Spectrometer Setup


start UXNMR:
************
uxnmr, or xwinnmr
uxnmr -r removing shared memories and other jobs
shmrm removing shared memories



Setup:
******
te temperature
teset
edte temp control unit

lock power H2O: -17 to -20, D2O: -20 to -30
shim use "gradshim" (for shigemi: 10, 12, 14 points)
autoshim during acquisition:
active shims use bsmsdisp (in XWINnmr), go to autoshim
interval sampling interval (sec) > d0 (BSMS, 2nd left, bottom row)
Further info: Bruker Acquisition Manual
wobb
wbsw
wbst

ased set parameters
eda gradients/progs, decoupling, sel. pulses, etc
edasp amplifiers, connections, frequencies (compilation errors)
edcpd composite pulse decoupling
edgp gradient pulse programs
expt calculate time of experiment
asl absolute lock shift (12125263 @ 600 MHz)
setres user interface settings



Tools:
******
bsmsdisp BSMS interactive display
pulsdisp display pulse sequence (set ds to 0, ns to 1)
acbdisp display power output
xshape generate shaped pulses



Processing:
**********
qsin sin bell apodization (ssb: phase shift)
qfp (1,d) qsin, ft, pk (rser1, dual)
wrp n write processed data (2D)
tr write current memory byffer to disc



Files:
******
PP /u/exp/stan/nmr/lists/pp
GP /u/exp/stan/nmr/lists/gp
shims /u/exp/stan/nmr/lists/bsms
AU /u/exp/stan/nmr/au (/src)
mac /u/exp/stan/nmr/lists/mac



Power: P'/P dB = 20*log(P'/P)
****** P'/P = 10^(dB/20)
1 dB 1.122 89%
2 dB 1.259 79%
3 dB 1.412 71%
4 dB 1.585 63%
5 dB 1.778 56%
6 dB 1.995 50%
10 dB 3.162 32%
12 dB 3.981 25%
14 dB 5.012 20%
20 dB 10 10%
40 dB 100 1%



Selective Pulses:
*****************
p90, null for C' = sqrt(15)/(4*Omega)] = 0.968/Omega
1/2 p180, null for C' = sqrt(3)/(4*Omega)] = 0.433/Omega



Problems:
*********
boot: as SUPER-USER
init 0 bring computer down
init 1..5 bring computer down and up to different lewels
init 6 bring computer down and completely up

CPR problems:
-------------
reviveccu if no licence available (CPR) (as SUPER-USER)
cf
or:
telnet spect (user root)
init 6

BSMS problems:
--------------
reset first cage, bottom part, left top
off/on first cage, bottom part, bottom right
if red light on "TRANS P-DOWN" (top right on BSMS board):
acbdisp -> Controls, -> ACB Reset (=> red light off)



Important Numbers:
******************
600:
ASL 12125263
lock freq 3980
O1 10778



Change SCSI:
************
init 0
turn computer off (round button)
reconnect disks/tape drives (make shure, address is correct)
restart computer (round button)

if new (eg. disk drive)
hinv (check address)
disk manager -> open new SCSI -> initialize -> ok
mkdir /disk4
disk manager -> open new SCSI -> mount



Load new software:
******************
make backups!
load disk (/CDROM) [/u ~ 140 MByte]
click on "startme"
cp -rp /u/exp/sstan/nmr/lists: bsms, cpd, eurotherm, f1, gp, mac,
pp, preemp, v*, wave
/u/exp/sstan/nmr/au/src
/u/conf/instr: boss, curinst, probehead, spect
/u/data
uxnmr: "cf"
"setpre" (read, ...)



Miscellaneus:
*************
Set Date and Time (as super user):
date 1630

phtran (on AMX) qfp1, store, phtran (-> set values)

 

 

Pulse programming

pulsedisp display of pulse prog
ed(c)pul edit pulse prog
eda / pulprog set pulse prog
edasp define channels
edcpd edit composite pulse decoupling (cpd) sequence
with order duration[*multiplier:shape]:phase
edlist edit a list (for variable pulses, frequencies, delays)
shape/xshape create shaped pulses



syntax
******

Pulses (length, frequency, phase, power):
-----------------------------------------
p0-p31 pulse length
10mp fixed pulse with 10 ms length (up, mp, sp)
vp variable list pulse (-> edlist)

f1-f8 channel 1-8 with frequency SFO1-8, f1 = default (-> edasp)
fq1-fq8 change frequency according to FQ1(-8)LIST (-> edlist, eda)

ph0-ph31 phase, example: ph1 = (5) {1 2}*2^1 [= (5) 1 2 1 2 2 3]
ph3^ = ipp3 increment phase pointer (here of phase 3) |
ph4:r all phases incremented by PHCOR4 (-> eda) |
ip5 increment phase 5 by 1 (usually 90 deg) | need delay!
dp5*2 decrement phase 5 by 2 (usually 180 deg) |
rp5 reset phases 5 to original values |

pl0-pl31:f1 set power level 0-31 for channel 1 (needs delay > 2us)
defaults of f1-f8 according to PL1-PL8
sp0-sp15 shaped pulses (-> eda, click on SP07, -> shape/xshape
stored in /u/exp/stan/nmr/lists/wave/)

examples:
(p1*2 ph1):f1 180-pulse, phase, channel 1 (optional if f1)
d11 pl6:f1 delay 11, set power level 6 for channel 1
d14 fq2:f3 delay 14, change frequency of channel 3 according to FQ2LIST
(p1:sp2 ph7):f1 generation of a shaped pulse



Delays:
-------
d0-d31 delay according to acquisiton parameter D0-D31 (-> eda)
id0 increment delay 0 according to IN0 |
dd3 decrement delay 3 according to IN3 | need delay!
rd5 reset delay 5 to D5 |
1u, m, s delay of fixed length: 1 us, ms, s
vd, ivd variable delay looked up/increased (needs delay) in table (-> edlist)

examples:
d1 ivd delay D1, variable delay increased
d2*2 delay D2 times 2
"d13=d13 + (p1*3 - 2m)*td" recalculation of a delay




Decoupling:
-----------
cw continuous wave decoupling
hd homodecoupling
cpds1-cpds8 composite pulse dec. with seq. 1-8, synchronous mode (-> edcpd)
cpd1-cpd8 composite pulse dec. with seq. 1-8, asynchronous mode
cpd sequence according to CPDPRG1-8, e.g. WALTZ16, GARP, etc
do:f1 decoupling off

examples:
d1 (cw ph1):f1 turn on cw-decoupler (with phase 1) on channel f1 when d1 starts
0.1u cpds1:f1 turn decoupler on (sequence1, channel1)
0.1u do:f1 turn decoupler off (channel 1)



Conditional pulse programming:
------------------------------
#define FLAG |
#ifdef FLAG, #ifndef FLAG | conditions evaluated
#endif | at compile time
#define macro1 (p1 d1) (p2):f2 |

if expression goto label | conditions evaluated
if (trigger) goto label | at run time



Start data acquisition:
-----------------------
go=label acquisiton scan, go to label
gosc acquisiton scan
gonp=label acquisiton scan, go to label | no automatic
goscnp acquisiton scan | phase incrementation

adc/rcyc=label

ze reset scan counter to 0, enable dummy scans
zd same as ze, but no dummy scans

examples:
go=2 ph31 acquisiton of one scan, loop to 2 until NS scans (preceded by DS)
receiver phase is changed according to phase table 31



Writing to disc:
----------------
wr #0 write fid
if #0 advance the disk file pointer by TD*NBL

examples:
d11 wr #0 if #0 id0 zd during delay 11 write to current data set, advance
file pointer, increment d0 by IN0, no dummy scans


Gradients:
----------
gron0-31 rectangular gradient field on using strength GPX0, GPY0, GPZ0
groff gradient off
p1:gp0-31 gradient pulse 0-31 with duration of p1 (-> eda, GP031-button)
shape: -> shape/xshape




Miscellanous:
-------------
; comment
lo to x times y loop to label x for y times (y = number, td, td1, l1, c)
l0-l31 loop counter (L0-L31 in -> eda)
iu0, du0, ru0 increment, decrement l0 by 1, reset l0 to L0
goto label go to label



Specials:
---------
#include <file.incl>


define pulse/delay VariableName
(p1 ph1):f1 (d1) (p2 ph2):f2 simultanous pulses and delays