Institut für Technische Chemie und Makromolekulare Chemie

Size: px
Start display at page:

Download "Institut für Technische Chemie und Makromolekulare Chemie"

Transcription

1 Rheinisch-Westfälische Technische Hochschule Aachen Institut für Technische Chemie und Makromolekulare Chemie Lehrstuhl für Makromolekulare Chemie MARC Zentrum für Magnetische Resonanz Annual Report 2001 Redaction: All members of the institute (eds.: B. Blümich, G. Breuer, cover: Klaus Kupferschläger)

2 2 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie Contents 1. A Review of The Institute Staff How to Reach the Institute 9 3. Teaching Lectures and Courses Practical Lab Courses Research Reports Public Activities Publications Talks Posters Honorary Activities Lectures of Visitors to the Institute 82

3 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 3 1. A Review of 2001 NMR at ITMC Nuclear Magnetic Resonance or NMR is a surprisingly versatile method of radiofrequency spectroscopy. Telecommunication with radio waves between spectrometers in a laboratory with magnetic nuclei of atoms in magnetic fields can be used for a manifold of purposes: NMR spectroscopy is probably the most important analytical method the chemist uses for structural analysis of molecules. NMR imaging or magnetic resonance tomography is a well known diagnostic tool in medicine. Mobile NMR spectrometers are operating in bore holes for oil well logging to help analyze the surrounding porous rock formations for oil, water and gas contents, and small portable NMR sensors are being developed for product and process control in the food and polymer industries. In a different context most of these types of NMR are the subject of research of Prof. Blümich s team at the Institute of Technical Chemistry and Macromolecular Chemistry (ITMC). The governing topic is material science, in particular polymer science, and NMR. The research work focuses on NMR methods and hardware guided by applications to polymers and elastomers, to fluid flow in chemical engineering, and to noninvasive product and process control in a manufacturing environment. Close contact to industrial and engineering partners defines the topics of diploma and doctoral work in the area of the applied sciences. Magnetic Resonance Center MARC The NMR spectrometers are accommodated in the magnetic resonance center MARC (Fig. 1). The center serves the analytical needs of the chemistry research groups at the Seffent-Melaten campus of RWTH. At the same time it forms a nucleus for interdisciplinary research. The spectrometers available at MARC are listed in Tab. 1. Two 300 MHz spectrometers are used for routine high-resolution liquid-state NMR. Following the retirement of Dipl.-Ing. B. Dederichs, Frau Ines Bachmann now coordinates the user activities and service measurements. One 500 MHz spectrometer is dedicated to solid-state NMR spectroscopy. It is used for research and routine work and is accessible to the members of the chemistry department. Dr. Marko Bertmer is in charge of its operation. A 200 and a 300 MHz spectrometer are used for imaging and flow studies with Dr. D. E. Demco and Dr. S. Stapf as Fig. 1: View of the Magnetic Resonance Center MARC with the DMX 300, DSX 200, and DSX 500 solid-state spectrometers. The DSX 200 and DMX 300 spectrometers are also suitable for imaging.

4 4 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie Table 1. Spectrometers in MARC spectrometer use manufactured/renovated DMX 300 imaging, flow NMR 1994/2000/2001 DSX 200 imaging, flow NMR 1997 DSX 500 solid-state NMR spectroscopy 1998 DPX 300 liquid-state NMR spectroscopy 1994 AC 300 liquid-state NMR spectroscopy 1995 Stelar field cycling relaxometer 2001 ESR electron spin resonance 1983/1992 supervisors. Furthermore, Dr. Stapf has acquired a field cycling spectrometer, which now further widens the broad range of NMR instruments at the center. In an annex to MARC, the so-called MOUSEoleum, work on the NMR-MOUSE is pursued, and the members of the DFG-Research consortium on Surface NMR of Elastomers and Biological Tissues construct and test a unilateral NMR imager. Furthermore, a section of the annex has been reserved for setting up a polarizer for NMR with hyperpolarized Xenon gas, an activity headed by Dr. Stephan Appelt from the Research Center in Jülich in cooperation with Dr. Peter Blümler in Mainz and Dr. Song-I Han, who received her doctoral degree from RWTH in 2001 and is now supporting the contacts of the Xenon NMR activities in Jülich, Aachen, and Mainz. Research Activities The research activities can be grouped by method into the three categories: NMR spectroscopy, NMR imaging, and mobile NMR. These methods are applied to different fields of investigation, where the methods provide the links between the Fig. 2: NMR methods and research topics

5 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 5 Table 2. Projects, cooperation partners, and sponsors Project Coordinator Cooperation partners Sponsors Functional supramolecular materials Bertmer MnemoScience, INTECH BMBF Dynamically loaded Elastomers NMR in medicine and material science Chemical extraction and reaction Demco Bayer, DIK, Freudenberg, INTECH, Parker, Rheinchemie, TUHH, Vibracoustic DLR Demco MPI Köln, MPI Leipzig, Tel Aviv BMBF University Stapf Engineering at RWTH Aachen DFG (SFB) Surface NMR Blümich Medicine, electrical and mech. Engineering at RWTH Aachen State assessment of electrical insulations Biocompatibility of implant materials Blümich Institute for High-Voltage Engineering Bertmer DWI, INTECH, MnemoScience BMBF DFG Forschergruppe DFG Schwerpunktprogramm Cultural Heritage Blümich Bruker, CNR Rome EUREKA different types of projects (Fig. 2). Each project group is headed by one or more senior staff members who are coordinating individual research projects (Tab. 2). The projects on functional materials deal with investigations of model and technical polymer materials for particular applications. One example is polymers in medicine, which may require shape memory and drug release functionalities. The activities in flow and diffusion NMR are an expanding field of research, which is a logical continuation of NMR imaging. In flow NMR gradient-field pulses are used to encode difference images which provide information on distances that molecules travel in a given time. Equivalent information is obtained by measuring velocity and acceleration distributions, which provide a sensitive means for characterizing all kinds of phenomena associated with translational motion such as diffusion and flow of fluids and granular media. Applications of such studies are in chemical extraction and polymer processing technologies. Extensive collaborations exist at RWTH with chemical engineering in studying fluid dynamics and reaction associated with chemical extraction (SFB). Research in catalysis is continuing in collaboration with Prof. Dr. A. Jess who has left Aachen to assume a Chair at the University of Bayreuth. In this project the chemical and the morphological structures of heterogeneous catalysts are studied by spectroscopy and flow NMR following coking and regeneration processes. Relaxometry is a new activity initiated by Dr. Stapf, who acquired a field-cycling spectrometer for his research on molecular dynamics via field-dependent NMR relaxation studies. Such investigations are important to help understand the interactions and type of motions of molecules in confined environments, where the confinement may arise from cross-links in elastomers or from the porous structure of a host matrix like a heterogeneous catalyst. Work in mobile NMR deals with the NMR-MOUSE as a unilateral NMR sensor for noninvasive inspection of large objects. Product and quality control in the rubber industry are the central objective with perspectives in process control as well as in the inspection of historical objects of art such as buildings and monuments. In the

6 6 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie research consortium Surface NMR of Elastomers and Biological Tissue, the NMR- MOUSE is further developed into a unilateral NMR imager with potential applications in medicine and the rubber industry. NMR of Elastomers is a traditional field of research in the group. Starting from NMR imaging and an analysis of relaxation contrast, the field is evolving into investigating more basic concepts of elastomer networks by calculating and measuring the angular dependent NMR response of strained and deformed elastomers networks considering relaxation times and multi-quantum signals. There is a close interaction with the activities in mobile NMR, because strained elastomers are very conveniently measured by unilateral NMR devices. In addition to addressing fascinating questions in fundamental science, the implications of this work are also of interest to developing concepts of NMR fur use on the factory floor. The NMR service includes the measurement of conventional high-resolution 1D and 2D liquid-state spectra for structural chemical analysis and the measurement of high-resolution solid-state spectra. Both types of spectroscopy are operated in a users mode, where operators from different research teams learn how to operate the NMR spectrometers under supervision of Frau Bachmann or Dr. Bertmer and subsequently run their own spectra. The service of liquid-state NMR is mostly used by the members of ITMC and the neighboring Biology department. The solid-state NMR facilities are mainly used by ITMC and the Institute of Fuel Chemistry. An exciting new field of research is the work on NMR with hyperpolarized xenon. Xenon is an inert gas and its nuclear polarization can be enhanced by some 6 orders of magnitude through laser techniques. Dr. Stephan Appelt from the research center in Jülich is collaborating with us to transfer the xenon polarization to other nuclei for spectroscopy and imaging. This work is anticipated to link with projects in relaxometry, elastomers, imaging, and mobile NMR. A research triangle of Jülich, Aachen and Mainz has been formed where the collaboration partners focus on the method itself, materials applications, and medical applications. The scientific work of each group member is described in more detail in the following project abstracts. In addition to their research, each student working on a dissertation is responsible for some service aspect to the group. These tasks involve teaching laboratory courses in Macromolecular Chemistry, servicing the computer network, managing the literature, and coordinating the safety requirements and activities. Teaching The teaching duties in Macromolecular Chemistry comprise courses and labs in Physical Chemistry of Macromolecules for engineering students and courses in Macromolecular Chemistry for Chemistry majors as well as for teachers to be. Furthermore, 2 diploma theses and 9 dissertations were completed in 2001 (Tab. 3). Staff Dipl.-Ing. Bernhard Dederichs has retired from running the NMR service group and from his responsibilities in MARC. His successor is Ines Bachmann, who is rapidly growing into her new responsibilities. Unfortunately several staff positions have been cut and instead of a full-time position only a part time position is available to provide continuity and organize the service in liquid-state NMR. Ralf Eymael has completed his dissertation and subsequently became the head of the DFG research consortium Surface NMR of Elastomers and Biological Tissue. Several scientists have been visiting the NMR group. Among them Dr. Sofia Anferova from Kaliningrad with a

7 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 7 Table 3. Diploma theses and dissertations completed in 2001 Name Thesis Markus Küppers NMR-Untersuchungen zur enzymkatalysierten Reaktion im Geltropfen Mingfei Wang Heteronukleare Mehrquanten-NMR zum Effekt der Vernetzung und von Füllstoffen in Elastomeren und Polyamiden Song-I Han Correlation of Position and Motion by NMR: Pipe Flow, Falling Drop, and Salt Water Ice Ralf Eymael Methoden und Anwendungen der Oberflächen-NMR: Die NMR MOUSE Simone Baer-Lang NMR mit hyperpolarisiertem Xenon in hohen und niedrigen Magnetfeldern Christian Heine NMR von rotatorischer und translatorischer Dynamik Klaus Weingarten Ein- und zweidimensionale Hadamard-Kernresonanz- Spektroskopie Jan Plaß NMR-Studien an grenzflächenaktiven Verbindungen in kosmetisch relevanten Systemen Rolf Haken Entwicklung und Anwendung mobiler NMR-Sonden Annette Wiesmath NMR Methods for Strongly Inhomogeneos Magnetic Fields: Application to Elastomers Using the NMR-MOUSE Gerd Fink NMR-Bildgebung an periodisch bewegten Systemen stipend of the Daimler-Benz-Foundation, Prof. V. Anferov and Prof. H. Singh as guests of the research consortium Surface NMR. Funding Funding of the group derives largely from the outstanding support by the Deutsche Forschungsgemeinschaft (DFG) in terms of personal projects by Dr. Stapf, Dr. Bertmer, Prof. Demco, and Prof. Blümich as well as by projects in context with the Sonderforschungsbereich on Chemical Extraction and the Forschergruppe Surface NMR. Further funding is received from a German-Israeli collaborative project (DIP), the Bundesministerium für Bildung und Forschung (BMBF), the Fonds der Chemischen Industrie (FCI), and from industrial cooperations. Administration of financial resources are in the competent hands of Dr. F. Kowaldt and Frau K. Charlier, while teaching, personnel resources, and safety issues are managed by Dr. H.-J. Helbig. Förderverein Zentrum für Magnetische Resonanz e.v. The slowly but continuously tightening of funding in particular by the University has led to the formation of a non-profit organization Zentrum für Magnetische Resonanz e.v. the purpose of which is to support the NMR activities of the ITMC group with the help of sponsors and by acquiring projects. One activity of the Förderverein was to support the First International Summer School on Mobile NMR, which was organized by Peter Blümler on the Stahleck Castle in Bacherach overlooking the Rhine river. Here an interesting mix of participants from the University of Kent (Mike Mallet s group), the MPI in Mainz (Peter Blümler s new partners), the Aachen group, and different partners from industry discussed the basics, perspectives, and applications of mobile NMR. Furthermore, the Verein has helped a number of foreign students on arriving in Germany with a loan to get settled until their regular salaries arrived. Aachen, February 2002 Bernhard Blümich

8 8 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie 2. Lehrstuhl für Makromolekulare Chemie 2.1 Staff 2001 Function Name ++49-(0) extension Head of the institute Prof. Dr. Bernhard Blümich 26420/21 Staff scientists Dr. Marko Bertmer Prof. Dr. Dan Demco Dr. Ralf Eymael Dr. Hans-Joachim Helbig Dr. Siegfried Stapf Guest scientist Dr. Sofia Anferova Ph. D. students Dipl.-Chem. Irene Bartusseck Dipl.-Phys. Alina Buda Dipl.-Phys. Radu Fechete Dipl.-Chem. Christa Gehlen Dipl.-Chem. Kidist Hailu Dipl.-Chem. Song-I Han Dipl.-Phys. Sobiroh Kariyo Dipl.-Chem. Martin Klein Dipl.-Chem. Holger Kühn Dipl.-Chem. Markus Küppers Dipl.-Chem. Marion Menzel Dipl.-Chem. Ing. Xiaohong Ren Dipl.-Chem. Andrea Schwaiger Dipl.-Chem. Shatrughan Sharma Dipl.-Chem. Mingfei Wang Dipl.-Chem. Anette Wiesmath Diploma students Cand. Chem. Kerstin Kletzke Cand. Chem. Kai Kremer Technical staff Dipl.-Ing. Michael Adams Ines Bachmann-Remy Klaus Kupferschläger Günter Schroeder Secretaries Gerlind Breuer Ingrid Schmitz Financial resources Karin Charlier Renate Lemmens 26464

9 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie How to reach ITMC Address: Prof. Dr. Bernhard Blümich Institute for Technical Chemistry and Macromolecular Chemistry Lehrstuhl für Makromolekulare Chemie Sammelbau Chemie, Raum 38 B 121 RWTH Aachen Worringerweg 1 D Aachen Germany Phone: ++49-(0) Fax: ++49-(0) bluemich@mc.rwth-aachen.de WWW: and Airports: Köln/Bonn, Germany (85 km to Aachen via A4) Düsseldorf, Germany (90 km to Aachen via A44) Brussels, Belgium (143 km to Aachen) Maastricht-Aachen, The Netherlands (35 km to Aachen) Frankfurt, Germany (300 km to Aachen) The Airport-Aixpress is a direct bus connection between Aachen and the airports in Düsseldorf (12 times a day) and Köln/Bonn (4 times a day). The transfer takes about 60 to 90 minutes. Arriving by train Take a train to Aachen, preferably to station Aachen-West. On the left from the stations exit you will find a bus stop. Take line 33 (direction Klinikum or Vaals (NL) and leave at bus stop Wendlingweg (7 th stop) directly in front of the institute. At working hours there is a bus every 15 minutes. Not all trains stop at Aachen-West. If you have to leave at Aachen-Hbf (main station) you have to cross the square in front of the station. Across the street there are bus stops. Take line 3 to Klinikum. Facing the Klinikum (factory-like hospital) turn to the right and walk about 200 m following the street. At working hours there is a bus every 15 minutes. Arriving by car From Cologne (Köln) take freeway A4 or from Düsseldorf take A44. At the Aachener Kreuz take A4 towards Antwerpen/Heerlen. Leave the freeway at exit Aachen- Laurensberg (last exit before the border to The Netherlands, Fig. 1). Directly after the exit turn right towards Aachen. After about 1 km follow the highway to the right (follow signs Klinikum with a red cross). On the highway stay in the right lane and bear to the right following the signs to the Klinikum (about 2 km after the intersection and through a tunnel) until you are guided on top of a bridge ( Valkenburger Str., Fig. 2).

10 10 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie Fig. 1: Aachen and highway access. Klinikum SB Chemie Stay right and make almost a U-turn following the signs RWTH-Melaten or MTZ. After about 100 m there are parking lots on the left, enter the fourth one with the sign Chemie. The institute is in Sammelbau Chemie across the parking lots and across the street. It is readily recognized by the octogonal green glass towers which accomodate stair cases. Figure 3 on tghe following page shows an aerial view of the building. P Fig. 2: Detailed location map.

11 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 11 Fig. 3: Aerial view of the building.

12 12 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie 3. Teaching 3.1 Lectures and Courses (Prof. Blümich) Macromolecular Chemistry II (SS 01) V2, 2 hours/week Macromolecular Chemistry IVc/ Instrumental Analysis of Polymers (SS 01) V2, 2 hours/week, (together with Dr. S. Stapf) Physical Chemistry of Polymers I (SS 01) V2, 2 hours/week, (together with Dr. S. Stapf) Physical Chemistry of Polymers II (SS 01) V2, 2 hours/week (together with Dr. S. Stapf) Introduction to Technical Chemistry and Macromolecular Chemistry (WS 01/02) V2, 2 hours/week, (together with Prof. Dr. W. Leitner) General Technical Chemistry and Macromolecular Chemistry (WS 01/02) V2, 2 hours/week, (together with Prof. Dr. W. Leitner) Macromolecular Chemistry IVc/NMR-Spectroscopy (WS 01/02) V2, 2 hours/week, (together with Prof. Dr. D. Demco) Physical Chemistry of Polymers I (WS 01/02) V2, 2 hours/week, (together with Dr. S. Stapf) 3.2 Practical Lab Courses Together with Prof. Dr. H. Baumann, Prof. Dr. H. Höcker and Dr. M. Bertmer: Technical Chemistry and Macromolecular Chemistry, lab course (SS 01) all day 8-17 h Macromolecular Chemistry, lab course (SS 01) T, all day 8-17 h Macromolecular Chemistry, lab course (SS 01) T, all day 8-17 h Macromolecular Chemistry, lab course (SS 01) T, all day 8-17 h Macromolecular Chemistry, lab course (SS 01) T, all day 8-17 h (1/2 sem.) Macromolecular Chemistry, lab course (SS 01) T, all day 8-17 h (2 weeks)

13 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 13 Elective lab course in Macromolecular Chemistry (textile chemistry, analysis of polymers, preparative macromolecular chemistry, biopolymers, polymers in medicine) (SS 01) T, all day 8-17 h (1/2 sem.) Lab course for Chemistry of Macromolecular Material (SS 01) all day 8-17 h (1 week) Seminar to lab courses , , , , and (SS 01) Ü2, 2 hours/week Lab course for Chemistry of Macromolecular Materials (SS 01) all day 8-17 h (1 week) Seminar about Elective Capters of Magnetic Resonance (SS 01) Ü2, 2 hours/week Technical Chemistry and Macromolecular Chemistry, lab course (WS 01/02) T, all day 8-17 h Macromolecular Chemistry, lab course (WS 01/02) T, all day 8-17 h Macromolecular Chemistry, lab course (WS 01/02) T, all day 8-17 h Macromolecular Chemistry, lab course (WS 01/02) T, all day 8-17 h(1/2 sem.) Macromolecular Chemistry, lab course (WS 01/02) T, all day 8-17 h Elective lab course in Macromolecular Chemistry (textile chemistry, analysis of polymers, preparative macromolecular chemistry, biopolymers, polymers in medicine) (WS 01/02) T, all day 8-17 h (1/2 sem.) Seminar to lab courses , , and (WS 01/02) Ü 2, 2 hours/week Lab course for Chemistry of Macromolecular Materials (WS 01/02) all day 8-17 h (1 week) Seminar about Elective Capters of Magnetic Resonance (WS 01/02) Ü2, 2 hours/week

14 14 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie 4. Research Reports Group photogragh From left to right: First line: Bernhard Blümich, Christa Gehlen, Günter Schroeder, Martin Klein, Kidist Hailu, Radu Fechete, Shatrughan Sharma, Stephan Appelt, Federico Casanova, Beatrice Lego, Michael Adams. Middle line: Klaus Kupferschläger, Alina Buda, Christian Kölker, Song-I Han, Markus Küppers, Mirko Krüger, Kerstin Kletzke, Sobiroh Kariyo, Marion Menzel, Marko Bertmer, Holger Kühn. Upper line: Mingfei Wang, Irene Bartusseck, Xiahong Ren, Ingrid Schmitz.

15 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 15 Main Research Topic NMR investigations of translational motion Application of NMR methods to molecular motion encompasses a wide range of techniques depending on the scale where motion is taking place. By a suitable combination of spectroscopy, relaxation and field gradient techniques, molecular dynamics were probed over eight orders of magnitude in length and time. On the small scale, an indirect detection of spin dynamics is obtained by analyzing the relaxation behavior of the sample. Relevant time scales are the reciprocal Larmor frequencies in T 1 and T 1ρ experiments and the pulse separation in T 2 measurements. A wide range of frequencies is accessible by performing the investigation at different Larmor frequencies and, hence, different magnetic field strengths, a possibility which is exploited in the field-cycling technique of electronically controlled field changes. While relaxometry is sensitive to motions in the nanometer scale, larger displacements become directly accessible by encodings brought about via two or more pulsed field gradients (PFGs). The technique, in principle being aimed at the determination of diffusion and dispersion coefficients, has triggered the development of advanced pulse sequences and their theoretical description. Mass transport phenomena on scales of seconds or less are accessed by experiments employing a suitable set of PFGs encoding k -space (position) or q-space (displacement), where k and q are defined by the area of the gradients. Here, flow processes lead to a shift in the phase of the detected signal, while the nature of incoherent motion can be understood from measurements of the decaying signal intensity as a function of time or gradient strength. By combining pulse sequence modules for the encoding of spin density, displacement and chemical shifts with further contrast parameters, a versatile tool for investigating the microscopic and macroscopic dynamics in complex systems is generated.

16 16 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie Correlations in Displacements The most direct realization of the basic concept of multiple position encoding is achieved by sampling n-dimensional k-space via independent variation of n gradient pulses and subsequent Fourier transformation into positional space. The method allows to correlate positions at successive times with each other and therefore renders direct information of the temporal evolution in systems subject to diffusion and flow. The two-dimensional version of this so-called POXSY experiment and the related VEXSY experiment were compared for flow in various geometries. Onedimensional variants are employed to obtain distributions of velocity changes and can be used for a quantitative analysis of the temporal evolution of correlations for limited experimental times. Sequences such as the RODENT scheme which allow the determination of certain statistical parameters of the flow field in much shorter time have been described. See also report by S.Han. Restricted and Anisotropic Diffusion Restricted self-diffusion within geometrical confinements reveals itself either by a displacement distribution function, or propagator, which deviates from the Gaussian shape observed for unhindered diffusion, or by a reduced effective diffusivity. An analysis of the propagator obtained experimentally for fluids in a porous medium thus allows one to determine the tortuosity of the matrix or even to estimate its average structural size. On a smaller scale, relaxometry contributes to the understanding of fast molecular motions via their reorientational dynamics. Both the surface properties which influence the relaxation behaviour, and the geometry of the pore space itself in which diffusion takes place, can be varied in a controlled way in order to provide insight into the dynamical processes of the confined fluid and thus the porous medium itself. Surface deposits and partial fluid freezing are two of the main boundary conditions which have been investigated in detail. Knowledge of the structural

17 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 17 parameters and the interaction of liquids with the surrounding medium is of exceptional importance for the prediction of diffusion-dominated transport and reaction processes which can be of great industrial or environmental relevance. Moreover, the presence of anisotropies in the diffusional behavior represents a powerful tool for the description of material properties and functionalities in liquid-filled systems. Examples under investigation cover the wide range from natural and artificial building materials via the pore space in salt water ice to mesoporous catalyst support materials. See also reports by M.I.Menzel, X. Ren, S. Sharma. Diffusion and Flow in Multicomponent Liquid Systems The development of NMR pulse sequences which allow the investigation of material transport processes in combination with spatial and chemical selectivity represents the main topic of several collaborations of the NMR group with engineering faculties inside and outside the RWTH Aachen. The application of such techniques to realistic problems in the field of process engineering is the centerpiece of the three projects which receive funding from the Sonderforschungsbereich 540 of the RWTH which started in mid Self-diffusion and interdiffusion in multicomponent liquid systems are investigated in order to provide an experimental frame for numerical simulations of molecular and macroscopic transport processes. Similar problems are addressed for reactive systems such as gel-stabilized drops where the optimization of the reaction efficiency depends on the successful prediction of the diffusion into and within the drop volume. Both subjects exploit the potential provided by NMR methods to monitor the mixing process of different chemical species simultaneously and in real time. Statistical descriptions of motional parameters and direct visualization employing imaging methods are combined in order to achieve a thorough understanding of the efficiency of fixed-bed catalyst support reactors. For different geometries of the reactor, however, the experimental challenge is often found in the restrictions imposed by the sample geometry and the necessity to acquire information from a fast moving object while accumulating sufficient data to allow for a

18 18 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie multidimensional representation of positional, motional, and spectroscopic parameters. Falling drops and fluid films are exceptional examples which demonstrate the enormous potential which PFG-NMR techniques possess when combined with state-of-the-art spectrometer technology. See also reports by I.Bartusseck, S.Han, M. Küppers, X. Ren. Segmental Dynamics in Chain Molecules under external boundary conditions The conditions which are observed in physically entangled macromolecules are similar to those which determine the motion of small confined molecules; instead of the interaction with the surface, which acts both as a relaxation sink and as an obstacle to the free molecular self-diffusion, in the case of polymers the intersegmental correlations have to be taken into account. NMR relaxometry and diffusometry has contributed considerably to an understanding of the relevant dynamical processes and has aided to discriminate between various available theoretical descriptions. By removing certain degrees of freedom of the molecular motion, the relevance of individual contributions to the total polymer dynamics can be investigated in more detail. The most important introduction of external boundary conditions is given by the cross-linking of polymers; the properties of these elastomers are of interest not only from the theoretical point of view but also with respect to routine investigations and quality control of technical rubbers. NMR fieldcycling relaxometry provides a powerful technique to probe the change of the segmental dynamics under the influence of restrictions in the frequency range below 10 MHz, which can suitably be combined with more detailed studies employing portable (MOUSE) and high-field spectrometers which even allow the selective measurement of orientation-dependent parameters in anisotropic, stretched elastomer samples. See also reports by K. Hailu, S. Kariyo, A. Wiesmath.

19 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 19 Main Research Topic NMR investigations of elastomers An important objective in materials science is the establishment of relationships between the microscopic structure or molecular dynamics and the resulting macroscopic properties. Once established, this knowledge then allows the design of improved materials. Thus, the availability of powerful analytical tools such as NMR spectroscopy and imaging is a great advantage in polymer science. The unique chemical selectivity and high flexibility of NMR allows one to study structure, chain conformation, and chain dynamics in much detail and depth. Applications of NMR imaging for which non-destructiveness and contrast are essential are competitive with other imaging techniques in the information gained and cost of the experiment. A technologically important class of materials is that of elastomers. From the viewpoint of NMR, elastomers and other viscoelastic polymers above their glasstransition temperature exhibit both, solid-like and liquid-like features. Whereas the segmental motions give rise to the liquid-like behaviour, the presence of permanent or transient cross-links leads to residual dipolar couplings, that are responsible for the solid-like properties. Compared to the wealth of information obtained by advanced NMR techniques for liquids and solids, NMR has not be widely applied to viscoelastic polymers. These methods can provide important information on the dynamics of chains and functional groups, residual dipolar couplings induced by cross-links and topological constraints, inter-chain interactions, the effects of fillers, mechanical stress, plasticizers, and swelling of polymer networks. Moreover, the information and methods developed in the field of elastomers can be extended to the broad class of soft solids and ordered tissues. Applications of NMR imaging to elastomers concern distributions in temperature, stress, cross-link density, modulus, and the dynamics of fluid absorption and swelling. The main goals of our investigations of elastomers are:

20 20 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie Measurements of the segmental chain order Measurements of the segmental chain order in elastomers with different cross-link density, elongation ratio, orientation of the uniaxial strain relative to the direction of the magnetic field, filler content, and solvent uptake. The methods used determine 1 H- 1 H or 1 H- 13 C residual dipolar couplings. They are based on one-dimensional (1D) and two-dimensional (2D) NMR spectroscopy for static samples and for samples undergoing magic-angle spinning (MAS). A model-free method to measure residual van Vleck moments based on magic and Hahn echoes (mixed echo) was developed and applied to natural rubber under various conditions. The technique is superior to other methods allowing to take into account the multi-spin dipolar network and to separate the solid-like and liquid-like spin responses. Homo- and heteronuclear residual dipolar couplings were measured by different multipolar spin states for thermoplastic elastomers and elastomers series with different compositions and cross-linking. These states include dipolar encoded longitudinal magnetization, double-quantum coherences, and triple-quantum coherences. Moreover, method like SEDOR and REDOR are applied to this purpose for the first time. Characterization of chain dynamics Characterization of chain dynamics by the multi-spin dipolar correlation effect through use of mixed echo. The intermediate and ultra-slow motion regimes were explored by different versions of the method. A model which allows the evaluation of the dipolar correlation function was developed with the assumption of a distribution of correlation times. The second van Vleck moment and the parameters of the distribution of correlation times were determined for an elastomer series with different cross-link density, elongation ratio and orientation relative to the direction of the magnetic field. Various models of polymer networks were used to interpret the data. NMR parameter maps NMR parameter maps of 1 H residual dipolar couplings were recorded for elastomers with heterogeneities produced by a distribution of cross-link density and mechanical stress. For the first time a triple-quantum image of a phantom made of poly(isoprene) samples with different cross-link densities was recorded. Two-dimensional 1 H maps of

21 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 21 the stress distribution were obtained for a strained natural rubber band with a cut on one side based on dipolar encoded longitudinal magnetization and double-quantum coherences filters. The results of this investigation underline the benefits of 1 H NMR imaging for the analysis of stress-strain effects in elastomers as compared to 2 H images of deuterated oligomers incorporated into elastomers. Rubber materials from industry and elastomer biomaterials Rubber materials from industry and elastomer biomaterials have been extensively investigated by NMR spectroscopy, NMR imaging and the NMR-MOUSE. NMR methods can characterize elastomer samples based on chain stiffnes as reference. The effects of use of elastomer products based for high-voltage cable isolation was investigated using a combination of NMR methods. Moreover, it was shown that measurements of the spin-lattice relaxation times in the rotating frame (T 1ρ) by the NMR-MOUSE can reveal the distribution of the macroscopic heterogeneities and defects in large elastomer materials. Proton double-quantum filtered images performed on silicon breast implant envelopes show a contrast increase for better identification of defects compared to T 2 weighted images. Methodological developments Methodological developments of the methods discussed above were also performed. The possibility to excite and detect 1 H double-quantum coherences in strongly inhomogeneous magnetic fields was demonstrated on natural rubber. The sensitivity of the dipolar encoded longitudinal magnetization decays and double-quantum buildup curves to differences in cross-link density and strain was shown. This results suggest the possibility to use the NMR-MOUSE for characterization of tissue order in connective tissues, muscles, and blood vessels. A new method to measure residual dipolar couplings via J-couplings in a 2D double-quantum MAS NMR experiment performed under rotational resonance conditions was introduced and applied to a sample series from natural rubber. For static samples a sensitive, accurate and robust method was developed to measure residual van Vleck moments by magic and Hahn echoes.

22 22 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie Main Research Topic Mobile NMR Usually the sample is carried to the NMR spectrometer and is prepared to fit the size of the NMR tube or sample holder. Mobile NMR denotes NMR investigations where the equipment is carried to the sample. Thus mobile NMR spectrometers are used which typically operate at frequencies lower than 20 MHz and are operated by PCbased microcomputers. If mobile NMR is combined with unilateral NMR, where the magnetic polarizing and radio-frequency fields are applied to the sample from one side, arbitrarily large samples can be investigated at selected volume elements in the vicinity of the applied magnetic fields. This type of NMR was invented in the early fifties of the last century with the intention to lower NMR equipment down bore holes and investigate the fluids in surrounding rocks for its hydrocarbon contents. While the first such experiments were carried out in the earth s magnetic field the field from permanent magnets was soon discovered to provide better signal strength. But only about a decade ago were the first commercial mobile spectrometers successfully tested in oil wells down to depths of 10,000 m. The same principle of NMR has been suggested by the inventors of well-logging NMR to be used for process analysis and product stream control. Some engineering applications of this type of NMR to water analysis in concrete structures have sporadically been reported but did not find much attention in the scientific NMR community. When setting up research in Aachen with expensive equipment on order, the long-standing idea of Peter Blümler and Bernhard Blümich to build a simple NMR spectrometer with an ultrasoundhead-like sensor was finally realized by Gunnar Eidmann, one of the first doctoral students of the young NMR team at RWTH Aachen. This sensor was given the name NMR-MOUSE for MObile Universal Surface Explorer which is now a registered trademark of RWTH Aachen. It soon turned out, that signals could be received with the NMR-MOUSE from about any proton-bearing object, including the fixtures of the rf coil. Rubber proved to be an excellent class of materials suitable for investigations by the NMR-MOUSE, because of long transverse relaxation times and the absence of translational diffusion. Even steel in the vicinity of

23 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 23 the sensitive volume of the device is not necessarily harmful to the measurement, because inhomogeneous magnetic fields are employed in the first place. Contrary to well-logging NMR, where fluids are being measured, no attention was paid to achieve a low gradient field. In this way higher field strength could be obtained and better sensitivity. Staying with the basic concept of a U-shaped magnet with the rf coil inside the magnet gap, several NMR methods were explored for their use in strongly inhomogeneous magnetic fields. It was soon discovered, that many rf pulse sequences work. Examples are the Hahn echo, the solid echo, the stimulated echo, the quadrupolar echo, the magic echo, the mixed magic echo, various multi-pulse versions of these echo sequences, inversion and saturation recovery sequences with echo detection, diffusion measurements exploiting averaged gradient fields within the sensitive volume, and multi-quantum NMR. Therefore, a wide arsenal of basic NMR methods is available to work in the inhomogeneous magnetic fields of the NMR- MOUSE, although the distribution of flip angles leads to signal contributions averaged over experiments with different flip angles in different volume elements. As a consequence, the measured quantities depend on the pulse sequence and the geometry of the magnetic fields generated by the particular sensor. Nevertheless, the parameters scale with many material properties such as cross-link density, the glass transition temperature, and the shear modules of polymers in the rubbery state. Also many fluids can be discriminated based on a combination of their transverse relaxation times and their self-diffusion constants. Consequently basic research is conducted with many applications in mind for the rubber industry and for chemical engineering. An important stimulus for the development of the NMR-MOUSE into a useful analytical tool is the interdisciplinary, DFG-funded research consortium (Forschergruppe) Surface NMR of Elastomers and Biological Tissues, which was refereed in late 2001 for a second funding period of three years. The goal of this Forschergruppe is to develop a unilateral NMR imager and to explore applications in medicine and polymer processing. One of the remarkable discoveries is, that the anisotropy of many types of NMR parameters can be observed with the NMR-MOUSE for macroscopically ordered matter such as tendon and strained elastomers (see reports by A. Schwaiger, R. Eymael, and K. Hailu). Furthermore, new sensor geometries and rf coils have been developed together with Prof. V. Anferov, a visiting

24 24 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie scientist from the Kaliningrad State University, and Dipl.-Ing. M. Adams from RWTH (see report by M. Klein). It is now possible to observe the signal of a 90 µm thin rubber membrane in a single shot with a signal-noise-ratio of better than 5. This is a dramatic improvement compared to the old NMR-MOUSE design. Also the dead-time has been shortened so that echo times of less than 20 µs can be achieved without Q switching. This enables us to measure also the NMR signal from rigid polymers including cellulose in paper and cotton. In a EUREKA project historic objects from our cultural heritage shall be studied by the NMR-MOUSE, for example the pore-size distribution on monuments and historic buildings exposed to water and the quality of paper in old books (see reports by S. Sharma and S. Anferova). It appears, that many more applications for the NMR-MOUSE are waiting to be explored including product and process control in industry (see report by K. Kremer), and possibly a return of the NMR-MOUSE to bore-hole NMR. This requires continuous innovation also of the hardware which benefits from the enthusiastic efforts of Dipl.-Ing. M. Adams, G. Schroeder and K. Kupferschläger.

25 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 25 Dr. Sofia Anferova Visiting Scientist Recent developments of the NMR MOUSE In anticipation of support by EUREKA project Eurocare-MOUSE of the European Community The planar surface coils are used in the NMR MOUSE. Those coils can be milled or etched from a standard printed circuit board. They have the following advantages compared to simple solenoidal coils: short background signals (about µs), high sensitivity, exellent reproducibility, easy and inexpensive manufacturing. This concept permits the use of the NMR MOUSE for investigations of objects of cultural heritage like books, paintings, cloth, wooden constructs, and building materials where relaxation times are short due to the lack of mobile protons. The NMR signals from paper reveal detailed information about the type of cellulose, the structural molecules of paper, and the degradation of these molecules during the ages. The measurements on the paper quality of old books will be conducted in Rome. The results of these measurement will not only provide a first data base as a reference for future measurements but they will also enter into the development of novel NMR instrumentation by Dr. Giovanni Bizzarro and his team at Bruker, Milano dedicated to help preserve our cultural treasures from the past. Fig. 1: The NMR MOUSE with figure-8 coil and the Hahn Echo decay from the historical paper

26 26 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie Dipl.-Chem. Irene Bartusseck Doctoral student Diffusion analysis in multicomponent systems with NMR supported by SFB 540 (DFG) Knowledge of diffusion coefficients is one of the basic requirements for the calculation of material transport processes. Chemical industry, process engineering, and medicine benefit from the description of diffusive mass transport that can occur, for example, through phase interfaces and at walls in catalysts. Concerning multicomponent diffusion, the information available from measurements and models describing the processes is still insufficient. The topic of the project is the experimental investigation of diffusion in binary and ternary liquid mixtures. Concentration dependent self-diffusion coefficients in the equilibrium state are measured as well as concentration profiles of two interdiffusing Fig. 1: Data points and concentration dependence of the self-diffusion coefficients for the ternary system n-hexane/1,4-dioxane/toluene.

27 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 27 liquids, which enable the calculation of interdiffusion coefficients. With these data, the prediction of diffusion coefficients shall be tested. NMR pulsed field gradient methods are a common way to measure self-diffusion coefficients. A discrimination of different chemical compounds is possible if they can be separated spectroscopically. Figure 1 shows the concentration dependence of the self-diffusion coefficients in the nearly ideal ternary system n-hexane/1,4- dioxane/toluene. The results show a linear dependence and only minor deviations between the values for the different liquids in a given mixture. It is therefore possible to interpolate other data points. These data can be used to correlate self-diffusion coefficients employing interdiffusion coefficients by different models from the literature that describe the relation between both quantities. The determination of self-diffusion coefficients can be combined with spatial information by applying read-gradients during data acquisition. This is possible using CPMG methods with diffusion gradients before and after the refocusing pulses. The amplitude is influenced by both the T 2 relaxation and the diffusion gradients and contains information about either processes. The experiment has to be performed with and without diffusion gradients to eliminate the T 2 decay. It allows to trace the diffusion information in systems with changing diffusion coefficients, i.e. during reactions or interdiffusion processes. An example is shown in Fig. 2, where the interdiffusion process of 1,4-dioxane and deuterated toluene is Fig. 2: Self-diffusion coefficients of 1,4-dioxane during the interdiffusion of deuterated toluene and dioxane. mapped. Due to the presence of a gradient during acquisition, spectroscopic information is lost, but can be obtained by chemicalshift selective excitation if the substances are spectroscopically distinguishable.

28 28 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie Dr. Marko Bertmer Staff scientist Application of solid state NMR techniques Main research interests modern polymers: structure & dynamics, correlation with materials properties nanostructured materials surface and interface characteristics elastomers: crosslink density, heterogeneity, segmental order thermoplastic elastomers: morphology, interaction between hard and soft segments development of pulse sequences and simulation strategies to study selected information of solids Research Projects Nanostructured materials (M. Wang) Characterization of shape-memory polymers (see by A. Buda, together with A. Lendlein, German Wool Research Institute at RWTH Aachen) Segmental order in elastomers (see report by M. Wang) Study of grafted polymers (M. Wang) Spin diffusion on thermoplastic elastomers, block copolymers, and nylon fibers (see report by A. Buda; together with V. Litvinov, DSM Research) Diffusometry, relaxometry and multinuclear spectroscopy in naphtha reforming catalysts (X. Ren, S. Stapf, H. Kühn, D. Demco; together with Lehrstuhl für Technische Chemie und Petrolchemie, RWTH)

29 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 29 Analysis of pesticide residues and degradation in biological environments (together with Institute of Biology V, Ecology, RWTH) Additional Functions Teaching: Organization of laboratory courses in Macromolecular Chemistry Teaching: Seminars in Macromolecular Chemistry for chemistry students Supervision of Avance DSX 500 solid state NMR spectrometer Advisor in solid state NMR for members of other research groups Coordination of research proposals concerning solid state NMR

30 30 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie Dipl.-Phys. Alina Buda Doctoral student Solid state NMR studies of shape-memory polymers and nylon fibers supported by Deutsche Forschungsgemeinschaft DFG A. Shape memory polymers (in collaboration with Dr. A. Lendlein, DWI) Polymeric materials that are able to change their shape in response to temperature have attracted much attention in the last years because of the wide range of possible applications. These polymers have a memory that allows them to be deformed into a temporary configuration and then to be restored to their original parent geometry within a few seconds by applying heat. Compared to other shape memory materials polymeric materials offer much greater deformation capabilities, substantially easier shaping procedures and high shape stability. Investigations of a biocompatible and biodegradable shape memory polymer with potential medical application were conducted using NMR mehods sensitive to the local motion and segmental chain order. Of importance is the question which NMR accessible parameters are sensitive to the change of shape. For this, 1 H and 13 C spectra, relaxation times and double- quantum build-up curves under MAS and in static conditions were measured in the temperature range of C for unstretched and stretched samples. As an example, Fig. 1 shows the DQ-build up curves recorded under static conditions. For the sample stretched at 80% the maximum occurs at shorter Fig.1: Double-quantum build up curves for shape memory polymer samples with different stretching ratios recorded in static conditions.

31 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 31 excitation times, reflecting a larger dipolar coupling due to the chain ordering. Furthermore, we were able to detect the 13 C signal at the crosslinking point which permits a correlation to be established with the segment length. B. Morphology of semicristalline polymers and nylon 6 fibers by NMR spindiffusion (in collaboration with Dr. V. Litvinov, DSM) Investigations of the morphology and domain sizes in different polymer materials were made using NMR spin-diffusion in addition with SAXS. General analytical solutions valid for the full range of spin-diffusion times were obtained in the case of three domains for an one-dimensional process. They have been tested in the limit of a system with two domains and by predicting the domain sizes for a poly(styrene-methyphenylsiloxane) diblock copolymer and semicrystalline poly(ethylene oxide). The results were compared with previously reported data (see Fig. 2). Fig. 2: Proton spin-diffusion build-up curves for the crystalline component of PEO. The simulations were made using our analytical model but with the earlier parameters (dashed line) and with the refined parameters (solid line). Fig. 3: Proton spin-diffusion decay curves of the mobile amorphous component in different nylon 6 fibres. Our new analytical model was applied to analyze the NMR data of high-speed melt-spun nylon 6 fibers swollen in D 2O. Amorphous, interface, and crystalline domains perpendicular to the fiber direction were investigated using a magic-echo dipolar filter. The changes in domain sizes were correlated with the spinning speed of nylon 6 fibers.

32 32 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie Prof. Dr. Dan E. Demco Staff Scientist NMR on advanced materials Main research interests Segmental order and chain dynamics of soft-solids (elastomers, thermoplastic elastomers) Characterization of heterogeneous distributions of chain dynamics of grafted polymer systems Nanostructured polymer films and nanocomposite materials Morphology and domain sizes in multi-block polymers and nylon fibers Development of new methods for measuring residual dipolar couplings Decoupling and recouplings techniques in solid-state NMR Research Projects Application of self-diffusion to characterize polymer networks (DFG, DE 780/1-1, together with R. Fechete and M. Menzel) 129 Xe NMR on elastomers (DFG, DE 780/1-1, together with H. Kuhn) Characterization of segmental anisotropy in elastomers and ordered tissues by NMR methods (DFG, DE 780/1-1 and DIP, together with K. Hailu, A. Schwaiger, and R. Fechete) NMR in strongly inhomogeneous magnetic fields (DIP, Forschergruppe, industry, together with R. Fechete, A. Wiesmath, and M. Klein)

33 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 33 NMR study of deactivation and decoking of a naphta reforming catalyst (DFG BL231/25-1, together with X.-H. Ren, M. Bertmer, and S. Stapf) NMR investigation of supermolecular and nanostructured polymers (BMBF, together with M. Wang, A. Buda and M. Bertmer) Additional Functions Teaching: Seminar Analytical Methods for Polymers Teaching: Structure Determination for Chemists (Special Multi-dimensional NMR methods) Coordination of research activities DFG (DFG DE 780/1-1, DIP, BMBF-Umwelt) Supervisor of the ITMC library.

34 34 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie Dr. Ralf Eymael Staff Scientist Coordination of the DFG-Research Group Surface-NMR of Elastomers and Biological Tissues supported by Deutsche Forschungsgemeinschaft DFG, Forschergruppe Oberflächen-NMR an Elastomeren und biologischen Geweben The DFG-funded research group Surface-NMR works on the development of a lowfield NMR tomograph with an open magnet design like the NMR-MOUSE. The Forschergruppe is an interdisciplinary cooperation of six teams at the University of Aachen. Two teams each are focusing on hardware development, NMR-methods for inhomogeneous fields and image reconstruction, and the investigation of applications in the fields of material science and medical diagnostics. Figure 1 shows an overview of the structure of the research group, which started in spring The main part of coordinating the research group for the year 2001 was devoted to acquiring a further three-year funding period by DFG. The work and the progress reports of the six participating teams had to be organized, and a book prepared for refereeing the groups activities and project plans. The performance of the Fig. 1: Structure of the research group Surface-NMR research group was evaluated of Elastomers and Biological Tissues.

35 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 35 on October 23 rd by a committee of referees. On that day the posters and talks were presented to the referees, and demonstrations of new hardware, methods, and applications were conducted in the research group s lab attached to the MARC. One example was 1D imaging with an NMR-MOUSE supplemented by additional gradient coils, continuing the work of Pablo Prado et al from The challenge was to set up an experiment with a portable PC spectrometer (Bruker minispec), which can readily be performed, including the reconstruction of the image and comparison with the actual type of the sample. Figure 2 shows the basic imaging sequence, a photograph, and the 1D image for a sample prepared from natural rubber. The measurement with 64 space-encoding steps took about 6 minutes. For the reconstruction of the 1D image the data were zero-filled to 512 points, but no additional filtering was applied. The whole demonstration including the data processing could be reproducibly performed within a few minutes. Fig. 2: Pulse sequence, photograph, and 1D image of a sample prepared from natural rubber. Functions Coordination of the DFG-Forschergruppe Oberflächen-NMR an Elastomeren und biologischen Geweben. Administration of the NMR-MOUSE group, hands-on support to the students working with the NMR-MOUSE. Service and research projects concerning the NMR-MOUSE together with industrial and academic research partners. Advanced programming and testing of pulse sequences for the MOUSE spectrometers.

36 36 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie Dipl.-Phys. Radu Fechete Doctoral student NMR in Inhomogeneous and Homogeneous Fields supported by Deutsche Forschungsgemeinschaft (DFG) A. Numerical simulation of the spin system response in inhomogeneous fields. An important device in borehole exploration is the NMR sensor, an inside out tool. The NMR sensor has two magnets, which are opposed to each other. Spin system response is affected by the strong inhomogeneities in magnetic fields. In order to simulate the spin system response and to understand the effect of various parameters, an algorithm was derivate and a C ++ program was written. Using this program it is possible to: 1. Simulate Carr-Purcell (CP) and Carr-Purcell-Meiboom-Gill (CPMG) pulse sequences. 2. Sensitive volume of NMR sensor (see Fig. 1). 3. The effect of T 1 and T The effect of self-diffusion. 5. The effect of pulse shape and composite pulses. 6. The effect of z-motion of the NMR sensor in two cases: i) on the duration of CPMG (see Fig. 2); ii) between two pulse sequences. Fig. 1. One side of the Sensitive volume of the NMR sensor a) b) Fig. 2. CPMG echo trains for a static NMR sensor (a) and with a z-axial motion (b)

37 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 37 B. NMR investigation of elastomer with MOUSE NMR sensor and NMRimaging The longitudinal nuclear magnetization relaxation in the rotating frame (T 1ρ) is a sensitive parameter to the slow molecular motions, which are present in elastomers. a) P o s 1 1 T 1 r h o = m s P o s 5 T 1 r h o = m s P o s 6 T 1 r h o = m s P o s 3 T 1 r h o = m s P o s 9 T 1 r h o = m s P o s 1 2 T 1 r h o = m s P o s 1 T 1 r h o = m s P o s 4 T 1 r h o = m s P o s 1 0 T 1 r h o = m s P o s 7 T 1 r h o = m s P o s 8 T 1 r h o= m s P o s 2 T 1 r h o = m s b) Fig. 3. a) Distribution of measured T 1ρ value on a centimetres scale. b) NMR image encoded by spin density and T 2 for a piece of rubber on millimetre scale (shown in (a)) The frequency window of T 1ρ relaxations is in the same range as that given by transverse magnetization relaxation T 2. Therefore, T 1ρ is expected to be sensitive to the changes in the cross-link density and filler contents. The T 1ρ parameter was measured using a pulse sequence adapted to the NMR- MOUSE. The T 1ρ measurements are more sensitive to the presence of carbon fillers compared with T 2 measurements. This is due to the integrated dispersion of T 1ρ in the strong inhomogeneous fields of NMR-MOUSE. In our investigation this effect was used to put in evidence the presence of a strong heterogeneity in sample at position no. 5 (see Fig. 3a).

38 38 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie This investigation shows the ability of the NMR-MOUSE sensor for characterizing the space distribution of the cross-link density and filler content on the centimeter scale. The sensor is less expensive compared to a NMR tomograph and the measurements can be done easily. C. Segmental order and chain dynamics in elastomer by magic/hahn echoes A new method to measure the multi-spin dipolar correlation function (DCF) was developed. It is based on the mixed echo composed by a superposition of magic and Hahn echoes. This multi-spin DCF gives information on the segmental chains order via the residual second van Vleck moment. Moreover, a distribution of correlation times describing chain dynamics was implemented for the evaluation of the DCF. a) b) c) Fig. 4. a) Normalized magic/hahn echo decay for natural rubber (NR) samples with different cross-link density. b) The dependence of the square root of the residual second van Vleck moment on cross-link density measured in phr sulphur. c) The dependence of correlation time on cross-link density.

39 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 39 The residual dipolar couplings measured via second van Vleck moment show a linier dependence on cross-link density (see Fig. 4 b). The centre of gravity for the correlation time distribution is increasing with the phr value. Other Scientific Projects Explorative projects for industrial partners. QuickField 2D simulations for DIP project. Collaboration in the DFG project on anisotropy of segmental orientation in elastomer Additional Functions Web manager.

40 40 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie Dipl.-Chem. Christa Gehlen Doctoral student NMR Imaging of Silicone Breast Implant Envelopes and Intervertebral Discs In collaboration with: Institut für Klinische Radiologie, Universität Münster, Orthopädische Klinik, Universitätsklinikum RWTH Aachen; bwa (Aachen Centre of Excellence: Biomaterials) NMR imaging can successfully be used in materials research to map material properties. On account of the noninvasive nature and nondestructiveness of NMR, the technique is particularly useful for investigations of biomaterials. Proton NMR dipolar filters based on double-quantum coherences and dipolar encoded longitudinal magnetization have been used for investigating aging processes of silicon breast implants envelopes in vitro. Parameter images revealing the space distribution of segmental order can be recorded combining the dipolar filtered images with the T 2 encoded images. T 2-weighted images can show a defect in an implanted silicone breast implant envelope which is neither shown in a photo nor under the microscope (Fig. 1). Fig. 1. Left: 1 H T 2-weighted image of silicone breast implant envelope implanted for 60 days. A defect is visible in the middle of the envelope. Right: A photo of the same sample. The defect is not visible also not under a microscope. Dipolar filters based on multiquantum coherences have been implemented. Application of 1 H NMR contrast filters based on dipolar encoded longitudinal magnetization and DQ coherences for recording 1 H NMR images of silicon breast

41 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 41 implant envelopes in vitro are shown in Fig. 2. The different signal intensity can give more and other information about the structure of the envelope. Fig. 2. Left: 1 H T 2-weighted image of a silicone breast implant envelope after 3 years of implantation. Right: Double quantum dipolar filtered image of the same envelope. Intervertebral discs are used for pressure transfer between the vortices and introduce flexibility in the intervertebral column. An intervertebral disc consists of a liquid-like part in the middle called nucleus pulposus and a more solid-like part on the edge called annulus fibrosus. The aging of nucleus pulposus entails a restriction of the movement. We extract the dissolved and aged parts and will try to replace them afterwards with a substitute (Fig. 3). 2*10 7 2*10 7 0a.u frequence in khz a.u frequence in khz Fig. 3. Spectra of an explanted nucleus pulposus following treatment with different solutions. Left: Spectrum at the start of the dissolving the aged parts. Right: Spectrum after 40 min. The signal rise of the left peak shows the inflow of the dissolving solution. Additional Functions Administration of research and development projects in collaboration with bwa. Service measurements at the DMX 300 spectrometer. User training for the DMX 300 spectrometer. Administration and maintenance of the DMX 300 Spectrometer (together with M. Küppers and M. Adams).

42 42 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie Dipl.-Chem Kidist Hailu Doctoral student Anisotropy of T 2 in natural rubber under uniaxial deformation measured with the NMR-MOUSE supported by Deutsche Forschungsgemeinschaft DFG The angular dependence of transverse relaxation T 2 in strained natural rubber was investigated with the NMR-MOUSE. In the unstrained state the end-to-end vectors of the chain segments between the cross-links are isotropically distributed. Uniaxial deformation induces segmental chain orientation along the direction of the force, and as a consequence the strength and the distance of the end-to-end vectors change. In spite of the inhomogeneities of the static and radio-frequency magnetic fields of the NMR-MOUSE it is possible to observe the angular dependence of T 2 by using the Hahn-echo pulse sequence. 0 Λ = 1-11 The anisotropy behavior of T 2 for several stretching 1.2 ratios λ = L/L 0, where L 0 and L are the length of the network along the straining direction before and after elongation, respectively, was measured in slightly cross-linked natural rubber band by keeping λ constant and varying the orientation angle Θ with Figure 1: The anisotropy behavior of T -1 2 for uniaxial strained natural rubber at different elongation ratios respect to B 0. The angle λ. The relaxation rate varies with the orientation Θ corresponds to the direction angle and shows a minimum near the magic angle, Θ = 54,7. of the magnetic field. The angle was changed in steps of 10 and, near the magic angle in steps of 5. As relaxation rate [ms ] -1

43 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 43 expected, in unstrained natural rubber (λ = 1) the measured transverse relaxation rates show no angular dependence, resulting in circular distribution in the polar plot (Fig.1). At λ > 1 the circle starts to deform and at larger elongation ratios (λ > 2), the sphere becomes almost an ellipsoid with a minimum value of T -1 2 between 50 60, near the magic angle. The measured relaxation rate T -1 2 reflects the anisotropy effect which is induced in the polymer network by uniaxial deformation. The angular dependence of T -1 2 can be described by a second order Legendre polynomial P 2(cos Θ) = (1/2)[3cos 2 Θ - 1], where Θ is the angle between the polarizing magnetic field and the elongation direction. Figure 2 depicts the change of T -1 2 with the extension ratio λ at a fixed orientation (Θ = 0 ). A change in curvature near the values of λ = 2 2,5 was detected. This change in the λ -1 dependence of T 2 with the extensions above λ = 2 can be explained by the stress-induced crystallization which is well known for natural rubber and extensively discussed in the literature. Figure 2: Plot of T -1 2 versus the extension ratio λ for the orientation angle Θ = 0. The curvature for values of λ = 2 2,5 correlates with results found in tensile tests. Spacial distribution of chain segmental anisotropy Furthermore it was possible to detect the spacial distribution of chain segmental anisotropy induced in a natural rubber plate with a circular cut in the middle (Fig. 3). The NR plate was uniaxially strained with the extension ratio λ = 2,9. Under strain the cut assumed the shape of an Figure 3: Different positions were measured to detect the distribution of the strain induced by uniaxially deformation of a NR band with a circular cut. Under deformation the cut changes to an ellipsoid.

44 44 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie ellipsoid. T -1 2 was measured at different positions and two orientation angles Θ = 0 and Θ = 90 relative to the direction of the straining force. The values of the anisotropy contrast defined by (T -1 2 ) T -1 2 (Θ = 0 ) - T -1 2 (Θ =90 ) are shown as white numbers in Fig. 3. The largest anisotropy was detected for the positions 1 and 2 compared to positions 3 and 4. In the limit of experimental error the anisotropy contrast has the same values for the positions symmetrically placed around the cut. Additional Functions Teaching assistant in laboratory studies of Macromolecular Chemistry. Execution of service and research project concerning the NMR-MOUSE cooperation with industrial and academic research partners. in

45 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 45 Dipl.-Chem Song-I Han Doctoral student NMR Imaging of a Falling Drop supported by Deutsche Forschungsgemeinschaft DFG as part of SFB540 The falling drop is a simple model for studying chemical extraction where two immiscible phases are dynamically blended to promote the transport of solute molecules from one phase to the other. Convective motion inside the drop significantly influences the extraction efficiency. Whereas optical and tracer methods are model bound or invasive, NMR imaging is noninvasive, direct, and applicable to non-transparent media. The first NMR measurements of free falling fluid drops through air are reported and demonstrate that NMR imaging is able to confirm the presence of large-scale convection rolls and visualize the structure of the inner vortexdynamics in a falling drop directly. Water drops with and without surfactant were generated to fall free through air. The setup consisted of a glass pipette plugged vertically inside a 4.7 T magnet and an infrared photo sensor, which triggers the spectrometer each time the drop obstructs its light path. In this work, drops falling with 2 m/s, hence remaining only for about 10 ms within the sensitive volume of the resonator, were studied. As a consequence, any ultra-fast NMR imaging method is incapable of completing the measurement within the residence time of a single drop; using triggered cyclic acquisition was the only possibility for signal accumulation as well as for multidimensional experiments. Here, the uniformity in shape of each drop is an indispensable condition, which was proven by various NMR imaging methods. Excellent agreement of 1D projections obtained by the frequency encoding method with different numbers of accumulations and the phase encoding method was found (variance < 1%), thus excluding random variation of the drop formation. 3D spin density images with remarkable quality were obtained, showing different shapes and the reduction in drop size of drops consisting of pure water to those of surfactant solution. Spatial distributions of vertical (z) and transverse (x) velocities within the

46 46 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie drop along the cross-section of the drop have been analyzed, revealing small scale variations for surfactant drops and large-scale structures for water drops. In order to directly visualize the internal fluid dynamics, both v z and v x components were measured in each pixel of the zx-plane simultaneously within a single experiment to combine these into a vectorial representation (Fig.1). The obtained vector plot unambiguously visualizes the notion of the presence of stable vortices within the water drop. Additionally, an overlapping oscillation was observed, which can be expected given the high Reynolds number of about 400, well outside the regime of stationarity. It is confirmed by optical observation of drops under comparable conditions. Fig 1: Velocity components v z, v x for a drop or pure water as a function of the position along the zx plane. The magnitudes of the velocities are indicated by the lengths of the arrows. The v z components is scaled relative to the average falling velocity of 2 m/s. A pair of vortices is readily identified. Other Scientific Projects NMR imaging on a levitating drop. Imaging with hyperpolarized xenon. Additional Functions Coordination of some projects in SFB 540.

47 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 47 Dipl.-Phys. Sobiroh Kariyo Doctoral Student NMR Relaxation Dispersion of Cross-Linked Elastomers supported by Deutsche Forschungsgemeinschaft DFG The molecular dynamics of polymer melts with molecular weights above the critical value have successfully been described by a power law dependence of the spinlattice relaxation time on the Larmor frequency. This so-called relaxation dispersion is explained, for instance, by the Doi/Edwards limits of time dependence of mean square displacement of a chain segment [1, 2, 3]. Four different regimes of power laws describing the relaxation dispersion of polymers are distinguished and have been observed experimentally for several different polymer types [4]. Nevertheless, the influence of restrictions to motion on this behavior is not well understood. Therefore, in this study, the influences of cross-link density on the molecular dynamics of natural rubbers at various temperature were investigated by using field cycling relaxometry. The relaxometer used here provided information of relaxation dispersion in a frequency range from 5 khz to 20 MHz. T 1 /s 10-2 NR1/1 NR2/2 NR3/3 NR4/4 NR5/5 NR6/6 NR7/7 T=296 K Figure 1: Relaxation dispersion of natural rubber with different cross-link density; NR1/1 NR7/7 correspond to sulphur and accelerator contents of 1 to 7 phr, respectively ν /MHz

48 48 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie Strong relaxation dispersions were observed at high fields with a weak dependence on cross-link density as shown in Fig. 1. At low field, a much weaker relaxation dispersion is found with a strong and systematic dependence on the cross-link density. The crossover points are shifted toward lower fields with increasing cross-link density but the values of the exponents in the relation T 1 ν γ were left unchanged: γ 0.16 at low field and γ 1.2 at high field. The relaxation dispersions at low field which were below crossover points can be described as a region II according to the common power law relations for polymers. However the exponential value was smaller than those for the tube model as described in the literature. This might be from shorter time scales of reorientations of semi-local nature of these samples. The same tendency was also observed by changing the temperature of the samples as shown in fig. 2. Both increasing the cross-link density and decreasing the temperature of the samples caused the shift of crossover points to lower fields NR 1/ K 323 K 313 K 303 K 296 K 288 K 283 K 275 K NR 5/5 333 K 323 K 313 K 303 K 296 K 288 K 283 K 275 K T 1 /s T 1 /s ν /MHz ν /MHz a) b) Figure 2: Relaxation dispersion of natural rubbers measured at various temperature; a) Natural rubber with 1 phr of sulphur and b) Natural rubber with 5 phr of sulphur In this study, the relaxation dispersion related to the molecular motions of natural rubber with different cross-link density was observed. Further investigations employing field cycling relaxometry will focus on other physical constraints on the molecular dynamics such as mechanical stress. [1] M. Doi, S. E. Edwards, The Theory of Polymer Dynamics. Clarendon Press, Oxford, [2] R. Kimmich, H. W. Weber, J. Chem. Phys. 98, 5847 (1993). [3] N. Fatkullin, R. Kimmich, J. Chem. Phys. 101, 822 (1994). [4] H. W. Weber, R. Kimmich, Macromolecules 26, 2597 (1993).

49 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 49 Dipl.-Chem. Martin Klein doctoral student The Strayfield NMR-MOUSE supported by the Deutsch-Israelische Projektkooperation (DIP) The Strayfield NMR-MOUSE is a new handheld NMR sensor for relaxation experiments and 1D- and 2D-imaging. In contrast to the normal NMR-MOUSE it explores the strayfield of a simple bar magnet to produce B 0. The B 1 Field is generated by a flat coil on top of the device [Fig. 1] [Fig. 2] 40 mm Rf-coil N S z y 40 mm N 40 mm A Rf-coil x y 45 mm B Fig. 1 Left: Concept of the new probe; Right: Open device including Magnet, rf and gradient coils. The operatival probe is now optimized by shieldings and in its dimensions to avoid magnetostriction and electroacustic ringing. As a result of the work the dead time of this device was minimized from 2 ms to less than ms. The improvement in the signal to noise ratio allows us to detect a Hahn-Echo in a one-scan experiment.

50 50 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie Additionally an assortment of different coils has been developed and optimized by Fig. 2: 1) FEM simulation of a rf-coil; Hall probe measurements: 2) of one field component of a rf-coil; 3) of the B 0z component; 4) of a gradient system. finit element calculations (Quickfield ) [Fig. 2] to increase the penetration depth, to homogenize the B 1-Field or to avoid external noise. A special pole shoe has been simulated, built and investigated in order to concentrate the field lines of the B 1 field. Other Scientific Projects Investigations of particle motions in granular media by the NMR-MOUSE Detection of aging process of polymers NMR on snow in highly inhomogenious fields Additional Functions Teaching assistant in laboratory studies of Macromolecular Chemistry.

51 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 51 Cand. Chem. Kerstin Kletzke Diploma student NMR-Investigation of the Anesthetic Activity of Xenon in Myocard Cells supported by the START program of the faculty of medicine (University Hospital Aachen) The application of xenon for anesthesia has recently received renewed interest due to its nearly ideal properties as an anesthetic regarding intraoperative hemodynamic stability and the favorable recovery period. In contrast to common anesthetics (e.g. halothane) xenon shows very modest side effects on the cardiac circulatory system, and for this reason it is often applied to patients with cardiac problems. Nevertheless the anesthetic activity of the inert gas xenon and its interaction with the heart have hardly been investigated. The aim of this project is the experimental investigation of the molecular mechanism of the biological activity of the noble gas xenon in isolated myocard cells of adult rats. 129 Xe is an NMR-active nucleus with great sensitivity of its NMR parameters to the local environment. Its chemical shift changes in a wide range (as much as 200 ppm in this case) depending on the state of the matter. So with NMR spectroscopy it is possible to differentiate e.g. between xenon in the gaseous state, dissolved xenon in the aqueous solution, in which the cells are suspended, and xenon inside the cells (Fig. 1). In applied NMR research relaxation- and diffusion measurements are common methods to characterize tissue properties. The relaxation time is directly influenced by the mobility of the observed nuclei resp. molecules. An intense interaction with surfaces, dissolved macromolecules as well as an enhancement of the viscosity of the medium leads to a reduction of the relaxation time. The measurement of the

52 52 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie Fig. 1: In-vitro NMR spectrum of isolated heart muscle cells in aqueous solution fumigated with 20 bars Xe, depicting the different chemical shifts of intra- and extracellular Xe. diffusion coefficient serves to assess the translational mobility of the xenon atoms and their restriction e.g. by cell membranes. The ability of xenon to be hyperpolarized by means of optical pumping provides an extraordinary advantage for NMR. Optical pumping is a mechanism for the transfer of angular momentum from circularly polarized light to electronic and nuclear spins. Laser-polarized noble gas NMR has attracted special attention in material science, solid state chemistry, and clinical medicine. Under optimized conditions hyperpolarized xenon can give sensitivity enhancement of as much as 10 5 compared to thermally polarized xenon. This signal enhancement provides the opportunity to obtain spectra in a single acquisition and to observe dynamic processes. Due to the reduction of the measurement time it is now possible to measure under in-vivo conditions.

53 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 53 Cand. Chem. Kai Kremer Diploma student Curing of Adhesives in Glass-Metal-Compounds by unilateral NMR Supported by and in collaboration with: EFTEC AG, Switzerland The aim of this work was to investigate the possibility of non-destructive on-line monitoring of adhesive curing for front window panes of cars by use of the NMR- MOUSE. The samples were heat-cured as well as moisture-cured polyurethane rubber and 2K rubber adhesive. The adhesives were positioned in between sheets of 6 mm glass and 0.8 mm metal. The T 2-measurements took place at a depth of 7-9 mm using a CPMG sequence. Cured and uncured PUR differed in T 2 by a factor 2. Measurements at temperatures in between 10 C and 45 C showed that T 2 depends on temperature. Four different rubber tyres could be distinguished by T 2 measurements. All these measurements showed the possibility of detecting the change of molecular mobility following the curing process. Fig. 1: CPMG data of cured and uncured PUR.

54 54 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie For the moisture cured and the 2K PUR samples the complete curing processes was followed in tune. A striking result was, that curing of moisture-curing PUR takes much longer than expected. Furthermore, defects in moisture cured samples could be detected by the NMR-MOUSE by changes in the amplitudes. Fig. 2: Temperature dependence of relaxation times for moisture cured PUR samples. Other Scientific Projects Imaging with the NMR-MOUSE. Additional Functions Teaching assistant in laboratory studies of Macromolecular Chemistry. Administration of research and development projects in collaboration with industry.

55 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 55 Dipl.-Chem. Holger Kühn Doctoral student NMR Investigation of Solvents with Hyperpolarized Xenon at High Magnetic Fields The limitations imposed by the lack of sensitivity is the main drawback of nuclear resonance spectroscopy. In case of noble gases the degree of polarization can be increased by hyperpolarization. The main advantage of hyperpolarized noble gases is that the nuclear spin polarization is independent of the external magnetic field. This benefit can be exploited for NMR both in high and very low magnetic fields. The xenon isotope 129 (nuclear spin I=1/2) became a very popular probe for investigations of microporous media. The natural abundance of 129 Xe is 26.44%, its sensitivity of relative to 1 H is comparable to that of 13 C. The disadvantage of its low gyromagnetic ratio is compensated by hyperpolarization. Optically polarized xenon has found widespread applications in NMR spectroscopy. It is used in physical chemistry, geophysics, biotechnology, and medical imaging. An enormous potential of hyperpolarized xenon lies in transferring its large polarization to other nuclei via the Spin Polarized Induced Nuclear Overhauser Effect (SPINOE). It is a challenge to find a carrier system which transports the polarized gas to the sample which is examined. For medical application (e. g. imaging of the stomach) especially water and ethanol represent two interesting solvents in consideration of well suited transport systems. In this study pure water, pure ethanol, and ethanol / water mixtures (50/50, 70/30, 80/20, 90/10) have been investigated by hyperpolarized xenon. Using a Rb-Xe gas flow hyperpolarizer, based on Rb-Xe spin exchange optical pumping at high gas pressure, with a trap of liquid nitrogen hyperpolarized xenon was frozen on top of a solvent layer. At the beginning of the measurement (single-shot experiments, pulsewidth: 0.5 µs) at a magnetic field of 7 T when the sample temperature is about 100 K huge signals arising from xenon ice and liquid xenon are detected (δ Xe(s): 305 ppm, δ Xe(l): 245 ppm). These signals are degrading with

56 56 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie increasing temperature. In the case of pure water the formation of Xe/H 2O clathrates takes about 3 minutes at a gas pressure of 7 bars. Broad signals of two different cages are observed: dodecahedral ( ppm) and tetrakaidecahedral ( ppm). The signal of hyperpolarized Xe in water has a chemical shift of 193 Fig. 1: Chemical shifts of hyperpolarized Xe in ppm at room temperature. Ethanol EtOH/H 2O at equilibrium. is known to pass through different polymorphic forms (crystal I, crystal II, glassy liquid, glassy crystal II, supercooled liquid, liquid) in a temperature range of 77 to 300 K, a fact which makes the classification of observed signals more difficult. At equilibrium the signal of hyperpolarized xenon dissolved in ethanol has a chemical shift of 164 ppm. Mixtures of ethanol and water show xenon signals between 193 and 164 ppm (see figure 1). The dynamics of the formation of the clathrates in ethanol/water mixtures are quite different compared to the pure liquids (see figure 2). The spectra of the mixtures show near the free gas (A) a signal which arises from void spaces (B) due to a competition between ethanol and water during the formation of different clathrates (C+D). With increasing temperature the void spaces are growing and the signal (B) is shifted towards the signal of the free gas (A). The signal of the liquid xenon (E) disappears 40 seconds after starting the measurement. Further information about the formation of clathrates can be obtained using Fig. 2: NMR spectrum of a EtOH/H 2O mixture (80/20) 30 s after starting the measurement. spectroscopic imaging methods.

57 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 57 Other Scientific Projects Investigation of elastomers by 1 H NMR in homogenous and inhomogenous magnetic fields. Investigation of elastomers by 129 Xe NMR in homogenous magnetic fields. Additional Functions Teaching assistant in laboratory studies of Macromolecular Chemistry.

58 58 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie Dipl.-Chem. Markus Küppers Doctoral student MRI of a multicomponent diffusion driven system supported by Sonderforschungsbereich 540 (DFG) A major economic interest in the chemical industry is the continuous optimization of the production of chemical substances, to assure quality of the product while at the same time respecting the need of minimizing the consumption of resources and energy. One example for such a new production technique is the enzyme driven esterification reaction. Enzymes used in such processes can only be active in an aqueous environment and can only cope with a limited range of reactant concentrations. A common approach for such an optimization uses the physical separation of the aqueous reaction compartment and the organic solvent by enclosing the enzyme in a matrix of alginate gel. By dispersing the matrix as spherical drops within the reactant solution a diffusion driven exchange of reactants and reaction products through the gel allows a constant replacement of all the chemical substances involved. A major problem, however, in designing such microreactors is the lack of understanding of the exact properties and timescale of material transport within the gel drops. The ingress of all of the involved reactants as well as the expulsion of both reaction products was investigated by means of 1D 1 H concentration mapping and 2D FLASH imaging, acquiring typically images over a period of h. The results of the investigations presented enter the development of even smaller microreactors with improved enzyme distribution and gel matrices in order to achieve more efficient ester production and release rates for potential industrial-scale applications.

59 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 59 Figure 1: Maps on loss of water of the gel drop when in contact with propionic acid acquired with a chemical shift resolved 1D pulse sequence. The spatial dimension is shown on the horizontal axis, chemical shift information on the perpendicular axis. Other Scientific Projects MRI research on Cable isolation (in cooperation with A. Wiesmath and S. Sharma) MRI research on polymer degeneration (in cooperation with the German Wool Institute) Additional Functions Administration of Windows NT / 2000 / Linux / Irix workstations and servers , internal computer network, and telephone system administration Administration and maintenance of the Bruker Spectrometer (together with M. Adams) Coordination of some projects in SFB 540.

60 60 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie Dipl.-Chem. Marion I. Menzel Doctoral student NMR on contaminated sea ice supported by Studienstiftung des deutschen Volkes The most important feature of the polar seas is the presence of a seasonally changing sea ice cover. The knowledge of the porous, brine filled sea ice microstructure and its formation is a prerequisite for understanding the interaction and influence of sea ice with the atmosphere and global climate and for evaluating threats to the polar ecosystem in form of anthropogenous sources of pollution. Investigations of the physico-chemical properties of sea ice are carried out with various invasive and noninvasive methods, but the application of nuclear magnetic resonance (NMR) to investigate sea ice has been reported only a few times [1-6]. Fast 1 H-NMR imaging was applied to reveal phase transitions in ice. The dynamics of the freezing process of salt water was surveyed by 1 H-FLASH imaging with a temporal resolution of 2 minutes. Figure 1 depicts a cross section of a brine filled tube, showing the initial formation of crystallites, which rapidly grow together. Fig.1: Freezing process of 3.5% NaCl solution. After initial formation, the crystallites rapidly grow together, forming a complex porous network. The first three images are not shown.

61 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 61 1 H-NMR self-diffusion was used to probe the porous structure and brine mobility of sea ice below the spatial resolution limit of NMR imaging. Anisotropic and restricted diffusion was found in ice, indicating smaller elongated pores of approximately 30 µm. Brine 1 H-NMR self-diffusion coefficients in sea ice were determined for observation times between 0.1 and 2.0 s and were found to vary between 1.0 and 4.0 x [m 2 s -1 ], depending on the observation time and the direction of the observed diffusion. Self-diffusion along the main axis of diffusion was observed to be twice as fast on average as in perpendicular directions. A full characterization of brine self-diffusion can be achieved by measuring the spatially resolved 1 H-NMR self-diffusion tensor. The relative orientation of the principal axis system of diffusion with respect to the laboratory coordinate frame was determined, and indicates an orientation of the main diffusivity direction along the growth direction of the ice sample. The analysis of the self-diffusion tensor included the development of a software program in PV-Wave and the investigation of two model systems, 3.5% NaCl-solution as an isotropic system and a rhubarb stalk as an anisotropic system. [1] Weeks, W. F., Ackley, S. F., CRREL Rep (1982). [2] Richardson, C., Keller, E., J. Glaciol., 6, 89 (1966). [3] Edelstein, W. A., Schulson, E. M., J. Glaciol., 37, 177 (1991). [4] Callaghan, P. T. et al. J. Magn. Reson. 133, 148 (1998). [5] Callaghan, P. T., Dykstra, R., Eccles, C.D., Haskell, T.G., Seymour, J.D., Cold Regions Science And Technology (29)2 153 (1999). [6] Menzel, M. I., Han, S., Stapf, S., Blümich, B., J. Magn. Reson. 143, 376 (2000). Other Scientific Projects Research stay with Prof. Callaghan at the Institute of Fundamental Sciences, Massey University, Palmerstone North, New Zealand (March May 2001). Topic: Spatially resolved diffusion tensor on salt water ice Additional Functions spectrometer maintenance

62 62 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie Dipl.-Chem. Jan Plaß Doctoral student 31 P NMR Studies on Alkyl Phosphate Emulsifiers in Cosmetic Oil-in-Water Emulsions supported by Beiersdorf AG Hamburg Cosmetic oil-in-water emulsions with a stearyl phosphate emulsifier are examined by means of static and dynamic 31 P nuclear magnetic resonance (NMR) techniques to characterize the molecular properties of the emulsifier in situ. The interfacially bound emulsifier can be detected by high-resolution NMR spectroscopy, whereas the excess emulsifier exists as a solid lipid phase not detectable by this technique. The emulsions and the emulsifier raw material, consisting of monostearyl phosphate as well as distearyl phosphate, are examinated by solid state cross polarization magic angle spinning NMR spectroscopy to prove the existence of solid emulsifier phases in the emulsions. By applying dynamic 31 P NMR methods to the interfacially bound emulsifier, information about the molecular dynamics at the interface is obtained. The results of the T 1 and T 2 relaxation time measurements indicate a restricted motion of the molecules that is dependent on the oil droplet size in the emulsions. This is verified by 31 P NMR pulsed gradient spin echo self-diffusion measurements on emulsions with different droplets sizes. Only about 5 wt% of the total emulsifier used is bound at the interface; the excess forms solid lipid phases. The coverage of the interface seems to be independent of the emulsifier concentration. Only the monoester of the emulsifier raw material shows interfacial activity. Its mobility indicates the two-dimensional environment of the molecules on the surface of the oil droplets [1]. [1] J. Plass, D. Emeis, B. Blümich, 31 P Nuclear Magnetic Resonance Studies on Alkyl Phosphate Emulsifiers in Cosmetic Oil-in-Water Emulsions, J. Surfact. Deterg. 4, (2001).

63 Annual Report 2001 ITMC Lehrstuhl für Makromolekulare Chemie 63 Dipl.-Chem. Ing. Xiaohong Ren Doctoral student, DAAD scholarship Flow propagator and flow imaging in packed beds of low tube-to-particle diameter ratio Detailed knowledge of the fluid flow profile is essential for proper design of fixed bed processes. Due to the non-uniform radial distribution of voidage, permeability, and interstitial velocity in a critical region close to the wall, the ratio of tube diameter (d t) and particle diameter (d p) may influence transport properties in fixed bed catalytic reactors. Despite the multitude of publications, systematic investigations for low dimensionless tube diameters d t/d p are missing, especially for non-spherical particles. In this work, magnetic resonance imaging (MRI) and pulsed gradient stimulated echo (PGSTE) nuclear magnetic resonance experiments are used to probe the velocity profile and velocity distribution in packed beds at low tube-to-particle diameter ratio. The influence of flow rate F v (1.0 ml/s 13 ml/s), the dimensionless tube diameter d t/d p (1.3 30), as well as the shapes of the catalyst pellets has been examined. averaged propagator cylindrical platin catalyst, a φ 2x6 mm, F v =6.38 ml/s, a) = 150 ms b) = 250 ms b c) = 350 ms d) = 500 ms c d e) = 750 ms e averaged propagator a b c d e F v =2.9 ml/s, =750 mm glass beads e) φ 2 mm c) φ 4 mm spherical catalyst b) φ 2mm cylindrical catalyst, d) φ2x6 mm a) φ4.5x4.5 mm displacement [mm] displacement [mm] Fig. 1: Averaged propagator in dependence of the observation time in a packed bed with cylindrical platinum catalyst. Fig. 2: Comparison of the averaged propagator in fixed beds filled either with glass beads or porous catalysts.

64 64 Annual Report 2000 ITMC Lehrstuhl für Makromolekulare Chemie A typical results for the averaged flow propagator in dependence of the observation time is shown in Fig. 1. Stagnant and moving fluid fractions can be distinguished in the experimental data. While the molecules in the streaming fluid migrate over steadily increasing distance with growing observation time, the stagnant fluid fraction decreases continuously. The dimensionless tube diameter did not change the profile of the averaged displacement propagator in packed glass beads beds, but the shape and the type of the porous catalysts has an influence on the averaged propagator (Fig. 2). The fluid confined in the pores of the cylindrical and the spherical Pt/Ni-Al 2O 3 catalyst pellets contributes more significantly to the stagnant phase, and the spread of the velocity distribution is much broader and more heterogeneous, which leads to a smaller fraction of moving fluid. This was also proved by the spatial velocity distribution employing NMR imaging. As Fig. 3: Velocity distribution in the packed packed bed with spherical shown in Fig. 3, a significant heterogeneity catalyst (d p=2 mm, F V=6.38 ml/s) in the flow was observed. In particular, the flow profiles show higher velocities in the vicinity of the wall. Moreover, from the average displacement flow propagator derived by the PGSTE experiments, the dispersion coefficients are determined at a range of observation times over which the flow develops. The dispersion properties obtained from these velocity profiles have been shown to compare well with the results of non spatially resolved traditional chemical engineering methods, but provide a much more detailed description of the spatial dependence of the flow process. Other Scientific Projects Supervision of advanced laboratory studies in Macromolecular Chemistry. Additional Functions Teaching assistant in laboratory studies of Macromolecular Chemistry.

Annual Report. MARC Zentrum für Magnetische Resonanz. Lehrstuhl für Makromolekulare Chemie. Redaction:

Annual Report. MARC Zentrum für Magnetische Resonanz. Lehrstuhl für Makromolekulare Chemie. Redaction: Rheinisch-Westfälische Technische Hochschule Aachen Institut für Technische Chemie und Makromolekulare Chemie Lehrstuhl für Makromolekulare Chemie MARC Zentrum für Magnetische Resonanz Annual Report 2000

More information

Annual Report. Zentrum für Magnetische Resonanz. Editorial: 1 Annual Report 2003 ITMC Lehrstuhl für Makromolekulare Chemie

Annual Report. Zentrum für Magnetische Resonanz. Editorial: 1 Annual Report 2003 ITMC Lehrstuhl für Makromolekulare Chemie 1 Annual Report 2003 ITMC Lehrstuhl für Makromolekulare Chemie Rheinisch-Westfälische Technische Hochschule Aachen Institut für Technische Chemie und Makromolekulare Chemie Lehrstuhl für Makromolekulare

More information

Referinta bibliografica ai ni nefi ai/neffi

Referinta bibliografica ai ni nefi ai/neffi Indeplinirea standardelor indicatorilor I si P Conf. Dr. Radu Fechete Universitatea Tehnica din Cluj-Napoca Numarul publicatiei 1 Referinta bibliografica ai ni nefi ai/neffi Single-quantum nmr spinning-side-band

More information

Mobile NMR for geophysical analysis and materials testing

Mobile NMR for geophysical analysis and materials testing Pet.Sci.(2009)6:1-7 DOI 10.1007/s12182-009-0001-4 1 Mobile NMR for geophysical analysis and materials testing BLÜMICH Bernhard, MAULER Jörg, HABER Agnes, PERLO Juan, DANIELI Ernesto and CASANOVA Federico

More information

Unilateral NMR of Activated Carbon

Unilateral NMR of Activated Carbon Unilateral NMR of Activated Carbon Stuart Brewer 2, Hans Adriaensen 1, Martin Bencsik 1, Glen McHale 1 and Martin W Smith 2 [1]: Nottingham Trent University (NTU), UK [2]: Defence Science and Technology

More information

Principles of Nuclear Magnetic Resonance Microscopy

Principles of Nuclear Magnetic Resonance Microscopy Principles of Nuclear Magnetic Resonance Microscopy Paul T. Callaghan Department of Physics and Biophysics Massey University New Zealand CLARENDON PRESS OXFORD CONTENTS 1 PRINCIPLES OF IMAGING 1 1.1 Introduction

More information

NMR Spectroscopy of Polymers

NMR Spectroscopy of Polymers UNESCO/IUPAC Course 2005/2006 Jiri Brus NMR Spectroscopy of Polymers Brus J 1. part At the very beginning the phenomenon of nuclear spin resonance was studied predominantly by physicists and the application

More information

Unilateral Nuclear Magnetic Resonance for Quality Control

Unilateral Nuclear Magnetic Resonance for Quality Control Unilateral Nuclear Magnetic Resonance for Quality Control The NMR-MOUSE B. Blümich, S. Anferova, K. Kremer, S. Sharma, V. Herrmann, and A. Segre N uclear magnetic resonance (NMR) spectroscopy and NMR imaging

More information

NMR Imaging in porous media

NMR Imaging in porous media NMR Imaging in porous media What does NMR give us. Chemical structure. Molecular structure. Interactions between atoms and molecules. Incoherent dynamics (fluctuation, rotation, diffusion). Coherent flow

More information

Table 1 Types of solvents with spherical and linear molecules absorbed in EPDM and the mass uptake Q w. EPDM rubber with various solvents (60 phr)

Table 1 Types of solvents with spherical and linear molecules absorbed in EPDM and the mass uptake Q w. EPDM rubber with various solvents (60 phr) normalized distributions normalized distributions Scientific report related to the implementation of project: Structure-dynamics-properties relationships and aging effects in nanocomposite elastomers and

More information

MRI Physics I: Spins, Excitation, Relaxation

MRI Physics I: Spins, Excitation, Relaxation MRI Physics I: Spins, Excitation, Relaxation Douglas C. Noll Biomedical Engineering University of Michigan Michigan Functional MRI Laboratory Outline Introduction to Nuclear Magnetic Resonance Imaging

More information

Dependence of Order and Dynamics in Polymers and Elastomers under Deformation Revealed by NMR Techniques

Dependence of Order and Dynamics in Polymers and Elastomers under Deformation Revealed by NMR Techniques Vol. 108 (2005) ACTA PHYSICA POLONICA A No. 2 Proceedings of the XXI International Meeting on Radio and Microwave Spectroscopy RAMIS 2005, Poznań-Bȩdlewo, Poland, April 24 28, 2005 Dependence of Order

More information

MAGNETIC RESONANCE IMAGING OF SOLVENT TRANSPORT IN POLYMER NETWORKS

MAGNETIC RESONANCE IMAGING OF SOLVENT TRANSPORT IN POLYMER NETWORKS * - 9 I MAGNETIC RESONANCE IMAGING OF SOLVENT TRANSPORT IN POLYMER NETWORKS Robert E. Botto and George D. Cody Chemistry Division, Argonne National Laboratory The spectroscopic technique of magnetic resonance

More information

General NMR basics. Solid State NMR workshop 2011: An introduction to Solid State NMR spectroscopy. # nuclei

General NMR basics. Solid State NMR workshop 2011: An introduction to Solid State NMR spectroscopy. # nuclei : An introduction to Solid State NMR spectroscopy Dr. Susanne Causemann (Solid State NMR specialist/ researcher) Interaction between nuclear spins and applied magnetic fields B 0 application of a static

More information

Principles of Nuclear Magnetic Resonance in One and Two Dimensions

Principles of Nuclear Magnetic Resonance in One and Two Dimensions Principles of Nuclear Magnetic Resonance in One and Two Dimensions Richard R. Ernst, Geoffrey Bodenhausen, and Alexander Wokaun Laboratorium für Physikalische Chemie Eidgenössische Technische Hochschule

More information

Magnetic Resonance Imaging. Pål Erik Goa Associate Professor in Medical Imaging Dept. of Physics

Magnetic Resonance Imaging. Pål Erik Goa Associate Professor in Medical Imaging Dept. of Physics Magnetic Resonance Imaging Pål Erik Goa Associate Professor in Medical Imaging Dept. of Physics pal.e.goa@ntnu.no 1 Why MRI? X-ray/CT: Great for bone structures and high spatial resolution Not so great

More information

4 Spin-echo, Spin-echo Double Resonance (SEDOR) and Rotational-echo Double Resonance (REDOR) applied on polymer blends

4 Spin-echo, Spin-echo Double Resonance (SEDOR) and Rotational-echo Double Resonance (REDOR) applied on polymer blends 4 Spin-echo, Spin-echo ouble Resonance (SEOR and Rotational-echo ouble Resonance (REOR applied on polymer blends The next logical step after analyzing and concluding upon the results of proton transversal

More information

Everyday NMR. Innovation with Integrity. Why infer when you can be sure? NMR

Everyday NMR. Innovation with Integrity. Why infer when you can be sure? NMR Everyday NMR Why infer when you can be sure? Innovation with Integrity NMR Only NMR gives you definitive answers, on your terms. Over the past half-century, scientists have used nuclear magnetic resonance

More information

Mechanical properties of polymers: an overview. Suryasarathi Bose Dept. of Materials Engineering, IISc, Bangalore

Mechanical properties of polymers: an overview. Suryasarathi Bose Dept. of Materials Engineering, IISc, Bangalore Mechanical properties of polymers: an overview Suryasarathi Bose Dept. of Materials Engineering, IISc, Bangalore UGC-NRCM Summer School on Mechanical Property Characterization- June 2012 Overview of polymer

More information

Permanent Magnet Arrangements for Low-Field NMR

Permanent Magnet Arrangements for Low-Field NMR Excerpt from the Proceedings of the COMSOL Conference 2009 Milan Permanent Magnet Arrangements for Low-Field NMR Carsten Horch, Stefan Schlayer, Frank Stallmach Faculty of Physics and Earth Sciences, University

More information

Detection at a Distance for More Sensitive MRIDetection at a D...

Detection at a Distance for More Sensitive MRIDetection at a D... March 15, 2004 Detection at a Distance for More Sensitive MRI Contact: Paul Preuss, paul_preuss@lbl.gov Advanced Search Search Tips BERKELEY, CA! Alexander Pines and his colleagues have discovered a remarkable

More information

PROTEIN NMR SPECTROSCOPY

PROTEIN NMR SPECTROSCOPY List of Figures List of Tables xvii xxvi 1. NMR SPECTROSCOPY 1 1.1 Introduction to NMR Spectroscopy 2 1.2 One Dimensional NMR Spectroscopy 3 1.2.1 Classical Description of NMR Spectroscopy 3 1.2.2 Nuclear

More information

Structure, dynamics and heterogeneity: solid-state NMR of polymers. Jeremy Titman, School of Chemistry, University of Nottingham

Structure, dynamics and heterogeneity: solid-state NMR of polymers. Jeremy Titman, School of Chemistry, University of Nottingham Structure, dynamics and heterogeneity: solid-state NMR of polymers Jeremy Titman, School of Chemistry, University of Nottingham Structure, dynamics and heterogeneity Structure Dynamics conformation, tacticity,

More information

Relaxation times in nuclear magnetic resonance

Relaxation times in nuclear magnetic resonance Relaxation times in TEP Related topics Nuclear spins, atomic nuclei with a magnetic moment, precession movement of the nuclear spins, Landau-Lifshitz equation, Bloch equation, magnetisation, resonance

More information

RADIOLOGIV TECHNOLOGY 4912 COMPREHENSEIVE REVIEW/MRI WORSHEET #1- PATIENT CARE AND SAFETY/PHYSICAL PRINCIPLES

RADIOLOGIV TECHNOLOGY 4912 COMPREHENSEIVE REVIEW/MRI WORSHEET #1- PATIENT CARE AND SAFETY/PHYSICAL PRINCIPLES RADIOLOGIV TECHNOLOGY 4912 COMPREHENSEIVE REVIEW/MRI WORSHEET #1- PATIENT CARE AND SAFETY/PHYSICAL PRINCIPLES 1. What are potential consequences to patients and personnel should there be a release of gaseous

More information

High-Resolutio n NMR Techniques i n Organic Chemistry TIMOTHY D W CLARIDGE

High-Resolutio n NMR Techniques i n Organic Chemistry TIMOTHY D W CLARIDGE High-Resolutio n NMR Techniques i n Organic Chemistry TIMOTHY D W CLARIDGE Foreword Preface Acknowledgements V VI I X Chapter 1. Introduction 1.1. The development of high-resolution NMR 1 1.2. Modern

More information

CHEMISTRY (CHEM) CHEM 5800 Principles Of Materials Chemistry. Tutorial in selected topics in materials chemistry. S/U grading only.

CHEMISTRY (CHEM) CHEM 5800 Principles Of Materials Chemistry. Tutorial in selected topics in materials chemistry. S/U grading only. Chemistry (CHEM) 1 CHEMISTRY (CHEM) CHEM 5100 Principles of Organic and Inorganic Chemistry Study of coordination compounds with a focus on ligand bonding, electron counting, molecular orbital theory,

More information

NMR and Core Analysis

NMR and Core Analysis NMR and Core Analysis Technical Datasheet Introduction Most people involved in core analysis know that NMR (Nuclear Magnetic Resonance) has been part of the available suite of well logging measurements

More information

Spin Dynamics Basics of Nuclear Magnetic Resonance. Malcolm H. Levitt

Spin Dynamics Basics of Nuclear Magnetic Resonance. Malcolm H. Levitt Spin Dynamics Basics of Nuclear Magnetic Resonance Second edition Malcolm H. Levitt The University of Southampton, UK John Wiley &. Sons, Ltd Preface xxi Preface to the First Edition xxiii Introduction

More information

NUCLEAR MAGNETIC RESONANCE. The phenomenon of nuclear magnetic resonance will be used to study magnetic moments of nuclei.

NUCLEAR MAGNETIC RESONANCE. The phenomenon of nuclear magnetic resonance will be used to study magnetic moments of nuclei. 14 Sep 11 NMR.1 NUCLEAR MAGNETIC RESONANCE The phenomenon of nuclear magnetic resonance will be used to study magnetic moments of nuclei. Theory: In addition to its well-known properties of mass, charge,

More information

Doppler echocardiography & Magnetic Resonance Imaging. Doppler echocardiography. History: - Langevin developed sonar.

Doppler echocardiography & Magnetic Resonance Imaging. Doppler echocardiography. History: - Langevin developed sonar. 1 Doppler echocardiography & Magnetic Resonance Imaging History: - Langevin developed sonar. - 1940s development of pulse-echo. - 1950s development of mode A and B. - 1957 development of continuous wave

More information

Suppression of Static Magnetic Field in Diffusion Measurements of Heterogeneous Materials

Suppression of Static Magnetic Field in Diffusion Measurements of Heterogeneous Materials PIERS ONLINE, VOL. 5, NO. 1, 2009 81 Suppression of Static Magnetic Field in Diffusion Measurements of Heterogeneous Materials Eva Gescheidtova 1 and Karel Bartusek 2 1 Faculty of Electrical Engineering

More information

M R I Physics Course. Jerry Allison Ph.D., Chris Wright B.S., Tom Lavin B.S., Nathan Yanasak Ph.D. Department of Radiology Medical College of Georgia

M R I Physics Course. Jerry Allison Ph.D., Chris Wright B.S., Tom Lavin B.S., Nathan Yanasak Ph.D. Department of Radiology Medical College of Georgia M R I Physics Course Jerry Allison Ph.D., Chris Wright B.S., Tom Lavin B.S., Nathan Yanasak Ph.D. Department of Radiology Medical College of Georgia M R I Physics Course Spin Echo Imaging Hahn Spin Echo

More information

Magnetic resonance imaging MRI

Magnetic resonance imaging MRI Magnetic resonance imaging MRI Introduction What is MRI MRI is an imaging technique used primarily in medical settings that uses a strong magnetic field and radio waves to produce very clear and detailed

More information

NMR Spectroscopy of Polymers

NMR Spectroscopy of Polymers r NMR Spectroscopy of Polymers Edited by ROGER N. IBBETT Courtaulds Research and Technology Coventry BLACKIE ACADEMIC & PROFESSIONAL An Imprint of Chapman & Hall London Glasgow New York Tokyo Melbourne

More information

Introduction to Biomedical Imaging

Introduction to Biomedical Imaging Alejandro Frangi, PhD Computational Imaging Lab Department of Information & Communication Technology Pompeu Fabra University www.cilab.upf.edu MRI advantages Superior soft-tissue contrast Depends on among

More information

CONTENTS. 2 CLASSICAL DESCRIPTION 2.1 The resonance phenomenon 2.2 The vector picture for pulse EPR experiments 2.3 Relaxation and the Bloch equations

CONTENTS. 2 CLASSICAL DESCRIPTION 2.1 The resonance phenomenon 2.2 The vector picture for pulse EPR experiments 2.3 Relaxation and the Bloch equations CONTENTS Preface Acknowledgements Symbols Abbreviations 1 INTRODUCTION 1.1 Scope of pulse EPR 1.2 A short history of pulse EPR 1.3 Examples of Applications 2 CLASSICAL DESCRIPTION 2.1 The resonance phenomenon

More information

The Neutron Scattering Society of America

The Neutron Scattering Society of America The Neutron Scattering Society of America www.neutronscattering.org Press Release, February 4, 2008 The Neutron Scattering Society of America is pleased to announce the 2008 recipients of its 3 major prizes.

More information

Technical University of Denmark

Technical University of Denmark Technical University of Denmark Page 1 of 11 pages Written test, 9 December 2010 Course name: Introduction to medical imaging Course no. 31540 Aids allowed: none. "Weighting": All problems weight equally.

More information

Nuclear Magnetic Resonance Imaging

Nuclear Magnetic Resonance Imaging Nuclear Magnetic Resonance Imaging Simon Lacoste-Julien Electromagnetic Theory Project 198-562B Department of Physics McGill University April 21 2003 Abstract This paper gives an elementary introduction

More information

NMR Spectroscopy. Guangjin Hou

NMR Spectroscopy. Guangjin Hou NMR Spectroscopy Guangjin Hou 22-04-2009 NMR History 1 H NMR spectra of water H NMR spectra of water (First NMR Spectra on Water, 1946) 1 H NMR spectra ethanol (First bservation of the Chemical Shift,

More information

Chemistry Departmental Mission Statement: Communicating Plus - Chemistry: Requirements for a major in chemistry:

Chemistry Departmental Mission Statement: Communicating Plus - Chemistry: Requirements for a major in chemistry: Chemistry Professors Colleen M. Byron (Chair); Dean A. Katahira; Associate Professor Joseph D. Scanlon; Assistant Professor Patrick H. Willoughby; Stockroom Supervisor Barbara Johnson Departmental Mission

More information

Agricultural. Chemistry. Agricultural production: crops and livestock Agrichemicals development: herbicides, pesticides, fungicides, fertilizers, etc.

Agricultural. Chemistry. Agricultural production: crops and livestock Agrichemicals development: herbicides, pesticides, fungicides, fertilizers, etc. Agricultural Agricultural production: crops and livestock Agrichemicals development: herbicides, pesticides, fungicides, fertilizers, etc. Agrichemicals testing Environmental testing Regulation Government:

More information

The physics US and MRI. Prof. Peter Bogner

The physics US and MRI. Prof. Peter Bogner The physics US and MRI Prof. Peter Bogner Sound waves mechanical disturbance, a pressure wave moves along longitudinal wave compression rarefaction zones c = nl, (c: velocity, n: frequency, l: wavelength

More information

V27: RF Spectroscopy

V27: RF Spectroscopy Martin-Luther-Universität Halle-Wittenberg FB Physik Advanced Lab Course V27: RF Spectroscopy ) Electron spin resonance (ESR) Investigate the resonance behaviour of two coupled LC circuits (an active rf

More information

The Superfluid Phase s of Helium 3

The Superfluid Phase s of Helium 3 The Superfluid Phase s of Helium 3 DIETER VOLLHARD T Rheinisch-Westfälische Technische Hochschule Aachen, Federal Republic of German y PETER WÖLFL E Universität Karlsruhe Federal Republic of Germany PREFACE

More information

MATERIALS SCIENCE POLYMERS

MATERIALS SCIENCE POLYMERS POLYMERS 1) Types of Polymer (a) Plastic Possibly the largest number of different polymeric materials come under the plastic classification. Polyethylene, polypropylene, polyvinyl chloride, polystyrene,

More information

MRI in Review: Simple Steps to Cutting Edge Part I

MRI in Review: Simple Steps to Cutting Edge Part I MRI in Review: Simple Steps to Cutting Edge Part I DWI is now 2 years old... Mike Moseley Radiology Stanford DWI, b = 1413 T2wt, 28/16 ASN 21 San Francisco + Disclosures: Funding NINDS, NCRR, NCI 45 minutes

More information

Electrical Engineering 3BA3: Structure of Biological Materials

Electrical Engineering 3BA3: Structure of Biological Materials Electrical Engineering 3BA3: Structure of Biological Materials Day Class Instructor: Dr. I. C. BRUCE Duration of Examination: 3 Hours McMaster University Final Examination December, 2004 This examination

More information

Annual Report Editors: B. Blümich, M. Küppers Cover: K. Kupferschläger RHEINISCH-WESTFÄLISCHE TECHNISCHE HOCHSCHULE AACHEN

Annual Report Editors: B. Blümich, M. Küppers Cover: K. Kupferschläger RHEINISCH-WESTFÄLISCHE TECHNISCHE HOCHSCHULE AACHEN RHEINISCH-WESTFÄLISCHE TECHNISCHE HOCHSCHULE AACHEN INSTITUT FÜR TECHNISCHE UND MAKROMOLEKULARE CHEMIE LEHRSTUHL FÜR MAKROMOLEKULARE CHEMIE ZENTRUM FÜR MAGNETISCHE RESONANZ Annual Report 2009 Editors:

More information

QDTL. Liquid Mass Transfer and Diffusion Coefficient Unit PROCESS DIAGRAM AND UNIT ELEMENTS ALLOCATION. Electronic console

QDTL. Liquid Mass Transfer and Diffusion Coefficient Unit PROCESS DIAGRAM AND UNIT ELEMENTS ALLOCATION. Electronic console Engineering and Technical Teaching Equipment Liquid Mass Transfer and Diffusion Coefficient Unit QDTL Electronic console PROCESS DIAGRAM AND UNIT ELEMENTS ALLOCATION ISO 9001: Quality Management (for Design,

More information

EL-GY 6813/BE-GY 6203 Medical Imaging, Fall 2016 Final Exam

EL-GY 6813/BE-GY 6203 Medical Imaging, Fall 2016 Final Exam EL-GY 6813/BE-GY 6203 Medical Imaging, Fall 2016 Final Exam (closed book, 1 sheets of notes double sided allowed, no calculator or other electronic devices allowed) 1. Ultrasound Physics (15 pt) A) (9

More information

Basic MRI physics and Functional MRI

Basic MRI physics and Functional MRI Basic MRI physics and Functional MRI Gregory R. Lee, Ph.D Assistant Professor, Department of Radiology June 24, 2013 Pediatric Neuroimaging Research Consortium Objectives Neuroimaging Overview MR Physics

More information

Porous and granular materials: Applications in modern Science and Technology

Porous and granular materials: Applications in modern Science and Technology Porous and granular materials: Applications in modern Science and Technology Course Instructor: Prof. Arzhang Khalili, Max Planck Institute for Marine Microbiology, Germany Course Coordinator Dr. Shanmugam

More information

CHEMICAL ENGINEERING (CHE)

CHEMICAL ENGINEERING (CHE) Chemical Engineering (CHE) 1 CHEMICAL ENGINEERING (CHE) CHE 2033 Introduction to Chemical Process Engineering Prerequisites: CHEM 1515 and ENSC 2213 Description: Concurrent enrollment in MATH 2233 or 3263,

More information

NUCLEAR MAGNETIC RESONANCE STUDIES OF BIOLOGICAL AND BIOGEOCHEMICAL PROCESSES. Sarah Jane Vogt

NUCLEAR MAGNETIC RESONANCE STUDIES OF BIOLOGICAL AND BIOGEOCHEMICAL PROCESSES. Sarah Jane Vogt NUCLEAR MAGNETIC RESONANCE STUDIES OF BIOLOGICAL AND BIOGEOCHEMICAL PROCESSES by Sarah Jane Vogt A dissertation submitted in partial fulfillment of the requirements for the degree of Doctor of Philosophy

More information

Polymer dynamics. Course M6 Lecture 5 26/1/2004 (JAE) 5.1 Introduction. Diffusion of polymers in melts and dilute solution.

Polymer dynamics. Course M6 Lecture 5 26/1/2004 (JAE) 5.1 Introduction. Diffusion of polymers in melts and dilute solution. Course M6 Lecture 5 6//004 Polymer dynamics Diffusion of polymers in melts and dilute solution Dr James Elliott 5. Introduction So far, we have considered the static configurations and morphologies of

More information

Chapter 7. Nuclear Magnetic Resonance Spectroscopy

Chapter 7. Nuclear Magnetic Resonance Spectroscopy Chapter 7 Nuclear Magnetic Resonance Spectroscopy I. Introduction 1924, W. Pauli proposed that certain atomic nuclei have spin and magnetic moment and exposure to magnetic field would lead to energy level

More information

A method for imaging and spectroscopy. using γ-rays and magnetic resonance

A method for imaging and spectroscopy. using γ-rays and magnetic resonance A method for imaging and spectroscopy using γ-rays and magnetic resonance Y. Zheng et al. Nature 537, 19775 (Sep 2016) Parker Brue PHY 492 Abstract Background: Magnetic resonance imaging and Nuclear imaging

More information

Introduction to MRI. Spin & Magnetic Moments. Relaxation (T1, T2) Spin Echoes. 2DFT Imaging. K-space & Spatial Resolution.

Introduction to MRI. Spin & Magnetic Moments. Relaxation (T1, T2) Spin Echoes. 2DFT Imaging. K-space & Spatial Resolution. Introduction to MRI Spin & Magnetic Moments Relaxation (T1, T2) Spin Echoes 2DFT Imaging Selective excitation, phase & frequency encoding K-space & Spatial Resolution Contrast (T1, T2) Acknowledgement:

More information

Lecture 02 Nuclear Magnetic Resonance Spectroscopy Principle and Application in Structure Elucidation

Lecture 02 Nuclear Magnetic Resonance Spectroscopy Principle and Application in Structure Elucidation Application of Spectroscopic Methods in Molecular Structure Determination Prof. S. Sankararaman Department of Chemistry Indian Institution of Technology Madras Lecture 02 Nuclear Magnetic Resonance Spectroscopy

More information

The NMR Inverse Imaging Problem

The NMR Inverse Imaging Problem The NMR Inverse Imaging Problem Nuclear Magnetic Resonance Protons and Neutrons have intrinsic angular momentum Atoms with an odd number of proton and/or odd number of neutrons have a net magnetic moment=>

More information

Decoupling Theory and Practice

Decoupling Theory and Practice Decoupling Theory and Practice General Concepts We have spent the last two lectures discussing the structural implications of -coupling analysis and overall have discovered that the interaction may readily

More information

Biophysical Chemistry: NMR Spectroscopy

Biophysical Chemistry: NMR Spectroscopy Relaxation & Multidimensional Spectrocopy Vrije Universiteit Brussel 9th December 2011 Outline 1 Relaxation 2 Principles 3 Outline 1 Relaxation 2 Principles 3 Establishment of Thermal Equilibrium As previously

More information

Nanophysics: Main trends

Nanophysics: Main trends Nano-opto-electronics Nanophysics: Main trends Nanomechanics Main issues Light interaction with small structures Molecules Nanoparticles (semiconductor and metallic) Microparticles Photonic crystals Nanoplasmonics

More information

Undergraduate Research Opportunities in Chemistry. Marquette University. Department of Chemistry

Undergraduate Research Opportunities in Chemistry. Marquette University. Department of Chemistry Undergraduate Research Opportunities in Chemistry Marquette University Department of Chemistry Undergraduate Research Experiences in Chemistry The undergraduate research experience is a key ingredient

More information

Plan of the course PHYSICS. Academic year 2017/2018. University of Zagreb School of Dental Medicine

Plan of the course PHYSICS. Academic year 2017/2018. University of Zagreb School of Dental Medicine University of Zagreb School of Dental Medicine Plan of the course PHYSICS Academic year 2017/2018 Course coordinator: Assistant Professor Sanja Dolanski Babić, PhD 1 I. COURSE AIMS The goal of physics

More information

Two-Dimensional NQR Spectroscopy for the Characterization of Crystalline Powders

Two-Dimensional NQR Spectroscopy for the Characterization of Crystalline Powders Two-Dimensional NQR Spectroscopy for the Characterization of Crystalline Powders P. K ä u p e r 1, V. Göbbels, P. Blümler, a n d B. Blümich Lehrstuhl für Makromolekulare Chemie und Zentrum für Magnetische

More information

Elec Eng 3BA3: Structure of Biological Materials

Elec Eng 3BA3: Structure of Biological Materials Elec Eng 3BA3: Structure of Biological Materials Page 1 of 12 Day Class Instructor: Dr. I. C. BRUCE Duration of Examination: 3 Hours McMaster University Final Examination December 5, 2008 This examination

More information

NUCLEAR MAGNETIC RESONANCE. Introduction. Vol. 10 NUCLEAR MAGNETIC RESONANCE 637

NUCLEAR MAGNETIC RESONANCE. Introduction. Vol. 10 NUCLEAR MAGNETIC RESONANCE 637 Vol. 10 NUCLEAR MAGNETIC RESONANCE 637 NUCLEAR MAGNETIC RESONANCE Introduction An important objective in materials science is the establishment of relationships between the microscopic structure or molecular

More information

Measuring Spin-Lattice Relaxation Time

Measuring Spin-Lattice Relaxation Time WJP, PHY381 (2009) Wabash Journal of Physics v4.0, p.1 Measuring Spin-Lattice Relaxation Time L.W. Lupinski, R. Paudel, and M.J. Madsen Department of Physics, Wabash College, Crawfordsville, IN 47933 (Dated:

More information

Explorative Study of NMR Drilling Fluids Measurement

Explorative Study of NMR Drilling Fluids Measurement ANNUAL TRANSACTIONS OF THE NORDIC RHEOLOGY SOCIETY, VOL. 15, 2007 Explorative Study of NMR Drilling Fluids Measurement Rizal Rismanto, Claas van der Zwaag University of Stavanger, Dep. of Petroleum Technology,

More information

ENAS 606 : Polymer Physics

ENAS 606 : Polymer Physics ENAS 606 : Polymer Physics Professor Description Course Topics TA Prerequisite Class Office Hours Chinedum Osuji 302 Mason Lab, 432-4357, chinedum.osuji@yale.edu This course covers the static and dynamic

More information

NMR THEORY AND LABORATORY COURSE. CHEN: 696-Section 626.

NMR THEORY AND LABORATORY COURSE. CHEN: 696-Section 626. NMR THEORY AND LABORATORY COURSE. CHEN: 696-Section 626. 1998 Fall Semester (3 Credit Hours) Lectures: M, W 10-10.50 a.m., Richardson: 910 Laboratory Fri. 10-12, Richardson 912. Instructor: Parameswar

More information

Faculty: Andrew Carr, Ryan Felix, Stephanie Gould, James Hebda, Karla McCain, John Richardson, Lindsay Zack

Faculty: Andrew Carr, Ryan Felix, Stephanie Gould, James Hebda, Karla McCain, John Richardson, Lindsay Zack CHEMISTRY Chair: Bradley Smucker (Fall 2017) and Andrew Carr (Spring 2018) Faculty: Andrew Carr, Ryan Felix, Stephanie Gould, James Hebda, Karla McCain, John Richardson, Lindsay Zack Adjunct Instructor:

More information

Spectroscopy of Polymers

Spectroscopy of Polymers Spectroscopy of Polymers Jack L. Koenig Case Western Reserve University WOMACS Professional Reference Book American Chemical Society, Washington, DC 1992 Contents Preface m xiii Theory of Polymer Characterization

More information

NUMERICAL ANALYSES OF ELECTROMAGNETIC FIELDS IN HIGH VOLTAGE BUSHING AND IN ELECTROMAGNETIC FLOW METER

NUMERICAL ANALYSES OF ELECTROMAGNETIC FIELDS IN HIGH VOLTAGE BUSHING AND IN ELECTROMAGNETIC FLOW METER Intensive Programme Renewable Energy Sources May 2011, Železná Ruda-Špičák, University of West Bohemia, Czech Republic NUMERICAL ANALYSES OF ELECTROMAGNETIC FIELDS IN HIGH VOLTAGE BUSHING AND IN ELECTROMAGNETIC

More information

CHARACTERIZATION OF INTERACTION BETWEEN OIL/BRINE/ROCK UNDER DIFFERENT ION CONDITIONS BY LOW FIELD SOLID-STATE NMR

CHARACTERIZATION OF INTERACTION BETWEEN OIL/BRINE/ROCK UNDER DIFFERENT ION CONDITIONS BY LOW FIELD SOLID-STATE NMR SCA2016-077 1/6 CHARACTERIZATION OF INTERACTION BETWEEN OIL/BRINE/ROCK UNDER DIFFERENT ION CONDITIONS BY LOW FIELD SOLID-STATE NMR Shijing XU 1, Xiaoliang WANG 2, Weifeng LV 1, Qingjie LIU 1, Jiazhong

More information

Physical fundamentals of magnetic resonance imaging

Physical fundamentals of magnetic resonance imaging Physical fundamentals of magnetic resonance imaging Stepan Sereda University of Bonn 1 / 26 Why? Figure 1 : Full body MRI scan (Source: [4]) 2 / 26 Overview Spin angular momentum Rotating frame and interaction

More information

Qualification of Automated Low-Field NMR Relaxometry for Quality Control of Polymers in a Production Setting

Qualification of Automated Low-Field NMR Relaxometry for Quality Control of Polymers in a Production Setting UCRL-JRNL-231834 Qualification of Automated Low-Field NMR Relaxometry for Quality Control of Polymers in a Production Setting S.C. Chinn, A. Cook-Tendulkar, R.S. Maxwell, H. Wheeler, M. Wilson, Z.H. Xie

More information

PII S X(98) FLOW AND TRANSPORT STUDIES IN (NON)CONSOLIDATED POROUS (BIO)SYSTEMS CONSISTING OF SOLID OR POROUS BEADS BY PFG NMR

PII S X(98) FLOW AND TRANSPORT STUDIES IN (NON)CONSOLIDATED POROUS (BIO)SYSTEMS CONSISTING OF SOLID OR POROUS BEADS BY PFG NMR PII S0730-725X(98)00052-6 Magnetic Resonance Imaging, Vol. 16, Nos. 5/6, pp. 569 573, 1998 1998 Elsevier Science Inc. All rights reserved. Printed in the USA. 0730-725X/98 $19.00.00 Contributed Paper FLOW

More information

Vapor contribution to the time dependence of the effective diffusion coefficient in partially filled porous glasses

Vapor contribution to the time dependence of the effective diffusion coefficient in partially filled porous glasses The Open-Access Journal for the Basic Principles of Diffusion Theory, Experiment and Application Vapor contribution to the time dependence of the effective diffusion coefficient in partially filled porous

More information

Metrology is not a cost factor, but a profit center

Metrology is not a cost factor, but a profit center Edition February 2018 Semiconductor technology & processing Metrology is not a cost factor, but a profit center In recent years, remarkable progress has been made in the field of metrology, which is crucial

More information

Spin Track TD-NMR Spectrometer. Applications and Instrumentation Review

Spin Track TD-NMR Spectrometer. Applications and Instrumentation Review Spin Track TD-NMR Spectrometer Applications and Instrumentation Review "Spin Track" Time-Domain (TD) NMR spectrometer is a high quality time-domain NMR instrument with wide range of applications, advanced

More information

Department of Physics (857) University of California, Santa Barbara, Santa Barbara, CA

Department of Physics (857) University of California, Santa Barbara, Santa Barbara, CA Christopher Blake Wilson Curriculum vitae Department of Physics (857) 209-4798 University of California bwil@physics.ucsb.edu Santa Barbara, CA 93106 Education University of California, Santa Barbara,

More information

Outline of the talk How to describe restricted diffusion? How to monitor restricted diffusion? Laplacian eigenfunctions in NMR Other applications Loca

Outline of the talk How to describe restricted diffusion? How to monitor restricted diffusion? Laplacian eigenfunctions in NMR Other applications Loca Laplacian Eigenfunctions in NMR Denis S. Grebenkov Laboratoire de Physique de la Matière Condensée CNRS Ecole Polytechnique, Palaiseau, France IPAM Workshop «Laplacian Eigenvalues and Eigenfunctions» February

More information

CHEMISTRY (CHEM) Chemistry (CHEM) 1

CHEMISTRY (CHEM) Chemistry (CHEM) 1 Chemistry (CHEM) 1 CHEMISTRY (CHEM) CHEM 100 Chemistry: Issues and Answers (3 crs) Prerequisite: No credit if taken after CHEM 101, CHEM 103, or CHEM 115. An exploration into the world of atoms and molecules,

More information

Ferdowsi University of Mashhad

Ferdowsi University of Mashhad Spectroscopy in Inorganic Chemistry Nuclear Magnetic Resonance Spectroscopy spin deuterium 2 helium 3 The neutron has 2 quarks with a -e/3 charge and one quark with a +2e/3 charge resulting in a total

More information

Basic Laboratory. Materials Science and Engineering. Atomic Force Microscopy (AFM)

Basic Laboratory. Materials Science and Engineering. Atomic Force Microscopy (AFM) Basic Laboratory Materials Science and Engineering Atomic Force Microscopy (AFM) M108 Stand: 20.10.2015 Aim: Presentation of an application of the AFM for studying surface morphology. Inhalt 1.Introduction...

More information

MOISTURE TRANSPORT AND DEHYDRATION IN HEATED GYPSUM, AN NMR STUDY

MOISTURE TRANSPORT AND DEHYDRATION IN HEATED GYPSUM, AN NMR STUDY MOISTURE TRANSPORT AND DEHYDRATION IN HEATED GYPSUM, AN NMR STUDY G.H.A. van der Heijden (1), L. Pel (1) and K. Kopinga (1) (1) Transport in Porous materials, Applied Physics, Eindhoven University of Technology,

More information

Chemistry. Faculty. Major Requirements for the Major in Chemistry

Chemistry. Faculty. Major Requirements for the Major in Chemistry Chemistry 1 Chemistry Website: chemistry.sewanee.edu Chemistry is often referred to as the central science. As such, it interfaces with and illuminates numerous disciplines including physics, biology,

More information

Slow symmetric exchange

Slow symmetric exchange Slow symmetric exchange ϕ A k k B t A B There are three things you should notice compared with the Figure on the previous slide: 1) The lines are broader, 2) the intensities are reduced and 3) the peaks

More information

InterdepartmentalCenter for Materials Science and Engineering. University of Pisa

InterdepartmentalCenter for Materials Science and Engineering. University of Pisa InterdepartmentalCenter for Materials Science and Engineering University Some history. On 1989, in the framework of the Engineering Faculty, the Center for Material Engineering (CIIM) was founded, regrouping

More information

MATERIALS CHARACTERIZATION AND TESTING PLATFORM

MATERIALS CHARACTERIZATION AND TESTING PLATFORM service offer MATERIALS CHARACTERIZATION AND TESTING PLATFORM Materials Materials Characterization and Testing Platform LIST's Materials Characterization and Testing Platform supports all Luxembourg and

More information

Catalysis a Key to Sustainability Matthias Beller

Catalysis a Key to Sustainability Matthias Beller Catalysis a Key to Sustainability Matthias Beller Catalysis is the science of accelerating chemical transformations. In general, readily available starting materials are converted to form more complex

More information

Clark Atlanta University Center for Surface Chemistry and Catalysis Instrument Capabilities

Clark Atlanta University Center for Surface Chemistry and Catalysis Instrument Capabilities Center for Surface Chemistry and Catalysis Instrument Capabilities For information contact: Dr. Eric Mintz Research Center for Science and Technology Clark Atlanta University Atlanta, Georgia 30314 Phone:

More information

Master Projects in Materials Physics, 2014 / 2015

Master Projects in Materials Physics, 2014 / 2015 Master Projects in Materials Physics, 2014 / 2015 X-ray based characterization of functional materials Are you interested in experimental physics and/or advanced data analysis? - Then we have the right

More information

Basic One- and Two-Dimensional NMR Spectroscopy

Basic One- and Two-Dimensional NMR Spectroscopy Horst Friebolin Basic One- and Two-Dimensional NMR Spectroscopy Third Revised Edition Translated by Jack K. Becconsall WILEY-VCH Weinheim New York Chichester Brisbane Singapore Toronto Contents XV 1 The

More information

240EQ016 - Polymers and Biopolymers

240EQ016 - Polymers and Biopolymers Coordinating unit: Teaching unit: Academic year: Degree: ECTS credits: 2018 295 - EEBE - Barcelona East School of Engineering 713 - EQ - Department of Chemical Engineering MASTER'S DEGREE IN CHEMICAL ENGINEERING

More information

DOE SBIR & STTR FY 2019 Phase 1, Release 1 Topics

DOE SBIR & STTR FY 2019 Phase 1, Release 1 Topics Source: InternetCoast BUSINESS OPPORTUNITIES web page>>> Letter of Intent Deadline: September 4, 2018 Application Deadline: October 15, 2018 Download Solicitation Topic Details>>> 1. TECHNOLOGIES FOR MANAGING

More information