C.
2D NMR Experiments:
Since 2D Experiments are more difficult to set up, than 1D Experiments,
every user should be
extremely cautious when attempting to start the procedure.
The preparation of the experiments requires a lot of interaction of
the user with the spectrometer.
If you are not 100% certain about the procedure, you should ask the
NMR Specialist for assistance. Otherwise you might do serious damage to
the equipment.
All 2D experiments can be broken down into 4 steps:
I. Preparing
the 1D projections (These will be used when you plot the 2D spectra.)
II. Preparing
and starting the 2D experiment (Enter all parameters for the 2D experiment.)
III. Processing the 2D data
set.
IV. Plotting the 2D spectrum.
The following is a list of experiments which are currently
available and will be continuously expanded:
(The substrate requirements show the amount of sample needed, to obtain
a clean spectrum
in the indicated time period. A molecular weight of 500 is assumed.)
-
H,H COSY: to identify protons, which couple with
each other
Substrate requirement: 5 - 10 mg,
30 minutes
-
H,H NOESY: to identify the distance between different
protons
Substrate requirement: 10 - 20 mg,
4 hours
-
H,H TOCSY: to see the complete coupling networks
between protons
Substrate requirement: 5 - 10 mg,
1 hour
-
J-resolved H,H correlation: to separate overlapping
1H
multiplets
Substrate requirement: 5 - 10 mg,
1 hour
-
C,H Correlation: to identify directly connected
protons and carbon atoms
Substrate requirement: 50 - 100 mg,
1 hour
-
COLOC: long range (2,3 bonds) C,H correlation
LOCOF1: same as COLOC, plus: long range C,H
couplings resolved in F1
Substrate requirement: 50 - 100 mg
overnight
-
J-resolved C,H Correlation: to separate overlapping
13C
multiplets
Substrate requirement: 50 - 100 mg
1 hour
-
C,C INADEQUATE: to identify directly connected
carbon atoms
Substrate requirement: >1000 mg
>24 hours
All the instructions have to be followed precisely
and in the order in which they are listed!
C.I Preparing
the 1D Projections
-
Record a routine Proton NMR Spectrum. Process it as usual (Fourier transformation,
phase correction, baseline correction, calibration).
-
Set CX = 15, CY = 15, MAXY = 17.
-
Write the spectrum to the disk. (Use only numbers in the extension, no
letters!)
(You have to save it NOW, NOT later!)
-
Enter the EP mode and press "Ctrl-R" to display the complete spectrum.
-
Set the cursor in front of the first signal in the spectrum (you may ignore
a solvent signal, if it is far away from the signals of your compound.)
-
Press "R" to define the start of the relevant spectrum.
-
Move the cursor behind the last signal in the spectrum and press "R"
again to define the end. Now the display should show only the desired region.
Be careful, not to exclude any signals from your compound!
-
Do NOT press "enter", or you will have to repeat step 4.
-
At this point press "Ctrl-O". This will leave the EP mode and display
the changed values for O1 and SW. Type SW« and increase its
value by approx. 20%.
-
Write down O1, SW and SR, you will need them later.
-
This spectrum must not be stored to disk, as it is useless now!!
-
Repeat steps 1 to 5 for Carbon-13, you should change CX to 18 in step 2.
(The C-13 projection is only necessary for those 2D experiments, which
involve the C-13 nucleus like the C,H correlations and the INADEQUATE experiment.)
-
Continue with the preparation of the individual 2D experiments.
C.II Preparing
the 2D Experiment:
ONLY use the procedure, which describes YOUR experiment. Please follow
it exactly!
Now you will need your list with the O1, SW and SR values from step
C.I.5.
C.IIa
H,H COSY
-
Read your PROTON projection: RE filename.extn « PJ filename.extn
«
-
Set the following parameters:
NOBC = 0, SI
= 1K, ND0 = 1, MC2
= M, RG = 8,
WDW1 = S, WDW2 = S, SSB1
= 3, SSB2 = 3,
SR1 and SR2 = the SR from the proton
spectrum.
O1 = O2 = O11 = the O1 you
found for the proton spectrum.
SW2 = the SW you found for the proton spectrum,
SW1
= half of SW2.
-
Set up the COSY experiment: AS COSYDQF.AU «
This will display the complete microprogram and then (maybe after a
few " « ") it will print out the parameters it needs on the
LCD display or on the screen.
You may accept them by hitting return or you may change them one by
one by entering your new values. Recommended are:
D1 = 2
P1 = 12.5 D0 = 3U
D2 = 50M
D3 = 3U
RD = 0
PW = 0 DE must
not be changed!
NS = 16
DS = 2
NE = 256 IN must not be changed!
Please keep in mind that you must not press " « " after
pressing a letter key!
If you do so by mistake, press Ctrl-Q and repeat step 3.
-
Type ST2D « to bring up the 2D parameter screen.
-
Adjust SI and NE simultaneously (only values of 2n
are allowed here) and repeat
step 4 until the resolution (Hz/Pt) is between 3 and 6.
-
If you need a better resolution, there is a better experiment.(Ask the
NMR specialist.)
-
Type EXPT« to display the duration of the experiment.
If the duration is too long, decrease D1 (but not below "1") or NE
(decrease not by more than 25%, even numbers only) and check the duration
again until it is acceptable.
Do not type ST2D after changing NE!!
You may also change NS to 8, if the sample is concentrated enough (>10
mg) or to multiples of 16 if the sample is very dilute (<2mg).
-
Check I2D, if it is not = 1.0 ±2% then you must start over
from step 1!!
-
Check SF1 and SF2. If they are not equal to the proton frequency,
start over from step 1!!
-
Write the parameters to the disk: WJ2D filename.2DP «
-
Turn off sample spinning and increase the "LOCK GAIN" to the top
edge of the screen.
-
Start the experiment: AU COSYDQF.AU «
Enter the requested filename. The extension ".SER"
is required!!
-
Watch the FID during the first scan. If it is too big (±1 box from
the center) or too small, press "Ctrl-H", change the setting for
RG
and restart the experiment with AU«.
Processing
C.IIb
H,H NOESY
-
Read your PROTON projection: RE filename.extn «
PJ filename.extn «
-
Set the following parameters:
SI = 1K, ND0
= 2, MC2 = W,
REV = Y, REDF = N,
WDW1 = S, WDW2 = S, SSB1
= 3, SSB2 = 3, RG = 8,
NOBC = 1
O1 = O2 = O11 = the O1 you
found for the proton spectrum.
SR1 and SR2 = the SR you found for
the proton spectrum.
SW2 = the SW you found for the proton spectrum,
SW1
= half of SW2.
-
Set up the NOESY experiment: AS NOESYPH.AU «
This will display the complete microprogram and then (maybe after a
few " « ") it will print out the parameters it needs on the
LCD display or on the screen.
You can change them one by one by entering the new values. Recommended
are:
D1 = 2
P1 = 12.5 D0 = 3U
P2 = 12.5
D9 = 2
P3 = 12.5 RD = 0
PW = 0 DE must not be changed!
NS = 16 DS = 2
NE = 512 V9 = 1
IN must not be changed!
Please keep in mind that you must not press " « " after pressing
a letter key!
If you do so by mistake, press Ctrl-Q and repeat step 3.
-
Type ST2D « to bring up the 2D parameter screen.
-
Adjust SI and NE simultaneously (only values of 2n
are allowed here) and repeat step 4 until the resolution (Hz/Pt) is between
3 and 6.
-
Type EXPT« to display the duration of the experiment.
-
If the duration is too long, decrease D1 (but not below "1") or NE (decrease
not by more than 25%, even numbers only) and check the duration again until
it is acceptable.
Do not type ST2D after changing NE!!
It is not advisable to change NS, but if you do, then only in multiples
of 8.
-
Check I2D, if it is not =1.000 then you must start over from step
1!!
-
Check SF1 and SF2. If they are not equal to the proton frequency,
start over from step 1!!
-
Write the parameters to the disk: WJ2D filename.2DP «
-
Turn off the sample spinning and increase the "LOCK GAIN" until
the lock signal is at the top edge of the screen.
-
Start the experiment: AU NOESYPH.AU «
Enter the requested filename. The extension ".SER"
is required!!
-
Watch the FID during the first scan. If it is too big (±1 box from
the center) or too small, press "Ctrl-H", change the setting for
RG and restart the experiment with AU«.
Processing
C.IIc
H,H TOCSY (possible only in inverse mode)
Switch the spectrometer to inverse
operation mode. (Ask the NMR specialist for help.)
-
Read your PROTON projection: RE filename.extn « PJ filename.extn
«
-
Set the following parameters:
SI = 2K, ND0
= 2, MC2 = W,
REV = Y, REDF = N,
WDW1 = S, WDW2 = S, SSB1
= 6, SSB2 = 6,
RG = 8, NOBC = 1
O1 = O2 = O11 = the O1 you
found for the proton spectrum.
SR1 and SR2 = the SR you found for
the proton spectrum.
SW2 = the SW you found for the proton spectrum,
SW1
= half of SW2.
-
Set up the TOCSY experiment: AS TOCSY2D.AU «
This will display the complete microprogram and then (maybe after a
few " « ") it will print out the parameters it needs on the
LCD display or on the screen.
You can change them one by one by entering the new values. Recommended
are:
D1 = 2
S1 = 8H P1 = 38
D0 = 3U P3 = 2500
P2 = 76
L6 = 50 P4 = 2500
RD = 0 PW =
0
DE must not be changed! NS = 16
DS = 2 NE =
1024
IN must not be changed!
Please keep in mind that you must not press " « " after pressing
a letter key!
If you do so by mistake, press Ctrl-Q and repeat step 3.
-
Type ST2D « to bring up the 2D parameter screen.
-
Adjust SI and NE simultaneously (only values of 2n
are allowed here) and repeat step 4 until the resolution (Hz/Pt) is between
3 and 6.
-
Type EXPT« to display the duration of the experiment.
-
If the duration is too long, decrease D1 (but not below "1") or NE (decrease
not by more than 25%, even numbers only) and check the duration again until
it is acceptable.
Do not type ST2D after changing NE!!
-
It is not advisable to change NS, but if you do, then only in multiples
of 8.
-
Check I2D, if it is not =1.000 then you must start over from step
1!!
-
Check SF1 and SF2. If they are not equal to the proton frequency,
start over from step 1!!
-
Write the parameters to the disk: WJ2D filename.2DP «
-
Turn off sample spinning and increase the "LOCK GAIN" to the top
edge of the screen.
-
Start the experiment: AU TOCSY2D.AU «
Enter the requested filename. The extension ".SER"
is required!!
-
Watch the FID during the first scan. If it is too big (±1 box from
the center) or too small,
press "Ctrl-H", change the setting for RG and restart
the experiment with AU«.
Processing
C.IId
J-resolved H,H correlation
-
Read your PROTON projection: RE filename.extn « PJ filename.extn
«
-
Set the following parameters:
SI = 4K, ND0
= 2, MC2 = M,
REV = N, REDF = N,
WDW1 = S, WDW2 = S,
SSB1 = 4, SSB2 = 4,
RG
= 8, NOBC = 0
O1 = O2 = O11 = SR1
= the O1 you found for the proton spectrum.
SR2 = the SR you found for the proton spectrum.
SW2 = the SW you found for the proton spectrum,
SW1
= "30.0".
-
Set up the J-resolved experiment: AS JRES.AU «
This will display the complete microprogram and then (maybe after a
few " « ")it will print out the parameters it needs on the
LCD display or on the screen.
You can change them one by one by entering the new values. Recommended
are:
D1 = 2
P1 = 12.5
D0 = 3U
P2 = 25.0
RD = 0
PW = 0
DE must not be changed!
NS = 16
DS = 2
NE = 64
IN must not be changed!
Please keep in mind that you must not press " « " after pressing
a letter key!
If you do so by mistake, press Ctrl-Q and repeat step 3.
-
Type ST2D « to bring up the 2D parameter screen.
Adjust SI (only values of 2n are allowed here) and
repeat step 4 until the resolution (Hz/Pt) in the F2 dimension is between
0.5 and 1.5.
-
Type ST2D « and then type EXPT« to display the
duration of the experiment.
If the duration is too long, decrease D1 (but not below "1") or NE
(decrease not by more than 25%, even numbers only) and repeat step 5 until
the duration is acceptable.
It is not advisable to change NS, but if you do, then only in multiples
of 8.
-
Type I2D « and enter the 2n-number closest to the
displayed value.
(i.e. set it to . . ., 0.25, 0.5, 1, 2, 4, 8, 16, . . .; only 2n-values
are allowed!)
-
If you want to improve the resolution: double SI2 and set SI1 to
"256W".
-
Check SF1 and SF2. If they are not equal to the proton frequency,
start over from step 1!!
-
Write the parameters to the disk: WJ2D filename.2DP «
-
Turn off the sample spinning and increase the "LOCK GAIN" until
the lock signal is at the top edge of the screen.
-
Start the experiment: AU JRES.AU «
Enter the requested filename. The extension ".SER"
is required!!
-
Watch the FID during the first scan. If it is too big (±1 box from
the center) or too small, press "Ctrl-H", change the setting for
and restart the experiment with AU«.
Processing
C.IIe
C,H Correlation
-
Read your CARBON-13 projection: RE filename.extn « PJ filename.extn
«
-
Set the following parameters:
SI = 1K, ND0
= 2, MC2 = M,
REV = N, REDF = N,
WDW1 = S, WDW2 = S,
SSB1 = 4, SSB2
= 4, NOBC = 0
O2 = O11 = the O1 you found for the
proton spectrum.
O1 = the O1 you found for the carbon spectrum.
SR1 = the SR you found for the proton spectrum.
SR2 = the SR you found for the carbon spectrum.
SW1 = half of the SW you found for
the proton spectrum.
SW2 = the SW you found for the carbon spectrum.
-
Set up the C,H correlation experiment: AS XHCORRD.AU «
This will display the complete microprogram and then (maybe after a
few " « ")it will print out the parameters it needs on the
LCD display or on the screen.You can change them one by one by entering
the new values. Recommended are:
D1 = 2
S1 = 0H P1 = 10.4
D0 = 3U D3 = 3.4M
P2 = 21 P4 =
10.4 P3 = 5.2
D4 = 1.7M S2 = 16H (careful !!)
RD = 0
PW = 0 DE must not
be changed!
NS = 32 DS = 0
P9 = 80
NE = 128 IN must not be changed!
Please keep in mind that you must not press " « " after pressing
a letter key«
If you do so by mistake, press Ctrl-Q and repeat step 3.
-
Type ST2D « to bring up the 2D parameter screen.
Adjust SI and NE (only values of 2n are allowed here) and
repeat step 4 until the Hz/Pt resolutions are between 3 and 6 in F1 and
between 10 and 20 in F2.
-
Type EXPT« to display the duration of the experiment.
If the duration is too long, decrease D1 (but not below "1") or NE
(decrease not by more than 25%, even numbers only) and check the duration
again until it is acceptable.
It is not advisable to change NS, but if you do, then only in multiples
of 8.
-
Check SF1 and SF2. If they are not equal to the 13C
frequency, start over from step 1!!
-
Change SF1 to the proton frequency (360.13).
-
Write the parameters to the disk: WJ2D filename.2DP «
-
Turn off the sample spinning and increase the "LOCK GAIN" until
the lock signal is at the top edge of the screen.
-
Start the experiment: AU XHCORRD.AU «
Enter the requested filename. The extension ".SER"
is required!!
Processing
C.IIf
COLOC - Long Range C,H Correlation
LOCOF1 - Bauer-Freeman-Wimperis Variant of COLOC
(resolves long range C,H couplings in F1)
-
Read your CARBON-13 projection: RE filename.extn «
PJ filename.extn «
-
Set the following parameters:
SI = 1K,
ND0 = 2, MC2
= M, REV = Y,
REDF = N,
WDW1 = S, WDW2 = S,
SSB1 = 4, SSB2
= 4, NOBC = 0
(LOCOF1 : SI = 4K, SSB1 = 0,
SSB2 = 4)
O2 = O11 = the O1 you found for the
proton spectrum.
O1 = the O1 you found for the carbon spectrum.
SR1 = the SR you found for the proton spectrum.
SR2 = the SR you found for the carbon spectrum.
SW1 = half of the SW you found for the proton
spectrum.
SW2 = the SW you found for the carbon spectrum.
-
Set up the C,H correlation experiment: AS COLOC.AU «
This will display the complete microprogram and then (maybe after a
few " « ") it will print out the parameters it needs on the
LCD display or on the screen.
You can change them one by one by entering the new values. Recommended
are:
D1 = 2
S1 = 0H P1 = 10.4
D0 = 3U D3 = 150M
P2 = 21
P4 = 10.4 P3 = 5.2
D4 = 50M S2 = 16H (careful !!)
RD = 0
PW = 0 DE must not be changed!
NS = 64
DS = 0 P9 = 80
NE = 128 (NE = 512 for LOCOF1)
IN must not be changed!
Please keep in mind that you must not press " « " after pressing
a letter key!
If you do so by mistake, press Ctrl-Q and repeat step 3.
-
Type ST2D « to bring up the 2D parameter screen.
Adjust SI and NE (only values of 2n are allowed here) and
repeat step 4 until the Hz/Pt resolutions are between 3 and 6 in F1 and
between 10 and 20 in F2.
(for LOCOF1: ~0.5 Hz in F1 and ~3 Hz in F2)
-
Type EXPT« to display the duration of the experiment.
If the duration is too long, decrease D1 (but not below "1") or NE
(decrease not by more than 25%, even numbers only) and check the duration
again until it is acceptable.
It is not advisable to change NS, but if you do, then only in multiples
of 8.
-
Check SF1 and SF2. If they are not equal to the 13C
frequency, start over from step 1!!
-
Change SF1 to the proton frequency (360.13).
-
Find out the values for NE and IN and set D3 = (NE
* IN)
-
Write the parameters to the disk: WJ2D filename.2DP «
-
Turn off the sample spinning and increase the "LOCK GAIN" to bring
up the lock level.
-
Start the experiment: AU COLOC.AU «
Enter the requested filename. The extension ".SER"
is required!!
Processing
C.IIg
J-resolved C,H Correlation
-
Read your CARBON-13 projection: RE filename.extn « PJ filename.extn
«
-
Set the following parameters:
SI = 4K, ND0
= 2, MC2 = M,
REV = N, REDF = N,
WDW1 = S, WDW2 = S,
SSB1 = 3, SSB2
= 3, NOBC = 0
O2 = O11 = the O1 you found for the
proton spectrum.
O1 = the O1 you found for the carbon spectrum.
SR1 = the O1 you found for the proton spectrum.
SR2 = the SR you found for the carbon spectrum.
SW1 = "300" and
SW2 = the SW you found for the carbon spectrum.
-
Set up the C,H correlation experiment: AS INEPT2D.AU «
This will display the complete microprogram and then (maybe after a
few " « ") it will print out the parameters it needs on the
LCD display or on the screen.
-
You can change them one by one by entering the new values. Recommended
are:
D1 = 2
S1 = 0H P1 = 10.4
D2 = 1.7M P2 = 21
P4 = 10.4 P3 = 5.2
D0 = 250U S2 = 16H (careful !!)
RD = 0
PW = 0 DE must not
be changed!
NS = 32 DS = 2
P9 = 80
NE = 128 IN must
not be changed!
Please keep in mind that you must not press " « " after pressing
a letter key!
If you do so by mistake, press Ctrl-Q and repeat step 3.
-
Type ST2D « to bring up the 2D parameter screen.
Adjust SI and NE (only values of 2n are allowed here) and
repeat step 4 until the Hz/Pt resolutions are below 2 in F1 and between
5 and 10 in F2.
-
Type EXPT« to display the duration of the experiment.
If the duration is too long, decrease D1 (but not below "1") or NE
(decrease not by more than 25%, even numbers only) and check the duration
again until it is acceptable.
It is not advisable to change NS, but if you do, then only in multiples
of 8.
-
Check SF1 and SF2. If they are not equal to the 13C
frequency, start over from step 1!!
-
Change SF1 to the proton frequency (360.13).
-
Write the parameters to the disk: WJ2D filename.2DP «
-
Turn off the sample spinning and increase the "LOCK GAIN" until
the lock signal is at the top edge of the screen.
-
Start the experiment: AU INEPT2D.AU «
Enter the requested filename. The extension ".SER"
is required!!
Processing
C.IIh
INADEQUATE
-
Read your CARBON-13 projection: RE filename.extn « PJ filename.extn
«
-
Set the following parameters:
SI = 1K,
ND0
= 2, MC2 = M,
REV = N,
REDF = N,
WDW1 = S, WDW2 = S,
SSB1 = 3, SSB2
= 3, NOBC = 0
O1 = O11 = the O1 you found for the
carbon spectrum.
O2 = the O1 you found for the proton spectrum.
SR2 = the SR you found for the carbon spectrum.
SR1
= O1.
SW2 = the SW you found for the carbon spectrum.
SW1
= 0.25 * SW2
Set up the C,H correlation experiment: AS INADSYM.AU «
This will display the complete microprogram and then (maybe after a
few " « ") it will print out the parameters it needs on the
LCD display or on the screen.
-
You can change them one by one by entering the new values. Recommended
are:
D1 = 5
P9 = 80
S1 = 18H D3 = 5M
S2 = 16H
P1 = 5.2 D2 = 6.5M
P2 = 10.4 D0 = 2U
P3 = 7
RD = 0
PW = 0
DE must not be changed!
NS = 32 DS = 0
LO VCLIST.001
1 = 1, 2 or 4
2 = EN
NE = 256
IN must not be changed!
Please keep in mind that you must not press " « " after pressing
a letter key!
If you do so by mistake, press Ctrl-Q and repeat step 3.
-
Type ST2D « to bring up the 2D parameter screen.
Adjust SI and NE simultaneously (only values of 2n are allowed
here) and repeat step 4 until the Hz/Pt resolutions are around 20.
-
Type EXPT« to display the duration of one experiment.
Multiply with the value in the VCLIST to get the total duration. If
the duration is too long, decrease NE (decrease not by more than 25%, even
numbers only) or VC and check the total duration again until it is acceptable.
NS must stay "32"!!
-
Check SF1 and SF2. If they are not equal to the 13C
frequency, start over from step 1!!
-
Write the parameters to the disk: WJ2D filename.2DP «
-
Turn off the sample spinning and increase the "LOCK GAIN"to bring
up the lock signal.
-
Start the experiment: AU INADEQUATE.AU «
Enter the requested filename. The extension ".SER"
is required!
Processing
C.III
Processing the 2D Data
-
RE filename.SER «
(read the experimental data)
RJ filename.2DP «
(read the corresponding parameters
PJ filename.2DP «
for acquisition, plotting
RJ2D filename.2DP «
and 2D processing)
Do not change the order of these commands!
-
The default processing parameters usually work fine, but sometimes it may
be necessary to change the window functions WDW1, WDW2 and their parameters
SSB1, SSB2, LB1, LB2, GB1, GB2, TM1, TM2 to get cleaner spectra.
-
Additional steps for TOCSY and NOESYPH only:
-
Set NOBC = 1, type FT«, enter EP and
perform a manual phase correction to make all signals negative. Exit the
EP mode.
-
Type TY«, enter the values 0PHZ as PC0 and 1PHZ as
PC1.
Type PZ«.
-
For all experiments type XFB «. Depending on the size of the
2D matrix this step can
take from a few seconds to several minutes. Check the progress on the
top of the screen.
-
Additional steps for TOCSY and NOESYPH only:
-
Type AP2D «, press 'Ctrl-B' to see positive and negative
levels and move the cursor to a row with well separated signals. Press
'R' to display the row and 'D' or 'I' to de- or increase
the row number, until you find the strongest signals.
Write down this row number and memorize the shape of this 1D spectrum.
-
Press 'Esc' and then 'X' to exit.
-
Type RSC.SMX 'row number' « and correct the phase of the spectrum,
until it looks exactly like the row in AP2D.
-
Type TY«, enter the values 0PHZ as PC0 and 1PHZ as
PC1.
Type PZ«.
-
For TOCSY only: Type XF1P«
and then SYM«
For NOESYPH only: Type XF1P« and then
SYMA«
For JRES only:
Type TILT« and then SYMJ«
For COSY and INADEQUATE only: Type SYMA«.
-
Type AP2D« and adjust the intensity with the vertical display
buttons. The correct level will display only cross- and diagonalpeaks and
as little noise as possible.
-
In case the calibration of one or both of the two dimensions is wrong,
press 'P', then '1' or '2' for the F1 or F2 projection
and then 'E', Press 'Ctrl- R' to see the whole spectrum.
Calibrate the chemical shift scale with a known signal from the 1D
spectrum.
Hit "«" until you are back in the 2D display.
-
Press 'L' and define an expanded region with the wheels A - D. Pressing
'X' will expand. The button combination 'M' / 'Y'
defines the plotting region.
-
Press 'Esc' and then 'X' to exit AP2D.
C.IV Plotting
the 2D spectra
-
Type DPO « and answer the following questions: (the bold answers
are mandatory)
Draw X-Axis? Y Offset: 0.2
Mark Separation: 0.1P for proton, 1.0P
for carbon-13
Mark cm: - 0.2 Draw Y-axis? Y
Mark Separation in F1 Dimension: 0.1P for
proton, 1.0P for carbon-13
Parameters? Y for homonuclear, N for
heteronuclear experiments
Parameters in upper left corner? N
Rotate? N
Title? Y
> (enter the title here, up to 80 characters)
Center Title? N
-
Set MAXX = 25, MAXY = 17, X0 = 0, Y0 = 0, CY
= 15
-
Set CX = 15, if the F1 and F2 dimensions are symmetrical
(COSY, NOESYPH, TOCSY, INADEQUATE)
or set CX = 18 for experiments with non-symmetrical chemical
shift axes.
-
Start the plotting sequence:
- for COSY and TOCSY: CP2P «
F1 Projection: (filename
of the 1D proton spectrum)
F2 Projection: (filename
of the 1D proton spectrum)
Number of Levels: (up to
7)
Number of Pens: (up to 7)
Plot Frame? Y
Grid wanted? N
- for C,H correlation and COLOC: CP2P «
F1 Projection: (filename
of the 1D proton spectrum)
F2 Projection: (filename
of the 1D carbon spectrum)
Number of Levels: (up to
7)
Number of Pens: 1
Plot Frame? Y
Grid wanted? N
- for NOESYPH: C2PB «
F1 Projection: (filename
of the 1D proton spectrum)
F2 Projection: (filename
of the 1D proton spectrum)
Which levels to plot: 0
(zero)
Pen no. for positive levels:
1 (use a black pen in position 1)
Pen no. for negative levels:
2 (use a different color in position 2)
Number of Levels: (up to
7)
Plot Frame? Y
Grid wanted? N
- for INADEQUATE and JRES: CPLP «
F2 Projection: (filename
of the 1D spectrum)
Number of Levels: (up to
7)
Number of Pens: up to 7
Plot Frame? Y
Grid wanted? N
- for JRES (alternate method):
Set CX = 10, CY
= 0, MAXY = 15 and customize DPO.
Enter AP2D« and
print selected columns:
press 'C' to select a column
'I' and 'D' to step through the slices to find the best trace
'E' to enter the EP mode
'Ctrl-R' to display the whole spectrum
'X' to plot
(C)1998 Jürgen
Schulte