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Canadian NMR News (updated regularly) >>>
What's
new at the NMR Facility
86)
Aaron J. Lussier, Yassir Abdu, Frank C. Hawthorne, Vladimir K. Michaelis,
Pedro M. Aguiar and Scott Kroeker, "Oscillatory zoned liddicoatite
from Anjanabonoina, central Madagascar. I. Crystal chemistry and structure
by SREF and 11B and 27Al MAS NMR spectroscopy," Canadian Mineralogist
(2010) in press.
85) Cory M. Widdifield and David L. Bryce, "Solid-State 127I NMR
and GIPAW DFT Study of Metal Iodides and their Hydrates: Structure, Symmetry,
and Higher-Order Quadrupole-Induced Effects," Journal of Physical
Chemistry A (2010) in press.
84) Luke A. O’Dell and Igor Moudrakovski, "Testing the Sensitivity
Limits of 33S NMR: An Ultra-wideline Study of Elemental Sulfur," Journal
of Magnetic Resonance (2010) accepted.
Other research publications enabled by the NMR Facility (complete list)
83)
Luke A. O’Dell and Christopher I. Ratcliffe, "Ultra-wideline
14N NMR spectroscopy as a probe of molecular dynamics," Chemical Communications
46 (2010) online. http://dx.doi.org/10.1039/c0cc01902j
82) Qin Li and Venkataraman Thangadurai, "A comparative 2 and
4-probe DC and 2-probe AC electrical conductivity of novel co-doped Ce(0.9-x)RExMo0.1O(2.1–0.5x)
(RE=Y, Sm, Gd; x = 0.2, 0.3)," Journal of Materials Chemistry (2010)
online. http://dx.doi.org/10.1039/c0jm01324b
Other research publications enabled by the NMR Facility (complete list)
Dear NMR Facility Users:
we are preparing our 2009-2010 Annual Report and we would like to receive the following information from you by the August 15th deadline:
1) a brief progress report for each of your research projects. Please prepare a separate report for each project, regardless of whether the project has ended or not. Each report should illustrate for non-NMR specialists major project findings and should normally not exceed one-two pages (text and figures) (preferably MS Word format, or an ASCII text + figures separately). Selected progress reports will be included in the printed version of the Annual Report (previous reports)
2) all 2009-2010 research publications featuring results from the 900 instrument (published, accepted, submitted)
3) invited lectures and oral presentations in 2009-2010
4) poster presentations in 2009-2010
5) 2009-2010 : Honor thesis, Ph.D. thesis and similar works by your students using the 900 results (please indicate name of the student, department, title of thesis, date of the defense)
6) any other relevant information you may consider useful including in our report
Let me know if any questions, and thank you for your contribution!
On behalf of the Facility Steering Committee,
Victor Terskikh (E-mail)
Opportunities for studying polymorphs and cement-based materials via Ca-43 solid-state NMR
June 11, 2010, University of Ottawa
Calcium is an important component in diverse materials and biochemicals. However, NMR spectroscopy of the only spin-active calcium isotope, Ca-43, is notoriously challenging due to its low natural abundance (0.14 %), low resonance frequency, and quadrupolar nature. Recently, researchers from the University of Ottawa, the NRC Steacie Institute for Molecular Sciences (SIMS-NRC), and Dalhousie University have independently reported advances in studies of inorganic polymorphs and cement-based materials using Ca-43 solid-state NMR spectroscopy.
"In spite of the great complexity of the calcium silicate chemistry involved in the hydration of Portland cement, we have shown that Ca-43 solid-state NMR provides useful new insights into cement chemistry", says Igor Moudrakovski (SIMS-NRC) of his collaboration with the Institute for Research in Construction (SIMS-IRC). Josef Zwanziger (Dalhousie) and his academic and industrial partners have similarly applied Ca-43 NMR in their project on the development, optimization and commercialization of high performance cement based composite materials.
Zwanziger explains, "we are trying to understand the nature of the composite-cement interface, and the mechanisms of toughening and strengthening in concrete composites. Calcium NMR is one of the many tools which is shedding light on the nature of the interface." At the University of Ottawa, David Bryce and his research group have demonstrated the utility of calcium NMR in understanding polymorphism in solids. This work has implications for understanding biomaterials as well as inorganic materials.
Because Ca-43 NMR in solid state requires a very strong magnetic field for sensitivity reasons, all these experiments were carried out at the National Ultrahigh-Field NMR Facility for Solids, a national user facility managed by the University of Ottawa and housed on NRC's Ottawa campus, which houses Canada's only 21.1 T (900 MHz) NMR spectrometer.
The latest calcium NMR research has been published in PCCP and J. Am. Chem. Soc., and a perspective on the state of the field is now available in Dalton Transactions (Bryce, 2010).
David L. Bryce "Calcium Binding Environments Probed by 43Ca NMR Spectroscopy," Dalton Transactions (2010) online. http://dx.doi.org/10.1039/c0dt00416b
Igor
Moudrakovski, Rouhollah Alizadeh, James J. Beaudoin, "Natural abundance
high field 43Ca solid state NMR in cement science," Physical Chemistry
Chemical Physics 12 (2010) 6961-6969. http://dx.doi.org/10.1039/c000353k
David L. Bryce, Elijah B. Bultz, and Dominic Aebi, "Calcium-43 Chemical Shift Tensors as Probes of Calcium Binding Environments. Insight into the Structure of the Vaterite CaCO3 Polymorph by 43Ca Solid-State NMR Spectroscopy," Journal of the American Chemical Society 130 (2008) 9282–9292. http://dx.doi.org/10.1021/ja8017253
80)
Jianfeng Zhu, Eric Ye, Victor Terskikh, and Gang Wu, "Solid-State
17O NMR Spectroscopy of Large Protein-Ligand Complexes," Angewandte
Chemie (2010) accepted.
79) David L. Bryce "Calcium Binding Environments Probed by 43Ca
NMR Spectroscopy," Dalton Transactions (2010) online. http://dx.doi.org/10.1039/c0dt00416b
78) Darren H. Brouwer, Igor L. Moudrakovski, Richard J. Darton, Russell
E. Morris, "Comparing quantum chemical calculation methods for structural
investigation of zeolite crystal structures by solid-state NMR spectroscopy",
Magnetic Resonance in Chemistry (2010) accepted.
Other research publications enabled by the NMR Facility (complete list)
The
National Ultrahigh-Field NMR Facility for Solids wishes to extend its sincere
thanks to Yining Huang (Western), the outgoing member of the Facility
Steering Committee who served in 2006-2010. Yining has done a great job as
the representative for Ontario Universities. His valuable insights and suggestions
have certainly helped to improve the Facility and broaden its userbase.
The Facility is pleased to announce that Gang Wu (Queen's) has been
appointed to serve on the Facility Steering Committee as the representative
for Ontario Universities for the next three years. Gang Wu is a long-time
facility user and his first-hand experience will be very useful in managing
the Facility. Welcome aboard, Gang!
To contact members of the Facility Steering Committee
the Facility International Advisory Board meeting took place on May 30, 2010 during CSC 2010 in Toronto.
Les Chercheurs
Dans
le cadre de notre série sur les Chercheurs, nous recevons cette
semaine David Bryce, professeur agrégé au Département
de chimie et chercheur au Centre de recherche et d'innovation en catalyse
de l'Université d'Ottawa (Radio-Canada).
the Facility Steering Committee meeting took place at the NMR Facility on May 20, 2010.
72)
Igor Moudrakovski, Rouhollah Alizadeh, James J. Beaudoin,
"Natural abundance high field 43Ca solid state NMR
in cement science," Physical Chemistry Chemical
Physics 12 (2010) online. http://dx.doi.org/10.1039/c000353k
Other
research publications enabled by the NMR Facility (complete
list)
Solid-State
NMR Workshop at CSC 2010 (May
1/10)
The
National Ultrahigh-Field NMR Facility for Solids and Bruker
Canada are pleased to present the 5th Annual Solid-State
NMR Workshop at the 93rd Canadian Chemistry Conference and
Exhibition in Toronto (CSC
2010). The workshop will take place on Saturday afternoon,
May 29, 2010 in the Metro Toronto Convention Centre
MTCC.
This annual Canadian solid-state NMR event focuses on the
latest developments in solid-state NMR spectroscopy with
emphasis on practical aspects and applications in materials
and life sciences. The workshop will be of interest not
only to NMR spectroscopists, but also to students and other
researchers interested in using modern NMR techniques in
their research practice.
Download
the Workshop Program and Abstracts (PDF)
Workshop program
Session
1 (MTCC, room 203B)
Chair John Ripmeester (NRC Canada)
13:00-13:30
Scott Kroeker (University of Manitoba) "Further
Adventures with 73Ge NMR of Solids: Halides and Oxides"
13:30-14:00 Andre Sutrisno (University of
Western Ontario) "Natural Abundance Solid-State 73Ge
and 67Zn Wideline NMR Studies at Ultrahigh Magnetic Field"
14:00-14:30 Leigh Spencer (McMaster University)
"Materials for Lithium Ion Batteries: A Solid-State
NMR Analysis"
14:30-15:00 Fabien Aussenac (Bruker France) "Solid-State NMR Dynamic Nuclear Polarization at 263 GHz"
15:00-15:15
Coffee Break
Session 2 (MTCC, room 203B)
Chair Roderick Wasylishen (University of Alberta)
15:15-15:45 Alex Bain (McMaster University) "Probing Spectra of Big Quadrupoles"
15:45-16:15 Cory Widdifield (University of Ottawa) "Solid-State 127I NMR Spectroscopy and GIPAW DFT Calculations of Inorganic Iodide Systems: Structure, Symmetry, and 'Beyond Second-Order" Quadrupole-Induced Shifts"
16:15-16:45
Peter Pallister (Carleton University) "33S Ultrahigh-Field
Solid-State NMR and First Principles Calculations in Various
Sulfate Systems"
16:45-17:15 Faciliy Users Meeting David
Bryce & Victor Terskikh "National Facility
user survey results and overview of application procedures"
17:15
Reception sponsored by Bruker
Canada
Natural Sciences and Engineering Research Council of Canada
(NSERC) has announced results of the 2010 NSERC competition
in the Discovery Grants Program (DG), Research Tools
and Instruments Grants (RTI) and Scholarship programs.
The National Ultrahigh-Field
NMR Facility for Solids has received NSERC RTI funding
for a cryogen-free cooler for the 900 MHz NMR spectrometer.
Once installed, the sample cooler will provides powerful,
stable and reliable cryogen-free cooling down to -80oC to
samples in existing MAS and static NMR probes. This successful
application to NSERC was a collaborative effort of three
of the Facility users, David Bryce (University of
Ottawa), Roderick Wasylishen (University of Alberta),
and John Ripmeester (Carleton University).
Share your success with the Canadian NMR community (E-mail).
the Facility Steering Committee meeting took place at the NMR Facility today, March 10, 2010.
Our
first NMR probe capable of triple resonance experiments,
4mm HCN CP/MAS Bruker, was delivered in 2008. While work
at the Facility is underway to develop a broadband HXY probe,
the existing probe has been modified to allow our users
to perform a broader range of triple resonance experiments.
Most recently this probe was successfully tested in the
H/B/N modification, with performance on 11B channel meeting
our expectations. It is now possible to adjust the high
frequency (X) channel to any desirable frequency between
13C and 11B, which covers such important nuclei as 27Al,
23Na, 79/81Br, and 129Xe. We are investigating if similar
modifications can be done for the low frequency channel.
This exciting for many our users development was made possible
due to efforts of our NMR probe technician, Paul Morris.
Thank you, Paul !
For more information on available NMR probes follow
this link.
The National Ultrahigh-Field NMR Facility for Solids is conducting the Facility user survey. Please contact Victor Terskikh if you would like to participate.
The
Avance II 900 NMR spectrometer has been in service for over four
years already, acquiring spectra 24/7 with virtually no downtime.
To ensure the best system performance and improved reliability for
many years to come the Facility Steering Committee has approved
a series of upgrades which are currently being implemented.
Last
week the software was upgraded from TopSpin 1 to TopSpin 2, which
also involved the complete workstation replacement. All user accounts
and data have been successfully transferred over. The
satellite data backup and archival server is in the process of replacement.
As part of this upgrade and also as preventative maintenance some
hardware components in the spectrometer have been replaced with
newer and more advanced versions.
Our NMR Facility strives to be at the forefront of solid-state NMR
research providing the Canadian NMR community with the state-of-the-art
instrumentation. Thank you for supporting our efforts!
 |
Crystalline beta-Barium Borate is an important nonlinear optical material often used in frequency mixing. Interestingly enough, even though beta-Barium Borate has been known for years, there still exists a controversy about its true crystallographic space group. That is existed until now! In this cover article in the Journal of Physical Chemistry C a research team from the University of Western Ontario has solved this problem using ultrahigh-field solid-state NMR spectroscopy and quantum chemical calculations. |
Andre
Sutrisno, Cheng Lu, Robert Lipson, Yining Huang, "Combined
135/137Ba Solid-state NMR at an Ultrahigh Magnetic Field and Computational
Study of beta-Barium Borate," Journal
of Physical Chemistry C 113 (2009) 21196–21201.
(Cover Article) http://dx.doi.org/10.1021/jp9044786
This is a seventh cover article featuring results obtained
using resources of the National Ultrahigh-Field NMR Facility for
Solids. See our cover gallery and the complete list of research
publications enabled by the Facility here (complete
list).
Our
congratulations to recent travel grant recipients !
Margaret Hanson (University of Western Ontario)
Vladimir Michaelis (University of Manitoba)
Brandon Greer (University of Manitoba)
Andre Sutrisno (University of Western Ontario)
Travel
support program for students and young scientists
Students and young scientists from Canadian Universities are welcome
to apply for a travel stipend towards full or partial reimbursement
of their travel expenses incurred while visiting the 900 NMR Facility.
All requests should be submitted by a supervisor in advance of the
trip and include a cost estimate. Requests should be forwarded to
the Facility manager for review and
approval by the Steering Committee.
Magic
angle adjustment in MAS probes is commonly performed by observing ST spinning
sidebands in 79Br MAS NMR spectra of KBr at low spinning speeds. The magic
angle is set correctly when the sidebands have the highest intensity.
A Hall effect magnetic flux sensor can be used for the same purpose [1],
for example in low-gamma MAS probes incapable of 79Br NMR. We have recently
tested this approach at the 900 NMR Facility: The figure shows the normalized
intensity of the 79Br ST spinning sidebands in KBr versus the Hall voltage
measured. This Hall sensor will be used for magic angle setup in a 2.5
mm boron-free MAS probe which is currently under construction.
For
more information see
[1] S. Mamone, A. Dorsch, O.G. Johannessen, M.V. Naik, P.K. Madhu, M.H. Levitt, "A Hall effect angle detector for solid-state NMR," Journal of Magetic Resonace 190 (2008) 135-141. http://dx.doi.org/10.1016/j.jmr.2007.07.012
the Facility Steering Committee meeting took place at the NMR Facility on November 5th, 2009.
 |
2008-2009
Annual Report (Oct 29/09) |
 |
This high-profile special issue of PCCP guest-edited by Paul Hodgkinson (Durham, UK) and Stephen Wimperis (Glasgow, UK) will be presented to the participants of the upcoming 6th Alpine Conference on Solid-State NMR in September 2009 (conference web-site). Among many excellent reviews and research papers highlighting recent trends and progress in the field of solid-state NMR spectroscopy there are three 900 papers, including the front cover article by Gang Wu's group from Queen's. Physical Chemistry Chemical Physics, volume 11, issue 32, 2009 |
Jianfeng
Zhu, Amanda J. Geris and Gang Wu, "Solid-state 17O NMR as a sensitive
probe of keto and gem-diol forms of alpha-keto acid derivatives," Physical
Chemistry Chemical Physics 11 (2009) 6972-6980.
(Cover Article, Themed
Issue) http://dx.doi.org/10.1039/b906438a
Rebecca P. Chapman and David L. Bryce, "Application of Multinuclear Magnetic Resonance and Gauge-Including Projector-Augmented Wave Calculations to the Study of Solid Group 13 Chlorides," Physical Chemistry Chemical Physics 11 (2009) 6987-6998. (Invited Article, Themed Issue) http://dx.doi.org/10.1039/b906627f
Luke
A. O'Dell and Robert W. Schurko,
"Static solid-state 14N NMR and computational studies of nitrogen
EFG tensors in some crystalline amino acids," Physical Chemistry
Chemical Physics 11 (2009) 7069-7077. (Invited Article, Themed
Issue) http://dx.doi.org/10.1039/b906114b
 |
Quadrupolar
halogens find widespread use i.e. in pharmaceutical formulations.
Solid-state NMR provides a direct mean to probe local halogen |
Rebecca
P. Chapman, Cory M. Widdifield and David
L. Bryce,
"Solid-State NMR of Quadrupolar Halogen Nuclei," Progress
in Nuclear Magnetic Resonance Spectroscopy 55 (2009) 215–237.
(Invited Review) http://dx.doi.org/10.1016/j.pnmrs.2009.05.001
See other publications enabled by the 900 NMR Facility here
 |
Unique instrumentation available at the 900 NMR Facility allows our users to deal with systems and nuclei inaccessible before with NMR at lower fields. One example is 73Ge NMR in solids which was previously limited only to highly symmetric environments. In this cover article just published by Chemical Communications a research team from the University of Manitoba and NRC-SIMS is reporting natural abundance 73Ge NMR spectra in much more challenging amorphous and crystalline germanium oxides. Work continues on even more complex glasses and crystalline phases to address long-standing fundamental questions in glass science, such as the ‘‘germanate anomaly’’. |
Vladimir K. Michaelis, Pedro M. Aguiar, Victor V. Terskikh and Scott Kroeker, "Germanium-73 NMR of Amorphous and Crystalline GeO2," Chemical Communications (2009) 4660-4662. (Cover Article) http://dx.doi.org/10.1039/b906642j
See other publications by users of the 900 NMR Facility here
Dear NMR Facility Users:
we are preparing our 2008-2009 Annual Report, and we would like to receive the following information from you by the end of August:
1) a brief progress report for each of your research projects. Please prepare a separate report for each project, regardless of whether the project has ended or not. Each report should illustrate for non-NMR specialists major project findings and should normally not exceed one-two pages (text and figures) (preferably MS Word format, or an ASCII text + figures separately). Selected progress reports will be included in the printed version of the Annual Report (previous reports)
2) all 2008-2009 research publications featuring results from the 900 instrument (published, accepted, submitted)
3) invited lectures and oral presentations in 2008-2009
4) poster presentations in 2008-2009
5) 2008-2009 : Honor thesis, Ph.D. thesis and similar works by your students using the 900 results (please indicate name of the student, department, title of thesis, date of the defense)
6) any other relevant information you may consider useful including in our report
Let me know if any questions, and thank you for your contribution!
On behalf of the Facility Steering Committee,
Victor
Terskikh (E-mail)
The
annual meeting of the Facility International Advisory Board took place in
Ottawa on May 11, 2009.
the 900 team (left to right): Victor Terskikh (NMR Facility), John Ripmeester (NRC-SIMS), Marek Pruski (Ames Laboratory, Iowa State University), Timothy Cross (National High Magnetic Field Laboratory, Tallahassee), Michèle Auger (Université Laval), Arno Kentgens (Radboud University, Nijmegen), David Bryce (University of Ottawa), Roderick Wasylishen (University of Alberta), Yining Huang (University of Western Ontario). Not pictured: Jamie Bennett (NRC-SIMS), Eric Ye (NMR Facility), Paul Morris (NMR Facility).
A
WURST-QCPMG NMR technique has recently been introduced by Luke O'Dell and
Rob Schurko (Windsor)
to achieve uniform excitation of quadrupolar nuclei across very wide bandwidth.
Using this approach wideline spectra of stationary samples can now be acquired
with no need or just minimal transmitter frequency adjustment. The spectrum
shown was acquired in about 1 hour by co-adding 10 individual pieces. Experiments
were performed by Luke O'Dell, who also kindly provided the WURST-QCPMG pulse
sequence for the 900 MHz NMR instrument. This pulse program is now available
to our users. For more information about WURST-QCPMG:
L.A. O'Dell and R.W. Schurko, "QCPMG Using Adiabatic Pulses for Faster Acquisition of Ultra-Wideline NMR Spectra," Chem. Phys. Lett. 464 (2008) 97-102. http://dx.doi.org/10.1016/j.cplett.2008.08.095
Another
milestone has been reached with the publication of the 50th peer-reviewed paper
featuring results obtained on the Facility's 900 MHz NMR instrument. The paper
just accepted by the Journal of Physical Chemistry deals with 47/49-Ti
NMR in layered titanium phosphates. Titanium NMR is notoriously difficult in
solid state, yet using the Facility's unique resources this challenging task
has been successfully tackled by a team of researchers from the University of
Western Ontario and the University of Ottawa.
Jianfeng Zhu, Nick Trefiak, Tom Woo, Yining Huang, "A 47/49Ti Solid-State NMR Study of Layered Titanium Phosphates at Ultrahigh Magnetic Field," Journal of Physical Chemistry C 113 (2009) 10029–10037. http://dx.doi.org/10.1021/jp901235w
Kudos to them and to all our users who continue to impress the international NMR community with the high level of solid-state NMR research in Canada.
See other research publications enabled by the Facility here.
The
National Ultrahigh-Field NMR Facility for Solids is very pleased to announce
that our application to NSERC for continued Major Resources Support (MRS)
funding has been successful. Funding has been approved at a level of $88,600
per year for each of the next five years. This award is critical to the ongoing
operations of the facility. The funding also means that the Facility will
be able to continue to provide travel grants for users, increase outreach
activities, hold annual workshops, and sponsor regional NMR meetings. I would
like to thank Victor Terskikh for his outstanding contributions to the operation
of the Facility and also to the preparation of the grant proposal. Thanks
also to all co-applicants on the proposal: John Ripmeester, Rod Wasylishen,
Christian Detellier, Michèle Auger, Yining Huang, Rob Schurko, Scott
Kroeker, Gillian Goward, Gang Wu, and Simon Sharpe.
David Bryce, chair of the Facility Steering Committee
The
National Ultrahigh-Field NMR Facility for Solids wishes to extend its sincere
thanks to the outgoing members of our International Advisory Board (IAB) serving
in 2005-2008. Over the past three years, Prof. Jean-Paul Amoureux (Lille,
France), Dr. Paul Ellis (PNNL, USA), and Prof. Mark Smith (Warwick,
UK) have provided the Steering Committee with invaluable input and advice
on facility operations and helped keep us abreast of new opportunities.
The Facility is proud to announce that Dr. Mona Nemer, the Vice-President
(Research) of the University of Ottawa, and Dr. Pierre Coulombe, the President
of the National Research Council Canada, have jointly appointed Prof. Timothy
Cross (Florida, USA), Prof. Arno Kentgens (Nijmegen, The Netherlands),
and Prof. Marek Pruski (Iowa, USA) to serve on the IAB for the next
three years.
Prof.
Cross is the NMR Spectroscopy and Imaging Program Director at the
National High Magnetic Field Laboratory in Tallahassee. Prof.
Kentgens is the Head of the Dutch National Solid-State NMR Facility
for Advanced Materials Science. Prof.
Pruski is a Senior Scientist in the Ames Laboratory at Iowa State
University. We look forward to the suggestions and recommendations of these
highly distinguished NMR experts to keep the Facility at the forefront of
solid-state NMR research.