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: