Agilent Technologies VARIAN Dual User manual

Dual and Dual
Broadband NMR
Probes Installation
Varian, Inc. NMR Spectrometer Systems
Pub. No. 01-999124-00, Rev. J 0606
NOTICE: This document contains references to Varian.
Please note that Varian, Inc. is now part of Agilent
Technologies. For more information, go to
www.agilent.com/chem.

01-999124-00 J 0606 Dual and Dual Broadband NMR Probes Installation 1
Dual and Dual
Broadband NMR
Probes
Varian, Inc. NMR Spectrometer Systems
• Overview, page 2
• Safety Precautions, page 2
• Installing the Probe, page 3
• Connecting to VnmrS Systems, page 3
• Connecting to UNITY-Series, page 3
• Connecting to MERCURY-Series, page 4
• Tuning the Probe, page 5
• Returning to Normal Operation, page 6
• Tuning Ranges for Dual and Dual Broadband Probes, page 6
• Sample Tube Specification, page 7
• Testing Probes on VnmrS and UNITYINOVA Systems, page 8
• Testing Probes on MERCURYplus, page 18
• Test Results, page 27
Pub. No. 01-999124-00, Rev. J 0606

Dual and Dual Broadband NMR Probes
2Dual and Dual Broadband NMR Probes Installation 01-999124-00 J 0606
Overview
DualandDual Broadband probes enable observation anddecouplingof high-frequency and
low-frequency broadband nuclei. This manual covers the following probes:
Safety Precautions
CAUTION: Forced turning can cause mechanical damage to the probe,
requiring factory repair. Do not force the tuning capacitors to turn
past the end of their ranges. The end of the range is indicated by
an increase in torque and not necessarily a stop to the rotation.
Magnet
(MHz) Bore (mm) Sample Size (mm) Range Probe Part No.
200 54 5 1H/13C 01-904927-00
200 89 5 1H/13C 01-910580-00
200 PFG 54 5 1H/13C 01-911985-00
200 PFG 89 5 1H/13C 01-911988-00
200 PFG 54 5 1H–19F/15N–31P 01-910552-00
200 PFG 89 5 1H–19F/15N–31P 01-911991-00
200 54 5 1H–19F/15N–31P 01-902651-00
200 89 5 1H–19F/15N–31P 01-902654-00
300 89 5 1H/13C 01-910554-00
300 54 5 1H/13C 01-904510-01
300 PFG 89 5 1H/13C 01-911973-00
300 PFG 54 5 1H/13C 01-910556-00
300 PFG 89 5 1H–19F/15N–31P 01-911982-00
300 PFG 54 5 1H–19F/15N–31P 01-910558-00
300 89 5 1H–19F/15N–31P 01-902635-01
300 54 5 1H–19F/15N–31P 01-902632-01
400 54 5 1H/13C 01-910561-00
400 89 5 1H/13C 01-910562-00
400 PFG 54 5 1H/13C 01-910564-00
400 54 5 1H–19F/15N–31P 01-905069-02
400 89 5 1H–19F/15N–31P 01-905530-02
400 PFG 54 5 1H–19F/15N–31P 01-910566-00
400 PFG 89 5 1H–19F/15N–31P 01-910567-00
500 PFG 51 5 1H/13C 01-915813-00
500 PFG 51 5 1H–19F/15N–31P 01-904937-02

01-999124-00 J 0606 Dual and Dual Broadband NMR Probes Installation 3
Installing the Probe
Installing the Probe
1. Verify proper installation and adjustment of the upper barrel and probe mounting
flange as follows:
• The upper barrel is seated against the room-temperature shim coil.
• The probe flange set screws is backed off from the probe shield allowing the
flange to slide (with some effort) along the shield.
Probes used with widebore (89-mm) magnets require a widebore adaptor (a white
plastic ring shipped in the probe case). Position the adaptor at the midpoint of the
probe shield and secure in place with the three set screws. Placing the adaptor too
close to the NMR coil region causes lineshape difficulties.
2. Insert the probe into the bottom of the magnet.
3. Push the probe up until contact is made with the upper barrel.
4. Do the following for PFG probes:
• Apply pressure while rotating the probe until the probe shield key engages; this
aligns the PFG pins with the sockets in the upper barrel.
• Continue to push the probe up until the pins engage and the upper barrel rises
slightly (this ensures a good seal between the upper barrel and probe).
5. Secure the probe flange to the magnet with the thumbscrews.
6. Press the upper barrel down until it seats into the room-temperature shim coil.
7. Tighten the three set screws in the probe flange against the probe shield.
CAUTION: Overtightening the set screws will dent the probe shield.
Connecting to VnmrS Systems
1. Connect the decoupler or proton port of the probe to the high band or proton port of
the r.f. front end.
2. Connect the 13C or X port of the probe to the X or low band port of the r.f. front end.
3. Connect the lock port of the probe to the lock port of the r.f. front end.
Connecting to UNITY-Series
UNITY-Series includes the UNITYINOVA, UNITYplus, and UNITY systems.
1. Connect the LK PROBE connector (P5205), which is inside the magnet leg on top
of the lock preamplifier,to the 250-MHz low-pass filter mounted on the back of the
magnet leg, and then connect the filter to the LOCK connector on the probe.
2. Connect the observe low band cable using the appropriate step below:
Connect an appropriate low-pass and notch filter in line to the B BAND or
OBSERVE NORMAL port on the magnet-console interface (magnet leg). Connect
a cable from the filters to the X CHANNEL port on the probe.
•500-MHz systems using dual preamplifier – Connect an appropriate low-pass
and notch filter in line to the PROBE port (J5311) on the broadband

Dual and Dual Broadband NMR Probes
4Dual and Dual Broadband NMR Probes Installation 01-999124-00 J 0606
preamplifier, and thenconnect a cable from the filters to the X CHANNEL port
on the probe.
Omit thenotch filter when observing 2H or other nuclei whose resonance frequency
is close to 76 MHz.
3. Connect the decoupler cable using the appropriate step below:
•Systems using 1H/19F OBS preamplifier – Connect acable anda high-pass filter
between the 1H/OBS/DEC port on the magnet-console interface (magnet leg)
and the PROTON port on the probe.
•Systems using broadband preamplifier – Connect a cable and a high-pass filter
between the H BAND or 1H/OBS/DEC port on the preamplifier and the
PROTON port on the probe.
•500-MHz systems using dual preamplifier – Connect a cable and a high-pass
filter between the PROBE port (J5301) and the PROTON port on the probe.
4. Select an external quarter-wavelength cable to match the frequency of the observe
nucleus. Attach this cable between the two BNC connectors labeled 1/4
WAVELENGTH on the preamplifier.
5. Connect the cable from the variable temperature controller (VTC) to the 9-pin
connector (VT Control) on the probe.
6. Connectthe VT nitrogengas hose to the stub tee onthe glass dewar projecting to the
side at the base of the probe.
7. Connect the body-cooling air hose to the hose barb protruding from the bottom of
the probe.
Connecting to MERCURY-Series
MERCURY-Series includes the MERCURYplus, MERCURY VxWorks Powered, and the
MERCURY systems. Newer production MERCURYplus system have a Magnet Interface
Box and older MERCURY-Series systems have a Magnet Leg. Use the procedure that is
appropriate for the instrument with which this probe is to be used.
Magnet Interface Box
1. Connect a band-pass notch filter to From Probe Lock J6002on the Shimming Relay.
Connect the filter to the LOCK connector on the probe.
2. Connecta low passfiltertoFrom BB Probe J6001,on theShimmingRelay,and cable
from the filter to the OBS connector on the probe.
3. Connectacable from J5102HiBndPreAmp to the PROTON connectoron theprobe.
4. Connect the appropriate quarter wavelength cable between J5304 and J5305, see
Table 1.
5. Continue with VT Connections, this page.
Magnet Leg
1. Connect the LK PROBE connector (P5202) to a band-pass notch filter, and then
connect the filter to the LOCK connector on the probe.
2. Connect a cable from the 13C connector (J5302) on the left magnet leg to the X-
CHANNEL connector on the probe.

01-999124-00 J 0606 Dual and Dual Broadband NMR Probes Installation 5
Tuning the Probe
3. Connect the appropriate quarter-wavelength cable between J5304 and J5305 on the
magnet leg, see Table 1.
4. Connect the decoupler cable (from the 1H connector J5102) to the PROTON
connector on the probe.
5. Continue with VT Connections, this page.
VT Connections
1. If the VT option is present, connect the cable from VT controller to the 9-pin
connector (VT Control) on the probe, and connect the VT nitrogen gas hose to the
stub tee on the glass dewar projecting to the side at the base of the probe.
2. Connect the body-cooling air hose to the hose barb on the bottom of the probe and
adjust the air flow to optimize sample insertion, ejection, and spinning.
Tuning the Probe
Place the sample to be analyzed in the probe during tuning and follow the 1H channel and
X channel tuning procedures every time you change samples.
The Dual and Dual Broadbandprobes, shown in Figure 1, incorporates a numerical counter
system and probe label on the broadband channel that corresponds to the tuning of the
nuclei to be decoupled/observed. The knurled tune knob changes the values on the
numerical counter, while the smooth knob operates the matching capacitor. The lower the
frequency of the nucleus, the more the smooth match knob needs to be turned clockwise.
Tuning the 1H Channel
Alternately adjust the match and tune knobs to find the minimum reflected power on the
tune meter. The knurled knob with the red PROTON inset label turns thetuning capacitors,
while the smooth lower knob turns the match capacitor (see Figure 1). When tuning to 19F,
adjust the knurled knob in the counter-clockwise direction and adjust the match capacitor.
Tuning the X Channel
Turn the knurled X CHANNEL knob, shown in Figure 1, to a numerical counter value that
corresponds to the nucleus to be observed. The probe label shows four popular nuclei. To
fine tune, alternately adjust the smooth and knurled X CHANNEL match and tune knobs
to find the minimum reflected power on the tune meter.
Table 1. Quarter Wavelength Cables for MERCURY-Series
Frequency (MHz) Cable (Color)
44–178 Yellow
37–118 Black
11–45 Blue

Dual and Dual Broadband NMR Probes
6Dual and Dual Broadband NMR Probes Installation 01-999124-00 J 0606
1H/13C Dual Probe Tuning Controls
Dual probes have three controls that are operated by color-coded controls extending from
the bottom of the probe:
The carbon observe coil tuning and matching controls are used to tune and match the
transmitter/receiver coilin the probe to resonance at the observe transmitter frequency. The
decoupler coil tuning control is used to tune the coil in the probe to resonance at the proton
transmitter frequency. The probe may need to be tuned after a sample or solvent ischanged.
Returning to Normal Operation
After tuning the probe, enter dm='n' su to make sure the decoupler is not inadvertently
left on. Check the 1H channel tuning after X-channel tuning and after a sample change.
Tuning Ranges for Dual and Dual Broadband Probes
Ranges are approximate and valid for empty probes only. Ranges are slightly lower with a
sample in a probe
Function Color
13C observe coil tuning green
13C observe coil matching blue
1H observe/decoupler coil tuning red
Figure 1. Probe Connectors and Tuning Controls
Tune and
match
controls

01-999124-00 J 0606 Dual and Dual Broadband NMR Probes Installation 7
Sample Tube Specification
Tuning Ranges for 200-MHz Dual And Dual Broadband Probes
Tuning Ranges for 300-MHz Dual And Dual Broadband Probes
Tuning Ranges for 400-MHz Dual And Dual Broadband Probes
Tuning Ranges for 500-MHz Switchable Probes
Sample Tube Specification
Tests are performed with the following sample tubes:
• 5-mm probes: 5-mm tubes with 0.38-mm wall (Wilmad 528-PP, or equivalent).
• Using sample tubes with thinner wall thickness (e.g., Wilmad 5-mm 545-PPT, or
equivalent) increases signal-to-noise.
Capacitor Stick
(pF) Range (MHz) Capacitor Stick (pF) Range (MHz)
none 43–83 36 25–28
11 34–45 50 22–24
19 30–37 66 19.5–22
27 27–31
Capacitor Stick
(pF) Range (MHz) Capacitor Stick (pF) Range (MHz)
none 55–125 30 32–36
11 42–57 36 30–33
23 35–42 40 28–31
Capacitor Stick
(pF) Range (MHz) Capacitor Stick (pF) Range (MHz)
none 85–165 33 47–52
9 66–88 36 44–48
17 57–67 43 42–45
26 51–58 48 39.5–42
Capacitor Stick
(pF) Range (MHz) Inductor Stick (turns) Range (MHz)
none 88–180 (13C) 13 180–202 (31P)
7 67–88
14 59–67
21 53–59
27 50–53 (15N)

Dual and Dual Broadband NMR Probes
8Dual and Dual Broadband NMR Probes Installation 01-999124-00 J 0606
Testing Probes on VnmrS and UNITYINOVA Systems
This section contains test and calibration procedures for the dual (1H/13C) and dual
broadband (1H–19F / 15N–31P) probes on VnmrS and UNITYINOVA systems:
•Table 2 lists the tests appropriate for each probe type.
•Table 3 lists the test samples.
Table 2. Probe Test Order
Test 200 & 300
Dual
200, 300, 400,
Dual
Broadband
500
PFG
Dual
500 PFG
Dual
Broadband
γH2Calibration, page 9 ****
1H Observe 90° Pulse Width, page 9 ****
1H Spinning Resolution & Lineshape, page 10 ****
1H Spinning Sidebands, page 10 ****
PFG Profile and Recovery, page 11 PFG Probes — **
1H Sensitivity, page 12 ****
19F Observe 90° Pulse Width, page 12 —*—*
19F Sensitivity, page 13 —*—*
31P Observe 90° Pulse Width, page 13 —*—*
31P Sensitivity, page 14 —*—*
13C Observe 90° Pulse Width, page 14 ****
13C Spinning Resolution & Lineshape, page 15 ****
13C Spinning Sidebands, page 15 ****
13C Sensitivity, page 16 ****
15N Sensitivity, page 17 —*—*
Table 3. Acceptance Tests and Samples
NMR Test Sample Part No.
1H PW90, 1H sensitivity 0.1% ethylbenzene, 0.01% TMS
99.89% deuterochloroform (CDCl3)00-968120-70
1H spinning res. & lineshape,
1H spinning sidebands 1% chloroform in acetone–d600-968120-89
PFG Profile and recovery 4-Hz 1% H2O, 99% D2O01-901855-01
19F PW90, 19F sensitivity 0.05% trifluorotoluene in benzene–d600-968120-82
31P PW90, 31P sensitivity 0.0485 M triphenylphosphate in CDCl300-968120-87
13C PW90*, 13C sensitivity
*40% p-dioxane in benzene–d6(ASTM) 0.2% Cr(acac) (00-968120-91) can also be used.
40% p-dioxane in benzene–d6(ASTM) 00-968120-69
13C spinning res. & lineshape,
13C spinning sidebands 40% p-dioxane in benzene–d6(ASTM) 00-968120-69
15N PW90 90% formamide in DMSO–d600-968120-83

01-999124-00 J 0606 Dual and Dual Broadband NMR Probes Installation 9
Testing Probes on VnmrS and UNITYINOVA Systems
γH2Calibration
1. Insert the appropriate ASTM sample in the probe and spin it.
2. Enter rtp('/vnmr/tests/gammaH2') su to retrieve the test parameter set to
the current experiment.
3. Install the appropriate quarter-wavelength cable for 13C.
4. Tune the probe.
5. Enter pw=10 tpwr=46 ga.
After determining the 13C 90°pulse width, repeat this calibration by setting pw to
the 13C 90°pulse width and tpwr to the power used to achieve the 13C 90°pulse
width.
6. Enter dm='nny' dpwr=30 d1=10 ga.
Each spectrum shows a triplet.
7. Analyze the results as follows:
a. Measure the distance in Hz between the center peak and one of the outer peak
using the cursors.
b. Use the same outer peak (either the one on the right or the one on the left) for
the measurements of both spectra.
The two measurements are used as input for the h2cal command which
calculates the γH2for a given decoupler power level.
8. Enter h2cal to calculate γH2.
9. Record the result and use it during the 13C 90° pulse width test.
1H Observe 90° Pulse Width
1. Install the 1H quarter-wavelength cable.
2. Enter rtp('/vnmr/tests/H1sn') su.
3. Tune the probe on the ethylbenzene sample.
4. Enter pw=5 at=1 lb=1.
5. Obtain the spectrum and adjust the phase for a positive signal.
6. Determine the correct tpwr as follows:
a. Enter tpwr=50 pw=7 ga.
b. Enter aph to phase the spectrum after the acquisition is complete.
c. Setthepw to twicethepw90 specificationfortheprobe andarraytpwr from
48 to 58.
Observe the spectra as it is collected. When the peak of interest passes
through the null and goes negative, the acquisition can be halted by entering
aa. The tpwr value corresponding tothe first negative spectrumshould then
be used for pw90 calibrations.
7. Expand the spectrum so that the quartet is centered on the screen with wp=250.
8. Enter ai.
9. Set vs so that the signal occupies about half the vertical size of the screen.
10. Enter vp=50.
11. Set up the following array for determining the pw90 for a probe:

Dual and Dual Broadband NMR Probes
10 Dual and Dual Broadband NMR Probes Installation 01-999124-00 J 0606
a. Enter r1=xx/5, where xx is the specified pw90 specification for the probe.
b. Enter array('pw',20,r1,r1) to create a pw array covering
approximately 360 degrees of nutation.
12. Enter ga.
13. Enter dssh after the last spectrum.
14. Determine pw form the first minimum.
This is the 180°pulse and the 90°pulse is one-half the 180°pulse.
15. Write the results for each probe in the forms provided in Test Results, page 27.
16. Note the results for use in the 15N sensitivity test.
1H Spinning Resolution & Lineshape
This test measures the 50%, 0.55%, and 0.11% levels of the CHCl3sample. This test and
the 1H spinning sidebands test (the next test) must be passed simultaneously.
1. Put the appropriate CHCl3sample in the probe and spin it.
2. Enter rtp('/vnmr/tests/H1lshp') nt=1 vs=1000 su to set up the
system hardware.
3. Enter a value for pw appropriate for your sample:
4. Enter ga to acquire the spectrum.
5. Phase the spectrum and plot it using wp=250.
6. Normalize the spectrum, enter
vs=10k, and plot the expanded
spectrum.
If floor vibration results in excessive
noisearoundthebaseofthepeak,nt
can be changed to a larger value
(e.g., nt=4 or nt=16); however, if
extreme vibrations are present, it
may be impossible to measure the
lineshape accurately.
7. Measure lineshape as the linewidth
of the CHCl3peak at 50%, 0.55%,
and 0.11% of the main peak
amplitude, refer to Figure 2.
8. Write the results for each probe in the forms provided in Test Results, page 27.
1H Spinning Sidebands
This test and the 1H lineshape test (the previous test) must be passed simultaneously.
1. Using the appropriate CHCl3sample, measure the 1H spinning sidebands on the
same spectrum as 1H lineshape.
Sample (Part No.) Value for pw
1% CHCl3(00-968120-89) 90°pulse
5% CHCl3(00-968120-99) 90°pulse
20% CHCl3(00-968120-76) 20°pulse
Figure 2. 1H Lineshape Spinning
Measurement
H
z
-120-100-80-60-40-20020406080100120
1
40
13C satellite 13C satellite
CHCl3peak
0.11%
0.55%

01-999124-00 J 0606 Dual and Dual Broadband NMR Probes Installation 11
Testing Probes on VnmrS and UNITYINOVA Systems
2. Use the spectra and parameter set from the 1H lineshape test. Plot the spectrum again
using a large enough value of wp to show all the spinning sidebands.
3. Measure spinning sideband amplitudes as a percentage of the main peak.
Spinning sidebands occur at frequency intervals on either side of the central peak
equal to the spinning rate. The sidebands may not be split.
The standard test requires nt=1 or nt=4. Do not repeat the test at nt=16 if the
sideband specification is met at nt=4.
4. Write the results for each probe in the forms provided in Test Results, page 27.
PFG Profile and Recovery
Run these tests for PFG capable probes. The profile test calibrates the G/cm-DAC units for
the user global real-valued parameter gcal.
PFG Profile
1. Insert the 4 Hz D2O/H2O sample and tune the probe.
2. Enter rtp('/vnmr/tests/shmd2o') su.
3. Check the values of tpwr, p1, and pw: p1=1H 90° and pw=2*p1.
4. Enter profile.
5. Enter the appropriate value for gzlvl1:
• Performa I: gzlvl1=250
• Performa II: gzlvl1=4000
6. Enter ga and acquire a spectrum.
7. Enter f full dc vsadj.
A peak (about 16 kHz for Performa I or
about 50 kHz for Performa II) similar to
Figure 3 is displayed.
8. Use the cursors to find the width of this
peak at 20% of the height.
9. Enter setgcal to convert the width of this plateau (delta) and the gradient
strength (gzlvl1) to a gradient strength per DAC value (gcal).
The setgcal macro needs the physical extent of the rf sensitivity region (1.6 cm),
as well as the gradient strength (gzlvl1) and the resulting plateau width (delta).
When the system asks “Set this value?” respond with y.
The value of gcal times the appropriate value below gives the maximum
achievable gradient strength.
• Performa I: gcal ×2048
• Performa II: gcal ×32767
10. Repeat the experiment with gzlvl1 set to oneof the following.The delta should
be equal to that previously measured.
• Performa I: gzlvl1=–250
• Performa II: gzlvl1=–4000
Figure 3. Z-Gradient Profile
Measurement Using 1% Doped D2O
Hz100002000030000400005000060000700008000090000
delta

Dual and Dual Broadband NMR Probes
12 Dual and Dual Broadband NMR Probes Installation 01-999124-00 J 0606
PFG Recovery
1. Enter rtp('/vnmr/tests/grecovery').
2. Enter grecovery.
3. For Performa I, enter at=1 in='n' and set
tpwr and pw for the 90° pulse width.
4. Enter the appropriate value of gzlvl1:
• Performa I: gzlvl1=10/gcal to change
gzlvl1 to a value that equals 10 G/cm.
• Performa II: gzlvl1=30/gcal to change gzlvl1 to a value that equals
30 G/cm.
5. Enter ga to start the acquisition.
6. Enter wft ds(arraydim).
7. Phase the final spectrum, adjust its vertical scale, and enter dssh.
The resulting profile should show a smooth and monotonicrecovery pattern, similar
to Figure 4.
1H Sensitivity
1. Enter rtp('/vnmr/tests/H1sn') su.
2. Insert the ethylbenzene sample.
3. Tune the probe.
4. Determined the pw90 on this sample using
the procedure in 1H Observe 90° Pulse
Width, page 9 or determine the pw90 from
the pw360 and dividing that value by 4.
5. Enter ga to acquire the spectrum.
6. Phase the spectrum and display the quartet,
using the region from the right of the
aromatic peak to the right of the quartet.
7. Use the cursors to locate the best 200-Hz
noise region to the left (downfield) of the
quartet (see Figure 5).
8. Enter dsnmax(200).
The computer calculates the S/N ratio.
9. Answer 'y' to plot the results.
10. Write the results for each probe in the forms provided in Test Results, page 27.
19F Observe 90° Pulse Width
1. Enter rtp('/vnmr/tests/F19sn') su.
2. Insert the trifluorotoluene sample.
3. Tune the probe.
4. Determine the correct tpwr as follows:
a. Enter tpwr=50 pw=7 ga.
b. Enter aph to phase the spectrum after the acquisition is complete.
Figure 4. Gradient Recovery
Pattern Profile
H
z
2000220024002600280030003200340036003800
Figure 5. 1H Sensitivity
Measurement
Quartet
Aromatic
peak

01-999124-00 J 0606 Dual and Dual Broadband NMR Probes Installation 13
Testing Probes on VnmrS and UNITYINOVA Systems
c. Setthepw to twicethepw90 specificationfortheprobe andarraytpwr from
48 to 58.
Observe the spectra as they are being collected. When the peak of interest
passes through the null and goes negative, the acquisition can be halted by
entering aa. The tpwr value corresponding to the first negative spectrum
should then be used for pw90 calibrations.
5. Setup the following array to determine the pw90 for a probe:
a. Enter r1=xx/5, where xx is the specified pw90 specification for the probe.
b. Enter array('pw',20,r1,r1) to create a pw array covering
approximately 360 degrees of nutation.
6. Enter dssh after the last spectrum is obtained.
The first null spectra is the 180°pulse; therefore, the 90°pulse width is one-half the
180°pulse.
7. Write the results for each probe in the forms provided in Test Results, page 27.
19F Sensitivity
1. Enter rtp('/vnmr/tests/F19sn') su.
2. Insert the trifluorotoluene sample.
3. Tune the probe.
4. Set the 19F 90°pulse width as determined in 19F Observe 90° Pulse Width, page 12.
5. Enter ga to acquire the spectrum.
6. Enter dsnmax(200).
The computer calculates the S/N ratio.
7. Answer 'y' to plot the results.
8. Write the results for each probe in the forms provided in Test Results, page 27.
31P Observe 90° Pulse Width
1. Enter rtp('/vnmr/tests/P31sn') su.
2. Insert the triphenylphosphate sample.
3. Tune the probe observe channel without using the filter.
4. Enter gain=50 ga.
5. Phase the spectrum, place the cursor on the 31P resonance, and enter movetof.
6. Determine the correct tpwr as follows:
a. Enter tpwr=50 pw=7 ga.
b. Enter aph to phase the spectrum after the acquisition is completed.
c. Setthepw to twicethepw90 specificationfortheprobe andarraytpwr from
48 to 58.
Observe the spectra as they are being collected. When the peak of interest
passes through the null and goes negative, the acquisition can be halted by
entering aa. The tpwr value corresponding to the first negative spectrum
should then be used for pw90 calibrations.
7. Setup the following array to determine the pw90 for a probe:
a. Enter r1=xx/5, where xx is the specified pw90 specification for the probe.

Dual and Dual Broadband NMR Probes
14 Dual and Dual Broadband NMR Probes Installation 01-999124-00 J 0606
b. Enter array('pw',20,r1,r1) to create a pw array covering
approximately 360 degrees of nutation.
8. Enter dssh after the last spectrum is obtained.
The first null spectra is the 180°pulse and the 90°pulse width is one-half this pulse.
9. Write the results for each probe in the forms provided in Test Results, page 27.
31P Sensitivity
1. Enter rtp('/vnmr/tests/P31sn') su.
2. Insert the triphenylphosphate sample.
3. Tune the probe observe channel without using the filter.
4. Set the 31P 90°pulse width to the value determined in 31P Observe 90° Pulse Width,
page 13.
5. Enter ga.
6. Enter dsnmax(2000).
The computer calculates the S/N ratio.
7. Answer 'y' to plot the results.
8. Write the results for each probe in the forms provided in Test Results, page 27.
13C Observe 90° Pulse Width
1. Enter rtp('/vnmr/tests/C13sn') su.
2. Tune the probe.
3. Change dpwr to 3 or 4 dB below the dpwr of γH2.
4. Enter dm='nny' d1=10 ga.
5. Array dof to set the decoupler frequency on the dioxane 1H resonance.
Optimize the position of the decoupler (dof) to within 0.4 Hz of the correct
frequency to obtain the best possible resolution.
6. Enter pw=5 ga.
7. Adjust the phase for a positive signal.
8. Expand the spectrum so that the signal is centered on the screen with wp=100.
9. Enter ai.
10. Change vs so that the signal occupies about half the vertical size of the screen.
11. Set vp=50.
12. Determine the correct tpwr as follows:
a. Enter tpwr=50 pw=7 ga.
b. After the acquisition is complete, enter aph to phase the spectrum.
c. Setthepw to twicethepw90 specificationfortheprobe andarraytpwr from
48 to 58.
Observe the spectra as they are being collected. When the peak of interest
passes through the null and goes negative, the acquisition can be halted by
entering aa. The tpwr value corresponding to the first negative spectrum
should then be used for pw90 calibrations.
13. Setup the following array to determine the pw90 for a probe:

01-999124-00 J 0606 Dual and Dual Broadband NMR Probes Installation 15
Testing Probes on VnmrS and UNITYINOVA Systems
a. Enter r1=xx/5, where xx is the specified pw90 specification for the probe.
b. Enter array('pw',20,r1,r1) to create a pw array covering
approximately 360 degrees of nutation.
c. Do the following if the sample does not contain 0.2% Cr(acac):
Enter d1=30 ga.
14. Enter dssh after the last spectrum is obtained.
The pw for the first minimum is the 180°pulse and the 90°pulse is half this value.
15. Write the results for each probe in the forms provided in Test Results, page 27.
13C Spinning Resolution & Lineshape
This test measures the 50%, 0.55%, and 0.11% levels of the ASTM sample. This test and
the 13C spinning sidebands test (the next test) must be passed simultaneously.
1. Insert the ASTM sample in the probe and spin it.
2. Enter rtp('/vnmr/tests/C13res') su.
3. Tune the probe.
4. Enter:
• VnmrS and INOVA— nt=1.
•Mercury—nt=4.
5. Set the decoupler modulation to dmm='c' and d1=60.
6. Set the sample spinning rate at 20 ±5 Hz.
7. Change the decoupler power:
• VnmrS and INOVA—dpwr to 30 to 42 dB
•Mercury—dpwr to 3 or 4 dB below the dpwr of γH2.
8. Array dof to set the decoupler frequency on the dioxane 1H resonance.
To obtain the best possible resolution, it may be necessary to optimize the position
of the decoupler (dof) to within 0.4 Hz of the correct frequency.
9. Enter ga to acquire the spectrum.
10. Set dof to the value that produced the best resolution.
11. Enter ga to acquire the spectrum.
12. Plot the spectrum using wp=50.
13. Enter dres to determine the linewidth at 50% of the decoupled peak.
14. Increase vs by 100 times, plot the expanded spectrum, and measure the linewidth at
0.55% and 0.11%.
15. Write the results for each probe in the forms provided in Test Results, page 27.
16. Continue with 13C Spinning Sidebands, page 15.
13C Spinning Sidebands
This test and the 13C spinning resolution and lineshape est (the previous test) must be
passed simultaneously.
1. Measure the 13C spinning sidebands on the same spectrum as 13C lineshape and
resolution.

Dual and Dual Broadband NMR Probes
16 Dual and Dual Broadband NMR Probes Installation 01-999124-00 J 0606
2. Plot the spectrum again using a large enough value of wp to show all the spinning
sidebands, including fourth order.
3. Measure spinning sideband amplitudes as a percentage of the peak.
Spinning sidebands occur at frequency intervals on either side of the central peak
equal to the spinning rate.
The standard test requires nt=1 or nt=4. Do not repeat the test at nt=16 if the
sideband specification is met at nt=4.
4. Write the results for each probe in the forms provided in Test Results, page 27.
13C Sensitivity
The specification for the 13C spinning resolution and lineshape test must be met before
performing this test.
1. Enter rtp('/vnmr/tests/C13sn') su.
2. Tune the probe.
3. Set the 13C 90°pulse width to the value determined in 13C Observe 90° Pulse
Width, page 14.
4. Enter ga.
Wait at least 8 minutes between acquisitions to ensure that the C6D6lines are fully
relaxed.
5. The signal of interest is the highest line of
the C6D6triplet (see Figure 6).
Use the cursors to select the best 1400 Hz
noise region between the dioxane and
benzene peaks.
6. Enter dsnmax(1400).
The computer calculates the S/N ratio.
7. Answer 'y' to plot the results.
8. Write the results for each probe in the forms
provided in Test Results, page 27.
15N Observe 90° Pulse Width
Use this procedure to determine the 15N PW90 value to be used in the 15N sensitivity test.
1. Enter rtp('/vnmr/tests/N15sn') su.
2. Tune the probe observe channel without using the filter.
3. Change dpwr to the 1H γH2value used in the procedure WALTZ 1H Decoupling
Using High-Performance RF Waveform Generator. If a High-Performance RF
Waveform Generator is not present, use the procedure for WALTS 1H Decoupling
Using Pre-programmed Pulse Modulation.
4. Change dmf to 4*γH2.
5. Enter ga.
6. Enter dm='yyy' d1=45 su.
7. Determine the correct tpwr as follows:
a. Enter tpwr=50 pw=7 ga.
Figure 6. 13C Sensitivity
H
z
7000800090001000011000120001300014000
p-Dioxan
e
Benzene-d6

01-999124-00 J 0606 Dual and Dual Broadband NMR Probes Installation 17
Testing Probes on VnmrS and UNITYINOVA Systems
b. Enter aph to phase the spectrum after the acquisition is complete.
c. Setthepw to twicethepw90 specificationfortheprobe andarraytpwr from
48 to 58.
Observe the spectra as they are being collected. When the peak of interest
passes through the null and goes negative, the acquisition can be halted by
entering aa. The tpwr value corresponding to the first negative spectrum
should then be used for pw90 calibrations.
8. Setup the following array to determine the pw90 for a probe:
a. Enter r1=xx/5, where xx is the specified pw90 specification for the probe.
b. Enter array('pw',20,r1,r1) to create a pw array covering
approximately 360 degrees of nutation.
9. When the last spectrum is obtained, enter dssh.
The first null spectra is the 180°pulse; therefore, the 90°pulse width is one half the
180°pulse.
15N Sensitivity
1. Enter rtp('/vnmr/tests/N15sn') nt=1 su.
2. Tune the probe.
3. Setthe 15N 90°pulse width to thevaluedetermined in15N Observe 90° Pulse Width,
page 16.
4. Set dpwr to the 1H γH2value used in the procedure WALTZ 1H Decoupling with
High-Performance RF Waveform Generator. If a High-Performance RF Waveform
Generator is not present, use the procedure for WALTS 1H Decoupling Using Pre-
programmed Pulse Modulation.
5. Change dmf to 4*γH2. Enter ga.
6. Enter dsnmax(100).
The computer calculates the S/N ratio.
7. Answer 'y' to plot the results.
8. Write the results for each probe in the forms provided in Test Results, page 27.

Dual and Dual Broadband NMR Probes
18 Dual and Dual Broadband NMR Probes Installation 01-999124-00 J 0606
Testing Probes on MERCURYplus
This section contains test and calibration procedures for dual (1H/13C) and dual broadband
(1H–19F / 15N–31P) probes on MERCURYplus NMR spectrometers using versions of
VNMR 6.1C or earlier software and versions of VnmrJ with the Classical VNMR interface.
Systems with VnmrJ 2.1B or newer, use the calibration procedures in the VnmrJ
Installation and Administration manual and order of the tests as listed in Table 4.
•How to Test a Probe, this page, lists the standard testing steps.
•Probe Calibration Files, page 18
How to Test a Probe
This section provides the basic steps for testing a probe.
1. Create a probe calibration file as described in Probe Calibration Files, page 18.
2. Follow the test procedures listed in Table 4.
3. After the appropriate tests are completed for the probe, print the corresponding
probe calibration file by entering ACreport in the VNMR input window.
4. Follow the instructions in Setting Up the Solvent-Based Shim Files, page 25 for
configuring solvent-based shims and the setlk macro for proper GLIDE and
automation operation.
Probe Calibration Files
Probe calibration files (in /vnmr/probes) contain pw90, tpwr, dmf, dpwr, and pwx
settings for each probe used with the system. GLIDE, automation, and manual operation
using macros—including h1, hcosy, and dept—retrieve appropriate power levels, the
pw90 value, and the dmf value from the probe calibration file, instead of using preset
values in the parameters files.
Table 4. MERCURY Probe Test Order
Test 200 & 300
Dual 200, 300, 400, Dual Broadband
Probe Calibration Files, page 18 **
1H Spinning Resolution & Lineshape, page 19 **
1H Spinning Sidebands, page 20 **
13C Lineshape Test, page 21 **
1H Observe 90° Pulse Width, page 21 **
19F Observe 90° Pulse Width, page 22 —*
31P Observe 90° Pulse Width, page 22 —*
13C Observe 90° Pulse Width and γH2, page 22 **
1H Sensitivity, page 23 **
19F Sensitivity, page 24 —*
31P Sensitivity, page 24 —*
13C Sensitivity, page 24 **
Setting Up the Solvent-Based Shim Files, page 25 **
Configuring the setlk Macro, page 26 **

01-999124-00 J 0606 Dual and Dual Broadband NMR Probes Installation 19
Testing Probes on MERCURYplus
Successful operation depends on the existence of a probe calibration file for each probe
that is used with the system.
When the MERCURYplus NMR spectrometer is installed,the proper probecalibration files
are set up, so that the system is ready to use when the installer leaves the site. Customers
must update these files regularly to maintain optimal system performance.
The probe calibration files must be created when the system is installed or the first time a
probe is used. Create or change the probe calibration file as follows:
Creating a Probe Calibration File
Perform these steps for each probe that is tested.
1. Log in as vnmr1.
2. Enter the following command in the VNMR input window:
addprobe(probe<,'system'>)
where probe is adescriptive name forthe probe (e.g., addprobe('id5mm') for
an 5-mm indirect detection probe).
The 'system' keyword (e.g., addprobe('id400','system') makes the
probe calibration files for this probe available to all users by placing the files in
/vnmr/probes. Without the keyword, the files are placed in the vnmrsys
directory of the user entering the command (e.g., ~vnmr1/vnmrsys/probes)
and are only available to that user.
The values for power, pw90, dmf, and pp are initially set to 0 and filled in later by
running the calibration procedures for the appropriate nuclei using GLIDE.
Changing to a Different Probe Calibration File
Use this procedure to switch to the appropriate calibration file when a different probe is
installed after a probe is tested and calibrated,.
1. Log in as vnmr1.
2. Enter the following command in the VNMR input window:
probe=probe_dir
Where probe_dir the name of the existing probe directory in /vnmr/probes
named for the new probe (e.g., probe='sw5mm').
1H Spinning Resolution & Lineshape
This test measures the 0.11%, 0.55%, and 50% levels of the CHCl3sample. This and the
1H spinning sidebands test (the next test) must be passed simultaneously and both tests
plotted together.
1. Insert the appropriate CHCl3sample in the magnet and spin it.
2. Enter rtp('/vnmr/tests/H1lshp') nm nt=1 vs=100 su.
3. Tune the probe.
4. Enter a value for pw appropriate for your sample:
Sample (Part No.) Value for pw
1% CHCl3, (00-968120-89) 90° pulse
5% CHCl3, (00-968120-99) 30° pulse
20% CHCl3, (00-968120-76) 20° pulse