Bruker Fourier 300 Instruction Manual

Version
Innovation with Integrity
Fourier
001
NMR
Fourier 300
QuickStart Installation Guide

Copyright© by Bruker Corporation
All rights reserved. No part of this publication may be
reproduced, stored in a retrieval system, or transmitted, in
any form, or by any means without the prior consent of the
publisher. Product names used are trademarks or
registered trademarks of their respective holders.
This manual was written by
Diether Maier
© December 20, 2011: Bruker Corporation
Rheinstetten, Germany
P/N: Z33048
DWG-Nr.: Z4D11877
For further technical assistance on the Fourier unit,
please do not hesitate to contact your nearest BRUKER
dealer or contact us directly at:
BRUKER Corporation
am Silberstreifen
D-76287 Rheinstetten
Germany
Phone:+ 49 721 5161 0
FAX:+ 49 721 5171 01
E-mail:[e-mail]
Internet:www.bruker.com

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Table of Contents
Contents
1 Getting Started...............................................................................................5
1.1 This Manual.............................................................................................................. 5
1.2 Before You Begin ..................................................................................................... 5
1.3 Unpacking the Console ............................................................................................ 5
1.4 Console Connections ............................................................................................... 6
1.5 External Filters ......................................................................................................... 6
1.6 Adjusting the Air Pressure........................................................................................ 7
1.7 Switching On the Console the First Time ................................................................. 7
1.7.1 Verifying That the Console Has Booted ................................................................... 7
1.8 Copying the Probe Data to the PC System .............................................................. 8
1.9 Setting the Magnet to the Correct Field.................................................................... 9
1.10 Setting the Spin Safety Threshold............................................................................ 9
1.11 Initial Shimming ...................................................................................................... 11
1.12 Finding the Lock Field and Phase .......................................................................... 11
1.13 Manual Shimming to Lineshape ............................................................................. 12
1.14 Converting the Parameter Set to the Actual BF1 ................................................... 12
1.15 Creating a Shim Map for Gradshim........................................................................ 13
1.16 ATP Tests and Customer Acceptance ................................................................... 14
A Appendix ......................................................................................................17
A.1 Main Differences Between Fourier and AVANCE .................................................. 17
1.2 Figures ................................................................................................................... 19

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Table of Contents

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1 Getting Started
1.1 This Manual
This manual is intended to be a quick-start reference guide for Bruker service techni-
cians. It provides basic information for installing and setting up the Fourier 300 system.
Carefully read the information in this manual, as well as, the safety information
provided in the Service Manual before working on the device!
This manual provides only the basic information required for installation and set-up, for
complete information refer to the service manual.
1.2 Before You Begin
This guide assumes that the magnet has been evacuated, cooled down, and that all the
equipment for energizing that magnet is available on site.
Three test samples, two spinners and a sample gauge are shipped with the system.
• 3% CDCl3 in Chloroform (lineshape)
• 0.1% EB in CDCl3 (1H SINO)
• ASTM (C13 SINO)
To shim the magnet and perform the ATPs test you will need to bring some additional
samples:
• Urea in DMSO (Pulse Length adjustment)
• 100mg or 1g Cholac in CDCl3 (DEPT)
• Cyclosporine in C6D6 (2D Examples)
1.3 Unpacking the Console
Do not attempt to lift the Fourier console out of the carton, rather:
1. Slide the carton sleeve up and over the console.
2. Slide the console off the pallet.
The console has wheels and can be moved around freely using the handle on the back.
Retain the packaging in case the console has to be returned for repair/exchange.

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Getting Started
1.4 Console Connections
Figure 1.1 Console Connections
1.5 External Filters
Some earlier models come with three external filters:
• Z13383 is connected to the 1H connector on the rear of the console.
• Z14331 is connected to the C13 connector on the rear of the console.
• Z00116 is connected to the C13 connector of the probe.
Later models have just two external filters:
• E1451420 is connected to the 1H connector to the rear of the console.
• E1451430 is connected to the C13 connector to the rear of the console.

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Getting Started
1.6 Adjusting the Air Pressure
Adjust the air pressure so that the manometer in the console reads between 3.5 and 4
bar. This way the default spin and lift parameters will be sufficient to get you started.
1.7 Switching On the Console the First Time
The console has three modes:
• OFF (blue light OFF), the switch on the rear panel is set to OFF.
• STAND BY (blue light BLINKING), the switch on the rear panel set to OFF, the ON/
OFF button on the top of console is not yet pressed.
• ON (blue light ON).
It is IMPORTANT to switch the console on BEFORE switching on the PC, since the con-
sole contains the Ethernet hub, and the DHCP server will not start if a network is not
found.
1.7.1 Verifying That the Console Has Booted
This procedure takes 30-60 seconds, provided the DCHP server is already running.
There is no visual indication on the console indicating that the console has booted, but
the easiest way to check is to see if the three main Ethernet devices (main board, lock
and VTU) can be reached via ping or a Web browser. Their addresses will usually be in
the range:
149.236.99.25x
To access any of the Web server sites, the following password and user name are
required:
User: root
Password: BRUKER (in capitals!)
If you are not sure the DHCP Server is running, you can check by opening:
Control Panel -> Administrative Tools -> Services -> Bruker DCHP Server
Figure 1.2 Bruker DCHP Server

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Getting Started
If you are not sure what addresses have been assigned, you can check by opening the
following file:
Bruker\Diskless\dchpd.leases
lease 149.236.99.254 {
starts 4 2010/08/19 11:08:55;
ends 2 2038/01/19 03:14:06;
tstp 2 2038/01/19 03:14:06;
binding state active;
next binding state free;
hardware ethernet 00:00:ad:11:4f:12;
uid "\001\000\000\255\021O\022"; }
lease 149.236.99.253 {
starts 4 2010/08/19 11:08:58;
ends 2 2038/01/19 03:14:06;
tstp 2 2038/01/19 03:14:06;
binding state active;
next binding state free;
hardware ethernet 00:00:ad:13:34:12;
uid "\001\000\000\255\0234\022"; }
lease 149.236.99.252 {
starts 4 2010/08/19 11:09:01;
ends 2 2038/01/19 03:14:06;
tstp 2 2038/01/19 03:14:06;
binding state active;
next binding state free;
hardware ethernet 00:00:ad:12:85:12;
uid "\001\000\000\255\022\205\022";
Once you are sure that all three devices have booted, you can start TopSpin. Normally,
the PC will come with the hardware configuration (CF) having already been carried out.
If you receive an error message stating that one or more devices cannot be found, you
may have to repeat CF (refer to Chapter 9 of the NMR Experiments User Manual).
1.8 Copying the Probe Data to the PC System
Since the Fourier system always comes with the same type of probe, there is no PICS
interface on the Fourier console. Instead a CD-ROM with the probe data is delivered
with the system. Before running EDHEAD, copy the probe.ph file from the CD-ROM to
the directory:
“conf/instr/FOURIER300”

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Getting Started
1.9 Setting the Magnet to the Correct Field
The magnet is designed to be operated at 300.18 MHz, with the current in the H0 field
coil of the shim system set to zero. At this frequency the synthesizers are “cleanest” and
least likely to create spurious problems.
When the lock is powered up from a cold start, the field DAC is not automatically set.
In order to make sure the current in the field coil is set to zero:
1. Open the BSMS panel.
2. Set the field value to 2048.
3. Switch the lock to “ON” once, then switch it off again while the magnet is being
charged to the correct field and the cryo-shims are adjusted.
1.10 Setting the Spin Safety Threshold
The spin has a safety function that shuts the spin off as soon as the Lift is turned on,
either manually, or during the initialization of the sample changer. In order to do this, the
analog sensor that monitors the spinner has to be calibrated. The sensor has three volt-
ages for the three possible states:
No spinner (typically 0.1 to 0.6V)
Black (typically 0.6 to 1.5V)
White (typically 2.5 to 4.5 V)
Since the values vary between shim stacks, and also depend somewhat on the spinner
type, it is necessary to calibrate this value. Usually this only has to be done once at
installation.
1. Open the Web server of the VTU and go to -> peripheral control -> spin

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Getting Started
Figure 1.3 Setting the Spin Safety Threshold
2. Remove the sample, or activate the sample lift, and annotate the “empty” spin volt-
age.
3. Insert, or lower the sample, and switch on the spin (either from the BSMS panel or
from the Web server).
4. Repeatedly read the spin voltage and annotate the two values that can be read
while the sample is spinning.
5. Set the “sample down threshold voltage” to about halfway between the lower of the
two “black/white” spin voltages, and the “empty” spin voltage.
Everything is set correctly when the spin does not cut off during normal operation, but
cuts off immediately when the lift is activated.
Note: The “Spin DC Voltage Counter” sets the number of times the value has to be
below the threshold, before the safety shut off is activated. It should be set to 10 to avoid
the spin cutting off with just a single bad reading.

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Getting Started
1.11 Initial Shimming
First level shimming is done in the usual way by first setting the currents given in the
magnet manual and then seeing if the base shim can be improved in the GS mode.
Once the cryo-shims are set, continue adjusting the lower orders of the BOSS1 shim
system in the GS mode until your FID half height has reached approximately 100 ms.
1.12 Finding the Lock Field and Phase
Once your shim has reached a certain level, your lock should begin to show a signal.
1. Enable the Lock sweep mode in the BSMS panel.
2. Adjust the field and phase such that the “wiggles” are centred around zero and the
first wiggle is positive in both directions.
Due to sidebands, there will be more than one lock field value that gives a lock signal.
You can check which is the correct one by making a measurement, and checking that
the spectrum has the correct ppm scale (e.g 4.7 ppm for water, 7.2 ppm for a C6D6 sol-
vent peak).
Alternatively, you can use the Fourier AU program “flock”, which queries for the lock sol-
vent, creates a temporary 2H data set and starts an acquisition to find the lock signal in
the 2H spectrum. Flock compares the ppm shift of the 2H signal to the default value from
the edlock table. The difference in ppm is then converted to a shift in the lock field. The
new lock field is displayed in a pop-up window. Additionally, flock informs the operator
how many solvent peaks have been found and if this number is in agreement with the
number of resonance lines for the selected lock solvent. When the number of signals is
different from the expected value, flock uses the peak with the highest intensity to calcu-
late the lock shift. The new shift value is set in the Fourier and a normal lock procedure is
started.
Figure 1.4 Results of the AU Program FLOCK
The flock command also works with solvents with more than one peak and can be fine
tuned. Refer to the service manual for details.

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Getting Started
Any time, the lock field changes by a large amount, the following message is shown:
Figure 1.5 Updating the BSMS Field Value in the edlock Table
Pressing OK updates the BSMS field value in the edlock table. A subsequent lock proce-
dure should be able to find the lock signal in the usual way.
1.13 Manual Shimming to Lineshape
Follow the usual procedure, referring to the Fourier NMR Experiments User Manual
when more information is needed.
Since the shimming process may have an effect on the B0 field, it may be necessary to
redefine BF1 after shimming and lock have been optimized. The ideal BF1 is close to
300.18 when the lock field DAC is close to 2000 (± 500).
1.14 Converting the Parameter Set to the Actual BF1
Before converting the parameter set, make a backup copy of the PAR directory, e.g:
C:\Bruker\TopSpin3.1.b.12\exp\stan\nmr\par
This can be done using CF, followed by “expinstall”. However, the preferred way is to use
CF, followed by the command “paracon”, since it also converts parameter sets in the
user directory. Ignore any error messages when starting, and press “Select all” in both
categories, then execute.

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Getting Started
Figure 1.6 Parameter Set Conversion
iNOTE: If the BF1 has been changed, you will need to restart the console after perform-
ing CF, or paracon has been carried out. Otherwise, the lock frequency will not be
updated.
1.15 Creating a Shim Map for Gradshim
Gradshim works best when the shim map was made using a well shimmed magnet.
Also important for the success of gradshim are that:
• The gradient echo is nicely centered in the spectral width – check by loading the
experiment gradshim 1D2H.
If the gradient echo doesn't look like the figure below, it may be that the parameter
sets have not been converted properly to the correct BF1.

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Getting Started
Figure 1.7 The Gradient Echo Centered in the Spectral Width
• The 2H pulse length is correct. This is normally around 50 µs at 40 W and can be
checked using a zg experiment, where 2H is selected as the observe nucleus. If the
lock is still running when you do this, there will be spikes in the 2H spectrum!
Important Note:
Gradshim uses different parameters on a Fourier than on an AVANCE system. Be sure
to define the parameter sets Gradshim 1d1h_f or Gradshim 1d2h_f when creating a
shim map.
In order for gradshim to work from the “shim” button of the flow bar, and also from Icon-
NMR, it is necessary to store the current configuration for automation (Setup -> Store for
automation). The flow bar or IconNMR will call either a 1H or a 2H gradshim, depending
on what was selected, when the setup was stored for automation.
1.16 ATP Tests and Customer Acceptance
The required Hardware Tests (HWT) for the Fourier 300 are carried out during console
end testing and are not intended to be repeated at the customer site. The following ATP
tests are relevant for the Fourier:
• Determination 90 degree 2H observe pulse
• Determination 90 degree 1H observe pulse
• Determination 90 degree 13C observe pulse
• Determination 90 degree 1H decoupling (CPD) pulse
• Determination 90 degree 1H high power decoupling pulse
• Determination 90 degree 13C low power decoupling pulse

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• Lineshape test for 1H with rotation
• Resolution test for 1H
• Sensitivity test for 1H
• Lineshape Test for 13C with rotation
• Resolution test for 13C
• Sensitivity test for 13C (ASTM)
• Sensitivity test for 13C (EB)
• HSQC experiment with Z?gradient (console test)
• COSY experiment with Z?gradient (console test)
• DEPT?90 experiment
• DEPT?135 experiment
There are only three hardware specifications for the Fourier required for a customer sign
off:
Lineshape using 3% CDCl3 in Acetone: 0.5/8/16 Hz (non-spinning)
1H Sensitivity (0.1% EB in CDCL3): > 120:1 (after gradshim)
C13 Sensitivity (ASTM): > 85:1 (after gradshim).
The remaining ATP tests implicitly demonstrate the systems remaining functions:
• Sample Spin & Lift
•Auto-Locking on various solvents
•Gradient Functionality (2Ds & Gradshim)
•Gradshim reproducibility
•Lock and Temperature Stability (COSY & HSCQ)
•Baseline & Spectral Purity (DEPT)*
Certain artefacts are normal and have been considered acceptable for the intended use
of the Fourier:
• A moderate amount of T1 noise in 2D experiments.
• Some “digital noise” on strong signals that require RG < 10. Use zg30 instead of zg
if that happens, in order to be able to increase the RG.
• Some vibration noise close to the feet of very narrow lines (e.g. lineshape samples).
This can be improved with vibration damping if required.
• Some very small spurious spikes in the first few scans of C13 spectra. These should
average out after NS > 64.
• “Asymmetric smileys” in some 1D spectra with high intensity. This can also be seen
as reduction in the level of noise of about 200 Hz from the right edge of some 1D

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and 2D spectra. If this part contains spectral information, simply increase the spec-
tral width.
iNote: If you obtain reproducible “spurious spikes” in 1H spectra it may be due to an
unfavorable BF1 frequency. The Fourier DDS are “clean” for at least 200 ppm at around
300.18 MHz.

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Appendix
Appendix A
A.1 Main Differences Between Fourier and AVA N CE
The main differences between the Fourier and AVANCE are that with the Fourier:
• The lock works at 1 kHz instead of 6 kHz, which means that sidebands are closer
together. Also, the lock parameters have different units for BSMS values.
• The shims and the BSMS field are not automatically set after power up. You will
need to load a valid shim set using “rsh” to set the shim currents, and switch on the
lock in the BSMS panel to set the current BSMS DAC value.
• The shim values range from -32768 to 32768. When converting from an AVANCE
shim file, you will need to halve the values to get a good starting point.
• There is no PID self tune for the lock, VTU and spin parameters. Since the Fourier is
only sold with one probe, the defaults, when operated at 4 bar, are usually good
enough for all experiments. Refer to the service manual for defaults.
• There is no PICS. You will need to copy “probe.ph” to the corresponding directory.
•The “wobb” command doesn't work from within TopSpin. There is a wobble function
using a stand-alone program. Refer to the service manual for details.
• There is a different pulse programmer language. Refer to the service manual for
details.
• The Digitizer Type must be set to “DRMS”.
•The Aq.mod must be set to qsim.
•The Fn_Mod must be set to TPPI or QF.
•The BC-Mod must always be set to OFF.
•The GPNAM must always be RECT.1.
Table 1.1. Typical BSMS Values for the Fourier
P: 0.1 to 0.8 depending on solvent. Higher values mean more proportional
gain.
I: 0.1 to 0.8 depending on solvent. Higher values mean more integral gain.
Power: -12 to -28 dBm depending on solvent.
Note: The values shown in the BSMS panel are attenuations from 0 dBm.
Filter: 4 for strong solvents, 1000 for weak solvents. The numbers are not the
bandwidth in Hz but the number of averages per second. A value of 1000
is equivalent to 1 Hz, 4 is equivalent to 250 Hz.
Field: 0 to 4095. A value of 2048 means no current flowing in H0 Coil. The ideal
value is between 1500 and 2500, to allow for magnet drift. The BSMS
field has the opposite polarity, i.e increasing the value of the field DAC by
1000 steps will cause a shift left (i.e increase the frequency) by 20 ppm.

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Main Differences Between Fourier and AVANCE

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Figures
1.2 Figures
Figure 1.1 Console Connections............................................................................. 6
Figure 1.2 Bruker DCHP Server.............................................................................. 7
Figure 1.3 Setting the Spin Safety Threshold ....................................................... 10
Figure 1.4 Results of the AU Program FLOCK ..................................................... 11
Figure 1.5 Updating the BSMS Field Value in the edlock Table ........................... 12
Figure 1.6 Parameter Set Conversion................................................................... 13
Figure 1.7 The Gradient Echo Centered in the Spectral Width............................. 14

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Figures