Agilent Technologies VARIAN Dual Bedienungsanleitung

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

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:

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