rd CTAS Annual Workshop & Exhibition · and K. S. Rane$ SB Arts and KCP Science College, Bijapur, Karnataka, India $ Rani Channamma University, Belgaum-591156, Karnataka, India Poster

23rd CTAS Annual Workshop & Exhibition

May 7-8, 2013

University of Ontario Institute of Technology Oshawa, Ontario, Canada

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CANADIAN THERMAL ANALYSIS SOCIETYAN AFFILIATE OF THE NORTH AMERICAN THERMAL ANALYSIS SOCIETY

www.CTAS.org

Tuesday May 7, 2013

Training SessionEnergy Research(ER) Building, Room 1094

8:30 – 9:15 Registration

9:15 – 10:15 Application of thermal analysis in sol-gel synthesis of mixedmetal oxides having potential magnetic, electric andphotoluminescence propertiesRanjit K. VermaUniversity Department of Chemistry, Magadh University, BodhGaya-824234, India

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Introduction and Applications of Thermal Analysis andCalorimetrySubhash C. MojumdarDepartment of Chemistry, University of Guelph, Guelph, ON,CanadaDepartment of chemical Technology and Environment, TrencinUniversity of A. Dubceck, Puchov, Slovakia

10:15 – 10:45 Exhibition, Posters & Coffee break at ER1056 and ER Hall

10:45 – 11:30

11:30 – 12:00

Kinetics from TG and DSCChristopher BadeenNatural Resources Canada, Canadian Explosives ResearchLaboratory, 1 Haanel Drive, Ottawa, Ontario K1A 1M1 Canada

Characterization of Thermosets by Modulated DSC®)

Kadine Mohomed and Charles Potter, TA Instruments, New Castle,DE USA

12:00 – 13:30 Lunch at UB Mezzarine (next to ER building)

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13:30 – 14:00

14:00 – 14:30

Introducing New Fully-Integrated TGA-GC-MS and TGA-FTIRSystems for Characterization of Materials Including Polymers,Petrochemicals, Biomass, And MoreRobert PieperNETZSCH Instruments N.A., LLC, 129 Middlesex Turnpike,Burlington, MA 08103, United States

Review of Thermal Conductivity MethodsAdam Harris, Jarrett Nickerson and Robert BatemanC-Therm Technologies Ltd., 921 College Hill Rd, Fredericton, NB

14:30 – 15:00 Examples of Advantages of 'Multi-Curve' ExperimentsMelanie NijmanMettler-Toledo AG, Business Unit Analytical, Sonnenbergstr. 74,8603 Schwerzenbach, Switzerland

15:00 – 15:30 Thermal Analysis of Soft Materials and Heat-Induced ChemicalReactionsD. V. SoldatovDepartment of Chemistry, University of Guelph, Guelph, Ontario,Canada

15:30 – 15:45 Coffee break at ER Hall

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Vendor PresentationsEnergy Research(ER) Building, Room 1094

15:45 – 16:00 TA Instruments

16:00 – 16:15 Mettler-Toledo Inc.

16:15 – 16:30 C-Therm Technologies Inc

16:30 – 16:45 Setaram Inc.

16:45 – 17:00 Netzsch Instruments Inc.

17:00 – 17:15 Spectra Research Corporation

Social EventUB Mezzarine (next to ER building).

Mixer/Dinner

17:30 – 19:30

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Wednesday May 8, 2013

Technical SessionEnergy Research(ER) Building, Room 1094

08:30 – 9:00 Registration

09:00 – 09:45 Plenary LectureThe use of thermal analysis in the development of novel fuelcell materialsE. Bradley EastonFaculty of Science (Chemistry), University of Ontario Institute ofTechnology, Oshawa, ON Canada L1H 7K4

09:45 – 10:30

10:30 – 11:00

Plenary LectureThermodynamic Modelling of Inorganic Compounds inAqueous Process SolutionsVladimiros G. PapangelakisUniversity of Toronto, Dept. of Chemical Engineering and AppliedChemistry, 200 College Street, Toronto, ON, Canada M5S 3E5

Exhibition, Posters & Coffee break at ER1056 and ER Hall

11:00 – 11:30 Invited LectureUsing the Iso-Conversional Model to Identify Growth Modes of aLipid NetworkSuresh S. NarineDepartments of Physics & Astronomy and Chemistry, TrentUniversity,1600 West Bank Drive, Peterborough, Ontario, K9J 7B8,Canada

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11:30 – 11:45 Chemical Modeling Aqueous Process Systems Using OLIMichael Carlos and Vladimiros G. PapangelakisDepartment of Chemical Engineering and Applied Chemistry,University of Toronto,200 College Street, Toronto, Ontario M5S 3E5,Canada

11:45 – 12:00 Annual General Meeting

12:00 – 13:30

13:30 – 13:45

Lunch at UB Mezzarine (next to ER building)

Thermally Induced Intramolecular Condensation in SolidLeucyl-AlanineF. I. Ali and D. V. SoldatovDepartment of Chemistry, University of Guelph, Guelph, Ontario,Canada

13:45 – 14:00 Misinterpretation of cure data analysis in epoxy-basednanocompositesGeoff Rivers1, Allan Rogalsky1, Pearl Lee-Sullivan1 and Boxin Zhao21Department of Mechanical and Mechatronics Engineering,2Department of Chemical Engineering, University of Waterloo, 200University Avenue, Waterloo, Ontario, Canada N2L 3G1

14:00 – 14:15 The Curie Point Method for TGA Temperature CalibationCharles PotterTA Instruments, New Castle, DE USA

14:15 – 14:30 Standard Partial Molar Properties of Adenine and its Ions inHigh Temperature Aqueous Systems and Relevance toModeling the Origins of LifeAlexander R. Lowe, Jenny S. Cox, and Peter TremaineUniversity of Guelph, Dept Chemistry, 50 Stone Road East Guelph,Ontario, Canada N1G 2W1

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14:30 – 14:45 Reaction Kinetics and Mechanisms of the ThermalDecomposition of Copper Chlorides and OxidesZhaolin Wang1, Gabriel Marin2, Greg Naterer3, Kamiel Gabriel41, 4Faculty of Engineering and Applied Science, University of OntarioInstitute of Technology, 2000 Simcoe St N, Oshawa, Ontario,Canada, L1H 7K4.2 Colorado Salt Products, 3910 Joliet St, Denver, CO, 80239.3Faculty of Engineering and Applied Science, Memorial University ofNewfoundland, St. John’s, Newfoundland, Canada, A1B 3X5

14:45 – 15:00 Standard partial molar heat capacities of aqueous aluminateunder hydrothermal conditions from integral heat of solutionexperiments.Y. Coulier1 and Peter R. Tremaine1

1 Department of Chemistry, University of Guelph, 50 Stone RoadEast, GUELPH ON, N1G 2W1 Canada

15:00 – 15:15 Exhibition, Posters & Coffee break at ER1056 and ER Hall

15:15 – 15:30 Modification of a DSSC photoanode with carbon nanotubes andTiO2 nanoparticles with different morphologySimone Quaranta, Donald McGillivray, Liliana Trevani and FrancoGaspariFaculty of Science, University of Ontario Institute of Technology

15:30 – 15:45 Evaluating the activity and durability of Pt-based fuel cellcatalystsFarhana S. Saleh and E. Bradley EastonFaculty of Science, University of Ontario Institute of Technology,2000 Simcoe Street North, Oshawa, Ontario, Canada L1H 7K4

15:45 – 16:00 Analysis of Metastable Materials at high heating ratesMelanie NijmanMettler-Toledo AG, Business Unit Analytical, Sonnenbergstr. 74,8603 Schwerzenbach, Switzerland

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16:00 – 16:15 High-Pressure Thermal Conductivity Characterization ofMaterialsAdam Harris, Jarrett Nickerson and Robert BatemanC-Therm Technologies Ltd., 921 College Hill Rd, Fredericton, NB

16:15 – 16:30

16:30 – 16:45

16:45 – 17:00

Multi-Length-Scale Structural Elucidation of MechanismResponsible for Inhibiting FAME CrystallizationAthira Mohanan, Laziz Bouzidi and Suresh S. NarineTrent Centre for Biomaterials Research, Departments of Physics andAstronomy and Chemistry, Trent University, Peterborough, Ontario,K9J 7B8

Investigating the Stability of Linear Diesters Derived fromVegetable Oils: Dependence on the β-Hydrogen and its EnvironmentLatchmi Raghunanan and Suresh S. NarineTrent Centre for Biomaterials Research, Departments of Physics andAstronomy and Chemistry, Trent University, Peterborough, Ontario,K9J 7B8

Vegetable Oil Derived Lubricants: Improvement of ThermalProperties by Structural ModificationsLaziz Bouzidi, Latchmi Raghunanan, Shaojun Li and Suresh NarineTrent Centre for Biomaterials Research, Departments of Physics &Astronomy and ChemistryTrent University, 1600 West Bank Drive, Peterborough, K9J 7B8,Ontario Canada

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17:00 – 17:15 Synthesis, Characterization and Thermal Analysis of the 1st rowTransition Metals:Part-I: Oxalate Hydrazinate ComplexesYogita U. Jambalekar, Satish A. Tarale, Suraj M. Sutar , Santosh P.Chougule, R. M. Babshet and K. S. RaneBK College, Jyoti College Campus, Club Road, Belgaum, Karnataka,IndiaPart-II: Formate HydrazinatesSurekha S. Hadnur, Saroja U. Nemagouda, Mallikarjun S. Yadaweand K. S. Rane$

SB Arts and KCP Science College, Bijapur, Karnataka, India$ Rani Channamma University, Belgaum-591156, Karnataka, India

Poster SessionER Hall

Structure and Stability of Solid OligoglycinesA. J. Smith and D. V. SoldatovDepartment of Chemistry, University of Guelph, Guelph, Ontario, Canada

Study of the Oxidation Enthalpy of PyriteS. C. Mojumdar, I. Bylina and V. G. PapangelakisDepartment of Chemical Engineering and Applied Chemistry, University of Toronto,200 College Street, Toronto, Ontario, Canada M5S 1A4

Thermal Analysis of Pt-Mn Alloys to Find the Most Effective Temperature for HeatTreatment and Enhancing the Ethanol Oxidation in PEM Fuel CellM. R. Zamanzad Ghavidel and E. Bradley Easton,Faculty of Science (Chemistry), University of Ontario Institute of Technology, 2000Simcoe St. N., Oshawa, ON, Canada L1H 7K4


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Performance of Composites with Metakaolin-Blended CementsĽudovít Krajči, Subhash C. Mojumdar, Ivan Janotka, Francisca Puertas■, MartaPalacios, Marta Kuliffayová Institute of Construction and Architecture, Slovak Academy of Sciences, Dubravska

cesta 9, 845 03 Bratislava, Slovakia University of Guelph, Department of Chemistry, Guelph, ON, Canada Building Testing and Research Institute, Studena 3, 821 04 Bratislava, Slovakia,■Eduardo Torroja Institute for Construction Sciences, IETcc-CSIC, Serrano Galvache 4,

280 33 Madrid, Spain Swiss Federal Institute of Technology Zürich, Institute of Building Materials,

Schafmattstraße 6, 8093 Zürich, Switzerland

Deposition of Silver Nanoparticles on Cellulosic Substrates for BiomedicalApplicationsCassandra Scott, Liliana Trevani, Janice StrapFaculty of Science, UOIT, 2000 Simcoe St N. Oshawa, ON, L1H7K4

The Investigation and Characterization of Next Generation Proton ExchangeMembranes for Fuel Cell-Based Ethanol Sensors

Jesse T.S. Allan and E. Bradley Easton

Faculty of Science (Chemistry), University of Ontario Institute of Technology, 2000Simcoe St. N., Oshawa, ON, CANADA L1H 7K4

Examination of Ceramic Carbon Electrodes for Low Humidity Fuel CellApplicationsJennie I. Eastcott and E. Bradley EastonFaculty of Science (Chemistry), University of Ontario Institute of Technology2000 Simcoe St. N., Oshawa, ON L1H 7K4

Physical and electrochemical properties of novel anode materials for use in theCu-Cl thermochemical cycle for the production of hydrogenP. E. Edge and E.B. EastonFaculty of Science, University of Ontario Institute of Technology, 2000 Simcoe StreetNorth, Oshawa, ON L1H 7K4

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Polymorphism of Guaiacol and Crystal Structure of the Trigonal FormT. Fillion and D. V. SoldatovDepartment of Chemistry, University of Guelph, Guelph, Ontario, Canada

Replication of Bacterial Cellulose Nanoarchitecture with Metal Oxide CatalystsUtilizing a Facile Supercritical Carbon Dioxide Aided MethodNick-Hugh Wisdom, Andrew Vreugdenhil, Janice Strap and Liliana TrevaniFaculty of Science, University of Ontario Institute of Technology

Supercritical Fluid Synthesis of Metal Oxide Platinum Catalysts with High Activityand Stability for Fuel Cell ApplicationsOdetola Chris, Liliana Trevani and E. Bradley EastonFaculty of Science, University of Ontario Institute of Technology

Characterization of ADN and ADN-based PropellantsQ.S.M. Kwok, M. Vachon, C. Badeen, W. Ridley, D.E.G. Jones and S. SinghCanadian Explosives Research Laboratory, 1 Haanel Drive, Ottawa, Ontario K1A 1M1Canada

CANADIAN THERMAL ANALYSIS SOCIETY AN AFFILIATE OF THE NORTH AMERICAN THERMAL ANALYSIS SOCIETY

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Plenary Lecturers and Trainers

Professor Ranjit Kumar Verma

International Responsibilities The Secretary, ICTAC (International Confederation for Thermal Analysis and

Calorimetry (www.ictac.org) (20012-16) Regional Editor, Journal of Thermal Analysis and Calorimetry (Springer

Science)(2010) (www.springeronline/jtac) Guest Editor, SATAC-ICC Spl issue, J.Thermal Anal. Calorim, (Vol 107 No.1) Guest editor, SATAC-NCCT Spl issue, J.Thermal Anal. Calorim, (Vol 110 No.2) International Chairman, ICTAC Education Committee(2008-2012); Also ex-

Councilor & India’s Representative, ICTAC (2004-2006) MEMBER, INTERNATIONAL SCIENTIFIC AWARDS COMMISSION, ICTAC

(2008) India’s Representative, International Planning Committee (IPC), Int’l Conf. of

Coordination Chemistry (ICCC) 97, 98

National Responsibilities The Hony. Editor (Inorganic and Analytical), J. Indian Chem. Soc. (2007-10);

Associate Editor, J. Indian Chem. Soc. (1995-96; 1999-2000) Scientist-in-Charge (Sectional President), Inorganic Chemistry Section, Indian

Chemical Society, 37-39th Annual Conventions of Chemists (Haridwar, Jodhpur and Nagarjunanagar, India, 2000-2002); Actg. Scientist I/c, Analytical and Envir. Chem. Section, 40th Annual Convention of Chemists, Jhansi 2003. Also, Executive Council Member, Indian Chemical Society (1997-1999, 2003-2005, 2011-2013)

Sectional President, Inorganic Chemistry Section, 22nd Annual Conference of Indian Council of Chemists (IIT, Roorkee, 2003);Vice President, Indian Council of Chemists (2004-2008, 2009-2014)

Member, National Council (2008-2011) and Member, Executive Committee, Indian Science Congress Association (ISCA)(2006-07,2011-12, 2013-14)

Vice President, Association of Chemistry Teachers (Homi Bhabha Centre, Mumbai)(2005-10)

Vice President, Indian Thermal Analysis Society(B.A.R.C.)(2012-14)

Convener, Bihar Academy of Sciences, BCST, Dept of S & T, Govt of Bihar (2012- 13)

Chairman, SATAC-2010, SATAC-2011

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Subhash C. Mojumdar, Ph.D.

Dr. S. C. Mojumdar obtained his B.Sc.-M.Sc. and Ph.D. degree in Chemical- Biochemical and Biomedical Engineering, respectively. Since then he worked in

many research fields such as polymeric thin films, antibiotics, antioxidants, organometallics, glasses, ceramics, cements and many other bio and

nanomaterilas. He extended his research activities from medicine through construction to nanotechnology using many thermoanalytical techniques such as

TG, DTG, DTA, DSC, DMA, TMA, optical transmittance (light beam) thermal analysis, EGA, calorimetry, conduction calorimetry, isothermal pressure transducer analysis, heating microscopy, thermal conductivity etc. He has already published

over 300 research articles in the field of medicine, chemistry, biochemistry, materials science, nanotechnology, thermal analysis and many other fields. He delivered 40 training, invited and plenary lectures throughout the globe and has

been selected an examiner for several M. Sc. and Ph.D. theses. He is a member of 15 professional organizations and presently acting as the Vice-President of the

Canadian Thermal Analysis Society (CTAS) and served CTAS as The President and Acting President in the past. He is also the Chair of the Board of the Examiners of the ACPO, Local Sections Chair, NATAS and an Educational Committee member

of ICTAC. Dr. Mojumdar is the Editor-in-Chief of the Chartered Chemist News (CCN) and also a member of the editorial board of several journals such as Journal

of Thermal Analysis and Calorimetry (JTAC) and Research Journal of Chemistry and Environment, Advances in Bioscience and Biotechnology, Journal of

Environmental Protection, Global Journal of Analytical Chemistry andInternational Journal of Chemistry

Mr. Chris Badeen

Mr. Chris Badeen obtained his Masters degree in chemical engineering in 2000 from the University of Ottawa. In 2001, he joined the Research group at the Canadian

Explosives Research Laboratory, where he has used a variety of thermal analysis techniques to study energetic materials.



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Charles A. Potter, Ph.D.

Dr. Charles Potter is an analytical chemist with years of experience as a thermal analyst, calorimetry, and instrument development in the specialty chemical industry.

Having worked with everything from rocket motors to baby diaper and stability testing, Charles welcomes the opportunity to share diverse application of thermal analysis,

moisture sorption, and calorimetry.

Dmitriy V Soldatov, Ph.D.

Dr. Dmitriy Soldatov has almost 25 years of experience in thermal analysis and its applications in coordination, supramolecular and materials chemistry. He obtained his

MSc degree in inorganic chemistry from Novosibirsk State University, Russian Federation, in 1991. His PhD project, conducted at the Institute of Inorganic Chemistry (Russian Academy of Sciences, Novosibirsk) and the Institute of Physical Chemistry

(Polish Academy of Sciences, Warsaw), was sccessfully completed in 1995. After that Dmitriy led a research group at the Institute of Inorganic Chemistry, acquired

postdoctoral experience at the Steacie Institute, National Research Council Canada, and finally joined the faculty of the Department of Chemistry, University of Guelph in

2007, where he is now an Associate Professor. Dmitriy has nearly 100 publications in refereed jounals and editions, received several awards including Margaret Etter Award from the American Crystallographic Association (2001), serves as Executive Editor for

the Journal of Structural Chemistry (since 2006) and acts as Canadian contact for Cambridge Crystallographic Data Centre (since 2008).

E. Bradley Easton, Ph.D.

Dr. Brad Easton was born and raised in St. John’s, Newfoundland. He obtained both his B.Sc. (1998) and his Ph.D. (2003) in Chemistry at Memorial University of

Newfoundland. Easton then worked as an NSERC postdoctoral fellow at Simon Fraser University (2003 – 2004) and Dalhousie University (2004 – 2006). In 2006, he joined

Faculty of Science at UOIT where he is currently an Associate Professor of Chemistry and leads a research group in materials chemistry that prepares and characterizes new

materials with primary applications in electrochemical systems.



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Application of thermal analysis in sol-gel synthesis of mixed metal oxides having potential magnetic, electric and photoluminescence properties

Ranjit K Verma

University Department of Chemistry (DST-FIST Sponsored and UGC-BSR Supported), Magadh University, Bodh Gaya-824234 (India)

Ferrite, chromite and aluminate nanoparticles have tremendous application potentialities owing to their interesting magnetic, optical, electrical and catalytic properties. Out of the different synthetic options, the simpler sol-gel route has recently been tried using the citrate precursor method. A lower successful and more proper annealing temperature has been chosen on the basis of the TG-DSC data of the precursors and analysis of the latter taking multiple heating rate options for the kinetic trio. A comparative study of the precursors has been made before annealing, taking cobalt, copper, nickel, zinc, samarium and a few more metals as the “A” in ABO3 or the like materials obtained thereafter. XRD studies and their Rietveld refinements have been done besides SEM studies for understanding the particle nature and morphology. Coercivity, magnetization and photoluminescence studies indicate tremendous potentialities of the nanoparticles synthesized by such greener route. This establishes the importance of going for thermal analysis and calorimetry before opting for annealing in such cases.

Introduction and Applications of Thermal Analysis and Calorimetry

S. C. Mojumdar Department of Chemistry, University of Guelph, Guelph, ON, Canada

Department of chemical Technology and Environment, Trencin University of A. Dubceck, Puchov, Slovakia

Thermal Analysis (TA) provides testing for a wide range of materials including foods, medicine, thin films, glasses, ceramics, optical, electrical and construction materials, polymers, plastics, composites, laminates, adhesives, coatings, pharmaceuticals, various organic and inorganic materials, rubber, petroleum, chemicals, explosives, nanomaterials and biological samples. There are many thermoanalytical techniques such as thermogravimetric analysis (TG), high resolution thermogravimetric analysis (Hi-ResTM TG), derivative thermogravimetry (DTG), differential thermal analysis (DTA), thermometry, calorimetry, differential scanning calorimetry (DSC), modulated differential scanning calorimetry (MDSC), oscillating differential scanning calorimetry (ODSC), dynamic differential scanning calorimetry (DDSC), conduction calorimetry (CC), isothermal titration calorimetry (ITC), dynamic mechnical analysis (DMA),



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thermomechnical analysis (TMA), thermodilatometry (TD), dielectric thermal analysis (DEA), optical thermal analysis (OTA), thermally stimulated current (TSC), evolved gas analysis (EGA), emanation thermal analysis (ETA), thermomanometry, thermobarometry, thermoluminescence (TL), thermosonimetry or thermoacoustimetry, thermodiffractrometry, thermospectrometry, -thermal analysis (TA), nano-thermal analysis (Nano-TA), isothermal pressure transducer analysis (ITPTA), transient thermal analysis (TTA) and thermal conductivity (TC). Simultaneous thermal analysis (STA) is ideal for investigation of various issues such as the glass transition of modified glasses, binder burnout, dehydration of ceramic materials or decomposition behavior of inorganic building materials, also with gas analysis. Various TA and calorimetric techniques and their applications from medicine through nanotechnology to construction will be presented.

Kinetics from TG and DSC

Christopher Badeen Natural Resources Canada, Canadian Explosives Research Laboratory, 1 Haanel

Drive, Ottawa, Ontario K1A 1M1 Canada The speed at which chemical reactions occur is governed by the kinetics. In general, the kinetics of a chemical reaction are described by a rate equation that relates the degree of conversion of a reactant to the reaction rate. The rate equation is usually formulated as follows

( ) ( )

where is the degree of conversion, t is time, d / dt is the reaction rate, T is the absolute temperature, k(T) is the temperature-dependant rate constant and f () is a some function of conversion which is known as the kinetic model.

The temperature dependence of the reaction rate is typically modeled using the Arrhenius equation

( ) (

)

where Z is the preexponentional factor E is the activation energy, and R is the universal gas constant. The parameters Z, E, and f () are known as the kinetic triplet. Knowledge of the kinetic triplet allows the prediction the reaction rate and degree of conversion as a function of time and temperature, which has many practical applications.



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An introduction to several standard methods for obtaining kinetic parameters using Thermogravimety (TG) and Differential Scanning Calorimetry (DSC) will be provided. The concept and advantages of model-free kinetic analysis will be introduced and a method for obtaining the model-free kinetic parameter, a conversion-dependent apparent activation energy, E, will be presented. Potential pitfalls which must be avoided to in order to obtain meaningful kinetic parameters from TG and DSC data will be discussed.

Characterization of Thermosets by Modulated DSC®)

Kadine Mohomed and Charles Potter, TA Instruments, New Castle, DE USA

Thermosets are ubiquitous, from the epoxy resins in composites and adhesives, polyurethanes in cushions and shoe soles, polycyanurates, urea-formaldehyde resins, and many more. Differential scanning calorimetry (DSC) and temperature modulated DSC (MDSC®) are commonly used to characterize thermosets. The characterization can include the heat of cure, the extent of cure, the glass transition temperature, curing kinetics, and the complex changes in heat capacity during the curing process. Examples showing how DSC and MDSC® are used to provide a comprehensive characterization of epoxy thermosets will be shared.

Introducing New Fully-Integrated TGA-GC-MS and TGA-FTIR Systems for Characterization of Materials Including Polymers, Petrochemicals, Biomass and

More

Robert Pieper NETZSCH Instruments N.A., LLC, 129 Middlesex Turnpike, Burlington, MA 08103,

United States

Evolved Gas Analysis (EGA) is an ideal means for characterizing the thermal behavior of organic and inorganic solids or liquids in more detail and elucidating the chemistry behind them. This paper will focus on two new developments for evolved gas analysis including TGA-GC-MS and TGA-FTIR. The primary scope of fully-integrated TGA-GC-MS coupling is to detect, separate and analyze organic components. It is also possible to use the coupled GC-MS for detailed gas analysis to further improve the temperature-programmed pyrolysis of samples such as polymers and petrochemicals in the TGA or STA (Simultaneous DSC/DTA-TGA). The volatile products emitted during combustion processes can be determined with high sensitivity and resolution at various oxygen content levels. The fully-integrated TGA- FTIR system allows for analysis of decomposition, solid-gas reactions, compositional analysis, with the study of evaporation and outgassing.



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Review of Thermal Conductivity Methods

Adam Harris, Jarrett Nickerson and Robert Bateman

C-Therm Technologies Ltd., 921 College Hill Rd, Fredericton, NB

A general review of thermal conductivity methods will be presented covering the points of difference, "pros & cons", and theory behind the various methods available. The presentation will offer excellent primer for those newer to thermal analysis trying to get a handle on the various thermal conductivity methods. A comparison of traditional steady state techniques (guarded hot plate & guarded heat flow) and newer transient methods including: laser flash diffusivity, traditional transient plane source and the modified transient plane source will be offered. No single technique can do it all - learn where and when to apply the various methods in gaining a better understanding of their capabilities and limitations.

Examples of Advantages of 'Multi-Curve' Experiments

Melanie Nijman Mettler-Toledo AG, Business Unit Analytical, Sonnenbergstr. 74, 8603 Schwerzenbach,

Switzerland

Often, a single DSC measurement does not give the complete information about the sample being analyzed. The sample might e.g. change its structure or composition during the experiment, or undergo a chemical reaction. This presentation illustrates the benefits of multiple heating – cooling – heating segments for samples measured in DSC. We will also show examples where the use of different heating and cooling rates is beneficial.

To further increase the understanding of sample behavior one sometimes has to use also other thermal analysis techniques. Several examples will be shown for materials measured with multiple thermal analysis techniques.

Thermal Analysis of Soft Materials and Heat-Induced Chemical Reactions

D. V. Soldatov Department of Chemistry, University of Guelph, Guelph, Ontario, Canada

The term "soft materials" refers to bulk materials where molecular components

link weakly through non-valent interactions: van der Waals forces, hydrogen bonds, weak coordination, etc. The non-valent character of bonding results in a potential multitude of crystalline or non-crystalline forms for the same composition and low temperature limit for their existence. Therefore, thermal analysis at relatively low temperatures can reveal polymorphous transitions, congruent and other types of



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melting, dissociation or sublimation, gelation, glass transitions, and thus can help identify the stability limits of such materials.

Molecular crystals, inclusion compounds, co-crystals, organic and supramolecular polymers and many other types of soft materials can be studied with thermal analysis methods. Examples of such studies will be illustrated. A special attention will be given to recent examples from our own group where thermoanalytical methods were used to follow chemical transformations occurring in the soft materials in the solid state.

The use of thermal analysis in the development of novel fuel cell materials

E. Bradley Easton Faculty of Science (Chemistry), University of Ontario Institute of Technology

Oshawa, ON Canada L1H 7K4

Energy production is one of the most critical problems facing our global society. This problem requires new sources of energy to be both clean and efficient. There are several electrochemical technologies that have the potential to meet these demands. However significant fundamental scientific challenges must be overcome before these technologies can become viable. In general, all these challenges are related reducing cost without sacrificing the required performance. Many of these technologies rely on either costly materials (e.g., Pt) or simply cannot achieve the required performance and durability needed for widespread implementation.

Our research is focused on the development of new materials and methods for fuel cell systems, with possible application in other energy and sensory technologies. Materials of interest include both inorganic-organic hybrid materials based on siloxane copolymers formed through sol-gel chemistry, as well as surface functionalized carbon materials. We design and prepare these novel materials with specific properties that can either address or provide insight into these challenges. For example, we have created a series of Pt-transition metal alloy catalysts with enhanced activity for ethanol oxidation. In addition, we have employed functionalized silica materials to enhance the performance of membrane and electrode materials for use in H2/O2 fuel cells and hydrogen generation technologies.

One of our most useful non-electrochemical tools is our thermal analyzer. Thermal analysis is performed extensively for the determination of composition and thermochemical properties of our new materials. In this presentation, I will give an overview of the development of novel membrane and electrode materials and demonstrate how performance and composition are related, aided in part by the use of thermal analysis measurements.



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Thermodynamic Modelling of Inorganic Compounds in Aqueous Process Solutions

Vladimiros G. Papangelakis

University of Toronto, Dept. of Chemical Engineering and Applied Chemistry, 200 College Street, Toronto, ON, Canada M5S 3E5

Solubility measurements of inorganic compounds in aqueous solutions are used

to evaluate the performance of chemical models describing equilibrium conditions. They are also used to develop databases of model-specific parameters that allow modeling of solution chemistry, including solubility, under conditions outside the range of parameterization. Challenges develop when models developed on simple two or three- component systems are extended to multicomponent systems such as those encountered, for example, in the metals and minerals process industry. Hydrometallurgical processing deals with selective extraction of metals from natural or recycled resources by using aqueous solutions often dictating operation under aggressive conditions and temperatures from room to as high as 270 °C. The Mixed Solvent Electrolyte (MSE) model embedded in the OLI Systems software provides a self-consistent and reliable platform to model such aqueous processing systems. Examples from the use of the MSE model in two cases of industrial relevance are presented. The first example involves an experimental and theoretical investigation of calcium sulphate solubility in relation to scale formation in industrial reactors and the second example is taken from the nickel production industry and involves the optimization of sulphuric acid addition and control in autoclave reactors at 250°C.

Using the Iso-Conversional Model to Identify Growth Modes of a Lipid Network

Suresh S. Narine Departments of Physics & Astronomy and Chemistry, Trent University,1600 West Bank

Drive, Peterborough, Ontario, K9J 7B8, Canada

Lipids crystallise in metastable states, and the crystallization energetics can result in significant changes to the growth mode of the resulting lipid network. There are a number of mechanisms available to a crystallizing melt for growth of the network, and these growth mechanisms can be selected by altering the kinetics of growth. Furthermore, the growth modes that are defined can result in significantly different physical functionality of the finished network, which may be manipulated by the lipid processor to deliver unique performance characteristics of lipid-containing products. Theoretical underpinnings for the existence of different growth mechanisms will be presented, as well as kinetic and thermodynamic studies on a number of pure and complex lipid ensembles which provide convincing evidence for the existence of critical kinetics which select for specific growth modes.



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Chemical Modeling Aqueous Process Systems Using OLI

Michael Carlos and Vladimiros G. Papangelakis Department of Chemical Engineering and Applied Chemistry, University of Toronto, 200

College Street, Toronto, Ontario M5S 3E5, Canada

OLI Analyzer is a software package that uses the powerful Mixed Solvent Electrolyte (MSE) model capable of performing simulations of multicomponent electrolyte solutions from infinite dilution to the limit of fused salt, and from temperatures below the freezing point up to near critical temperature of the mixture. This speciation-based model offers reliable simulations by fully addressing speciation equilibria while solving simultaneously for complex phase equilibria. The thermodynamic framework of the OLI Analyzer involves the use of the Helgeson-Kirkham-Flowers-Tangers (HKFT) equation of state to estimate the standard state chemical potential of ions and aqueous species at wide temperature and pressure ranges coupled with the Mixed Solvent Electrolyte activity coefficient model. This communication reviews the basics of the model and provides some examples of modeling aqueous processing applications including selective extraction of metals from natural resources using MgCl2 brines which allow the recovery of expensive HCl and provide improved acid activity. The second example presents modeling results for iron rejection from high temperature processing of natural ores. Specifically, solubility modeling of iron as either hematite (Fe2O3) or sodium jarosite (NaFe3(SO4)2(OH)6) compounds and the influence of solution chemistry on the extent of iron removal is discussed.

Thermally Induced Intramolecular Condensation in Solid Leucyl-Alanine

F. I. Ali, D. V. Soldatov Department of Chemistry, University of Guelph, Guelph, Ontario, Canada

Solid state organic synthesis is a future alternative to traditional, solution-based

laboratory and industrial synthetic procedures. Solvent-free synthetic methods may contribute to green economy by reducing pollution, cutting the consumption of energy, and lowering the cost of production of various organic compounds. Although solid state reactions have been reported for almost all main classes of organic compounds and reaction types, solid state reactivity of peptides remains practically unexplored.

In this study, a thermally induced intramolecular cyclization of the leucyl-alanine dipeptide was studied. The reaction was conducted in a range of conditions using either ventilation oven or thermogravimetric analyzer. The observed mass loss corresponded to the release of one mole of water per one mole of dipeptide, as expected for a condensation reaction. After heating, the samples were tested with NMR spectroscopy



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and X-ray diffraction methods to identify the products and to estimate the yield and stereospecificity of the reaction.

Upon mild heating, the main product of the reaction cyclic leucyl-alanine was seen in the same absolute configuration as the initial dipeptide, but displayed an extensive polymorphism. Three crystal forms were identified with powder X-ray diffraction method. Two of the forms were isolated by crystallization and studied with single crystal X-ray diffraction analysis. Finally, the relative stability of the forms was investigated with DSC. Strong heating caused racemization of the cyclic product.

Misinterpretation of Cure Data Analysis in Epoxy-Based Nanocomposites

Geoff Rivers1, Allan Rogalsky1, Pearl Lee-Sullivan1 and Boxin Zhao2 1Department of Mechanical and Mechatronics Engineering, 2Department of Chemical

Engineering, University of Waterloo, 200 University Avenue, Waterloo, Ontario, Canada N2L 3G1

A literature review was conducted to determine the current understanding of the impact of silver, graphene and boron nitride nanoparticles on the curing behavior and glass transition temperature (Tg) of epoxy-based conductive nanocomposites. The majority of studies limit their cure analysis to a statement of the final Tg for a single composition. From these we are unable to draw conclusions. More useful studies provide a comparison of Tg across compositions and/or Tg of the neat matrix material. Among these, the nanoparticle effect is often overshadowed by the presence of residual solvent resulting from the common practice of adding nanoparticles as a suspension. Although the data is too sparse for strong conclusions, reductions in Tg seem to correlate with known residual solvent or mild degas conditions (i.e., low temperature, short duration), while increases are more likely when no solvent is used or after rigorous degas. This result is supported by our own experiments. If solvent must be used, we recommend that residual solvent content be quantified, and the Tg determined of a control sample with a representative solvent content and no nanoparticles. From the few studies that include representative controls or cure kinetics data, two conclusions can be drawn: i) nanoparticle surface chemistry has a significant effect; and ii) poor dispersion / aggregation results in a reduction in Tg.

The Curie Point Method for TGA Temperature Calibation

Charles Potter TA Instruments, New Castle, DE USA

For over 30 years, the Curie point method has been used to calibrate and verify the thermometric response of thermogravimetric analyzers (TGA). Certified and tracable Curie point materials, for this purpose, are readily available. But what experimental



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factors influence the Curie point materials and the thermometric response of a TGA? Experimental conditions, such as heating rate, sample size, purge gas type, and magnetic field strength will be discussed. For analysts using the Curie point method for performance verification, what is you day-to-day thermometric repeatability?

Standard Partial Molar Properties of Adenine and its Ions in High Temperature Aqueous Systems and Relevance to Modeling the Origins of Life

Alexander R. Lowe, Jenny S. Cox, and Peter Tremaine

University of Guelph, Dept Chemistry, 50 Stone Road East Guelph, Ontario, N1G 2W1

Apparent molar volumes, Vϕ, of aqueous solutions of adenine and adenine hydrochloride have been measured at temperatures from 15 to 90 oC under atmospheric pressure using an Anton Paar vibrating tube densitometer. Values for the aqueous adenine monosodium salt were measured from 10 to 40 oC. Apparent molar heat capacities, Cp,ϕ, of the identical solutions have been measured over the same temperature ranges at a pressure of 0.30 MPa using a fixed cell, power-compensation differential output, temperature-scanning calorimeter. Due to the solubility limits of adenine, these measurements required operating with extreme care near the detection limits of the densitometer and nanocalorimeter. The averaged values of these measurements yield temperature-dependent partial molar volumes, V°, and heat capacities Cp°, which can be extrapolated to hydrothermal conditions using the “HKF” and other equations of state. The molality and temperature dependent chemical shifts of neutral adenine, measured using a Bruker 600 Ultrashield NMR spectrometer, were used to calculate the equilibrium constant KA and enthalpy of the self association reaction. Using literature data for the ionization constants of the anionic and cationic forms of adenine, as well as V° and Cp° of HCl and NaOH, values of ΔrV° and ΔrCp° for the ionization and self association reactions of adenine are reported for the first time. These values can be used in thermodynamic models to predict the equilibrium distribution between adenine and its ions in deep ocean hydrothermal systems, in efforts to develop models for prebiotic chemistry and the origin of life.

Reaction Kinetics and Mechanisms of the Thermal Decomposition of Copper Chlorides and Oxides

Zhaolin Wang1, Gabriel Marin2, Greg Naterer3, Kamiel Gabriel4 1, 4 Faculty of Engineering and Applied Science, University of Ontario Institute of

Technology, 2000 Simcoe St N, Oshawa, Ontario, Canada, L1H 7K4. 2 Colorado Salt Products, 3910 Joliet St, Denver, CO, 80239.

3 Faculty of Engineering and Applied Science, Memorial University of Newfoundland, St. John’s, Newfoundland, Canada, A1B 3X5.



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The decomposition of copper oxychloride is the oxygen production process in the copper-chlorine thermochemical water splitting cycle for sustainable hydrogen production. The decomposition temperature, kinetics and mechanisms have a significant influence on the design, operation and economics of the cycle. In this paper, a simultaneous differential scanning calorimetry and thermogravimetric analysis (DSC / TGA) technique is used to determine the reaction temperature, kinetics and mechanisms of the thermal decomposition of a copper oxychloride compound, CuOCuCl2, and the mixture of CuO and CuCl2. The decomposition kinetics and mechanisms of CuOCuCl2 were deduced from the decomposition of CuCl2 and the mixture of CuO and CuCl2. The time-dependence of the mass change and heat flow in the decomposition process of CuCl2 was monitored with the DSC / TGA instrument. It was found that the CuCl2 decomposition temperature and kinetics are similar to the counterparts of the CuOCuCl2, indicating that the limiting step in the decomposition of the CuOCuCl2 is the CuCl2 decomposition. It is also concluded that the decomposition of the single compound CuOCuCl2 experiences two microscopic pathways, i.e., decomposition of CuCl2 for the release of Cl2, and then the Cl2 reacts with CuO to produce O2. The kinetics of CuCl2 decomposition determines the extents to which the CuOCuCl2 decomposition occurs, and impacts the overall efficiency of the cycle. The decomposition kinetics of CuOCuCl2 is modeled with the decomposition data of the mixture of CuO and CuCl2.

Standard partial molar heat capacities of aqueous aluminate under hydrothermal conditions from integral heat of solution experiments.

Y. Coulier and Peter R. Tremaine

Department of Chemistry, University of Guelph, 50 Stone Road East, GUELPH ON, N1G 2W1 Canada

Thermodynamic data for aqueous systems aluminum species are required to model the chemical equilibrium processes under hydrothermal conditions in a variety of systems for geochemical and industrial applications. Standard partial molar heat capacities and volumes are required to calculate the temperature and pressure dependence of the equilibrium constant and to advance the development of predictive models [1]. This study is aimed at determining standard partial molar heat capacities for the aqueous aluminate ion, Al(OH)4-(aq), by measuring the enthalpy of solution of sodium aluminate, NaAlO2(s), in aqueous sodium hydroxide solutions as a function of temperature. Heats of solution of NaAlO2(s) in aqueous solutions of sodium hydroxide (m = 0.12 and m = 0.2 mol•kg-1) were measured using a Tian-Calvet heat-flux calorimeter (Setaram, Model C80) from 100 to 275°C over a range of aluminate concentrations from 0.04 to 0.1 mol•kg-1. Standard molar enthalpies of solution, ΔsolnHo were determined from the experimental enthalpies by extrapolation to zero ionic strength. The temperature dependence of the standard molar heat of solution yields the standard partial molar heat capacity of reaction, ΔsolnCpo = (∂ΔsolnHo/∂T)p,



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from which values for the aqueous complex, Cpo[A1(OH)4-,aq] were calculated. Results from these calorimetric measurements are compared with the experimental values available in the literature [2-4] and with earlier predictions of the temperature dependence of the thermodynamic properties of A1(OH)4-(aq) [5].

References [1] E. L. Shock, D. C. Sassani, M. Willis, D. A. Sverjensky, Geochim. Cosmochim. Acta, 61, 907-950 (2007) [2] P. Caiani, G. Conti, P. Gianni, E. Matteoli, J. Solution Chem., 18, 447-461 (1989)

[3] Q. Chen, Y. Xu, L. G. Hepler, Can. J. of Chem., 69, 1685-1690 (1991) [4] S. Schrodle, Eric Konigsberger, P. M. May, G. Hefter, Geochim. Cosmochim. Acta, 74, 2368-2379 (2010) [5] J. K. Hovey, L. G. Hepler, P. R. Tremaine, J. Phys. Chem., 92, 1323-1332 (1988)

Modification of a DSSC photoanode with carbon nanotubes and TiO2 nanoparticles with different morphology

Simone Quaranta, Donald McGillivray, Liliana Trevani and Franco Gaspari

Faculty of Science, University of Ontario Institute of Technology

In this work, the photocatalytic activity of TiO2 nanoparticles with different morphology without and with the addition of multiwalled carbon nanotubes (MWCNTs) was investigated using the photodecomposition of methylene blue in aqueous solution. The most photoactive materials were used to prepare photoanodes and tested in a dye sensitized solar cell configuration. TiO2 and TiO2/MWCNTs materials were prepared using two alternative synthetic approaches: a sol-gel method in an organic media and a sol-gel supercritical aided route. The materials were characterized using X-ray diffraction, scanning electron microscopy, Raman spectroscopy and FTIR. Because of the multiple thermal treatments involved in the preparation of the materials and in the DSSC’s assembly step, thermal analysis has played a significant role in the overall project, particularly in finding the optimal conditions for each thermal step. The energy conversion efficiency of the DSSCs was evaluated by the I-V curves under sun simulator illumination. Electrochemical impedance spectroscopy was also used to examine the effect that different morphologies and CNTs have on the electron transport and recombination processes.



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Evaluating the activity and durability of Pt-based fuel cell catalysts

Farhana S. Saleh and E. Bradley Easton Faculty of Science, University of Ontario Institute of Technology, 2000 Simcoe Street

North, Oshawa, Ontario, Canada L1H 7K4

PEM fuel cells are promising power sources for stationary, portable and automotive applications. One essential component of determining the efficiency of PEM fuel cell is the catalyst. The efficiency of the catalyst is strongly correlated with monodisperse catalyst nanoparticles typically less than 3 nm, and a uniform distribution of these Pt nanoparticles on a carbon support, which can depend greatly on the deposition method employed. Another important factor is the choice of supporting material, since it surface characteristics greatly influences adhesion and dispersion of catalysts. Furthermore, the support must also have low electrical resistivity for efficient electron transport. Because of this, carbon nanotubes (CNTs) could potentially be an ideal support. However, for many applications it is necessary to functionalize CNT surfaces in order to achieve proper dispersion and obtain higher performances. Here we describe the microwave-assisted deposition of Pt onto activated multi walled carbon nanotubes (MWCNTs). The synthesized catalysts were characterized using thermogravimetric analysis (TGA), Transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and Raman spectroscopy. We also studied how the various processes of activation of MWCNTs influenced their electrochemical performance. In addition, the long-term durability of these catalysts was assessed using a simple accelerated testing protocol along with electrochemical impedance spectroscopy measurements.

Analysis of Metastable Materials at high heating rates

Melanie Nijman Mettler-Toledo AG, Business Unit Analytical, Sonnenbergstr. 74, 8603 Schwerzenbach,

Switzerland

The METTLER TOLEDO Flash DSC 1 is the first commercial chip-DSC allowing heating rates up to 2 400 000 K/min and cooling rates up to 240 000 K/min. With such an instrument one can analyze reorganization processes that were previously impossible to measure. The Flash DSC 1 is an ideal complement to conventional DSC. Using DSC 1 and FDSC 1 one can now cover a range of more than 7 decades.

Amorphous isotactic polypropylene (iPP) is produced by cooling from the melt at 4,000 K/s. The material obtained was measured at heating rates between 5 K/s and 30,000 K/s. The glass transition occurs just below 0 °C followed by an exothermic peak due to cold crystallization. The crystallites melt above 100 °C. At higher heating rates, the cold crystallization peak is shifted to higher temperatures and the melting peak to lower temperatures. With heating values above 1,000 K/s, the peak areas become



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significantly smaller until at 30,000 K/s cold crystallization and subsequent melting no longer occurs in the sample.

Examples of other metastable materials will be discussed in detail as well. Examples will be shown of the influence of sample size on the material behavior, of possibilities to distinguish materials directly from manufacture with a first heating run measurement, and for separation of effects normally overlapping at standard heating rates.

High-Pressure Thermal Conductivity Characterization of Materials

Adam Harris, Jarrett Nickerson and Robert Bateman C-Therm Technologies Ltd., 921 College Hill Rd, Fredericton, NB

The capability to understand the effective thermal conductivity of materials under

high pressure conditions is increasingly important to the oil and gas industry, particularly as it relates to gas hydrates. Gas hydrates offer tremendous potential as a possible hydrocarbon resource but also have significant potential impact in offshore drilling exploration. This paper focusses on the design of a High Pressure Cell (HPC) for use in the characterization of solids and liquids under high pressure conditions up to 134 bar. The HPC couples with the TCi Thermal Conductivity Analyzer in offering researcher expanded capabilities to test the effective thermal conductivity of various materials at elevated pressures via the modified transient plane source technique.

Multi-Length-Scale Structural Elucidation of Mechanism Responsible for Inhibiting FAME Crystallization

Athira Mohanan, Laziz Bouzidi and Suresh S. Narine

Trent Centre for Biomaterials Research, Departments of Physics and Astronomy and Chemistry, Trent University, Peterborough, Ontario, K9J 7B8

Unsaturated triacylglycerols (TAGs), particularly those with cis unsaturated fatty

acids at the sn-1 and sn-3 positions and a trans/saturated fatty acid at the sn-2 position, have been found to significantly reduce the crystallization onset of saturated fatty acid methyl esters (FAMES) at low loading. Detailed microstructure and crystal structure analyses by PLM and XRD of a model binary system made of 1,3-dioleoyl-2-palmitoyl



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glycerol (OPO) and methyl palmitate (MeP) were conducted in order to elucidate the mechanism of crystallization inhibition at drastically different length scales. Both the crystal structure and the microstructure of crystallized MeP were found to be profoundly disrupted by the TAG. The mechanism is proposed to be a limitation to growth of the FAME crystal lattice or a nucleus being formed in the melt due to the participation of the saturated fatty acid of the TAG in the crystal lattice or in the lamellae of a forming nucleus of the FAME, and the highly kinked cis unsaturated fatty acids also present on the TAG preventing any further packing of a similar nature. This both results in a disruption of the growth of the crystal as well as limitation of nucleation in the liquid melt due to a disruption of the growth of a forming nucleus into a size which is thermodynamically favourable for growth.

Investigating the Stability of Linear Diesters Derived from Vegetable Oils: Dependence on the β-Hydrogen and its Environment

Latchmi Raghunanan and Suresh S. Narine

Trent Centre for Biomaterials Research, Departments of Physics and Astronomy and Chemistry, Trent University, Peterborough, Ontario, K9J 7B8

Diesters derived from vegetable oils may be used in oleochemical syntheses, polymer syntheses, or lubricant formulations. Thermal stability is one of many physical properties which influence its suitability for an application. Herein, a novel series of linear symmetric diesters have been investigated to determine the effect of structure on thermal stability. FTIR and 1H-NMR have been used to show that ester groups in close proximity to each other result in a weakening of the C-O-C bonds and an increasing lability of the α- and β- hydrogens. These results imply that diesters whose ester groups are located closest to each other are the most destabilized. The most stable diesters were therefore obtained when the ester groups were furthest apart; no substantial increase in stability was observed past a distance of six-carbon atoms between the ester groups. A similar n-dependence of the thermal stability of the diesters was absent, indicating that the thermal stability of the diesters was not limited by intramolecular bond stability. Instead, a linear increase in weight loss temperatures with increasing n suggests that the diesters undergo high-temperature phase change. The latter was supported by TGA kinetic studies obtained using the Friedman isoconversional method.

Keywords: Thermal stability; diesters; β-hydrogen; thermogravimetric analysis; Friedman method; isoconversional analysis.



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Vegetable Oil Derived Lubricants: Improvement of Thermal Properties by Structural Modifications

Laziz Bouzidi, Latchmi Raghunanan, Shaojun Li and Suresh Narine

Trent Centre for Biomaterials Research, Departments of Physics & Astronomy and Chemistry

Trent University, 1600 West Bank Drive, Peterborough, K9J 7B8, Ontario Canada

Increasing environmental and sustainability concerns are driving research efforts towards the development of high - performance non-toxic biodegradable lubricants, waxes and gels from renewable sources. In this regard, the Trent Centre for Biomaterials Research is investigating a series of novel materials sourced from renewable feedstock such as vegetable oils and their derivatives to enable custom engineering and delivering optimal physical properties. The present study focuses on jojoba wax ester analogues, more than 46 model systems never investigated before, particularly suitable for use in high-grade lubricating oil formulations and additives as well as for a variety of other high-end wax and gel applications such as cosmetic and medical formulations, and foods. We have examined the structure - function relationships of linear mono- and di-esters and their branched derivatives produced from inexpensive renewable resources, i.e., fatty acids. A wealth of information have been gained on the influence of chain length, branching, symmetry, and functional groups on the physical properties such as crystallization, melt, polymorphism, solid fat content and flow behavior. The findings highlight relatively simple, inexpensive lipid- derived molecules with astonishingly low onsets of crystallization, and predictive structure – property relationships which are very promising in the formulation of renewable superior lubricants.

Synthesis, Characterization and Thermal Analysis of the 1st row Transition Metals:

Part-I: Oxalate Hydrazinate Complexes

Yogita U. Jambalekar, Satish A. Tarale, Suraj M. Sutar , Santosh P. Chougule, R. M. Babshet and K. S. Rane

BK College, Jyoti College Campus, Club Road, Belgaum, Karnataka, India

Part-II: Formate Hydrazinates

Surekha S. Hadnur, Saroja U. Nemagouda, Mallikarjun S. Yadawe and K. S. Rane

SB Arts and KCP Science College, Bijapur, Karnataka, India $ Rani Channamma University, Belgaum-591156, Karnataka, India



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A versatile hydrazine, N2H4, a rocket fuel and its hydrated form, N2H4·H2O, a universal oxygen scavenger to control the concentration of the dissolved oxygen in the boiler feed water to reduce the corrosion finds use to prepare the gas precursor, a metal hydrazine complex such as iron oxalate hydrazinate and iron nitrate hydrazinate for air bags where it behaves as a ligand. A nickel hydrazine nitrate, Ni(N2H4)3(NO3)2, is a lead free potential primary explosive for use in detonators. The potentiality of such a multipurpose hydrazine has been advantageously utilized by us in the synthesis of variety metal transition and rare earth carboxylate hydrazine complexes in the low temperature synthesis of nano-to submicron metal oxides [1-3] of narrow particle size distributions. In order to enhance the oxygen scavenging action of hydrazine cobalt salen hydrazine complex, [Co(C16O2H14N2)(N2H4)] has been synthesized [4]. And our experience says that it is the preparation technique and thermal analysis which are crucial in exploiting the potential of the metal hydrazine complexes. Metal hydrazine complexes are, in general, synthesized by solution method, but we found metal carboxylates prepared by standard method and equilibrated with hydrazine vapor in a reactor on decomposition yields superior quality metal oxides. Thermal path too gets modified. Thermal analysis the 1st row transition metal oxalate hydrazinates and formate hydrazinates prepared by solution method have been reported [5,6]. We are reporting here in the Part-I the results of the thermal analysis of the 1st row transition metal oxalate hydrazinates by the equilibrium method and that in the Part-II the formate hydrazinates.

References

1) ” The low temperature synthesis of metal oxides by novel hydrazine method ”, K. S. Rane, H. Uskaikar, R. Pednekar and R. Mhalsikar Journal of Thermal Analysis and Calorimetry, 90 (2007) 3, 627-638.

2) “ Innovative use of thermal techniques in aerosolized simple metal oxide precursors “, K.S.Rane, S. Basak, V. Borker, M. Shirodkar, Pratim Biswas, Proceedings of Indian Thermal Analysis Society of India, THERMANS-2008, Indiara Gandhi Centre for Advanced Research (IGCAR), Kalpakam, Feb.2008, India.

3) “Hydrazine-Assisted, Low-Temperature Aerosol Pyrolysis Method to Synthesize γ-Fe2O3”, Soubir Basak, Koyar S. Rane, Pratim Biswas, Chemistry of Materials, 20 (2008) 4906–4914.

4) Metal complexes as catalysts in enhancing oxygen scavenging action of hydrazine in boiler feed water: Part I and Part-II-Cobalt complexes, Sifali S. Bandodkar and K.S.Rane Proceedings of the 7th National Conference on Solid State Chemistry and Allied Sciences, ISCAS, New Delhi, November 24-26 2011

5) “Thermal reactivity of metal oxalate hydrazinates”, K.C. Patil, D. Gajapathy and K.Kishore, Thermochimica Acta, 52(1982)113-120

6) “Thermal reactivity of metal formate hydrazinates”, P. Ravindranathan and K.C.Patil, Thermochimica Acta, 71(1983)53-57



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Abstracts of Posters

Structure and Stability of Solid Oligoglycines

A. J. Smith and D. V. Soldatov Department of Chemistry, University of Guelph, Guelph, Ontario, Canada

Recent studies in our group suggest that molecular-size voids in crystalline

peptide matrices can be used as molecular containers and, possibly, nano-size reactors. It is important therefore to understand the stability limits and decomposition pathways of the peptide matrix itself, and especially the dependence of these properties on the composition, size, conformation and mutual arrangement of peptide molecules that build the molecular crystal.

In this work, a series of crystalline glycine-based oligopeptides, linear (Gly)n with n = 1 to 5, was studied. Single crystals of tetra- and pentaglycines were grown from aqueous solutions and investigated with X-ray diffraction analysis, while the crystal structure of the lower oligomers and monomeric glycine known from the literature. The molecular and crystal structure of oligoglycines in the series was compared in order to track the trends as a function of the number of amino acid residues.

The bulk samples of the same crystalline oligoglycines were examined with TGA-IR technique to evaluate their thermal stability limits and modes of decomposition. The thermal stability was related to the molecular structure and conformation of the molecules in the solid state, size of the molecule and charge separation in the zwitterionic form, and arrangement of the molecules in the crystal.

Study of the Oxidation Enthalpy of Pyrite

S. C. Mojumdar, I. Bylina and V. G. Papangelakis Department of Chemical Engineering and Applied Chemistry, University of Toronto,

200 College Street, Toronto, Ontario, Canada M5S 1A4

Pyrite is associated with other sulphide minerals, which are major carriers of base metals such as nickel, copper and zinc. In the metals industry is often subject to oxidative dissolution under oxygen pressure is aqueous solution at elevated temperatures in pressure vessels, by a process that is known in the field of hydrometallurgy as Pressure Oxidation. In the industrial practice, the oxidation of pyrite and its polymorph marcasite during storage under normal atmospheric conditions prior



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to Pressure Oxidation is also a known but not well-studied process. The purpose of this study was to evaluate the heats of oxidation of freshly ground vs. stored (for a year in contact with air) pyrite by calorimetric measurements. The amount of the heat evolved under Pressure Oxidation conditions is important for the heat balance and optimization of the autoclave design in the hydrometallurgical industry. The present study was performed with a Setaram DSC80 equipped with a commercial mixing cell on pure pyrite mineral particles (Valdenegrillos, Spain) at 150 ºC and partial oxygen pressure of 3.4 MPa. A calorimetric method for determining the enthalpy of Pressure Oxidation of sulfide minerals has been used to evaluate the enthalpies of oxidation of freshly ground as well as stored pyrite. Ground pyrite stored over time has long since been known to result in greater heat evolution during oxidative leaching. A likely mechanism for this phenomenon was uncovered: formation of ferrous sulfate and sulphuric acid during storage in contact with air influencing greater heat evolution at the outset of the reaction. Simultaneous TG-DSC on a Q600 from TA Instruments has also been used to determine oxidation product FeSO4.H2O and study the thermal stability of the pyrite and stored pyrite.

Thermal Analysis of Pt-Mn Alloys to Find the Most Effective Temperature for Heat Treatment and Enhancing the Ethanol Oxidation in PEM Fuel Cell

M. R. Zamanzad Ghavidel and E. Bradley Easton

Faculty of Science (Chemistry), University of Ontario Institute of Technology, 2000 Simcoe St. N., Oshawa, ON, Canada L1H 7K4

Increasing catalytic activity while also decreasing the cost associated with Pt-based catalysts is a major research challenge related to direct alcohol fuel cells (DAFC). Our previous studies have shown that Pt-Mn alloys display high ethanol oxidation reaction (EOR) activity, particularly those that are richer in Mn. However, thermogravimetric analysis (TGA), Raman scattering and x-ray diffraction (XRD) results showed that the deposits did not have uniform structure and that inactive Mn oxide phases were also present. Subsequently we have studied high temperature heat treatment and how it affects the structure and EOR activity. TGA data showed that several phase transitions occur at different temperatures. DSC results indicate that most of these transitions are endothermic except the carbon black lost at ~350oC. Additionally, the results displayed that the amount of Pt effects phase transition temperatures. By increasing the Pt content, the transition temperature shifted to lower temperature. Based on the TGA results, samples were annealed at 500, 700, 875 and 950oC for 1 hour in an inert atmosphere. The results indicated that the grain size was enlarged by increasing the temperature and the EOR activity decreased with heat treatment temperature up to 700oC. However, at 875oC the EOR was greatly enhanced, showing higher activity than



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the untreated samples. XRD analysis indicated that at 875oC a more ordered Pt-Mn intermetallic phase was formed which it is responsible for the EOR greater activity.

Performance of Composites with Metakaolin-Blended Cements

Ľudovít Krajči, Subhash C. Mojumdar, Ivan Janotka, Francisca Puertas■, Marta Palacios, Marta Kuliffayová

Institute of Construction and Architecture, Slovak Academy of Sciences, Dubravska cesta 9, 845 03 Bratislava, Slovakia

University of Guelph, Department of Chemistry, Guelph, ON, Canada, E-mail: [email protected]

Building Testing and Research Institute, Studena 3, 821 04 Bratislava, Slovakia, ■Eduardo Torroja Institute for Construction Sciences, IETcc-CSIC, Serrano Galvache 4,

280 33 Madrid, Spain Swiss Federal Institute of Technology Zürich, Institute of Building Materials,

Schafmattstraße 6, 8093 Zürich, Switzerland

Nowadays the blended cements acquire the merit of high significance due to the thermal, energetic and ecological demands for ordinary Portland cement (OPC) production. Metakaolin as a partial substitute of OPC represents important pozzolana contributing to production of effective cement composites with high quality. Pozzolanic reaction of metakaolinite with OPC in the presence of water is main reason of this statement. Comparison of three sorts of metakaolin sand (fineness below 60 μm) with different metakaolinite content (31-40 %) is presented in this study. The substitution of PC with metakaolin sand of the maximal metakaolinite content (40 %) leads to the highest compressive strengths of relevant composites. This is valid for composites with the highest substitution of PC by metakaolin sand in specimens (20 and 40 wt.%). The best effectiveness of pozzolanic reaction is given especially by the highest consumption of portlandite which represents composite with the maximal metakaolinite content in metakaolin sand (40 %) and the higher substitution level of PC by metakaolin sand in specimens. This fact is connected with the improvement of pore structure parameters resulting in the pore structure refinement as well as permeability decreases. Both 29Si MAS NMR and 27Al MAS NMR spectra of metakaolin sands and respective composites confirm the most intense pozzolanic reaction in the case of metakaolin sand with the highest metakaolinite content (40 %). The results are properly supplemented by scanning electron microscopy (SEM) identifying the formed typical phases. The study has shown that metakaolin sand with reduced metakaolinite contents is also applicable as a pozolanic addition to OPC in the on-coming building practice.

http://www.ctas.org/mailto:[email protected]


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Deposition of Silver Nanoparticles on Cellulosic Substrates for Biomedical Applications

Cassandra Scott, Liliana Trevani and Janice Strap

Faculty of Science, UOIT, 2000 Simcoe St N. Oshawa, ON, L1H7K4

Bacterial cellulose produced by Gluconacetobacter xylinus was impregnated with silver

nanoparticles using a Tollens type process. In this case, a [Ag(NH3)2]+ complex was

infused in bacterial cellulose and reduced using glucose as a reducing agent. The formation and average size of silver nanoparticles were determined by UV-Visible spectroscopy and scanning electron microscopy (SEM). Thermogravimetric analysis was used to determine the amount of water, as well as the loading of silver nanoparticles. These studies showed that the amount of silver loaded into the bacterial cellulose membranes depends on the glucose concentration. When the concentration of glucose relative to silver was increased, a blue shift in the visible spectrum absorption maximum was observed, indicating smaller particle size. The silver nanoparticle- impregnated cellulose was then dried under a vacuum and the dried cellulose was evaluated for antimicrobial properties against the gram-negative organism Pseudomonas aeruginosa.

The Investigation and Characterization of Next Generation Proton Exchange Membranes for Fuel Cell-Based Ethanol Sensors

Jesse T. S. Allan and E. Bradley Easton

Faculty of Science (Chemistry), University of Ontario Institute of Technology, 2000

Simcoe St. N., Oshawa, ON, CANADA L1H 7K4

Proton exchange membrane fuel cells (PEMFCs) are one of the most innovative and adaptable of fuel cell technology. One of the most important niches that PEMFCs have a proven commercial market is in sensory sensor devices. When configured for sensory operation the current produced in a fuel cell is proportional to how much fuel is passed through the device, one can take advantage of this as a sensor. If ethanol is used as the sample, it is possible to relate the current produced from an ethanol fuel cell to the concentration of ethanol used in the fuel. This type of sensing is most notably found in a breath alcohol sensor (BAS) commonly used to determine intoxication.

At the heart of the BAS is the proton exchange membrane (PEM). The goal of the PEM is to transfer protons from the anode to cathode. The PEM requires various characteristics to ensure adequate performance: high water-uptake, excellent conductivity and stability. Poly Vinyl Chloride (PVC) based materials impregnated with



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sulfuric acid are currently used in most state of the art commercial BASs. While PVC does show excellent conductive properties, it is known to dry out in low humidity environments. Consequently, there is a great desire to find alternative membrane materials for commercial applications.

The work presented here will look at what membrane properties have the greatest impact on BAS sensor performance. In particular, how relative humidity, aging and severe operating conditions affects the performance of the BAS, especially at low humidites (dry environments).

Examination of Ceramic Carbon Electrodes for Low Humidity Fuel Cell Applications

Jennie I. Eastcott and E. Bradley Easton

Faculty of Science (Chemistry), University of Ontario Institute of Technology 2000 Simcoe St. N., Oshawa, ON L1H 7K4

State-of-the-art electrodes for proton exchange membrane fuel cells contain platinum catalyst and a Nafion proton-conducting binder. Optimal conditions for Nafion functionality are at 80oC and 100% relative humidity (RH). Ceramic carbon electrodes (CCEs) may provide an alternative electrode structure by replacing Nafion in the catalyst layer with organosilane materials that have water retention capabilities. CCEs are also attractive as they have high surface area and a durable nature. We have determined that CCEs prepared with small quantities of sulfonated silane display a profound enhancement of catalytic activity and proton conductivity. Thermogravimetric analysis and BET analysis were used to determine composition and surface area, indicating that large quantities of sulfonated silane result in a detriment to surface area and pore size. MEAs prepared with CCE cathode catalyst layers were evaluated electrochemically alongside standard ELAT cathode layers at multiple relative humidities to compare performance in dry conditions. Examination of results from cyclic voltammetry, electrochemical impedance spectroscopy, and fuel cell polarization curves indicate that the CCE cathodes maintain performance and have improved water management capabilities at low %RH. Additionally, it is possible that maintaining high water retention in the cathode may promote membrane hydration and aid in fuel cell performance. An overview of electrochemical findings for both CCE and ELAT cathode catalyst layers will be presented.



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Physical and electrochemical properties of novel anode materials for use in the Cu-Cl thermochemical cycle for the production of hydrogen

P. E. Edge and E.B. Easton

Faculty of Science, University of Ontario Institute of Technology, 2000 Simcoe Street North, Oshawa, ON L1H 7K4

Current H2 gas supplies are primarily produced through steam methane reforming

and other fossil fuel based processes. This lack of viable large scale and environmentally friendly H2 gas production has hindered the wide spread adoption of H2 fuel cells. A potential solution to this problem is the Cu-Cl hybrid thermochemical cycle. The cycle captures waste heat to drive two thermochemical steps creating CuCl as well as O2 gas and HCl from CuCl2 and water. The CuCl is oxidized in HCl to produce H2 gas and regenerate CuCl2, this process occurs at potentials well below those required for water electrolysis. The electrolysis process occurs in a traditional PEM full-cell. In the aqueous anolyte media Cu(I) will form anionic complexes such as CuCl2 or CuCl3 The slow transport of these species to the anode surface limits the overall electrolysis process. To improve this transport process we have produced ceramic carbon electrode (CCE) materials through a sol-gel method incorporating a selection of amine containing silanes with increasing numbers of primary and secondary amines. When protonated these amines allow for improved transport of anionic copper complexes.

We will present the electrochemical and physical characterization of these CCE materials. Thermogravametric and differential thermal analysis was used to determine the relative amounts of organosilicate and carbon in the bulk CCE and scanning electron microscopy was used to assess the physical properties of the CCE’s. Electrochemical analysis was performed using cell polarization, cyclic voltammetry, and electrochemical impedance spectroscopy to determine the CCE’s potential for Cu+ oxidation.

Polymorphism of Guaiacol and Crystal Structure of the Trigonal Form

T. Fillion and D. V. Soldatov Department of Chemistry, University of Guelph, Guelph, Ontario, Canada

Guaiacol (ortho-methoxyphenol) is a naturally occurring compound with its

melting point close to room temperature (301 K). Guaiacol is a main component of many flavors and parent compound for a great family of aromas, flavors and pharmacologically important molecules, such as vanillin (vanilla), eugenol (cloves), zingerone (ginger), capsaicin (chili pepper) and apocynin (Canadian hemp). Surprisingly, the crystal structure of guaiacol has never been reported. Previous studies suggested the existence of at least two polymorphs that form when liquid guaiacol is frozen. Our earlier DSC experiments with guaiacol-containing samples revealed irreproducible results in the low-temperature region which were related to its polymorphism.

In order to further elucidate the polymorphism of guaiacol, we used variable temperature X-ray diffraction experiments on single crystals and frozen liquid samples



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of guaiacol. The crystals that form and exist at positive Celsius temperatures turned out to have a trigonal structure with three independent molecules in the unit cell. Cooling the trigonal crystal down to 100 K did not change the crystal structure. On the other hand, instantly frozen samples of liquid guaiacol revealed the formation of a glassy/amorphous solid. Slow annealing of these samples resulted to either the formation of the trigonal form or the formation of another, metastable polymorph. The metastable polymorph quickly transformed into the trigonal form once nucleation seeds of the later appeared in the samples. After multiple experiments, we located the melting point of the metastable polymorph at 2511 K.

Replication of Bacterial Cellulose Nanoarchitecture with Metal Oxide Catalysts Utilizing a Facile Supercritical Carbon Dioxide Aided Method

Nick-Hugh Wisdom, Andrew Vreugdenhil, Janice Strap and Liliana Trevani

Faculty of Science, University of Ontario Institute of Technology

Unlike plant based cellulose bacterial cellulose (BC) has a high degree of purity and crystallinity. The highly ordered tertiary structure consists of microfibrils which are cross- linked via an array of highly ordered hydrogen bonds. These hydrogen bonds impart significant mechanical strength to the cellulose membranes which make them attractive for a wide variety of applications such as filtration material, fuel cell proton exchange membranes and a myriad of other materials. The high porosity and specific surface area of cellulose aerogels derived from Bacterial cellulose alludes to its applicability as a scaffold for the synthesis of catalyst-polymer composites. The large amount of hydroxyl groups and surface adsorbed water makes BC a suitable substrate for the sol-gel synthesis of metal oxides. In this study the utility of the cellulose aerogels as a scaffold for the synthesis of TiO2 nano-rods and tubes. Field emission SEM results has indicated that cellulose aerogels derived from freeze drying results in sheets of agglomerated TiO2 nano particles whereas the aerogels derived from supercritical CO2 drying results in nano-rods and tubes with a good degree of uniformity. Thermogravimetric analysis was critical in determining the catalyst loading and will be a crucial in the optimization of the synthesis conditions in order to increase the yield. The photo-catalytic activity of the synthesized TiO2 particles was assessed by studying the effect on the photodecomposition of methylene blue. Preliminary results are promising and will be presented.



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+

3 4

Supercritical Fluid Synthesis of Metal Oxide Platinum Catalysts with High Activity

and Stability for Fuel Cell Applications

Odetola Chris, Liliana Trevani and E. Bradley Easton Faculty of Science, University of Ontario Institute of Technology

The heart of a typical fuel cell lies in the electrochemical oxidation and reduction reactions occurring at the anode and cathode respectively. The durability and performance of a proton exchange membrane fuel cell (PEMFC) are restricted by the slow kinetic of the oxygen reduction reaction (ORR), the stability of most active metal catalyst (platinum) and susceptibility of this carbon support to corrosion at extreme operating potentials. There is need to develop catalyst supports that will not corrode or with minimum corrosion level compared with convectional carbon black support. Modification in the synthesis and supercritical fluid drying were explored for uniform dispersion of platinum nanoparticles on single phase metal oxide catalyst support. Preliminary results will be presented.

Characterization of ADN and ADN-based Propellants

Q.S.M. Kwok, M. Vachon, C. Badeen, W. Ridley, D.E.G. Jones and S. Singh Canadian Explosives Research Laboratory, 1 Haanel Drive, Ottawa, Ontario K1A 1M1

Canada

Ammonium dinitramide (ADN), NH4N(NO2)2, has been considered as one of the potential new energetic oxidizers for replacing ammonium perchlorate (AP) in composite propellants. In this study, ADN crystals, prills and two ADN-based propellants having different relative amounts of ingredients were characterized. The concentration of dinitramide ion (DN) and NH4 in the crystals and the prills samples was determined using Ion Chromatography. The ratio of the concentration of DN in prills to that in crystals is 0.97. Trace amounts of K+, NO , Na+ detected in both the crystals and the prills.

or SO 2 were

The thermal behaviour of the crystals, prills and propellants was studied using DSC, simultaneous TG-DTA-FTIR-MS, ARC (accelerating rate calorimetry), HFC (heat flux calorimetry) and INC (isothermal nanocalorimetry). Decomposition of ADN was observed from all of the samples at temperatures above the melting point of ADN (~92 °C). Formation of N2O, NO2, H2O, CO2, CO, N2 and NO was detected during the ADN decomposition. The addition of coating agents in the prills and stabilizers in the propellants has no significant effect on the onset temperature of ADN decomposition, while it lowers the rate of ADN decomposition.



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The thermal stability of the ADN samples at temperatures below the melting point of ADN was studied using TG-DTA-FTIR-MS, HFC or INC. Early solid decomposition of ADN, which generates N2O and H2O, was observed at 60 °C from the TG-DTA-FTIR- MS results. The coating agents seem to have insignificant effects on the thermal stability of ADN at low temperature. Electrostatic discharge (ESD) and impact sensitiveness of the ADN samples were determined. The crystals and prills are sensitive to impact, while the two propellants are relatively less ESD and impact sensitive. The ESD and impact sensitiveness of the ADN crystals and prills are of the same magnitude as that of RDX.



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Vendor Presentations

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