solids, liquids, solids with liquid, solid or solid with gas

TN149 - Heat capacity determination

Explains the different methods for the determination of heat capacity

TN141 - Titration of 0,1 M HCl by 0,1 M NaOH

Shows the titration of a HCL solution by a NaOH solution

TN140 - Titration calorimeter

Explains what is a titration calorimeter

TN137 - Adsorption of ethanol on active carbon

Presents the adsorption of ethanol onactive carbon using the ampoule mixing vessel

TN136 - Wetting cell

Describes the ampoule mixing vessel which enables the determination of heat of wetting of a powder

TN124 - Cooling curve of MHTC96

Presents the cooling curve of a mHTC or other eqipment of the 96 line

TN123 - Cooling curves of Setsys TGA-Cryo and Setsys TMA-Cryo

Presents the cooling curve of a Setsys-cryo

TN122 - Cooling curve of Setsys Evolution TGA-18 and Setsys Evolution TMA-18

Presents the cooling curve of a Setsys

TN121 - Cooling curve of Labsys TGA-DSC

Presents the cooling curve of a Labsys

TN120 - Wetting cell

Describes the ampoule mixing vessel which enables the determination of heat of wetting of a powder

TN117 - Dissolution of KCl in water

Presents the determination of heat of dissolution of KCl in water on using reversing mixing vessel and reversing mechanismwith

TN116 - Cell for the mixing of two different substances

Presents the batch mixing vessel to be used with microDSC

TN106 - Determination of the size and shape of pores : thermoporometry

Describes the method of determination of pore size distribution by DSC or calorimetry

TN105 - Modification of a C80 Setaram calorimeter for measuring heat capacities of liquids at temperatures up to 548 K and pressures up to 20 MPa

A method is presented for obtaining Cp at constant pressure in the temperatur erange 343K to 548K at pressures up to 20MPa with an estimated accuracy of ± 0.003 Cp

TN096 - Melting of Indium under different atmospheres and vacuum

Presents the melting of inndium under helium, air, argon and vacuum

TN095 - Enthalpy of vaporization of water

Presents the determination of heat of vaporization of water : see also application note TN094 for description of the crucible

TN094 - Enthalpy of vaporization with TG-DSC111 (ref : S60/2437)

Presents a crucible enabling to measure the heat of vaporization of a liquid, See example of vaporization of water in TN095

TN091 - Thermogravimetry measurement under corrosive atmosphere

Presents an accessory which protects the inside of the furnace of setsys when corrosive atmosphere is to introduced

TN084 - Excess heat capacities of 1-butanol + toluene from 298 to 368 K

Presents the data of excess heat capacity of 1-butanol + toluene

TN081 - Heat capacities of fluoroaniline, fluorophenol and difluorobenzene in condensed phase

The Cp of different organic material is determined with an accuracy of better than 2%

TN028 - Inverse filtering of DSC curve

inverse filtering of DSC curve

PO026 - Monitoring of biodiesel synthesis reactions by isothermal microcalorimetry

Transesterification reaction of colza oil by ethanol using sodium hydroxide as a catalyst could be followed up by calorimetry. The high sensitivity and stability of the instrument allowed to get accurate data even with long term experiments.Three main thermal steps could be noticed: (i) fast direct saponification, (ii) ethanolate diffusion rate-limited step, (iii) Heat production acceleration that may be linked with the hydrolysis of some of the produced ester (could be confirmed by simultaneous spectroscopic methods).

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PO025 - Biomass pyrolysis reactions and products as studied by simultaneous thermal analysis techniques

Adapted analytic tools are necessary to achieve the challenges faced while improving biomass pyrolysis processes. While calorimetry allows acquiring key thermodynamic data such as heat of pyrolysis and heat capacity of biomass materials, thermogravimetry allows understanding the chemistry and kinetics of the involved decompositions. By coupling these techniques with gas analysis, the data offered allow selecting the best suited pyrolysis process conditions.

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PO024 - Coupled calorimetry / MS / volumetry for tritium sorption studies

The presented coupled system is a powerful tool to give a full insight of the sorption of gas on various media. It can be adapted to the study of tritium on solid or liquid media and the desorbed gas can be analysed by high resolution mass spectrometry.

PO023 - Recent development of large volume and sensitive calorimeter for nuclear material accountability

The calorimeters described, based on the principle of measuring differential heat flow, are especially dedicated to the nuclear field owing to their sensitivity, their high volume capacity, their measuring accuracy and precision. In our opinion these characteristics make these calorimeters formidable working tools suitable for the classification of both Tritium and Pu materials such as product, scrap & wastes according to their radioactivity which is directly proportional to the thermal power generated by the sample decay.

PO022 - MOF's Characterisation with innovative volumetric/calorimetric techniques

The accurate characterisation of high surface area sorption materials such as MOF's is very important for practical applications. It can be done with a volumetric Sievert's technique and thermal analysis technique to access to a full range of data. The characterisation methods presented here are not limited to the presented examples and can be extended to all type of solid or liquid media.

PO021 - Coupling of manometric and calorimetric measurements to probe unique characterization of solid hydrogen storage systems.

The accurate characterisation of hydrogen sorption materials is very important for practical applications. It can be done with a volumetric Sievert's technique and thermal analysis technique to access to a full range of data. The characterisations methods presented here are not limited to the presented examples and can be extended to all type of solid or liquid media.

PO020 - High pressure calorimetry as a tool for process optimization

Calorimetry has been extensively used to assess the subsequent effect of material exposure to high pressures, it can be noticed that high pressure calorimetry (or calorimetric experiments directly operated at high pressures) could be more widely employed.

PO019 - High-temperature calorimetry and thermal analysis of perovskites

The goal of this study is to obtain formation energies (enthalpy and Gibbs free energy) of CCTO (Calcium copper titanate CaCu3Ti4O12 ) using high temperature solution calorimetry and heat capacity measurements.

PO018 - Characterization of CO2 and CH4 sorption on coal using the volumetric technique

This present study investigates the CO2 and CH4 sorption on standard coals. The technique described here can be applied to numerous others applications taking advantage of the versatility of the presented sorption rig and attached accessories.

PO017 - New Process Safety Solutions provided by C80 + AKTS

Before scaling up the synthesis of an innovating active principle or of a chemical with unique properties, it is a key issue to make sure that no risk is encountered by the people or the materials involved in the running of this reaction. A major difficulty lies in the fact that stability or hazards tests can hardly be run with industrial time and mass scales.

PO016 - Characterization of Palm Oils at Different Temperature Scanning Rates by MicroDSC

Heat is involved at different steps in the preparation of foodstuffs (cooking, processing ...). When heating, cooling or freezing, the food products undergo different types of transformations: melting, crystallization, oxidation... All these transformations occur in a certain range of temperature and are associated with heat variations.

PO015 - High temperature thermogravimetry for oxidation and corrosion testing in dry and humid atmospheres

The symmetrical thermogravimetric technique provides a solution to follow the mass variations with a high accuracy under a controlled atmosphere. It allows the elimination of errors on the mass weighing due to the manipulations, providing a easier and faster way of experimentation. Moreover the thermogravimetric data obtained can be treated for kinetic evaluation of the oxidation or corrosion processes.

PO014 - Characterization of CO2 sorption on coal and other carbon-based samples

The characterization of the sorption of CO2 on the different medias (coal, basalt...) is crucial for the understanding of the mechanisms of safe, stable, and reliable storage of CO2 in geological storage. The Sievert's technique permits to quantify the CO2 uptake of a solid media. Equilibrium or Kinetic measurements can be done to have a full scope of sorption behaviours. In addition, heat of the different reactions can be collected using calorimeters.

PO013 - Instrumentation for BATTERY Development and Testing

We present a small sample of the experiments that can be obtained with some of our system (from assessing performance to "abuse testing" and of course for the development of new material)

PO012 - High pressure flow mixing calorimetry for the investigation of CO2 capture in amine solutions

The use of the chemical sorbents is today one of the most popular absorption technique for the CO2 capture in postcombustion techniques. In such an industrial process, the amine solution is introduced at the top of an absorption tower while the exhausted fume containing carbon dioxide is introduced at the bottom. As an intimate contact is reached in the absorption tower, the amine solution chemically absorbs the carbon dioxide from the gaseous stream. Such a process especially requires two types of thermodynamic parameters: gas solubility and enthalpy of absorption. The enthalpy of absorption, according to the amount of absorbed gas and the corresponding heat capacities of solutions, define the temperatures of the fluids when they exit the absorption columns. Flow mixing calorimetry is the ideal technique for measuring such enthalpies of absorption. In order to work under pressure, a dedicated high pressure mixing vessel is adapted to be used on the Setaram C80 calorimeter.

PO011 - DIFFERENTIAL MICROCALORIMETRY AND HIGH RESOLUTION X-RAY DIFFRACTION COUPLING FOR POLYMORPHISM INVESTIGATIONS

The structural changes of materials are associated with modifications of thermodynamic parameters. Techniques most frequently used for the study of the structural modifications are generally and respectively those of X-Ray diffraction and thermal analysis. However both types of characterization are generally obtained on independent apparatus operated by different operators that does not facilitate the correlation between both types of phenomena. In order to solve this problem, a coupling of time-resolved X-Ray diffraction at both small and wide angles with differential scanning calorimetry is introduced as a new technique that allows simultaneous characterization of thermal and structural properties of a sample. The apparatus called Microcalix is designed for laboratory bench and conventional source. The example of the study of polymorphism is presented as an application.

PO010 - DESORPTION OF A ZEOLITE STUDIED BY SIMULTANEOUS THERMAL ANALYSIS TECHNIQUES

Two major problems arise when interpreting TG-MS data: firstly, multiple fragmentation peaks can lead to a complex spectrum, especially when a lot of organic species are emitted by the decomposing substances at the same time. This can be bypassed thanks to new techniques such as FT-ICR (Fourier Transform Ion Cyclotron Resonance) and chemical ionisation. Secondly, species of different nature and / or conformation but same molecular weight can lead to similar peaks and thus confuse the data interpretation.

PO009 - Use of Calorimetry to Characterize Pharmaceutical Compounds and their Behavior under different conditions

Humidity Absorption of a Pharmaceutical Compound. CO2 Absorption of a Drug during Transportation.

PO008 - VistoMS: an innovative coupling between thermogravimetric analyzers and high resolution mass spectrometer

Understanding the physical degradation of organic materials and components (pyrolisis, oxidation, dehydration, loss of solvent...) is a major concern today. In this context, advanced technologies, using the coupling of thermal analyzers with other analytical instruments have been developed to study samples of gas emissions during the heating process. Real time monitoring of the compounds is therefore indispensable.The aim of this present work has been to develop innovative coupling between thermogravimetric analyzers and a high resolution compact mass spectrometer (FTICR-MS) with chemical ionization techniques.

PO007 - CO2 SORPTION PROPERTIES OF MATERIALS USED IN FOOD PACKAGING (GASEOUS BEVERAGES)

The food industry have great interest in precise measurement of CO2 gas sorption properties of well known packaging materials including PET. Such measurements would be a great aid in the development and testing of advanced packaging materials such as those used for soda or sparkling beverages containers.

PO006 - Advanced Methods and Challenges in Characterizing Hydrogen Storage Materials

The wide variety of materials being proposed for hydrogen storage today present a number of different challenges to the researcher from an analytical characterization perspective. These include both evaluating the true performance of the materials for real-world applications as well as understanding the underlying fundamental mechanisms controlling the materials properties.

PO005 - CHARACTERIZATION OF GAS HYDRATES FORMATION AND DISSOCIATION USING HIGH PRESSURE DSC

The usual way to determine the thermodynamic conditions of the formation of hydrates in drilling mud formulations is to use a PVT cell with visual observation and simultaneous temperature and pressure measurements. This technique requires heavy instrumentation and often cannot be used if solid particles are present in the formulation. Calorimetry is another way to determine compositions, dissociation enthalpies and heat capacities of hydrates. In order to work under high pressure, an innovative methodology (patent of the French Institute of Petroleum) has been developed using High Pressure MicroDSC to determine the thermodynamic properties and kinetics of gas hydrate formation. This technique allows the detection of phase transitions versus time, temperature and pressure.

PO004 - ADVANCED METHODS AND CHALLENGES IN CHARACTERIZING HYDROGEN STORAGE MATERIALS

State-of-the-art characterization of the hydrogen storage properties of advanced materials requires specialized measurement techniques and equipment for making a variety of measurements including: Pressure-Composition Isotherms (PCT). The PCTPro-2000 is the most advanced fully automated instrument for measuring gas sorption properties of materials, especially for hydrogen storage materials. It is specifically designed for high precision measurements over a wide range of sample sizes, pressures and temperatures.

PO003 - VOLUMETRIC INVESTIGATIONS OF GAS HYDRATES

Gas hydrates, or clathrate hydrates materials have become the focus of great interest in the development of energy and environment-related technologies. All of these applications require the ability to solve problems related to the rates of formation and decomposition of the hydrates, their gas storage capacities and stabilities. PCTPro-2000 is the most advanced fully automated instrument for measuring gas sorption properties of materials. It is specifically designed for high precision measurements over a wide range of sample sizes, pressures and temperatures appropriate for Hydrate investigations.

PO002 - PREDICTIVE CALORIMETRIC DETERMINATIONS FOR THE INVESTIGATION OF NUCLEAR MATERIALS

Calorimetry allows very precise and easy measurements of nuclear materials without any special preparation of the sample, but the major drawback of the technique is the relatively long time of measurement. This mainly depends on the time of response of the calorimeter, but also the thermal inertia due to the large heat capacity of the container. The problem can be numerically solved using a specific software for a predictive measurement of the calorimetric value.

PO001 - VERY HIGH SENSITIVE CALORIMETRY FOR THE CHARACTERIZATION OF FOOD INGREDIENTS

The calorimetric techniques, and especially DSC, are more and more used for the characterization of food ingredients (fatty compounds, starch, proteins, ...) such as glass transition, melting, crystallization, denaturation,... The very high sensitive calorimetry opens a new way of determination when the DSC technique is no more adapted. This technique uses very high sensitive detectors (semiconductors) and allows to work on large amounts of sample (volume available : 1 cm3). Very weak thermal effects such as denaturation of proteins in diluted state, gelification of polysaccharides, are detectable. The calorimetric technique is also adapted for mixing simulations such as dilution, dissolution, wetting, reaction and also enzymatic reactions.

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NEW VOLUMETRY PRODUCT
	A fully automated Sievert instrument for measuring Gas (CO2, CH4, C2H6, N2) Sorption properties of materials.

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Important PCTPro software updates
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Introduction of a new autosampling option for LABSYS, market leading TGA, STA and TG-DSC

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Our agenda

October 10, 2012 - October 12, 2012
GEFTA-STK Symposium
Saarbrücken, GermanyGEFTA-STK Symposium on Thermal Analysis and CalorimetryMore information coming soon
September 26, 2012 - September 28, 2012
International Conference
Darmstadt, GermanyInternational Conference on Chemical Looping 201226th to 28th of September 2012A Concept for Efficient and Clean Use of Fossil ResourcesThe Institute for Energy Systems and Technology (EST) at Technische Universität Darmstadt is pleased to announce the 2nd International Conference on Chemical Looping as „An Alternative Concept for Efficientand Clean Use of Fossil Resources”, to be held from Wednesday 26th to Friday 28th of September 2012 at Maritim Conference Hotel Darmstadt.
September 23, 2012 - September 28, 2012
TOFA 2012
Pula, CroatiaTOFA 2012DISCUSSOIN MEETING ON THERMODYNAMICS OF ALLOYSSCOPETOFA 2012 will be a single session conference based on invited lectures, selected oral presentations and poster sessions. TOFA 2012 aims to promote fundamental and practical aspects of the thermodynamics of alloys in relation to Advanced Materials Design.MAIN TOPICS1. Experimental and theoretical thermodynamics2. Phase diagrams3. Computational thermodynamics4. Thermodynamics of nanoparticles5. Structure of Alloys6. Metallic clusters7. Surface and interfacial phenomena8. Thermodynamic aspects of the reactivity9. Thermochemistry of metallurgical processes
September 16, 2012 - September 19, 2012
MOF 2012
Edinburgh, UKMOF20123rd International Conference on Metal-Organic Frameworks and Open Framework Compounds September 16, 2012 - September 19, 2012John McIntyre Conference Centre, Edinburgh Dechema and the IZA together with the local organising committee warmly invite you to attend MOF2012 in Edinburgh.The aim of MOF2012 is to address all questions concerning the community working with metal-organic frameworks, metal coordination compounds and related materials covering all aspects of MOFs from synthesis and characterization of new materials over properties of MOFs to all kinds of applications, e.g. in biology/medicine, catalysis, magnetism, luminescence and adsorption. We are looking forward to experimental, theoretical, and modelling contributions along with papers addressing key questions regarding potential industrial applications of this fascinating family of materials.
August 20, 2012 - August 24, 2012
ICTAC 2012
Osaka, JapanICTAC 201215th International Congress on Thermal Analysis and CalorimetryAug. 20-24, 2012 Kinki UniversityInternational Congress on Thermal Analysis and Calorimetry (ICTAC) is held every four years, with an aim to promote international understanding and to exchange ideas and findings in the field of thermal analysis and calorimetry. In 2012, memorable 15th ICTAC is held in Osaka, Japan. Osaka is located virtually in the center of Japan, and is near to ancient and beautiful cities of Kyoto and Nara.
August 12, 2012 - August 15, 2012
NATAS 2012
Orlando, Florida, USA40th Annual Conference of NATAS Technical ConferenceAugust 12-15, 2012Short CourseAugust 10-12, 2012Buena Vista Palace Hotel & SpaWith great pleasure, we invite you all to the 40th Annual Conference of NATAS that will take place in Orlando, Florida, 12-15 August 2012.
August 05, 2012 - August 10, 2012
ICCT 2012 and CALCON 2012
Búzios, BrazilICCT 2012 and the 67th Calorimetry ConferenceWe are delighted to invite you to take part in an event that that is unique in every way: the association of ICCT 2012 and the 67th Calorimetry Conference, being held together, both for the first time in Latin America.
July 15, 2012 - July 19, 2012
INMM
Orlando, Florida USAINMM 53rd Annual MeetingJuly 15-19, 2012Renaissance Orlando Resort at SeaWorldOrlando, Florida USAThe 53rd Annual Meeting will provide attendees with a professional forum for the exchange of the latest technical information in nuclear materials management. The meeting will address all aspects of nuclear materials management with papers and posters organized by the INMM Technical Program Committee.
July 15, 2012 - July 20, 2012
BZA 2012
Chester, EnglandThe 35th Annual British Zeolite Association Meeting15th - 20th July 2012University of Chester in northwest EnglandThe 2012 meeting of the British Zeolite Association will be held at the University of Chester in northwest England. This triennial, Chislehurst-style BZA meeting, organised along the lines of a Gordon Conference, will be limited to 120 participants.The BZA welcomes contributions from all fields of zeolite, microporous and mesoporous materials science, including synthesis, structure, applications, characterisation, catalysis and computational studies.
June 26, 2012 - June 29, 2012
CTEC 2012
Lyon, FranceCalorimetry and Thermal Effects in CatalysisCalorimetry and thermal analysis methods, alone or linked to other techniques, applied to the characterization of catalysts, supports and adsorbents, and to the study of catalytic reactions in various domains: air and wastewater treatment, clean and renewable energies, refining of hydrocarbons, green chemistry, hydrogen production and storage, CO2 capture...
June 18, 2012 - June 22, 2012
EU BC&E 2012
Milano, Italy20th European Biomass Conference and Exhibition18 - 22 June 2012 at the Milano Convention Centre in Milano, ItalyWith this event, we will continue the biomass specialist's role as the leading technical platform covering all aspects of biomass from research to industry and markets.
June 10, 2012 - June 15, 2012
SUMMER SCHOOL OF CALORIMETRY 2012
Lyon, FranceSummer School of Calorimetry 2012 "Calorimetry and thermal methods in catalysis"Calorimetry and thermal analysis methods, alone or linked to other techniques, applied to the characterization of catalysts, supports and adsorbents, and to the study of catalytic reactions in various domains: air and wastewater treatment, clean and renewable energies, refining of hydrocarbons, green chemistry, hydrogen production and storage, CO2 capture...
June 05, 2012 - June 08, 2012
AICAT 2012
Rome, ItalyAICAT 2012Sapienza University of RomeJune 5-8 2012AICAT 2012 is jointly organized by the Italian Association of Calorimetry and Thermal Analysis (AICAT) and by Interdivisional Group of Calorimetry and Thermal Analysis (GICAT) of the Italian Chemical Society (SCI) and represents the main scientific meeting of these Associations. The Congress aim is to provide to the scientists working in Calorimetry, Thermal Analysis and closely related topics an opportunity for an exchange of scientific information, critical discussion and advanced planning on fundamental and applied research aspects of interest in this field.
May 28, 2012 - June 01, 2012
2012 Fiery Ice
Sapporo, Hokkaido, Japan2012 Fiery Ice8th International Workshop on Methane Hydrate Research & DevelopmentWith great pleasure, we announce that 8th International Workshop on Methane Hydrate Research & Development (Fiery Ice from the Seas) is being held in Sapporo, Japan at refreshing season, 28th of May to 1st of June, 2012.
May 27, 2012 - May 31, 2012
BiPoCo 2012
Siófok, Lake Balaton - Hungary BiPoCo 2012,an International Conference onBio-Based Polymers and CompositesMay 27-31, 2012Siófok, Lake Balaton - HungaryDownload the First circular
May 22, 2012 - May 24, 2012
JCAT 2012
Toulouse, FranceThe 43rd Calorimetry and Thermal Analysis DaysDownload the conference flyer
May 20, 2012 - May 25, 2012
HTCPM 2012
Les Embiez, FranceHTCPM 20128th International Symposium on High-Temperature Corrosion and Protection of Materials20 - 25 May, 2012Les Embiez, France The goal of this international symposium is to reflect the interests of the major industries dependent on the successful application of high-temperature materials, providing a periodic updating on the current research and understanding in these areas.
May 16, 2012 - May 18, 2012
INNOSTOCK 2012
Lleida, SpainINNOSTOCK 2012The 12th International Conference on Energy Storage16-18 May 2012Innostock 2012 is part of the Stock conference series sponsored by the ECES IA of the International Energy Agency.Innostock 2012 will gather the world’s leading specialists and academic researchers within the field of energy efficiency through energy storage. Energy storage will present in all its topics:• Underground thermal energy storage• Sensible, latent and thermochemical energy storage• Electrical storage
May 14, 2012 - May 18, 2012
11th International Hydrocolloids Conference
Purdue University, USA11th International Hydrocolloids ConferenceBiofunctionality and Technofunctionality of Hydrocolloids14-18 May 2012, Whistler Center for Carbohydrate Research, Purdue University, USAThe 11th International Hydrocolloids Conference is organized by the world-renowned Whistler Center for Carbohydrate Research and will be held at The Stewart Center at Purdue University, Indiana, USA.
April 30, 2012 - May 03, 2012
Carbon Capture Utilization & Sequestration
Pittsburgh, Pennsylvania - United States 11th Annual Conference on Carbon Capture Utilization & Sequestration April 30 - May 3, 2012Pittsburgh, Pennsylvania The 2012 Conference program follows in the footsteps of the past 10 events, with an added emphasis this year on potential utilization of anthropogenic carbon emissions that is reflected in the new name of the conference. The focus is on systems and technologies that are being or could be deployed in the U.S. and North America.