th  - 1988 - 51st ENC Conference

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- - 206 THE WORLD AND WONDERS OF 3H NMR SPECTROSCOPY: Philip G. /i.lliam:s. ,* National Tritium Labeling Facility, Lawrence Berkeley Laboratory 75-123, mverslty of California, Berkeley, California 94720. The NTLF is a national User Facility, funded by the National Institutes of Health. The Facility combines e availability of high levels of carrier free tritium gas, extensive radiochemical purification resources, and an n-house NMR instrument dedicated to tritium NMR spectroscopy. The NTLF combines its User service unction with core and collaborative research based on the use of hydrogen isotopes. Tritium is an excellent nucleus for NMR observation, but NMR applications in the chemical and biological ciences have been very limited in number. "Onepulse" tritium measurements can quickly and cleanly give the hemical shift and relative abundance of tritons in a sample, and in combination with other physical methods an rapidly assure quality control in labelling experiments. In catalysis hydrogen isotope exchange is readily nonitored, with the relative incorporation at each position of a substrate yielding specificity rules for the atalyst as well as mechanistic detail. Hydrogenation and halogen replacement reactions are the cornerstone of high level tritium labelling procedures. Little is known about concomitant side-reactions, but these are extremely important when specific abelling is required. Observation of tritium NMR peaks from supposedly "unlabelled" positions obviates hese extra mechanisms, and allows the choice of appropriate precursors and reaction conditions for the lesired tritiation. As one example, allylic methyl exchange in the hydrogenation of I]-methyl styrene to yield n- ,ropylbenzene is readily detected, and the full range of isotopomers can be distinguished by J-resolved pectroscopy. Secondly, tritio-dehalogenation of 2-chloro-2'-deoxyadenosine with pure T2 does not give ,roduct with the theoretical specific activity, and factors influencing this "dilution" may be followed. Important and developing uses of tritium NMR spectroscopy include monitoring of the conversion of ntermediates in biological systems, studies of substrate binding, and as an aid in spectral elucidation of proton ~VMR spectra. The use of modern multipulse techniques in concert with simple and elegant older sequences aas the potential for giving a great deal of conformational and coupling information, through the interaction of I-H and 1-H atoms. NMR work at the Tritium Facility is intent on establishing the benefits and problems tssociated with tritium NMR spectroscopy of many diverse substrates - from simple organics to solids and nacromolecules. 202
Page No. ACEVEDO, H F 165 ACKERMAN, J J H 104 ACKERMAN, J L 155 ACKERMAN, J L 53 ADAMY, S 175 ALBRIGHT, M J 126 ALDERMAN, D W 141 ALDERMAN, D W 142 ALDERMAN, D W 141 ALLDRIDGE, N A 189 ALLEN, L 28 ALTOBELLI, S A 184 ANDERSEN, N H 155 ANDERSEN, N H 169 ANDERSON, M E 166 ARAJAN, S 139 ARMITAGE, I M 192 ARNOLD, B R 125 ARORA, S 177 ARUS, C 166 ASHCROFT, J 121 ASHIDA, J 113 AVRAM, H E 152 BACHOVCHIN, W H 38 BAIN, A D 108 BAIN, A D 127 BALASUBRAMANIAM, S 139 BANK, J F 143 BANK, S 143 BARBARA, T M 157 BARKER, G J 190 BARNES, R G 150 BASTI, M M 176 BAX, A 178 BAX, A 36 BAX, A 164 BAZZO, R 137 BECK, B 153 BECKER, N N 104 BEGEMANN, J 152 BEHLING, R W 61 BEHLING, R W 161 BELL, R F 45 BERNARDO, M 197 BIELECKI, T 38 BILDSOE, H 123 BISHOP, K D 146 BLUMICH, B 101 BODENHAUSEN, G 32 BOEHMER, J P 184 BOHLEN, J -M 32 BOLTON, P H 175 BORAH, B 131 BORDIA, R K 129 BORER, P 144 BORER, P 145 BORER, P 143 BORER, P N 146 BORK, V 130 BORNEMANN, V 162 203 BOTHNER-BY, A A BOTHNER-BY, A A BOTTO, R E BOTTO, R E BOUCHARD, D A BOUDREAU, E BOYD, J BOYER, R D BRANDOLINI, A J BRAUER, M BREKKE, T BRENNEMAN, M T BRENNEMAN, M T BRENNERT, G F BREY, W S BRIGGS, R W BRONNIMANN, C E BRONNIMANN, C E BROOKER, H R BROWN, S C BROWN, T R BROWN, T R BRUSCHWEILER, R BRYAN, R N BRYANT, R G BUCHANAN, G W BURNETT, L J BURUM, D P BUSHWELLER, C H BYRD, R A CABASSO, I CARDUNER, K R CARPER, W R CARRADO, K A CARVLIN, M CASTELLINO, S CASTELLINO, S CAU, F CAULEY, B J CAVA, R J CAYLEY, S C CERDAN, S CHACKO, V P CHARI, M CHEN, C-N CHESNICK, A S CHINN, M CHOBANIAN, M CHU, S COCKMAN, M D COFFIN, D B COLE, H B R COLLINS, M J CONWELL, E M COPIE, V CORY, D G COWBURN, D COZINE, M CREUZET, F CROCKETT, B Page No. 165 183 98 191 161 143 137 124 171 183 199 182 182 45 109 189 20 201 153 135 124 123 35 111 149 98 114 105 125 193 103 104 105 191 139 137 136 172 138 45 165 55 129 177 194 162 185 166 132 190 105 180 134 109 193 50 121 185 24 187
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29 th �� - 1988 Rochester
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PROGRAM: This conference program ha
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The Executive Committee of the 29th
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A A 0 0 ,-..1 I Z Z 0 "c N "1" i 0
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Restaurants in Rochester Restaurant
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8:30 a.m. 8:35- 10:05 10:05 - 10:25
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8:30 a.m. 8:35 a.m. 9:05 a.m. 9:15
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f~ I UNTRUNCATIO~I OF DIPOLE-DIPOLE
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MON 9:25 HIGH RESOLUTION ELECTROPHO
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• . r, 10:25 a.m. 10:55 a.m. 11:0
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~'-O-i 0 N i0:55 MEASUREMENTS OF TW
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MON 11:3S 12D CHEMICAL SHIFT ANISOT
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7:30 p.m. 8:00 p.m. 8:10 p.m. 8:40
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HON Eve 8:00 The 13C Relaxation Beh
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THE WORLD AND WONDERS OF 3H NMR SPE
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8:30 a.m. 9:00 a.m. 9:10 a.m. 9:20
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TWO DIMENSIONAL LINEAR PREDICTION N
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TUE 9"20 ] 2D ROTATING FRAME SPECTR
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10:40 a.m. 11:00 a.m. 11:20 a.m. 11
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TUE ii'00 J WATER SUPPRESSION TECHN
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TUE 11:30 J FREQUENCY SWITCHED INVE
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7:30 p.m. 8:00 p.m. 8:30 p.m. 8:50
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• . r T[-~-UE ~ t~ve 8:00! 63,65C
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TUE Eve 8-50 } Cu NQR OF YBa2Cu30 x
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~X [I'IED 8:30 I REMOVAL OF EXTRANE
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. r WED 9:25 ] A STATIC NMR IMAGE O
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WED 9" 45 IFLUID AND SOLID STATE NM
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i MULTIVOLUME SELECTIVE SPECTROSCOP
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[WED 11-10 I SELF SHIELDED GRADIENT
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[WED 11:45 ] ANGIOGRAPHY USING MAGN
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THU 8:30 "TETHERED" BIOLOGICAL SYST
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• / I DYNAMICS OF THE GRAMICIDIN
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I THU 9:40 I NMR STUDIES OF ANTI-SP
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THU 10"2S I NEW TECHNIQUES POR DYNA
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I THU 11 : 05 I DYNAMIC NUCLEAR POL
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THIS SECTION CONTAINS A LISTING OF
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9 ELIMINATION OF PHASE ROLL, SOLVEN
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25 NUCLEAR MAGNETIC RESONANCE STUDI
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~k 41 A HYPO-RELAXATION AGENT; SIMU
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57 STRUCTURAL STUDIES OF LIPIDS IN
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73 THE AUTOMATED NMR LABORATORY; SP
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89 13C NMR ASSIGNMENTS OF DNA OLIGO
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105 EVALUATION OF DOUBLE TUNED CIRC
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121 BROADBAND SPIN DECOUPLING IN TH
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137 TWO-DIMENSIONAL 13C{15N}, 13C{1
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153 NMR CHARACTERIZATION OF THE SOL
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169 SPECTROSCOPY WITH EXACT APODIZA
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185 PARSING THE EDITED 1H NMR SIGNA
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. z 201 THE CORRELATION OF 1H-19F C
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i m 3 I 31p SOLID STATE NMR STUDIES
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CALCULATION OF 2951MAS NMR CHEMICAL
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AN NMR STUDY OF MISCIBLE BLENDS IN
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15 II9F CRAMPS OF INORGANIC FLUORID
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19 I DIPOLARAND SPIN-ROTATION POLAR
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2 3- I A SOLID-STATE 2H and 13C NMR
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27 1 COLLECTION OF PHOSPHORUS-31 NM
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31 DELAYED REFOCUSSING TWO-DIMENSIO
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35 DYNAMIC NUCLEAR POLARIZATION STU
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I 39 2D NMR STUDIES AT 600 MHZ OF A
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43 Coherent Averaging Theory Under
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46 CARBON-13 SPECTRAL ASSIGNMENTS O
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a b 48 SEMUT SPECTRAL EDITING, CALI
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'--- V 5 2 j INTERCONWERSION OF VAL
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[ ~ THE SOURCE OF AN ARTIFACT IN TH
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60 GLUCOSE METABOLISM IN PERFUSED H
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. °- F 64 I MICROSCOPIC IMAGING OF
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68 69 CONFORMATIONAL ANALYSIS via V
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72 I SCUBA, A MAY TOHARDS COMPLETE
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76 NMR CHARACTERIZATION OF THE GLYP
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8o I HIGH RESOLUTION MR IMAGING AT
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A PROBE WITH HIGHER DECOUPLING EFFI
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88 I SOLID STATE ll3cd I~CLEAR }~GE
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- - 92 l CHARACTERIZATION OF NORMAL
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96 AN EVALUATION OF NEW PROCESSING
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. . I00 I NOVEL RESONATOR DESIGNS,
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Page 209 and 210: ZLOTNIK-MAZORIo T ZUMBULYADIS, N Pa
Page 211 and 212: David B. Bailey USI Chemicals Co. 1
Page 213 and 214: Yvan Boulanger Univ de Montreal Ins
Page 215 and 216: Helga Cohen Univ of So Carolina Che
Page 217 and 218: F. David Doty Doty Scientific Inc.
Page 219 and 220: Alan Freyer Pennsylvania State Univ
Page 221 and 222: Gordon Hamer Xerox Research Center-
Page 223 and 224: Timothy Hyman Syracuse University 3
Page 225 and 226: Robert A Kinsey BF Goodrich 9921Bre
Page 227 and 228: Jay J. Listinsky U of Rochester-Dep
Page 229 and 230: Dale Mierke Univ of Calif, San Dieg
Page 231 and 232: Jeanne C Owens Chemistry Dept., '.1
Page 233 and 234: Gade S. Reddy DuPont Experimental S
Page 235 and 236: Charles Schramm Catalytica Assoc. I
Page 237 and 238: Richard F. Sprecher U.S. Dept of En
Page 239 and 240: Steve Unger U. C. Davis NMR Facilit
Page 241: Toni Wirthlin Varian Associates 611
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