ictac news winter 2012-13dled by prof. yuko nishimoto. additionally, the following persons handled...

To begin this latest issue of ICTAC News, we want to introduce the new officers for the organization. After elections held in Osaka in August, the following will be the officers for the next period of time. Those denoted in blue were elected at the congress. President - Andrzej Malecki, Poland Vice-President - Wim deKlerk, Holland Past- President - Don Burlett, United States Secretary - Ranjit Verma, India Treasurer - Pierre LeParlouer, France Membership Secretary - Riko Ozao, Japan Scientific Commission - Crisan Popescu, Romania The Advisory Committee, a group of past officers with experience in organizational operations and congresses, is appointed and each member has accepted their position on this committee. The members of this committee are: Jean Rouquerol, France Eder Cavalheiro, Brazil Csaba Novak, Hungary Rosa Nomen, Spain These people, along with the councilors from all of our affiliate socie-ties, will provide the leadership for the next two to four years. The only po-sition that will come up for renewal in two years will be the Membership Sec-retary. We wish these officers the best in their new roles.

New Officers for ICTAC Inside this issue:

President’s Corner

2

ICTAC 15 3

Scientific Com-mission - Com-ments from the Chair

14

Young Scientist Awards

17

Technical Articles 40

Book Review 56

Meeting An-nouncements

58

Obituaries 19

News from Affili-ate Societies

21

ICTAC News Returns

We have begun issuing ICTAC News on a semi-annual basis again. The electronic reincarnation of this publication should provide up-to-date in-formation for all our members. Csaba Novak will be the editor of this publi-cation with Don Burlett acting as “publisher”. If you have news, suggestions, etc. for this publication, please contact one of these gentlemen.

ICTAC News

Winter 2012-2013 Volume 42, No. 1

The Future of ICTAC

According to the ICTAC Statutes and in result of decision of the Gen-eral Assembly of ICTAC upon completion of the 15th Congress in Osaka a new Executive Committee started to perform its duties. Usually the begin-ning of the new authorities activity is connected with résumé of previous achievements and it is the time to identify new tasks as well. The summary of the Executive Committee, Scientific Commissions, Working Groups and Members activity in the past term presented during meetings in Osaka by Dr. Don Burlett, the Past President of ICTAC, is a very important docu-ment which provides the basis for determining our goals and objectives for the future. However, before a conclusive formulation of the goals and tar-gets we need to answer two very important questions, namely:

♦ What do ICTAC members expect from our confederation? ♦ What are they ready to do for it?

The Executive Committee is just at the beginning of the term plans to launch a broad discussion among Members and Affiliate Societies for obtain-ing answers to these two key questions. Such an action should make all of us aware that the ICTAC cannot be identified only with the members of Ex-ecutive Committee but with individual Members, Institution Members and especially with Affiliate National Associations. We intend to address these questions to each Member and we expect that replies we will obtain allow us, after their thorough analysis, to formulate the program of ICTAC activi-ties for the next years.

We perceive the need for improving work of the ICTAC Scientific Commissions and Working Groups and so we request to prepare new pro-grams and to define the conditions and possibilities of their implementation.

We expect that Affiliate Councillors will do their best to ensure an efficient liaison between the Executive Committee and the National Associa-tions. We also expect them to provide our community (especially through the website and through ICTAC News) with periodical information about news, problems and achievements of their Association. Recent years have brought a significant increase in the number of confer-ences on thermal analysis and calorimetry organized jointly by the National Societies affiliated with the ICTAC. The Executive Committee essentially is not concerned about the reduction of the number of meetings, but the co-ordination of the dates is reasonable. We would like to know the opinion of ICTAC Members in this topic.

ICTAC has a well established relationship with the manufacturers of thermal analysis and calorimetry equipment and recognises the importance of their contribution to the scientific community. As part of the review process, ICTAC will be consulting the instrument manufacturers for their

President’s Column

ICTAC News

ICTAC News

Osaka Castle

There’s a reason why quadrennial ICTAC Congresses are so special. Great Science! Great People! Great Locations! What else do you need to be convinced this was the place to be? The recently concluded ICTAC 15 took place at Kinki University in Osaka, Japan under the masterful direction of Professor Takayoshi Kimura. The congress site was Kinki University, an urban university located in Higashi-Osaka. Even though it was tucked into a smallish campus, the surroundings were quite conducive for science conver-sation and interaction by all attendees. It was a rousing success because of the wide variety of science, culture and interactions fostered by the organiz-ers. We’d like to take a few moments to review the many aspects of this congress.

ICTAC15 - Japan

Volume 42, No. 1

We’re on the web. See us at www.ictac.org

President’s Column (continued)

opinion on how these links can be strengthened. The Executive Committee expects the cooperation and support of

all the Members in the realization of tasks put for ICTAC. On behalf of the Executive of ICTAC Prof. Andrzej Malecki President of ICTAC

Organizers

The conference was chaired by Prof. Takayoshi Kimura of Kinki Uni-versity. He was joined during organization by Honorary Chairs, Prof. Takeo Ozawa and Prof. Hiroshi Suga. Secretarial duties were handled by Prof. Riko Ozao and Assoc. Prof. Tadashi Kamiyama. Treasurer duties were han-dled by Prof. Yuko Nishimoto. Additionally, the following persons handled these various areas of the congress: Dr. Takahisa Tsugoshi (Public Rela-tions), Prof. Toshimasa Hashimoto (Fund-raising and Vice-Chair), Prof. Ka-tsuhide Terada (Fund-raising), Dr. Michiko Kodama (Fund-raising), Prof. Hatsumi Aki (Social Events), Prof. Yasuo Saruyama (Program Chair), Prof. Nobuyoshi Koga (Program Chair & JCCTA Joint Program), Prof. Katsuhide Terada (Program Chair) and Assoc. Prof. Junko Morikawa (Program Chair). These folks along with a long list of the local organizing committee (Chaired by Prof. Takayoshi Kimura), the Steering Committee (Prof. Toshio Maru-yama and Prof. Kazuhiko Ishikiriyama), the International Advisory Board and the Financial Auditor (Prof. Akira Inaba) made the congress run smoothly through all the various aspects. Also, I cannot proceed without expressing great thanks to the many students who worked tirelessly throughout the entire congress making sure that every attendee was treated well and their needs attended to. These students really did make a difference in the con-gress. A well deserved congratulation is offered by the executive of ICTAC and all the attendees to everyone that made this such a memorable event. Sessions

The Technical Sessions were divided into several sections. There were the standard oral sessions with topics including A Commemorative Special Session, Advanced Instrumentation, Thermodynamics and Thermo-chemistry, Environmental Technology and Green Chemistry, Colloid and Interface Science, Inorganic Materials, Polymer and Organic Materials, Phar-maceutical, Kinetic Phenomena in Practical Process, Biomaterial and Food, Energetics and A General Session. These were adjoined by workshops on Standardization and Data Bases and on Challenges in Education in Thermal Analysis & calorimetry. Poster sessions were also held in all these titled ar-eas.

ICTAC 15 (continued)

The process

of scientific

discovery is,

in effect, a

continual

flight from

wonder.

Albert Einstein

ICTAC News

Opening Ceremonies at ICTAC 15 (Osaka) There was also a joint session between ICTAC-15 and JCCTA48. There were both oral and poster sessions for this joint set of sessions. There was also a JCCTA48 series of sessions with award lectures, oral presentations and posters. Of keen interest were the student poster sessions which were judged by attendees of the congress. The quality and quantity of posters presented was quite impressive and bodes well for the future of thermal analysis and calorimetry as a technical area of material science. Plenary and Invited Lectures

The plenary and invited lectures were to be highlighted by the Robert MacKenzie Memorial Lecture to be given by awardee Prof. Takeo Ozawa, Past President of ICTAC. Unfortunately, due to health issues, Prof. Ozawa was unable to attend the congress and his lecture, entitled “Thermal Analysis – Review and Frontier” was presented by Prof. Nobuyoshi Koga. The TA In-struments Award Lecture was given by Prof. Jerzy Blazejowski (University of Gdansk, Poland) and was entitled “Thermal analysis and computational meth-ods in investigations of the thermal features, behavior and reactivity of crystal-


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crystalline solids”. The SETARAM Award Lecture was given by Prof. An-thony Beezer (University of London, United Kingdom) and was entitled “After 5 decades of change in Calorimetry, what is the next project?” Fi-nally, the ICTAC Young Scientist Award lecture was given by Dr. Severine A. E. Boyer (ISAE-ENSMA, France) and was entitled “Calorimetric-based advance to investigate the thermo-diffuso-mechanical behavior of polymers in tandem with their multi scale phase evolution under severe T and P con-ditions”. Invited lectures included presentations from Li-Xian Sun (Dalian In-stitute of Chemical Physics, China) entitled “New Hydrogen Storage/Phase Change Materials and Their Thermochemistry Studies”, Prof. Christoph Schick (University of Rostock, Germany) entitled “Calorimetry on Time Scales from Microseconds to Days” and Prof. Junko Morikawa (Tokyo Insti-tute of Technology, Japan) entitled “Micro-scale thermal imaging in visual thermal analysis”. These lectures were part of a large set of keynote lectures in the various technical sessions. Needless to say, the plenary, invited and keynote lectures were varied and very well presented. Attendance

The conference was well attended with about 215 regular registrants and 115 students. The attendees represented 26 countries including (not in alphabetical order) Australia, Japan, Germany, Hungary, Romania, Poland, Great Britain, United States, Switzerland, Taiwan, Malaysia, Greece, Slovakia, Spain, China, Belgium, Denmark, the Czech Republic, France, Brazil, India, Thailand, Finland, the Netherlands, Estonia and Sweden. The student popu-lation at the meeting was quite impressive and many were working for the congress in addition to attending sessions of lectures when they were free to do so. Many industrial, academic and institutional/government organiza-tions were represented at the meeting, indicating the wide range of organi-zations which find this scientific area valuable. Awards

Many awards are presented each congress at ICTAC and we have already noted the winners of the Robert McKenzie Memorial Lecture award, the TA Instruments Award (Thermal Analysis), the Setaram Award


The process

of scientific

discovery is,

in effect, a

continual

flight from

wonder.

Albert Einstein

ICTAC News

Young Scientist Travel Grant Award Winners


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Volume 42, No. 1

(Calorimetry) and the Young Scientist award. In addition to these major awards, a number of other awards were presented. Ever Congress, we award a number of Young Scientist Travel grants, to encourage participation by promising young scientists. This congress, 7 travel grants were awarded and 6 were used. The winners for this congress were: Giuseppe Lazarra (Italy), Loic Favergeon (France), Iolanda Fottichia (Italy), Alexander Kozlov (Russia), Roland Neher (Germany), Oana Stefanescu (Romania) and Imre Szilagyi (Hungary). Further two other sets of awards were made. There were two Young Scientist Oral Presentation Awards – D. G. Papageorgiou (Greece) for the paper entitled “Comparative Characterization and Study of Degradation Kinetics of Polypropylene Random Copolymers” and E. Roumeli (Greece) for the paper enti-tled “Thermal and Structural Characterization of Crosslinked High Density Poly-ethylene”. Another set of awards were presented for student posters given. The two winners were: M. Saito (Meiji University, Japan) entitled “Highly Sensitive Biochemical Calorimeter with MEMS Thermopile Sensor: and S. Inohata (Tsukuba University, Japan) entitled Negative Thermal Expansion and Phase Diagram of Sc2Mo3(1-x)W3xO12 Solid Solutions”. Reflecting upon the quality and quantity of young presenters both in oral and poster presentations, this was quite an impressive collection for an ICTAC congress and bodes well for the future.

Young Scientist Oral and Poster Award winners Governance

The Executive and Council of ICTAC meet at every congress to re-view reports from the various officers and committees. New proposals are discussed and decisions made that are eventually presented to the member-ship at the General Assembly. At the General Assembly of ICTAC, a num-ber of reports were presented. Prof. Takayoshi Kimura reported on the ICTAC Congress (including registration numbers and other details). Dr. Don Burlett presented the Treasurer’s report (for the absent Csaba Novak) indicating that society finances were sound and stable. Prof. Riko Ozao gave Membership Secretary’s report, indicating a modest decline in membership and the continuing change in distribution from the movement of congresses over time. Dr. Burlett presented the Secretary’s report (for the absent Prof. Eder Cavalheiro) and it was indicated that the most difficult part of the Secretary’s job is maintaining an accurate listing our councilors and other contacts for the affiliate societies. Prof. Rosa Nomen presented the report of the Scientific Commission and reviewed the activities of the various com-mittees in place currently. She pointed out again that communication from


The process

of scientific

discovery is,

in effect, a

continual

flight from

wonder.

Albert Einstein

ICTAC News

the committees was the most difficult aspect of this group. Dr. Burlett then announced the decision of Council for the next venue for the 16th ICTAC Congress in 2016. The decision of Council was for the congress to be hosted by the NATS organization, with a site selected to be Buena Vista, Florida, USA. The proposed dates were August 6-13, 2016. The nominations Committee, chaired by Prof. Jean Rouquerol, re-ported the following nominations for officers for the next four-year term. Prof. Andrzej Malecki (Poland) moves automatically to the President position from Vice-President. Ing. Wim de Klerk (The Netherlands) was nominated to be Vice-President, Prof. Ranjit Verma (India) was nominated for Secretary, Dr. Pierre LeParlouer (France) was nominated for Treasurer and Prof. Crisan Popescu (Romania) was nominated to be the new Chair of the Scientific Com-mission. Because there were no contested positions for the executive, the election was conducted by show of hands and all nominees were accepted.

Student Poster Session Three changes to the statutes of the organization were proposed after Coun-cil acceptance. One involved the designation of the Affiliate Councilor from societies, which involves the President or Councilor from that society inform-ing ICTAC of this designation. The second one involved the statement that


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“Membership shall begin on January first of the year subsequent to payment of dues”. Finally, the membership class “Institutional or Company Member” was recommended to be removed from the statutes. All three proposals were voted on by show of hands and approved. The award winner for Robert McKenzie Memorial Lecturer, Prof. Takeo Ozawa, was announced and this award was accepted by Prof. Yo-shida, President of the Japanese Society of Calorimetry and Thermal Analy-sis, and presented by Prof. Koga. It was also noted that the executive had recommended that the application process for the Young Scientist Award and the Young Scientist Travel Awards be combined and selected from the same pool of candidates. Dr. Burlett also reviewed the rebuilt ICTAC Website and the ongo-ing work to continue its upgrading. It was also noted that the ICTAC News publication (via electronic media) was to be continued and its frequency in-creased to twice a year. The new Executive and Council met at the end of the congress to assure that momentum from the meetings held would continue.

Student Helpers at the Congress


The process

of scientific

discovery is,

in effect, a

continual

flight from

wonder.

Albert Einstein

ICTAC News

Social and Cultural

As with any international meeting, the social and cultural op-portunities at an ICTAC Congress are very important and wonderfully inter-esting. The organizers of this Congress did an exceptional job of providing everyone with a wide variety of possibilities. The Congress began with a traditional reception on Monday evening in November Hall. The following morning, the Kinki University Philharmonic provided a morning concert in November Hall with a variety of musical pieces including a marching set of Beatles tunes and other music. That evening, a Welcome Concert was performed by the Kinki University Band. This band has won numerous awards in All Japan Band competitions and that was evi-dent from the musical performance. Our traditional excursion took place Thursday, as participants visited the Nara Park, celebrating the long history and former capital of Japan. It was wonderful to walk among the temples and other traditional buildings and see some of Japan’s history and culture.

Temple Area at Nara


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Following the excursion, we traveled back to Osaka for an evening banquet at the Taiko-En restaurant. Here we had the special pleasure of enjoying fresh tuna harvested that afternoon at the Kinki University tuna facility to the south. The tuna preparation was traditional and was a special treat for everyone. With food and socializing, a perfect evening was had by all.

Tuna Ceremony During the entire Congress, the original equipment used by Honda for Thermogravimetry was setup and shown to still be functional and accu-rate. (This exhibit was made possible by the Tokyo Institute of Technol-ogy.) Along with all these more or less traditional events, our hosts pro-vided many opportunities for socializing and meeting our colleagues. These were a Young Scientist Mixer, a Senior Scientist Mixer, a number of tradi-tional Japanese Tea ceremonies, and a number of lunches provided by the instrument manufacturers (Rigaku, Netzsch, Mettler-Toledo, TA Instru-ments and SII NanoTechnology). Additionally, city tours were available for family members and other support for social and cultural exploration


The process

of scientific

discovery is,

in effect, a

continual

flight from

wonder.

Albert Einstein

ICTAC News

Honda Balance Exhibit The Congress was a very large success for participants and for the so-cieties involved in its organization. Few will forget the experiences gained during this meeting. We hope to see you at the next Congress in four years. Don Burlett


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Volume 42, No. 1

SCIENTIFIC COMMISION The Scientific Commission of ICTAC is a construction intended to provide ICTAC organisation with a forum for both enlarging and focusing the appli-cation field of thermal analysis and calorimetry to meet the challenges of an ever demanding scientific community. The ultimate purpose is to have a flexible structure able to capture and respond fast to any scientific or tech-nologic request. For this purpose the Commission is composed of several working groups and committees created along the years and devoted to spe-cific problems. During the ICTAC 14 in Sao Pedro the ICTAC Council took steps for in-creasing the flexibility of the Scientific Commission stating that: 1. To simplify the present structure of committees and working groups by changing all into “committees” only. 2. Each committee should:

a. have a well-defined working plan; b. organize a workshop at ESTAC and/or at ICTAC; c. publish books / papers with the presentations and discussions; d. have a continuous activity.

At the ICTAC 15 meeting in Osaka further steps along the same lines were adopted by ICTAC Council and Executive, namely: 3. Each Chairperson may serve a period of 4 years for leading the group; the period is renewable for a single term of 4 more years. 4. ICTAC Council should approve the progressively closing down of the committees by observing the rule of ‘no-activity’ over years. During the same meeting it was also suggested that the Chairpersons of vari-ous Committees to invite awardees of ICTAC Young Scientist Award to participate to the activities of various groups. Figure 1 shows ICTAC Scientific Commission structure as it is now on the site: http://www.ictac.org/scientific_commission.html.

Report from the Chair of the Scientific Commission (continued)

Volume 42, No. 1

Figure 1: Main page on the web for the Scientific Commission Comments on each Committee as of the meeting of August 19th, 2012, dur-ing the ICTAC 15, Osaka, Japan: Education

Prof Verma is very active and has organized a very interesting workshop on Education for the congress.

Environmental Safety Prof Balek will be asked about the plans and reorganization of this Com-mittee.

Geosciences Prof Langier-Kuzniarova will be asked about the plans and reorganiza-tion of the Committee.

Lifetime prediction of materials Prof Popescu concluded an inter-laboratory calculation of lifetime for a given material. Results will be published soon.

Nomenclature Prof van Ekeren will be asked about the plans and reorganization of the Committee. Prof Charsley could possibly join the Committee.

Report from the Chair of the Scientific Commission (continued)

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ICTAC News

Pharmaceuticals Prof Riga will be asked about the plans and reorganization of the Com-mittee. It was also recommended to expand the Committee by attracting more people.

Polymers A chairperson for that Committee is required.

Sample Controlled Thermal Analysis Prof Gurli Mogensen informed us that Dr. Ole Toft Sørensen, passed away last autumn after a short period of illness. Prof Rouquerol contacted Prof Koga and Dr. Arii for finding a successor.

Standardization It was proposed to change the name of the Committee into: Standardiza-tion of TA Procedures. Dr. Ozao will talk to Dr. Kato for chairing the Committee.

Temperature Modulated Calorimetry We decided to close down this Committee, which will be deleted from the site.

Thermal Analysis Combined Techniques to Food Prof Relka will be asked about the plans and reorganization of the Com-mittee.

Thermal Reactivity of Solids Prof Malecka will be asked about the plans of this Committee.

Thermochemistry Dr. Roux retired and she proposed Sergey P. Verevkin, from the Institut fuer Chemie, Abt. Physikalische Chemie, Universitaet Rostock as a suc-cessor. He accepted the chair and will define the plans for the Commit-tee.

As it appears, ICTAC Scientific Commission is in full process of restructuring along the four points rose during the ICTAC-14 and ICTAC-15 meetings. We invite all ICTAC members to participate and bring contribution to this process. Prof. Dr. Rosa Nomen and Prof Crisan Popescu, Chair and Vice-Chair

Report from the Chair of the Scientific Commission

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ICTAC Young Scientist Award The ICTAC Young Scientist Award is given to an outstanding young scientist working in the field of thermal analysis and calorimetry. This award is based on a letter of nomination by the proposer, curriculum vitae, list of publications and a one page abstract of the paper that the candidate intends to present at the 15th ICTAC Congress. The award winner for the 15th ICTAC Congress was Dr. Severine Boyer (France) who presented a paper entitled “Calorimetric-based advance to investigate the thermo-diffusochemo-mechanical behavior of polymers in tandem with their multi scale phase evolution under severe T and P conditions”. ICTAC Young Scientist Travel Grant Awardees Another group of young scientists were nominated by their respec-tive affiliate societies for travel grants. The judging was based on the back-grounds and curriculum vitae provided by each candidates. Seven candi-dates were selected to receive travel grants for attending ICTAC 15. The winners were: Loic Favergeon, France Iolanda Fattichia, Italy Alexander Kozlov, Russia Giuseppe Lazarra, Italy Roland Neher, Germany Oana Stefanescu, Romania Imre Szilagyi, Hungary (unable to attend) These students and young scientists represent a bright future for thermal analysis and calorimetry and they should all be congratulated on both their work and their awards for this congress.

ICTAC Young Scientist Awards

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ICTAC NEWS EDITOR

We are happy to announce that former Treasurer of ICTAC, Csaba Novak, has agreed to act as editor of the ICTAC News newsletter. He will be assisted by “publisher” Don Burlett. Any suggestions or submissions should be made to both for inclusion in futures issues.

ICTAC needs your news!! Any news of your activities, society activities, meetings, awards, etc. is needed to help keep the society informed. If there are topics that we are not covering that you think are of value to our members, please contact the Edi-tor of ICTAC News to let him know. We’ll be happy to consider the con-tent and make the newsletter better. It’s you society and we can only pro-vide the information that we get and cover topics and ideas that we think of. So, be an active part of the society and the society will be better for you participation. Thanks. And enjoy the newsletter.

Society News

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OBITUARIES

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Professor Bernhard Wunderlich 1931-2012 It is with great sadness that we report the passing of Professor Bern-hard Wunderlich on the evening of August 16, 2012, in Knoxville, TN. Pro-fessor Bernhard Wunderlich, arguably the most influential thermal analyst of all times passed away at age 81. Professor Wunderlich immigrated from Germany to the U.S. in 1954 and received his Ph.D. from Northwestern University in Evanston, Illi-nois in 1957 under the leadership of Prof. Malcolm Dole. He was an instruc-tor at Cornell University until 1963. From 1963 until 1988 he was a Profes-sor of Chemistry at Rensselaer Polytechnic Institute in Troy, NY. He served as a consultant for the DuPont Company for many years. In 1988, he moved to Knoxville, TN and was appointed a Distinguished Scientist at both the University of Tennessee and Oak Ridge National Laboratory, until his re-tirement in 2001. In his scientific career Professor Wunderlich focused primarily on the thermal analysis of polymers. Among his many accomplishments the most important ones were the creation and characterization of equilibrium crystals (extended chain crystals) of polyethylene, the discovery of the rigid amorphous phase in semi-crystalline polymers, the precise measurement and publication of the heat capacity tables of macromolecules in the ATHAS (The Advanced Thermal Analysis System) databank, and publication of the detailed theory of Modulated Temperature Differential Scanning Calo-rimetry. He has authored ten books and 575 scientific publications. His stu-dents include many renowned scientists, several of whom are well-known thermal analysts. He is preceded in death by his parents, Richard and Johanne Wunderlich; and brother, Frank Wunderlich. He is survived by his wife, Adelheid "Heidi" Wunderlich; son, Brent Wunderlich; daughter, Caryn Wunderlich; brothers, Joachim Wunderlich and Manfred Wunderlich; and two grandchildren. We will be always proud of the fact that we learned thermal analysis from Professor Wunderlich. His former students:

R. Bruce Prime Joseph D. Menczel Larry Judovits Michael Jaffe Marek Pyda Maria Laura Di Lorenzo Stephen Z.D. Cheng Janusz Grebowicz

and the Executive Council of the North American Thermal Analysis Society

Prof. Wojciech Zielenkiewicz 1933 - 2010

Prof. Wojciech Zielenkiewicz was outstanding specialist in the field of thermochemistry and calorimetry, the creator of the Scientific School and tutor of the young generations of scientists. Career and scientific achievements of Prof. Wojciech Zielenkiewicz: • Pupil and successor of Prof. Wojciech Świętosławski • Professor from 1971 • Director of the Institute of Physical

Chemistry of PAS in Warsaw, Poland (1973-1990)

• Foreign Member of the Royal Academy of Sciences, Spain (from 1975)

• Corresponding member of the Polish Academy of Sciences (from 1977)

• IUPAC Associate and Titular Member (1977-1987) • Member of several Polish scientific societies • Member of editorial boards of several international scientific jour-

nals • Awarded Calvet Memorial Award and Medal (1991) by French As-

sociation of Calorimetry and Thermal Analysis • Author of about 250 scientific papers, including the number of

monographs • Supervisor of 15 PhD thesis

Prof. Zielenkiewicz services for the Polish Society of Calorimetry and Ther-mal Analysis PTKAT:

• Founder of PTKAT in 1985 • President of PTKAT 1985 – 1991 • Honorary president of PTKAT from 1991 • Initiator and organizer of first three CCTA conferences • Organizer of several international Symposia on thermokinetics and

calorimetry • Awarded W. Świętosławski Medal of the Polish Society of Calo-

rimetry and Thermal Analysis (1994)

OBITUARIES

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News from Affiliates and Groups

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News from PTKAT In 2012 Polish Society of Calorimetry and Thermal Analysis continued its activity both in the international and domestic domains. PTKAT had a substantial representa-tion at the ICTAC 15 in Osaka, Japan on 20-24 August 2012. President of PTKAT, Barbara Pacewska and six other members of the society partici-pated in this important event with lectures, oral and poster presentations. It was a great pleasure and the reason for satisfaction for the members of PTKAT that during ICTAC 15 Prof. Jerzy Błażejowski from Gdańsk Univer-sity (member of PTKAT authorities) was granted with the TA Instruments–ICTAC Award for his achievements in the field of thermal analysis. At the meeting of ICTAC Council which took place in Osaka just before ICTAC 15 the PTKAT representative had presented the proposal to organize the next ICTAC congress in 2016 in Kraków, Poland. The proposal was re-ceived with the great interest and, although the NATAS proposal was cho-sen, we hope that PTKAT will success in getting organization of ICTAC in 2020. Polish Society of Calorimetry and Thermal Analysis had its meeting form 9th to 13th September 2012 in Zakopane, Poland at the 11th Confer-ence on Calorimetry and Thermal Analysis and Calorimetry CCTA 11. Be-low the detailed report on CCTA 11 is placed. The meeting was organized by Barbara Małecka (Chair) and other staff members of the Faculty of Mate-rials Science and Ceramics of AGH University of Science and Technology, Kraków. It was also during this meeting that General Assembly of PTKAT took place which elected new board for the term 2012-2015. PTKAT Board 2012-1015: Barbara Małecka - President Barbara Pacewska - Vice-president Agnieszka Łącz - Secretary Małgorzata Jóźwiak - Treasurer The complete composition of PTKAT Board and other information con-cerning the society can be found at www.ptkat.agh.edu.pl. In plans for 2013 there is organization of the next courses for young scientists and researchers during the 7th School on Thermal Analysis which will be held in the Spring.


ICTAC News

ICTAC News

11th Conference on Calorimetry and Thermal Analysis and

Calorimetry, Poland 11th Conference on Calorimetry and Thermal Analysis and Calorimetry, CCTA 11 was held from 9th to 13th September 2012 in Zakopane, Poland. The Conference follows the tradition of the previous meetings organized traditionally in the heart of Tatra Mountains by the Polish Society of Thermal Analysis and Calorimetry (PTKAT). The co-organizer of the conference was the Faculty of Materials Science and Ceramics of AGH University of Science and Technology, Kraków, Poland. The aim of the CCTA conferences is promotion of the scientific discussions and exchange of ideas between researchers involved in calorimetry and thermal analysis not only in Poland but in other friendly countries as well. The main topics of the Conference were the applications of calorimetry and thermal analysis to studying inorganic, organic and biological materials, kinetics and reactivity of solids, solution calorimetry, food systems etc. Very important issue was the progress and new solu-tions in theory, instrumentation and technical applications.

Attendees of CCTA 11 CCTA 11 attracted 150 participants mainly from Poland but also from Czech, Ger-many, Hungary, Romania, Russia and Slovakia, who contributed to the conference program with a great success. In the program 170 papers were presented (among them 4 plenary lectures and 45 oral communications) in seven different sections. The Organizing Committee was happy to welcome a large number of Ph.D. students and other young researchers who contributed interesting works.


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11th Conference on Calorimetry and Thermal Analysis

and Calorimetry, Poland (continued)

During the opening ceremony the short tribute to Prof. Wojciech Zielen-kiewicz who passed in 2010 was presented. It is a tradition of CCTA conferences to honor the best young Polish scien-tist working in the field of thermal analysis and calorimetry with the PTKAT award. The award was assigned to Dr. Magdalena Szumera from AGH UST for her work on the effect of transition elements on the thermal properties of silicate-phosphate glasses.

Prof. Barbara Pacewska, Dr. Magdalena Szumera with the certifi-cate of PTKAT award for the best young Polish scientist, Prof. Barbara Malecka, Prof. Andrzej Malecki

The most important instrument manufacturers were present at the exhi-bition at the CCTA 11 and in addition they delivered lectures on the newest technical solutions. The weather was exceptional but it did not compete with the lectures deducing from the attendance in the hall, however there was enough time to appreciate the beauty of Tatra mountains too. The next CCTA conference is planned in 2015 year. I express my sincere gratitude to the organizing and scientific committees of CCTA 11, sponsors and all those who contributed to the success of this event.

Barbara Małecka Chairwoman of CCTA 11


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11th Conference on Calorimetry and Thermal Analysis

and Calorimetry, Poland (continued)

Table at conference dinner (from left): Prof. Henryk Piekar-ski, Prof. Csaba Novak, Prof. Andrzej Małecki


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News from GEFTA

GEFTA’s activities in Thermal Analysis and Calorimetry during the

last five years

GEFTA, the German Association for Thermal Analysis, is active on four main activity fields for many years already. As each similar organisation, we pay particular attention to our annual scientific meetings. They are often or-ganized together with the associations of our neighbouring European coun-tries provided the chosen conference site is close to the common border. From time to time we even meet on foreign ground, e.g. in May 2008 Serge Walter organized a trilateral joint symposium of the French AFCAT, the Ger-man GEFTA, and the STK from Switzerland in Mulhouse (Alsace, France) - an interesting conference appreciated by all participants. 2010 we met with our Polish and Czech colleagues from PTKAT and CWGT, respectively, in Dres-den. This year 2012 again, we had a joint German-Swiss symposium in Saar-brücken, focusing on nano and hybrid materials. Especially the German-Swiss cooperation has a long tradition - it was the fifth joint symposium in nearly four decades. The second and third column of GEFTA’s activities are formed by two reputed symposium series being held regularly in a bi-annual sequence: The Ulm-Freiberg Calorimetry Conferences (Founded by Günter W. Höhne and Wolf-gang Hemminger) the 20th symposium of which will be held in March 2013 in Freiberg (Saxony) and, furthermore, the Lähnwitz Seminars on Calorimetry (Founded and chaired by Christoph Schick) the youngest of which was held last summer in Rostock treating the topic Interplay between Nucleation, Crystalli-zation, and the Glass Transition. It is not exaggerated to state that, since many years already, the Lähnwitz Seminars are meetings of the Crème de la crème in ultra-fast and modulated techniques in calorimetry - people arrived from 17 countries from all over the world, i.e. from Japan, the United States, Russia, etc. The fourth column of our activities are the Autumn Schools held, if possible, every year. They represent an alternating sequence of Short courses for beginners and of Advanced specialist’s meetings. The list of sub-jects treated the last years might illustrate that we are trying to correspond to the participant’s expectations as flexible as possible: Applications of Ther-modilatometry (2007), Methods of Thermal Analysis (2009), Quantitative as-pects of EGA techniques (2010), Determination of thermophysical properties (2011), Calorimetry and TA of Non-equilibrium phases (2012). This educa-tional engagement of GEFTA is considered as an important way to extend our membership and the appreciation by people from industry and institutes


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News from GEFTA (continued) seems to confirm it. An important part of our work consists of honouring outstanding con-tributions to the fields of Thermal Analysis and Calorimetry. Since 1979, every two years the Netzsch-GEFTA Award is attributed to scientists for ex-traordinary achievements, and since the early 90s a Netzsch-GEFTA Young Scientist Award is sponsored as well. In an irregular way, TAInstruments lends out an Industrial Research Prize. This year, Professor Peer Schmidt (Senftenberg/Dresden) was hon-oured with the Netzsch-GEFTA Award 2012 (photo below) for his work on inorganic solid state chemistry, especially for his contribution made by equilib-rium and non-equilibrium investigations on pressure-depending systems. The 40th anniversary of the foundation of GEFTA will be commemo-rated in two years with an International symposium to be held at Humboldt University in Berlin (September 16-19, 2014) focusing on materials characteri-zation, novel materials, and coupled techniques in TA. We aspire to invite representative delegations of our neighbouring partner associations from the Czech Republic, France, Hungary, Poland, The Netherlands, and Switzerland. Who ever will have time to join us, you are welcome!

Michael Feist

GEFTA chairman

Professor Peer Schmidt receives the Netzsch-GEFTA Award 2012 from the GEFTA Chairman, Dr. Michael Feist (left) and Dr. Ekkehard Füglein (right) from Netzsch Gerätebau GmbH


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This year the annual Thermal Methods Group TAC Conference took place from 3rd - 4th April 2012 in the Division of Food Sciences, University of Nottingham in the pleasantly rural surroundings of their Sutton Bonington campus. The theme of the meeting was “Thermal Methods : including Applica-tion to Biological Materials”. Organised by Bill MacNaughtan and Val Street, the meeting proved very successful & attracted delegates from a wide range of academic & industrial backgrounds. In addition, there was a Manufacturers’ scientific section, a poster session and a comprehensive equipment exhibition. The Conference was preceded by the popular one day short course on ther-mal methods giving a broad overview of main thermal techniques and their applications. During the Conference the judging of the Cyril Keattch Early Career Scientist Award competition took place. The winner was Fuad Hajji from the School of Biosciences, University of Nottingham and the Award enabled him to present his paper entitled “The Intrinsic Influence of N-Methylmorpholine-N-Oxide on the Phase Transitions of Native and Physically Modified Starch” at the 15th ICTAC Congress in Osaka in August 2012.

Thermal Methods Group, Royal Society of Chemistry Report for ICTAC News December 2012

Queens University


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In November 2012, the TMG held a special meeting, organised by Simon Gaisford & Catherine Barnes, to celebrate the receipt of the 2012 Se-taram-ICTAC Award by Prof. Tony Beezer of the UCL School of Pharmacy, London. The theme of the meeting, which was held at the impressive GSK, Ware Conference Centre, was “Living & Breathing Calorimetry: Biopharma-ceutical & Biological Applications of Isothermal Calorimetry”. Many of Tony’s colleagues and former students were able to participate and we were particu-larly delighted to welcome a large number of contributors from outside the UK, including Prof. Ingemar Wadsö, the winner of the first Setaram-ICTAC Award. The next meeting of the Group is the TAC 2013 Conference which will be held at the University of Greenwich, Chatham. Kent on April 9th - 10th 2013. The theme of the meeting is “Modern Thermal Methods from an Industrial and Academic Perspective.” Both oral and poster presentations are invited and those interested in contributing should contact the Conference organiser Dr. Milan Antonijevic at [email protected]. The Con-ference will be preceded by a one day short course on April 8th 2013, which will provide a comprehensive overview of a wide range of thermal techniques. Further details of the meetings and of the Group’s activities can be found on our website:www.thermalmethodsgroup.org.uk. The current Officers of the TMG are: Chairman, Paul Gabbott (PerkinElmer); Vice Chairman, Dr. Vicky Kett (Queens University, Belfast); Immediate Past Chairman, Ian Priestley (Syngenta); Secretary, Catherine Bar-nes (Glaxo SmithKline); Treasurer, Simon Gaisford (UCL School Pharmacy). Ted Charsley UK ICTAC Affiliate Councillor IPOS Thermal Studies University of Huddersfield

Thermal Methods Group, Royal Society of Chemistry Report for ICTAC News December 2012


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Scope The Committee was established in 1973 with the intention to provide a forum for researchers, academics and experts in industry dealing with ther-mal analysis. The Committee currently has 39 regular and some 40 invited members. President: Gábor VÁRHEGYI, DSc, Chemical Research Center, Institute of Materials and Environmetal Chemistry, Hungarian Academy of Sciences, Bu-dapest, Pusztaszeri út 59-67. Mailing address: H-1525 Budapest, POBox 17. E-mail: [email protected] Secretary: Alfréd KÁLLAY-MENYHÁRD, Budapest University of Technol-ogy and Economics, Department of Physical Chemistry and Materials Science, H-1111 Budapest, Műegyetem rkp. 3, H/I. E-mail: [email protected] Web-site: www.termoanalitika.net

Activity The Committee holds two regular meetings annually (February 16 and November 23 this year). During these meetings recent advances in thermal analysis in different fields is discussed and the members report regularly on the progress of their research work. The 15th ICTAC in Osaka was attended by three members of the Committee. It was a great honour that the ICTAC Distinguished Service Award was conferred on Dr. Judit SIMON, Editor-in-Chief of the Journal of Thermal Analysis and Calorimetry in recognition of her tremendous efforts made through decades to bring the Journal to a level of becoming an interna-tionally respected forum for the whole thermal analysis community. A new initiative was the organization of the international “Short Course on Thermal Analysis” between October 15-17, 2012 with 30 partici-pants from 7 countries (Austria, Belgium, Czech Republic, Germany, Hungary, Poland and Romania). Among the topics covered were the principle and appli-cation of DSC, TMA and DMA in polymers, DSC in life sciences and pharma-ceuticals, TGA in biomass studies, selected applications of simultaneous and coupled techniques in the study of pharmaceuticals, thermal studies of thin films and nanocomposites, kinetic studies, etc.

REPORT on the activity of the

Working Committee for Thermal Analysis of the Hungarian

Academy of Sciences (2012)


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The committee members actively take part in the organization of two forthcoming conferences: the “4th Joint Czech-Hungarian-Polish-Slovak Ther-moanalytical Conference” (Pardubice, Czech Republic, June 24-27, 2013) and the “2nd Central and Eastern European Conference on Thermal Analysis and Calorimetry (Vilnius, Lithuania, August 27-30, 2013). Current state of thermal analysis in Hungary Thermal analysis is an indispensable tool in analytical chemistry and materials science. The most significant research teams are working in Buda-pest (Budapest University of Technology and Economic; Loránd Eötvös Uni-versity; Institute of Materials and Environmental Chemistry of the Hungarian Academy of Sciences), Veszprém (University of Pannonia), Szeged (University of Szeged) and Pécs (University of Pécs). Among the most important re-search topics are the study of drugs and pharmaceutical materials, biological systems and medical applications, nano-powders and surface-modified materi-als, biomass utilization and analysis, polymers and polymer composites, min-erals and clay organo-complexes. The Journal of Thermal Analysis and Calorimetry (impact factor: 1.604) is edited in Hungary by the members of the Committee ( Judit Simon Editor-in-Chief; Alfréd Kállay-Menyhárd Editor; György Liptay Consulting edi-tor). Relation to relevant organizations György Liptay is the member of the Scientific Awards Committee, and Csaba Novák is the member of the Advisory Committee of ICTAC. The Af-filiate Councilor is János Kristóf (University of Pannonia, H-8201 Veszprém, POBox 158, Hungary, e-mail: [email protected]). Another contact per-son if the representative is not available is Judit Simon ([email protected]) The Hungarian representatives of EUROSTAR (European Society for Thermal Analysis, Calorimetry, Thermodynamics and Reactivity) are György Liptay, Csaba Novák and György Pokol. The Hungarian representative of ES-TAC (European Symposium on Thermal Analysis and Calorimetry) is György Liptay. The Committee is closely cooperating with the Thermoanalytical Branch of the Hungarian Chemical Society (Chairman: Dénes Lőrinczy, University of Pécs, Hungary ([email protected]); co-chairman: Imre Miklós Szilágyi, Budapest University of Technology and Economics ([email protected])). Janos Kristof


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Reserved for Your

Affiliate Society

Report!!


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ASSOCIATION FRANCAISE DE CALORIMETRIE ET D'ANALYSE THERMIQUE

FRENCH ASSOCIATION OF CALORIMETRY AND THERMAL ANALYSIS The French Association of Calorimetry and Thermal Analysis had its annual meeting last 22-24 May 2012 in the town of Toulouse, in the southwest of France. Toulouse is one of the major centers of the European aerospace in-dustry. Its world renowned university is one of the oldest in Europe (founded in 1229) .

The venue was the Conference Room

of Hôtel d'Assezat, a town mansion in

the Renaissance style entirely restored

by the Toulouse town council. It was

built in the second half of the XVIth

century for Pierre Assézat, a prosper-

ous merchant in the “pastel” trade that

flourished at the time: pastel being that

light blue dye extracted from crushed,

fermented and dried leaves of the same

name. It houses the collections donated

by George Bemberg, a rich Argentinian

collector, to the city of Toulouse.

The Bemberg Foundation offers the

public the opportunity to admire the

collection of paintings and works or art

united throughout his lifetime. Particularly rich in works from the Renaissance

and the French modern school - notably with more than thirty Paintings by

Pierre Bonnard - the collection also includes furniture, bronzes, books and a

variety of works of art. The exhibit shows the sureness and eclecticism of its

author's tastes.

The meeting was organized by Eric Dantras (Chair), Colette Lacabanne and


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other staff members of the Physic of Polymers Laboratory, CIRIMAT, Paul

Sabatier University, Toulouse 3. It gave a great part to the Characterization of

Materials by Thermal Analysis and Calorimetry. There were sessions on Ma-

terials for Aeronautic, on Materials for Health completed by a free themes

session.

It was also during this meeting that the AFCAT-SETARAM Award was be-

stowed. This award was established in 1999. It is remitted every second year

to a young scientist for a set of remarkable scientific works in the fields of

calorimetry or thermal analysis”. Selected by an Awards Committee of 12

members chaired by Jean Rouquerol, the award-winner was this year Loïc

Favergeon, from SPIN laboratory, School of Mines of St Etienne (in the cen-

ter of the left picture, between Jean Rouquerol, P. Le Parlouer -Société Seta-

ram- and Prof. Jean-Marc Buisine -President of AFCAT). He delivered a nice

award lecture on “Mechanism and kinetic modeling of solid-gas reactions in-

volving outward growth”. Note that this was a great year for L. Favergeon,

since he was also a winner of an ICTAC travel grant to attend ICTAC 15 in

Osaka.


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On the right picture, the last two AFCAT-SETARAM awardees: L. Delbreilh,

in 2010 and L. Favergeon, in 2012.

The next annual meeting of AFCAT is planned to take place in Lyon, 21-23

May 2013 and will be organized by Aline AUROUX, Simona BENNICI

(IRCE-Lyon), Rodica CHIRIAC (LMI/UCBL 1) and Pierre LE PAR-

LOUËR (SETARAM). It will be mainly devoted to thermal analysis and

calorimetry applied to the study of clean and renewable energy.

Contact: Dr Aline AUROUX, IRCELYON Tel: +33 (0)4 72 44 53 98

[email protected]

http://calo.catalyse.cnrs.fr/JCAT2013/

Do not forget to visit the new AFCAT website : www.afcat.net

Jean Grenet (French IC-

TAC Councillor)


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http://www.hsta.gr The 4th Hellenic Conference on Thermal Analysis “THERMA 2010” was held at the University of Rio, Patras, in 23-24 October 2010. During the confer-ence, the HSTA Award was presented by the General Secretary of HSTA, Prof. Dr. George Papanicolaou, to Maria Lalia-Kantouri (President of HSTA for 10 years) in recognition of her outstanding and long-time contribu-tion to the Hellenic Society of Thermal Analysis.

Prof. Maria Lalia-Kantouri

Rio Bridge, Patras, Greece

NEWS from Hellenic Society of Thermal Analysis (HSTA)-


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The 5th Hellenic Conference on Thermal Analysis “THERMA 2012” along with the “1st Hellenic Summer School on Thermal Analysis and Calo-rimetry” was held at the Aristotle University of Thessaloniki, under the auspices of the Chemical and Physical Departments, in 25-27 May 2012. http://www.hsta.gr/Therma2012

Sunset in Thessaloniki (cover page of Ther-ma2012)

We welcome the new President of HSTA, Prof. Kostas Chrissafis and wish him success to the HSTA tradition.

Prof. Maria Lalia-Kantouri HSTA councilor to ICTAC, Past –President HSTA


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News from Czech Republic (CGTA) Web site: www.vscht.cz/ach/osta/ CGTA board: Chair: Prof. Petra Šulcová (University of Pardubice) Vice-Chair: Assoc. Prof. Václav Slovák (University of Ostrava) Members: Assoc. Prof. Jaromír Havlica (University of Technology, Brno), Ing. Pavel Holba (IMIP, Prague), Dr. Jana Kovářová (Inst. Macromol. Chemistry, Acad. Sci, Prague), Prof. Jiří Militký (Technical University, Liberec), Prof. Miloš Nevřiva (Inst. Chem. Technol., Prague), Dr. Vít Plaček (Nuclear Research Inst., Řež), Prof. David Sedmidubský (Inst. Chem. Technol., Prague), Prof. Jaroslav Šesták (Institute of Physics, Acad. Sci., Prague ICTAC councillor: Prof. Jiří Málek (University of Pardubice) ESTAC delegate: Assoc. Prof. Vladimír Balek (Nuclear Research Inst., Řež) The CGTA has been founded within Czechoslovak Chemical Society in 1972 and this year, so to celebrate 40. birthday. Its creation was inspired by International Confederation for Thermal Analysis. First chairman was Dr. Karel Habesberger (Inst. Chem. Technol., Prague) followed by Assoc. Prof. Vladimir Balek (Nuclear Res. Inst., Řež). From 1994 to 2008 the CGTA was chaired by prof. Jaroslav Šesták (Inst. Physics, Academy of Sciences, Prague). Current chairwoman is Prof. Petra Šulcová (University of Pardubice). The activities of the working group are manifold, ranging from the Czech-Slovak nomenclature [1], standardization tests for calibration of thermal analysis instruments, extensive publication activity in the field of thermal analysis, organization of summer schools as well as triennial conferences TERMANAL jointly with Slovak colleagues [2]. The most important result of this Czech – Slovak collaboration was indeed Czechoslovak Conference on Thermal Analysis that was organized together with 8th International Conference in Thermal Analysis in Bratislava in 1985. This tradition is continued by co-organizing fourlateral Czech-Hungarian-Polish-Slovak conferences.

The CGTA also participated in organization of Joint Czech-Hungarian-Polish-Slovak Conference on Thermal Analysis (the first Joint meeting has been organized by Hungarian Thermal Analysis Group - Sopron, 2007, the second under auspices of Polish Society of Calorimetry and Thermal Analysis – Zakopane, 2009, the third being organized by Slovak Working Group on Thermal Analysis and Calorimetry - Stará Lesná in High Tatras, 2011).


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News from the Czech Republic (cont.)

Next Joint Conference of Four States will be organized by CGTA in Pardubice, Czech Republic in 2013 (www.thermal-analysis.cz).

From left Vladimír Balek, David Sedmidubský, Václav Slovák, Jiří Málek, Pavel Holba, Petra Šulcová, Jaroslav Šesták and Miloš Nevřiva

2012 June In June 2012 a special session dedicated to Thermal Analysis and Calorimetry

Participants of Thermal Analysis and Calorimetry Session at annual Conference of Czech Chemical Societies in Olomouc


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News from Czech Republic (CGTA)

has been organized by CGTA during the 64th annual conference of Czech and Slovak Chemical Societies at the University of Olomouc (total 10 sessions for more than 300 participants). There were 12 lectures and 7 posters presented. Two invited lectures were given by prof. Jindřich Leitner (Ins. Chem. Technol., Prague) and Dr. Luis A. Pérez-Maqueda (CSIC-University of Seville, Spain). REFERENCES 1. J. Šesták, P. Holba, V. Fajnor, Chem. Listy 77 (1983) 1292. 2. P. Šulcová, J. Šesták, P. Holba, V. Balek, 40th anniversary of the establishment of the technical thermal analysis, historical roots, professional publications and citations review, Chem. Listy 105 (2011) 807.

Technical Articles

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EFFECT OF TRANSITION ELEMENTS ADDITION ON THE THER-

MAL PROPERTIES OF SILICATE-PHOSPHATE GLASSES MAGDALENA SZUMERA [email protected] AGH University of Science and Technology, Faculty of Materials Science and Ceramics, Department of Technology of Ceramics and Refractories The main field of my scientific activity is research and development of new materials dedicated to the natural environment protection. It is re-lated to design and manufacturing of glasses which are carriers of nutrients for plants. One of group of such materials are silicate-phosphate glasses, which structure consists of [SiO4] and [PO4] tetrahedral joined with such elements as Ca, Mg, K and metals as Cu, Fe, Mn and Zn. Thermal behavior of glasses can be described by a number of characteristic temperatures, or more precisely, temperature ranges in which physicochemical properties of the glasses undergo relatively fast changes. Characteristic thermal parame-ters are; glass transformation temperature (Tg) and change of molar heat capacity at this temperature (Dcp), as well as crystallization temperature (Tcryst) and enthalpy of crystallization (DH), or a parameter describing ther-mal durability of the glasses and assessed on the basis of Tcryst and Tg tem-peratures (DT=Tcryst-Tg). I mainly based structural investigations of glasses on the thermal analysis methods. They were used to determine the influence of modifying cations such as potassium, calcium and magnesium and transition metals cations e.g. copper, zinc, molybdenum or manganese on the course of vitri-fication and crystallization processes, and thermal stability of the investi-gated glasses. I started thermal characterization of the amorphous materials from sili-

cate-phosphate glasses from: SiO2-P2O5-K2O, SiO2-P2O5-K2O-MgO and

SiO2-P2O5-K2O-CaO systems. The investigated glasses consisted of 2 or 6

mol.% of P2O5. Amount of K2O in both groups of glasses was 6 mol.%,

while amounts of MgO and CaO changed at the cost of SiO2 introduced to

the glass. Eventually, 21 types of such glasses were manufactured. In order

to extend the investigations I designed 8 types of novel glasses from SiO2-

P2O5-K2O-MgO-CaO system in which both amounts of MgO and CaO were

changed and SiO2 content was constant [1, 2, 3, 4].

Precise and systematic analysis of the silicate-phosphate glasses re-quired enhanced studies on their synthesis, in which I used glasses from SiO2-P2O5-K2O-MgO-CaO system additionally modified with the introduc-tion of chemical microelements in the form of copper, zinc, iron, manga-

EFFECT OF TRANSITION ELEMENTS ADDITION ON THE THERMAL

PROPERTIES OF SILICATE-PHOSPHATE GLASSES

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manganese and molybdenum ions. All glasses were manufactured using syn-thetic chemicals such as: SiO2, K2CO3, CaCO3, MgO and CuO, ZnO, Fe2O3, MnO2 and MoO3. In the case of glasses containing CuO (13 types of glasses) two groups of glasses with different amount of P2O5 (2 and 6 mol.%) were synthesized. Both groups of glasses had constant amount of SiO2 and K2O and increasing content of CuO introduced at the cost of decreasing amounts of CaO and MgO which ratio was kept constant. In the case of glasses containing increas-ing amounts of ZnO (6 types of glasses), Fe2O3 (6 types of glasses) and MnO3 (10 types of glasses) amounts of SiO2 (41 mol.%), K2O (6 mol.%) and P2O5 (6 mol.%) were kept constant at the cost of decreasing amount of CaO and MgO, which ratio was kept constant. Additionally, the structural investigations were carried on the group of inverted glassy matrix i.e. phosphate-silicate (6 mol.% SiO2, 41 mol.% P2O5) modified with the addition of MoO3 (6 types of glasses) [6, 7, 8, 9, 10, 11, 12]. I used differential scanning calorimetry method to determine influence of the modifying cations on the course of glass phase transformation and crys-tallization process of the above mentioned glasses. The investigations showed that the glass phase transformation of the silicate-phosphate glasses which did not contain the microelements depends on type of the modifying cations. Its characteristic thermal parameters i.e. Tg, Dcp and Ea were decreasing in the presence of K+ cations, whereas they rose in the presence of Mg2+ and Ca2+ cations. Magnesium cation has stronger effect on the thermal parameters irrespective of the presence of only one or both modifiers. Thermal investigations on the effect of the microelements on the course of glass transformation led to conclusion, that introduction of increas-ing amounts of CuO, ZnO, Fe2O3, MnO2 and MoO3 into the structure of sili-cate-phosphate glasses (6 mol.% P2O5) causes gradual decrease of heir trans-formation temperature (Tg) as well as changes of their heat capacity (Dcp). Similar relation was observed in the case of introduction of increasing amounts of MoO3 into the structure of the inverted matrix glasses. The observed relations were explained on the basis of characteristics of atomic bonds and interaction of atoms in the structure of the investigated glasses. When comparing transformation temperatures of the glasses modified with a given transition metal (i.e. microelement) with the pure matrix glasses we can observe their decrease. It is caused by weakening of the glassy matrix by the presence of copper, zinc, manganese and molybdenum ions in voids of silicon-oxygen tetrahedra. Higher energy and thus higher Tg temperature is required by the glasses with higher content of magnesium and calcium, be-cause such elements strengthen glass structure and slow down reaching vis-cosity characteristic for glass phase transformation. Substitution of calcium and magnesium ions by ions of a given microelement which creates bonds



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with higher covalency makes the structure f silicate-phosphate glasses more rigid, which consequence is an increase of number of stresses present in the glass structure. Their relaxation requires smaller energy and thus the ob-served Tg values are lower. Apart form thermal investigations on the effect of modifying cations and selected elements on the course of vitrification of the silicate-phosphate glasses I also determined ability of the glasses to crystallization, a course of this process. In order to identify crystal phases appearing during crystallization of the silicate-phosphate glasses they were isothermally annealed at tempera-tures resulting from DSC measurements, and then analyzed using XRD method. Thermal durability of the glasses was also characterized. I found that the ability to crystallization, its course and type of crystallised phases in the case of the analyzed silicate-phosphate glasses depend on mutual proportions of glass matrix constituents i.e. MgO/SiO2, CaO/SiO2 and MgO/CaO. The effect of modifying cations on the crystallization process was espe-cially interesting. It turned out, that the glasses modified with increasing amount of MgO show increasing ability to crystallization, which was indicated by decrease of value of thermal durability indicator (DT). Their crystallization products were silicates of Mg2SiO4 type, whereas in the case of glasses modified with CaO the products were more diversified, and apart from calcium silicates of Ca2SiO4 type also calcium phosphates of Ca3(PO4)2 type appeared. It should be noted, that the type of crystal phases formed in the silicate-phosphate glasses during their heating was consistent with a character of domains pre-sent in the glasses and determined by spectroscopic methods [2, 4]. In the case of the silicate-phosphate glasses modified with addition of iron cations [6, 8] or copper ions [9, 10] I found that these ions have ten-dency to build into structure of phosphates such as Ca19Mg1.56Fe0.44[PO4]14 or Ca19Cu2(PO4)14, whereas glasses containing manganese [11] or zinc ions mainly appear in the structure of silicates (Mn7O8SiO4, Zn2SiO4). Increasing amount of MoO3 in structure of the silicate-phosphate glasses favours crystal-lisation of complex phosphates (Ca9MgK(PO4)2) but also silicates of CaMgSi2O6 or Ca2MgSi2O7 type. Molybdenum ions show tendency to crystallize in the form of calcium molyb-denate of powellite type (CaMoO4). While in the case of devitrificates based on the inverted matrix glasses (i.e. phosphate-silicate glasses) I found that in-crease of MoO3 content retards their crystallization process [12]. Determination of the course of crystallization of all investigated silicate-phosphate glasses was based on thermodynamic analysis of formation of com-pounds which are products of their crystallization by calculations of standard free enthalpy which defines probability of their formation. I demonstrated, that parameters determining type of the crystallizing phases are apart from



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from chemical affinity, factors of crystallochemical nature, which are related to strength of chemical bonds between oxygen ions and glass structure-forming and modifying ions. Investigations on type of phases crystallizing during heating of the ana-lyzed silicate-phosphate glasses also allowed to learn middle-range order of the glass structure and determination of chemical composition of domains of the middle-rage order in the glass structure and their effect on biochemical properties of the glasses. The results were consistent with the character of domain existing in the analyzed glasses and determined by the spectroscopic methods. Such approach to the glass structure analysis has not been so far used in the glass state science. My investigations enabled to widen the knowledge of glassy state crys-talochemistry of the silicate-phosphate glasses in relation to their structure. Results of the studies especially pointed out the role of crystalochemical fac-tors in establishing of their thermal durability and their chemical activity, which was shown by studies on solubility of the glasses. As a result of the in-vestigations, basing on the chemical bonds strength expressed in terms of the Görlich parameter between glass constituents, and for a wide range of com-positions of the model glass I was able to prove and explain coincidence be-tween seemingly different phenomena: glass crystallization (thermal durability) and glass solubility (chemical activity) in function of their chemical composi-tion [1-12]. Acknowledgments I would like to express a gratitude to Polish Society of Calorimetry and Thermal Analysis for appreciating my scientific work by “the W. Świę-tosławski award for the scientific achievements in calorimetry and thermal analysis for young scientist”. I would also address special thanks for Professor Irena Wacławska, who always supported me still encourages to scientific de-velopment. For me it is a great achievement, great honour and encourage-ment for further work. I cordially thank. References 1. I. WACŁAWSKA, M. SZUMERA, Thermal analysis of glasses for proecologi-

cal applications, Journal of Thermal Analysis and Calorimetry, 2003, vol. 72, 1065–1072.

2. M. SZUMERA, I. WACŁAWSKA, W. MOZGAWA, M. SITARZ, Spectro-scopic study of biologically active glasses, Journal of Molecular Structure, 2005, vols. 744–747, 609–614.



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3. I. WACŁAWSKA, M. SZUMERA, Influence of MgO(CaO) on the structure of silicate-phosphate glasses : TA and NMR study, Journal of Thermal Analysis and Calorimetry, 2006, vol. 84 no. 1, 185-190.

4. M. SZUMERA, I. WACŁAWSKA, Spectroscopic and thermal studies of sili-cate-phosphate glass, Journal of Thermal Analysis and Calorimetry, 2007, vol. 88 no. 1, 151–156.

5. I. WACŁAWSKA, M. SZUMERA, Reactivity of silicate-phosphate glasses in soil environment, Journal of Alloys and Compounds; 2009, vol. 468, 246–253.

6. I. WACŁAWSKA, M. SZUMERA, Thermal behaviour of Fe-doped silicate-phosphate glasses, Journal of Thermal Analysis and Calorimetry, 2010, vol. 101, 423-427.

7. I. WACŁAWSKA, M. SZUMERA, Influence of B2O3 on the structure and crystallization of soil active glasses, Journal of Thermal Analysis and Calo-rimetry, 2010, vol. 99, iss. 3, 879-886.

8. I. WACŁAWSKA, M. SZUMERA, P. STOCH, M. SITARZ, Structural role of Fe in the soil active glasses, Spectrochimica Acta, Part A: Molecular and Bio-molecular Spectroscopy, 2011, vol. 79, iss. 4, 728-732.

9. J. SUŁOWSKA, I. WACŁAWSKA, M. SZUMERA, Characterization of ther-mally induced of crystalline phases in CuO-containing silicate-phosphate glasses, Journal of Thermal Analysis and Calorimetry, 2012, vol. 108 iss. 2, 657-663.

10. J. SUŁOWSKA, I. WACŁAWSKA, M. SZUMERA, Effect of copper addition on glass transition of silicate-phosphate glasses, Journal of Thermal Analysis and Calorimetry, 2012, vol. 109 iss. 2, 705-710.

11. M. SZUMERA, I. WACŁAWSKA, Thermal study of Mn-containing silicate-phosphate glasses, Journal of Thermal Analysis and Calorimetry, 2012, vol. 108 iss. 2, 583-588.

12. M. SZUMERA, I. WACŁAWSKA, Effect of molybdenum addition on the thermal properties of silicate–phosphate glasses, Journal of Thermal Analysis and Calorimetry, 2012, vol. 109, 649-655.

Technical Articles

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Carbon aerogels – the new field for thermoanalytical studies Václav Slovák, Petra Veselá, Jana Štefelová, Monika Palkovská, Tomáš Zelenka Department of Chemistry, Faculty of Science, University of Ostrava e-mail: [email protected] 1. Introduction

Carbon is one of the elements which people use from the ancient times. All of the basic discoveries connected with carbon or carbonaceous matter can be considered as significant milestones in the human history. Con-trolling of combustion of carbonaceous materials (fire) was dramatic change in the life of early humans. Conversion of wood to charcoal gave a superior source of intensive heat for many applications. Charcoal usage in metallurgy and as a basic constituent of gunpowder had probably the greatest impact. The importance of coal in the history is undoubted and pyrolysis of coal to coke provided practically unlimited (in the 18th century) source of fuel for iron making. Increasing production of inexpensive iron was one of the circum-stances enabling the Industrial Revolution. Nowadays although it is often hid-den, carbon can be found in the background of many industrial processes from extra large scale productions of steel or rubber goods to more special-ized manufacturing of activated carbons, pigments, synthetic diamonds, etc. About 40 years ago the chemistry of carbon seemed to be well devel-oped and any surprising discoveries could not be expected. The situation can be illustrated by the fact that at the beginning of 1970s some chemists (E. Osawa [1], R. W. Henson [2]) theoretically predicted existence of stable spherical carbon molecules, but this idea was not accepted by scientific com-munity. From that time the situation has changed dramatically. Starting with discovery of fullerene C60 in 1985 (Nobel Prize in 1996), a large group of a new “spherical” carbons has been synthesized including different “nanoballs” and “nanotubes” (single- or multiwalled) which are commercially available to-day. Another great step in carbon chemistry was isolation of graphene – a sin-gle free-standing atomic layer of carbon – in 2004 (Nobel Prize in 2010). Cu-riously it was made by physicists by a very simple technique using adhesive tape (scientifically called micromechanical cleavage). The remarkable elec-tronic properties of graphene led to intensive study of these (and related) ma-terials and the interest continues till now. Fascinating growth of carbon chemistry in the last decades could be discussed but it is not the aim of this text. So let’s focus our attention just to one of the very new carbonaceous material – carbon aerogels.

Carbon aerogels – the new field for thermoanalytical

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2. Carbon aerogel – what is it? Gels are “jelly-like” materials which consist of three dimensional cross-linked solid network soaked with a liquid. This liquid phase forms the most of the gels mass. The term “aerogel” can be understood as gel in which liquid phase is replaced by air and the solid state network is conserved. The best way how to dry gels and preserve the solid structure is removing the liquid under su-percritical conditions when no gas-liquid interface (and no capillary tension) exists. This approach was used for the first time by S. S. Kistler [3] who used alcohol, ether or propane as liquids suitable for supercritical drying and was able to dry many different gels with no changes in their volume and structure. Today the most common is drying of supercritical CO2. Some authors use the term “aerogel” exclusively for materials prepared with supercritical drying and the other “dry gel”-like materials name as cryogels (freeze dried) or xe-rogels (dried under ambient pressure). In some literature, the term “aerogel” covers all of these groups of materials (as in this text). In 1989, R. W. Pekala and F. M. Kong [4] published the first synthesis of car-bon aerogel (CA) and their approach can be adopted as typical pathway of CAs preparation. The first step consists of condensation of suitable organic monomers in solu-tion, forming the organic gel and its curing. Pekala and Kong originally used alkaline catalysed condensation of resorcinol and formaldehyde in aqueous solution with subsequent cross-linking of the solid state structure in a weakly acid bath. Very different monomers, conditions and catalysts were tested from that time, but the resorcinol-formaldehyde (RF) gels are investigated till today and seem to be the best for many applications. Cellulose-based gels represent one of the perspective alternatives for RF gels which can be pre-pared from renewable sources (cellulose or its derivatives) by gelation and regeneration from suitable ionic liquids. The second step of CAs preparation is drying of organic gel to organic aerogel. It is often made by exchange of the gel liquid (water) with acetone which can be readily replaced with liquid carbon dioxide. Heating above criti-cal temperature of CO2 and slow depressurization gives dry organic gel. If the solid structure of the gel is strong enough, lyofilization or even drying under ambient pressure can be applied without significant lost of volume and degra-dation of the structure (Fig. 1).

Pyrolysis in inert atmosphere is the third and last step of CAs prepara-tion. Temperatures between 500 – 1200°C are commonly used; times of heating are usually in hours. Carbon aerogels are black solids with very low volumetric density (≈0.1 – 0.4 g cm−3), developed meso- and microporosity and high surface ar-eas (80 – 2000 m2 g−1), high thermal and chemical stability in inert atmos-phere, with good mechanical properties and electrical conductivity. The struc-


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Fig. 1 (a) Different resorcinol-formaldehyde aerogels (xerogels) dried at am-bient pressure, (b) freeze-dried aerogels (cryogels) from cellulose resp. cellu-lose acetate (white resp. orange coloured).

ture of RF carbon aerogels usually consists of the globular particles intercon-nected by necks. The holes between particles forms continuous mesoporos-ity, while inside the particles system of micropores can be developed. CAs based on cellulose can have different assembly of porosity (Fig. 2).

Fig. 2 SEM images of resorcinol-formaldehyde CA (a) and CA based

on cellulose (b). The basic advantage of CAs in comparison with activated carbons is the possi-bility of controlling of their porosity and surface properties. Since the relation between the parameters of preparation and the textural parameters is still under investigation it is strongly believed that preparation of CAs with prop-erties required for different applications will be available in the near future. The applications of CAs are based on their properties. They can be used as effective sorbents from liquid or gaseous phase (heavy metals, organic dyes, hydrocarbons, CO2, etc.) and their sorption capacity can serve the possibility of gas storage (H2). Their chemical stability together with possibility of their doping with metals enable their applications as catalyst supports for heteroge-neous catalysis. Electrical conductivity makes them suitable for the electro-chemical applications – electrodes in fuel cells and supercapacitors are proba-bly the applications with the highest attraction of scientific interest.


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3. Possibilities of thermal analysis in the field of carbon aerogels The following selection of results was obtained by the student re-search group of “carbon aerogelists” at Department of Chemistry, Faculty of Science, University of Ostrava. The team is focused on the study of two se-ries of CA’s: classical resorcinol-formaldehyde aerogels and cellulose based aerogels. The aims of the research can be summarized as:

• preparation of effective sorbents for heavy metals and organic pol-lutants removal from the aqueous environment;

• accelerating the pathway of carbon aerogels preparation; • excluding of supercritical drying from the preparation process.

Non-isothermal thermoanalytical experiments shown below were per-formed on apparatus allowing simultaneous TG/DSC measurement (Netzsch STA 449C or Setaram SetSys Evolution, the latter coupled with the mass spectrometer Pfeiffer QMG 700). The most of results were presented on conferences focused on ther-mal analysis or material science (e.g. [5-13]). 3.1. Thermoanalytical determination of temperature of pyrolysis Pyrolysis (heating in inert atmosphere) is widely used industrial and also laboratory process of carbonization of organic matter including organic aerogels. One of the basic problems in this field which can be solved by thermoanalyti-cal methods is selection of appropriate temperature level. The temperature has to be high enough to ensure required conversion but also as low as possi-ble to decrease energy requirements (economical point of view). Some types of organic aerogels (e.g. cellulose based CAs, [9,10]) show very simple pyrolytic behaviour and it is very easy to determine adequate tempera-ture from single TG measurement (Fig. 3).

Other samples undergo more complicated transformations during car-bonization (Fig. 4) [5–7] and simple selection of the highest temperature at which the last pyrolytic step is finished (about 800°C in Fig. 4) need not to be the optimal choice. Laboratory scale testing of pyrolysis of the same sample as in Fig. 4 (heating of tens of grams of the sample in laboratory tubular oven in the flow of nitrogen for an hour) showed that the temperature about 500°C is quite enough for evolution of high surface area of resulted CAs (Fig. 5).

For the explanation of this finding, evolved gases were analysed by mass spectrometer during repeated experiments [5,12]. The results are sum-marized in Fig. 6. Three typical steps of decomposition can be identified on the basis of TG measurements and evolved gas analysis. The residual humidity and other volatile components (formaldehyde) are lost below ≈200°C. Above this tem-


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Fig. 3 TG of different cellulose based aerogels pyrolysis and selection of ade-quate pyrolysis temperature (400 °C).

Fig. 4 TG and DTG of pyrolysis of resorcinol-formaldehyde organic aerogel. Three steps of decomposition can be identified (grey dotted lines).

temperature dehydroxylation (in the form of reaction water) and decarboxy-lation (evolution of CO2) starts. At higher temperatures (above ≈450°C) the cracking of C–C bonds in the aliphatic parts of structure, continuing degrada-tion of functionalities and dehydrogenation can be expected on the basis of observed evolution of hydrocarbons, CO2 and H2 (Fig 6).


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Fig. 5 Surface area (BET) of carbon aerogels prepared by laboratory scale pyrolysis of the same organic precursor (as in Fig. 4) at different tempera-tures.

Fig. 6 TG and DTG of pyrolysis of resorcinol-formaldehyde organic aerogel (as in Fig. 4) together with selected gas analysis (mass spectrometry). Red dotted line indicates sufficient temperature level for laboratory scale pyroly-sis.

Comparison of these experimental results with laboratory scale ex-periments shows that the sufficient temperature of pyrolysis can be derived from non-isothermal thermoanalytical measurements of pyrolysis as the tem-perature, at which the last pyrolysis step has been started. This temperature level enables finishing the pyrolysis processes when the system is kept at this temperature for appropriate time.


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3.2. Mass loss during pyrolysis and sorption properties of CAs One of our attempts to prepare carbonaceous aerogel-type materials for adsorption of metals from aqueous solutions includes incorporation of the nitrogen atoms into the carbonaceous structure. Nitrogen bonded as amino-, imino- or CN-groups should increase the surface alkalinity and capability of the sorbent to coordinate heavy metal ions. Different types of nitrogen-doped carbon aerogels were prepared [11–13] by adding of nitrogen containing compounds (3-hydroxypyridine, 3-aminophenol, melamine) to initial polycondensation mixture together with nitrogen free samples. Relation between their pyrolysis behaviour (parameters available from thermoanalytical measurements) and capacities for sorption of Ni(II), Pb(II) and Cu(II) was tested. It was found that with increasing mass loss during pyrolysis (the shape of TG and DTG curves was similar as in Fig. 4), adsorption capacities also in-crease for tested metal ions (an example in Fig. 7). Similar relationships were found for mass loses determined for heating to different temperatures (500°C or 1000°C) and even for mass loses determined from measurements with iso-thermal step added to the temperature program.

Fig. 7 Relation between mass loss of organic aerogels during pyrolysis and their ability to adsorb metal ions.

These results are quite surprising, because the opposite relationships (increasing adsorption capacity with decreasing mass loss) have been ex-pected. The correlation found can be probably explained by releasing the at-oms, molecules, groups etc. which are “not connected” with sorption during


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during pyrolysis. In other words, adsorption sites are “concentrated” with increasing amount of released gaseous products. Mass losses (and also ad-sorption capacities) were higher for two N-doped aerogels doped by 3-hydroxypyridine and melamine, thus, it can be expected that nitrogen atoms are in these two cases incorporated in the structure to positions that are available for adsorption and in thermally stable form. Extending this study with analysis of evolved ammonia during pyrolysis lead to conclusion that amino groups presented in N containing precursor and bonded to aromatic ring are lost during pyrolysis and has no effect to sorption properties while nitrogen bonded as a part of aromatic structure is more stable and can increase ability of carbon aerogel for sorption of metal ions.

3.3 Thermoanalytical measurements of condensation step of CAs preparation Condensation step of carbon aerogels preparation is not easily acces-sible for direct measurements as it starts in liquid phase and finishes in solid state. At the beginning of our “playing” with carbon aerogels we have just tried the possibility of thermoanalytical approach to this field [7,8]. The condensation reaction of resorcinol and formaldehyde is exother-mal; it is not accompanied with any mass change and it occurs in a tempera-ture range with upper limit given by the boiling point of water (used solvent in general). It should be possible to measure the extent of reaction by DSC techniques. Simultaneous TG signal can be used for checking the amount of evaporated water and searching the best conditions for its minimization with-out tight closing of the crucible (the measurement should be done under am-bient pressure). A series of experiments led to suitable experimental condi-tions: heating of 20-30 µl of polycondensation mixture from 30 to 100°C with heating rate 2 K min−1 in Pt/Rh crucibles covered by lid slightly sealed with laboratory grease gives reproducible mass loss of water in the range 13 – 15 %. DSC curve (Fig. 8) measured for condensation mixture consists of condensation itself and endothermal effect of water evaporation (red curve). As we proved, DSC signal of pure water (blue line) is well repeatable in ac-cordance with repeatable mass loss from TG, so it can be used as a baseline for correction of measured DSC signal. Simple subtraction of both DSC curves shows DSC signal for condensation itself (green line).

Testing of reproducibility of such measurements showed that the agreement of repeated measurements is satisfactory although we used the thermoanalytical equipment which is not primarily constructed for such low temperature range.


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Fig. 8 DSC curves of resorcinol-formaldehyde condensation (red line), water evaporation under the same conditions (blue line) and their subtraction (green line).

Developed methodology of DSC measurement enabled studying of the effect of catalyst concentration on the rate of condensation (Fig. 9) and con-firmed expected dependence – increasing content of catalyst leads to de-crease of temperature of condensation DSC peak (higher reaction rate).

Fig. 9 The effect of catalyst content (HCl) on the DSC curves of resorcinol-formaldehyde condensation.


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Consequently it was tried to relate rate of condensation step of CAs preparation with their surface properties. It was shown that (for group of analogous initial mixtures differing only in present catalysts) the temperature of DSC peak of condensation (which is the measure of reaction rate) is in good correlation with surface area of resulting carbon aerogel (Fig. 10).

Fig. 10 DSC curves of condensation of resorcinol and formaldehyde in the presence of different catalysts. The values of surface area were measured by adsorption of nitrogen at −196°C (BET).

4. Concluding remarks We believe that carbon aerogels are prospective new materials and after solving some problems with their controlled preparation they will become widely used in many applications. Thermal analysis is excellent technique which can be valuable in this field – above mentioned examples are only small selection and can not cover all the possibilities. Research area is opened at least in these other fields:

• kinetics and mechanism of measurable processes (pyrolysis, drying, condensation);

• testing of surface properties in terms of thermoporometry; • thermomechanical properties of organic and carbon aerogels; • activation of carbon aerogels by interaction with gases at higher

temperatures. Acknowledgement The work of our group is partly financed by the project Institute of environ-mental technologies, reg. no. CZ.1.05/2.1.00/03.0100 supported by Research and Development for Innovations Operational Programme financed by


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Structural Funds of European Union and from the means of state budget of the Czech Republic.

References [1] Osawa, E. Kagaku 1970, 25, 854. (in Japanese) [2] Thrower, P. A. Carbon 1999, 37 (11), 1677. (Acknowledgement to R. W. Henson in Editorial) [3] Kistler, S. S. Nature 1931, 127 (3211), 741. [4] Pekala, R. W.; Kong, F. M. Polym. Prepr. (Am. Chem. Soc., Div. Polym. Chem.) 1989, 30, 221. [5] Palkovská, M.; Slovák, V. Study of the mechanism of pyrolysis of organic aerogels by TA-MS. JUNIOR EUROMAT, Lausanne, 2012. [6] Slovák, V.; Veselá, P. Kinetics of pyrolysis of N-doped carbon aerogels. 3rd Joint Czech-Hungarian-Polish-Slovak Thermoanalytical Conference, Stará Lesná, 2011. [7] Slovák, V.; Martiníková, S.; Kalina, J. Thermal analysis and preparation of carbon aerogels. ESTAC10, Rotterdam, 2010. [8] Slovák, V.; Veselá, P.; Štefelová, J.; Palkovská, M. Carbon aerogels - the new field for thermoanalytical studies. CCTA11, Zakopané, 2012. [9] Štefelová, J.; Slovák, V. Cellulose based carbon aerogels. JUNIOR EUROMAT, Lausanne, 2012. [10] Štefelová, J.; Slovák, V. Subcritically dried cellulose - based carbon aerogels with high surface area. 4th EUCHEMS, Praha, 2012. [11] Veselá, P.; Slovák, V. Pyrolysis of N-doped organic aerogels with relation to sorption properties. J. Therm. Anal. Calorim. 2012, 108, 475. [12] Veselá, P.; Slovák, V. N-doped carbon aerogels: the possibilities of nitrogen incorporation into the structure with respect to adsorption usage. JUNIOR EUROMAT, Lausanne, 2012. [13] Veselá, P.; Slovák, V. TA-MS as a tool for monitoring of N-doped carbon aerogels preparation. CCTA11, Zakopané, 2012.

Book Review

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Földvári M.: Handbook of Thermogravimetric system of Minerals and its use in geological practice. 2011. Budapest, Occasional Pa-pers of Geological Institute of Hungary, Volume 213. p. 180. ISBN

978-963-671-288-4 Thermal analysis plays a specific role in the identification and quantita-tive determination of mineral components of rocks. In spite of the fact that minerals were the first group of materials studied regularly by using ther-moanalytical methods, the potential offered by these methods is still not fully utilized in the field of earth sciences. From quantitative phase analysis point of view it is very important that thermogravimetric measurements give direct and absolute values for thermal reactions making stoichiometric calculation possible. The author analyzed about 30000 geological samples over more than 40 years. Gained experiences over the decades enable the systematization of the thermal reactions of minerals and gave the grounds for the compilation of this book. In the first chapter basic information on thermal analysis, thermoana-lytical techniques, thermoanalytical nomenclature, thermoanalytical measure-ment parameters, the role of experimental conditions, calibration and stan-dardisation are summarized. This chapter also deals with different technical (derivative, second derivative methods, controlled rate thermal analysis, evolved gas analysis techniques) and evaluation (quantitative determination based on mass-change, calculation of virtual kinetic parameters, and using of corrected decomposition temperature which introduced by the author) methods. In the next part different kinds of possible thermal reactions of miner-als are systematised focusing on thermal decomposition reactions. An ample chapter discusses different water types in minerals and their thermoanalytical features. The most detailed part regarding this subject is the types of interlayer water in clay minerals. The system of decomposition reactions based on the electronegativity of the cation, related to given anions (bonding strength) and to the complex-ity of the structure (diffusion). In the chapter “Thermogravimetric curves and their interpretation by stoichiometric processes of minerals” a total of 148 figures show thermoana-lytical curves up to 1000 °C for 114 minerals investigated by the author dur-ing geological routine work. Thermal processes are interpreted on the basis of thermoanalytical reaction equations or the description of the reaction. For thermal reactions accompanied by mass changes a method for quantitative determination is also presented.

Book Review (continued)

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In the round of special geological applications many examples are dem-onstrated using corrected decomposition reactions. In a short chapter for instance there are publications from many fields of geology applying thermal methods for solving specific geoscientific problems. The book is illustrated by 220 figures and 74 tables. The number of references is 1195.

Meeting Announcements

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23rd CTAS ANNUAL WORKSHOP AND EXHIBITION

Dear Colleagues, Canadian Thermal Analysis Society (CTAS) will be holding its 23rd Annual Workshop and Exhibition on May 07-08, 2013 at the University of Ontario Institute of Technology, North Campus, 2000 Simcoe St. North, Oshawa, On-tario, L1H 7K4, Canada. The two-day CTAS Workshop and Exhibition will start with a one-day training session, followed by one-day technical session with oral and poster presentations while the Instrument exhibitions will occur on both days. There will be a special issue of the Journal of Thermal Analysis and Calo-rimetry (JTAC), dedicated to the 23rd CTAS Annual Workshop and Exhibition and the full papers will be published after the positive review at least by two referees. CTAS invites you to present a paper and/or poster in this Work-shop and submit the full papers to JTAC Associate Editor, Dr. Subhash Mo-jumdar ([email protected]). The subject matter may cover any aspect of thermal analysis techniques, hyphenated techniques and applications to various materials. To recognize the contribution by students to the field of thermal analysis, two awards will be presented to the student giving the best poster ($50) and oral ($200) presentations at the Workshop. This occasion is an excellent opportunity to meet other thermal analysts and exhibitors, and to learn new applications in thermal analysis. Please show your support to the Canadian thermal analysis community by attending, presenting a paper and/or exhibiting your instruments in the Workshop and Exhibition. Please visit www.ctas.org and/or contact Dr. Subhash Mojumdar for more information. The deadline for abstract submission is February 15, 2013. Please send your abstracts to Dr. Subhash Mojumdar ([email protected]), and your registration/membership and/or exhibi-tion reservation form to Dr. Pierre-Claver Nkinamubanzi ([email protected] or fax 613-954-5984). I look forward to meeting you at the 23rd CTAS Annual Workshop & Exhibition. Sincerely, Subhash Mojumdar CTAS Program Chair

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4th Joint Czech-Hungarian-Polish-Slovak Thermoanalytical C o n f e r e n c e , 2 4 . 6 . -

27.6.2013 Pardubice, Czech Republic WWW.THERMAL-ANALYSIS.CZ HISTORY AND SCOPE The 4th Joint Czech-Hungarian-Polish-Slovak Thermoanalytical Conference is another in a series of meetings of the four national thermoanalytical groups – Czech, Hungary, Polish and Slovak. The conference originated within 2005-2006 when the Heads of national thermoanalytical groups (J. Šesták – Czech Republic; Cs. Novák – Hungary; B. Pacewska – Poland; P. Šimon – Slovakia) decided to merge their local conference into an international one with a higher scientific impact. After Sopron (Hungary, 2007), Zakopane (Poland, 2009) and Stará Lesná (High Tatras – Slovakia, 2011), in 2013 the conference is held on 24-27 June 2013 in Pardubice (Czech Republic). The 4th joint thermoanalytical conference of four states is going to be organized by Czech Group for Thermal Analysis (Czech Chemical Society) and University of Pardubice, Faculty of Chemical Technology under the patronage of the Rector of University of Pardubice professor Miroslav Ludwig. TOPICS The main aim of the Joint Conference of four states is promoting the scientific discussions and exchange of ideas between researchers involved in thermal analysis and calorimetry. These techniques are used in various fields of scientific research. The main topics of the Conference are the applications of thermal analysis and calorimetry to studying inorganic, organic and biological materials, kinetics and reactivity of solids, solution calorimetry, food systems etc. Very important issue is the progress and new solutions in theory and instrumentations and technical applications. GENERAL INFORMATION Conference will be held from 24th to 27th June 2013. T h e l a n g u a g e o f c o n f e r e n c e i s E n g l i s h . The following presentations are planned: plenary lectures (40 min.), oral presentations (25 min.) and posters (90x110 cm). Registration will be open from January 2013 (on line on conference web site). Starting from January 2013 (up to 31.3.2013) the payment and full text (max. 4 pages) of lectures and posters will be accepted.


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4th Joint Czech-Hungarian-Polish-Slovak Thermoanalytical Conference (contd.) The accepted contributions can be published in the Special Issue of Journal of

Thermal Analysis and Calorimetry. IMPORTANT DEADLINES: Registration and full texts submission deadline: 31.3.2013 Payment: 31.3.2013

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MEDICTA2013 11th Mediterranean Conference on Calorimetry and Thermal Analy-

sis Athens, Greece June 12-15, 2013

2013 Mediterranean Conference on Calorimetry and Thermal Analysis (MEDICTA2013) is being jointly organized by the HSTA and the GECAT, AI-CAT, GICAT, IGTAC and CATPOR, which have successfully cooperating in the area of calorimetry and thermal analysis. The conference will be held from 12 15 June 2013 in Athens. It consists of plenary, key and invited lectures, oral and poster presentations, covering all the aspects of recent experimental, theoretical, simulation and applied devel-opments on thermal analysis and calorimetry.

Conference Chairman: Prof. Costas Demetzos Conference Agency: k.provoli ([email protected], Ms Vicky De-

lidimitriou)

Please visit web site http://www.hsta.gr.medicta2013

Good Day to All ICTAC Members, Please allow us to extend a warm invitation to join us in Orlando, Florida for the 2016 ICTAC Conference, hosted by your colleagues in NA-TAS (North American Thermal Analysis Society). We are currently in ne-gotiations to provide you with the best venue and activities possible for col-laboration and camaraderie. Please stay tuned to our website beginning in 2013 as we bring you continuous updates to our plans: http://www.natasinfo.org/ We are looking forward to a fruitful week that should be enjoyable for your family, too. While attendees are in comfortable, professional set-tings full of innovative ideas and discussions, your families can enjoy all that Orlando has to offer (at discounted rates of course!). The area is teeming with options such as Walt Disney World, Sea World, and Universal Studios. We want your experience with us to be an amazing combination of science and imagination that inspires you to succeed. In the words of Walt Disney, “If you can dream it, you can do it.” Sincerely, NATAS Executive Council

Tina Adams, Executive Councilor & 2016 Conference Chair Bob Howell, Meetings Councilor Eric Shoch, President Joe Menczel, Vice-President/President-Elect Tom Ramotowski, Treasurer Prashanth Badrinarayanan, Secretary Quentin Lineberry, Education Councilor Publications Councilor, Queenie Kwok

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