MSL-300 1H Operating Instructions
1. Check to see that the 1H probe is in the
magnet. Be sure to wipe the spinner and sample
with a Kimwipe.
2. Place the Sample in the Magnet.
a) Remove the cap from the top of the magnet.
b) Push the Orange
button and the Lift button on the AMOS panel (to the right of the
keyboard). Listen for the lift air.
c) Float the tube/spinner on top of the magnet.
d) Push the Lift-Off button.
Sample should sink down into the magnet.
e) Push the SPIN button. The light on the button should be
on.
3. Lock the Magnetic Field on the Deuterium Signal.
a) You should see a lock signal of some kind moving across the monitor.
Using ^L as needed
(^L is a 3 position toggle: lock only/lock
plus data/data only).
b) Push LOCK POWER and adjust it using the black knob. ( ~40
for CDCl3, 25 for
Acetone, and 30 for everything else.)
c) Push FIELD and use the knob to center the lock signal. (CDCL3
is at ~6430, D2O at
~6650, acetone at ~6930). The two triangles should
be spaced equally on each side of
center.
d) Push LOCK. When the light is on (not flashing) the
magnetic field is locked. Be noted that:
1) You may need to increase
the LOCK GAIN for the system to lock.
2) It may be of helpful
to move the field slightly to obtain the lock.
3) Push Dual Sweep to turn
it off if you were using it.
4. Shim, Using Z and Z2.
a) First, adjust LOCK GAIN so that the lock signal is between
the top two grid marks.
b) Shim using Z and Z2 by pushing the button and adjusting the knob.
Repeat the preceding
adjustment for maximum lock level. You may change
the LOCK GAIN accordingly to
keep the lock signal visible.
c) Push Stand-By when satisfied.
5. Entering Commands.
a) Most commands must be followed by a <Return>, with the
exception being in EP mode.
b) <Del> can be used to delete the last character typed.
c) ^O will delete the whole line.
d) If the instrument is not responding, type ^Q. Rebooting
the computer is not recommended
unless absolutely necessary.
e) Do not use <Bs> to erase mistakes!!!
6. Setting up the Spectrometer.
Read in a standard file by typing either: RJ H1.CDCL <Return>,
RJ H1.D2O <Return>, or RJ
H1.ACET <Return>.
An alternative to RJ is RE filename.ext <Return>
of an old file.
7. Type II <Return>
to set up parameters.
8. Collecting Data.
a) Type RGA <Return> and wait for this command to execute.
b) The standard files (except proton) have NS set to -1 so that
the spectrometer will collect
data until you stop it. You may change NS
by typing NS <Return> and entering the
number of scans desired, followed by a <Return>.
c) Type ZG<Return> to begin data acquisition. Scans are counted
in the upper left of the
screen. ^H or <Return> will stop
the data acquisition.
9. Saving Data.
a) If desired, type TI<Return> sample description <Return>.
b) Type WR filename.ext <Return>. Filename can be
up to 8 characters, the extension is 3
digits.
10. Looking at the Spectrum During Acquisition.
a) The data system is organized into 3 independent blocks (Jobs 1, 2,
3).
b) The number showed on the screen is the block you are currently in.
This can be changed
simply by typing the number of the block you wish
to be in.
c) You can only transfer the contents of the block you are currently
in. Transfer is initiated by
typing TR<Return>, and followed by
entering the number of the block you wish the data
to be transferred to. You can only transfer
the data to a block other than the one where
acquisition is occurring! A <Return> will
transfer the data to the block requested.
d) Example: If you are collecting data in block 1 and want to
transfer it to block 2, type a 1 if
you are not currently in this block, and then type
TR; <Return>; 2; <Return>.
e) When the data has been transferred out of the acquisition block,
it may be processed as
described in section 11.
f) Typing ^H or Bs will stop the acquisition.
11. Processing Data.
a) Type LB<Return> and enter the desired number followed by
a <Return>. Usually select
0.1 for proton and 1 for carbon. The minimum value
allowed is 0.01.
b) Type EF<Return> or EFP<Return>.
c) Type EP<Return>. This command enters the expand and phase
mode in which phasing,
chemical shift, plot limits, and peak heights can
be set.
1. A <Return> will exit the
EP mode.
2. ^R displays the entire spectrum,
^B allows the use of A and B knobs
3 Phasing
a) Turn the
A knob (left or right shift) until the biggest peak is displayed.
b) Type P
c) Turn the
C knob to phase the peak, type ^C to reverse the sense of
this knob if you
reach the end.
d) The vertical
display buttons (to the left of the keyboard) may be used to control
the
height and the B knob the width of the peak.
e) Turn the
A knob until a peak remote from the biggest peak is displayed.
f) Turn
the D knob to phase this peak, type ^D to reverse the sense
of this knob if you
reach the end.
g) Turn the
A knob to return to the biggest peak and repeat steps c-g if necessary.
h) Type M
to memorize the phase.
4. Setting the reference.
a) Turn the
A knob to locate the reference peak.
b) Use the C
knob to place the cursor on top of this peak. The D knob is fine
control of
the cursor.
c) Type Gxx<Return>
where xx is the chemical shift.
5. <Return>
exits EP mode.
12 Transferring the Data to Xwinnmr.
a) In an unused job, type RE filename.ext <Return>
b) type AU SEND.AU<Return>
13. Leaving the Instrument.
a) Type PO<Return> to turn off the decoupler.
b) Push <Return> to turn the Lock off.
c) Push the Orange Button and the Sample lift button to eject
sample.
d) Push Lift off to turn off eject air.
e) Put cap on top of magnet.
f) Log off CIA.
14. Process the Data on nmr or nmrtwo - the SGI
UXNMR Processing Computers.
a) Log-onto nmr or nmrtwo as usual, and start xwinnmr.
b) Type btran<Return>
c) First time users must select Edit Program Options. The
options should be:
/dat1/bruknet
(Current Destination)
msl300
(Current station)
bruker
(Current user)
dat1
(disk)
your username (owner)
d) Click SAVE
e) Select Select, Convert (no renaming), YourFile, Conv, Quit
f) The data should be in your directory now.
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