Procedures for Obtaining Routine ¹H and ¹³C Spectra

on Varian Mercury-VX 400 MHz Spectrometer

PUT NMR TUBE IN SPINNER:

fill tube to correct level

place spinner in holder

insert tube, inch-by-inch

clean tube and spinner with KimWipe

put sample in safe place

LOGIN:

sign in notebook

advspec/hope

click on spectrum

INSERT SAMPLE:

note whether standard is locked

click in top,left window

e (eject)

remove standard; put in safe place (caution: balance)

insert sample (caution: balance, hissing, bobbing)

i (insert)

wait for SPINNER: Regulated

LOCK AND SHIM SAMPLE:

Acqi

LOCK

Note Z0 for standard

If not locked

increase lock gain to maximum by -64+

off

adjust Z0 by -16+ -4+ until single wave appears

on

if necessary, adjust Z0 by -1+ until it locks

if necessary, increase lock power to maximum by -64+ and repeat

Note: LMB = decrease; RMB = increase

Want lock power = 20-25, lock gain > lock power, lock level >50%

Note lock power for next step

SHIM

Verify course Z menu (Z1, Z2, Z1C, Z2C)

Adjust lock gain so that level ~60

Maximize lock signal by adjusting Z1C with -16+ -4+ -1+

Maximize lock signal by adjusting Z2C with -16+ -4+ -1+

If major changes were made, cycle though Z1C and Z2C again

If lock level increase above 100%, reduce lock gain (caution: keep lock gain > lock power)

At end, adjust gain for lock level 70~80

Note: first and best buttons if you get lost

CLOSE

ACQUIRE SPECTRUM:

GLIDE

Setup

Experiment: RMB; choose type

Solvent: RMB; choose solvent

AutoLOCK: NO

AutoSHIM: NO

Save As: ######## (2 for initials; 4 for sample/experiment, e.g., WPIBH)

Text: description (e.g., WFP isobutanol 1H)

Setup

Custom (automatically selected)

Acquire

Accept or adjust settings

Do

Wait until spectrum is DONE (watch CT increase)

Custom

Process

Process

Box (change to box mode)

Set limits with LMB and RMB

Expand

Part Integral (for ¹H only; display partial integrals)

click LMB on known integral

Set Int (for ¹H only; set integral value)

enter new value for integral and press Return

Custom

Plot

Spectra Width: Displayed Spectrum

Plot Integral: Partial

Plot Parameters: Upper Left

Plot Peaks: Upper Right

Do Plot

Exit (exit Glide)

REPLACE STANDARD:

e (eject)

remove sample; put in safe place

check standard height in spinner with holder

clean tube and spinner with KimWipe

insert standard (caution: balance, hissing, bobbing)

i (insert)

wait for SPINNER: Regulated

LOCK STANDARD:

Acqi

LOCK

increase lock gain until it locks

if it doesn’t lock, adjust Z0 (you noted it before)

CLOSE

LOGOUT:

exit

click on tiny Exit sign and on OK

GLIDE.doc