NMR-3 User Guide

Department of Chemistry
Dalhousie University



Mike Lumsden
NMR-3 Facility Coordinator
Version 4.0 (September, 2011)

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1. Introduction
The Nuclear Magnetic Resonance Research Resource (NMR-3) is located on the ground (Room 127) and the
fourth floors (Rooms 426-431) of the Department of Chemistry, Dalhousie University. The facility is currently
home to five Bruker NMR spectrometers. Our flagship instrument is an AV-III 700 MHz system (installed 09,
jointly owned and operated with the Institute for Marine Biosciences) equipped with 5 mm and 1.7 mm TCI
cryoprobes. This state-of-the-art instrument provides researchers with access to 700 MHz NMR data at the
current maximum limits in both mass and bulk sensitivity. The facility also operates an AVANCE 700 MHz
spectrometer dedicated to the study of solids (installed 04, Room 127). This spectrometer represents, after the
900 MHz system at the NRC-Ottawa, the highest field NMR spectrometer dedicated to solid-state NMR
applications in Canada. The facility is also home to an AVANCE-500 (installed 03, Room 431, liquids only), a
DSX-400 (installed 04, Room 127, solids only), an AVANCE-300 (purchased used, installed 10, Room 431,
liquids only) and a Tecmag-upgraded AC-250 (originally installed 91, upgraded in 03, Room 426B, liquids
only). Further details regarding this equipment will be provided below. The facility operates with 2 Ph.D. level
staff members. Dr. Mike Lumsden (100% full-time, Room 428, (902) 494-1635) is the Facility Coordinator and
provides high-resolution NMR services and Dr. Ulrike Werner-Zwanziger (50% part-time, Room 127, (902) 494-
8085) is the solid-state NMR Coordinator and provides solid-state NMR services. The Facility Director currently
is Professor Jan Rainey. NMR-3 not only supports the NMR needs of scientists at Dalhousie University but also
at other universities as well as at chemical and pharmaceutical companies throughout the area.
In any given year, the facility provides walk-up NMR access for up to 100 undergraduate students,
graduate students, post-docs, and faculty. With such a large and diverse user base, a set of policies and
procedures has been adopted to ensure everyone has equal and fair access to the resources of the facility as
well as to ensure the safety of its users. In order to become a trained user of NMR-3, you will have to read and
understand the contents of this document in its entirety. Please be aware that one component of your NMR
training will require you to write a short quiz on the contents of this manual. You are also encouraged to provide
feedback regarding any of the policies and procedures. Feedback forms are available directly within the facility
or can be downloaded from the NMR-3 website (http://nmr3.chemistry.dal.ca).

2. Facility Access

2.1 Liquid-State NMR: Hands-on access to liquid-state NMR studies is currently available on the AVANCE
500, the AVANCE-300 and the Tecmag-AC 250 spectrometers. Training and scheduling is coordinated by Dr.
Lumsden. The list of courses, at the time of this writing, includes courses for using the AC-250, the AV-300, and
for automation on the AV-500. In addition, more specialized training is available that includes using reactive
sample slots on the AV-500 as well as variable temperature NMR experiments on all 3 spectrometers. Note that
in addition, a classroom tutorial on processing NMR data using Brukers TopSpin software is offered (when
there is sufficient demand). Spectrometer access can only be obtained after youve registered for and
successfully completed the appropriate training course. By default, training is provided each January, May, and
September, with the arrival of large numbers of new researchers, as well as other times throughout the year
when demand warrants. The training form is online at http://nmr3.chemistry.dal.ca/training/armrc_training.htm.
The form is to be completed, signed by your research supervisor, and submitted to Dr. Lumsden. You may only
register for training once you actually have a need for NMR results in your research program. All too often in the
past, people have completed the training but not needed NMR spectra for months down the road. By that time,
you will have forgotten most things you learned and will need re-training. Such a scenario is an inefficient use of
your time as well as the staff of NMR-3.
Upon completion of your training course(s), researchers have access to the facility resources 24 hours a
day, 7 days a week. The 2 rooms housing the 3 liquid-state NMR spectrometers are protected with numeric
keypad locks (access code is provided during training). Researchers within Dal Chemistry will already have the
necessary building access. For those working outside of Dal Chemistry, building access can be coordinated
through the Chemistry administration office (with a supporting note from your research Supervisor that the
access is needed).
The AV-500 spectrometer is the only instrument with automation hardware and walk-up access (no
reservation is required, unless you are making use of a reactive sample slot). The other spectrometers must be
reserved before using them. Reservations are made using the web-based booking software called FACES
(http://faces.ccrc.uga.edu). Once trained on a spectrometer, Dr. Lumsden will create a FACES account in your
name, after which you will receive an email containing the details of your account, including a temporary
password, which you are advised to change during your preliminary login. Finally, once you complete your
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training course, your email address will also be added to an email distribution list. Much of the communication
between NMR-3 staff members and the users is done via email.
Access to the AV-III 700 MHz instrument is currently available but specialized and must be coordinated
through Dr. Lumsden. This instrument is located at the Institute for Marine Biosciences (IMB) and consequently
additional security measures are in place. Experiments performed on this instrument tend to be more complex
and are typically performed on very dilute samples or macromolecular systems not easily studied at 500 MHz.

2.2 Solid-State NMR: Due to the complexity of solid-state NMR experiments, solid state NMR data are
typically obtained as service measurements. Hands-on access is only granted to experienced users after
substantial training one-on-one. If you need solid-state NMR data for your research, please contact Dr. Ulrike
Werner-Zwanziger ([email protected], (902) 494-8085) to be added to the solid-state NMR e-mail list and
to discuss further details.

3. The Spectrometers

3.1 AV-III 700 (Liquids): The Bruker AV-III 700 MHz spectrometer is a state-of-
the-art high-resolution spectrometer. It is a three-channel instrument with single-axis
Z-gradients and a standard-bore UltraShield Plus 16.44 Tesla magnet. The
spectrometer is controlled with a Linux workstation running TopSpin 2.1. For high-
throughput studies, the system has Brukers newest addition to their line of
automated sample changes, the SampleJet, which in turn is equipped with a sample
cooling feature for the temperature control of biological samples waiting for analysis.
The SampleJet has 47 positions for single tubes as well as 5 positions for 96 well
plate format tube racks, allowing for the handling of batches of up to 480 sample
tubes! NMR studies involving ultra-stable temperature control is provided with a
BCU-X refrigeration unit and a BVT-3000 temperature controller. The spectrometer
is equipped with 2 cryo-probeheads, both with the autotune & match feature (ATM).
A 5 mm version provides ultra-high bulk sensitivity for proton observation but also
extremely high sensitivity for
13
C studies. The 1.7 mm probehead provides state-of-
the-art sensitivity for mass limited samples.

3.2 AVANCE 500 (Liquids): The Bruker AVANCE 500 spectrometer is a
three-channel instrument with single-axis gradients and a narrow bore Bruker
Ultrashield 11.75 Tesla magnet. To minimize room and building vibrations, the magnet is supported by
integrated anti-vibration rubber pads. The spectrometer is controlled from a PC workstation running TopSpin v.
2.1. The system is protected with a 6-kVA uninterruptible power supply (UPS) and is fed 70 C dewpoint
compressed air from a desiccant air dryer. This ultra-dry air is routed through a Bruker BCU05 air-chiller to
produce -5 C air which is then re-warmed by the probes heater
before reaching the sample, greatly improving the temperature
stability during NMR experiments. The 500 has two 5mm
probes, both with a single axis Z-gradient coil. The TXI
probehead is an inverse probe with superior
1
H sensitivity,
lineshape, and water suppression capabilities. It is capable of
decoupling both
13
C and
15
N, making it a powerful tool for
structural elucidation of biological systems. The 5mm BBO
probehead is the workhorse probe with the inner coil tunable
from
109
Ag up to
31
P and a dedicated outer
1
H decoupler coil.
Despite this geometry, the probe still has excellent
1
H sensitivity
and, combined with the Z-gradient, performs amazingly well
with the inverse detected 2D experiments essential for modern
structural organic chemistry research. The BBO probe is also
equipped with Brukers ATMA feature (auto-tune and match accessory). The specs for these two probes are
summarized in Table I. For efficient sample throughput, the spectrometer is equipped with a sample changer
from Bruker called B-ACS (Bruker Automation Control System) which can accommodate a queue of 60
samples. In order to perform variable temperature NMR experiments, the spectrometer has a Bruker BVT-3200
temperature controller (essential for temperatures above and below ambient) along with a 25 L liquid nitrogen
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dewar and a nitrogen exchange coil which are used to generate cold nitrogen gas for NMR experiments below
ambient temperature. Training courses are available for hands-on access to the AVANCE 500.

3.3 AVANCE 300 (Liquids): The Bruker AVANCE 300
spectrometer is a two-channel instrument with single-axis
gradients and a narrow bore Bruker 7 Tesla magnet. To
minimize room and building vibrations, the magnet is supported
by a TMC vibration dampening platform. Like the AVANCE
500, the spectrometer is software controlled by Brukers
TopSpin 2.1. The spectrometer has a 5mm BBFO probe
equipped with the ATMA accessory and a Z-gradient coil. This
probe is used to observe nuclei ranging in frequency from
15
N
up to and including
19
F. The outer decoupler coil is dedicated
to
1
H. The specs for the 5mm BBFO probe are summarized in
Table I. Also of note is the inclusion of a Bruker BVT-3200
temperature controller which enables variable temperature
NMR experiments. Low temperature experiments also require a source of cold nitrogen gas, which can be
generated on the 300 using the liquid nitrogen evaporator and dewar supplied with the Tecmag/AC-250. A
training course is available for hands-on access to the AVANCE 300.

3.4 Tecmag/AC-250 (Liquids): The Bruker AC-250 narrow bore has served as our high resolution NMR
workhorse for the past 20 years and continues to provide great spectra. The instrument has two channels and
a single probe called a QNP probe with automatic tuning. It is configured to observe four nuclei,
1
H on the outer
decoupler coil and
13
C,
31
P, and
19
F on the inner coil. The system also has a Bruker BVT-1000 variable
temperature controller coupled with a nitrogen evaporator and a 25L liquid nitrogen dewar for variable
temperature NMR studies. The spectrometer was upgraded in 2003 with a DSPect data acquisition unit from
Tecmag Inc. to replace the ageing Bruker Aspect computer and software. The interface to the system is
Tecmags NTNMR software, run from a powerful Dell Windows XP-based PC. A training course is available for
hands-on access to this machine. QNP probe specs are summarized in Table I.


Table I: NMR-3 High Resolution Probe Specifications
Specification
250 QNP
(5 mm)
300 BBFO
(5 mm)
500 TXI
(5 mm)
500 BBO
(5 mm)
1
H S/N (2 ppm) 70 135 (2 ppm) 900 (200 Hz) 330 (2 ppm)
13
C S/N (ASTM) 70 100 N/A 220
31
P S/N (TPP) 60 100 N/A 120
15
N S/N (Formamide) N/A 15 N/A 32
19
F S/N (TFT)

70 180 N/A N/A
1
H Lineshape 7/15 0.6 / 6 / 12 0.45 / 5 / 10 N/A
1
H /2 pulse (s) <15 <15 <8 <15
13
C /2 pulse (s) <15 <10 <12 <10
31
P /2 pulse (s) <20 <12 N/A <15
15
N /2 pulse (s) N/A <15 <33 <15
19
F /2 pulse (s) <20 <15 N/A N/A

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3.5 AVANCE 700 (Solids): The Bruker AVANCE
700 MHz NMR Spectrometer was purchased by the
Institute for Research in Materials (IRM) and has been
incorporated into the NMR-3. Situated in room 127, this
spectrometer is dedicated to solid-state NMR
experiments. When fully equipped, the spectrometer
will work together with three NMR probeheads. Already
available is an H-F/X CP/MAS probe, suitable for the
study of protons, fluorine and other heteronuclei whose
Larmor frequencies lie between
13
C and
31
P. Samples
can be rotated around the Magic Angle up to 35 kHz in
rotors of 2.5mm diameter. Also available is a VTN
CP/MAS H/X probehead for X nuclei frequencies
between
15
N and
13
C with spinning speeds up to 15 kHz
in rotors of 4mm diameter. An additional triple
resonance probehead will be developed together with
Bruker engineers. The spectrometer operates under
XWINNMR from a Linux workstation. To acquire data on this spectrometer, please contact Dr. Ulrike Werner-
Zwanziger ([email protected], (902) 494-8085).

3.6 AVANCE DSX-400 (Solids): The Bruker AVANCE DSX-400 MHz spectrometer was originally
installed in 1997 at Indiana University. Professor Josef Zwanziger transferred the spectrometer with him from
Indiana and made it available for NMR-3 users. Reinstalled in 2004 in room 127, this spectrometer is also
exclusively dedicated to the NMR of solid samples. This spectrometer is equipped with 5 probeheads:
A triple resonance multinuclear VT CP/MAS probe with exchangeable inserts. Using rotors with
4mm diameter, this probe can spin up to 15 kHz.
A multinuclear VT MQ/MAS probe tuning from
69
Ga to
31
P, capable of proton and fluorine NMR
and optimized for minimum fluorine background. With 2.5 mm rotor diameters, the samples can
spin up to 35 kHz.
A multinuclear VT CP/MAS probe tuning the X nuclei frequency between those from
13
C to
31
P.
This double resonance probe features 4mm rotor sizes spinning up to 15 kHz. This is a real
workhorse for standard applications on this spectrometer. In addition to the usual MAS
housing, we can insert a boron depleted housing.
A VT CP/MAS probe tuning from
15
N to
31
P for the X-nuclei in conjunction with
1
H/
19
F cross-
polarization. Its 7mm rotor design gives more sample space for materials with less sensitivity
on the cost of spinning only up to 8 kHz.
A high power probe for wide line NMR applications including exchangeable rf coils and
matching inserts to allow the probe to tune from
109
Ag to
31
P. This probe is capable of extended
variable temperature applications up to 300
o
C
This spectrometer operates under XWINNMR from a SGI workstation. Low and high temperature operations are
available. Access to this spectrometer again is granted through Dr. Ulrike Werner-Zwanziger.

4. Data Processing and Analysis
Included with the purchase of the AV-III 700 spectrometer was a license for Brukers NMR software package
known as TopSpin, version 2.1. Our license supports 3 simultaneous running copies of the software and
enables users to bring their NMR data to their own labs or even home for work-up and analysis. It is important
to note that this software license is not limited to Dalhousie scientists but is available to all users. In addition to
these 3 licenses, the facility also has 6 licenses for TopSpin, version 1.3 (3 of these are shared with the older
xwin-nmr software program). The primary PC within the facility is running ftp server software, allowing users to
have around-the-clock remote ftp access to their NMR data acquired on any of the NMR spectrometers.
For those users who wish to do their processing within NMR-3, the facility possesses a number of PCs
for this purpose. Each has TopSpin 1.3 installed as well as the popular simulation software known as gNMR.
Also installed are several products from Advanced Chemistry Development, Inc., including their proton and
carbon prediction software and 1D/2D NMR processing software. Together, these software products provide
the facilitys users with powerful tools for analyzing and understanding their NMR research data. A networked
HP LaserJet 4050 is available for printing and plotting.
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Solid-state NMR spectrum simulation is possible by the program xedplot running on the SGI in room
C127. This program allows the fitting of spectra to determine isotropic and anisotropic chemical shift values as
well as quadrupole parameters for Magic Angle spinning and static applications.

5. Safety in the NMR Facility

5.1 Stray Magnetic Fields: Despite a very innocent appearance, superconducting magnets possess
dangerously strong attractive forces towards ferromagnetic materials/equipment. These forces are due to
stray magnetic fields which emanate in all directions from the magnet canister. If the force is large enough, the
equipment could move and become attached to the magnet. Small pieces of equipment like tools and metal
hardware can literally become projectiles and present a serious danger to all personnel within NMR-3, as well as
to the magnet. The strength of the force increases as the equipment moves closer to the magnet since the stray
fields increase in this direction. Also, the force increases as the mass of the equipment increases. Note that
moving ferromagnetic equipment/materials in the vicinity of the magnet affects the field homogeneity, adversely
affecting any NMR experiments in progress. Stray magnetic field strengths are quantified in units of Gauss. To
put this unit in perspective, the strength of the Earths magnetic field is, on average, ~ 0.5 Gauss whereas the
strength of a small fridge magnet is typically ~40 Gauss. Please refer to Table II for a description of the radial
(horizontal) fringe fields associated with the existing 5 superconducting magnets at NMR-3.


Table II: Radial Stray Field Characteristics
10 Gauss Line (m) 5 Gauss Line (m)
Tecmag-AC 250 1.19 1.58
AVANCE 300 1.46 1.87
AVANCE 500 Ultrashielded 1.15 1.35
DSX 400 1.25 1.60
AVANCE 700 2.25 2.50
AV-III 700 MHz @ IMB 0.88 1.00

For the benefit and safety of everyone who steps inside the doors of
NMR-3, the radial 5- and 10-Gauss lines are marked on the floor
around each magnet with yellow (5 Gauss) and red (10 Gauss) tape
and/or with plastic chain-link fencing. On the left is a picture of these
markings around the 250 magnet. It is extremely important that you
do not bring magnetic items inside the 10 Gauss line. Note that
magnetic media such as ATM/credit cards as well as some watches
and cameras can be damaged or erased inside the 5 Gauss line.
Finally, serious injury or death can occur to those people with
certain implanted or attached medical devices such as cardiac
pacemakers, surgical clips, or prostheses. These individuals
must stay outside the 5 Gauss marking!

5.2 Field Quenches: Although magnetic field quenches are
thankfully extremely rare, they can occur and so it is important for
facility occupants to be aware of the threat and to know how to
respond. A field quench can occur for a number of reasons, with the
end result that the cryogenic fluids inside the magnet (liquid nitrogen
and helium) are boiled off (sometimes violently) and the magnet is no
longer superconducting. To the right is a picture posted on the web of
a 700 magnet just after a quench occurred. The real danger
associated with this event is the displacement of oxygen in the
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magnet room and hence the threat of asphyxiation. If you are in any of the magnet rooms and a quench
were to occur (obvious from the noise of the expanding gas and the formation of a vapor cloud), your
instructions are very simple - get out! Once you reach safety, please phone an NMR-3 staff member and let
him/her know what has happened.

5.3 Other Safety Rules & Considerations: In addition to the above material dealing with the dangers
associated with stray magnet fields and quenches, please take note of and observe the following facility safety
rules:
No food or drink is permitted in the NMR facility, no exceptions!
Many of you will be dealing with toxic and dangerous compounds in your research. You are responsible for
understanding all of the dangers associated with your systems in case of a broken NMR tube and therefore
a toxic spill.
Nitrile/latex gloves as well as lab coats are not to be worn anywhere within the confines of the NMR facility.
Your NMR tubes should be properly cleaned in your own lab before bringing it to NMR-3 for analysis.
Eye protection is required the entire time you are in the NMR facility.
Access to the hands-on liquid-state spectrometers of NMR-3 is exclusively through the main door (marked
Rooms 426-431) off the 4
th
floor hallway, no exceptions. Appropriate warning signs about the perils of
strong magnetic fields are placed at this main entrance as well as in the individual spectrometer rooms.
Exercise caution when inserting your sample into a spinner. There have been cases over the years where
students have used a sample tube, which was too tight to fit the spinner properly. In such cases, it is very
easy to break an NMR tube and seriously cut your hand. The proper approach is to grip the tube as near to
the spinner as possible and use a twisting motion while inserting or removing the sample.

6. Facility Rules & Guidelines

6.1 Spectrometer Usage Rules: Every NMR-3 spectrometer has a unique set of guidelines governing
signup rules and usage. These guidelines change from time-to-time depending upon the time of year and the
needs of the individual research groups. Email notification is provided when the signup rules are modified. The
most up-to-date rules are always available on our website at http://nmr3.chemistry.dal.ca/faces_scheduling.htm.
In addition to the signup rules, spectrometer usage is governed by the following rules of conduct:
Only authorized (trained) researchers are permitted to use an NMR-3 NMR spectrometer.
Users are not permitted to use the AC-250 or AV-300 NMR spectrometers without first signing up for the time
in FACES. Using a spectrometer without a reservation is a serious problem as it interferes with the planning
of other potential users. Furthermore, it reduces usage statistics, which are an important component of
funding applications for NMR equipment and infrastructure.
Continuing to use a spectrometer beyond your reserved time because there is no booking following yours is
also strictly forbidden. All usage must have a corresponding FACES reservation, no exceptions.
Extending your available time beyond the allowed allotment by consecutively signing up in FACES in your
name and then somebody elses name, such as a lab colleague, is strictly forbidden.
Users are not permitted to use the spectrometers during liquid nitrogen or helium fills.
Users must never use or alter another users NMR data.
Users of the AV-500 and AV-300 spectrometers are permitted to use parameter sets starting with 1d_ or
2d_, only. No other parameter sets are available for routine users.
Do not browse the web or use email on any of the spectrometer workstations.
Ensure that the door to the spectrometer room closes behind you when you leave the NMR facility.
Get in the habit of backing up your NMR data frequently. The computers at NMR-3 are purged of user data
every 3 months.
Please report unusual spectrometer behavior to the facility coordinator as soon as you notice it.

6.2 Access Issues: Given the tremendous diversity in the access requirements of its large user base, it is
impossible that a single set of signup rules will be ideal for each user. Compromises are inevitable and access
to any given spectrometer may not be perfect for your research needs. If you need clarification on any of our
signup policies and the background rationale, feel free to speak to a staff member. However, if access
problems under the current guidelines are demonstrably hindering your research progress, it is important that
the coordinator of NMR-3 be made aware of this. Analogously, if you notice an infraction of the signup
guidelines, it is important that you inform the coordinator. The coordinator is solely responsible for the day-to-
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day operations of the facility, including scheduling of time on the spectrometers, and it is his/her responsibility to
address these concerns in a timely fashion. It is important to be aware that the director is not involved with
these everyday issues. If and only if, you are unable to resolve your problem/concern after discussions with
the coordinator are you invited to contact the NMR-3 Users Committee in writing, outlining in detail the nature of
your concern and your attempt(s) to resolve it. At the time of this writing, Professor Ian Pottie at Mount Saint
Vincent University is the chair of the NMR-3 Users Committee ([email protected]).

7. Rule Violations & Disciplinary Action
NMR-3 facility rules and guidelines are put in place and enforced to give all users equal access to the NMR
spectrometers and to help ensure the safety of the users and equipment within the facility. Therefore, it is
extremely important that these rules are strictly adhered to. To help enforce this, penalties are in place for rule
infractions. For a first-time offense, spectrometer access will be suspended for 1 week. For each additional
violation, you will be suspended for a total of TWO MONTHS. If it happens that the additional violation occurs
within the initial 1-week suspension period, the two month suspension will be imposed consecutively, not
concurrently.

8. Concerning High-Resolution NMR Samples
High resolution NMR spectroscopy of liquids demands the utmost attention to detail when it comes to preparing
samples. This is particularly true when it comes to
1
H spectroscopy, where linewidths can routinely get down to
a tenth of a Hertz in some solvents. To put this into perspective, 0.1 Hz for
1
H on the AVANCE 500 corresponds
to a magnet field deviation of less than 0.2 parts per billion over the volume of the sample! In order to realize
superior resolution such as this, you must observe the following:
Solution Homogeneity: Do not allow particles of solids to remain in your NMR tube under any
circumstances. If solubility proves to be a problem, filter your sample before putting it into the magnet. For
the same reasons, gas bubbles in the NMR sample also severely degrade resolution and should be
eliminated.
Sample Height: It is critical that the height of the column of liquid in your NMR tube measure at least two
times the height of the NMR receiver coil. If not, extensive shimming will be required. The precise height of
the relevant receiver coil depends upon the combination of probe and nucleus you are observing. To keep
this simple, a general rule of thumb for 5 mm NMR tubes is to use at least 700 l of liquid which
corresponds to a height of ~ 5 cm. Using more liquid than this is wasteful and will unnecessarily dilute your
sample and hence your sensitivity. Keep the height of the liquid column consistent from sample to sample
to minimize the time you spend shimming.
Tube Length: The shortest commercially available NMR tube in a 5 mm design is 7 and that is the
minimum acceptable height for use in NMR-3. If your tube breaks near the top, do not cut it off and
continue to use it this tube must be discarded. This rule is particularly important on the AV-500 in
automation as tubes shorter than 7 may not be retrieved properly by the robotic sample changer, posing a
serious risk for tube breakage.
Tube Quality: There is evidence available to suggest that poor quality &/or mistreated NMR tubes can lead
to damage of the delicate glassware inside the NMR probehead. Bruker has told me that one of our
probeheads for the AVANCE 500 has a tolerance of only 190 m between the NMR tube and the closest
glass component inside the probehead! To help protect the probes, NMR-3 has a tube rule in place for the
500 and 300 and is currently discussing a similar rule for the AC-250. For the 500 and 300, only Wilmad
tubes are permitted with the minimum tube quality set at the Wilmad model 506-PP. Please be aware that
this is not a 500 MHz quality NMR tube! 500 MHz quality NMR tubes from Wilmad cost on the order of $30
Canadian per tube and, in our opinion, are not necessary for everyday research use. What is necessary is
a tube of sufficient quality such that it poses no danger to the glassware inside the probehead and we
believe the 506-PP serves this purpose. These tubes can be purchased through Dal Chemistry Stores.
Flame-Sealed Tubes: Flame sealed NMR tubes are permitted in NMR-3 but these must not be spun,
including on the AC-250. Of particular concern is when researchers wish to study flame-sealed samples at
elevated temperatures. Please consult the NMR-3 Coordinator before performing any studies of this nature.
In general, this is normally permitted but you will first be asked to test the NMR sample of interest by letting
it sit in a water or oil bath at the highest temperature you wish to probe.
J-Young Tubes: All sealed tubes containing valves (i.e. J-Young tubes) are permitted but must not be spun
in any spectrometer. In addition, these tubes must be manually lowered and ejected from the magnet using
a piece of string. Please talk to the Facility Coordinator for further information.
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Tube Labels: NMR tubes are to be labeled either on the cap or along the side of the tube (just below the
cap) using a marker. Paper or other flag labels are not permitted in NMR-3.
Concerning Spinners: Always use the supplied depth gauge to position the sample in the spinner. Never
touch any NMR spinner with your bare hands! Make sure the sample tube is held tightly in the spinner. If
the tube is not held tight, it could move during insertion into the probe, causing problems with your NMR
experiment and risking damage to the probe. Tiny pieces of kimwipe wedged between the spinner wall and
the NMR tube wall for a tighter fit are not permitted under any circumstances!
Rinsing with Isopropanol: Every NMR sample, as a final step before placing it in the magnet, must be
rinsed with isopropanol and dried with a kimwipe.
Sample Spinning: In order to help minimize the chance of damage to the probehead glassware, the only
spectrometer where sample spinning is permitted is the Tecmag/AC-250 (provided the tube is not flame-
sealed or a J-Young tube).
Tube Care: Clean your tubes immediately after you are done analyzing your sample. Always perform a
final rinse with alcohol and allow to air dry. Using compressed air for quick drying and reuse of a tube is
fine. Do not place high quality NMR tubes in a hot oven under any circumstances! Note that brand new
NMR tubes straight out of the package should be cleaned before their first use.

9. Contact Information

NMR-3 Facility Contact Information

Professor Jan Rainey
Facility Director



Dept. Biochemistry, Room
10-N1
Tupper Medical Building
Dalhousie University
902-494-4632 (office)
902-4941355 (fax)
Jan. [email protected]
Dr. Mike Lumsden
Faciltiy Coordinator
(100% Full Time)


Dept. Chemistry, Room 428
Dalhousie University
902-494-1635 (office)
902-494-1310 (fax)
[email protected]
Dr. Ulli Werner-Zwanziger
Solid-State Coordinator
(50% Part Time)


Dept. Chemistry, Room 127
Dalhousie University
902-494-8085 (lab)
902-494-1310 (fax)
[email protected]
Professor Ian Pottie
Chair, Users Committee



Dept of Chemistry
Mount Saint Vincent University
902-457-6245 (office)
902-457-6656 (fax)
[email protected]

Mailing & Courier Address
Nuclear Magnetic Resonance Research Resource NMR
3

Department of Chemistry, Dalhousie University
6274 Coburg Road
P.O. Box 15000
Halifax, Nova Scotia, B3H 4R2

[email protected]
http://nmr3.chemistry.dal.ca