NNR IN RAPIDLY ROTATED METALS By - Nottingham eTheses ...

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-60- circuit was triggered by the leading edge of the preceding pulse. The trailing edge of the resulting pulse then triggered the delay on the next pulse unit, so the total delay time was the sum of the two settings. In this way pulse sequences requiring three pulses could be performed even when the delay time between the first and second pulses was shorter than that between the second and third. Such is the case for the Jeener and Brockaert pulse sequences as described in Sections 5.7 and 5.8. 5.3 VARIABLE TEMPERATURE MEASUREMENTS For measurements other than at room temperature the temperature*of the sample could be controlled using a Bruker B-ST 100/ 700 temperature control system. In this system nitrogen gas is passed through a heat exchanger immersed in liquid nitrogen and then to a glass dewar probe insert via a heater. The temperature of the gas immediately underneath the sample tube in the insert is monitored by a copper-constantan junction connected to the control unit. This automatically adjusts the current td the heat- ing coil so that the temperature of the junction corresponds with that selected. The low temperature measurements on the cuprous halides were performed using a small gas flow cryostat. The assembly shown in Figure 5.2 was supported in a glass dewar in the magnet gap. Although the Bruker control unit was used to adjust the flow of cooling gas the temperature immediately above and below the sample was measured independently via two calibrated copper-constantan thermocouples and a DVM. The lowest temperature was attained by
SCALE 3 cm j Cooling Gas ; tainiess Steel Sample Tube 3affle Plate "'lass Coil Former FIGURE 5.2 : The gas flow cryostat used for cuprous halide measurements
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NNR IN RAPIDLY ROTATED METALS By R.
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I wish to express my thanks to: ACK
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quadrupole relaxation. However theo
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2.3.5 Quadrupole Relaxation 26 (i)
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5.9 Sample Preparation 71 5.9.1 Cup
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1.1 BASIC THEORY -i- CHAPTER 1 INTR
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-3- Transforming to the rotating fr
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-5- lattice and T2 is the spin-spin
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and -7- Vd(t) f(w1)cos w't dw Sao -
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-9- where the terms represent the Z
Page 21 and 22:
- 11 - If rii = nrij = (Xli + X2j +
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- 13 - In powdered samples a weak i
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- 15 - This contact term manifests
Page 27 and 28:
- 17 - where 0 is the angle between
Page 29 and 30: - 19 - termed pseudo-dipolar. It is
Page 31 and 32: - 21 - the non-secular terms of the
Page 33 and 34: - 23 - to the lattice directly via
Page 35 and 36: - 25 - (2.25), can then be assumed
Page 37 and 38: - 27 - quadrupole moments to produc
Page 39 and 40: - 29 - where En are the Zeeman ener
Page 41 and 42: 3.1 INTRODUCTION - 31 - CHAPTER 3 N
Page 43 and 44: Aý T. B a A"T"B " - 33 - It is a g
Page 45 and 46: (-Ur Ho FIGURE 3.1. : Co-ordinate s
Page 47 and 48: D, (t) = 331 2 + 3YI2 sin 2a 4 - 36
Page 49 and 50: - 38 - X (t) = cos a cos ßp + sin
Page 51 and 52: - 40 - 3.7 THE EFFECT OF ROTATION O
Page 53 and 54: - 42 - observations are inconsisten
Page 55 and 56: - 44 - that it apparently offered n
Page 57 and 58: - 46 - bearings suffer from instabi
Page 59 and 60: SI FIGURE 4.1 SCALE il cm : The con
Page 61 and 62: N to 9 . ýC 8 Ü7 Z w D 06 w ax U.
Page 63 and 64: - 50 - The rotors used in this work
Page 65 and 66: Ip IJýi O 1 t - 1 - 1 p OI ý I ý
Page 67 and 68: - 52 - at rotation speeds around 4
Page 69 and 70: - 53 - the manufacture of which was
Page 71 and 72: PTFE Tape_ FIGURE 4.7 rotors SCALE
Page 73 and 74: 4.4.4 COMMENTS - 55 - For completen
Page 75 and 76: Clamp Pf-£-- SECTION II SECTION 11
Page 77 and 78: 5.1 EQUIPMENT - 58 - CHAPTER 5 EXPE
Page 79: - 59 - the range ±1 V are digitise
Page 83 and 84: Trensmitter EXL, FIGURE 5.3 : The s
Page 85 and 86: FIGURE $. 4 s The spectrometer prob
Page 87 and 88: Gas Tuning ransmi tter Input Receiv
Page 89 and 90: - 64 - phase can then be set so tha
Page 91 and 92: -66- The transient nuclear signals
Page 93 and 94: - 68 - 5.7.1 THE SOLID ECHO PULSE S
Page 95 and 96: - 70 - sequence may be repeated. In
Page 97 and 98: a° P/'rvu - 72 - p is the resistiv
Page 99 and 100: - 74 - combined with a low viscosit
Page 101 and 102: 6.2 RESULTS AND DISCUSSION - 76 - A
Page 103 and 104: IC 1 I. FIGURE 6.2 : Measured T1 va
Page 105 and 106: - 78 - TABLE 6.1. DEBYE TEMPERATURE
Page 107 and 108: - 80 - TABLE 6.2. RATIO OF TI VALUE
Page 109 and 110: - 82 - TABLE 6.3. DEPENDENCE OF T1
Page 111 and 112: - 84 - provides further evidence th
Page 113 and 114: - 86 - CHAPTER 7 EXPERIMENTAL RESUL
Page 115 and 116: - 88 - Lorentzian NMR lineshape of
Page 117 and 118: - 90 - at the top with epoxy glue.
Page 119 and 120: - 92 - (c) Bulk Susceptibility Effe
Page 121 and 122: - 94 - aluminium nuclei in the meta
Page 123 and 124: FIGURE 7.1 : 27A1 F. I. Ds and corr
Page 125 and 126: - 97 - TABLE 7.1. COMPUTED SECOND A
Page 127 and 128: - 99 - and Slichter(104) reported t
Page 129 and 130: - 101 - of this value would be requ
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N JL I F- 0 z J I0 0123456789 ROTAT
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-103- results obtained at a tempera
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T10 ms 3. O 2.5 2'C H 1"C o.. v 234
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0 - 106 - CHAPTER 8 MEASUREMENTS ON
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- 108 - process for vanadium the me
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- 109 - in the same way to the prec
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Qv == , 2 28 kHz -111- which is sli
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- 113 - from Cerac Inc. (USA). The
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- 115 - 8.4.3 SPIN-LATTICE RELAXATI
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tv D Xm =o N O Ul- X- z N O FIGURE
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which gives K=0.048 an ± 0.002 - 1
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- 118 - Lifetime broadening alone g
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- 120 - cannot be spun at low tempe
Page 157 and 158:
- 122 - 11. L. E. Orgel, J. Phys. C
Page 159 and 160:
- 124 - 59. P. J. Randall, Ph. D. T
Page 161 and 162:
- 126 - 101. H. R. Khan, J. M. Reyn
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