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515 articles

PO030 – A new microcalorimeter for the investigation of thermal properties of dispersed systems with multiple samples capability Private content

Microcalorimetry leads to key information on structure, stability, formation and dissociation mechanisms during temperature scanning and / or isothermal operations [1]. Gelatinized starch goes through retrogradation, which involves recrystallization of amylose and amylopectin. Retrogradation characteristics depend on parameters like botanic specie or water content. It is the main source of bread staling effect [2]. Ageing of bread crumb, maize and wheat starch dough was studied with the newly designed microcalorimeter

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

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.

PO022 – MOF’s Characterisation with innovative volumetric/calorimetric techniques Private content

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.

PO023 – Recent development of large volume and sensitive calorimeter for nuclear material accountability Private content

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.

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.

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).

PO027 – Characterization of CO2 clathrate formation and dissociation using High Pressure DSC Private content

Carbon capture and sequestration (CCS) technologies play a critical part in the attempts to reduce the atmospheric carbon dioxide content. Common CO2 sequestration techniques involve direct injection into geologic formations such as depleted oil or gas reservoirs, or deep unminable coal seams. An alternative approach is the injection of CO2 into natural methane
hydrate deposits in ocean sediments. In this case, formation of carbon dioxide hydrates is expected, together with a dissociation of methane hydrates. Examples include:
– SECOHYA (SEparation of CO2 by HYdrate Absorption, France)
– SUGAR (Submarine GAs hydrate Reservoirs, Germany)

PO028 – The input of microcalorimetric techniques for the characterization of latent and sensible heat storage materials Private content

Fatty acids, paraffins, organic substances, or inorganic salts can be used as thermal energy storage materials if they have high enough latent heat together with temperatures of phase change adapted to the application. Moreover, the sensible heat, or the heat capacity change over the temperature range of the considered phase change can play an important role, together with the thermal conductivity properties of the material. To be suitable for energy storage, a PCM has to possess the main following specifications:
– a large phase change enthalpy
– a phase change temperature adapted to a given energy storage
– a reproducible phase change
– a limited subcooling
All these parameters are measured via the calorimetric technique. The calorimeters and DSC’s that are able to investigate solid and liquid materials can apply for the determination of latent heat. However there are significant differences in term of sample volume and temperature scanning rate. The choice of these two parameters are of high importance in the thermal investigation of PCM’s. In order to solve the drawbacks of the DSC plate detector, the solution is to use larger amounts of sample and very low scanning rates. These specifications are
offered by the MicroDSC type detectors

PO029 – Use of the DSC and TG-DSC techniques for the investigations of gas interaction on zeolites Private content

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.

PO010 – DESORPTION OF A ZEOLITE STUDIED BY SIMULTANEOUS THERMAL ANALYSIS TECHNIQUES Private content

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.

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

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.

PO012 – High pressure flow mixing calorimetry for the investigation of CO2 capture in amine solutions Private content

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.

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

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.

PO015 – High temperature thermogravimetry for oxidation and corrosion testing in dry and humid atmospheres Private content

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.

PO017 – New Process Safety Solutions provided by C80 + AKTS Private content

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.

PO008 – VistoMS: an innovative coupling between thermogravimetric analyzers and high resolution mass spectrometer Private content

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.

AN696 – Wax Appearance Temperature (WAT) determination of crude oils usingthe DSC technique

The wax appearance temperature (WAT), also known as the cloud point, is an important characteristic to evaluate the possible wax precipitation of a given fluid. It is defined as the temperature at which a crude oil first precipitates. In the petroleum industry, such wax depositions in pipelines and reservoirs can lead to many issues,
including a reduced flow or even a blocked pipeline, with subsequent important production problems. Different techniques have been developed to measure the WAT of a crude oil but the method using DSC is commonly used for its rapidity, convenience and accuracy.

AN697 – Effects of pressure on the Wax Appearance Temperature (WAT) of crude oils Private content

In the petroleum industry, waxes crystallization resulting from the precipitation of paraffins contained in oils, can occur in reservoirs, pipelines and process equipment. Many major issues can be related to these deposits, including a modification of the flow characteristics, a reduced production or even a blocked line in the worst cases. To evaluate the possible wax precipitation of a given fluid, the wax appearance temperature has to be determined. It is defined as the temperature at which a crude oil first precipitates. Most of the studies about WAT are carried out under atmospheric pressure. However, WAT determination under experimental conditions close to real operating ones (particularly under pressure) is a key point to predict the crude oils behavior.

AN698 – Gas hydrate nucleation in water-in-oil emulsions Private content

Gas hydrates, also known as clathrates, are crystalline compounds made of gaseous molecules trapped in water cages. Most low molecular weight gases, such as methane, carbon dioxide or nitrogen can form hydrates at suitable low temperatures and high pressures. These solids can naturally be found in the deep ocean floor, in lake and ocean sediments but also undesirably in pipelines. In the latter case, hydrate crystals might agglomerate and cause flow assurance issues such as reduced flow, plugged line or equipment damage. To have a better understanding of the underlying conditions leading to their formation, differential scanning calorimetry, operated under high pressure, is a very useful technique to study thermodynamic and kinetic properties such as nucleation.

PO001 – VERY HIGH SENSITIVE CALORIMETRY FOR THE CHARACTERIZATION OF FOOD INGREDIENTS Private content

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.

PO002 – PREDICTIVE CALORIMETRIC DETERMINATIONS FOR THE INVESTIGATION OF NUCLEAR MATERIALS Private content

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.

PO003 – VOLUMETRIC INVESTIGATIONS OF GAS HYDRATES Private content

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.

PO004 – ADVANCED METHODS AND CHALLENGES IN CHARACTERIZING HYDROGEN STORAGE MATERIALS Private content

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.

PO005 – CHARACTERIZATION OF GAS HYDRATES FORMATION AND DISSOCIATION USING HIGH PRESSURE DSC Private content

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.

AN693 – Thermal analysis, calorimetry and molten salt Private content

A salt which is solid under standard temperature and pressure conditions and liquid at elevated temperatures can be designated as a molten salt. There is a growing interest for molten salts in different fields, including thermal energy storage, heat transfer, catalysis or chemistry. While for the two first cases, their interesting thermodynamic properties (heat capacity and thermal conductivity) are applied, in the two other cases they are used for their ability to dissolve substances (especially oxides, carbides, nitrides and metals). High temperature calorimetry can bring key information on the thermal properties of pure or blends of salts, like melting / crystallization temperatures, heat of melting, heat capacity and heat of mixing and / or dissolution.

PO006 – Advanced Methods and Challenges in Characterizing Hydrogen Storage Materials Private content

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.

AN694 – Characterization of proteins Private content

Research and development is of vital importance in the pharmaceutical industry. To obtain a perfectly characterized controlled and stabilized protein based drug, the researchers use different techniques among which differential scanning calorimetry holds an important place. Indeed when heated, a protein undergoes unfolding or denaturation, which is characterized by and endothermic effect on a DSC trace. Once unfolded, proteins can also go through an aggregation process which is typically exothermic.
SETARAM Instrumentation developed ?SC a new microcalorimeter with the following characteristics:
– Dual samples capacity
– Removable and cleanable cells that allow avoiding troubles linked with gel formation or aggregates deposition
– Improved limit of detection
– An extended temperature range from -40°C up to 200°C
Examples of application in the field of proteins characterization are detailed in the present document.

AN695 – Hydrogen sorption studied by manometric (Sievert’s) techniques alone and coupled to calorimetry

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 microdoser attachment of PCTPro can measure sample quantities down to mg’s.
The management of the heat released during the formation of a chemical hydride is critical for practical applications. This is particularly true when poorly stable chemical hydrides are involved. It is highly desirable to be able to quantify and validate reaction enthalpies in situ during a sorption measurement.
Metal-organic frameworks (MOFs) are interesting porous materials because their properties can be tailored for specific applications. Today these structures are envisaged for multiple applications in gas adsorption, like hydrogen storage, selective adsorption of CO2 against CH4, or CO2 against H2. The MOF-5 (fig 2.) is chosen as an example of a commercially available Metal Organic Framework to demonstrate the capacities of coupled Sievert’s technique and heat flow calorimetry at very low temperature.

AN679 – Temperature cycling stability of Phase Change Materials

Some materials have the capacity to store and release large amounts of energy by changing their
physical sate: they are called Phase Change Materials (PCM). They can be used for instance to minimize
the need of air conditioning and heating: incorporated into walls of buildings, they absorb heat when
outside temperature is high, and release it when temperature decreases. This keeps the house into a
“comfort temperature zone”. Another utilization of the PCM is the use of residual heat from exothermic
reaction in industry as a source of energy. An application fitting phase change temperature and a large
melting enthalpy are two obvious requirements for these materials. However, there is another
important parameter: the cycling stability, in order to use the PCM as many times for storage and
release of heat as required by an application

AN683 – Starch retrogradation and bread staling Private content

Gelatinized starch goes through retrogradation, which involves recrystallization of amylose and amylopectin. Retrogradation characteristics depend on parameters like botanic specie or water content. It is the main source of bread staling effect. Ageing of maize, wheat starch dough and of bread crumb, was studied with the state of the art µSC microcalorimeter.

AN684 – Unfolding and aggregation effects of Beta-lactoglobulin using MicroSC

Globular proteins are widely used in food and pharmaceutical industries because their unique folded structure leads to interesting active principle or flavor binding, water solubility, or gelation properties. The thermally induced structural modifications of a protein do not only depend of its origin and extraction, purification conditions, but also of its environmental conditions like pH, salt content, or solvent type. β-Lactoglobulin (β-LG) is the major whey protein of cow and sheep’s milk. β-LG is a well-characterized globular whey protein which exists mainly in its dimeric form between pH 3 and 7.

AN685 – Melting of NaCl and NaF using the TG-DSC technique Private content

The thermal properties of halides are characterized by melting and dehydration of water present at a particular stage during heating. Halite is the mineral form of NaCl and Villaumite is the mineral form of NaF. The two characteristic halides are investigated using the TG-DSC technique in order to investigate their stability

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.

AN686 – Oxidation Induction Time (OIT) of lubricating oil using the TG-DSC technique Private content

The Oxidation Induction Time (OIT) method is very widely used for testing the oxidative stability of polymeric materials but also organic materials such as oils, greases, lubricants… DSC is the standard technique used for such determination that is covered by different standards especially ISO11357-6. In this case , OIT is defined as the time to the onset of the exothermic oxidation peak for a sample exposed to air or oxygen at an elevated oxidation temperature. But it is less common to use the simultaneous TG-DSC technique for such a determination. This technique is applied on a lubricating oil.

AN673 – CO2 capture on aminated solid sorbents by thermogravimetry Private content

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

AN690 – GRAPHENE: A new field of applications for thermal analysis techniques Private content

Graphene is a two dimensional material consisting of a single layer of carbon atoms arranged in a honeycomb or chicken wire structure. It is the thinnest material known and yet is also one of the strongest. It conducts electricity as efficiently as copper and outperforms all other materials as a conductor of heat. Graphene is almost completely transparent, yet so dense that even the smallest atom helium cannot pass through it. All these new developments require a good knowledge of the physical and chemical properties of grapheme and the corresponding composites. As in many other new fields, thermal analysis offers a large range of methods to fulfil the experimental needs.
Some examples are given to illustrate the works that are done with Setaram thermoanalyzers.

AN674 – Gas adsorption on catalysts and adsorbents using a quartz tube reactor on a Calvet type DSC Private content

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.

AN691 – Thermogravimetry and calorimetry applied to the study of cement hydration Private content

The Romans built enduring structures from hydraulic cements 2000 years ago, but the way anhydrous starting materials convert into hydrates remains a mystery. Its understanding, and control remains a challenge especially in modern cement or concrete applications such as large constructions or oilwell industry where cement hydration conditions are particularly tough.

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

AN692 – Thermal analysis and volumetry solutions for the evaluation of gas sorption and porous properties Private content

Shale gas, coming from organic matter trapped in shale, is a major growing unconventional gas
resource. But there is a need for a more into depth understanding of phenomena linked with its
formation, with the determination of the amounts in place in a reservoir, and on its processes of
recovery. For instance: reliable sorption isotherms at high-pressure and high temperature conditions
which are conditions met in the shale geological formations.

AN676 – Cellulose pyrolysis investigation by thermogravimetry coupled with FTIR spectrometry Private content

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…)

AN677 – Evolution of CO2 released during pyrolysis of lignocellulosic biomass and its components Private content

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.

AN678 – Pyrolysis study of lignocellulosic biomass and its components by DSC Private content

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.

AN657 – Shrinkage temperature of bovine pericardium tissue for bioprosthetic heart valve application by MicroDSC Private content

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.

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

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

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

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.

AN671 – Polymorphic behavior of cocoa butter.Influence on chocolate tempering conditions Private content

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).

AN660 – Characterization of PTFE (Teflon) by DSC Private content

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.

AN661 – Characterization of PEN (PolyEthylene Naphtalate) by DSC Private content

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

AN662 – Characterization of a polyimide by DSC Private content

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.

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

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.

AN666 – Cyclic oxidation of metallic alloys by symmetrical TGA Private content

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

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.

AN656 – Melting of different types of chocolates by DSC Private content

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.

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

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

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

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

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.

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.

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.

AN654 – CO2 adsorption into coal measured by PCTPro-E&E Private content

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

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.

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

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.

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.

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

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

AN645 – Crystallization of palm oil by DSC Private content

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.