Table A.1. Shipping List
Item Quantity Description
1 1 HR-MAS probe
2 3 Zirconia rotors, each rotor including
3 KEL-F rotor caps,
1 pair of rotor spacers (upper and lower part),
1 sealing screw
3 1 Cylinder screw M2(25
4 1 HR spacer tool
5 1 Small screw driver
6 1 Rotor packer (hand tool)
7 1 Screw driver for tuning rods
8 1 Marker pen (black)
9 1 Cap removal assembly
10 1 Repair declaration form
11 1 Installation and Operation Manual.
B. Spherical Inserts B
Important Note: The rotor bore and the spacer must be absolutely clean. The lower spacer will be destroyed if it is removed after being inserted into the bore.
1. Spray the "lower spacer" with coolant spray, or dip it into liquid nitrogen, insert
it slightly into the rotor bore and align the rotor axis (figure B.1).
Figure B.1. Spray lower spacer with coolant spray
a) Spray the spacer a second time with coolant spray and press it com-pletely
into the bore. Apply more coolant spray if needed. (figure B.2) or
b) In the case where the spacer fits very tightly, first dip the rotor and spacer
in liquid nitrogen and let them cool. The spacer can now be inserted much
easier into the rotor (figure B.2)
Figure B.2. Inserting the rotor is now easier
2. Insert the sample into the rotor. Screw the cylinder head screw M2 x25 into the
"upper spacer", but do not tighten it! (figure B.3). Use the screw as a handle.
Spray the "upper spacer" with coolant spray or dip it into liquid nitrogen and
press it completely into the bore. Excessive sample will spill out through the
center hole and the thread.
Figure B.3. Spray upper spacer with coolant spray
3. Put the grub screw on a screwdriver and screw it completely into the upper
spacer. (figure B.4)
Figure B.4. Screw grub screw completely
When the assembly is done correctly, the distance between the end of the upper
spacer and the end of the rotor will be 3mm. The short end of the rotor packer
(K8111001) is 2.9 mm long, which will allow you to easily check for the correct fit.
4. 4) Push the rotor cap (KELF) all the way into the rotor. (figure B.5)
Figure B.5. Push the rotor cap into the rotor.
C. References C
1. H.D.H. St(ver and J.M.J. Fr3/4chet, Macromolecules, 1991, 24, 883
2. J.D. Gross, P.R. Costa, J.B. Dubacq, D.E. Warschawski, P.N. Lirsca, P.F. Devaux and R.G. Griffin, J. Magn. Reson, 1995, 106, 187
3. L. L. Cheng, C. L. Lean, A. Bogdanova, S. C. Wright, Jr., J. L. Ackerman, T. J.Brady and L. Garrido, Magn. Reson. Med. 1996, in press
4. K. Millis, W.E. Maas, S. Singer and D.G. Cory, Magn. Reson. Med. 1997, in press
5. R.C. Anderson, M.A. Jarema, M.J. Shapiro, J.P. Stokes and M. Ziliox, J.Org. Chem. 1995, 60, 2650
6. P. Keifer, L. Baltusis, D.M. Rice, A. Tymiak and J.N. Shoolery, J. Magn. Reson. 1996, A119, 65
7. S. K. Sarkar, R.S. Garigipati, J.L. Adams and P.A. Keifer, J. Am. Chem. Soc. 1996, 118, 2305
8. A.N. Garroway, J. Magn. Reson. 1982, 49, 168
9. A. Sodickson and D.G. Cory, submitted to J. Magn. Reson.
10. W.E. Maas, F.H. Laukien and D.G. Cory, J. Am. Chem. Soc. 1996, 118, 13085
11. R.E. Hurd and B.K. John, J. Magn. Reson. 1991, 91, 648
12. W.E. Maas, F.H. Laukien and D.G. Cory, J. Am. Chem. Soc. 1996, 118, 13085
13. M. Piotto, V. Saudek and V. Sklenar, J. Biomol.NMR 1992, 2, 661
14. P.C.M van Zijl and C.T.W. Moonen, J. Magn. Reson. 1990, 87, 18
15. High Resolution MAS Spectroscopy 27.
Figures
1 Introduction
Figure 1.1. 500 MHz proton spectra of a human Lipoma tissue.
2 System Description
Figure 2.1. Upper probe chamber with MAS stator in magic angle position.
3 Installation of the Probe and Peripherals
Figure 3.1. Pneumatic connections of the HR-MAS probe
Figure 3.2. Diagram for the pneumatic connections for operation at ambient temperature.
Figure 3.3. Set-up for low-temperature operation
Figure 3.4. Installation of the MAS sample changer.
4 Operation of the HR-MAS System
Figure 4.1. Zirconia rotor with Kel-F cap, upper spacer, cylinder head screw
Figure 4.2. Schematic drawing of the rotor with spherical insert.Figure 4.3. Schematic drawing of the cap removal tool.
Figure 4.4. MAS pneumatic unit control window.
5 Preparing the Probe for Experiments
Figure 5.1. Proton NMR spectra of BaClO3H2O
Figure 5.2. 79 Br FID's KBr.
Figure 5.3. 79 Br NMR spectra corresponding to the FID's shown in figure 5.2.
Figure 5.4. The magic angle spinner axis
Figure 5.5. Proton spectra of a plant leaf
6 Gradient HR-MAS Spectroscopy
Figure 6.1. Use of a z-gradient in MAS spectroscopy
Figure 6.2. Gradient field is directed along the magic angle spinner axis
Figure 6.3. Pre-emphasis controller window.
Figure 6.4. 8 consecutive FID's
Figure 6.5. Gradient profile for a spherical sample of water.
7 Application Examples 31
Figure 7.1. 1H hr-MAS NMR spectrum of small organic molecules
Figure 7.2. Comparison of proton spectra
Figure 7.3. Figure 23: 400 MHz proton spectra of a single 100 m bead .
Figure 7.4. 2D J-resolved proton spectrum of 2 mg sample on a Tentagel resin
Figure 7.5. Double Quantum filtered Cosy of a small organic molecule
Figure 7.6. Hr-MAS spectra of TLC-plate spots.
Figure 7.7. 500 MHz proton (top) and carbon (bottom) spectra
Figure 7.8. 2D TOCSY/ hr-MAS spectrum of orange peel,
Figure 7.9. 8 mg red perch filet, cut, flushed and measured in D 2 O.
Figure 7.10. Hr-MAS of benign versus malignant human prostate tissue .
Figure 7.11. TOCSY-presat of a living white worm (enchytraed) in 95% H 2 O/ 5% D 2 O.
Figure 7.12. Gradient COSY of a swollen Wang resin
Figure 7.13. 400 MHz 1 H-13 C HMQC spectra of an N-FMOC-N-Boc-L-Lysine
Figure 7.14. 400 MHz 1 H-13 C HMBC spectra of an N-FMOC-N-Boc-L-Lysine
Figure 7.15. 500 MHz 1 H-13 C Gradient hr-MAS HMBC spectrum
Figure 7.16. 500 MHz single pulse proton spectrum of an acrylamide hydro-gel
Figure 7.17. 500 MHz proton spectra of human high grade Pleiomorphic 43
Figure 7.18. 500 MHz STE diffusion spectra .
Figure 7.19. 500 MHz STE proton spectrum (top) and single pulse spectrum
A Shipping List
B Spherical Inserts
Figure B.1. Spray lower spacer with coolant spray
Figure B.2. Inserting the rotor is now easier
Figure B.3. Spray upper spacer with coolant spray
Figure B.4. Screw grub screw completely
Figure B.5. Push the rotor cap into the rotor
C References
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