Short Instructions for basic operation of the Bruker NMR
spectrometer (xwinnmr)
.
* Take out the plastic cap of the top of the sample insertion port.
(Do not use the
nitrogen valve as the place to store the cap).
* Put your sample into the spinner turbine. Make sure that NMR
tube is clean and
dry. Do not touch the turbine’s shaft by fingers.
Use the insert gauge to find out
the proper sample depth. To achieve a good shimming,
the length of a sample
should be larger than the length of corresponding
coil. We are using 5mm coils on
all spectrometers.
* Push the “Lift ON/Off” button on
BSMS keyboard, light will come on. After you
hear whistling gas coming from the top of the magnet
place sample on air cushion
and push the “Lift ON/OF
button. The sample will descend softly into the NMR
magnet.
* After you seen the green “sample down” light lit, press Spin
“ON/OFF" button.
The light will flash till the sample is at the set
speed, will stay lit.
* Log into your account on SGI workstation.
* Open the UNIX shell window. (if you need to change your password
type
“passwd” command and
follow prompts.
* Type “xwinnmr” at the prompt.
* When the xwinnmr window opens, under file menu select “ New”
Make sure that under “user” in this menu is your
login name and under “DU” is
the disk partition: /m
* At the prompt at he bottom of the xwinnmr window, type
“rpar”.
* For a proton experiment select “ stdh1.QNP or stdh1.BBI
or stdh1.BBO, etc.,”
(need to scroll down), and select “ Copy All” in the next window. For any other
nucleus select appropriate one.
* At the prompt, type “rsh” and select
the default shims. On nmr400 and nmr500
equipped with quattro nucleus probe the default shims
files has extension “QNP”
default.QNP. On other
nmr500 and nmr400 they might have extension “BBI
” or
“BBO”. The information which
one you should use can be found in the message
at the Unix window after you logged to your account.
* At the prompt type “lockdisp” and
resize it according to your needs.
* At the prompt type “lock” and select
your solvent from the list provided.
* Perform the magnet shimming.
* Select “Z” on the keypad, and rotate
the dial to maximize the signal
* Select “Z 2 ”, repeat maximization.
Normally, you do not need to shim higher orders.
* Repeat above steps until the signal is maximized.
*On 500MHz DMX press “ONAXIS” and
select “Z1” instead “Z
”
* Select “lockgain”, adjust until
the signal is within second line from the top.
* If the lock signal becomes saturated lower the lock power. Most
often the good
working lock power can be found in the range of –25 to –35 DB.
* Select “Standby”
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