Anal. Chem. lB82, 5 4 , 125R-131R (115) Solomon, T. Top. App/. Pbys. 1979, 36, 189-213. (116) Knights, J. C.; Lucovsky, G. CRC Crit. Rev. Solid State Mater. Sci. 1980, 9, 211-83. (117) Well, J. A. Hyperfine Mefact. 1981, 6 , 371-4.
(118) Bacquet, G.; Dugas, J. “Solid Electrolytes”; Hagenmuller, P.,Van Oool, W., Eds; Academic Pres: New York, 1978; pp 109-122. (119) Richards, P. M. Top. Curr. Phys. 1979, 75, 141-74. (120) Bjorkstam, J. L.; Villa, M. Magn. Reson. Rev. 1980, 6 , 1-57.
Nuclear Malgnetic Resonance Spectrometry John R. Wasson’ Kings Mountain Specialties, Inc., P.O. Box
I 173, Kings Mountain, North Carolina
28086
The books (2-,36a)on NMR spectrometry range from those containing introductory discussions to those dealing with state-of-the-art developments. The growth in other-thanproton spectroscopy and significant applications in polymer and medical areas are also reflected in the number of review articles. Table 1. lists review articles. For convenience, the references in Table I are collected separately in the bibliography.
Modification of the INEPT sequence enables application of the sequence to two-dimensional NMR and provides a simplified form of two-dimensional 13C J spectroscopy (52). Three-dimensional NMR imaging by Fourier reconstruction zeugmatography has been described (53). Reduction of spurious base line effects in broad line NMR has been discussed and a simple circuit to reduce them by a factor of 300 presented (54). A new noise-reduction filter has been described (55)which is capable of reducing the noise considerably and keeping the line width in the spectrum practically constant. A simple method for detection of zero-quantum transitions has been reported (56). A procedure has been described for obtaining absorption mode spin-echo NMR spectra of large molecules (57). A computer program has been described for the determination of diffusion coefficients from field-gradient spin-echo data (58). The reviews listed in Table I afford additional references to instrumental and technique developments.
APPARATUS AND TECHNIQUES
SPECTRAL ANALYSIS
Purification of chloroform for NMR can be achieved by using molecular sieves (37). A correction has been given to the static tube method for determination of magnetic susceptibilities of solutes in solution (38). Use of internal and external references in determinations of weak molecular complexes has been evaluated (39). Calibration of methanol and ethylene glycol thermometers has been verified and extended (40). A Mg-AT]? thermometer for 31PNMR studies of biological systems which is based on the temperature dependence of the chemical shift difference between the a P and p P resonances in neutral pH solutions of Mg-ATP has been reported (41). Am equinnolar solution of P h 3 P 0 and Ph3P in toluenedBhas been proposed as a thermometric system for 31Pdynamic studies (42). A method for temperature determination using the clearing point of liquid crystals has been recommended (43). A sensitive 59C0NMR thermometer for multinuclei FT-NMR has been described (44). Phosphorus-31NMR measurements with small surface coils have been used to observe phosphorus metabolism of perfused hearts within localized regions. The method allows for direct, noninvasive, sequential assessment of the altered regional metabolism resulting from myocardial infarction and response to drug treatment, which cannot be examined by conventional techniques (45). A simple, fast recovery, low-noise receiver amplifier for pulsed NMR experiments has been reported (46) as has a high-performance cryogenic pulsed spectrometer (47). Use of a commercial waveform analyzer in a pulse FT-NMR system (48) and a versatile pulse sequence generator for pulse NMR (49)have been described as has a heating element for a furnace that can work in an 8-T field of a superconducting magnet at temperatures up to 2200 K (50). A microprocessor-based device has been described (51) for controlling magnetic field gradients in three dimensions, including the design logic, the interface to a minicomputer and a NMR spectrometer, and the mathematical basis for a two-stage reconstruction method that may be used with the controller.
Estimation of errors in eigenvectors and eigenvalues from magnetic resonance results by use of linear data-fitting techniques has been refined (59). Both transient and steady-state expressions have been developed for X3-(A) Overhauser studies (60). Separation of the different orders of multiple-quantum transitions by use of pulsed field gradients has been described (61). The explicit analysis of zero quantum transition (ZQT) NMR for weakly coupled homonuclear spin systems has been given (62) as has a treatment of second-order dynamic frequency shifts in the spectra of spin 3/2 nuclei (63) and the theory of multiple quantum double resonance (64). A powerful method for computing NMR (and slow motional ESR) spectra has been developed by using the Lanczos algorithm modified to tridiagonalize complex symmetric matrices (65). An efficient method of simulating NMR line shapes of rigid multiproton molecules has been described (66). A data base of about 4000 13C NMR spectra has become available (67). A low cost data system has been reported which can be connected to existing spectrometers. Software and BASIC programs are idso described (68).Computer programs for interpreting and predicting 13C NMR spectra have been described (69). A computer progran, ASREY, has been developed for the analysis of spectra on a minicomputer (70). A possible mathematical model has been offered for the correlation tables used in spectroscopy (71). Reasons for the occasional failure of convergence of the LAOCOON 3 program have been discussed (7’2)as had error analysis in LAOCooN-like interative programs (73). A proposal has been made to overcome the methodical problem of additional unspecific shielding in studies of A + D AD reactions where D is an aromatic molecule (74). Density matrix theory of ABC ==AB’ C’ chemical exchange (75) and chemical shift equivalence and magnetic equivalence in conformationally mobile molecules (76)have been discussed. Analytical expressions have been given for magnetic resonance line shapes of powder samples with axially symmetric Hamiltonians (77). A semiempirical theory of boron chemical shifts using gauge-invariant atomic orbitals has been presented (78) as has simplex optimized INDO calculation of 13C chemical
This review covers thie published literature from July 1979 to July 1981 althou h a few references to other work are also included, As note in earlier reviews ( I ) the volume of literature published is imlpossible to summarize in such a short space. However, it is hoped that where this review fails as a review, it succeeds in capturing the flavor of this dynamic research area and serves as a useful guide to the applications and literature on NMFL spectrometry.
f
BOOKS AND REVIEWS
For biographical material, see the review on electron spin resonance.
0003-2700/82/0354125R$06.00/0 0 1982 American Chemical Society
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NUCLEAR MAGNETIC RESONANCE SPECTROMETRY
Table I. Reviews ref group theory and NMR nuclear shielding charge distributions in molecular systems ring current theories nuclear spin-spin coupling applications of the chemical shift solvent effects-quantum chemical aspects CIDNP CIDNP-novel aspects topical NMR applications of computers equilibration rates fast kinetics kinetic and mechanistic evaluation of NMR spectra kinetic studies-stopped-flow FT NMR nuclear spin relaxation in fluids field cycling in NMR relaxation spectroscopy spinecho F T NMR spin decoupling methods in 13CNMR sensitivity optimization high-performance large sample probe for the XL-1OC-15 spectrometer two-dimensional FT l3C NMR new pulsed excitation methods high-resolution 13CNMR of solid polymers new techniques in I3C NMR multiple magnetic resonance multiple-pulse NMR relaxation processes in multipulse NMR multiple-quantum NMR FT NMR FT NMR digitization and data processing two-dimensional FT NMR carbanions and carbocations carbocations alkali ion pairs of carbanions and nitroanions intermolecular interactions and intramolecular dynamics molecular conformation and conformational equilibrium-lanthanide probes sterodynamics of small molecules J method determination of small internal rotational barriers in solution conformational analysis partially oriented molecules in conforma. tional studies oriented molecules liquid crystals and micellar solutions one-bond C-C spin-spin coupling constants-data summary structure and I5N coupling constants I3C NMR-nonaromatic heterocyclic compounds nitrogen hetero~ycles-'~CNMR IH NMR acridizinium adducts complexation of synthetic macrocyclicmultidentate compounds with primary alkylammonium salts crown and cryptand complexes diamagnetic porphyrins organic single crystal~-'~Cchemical shift tensors water -f ood water in biological systems postmortem changes in meat 'H NMR-carbohydrate structures food-related disaccharides and trisaccharides
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1
2 3 4 5, 6 7, 8
9
10 11
12 13
14 15 16
17
18,19 20 21 22 23 24 25 26 27 28 29-31 32 33
34 35 36 37 38 39 40 41 42 43 44 45,46 47 48,49 50, 5 1 52 53 54 55 56 57 58
59 60 61
62 63 64 65
ANALYTICAL CHEMISTRY, VOL. 54, NO. 5, APRIL 1982,
ref sucrose analysis Agar-type polysaccharides isotopically enriched carbohydrates-13C NMR poly~accharides-~~C NMR carbohydrates fungal polysaccharides fiber science natural macromolecules natural p r o d u ~ t s - ~ ~NMR C alkaloids vitamin D, isomers NMR studies of heparins A and B aminoglycoside antibiotics catalytic groups of serine proteinases relaxation-geometry of enzyme bound substrates and analogues enzyme kinetics glutamine synthetase drug metabolism metabolism metabolite biosynthesis metabolic studies metabolic studies-lJC NMR blood membranes paramagnetic probes in membrane enzymes dynamics and mesophase structure of membrane lipids phospholipid bilayer membrane "C NMR-hormone structure and function intact cells and ti~sue--'~C NMR intact biological systems spin imaging NMR imaging-human body applications pulse FT NMR-redox proteins 19FNMR of proteins high field and photo-CIDNP-biological molecules ODMR-proteins and carcinogen-DNA adducts organisms and compounds of unnatural isotopic composition 170NMR-biological applications oriented systems in biochemistry and biophysics biopolymerssolid-state NMR high field spectroscopy of biological systems medical diagnosis clinical medicine metalloproteins paramagnetic broadening probes in biochemistry proton relaxation enhancement in biochemistry liquid binding binding and release of cations of biomolecules binary complexes of mono- and polynucleotides with metal ions tracing the fate of hydrogen in biosynthesis solution structure of proteins conformational mobility of proteins protein molecules-flexibility-2dimensional NMR conformation and interaction of peptides and proteins in solution nucleoside conformational properties molecular orientation in low density lipoproteins peptides-multinuclear NMR proton exchange and nucleic acids tRNA structure nucleotide conformational analysi~--~'PNMR phosphoryl transfer enzymes and metal nucleic of metalloproteins biological 3LPNMR
66 67 68 69,70 71,72 73 74
75,76 77,78 79 80 81
82 83
84 85 86 87 88 89
90 91 93 94-96 97 98 99 100 101 102,103 104 105 106 107 108
109 110 111
112 113 114 115 116
117 118
119
120 121 122 123 124, 125 126 127 128 129 130 131
132 133 134 135 136
NUCLEAR MAGNETIC RESONANCE SPECTROMETRY
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Table I (Continued) ref 31PNMR-nucleic acids and proteins 31PNMR saturation transfer nieasuremen ts of creatine kinase kinetics cellular applications of 31Pand I3C NMR cells, tissues, and ~rganelles-~~P NMR intact t i s s ~ e - ~ l PNMR 31PNMR perPused organs whole animals and humans-metabolic ~tudies-'~P NMR, synthetic podymers in dilute solution polycyclic aromatic compo~nds--'~C NMR shale oil cormponent/type analysis solid coals-pulse and multiple pulse NMR petroleum, oil shale, coal, petrochemicals, and polymers cross-polarization 13CNMR-magic angle spinning-fossil fuels and polymers I3C NMR-structure in hydrocarbon polymers high-resolution I3C NMR of bulk polymers copolymer characteri~ation-~~C NMR solid polymers long chain polymers-radiation effectspulsed NMR radiation effects in polymers-pulsed NMR interfacial effects on the NMR of composite polymers composite polymeric systems-pulsed NMR poly mer s chemical shift calculationsstereochemical structures of synthetic polymers organics the strongest type of hydrogen bonds inorganic and organometallic compounds silicon-29 NMR nitrogen NMR-inorganic, organometallic, and bioinorganic chemsitry oxygen-17 NMR metal ion NMR in coordination chemistry chemical shifts of nucleic of inorganic compounds less common quadrupolar nuclei paramagnetic species shift reagents and paramagnetic lanthanide complexes organo-transition metal complexesI3C NMR
13'7 138 139 140 141, 142 143 144 145 146 147 148 149 150 151 152 153 154 155 156 157 158 159,161 162 163,164 165 166-168 169,170 171 172 17 3 174 175 176,177 178 179
ref intermolecular exchange-organometallics organoiron compounds boranes, carboranes, and heteroatom borames I3C NMR of boron compounds oxygen NMR-characteristic parameters and applications platinum chemistry-multinuclear NMR approach platinum catalysts 31PNMR-catalytic systems containing rhodium complexes of' chelating diphosphines polyphosphine complexles of heavy metals transition metal-phosphorus chelate complexes metal colloids in ionic crystals solid electrolytes and solid solution electrodes superionic conductors NMR in chemistry NMR at high pressure two-dimensional NMR automation and control in high power pulsed NMIZ rare earth metals rare-earth metals, alloys, and compounds rare earth complexes-theory enhanced NMR in rare earths organometallic compounds of the f-elements uranocenes dioxouranium(V1) ion in nonaqueous solution impurity bands lamellar intercalation compounds surface properties and absorbed phases adsorption at liquid/liquid interfaces molecules physisorbed o n homogeneous surfaces chemical kinetics in adsorption systems micellaw interactions and catalysis high-resolution dipolar NMR spectra in solids magic-angle spinning in solid-state NMR I3C NMR and 15NNMR im solids dipolar oscillations and plhase interferom etory-solids pulsed NMR in solids high-resolution NMR in solids solid state heterogeneous systems table of NMR/ON experiments NMR/ON spin-glass dynamics nuclear orientation in solid-state physics librational modes of crystal water
180 181 182 183 184 185 186 187 188 189 190 191 192,193 194 195 196,197 198 199 200 201 202 203 204 205 206 207 208 209 2 10 211 212 213 214 215 216 217,218 219 220,222 223 224 225,226 227, 228 229 230
-shifts in hydrocarbons (79). The ultrafine second-order dynamic frequency shifts of single quantum coherence for the grouping of three identical spin nuclei have been calculated explicitly. Determination of reorientation correlation times for various interaction strengths and modulation anisotropies from simple line breadth ar uments may lead to significant errors (80). Assignment of 15C-13C couplings using DANTE excitation has been deslcribed (81) for the tracing of intact acetate units where the similarity of carbon environments gives rise to several IJ(CC) of the same magnitude.
ANAI,YTIC!AL APPLICATIONS The characterization of chemical or biological samples by multidimensional data followed by appropriate data analysis provides a means for the quantitative classification of new samples. Examples of this approach have been provided (82). Low-resolution '€3 NMFL affords a rapid and accurate technique for the determination of moisture in coal and of total
solids in aqueous coal slurries (83). Protein can be determined by using a pulsed NMR spectrometer in conjuction with a copper relaxation agent. The response to protein depends on the type of protein (84). MeC6H4R (R = CH,OH, CHzNHz, CONHz, C02Me) isomers can be estimated quantitatively by using IH NMR and Eu(fod) shift reagent (85). A simple and relatively fast method for determining primary, secondary, and tertiary amines by lH NMR is based on the addition of trifluoroacetic acid to the sample to convert the amines to their salts (86). A simple application of IH NMR allows determination of free Fe(1II) present in Fe(II1)-soil fulvic acid complexes and also gives the possibility of deducing the number of milligrams of bound metal ion per gram of fulvic acid (87). A process for rapid identification of polymers which employs structure-sensitive IR spectrum bands and NMR data has been described (88). Optimum conditions for crude oil and petroleum product analysis by lSCNMR have been determined (89) as have the optimum conditions for quantitative ANALYTICAL CHEMISTRY, VOL. 54, NO. 5, APRIL 1982
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NUCLEAR MAGNETIC RESONANCE SPECTROMETRY
Table 11. Analytical Applications ref phosphorus compounds in solution by 31PFT NMR a technique for measuring 30,in organic solvents degree of cure of photopolymers DL-amino acid enantiomers assay of P-lactamase protein determination in solids carboxymethylcellulose seed oil carvone in caraway and dill oils conjugated trienoic acid containing oil-l3C NMR simultaneous determination of vitamins B, and B, condrillasterol--'H NMR stilbestrol and some of its pharmaceutical preparations assay of methimazole sodium amobarbital and sodium se~obarbital--'~C NMR 0 3 and - O6-monacetylmorphinein heroin tests enantiomorphic composition of cocaine eodeine and codeine phosphate as well as detection and possible determination of morphine trimipramine maleate isoniazid nalidixic acid caffeine--" NMR griseofulvin nikethamide citric acid in mixtures assay of khellin and simultaneous detection and determination of visnagin methyl salicylate as a drug entity and in wintergreen oil rubber content in guayule bu~hes--'~C NMR crude oil and petroleum productsquantitative NMR and 'H NMR oligomer analysis of epoxy resins CY,CY,OI ,2,4-pentachlorotoluene n-butyllithium in hexane whole soils-cross polarization NMR
1 2 3 4 5 6 7
8 9 10
11 12
13
14 15 16 17
18 19
20 21 22 23
24 25 26 27
28 29 30 31 32 33
analysis by 13C NMR (90). A novel I3C NMR method for determining acidities of weak carbon acids (91) and fast searching for identical 13CNMR spectra via inverted files (92) have been described. 13C NMR in methanol containing 0toluidine as an internal standard can be employed for the quantitative analysis of mixtures of cresols (93). A simple excitation sequence usable with conventional spectrometers has been developed (94) for identifying with high precision and sensitivit quaternary, CH, CHz, and methyl carbon signals in the %C NMR of large molecules. A survey of 13C chemical shifts of aromatic hydrocarbons has been used to derive an assignment scheme which should be applicable to the majority of coal-derived materials as well as crude oils and aromatic resins (95). The displacement of 13C NMR shifts of aliphatic and alicyclic alcohols in carbon tetrachloride on addition of trifluoroacetic acid has been examined and found useful in estimating alcohol basicities (96) among other applications. 'H NMR and 13CNMR of supercritical-gas extracts of coals (96) and butylated coals (98) have been described as has the characterization of coal h drogenation products (99). Solid-state natural abundance C NMR of the major coat protein of phage fd were obtained (100) by proton-enhanced NMR and magic angle sample spinning. lP NMR of free magnesium ion, Mg-ATP, and Mg-ADP in intact Ehrlich ascites tumor cells has been described (101). Cross-polarization, ma ic angle 13CNMR of poly(p-phenylene) oligomers (102) and KH NMR data on 15 A-type and 3 k-type BenceJones proteins (103) have been reported. On the addition of L n ( f ~ d(Ln ) ~ = La Pr, Nd, Sm, and Eu) to a benzene solution of Al(acac)3 the hAl resonance lines due to the free and complexed A l ( a ~ a chave ) ~ separately been observed at 25 OC; the chemical exchange is slow on the NMR time scale and the separation of paramagnetic shifts into contact and pseudocontanct contributions implies a fairly large contact contribution and that the hyperfine splitting constant of the alu-
v
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ANALYTICAL CHEMISTRY, VOL. 54, NO. 5, APRIL 1982
minum nucleus is positive (104). A number of analytical applications of NMR are collected in Table 11; for convenience, the references for Table I1 are collected separately in the bibliography.
ACKNOWLEDGMENT The author is grateful to Linda B. Thomas for preparational assistance and to R. 0. Bach and J. Trull, Lithium Corporation of America, for use of library facilities. LITERATURE CITED (1) Wasson, J. R.; Salinas, J. E. Anal. Chern. 1980, 52, 90R-95R. (2) Silverstein, R. M.; Bassler, G. C.; Morrill, T. C. "Spectrometric Identification of Organlc Compounds", 4th ed.; Wiley: New York, 1981. (3) Bates, R. 6.; Beavers, W. A. "Carbon-I3 NMR Spectral Problems"; Humana: Clifton, NJ, 1981. (4) Kaufman, L., Crooks, L. E., Marguils, A. R., Eds. "Nuclear Magnetic Resonance Imaging in Medlcine", Igaku-Shoin: New York, 1981. (5) Fukushima, E.; Roeder, S.8. W. "Experimental Pulse NMR. A Nuts and Bolts Approach"; Addison-Wesley: Reading, MA, 1981. (6) Webb, G. A., Ed. "Annual Reports on NMR Spectroscopy"; Academic Press: New York, 1979; Vol. 9. (7) Simons, W. W. "The Sadtler Handbook of Proton NMR Spectra"; Sadtier Research Laboratories: Phiiadelphla, PA, 1978. (8) Beach, L. B., Ed. "Selected Carbon-I3 NMR Spectral Data, Supplementary Vol. No. G10"; Texas A&M Thermodynamics Research Center: College Statlon, TX, 1980. (9) Webb, G. A., Ed. "Annual Reports on NMR Spectroscopy"; Academic Press: New York, 1980; Vol. 10A. (10) Pham Quang Tho; Petiaud, R. "Proton and Carbon NMR Spectra of Polymers"; Heyden: Philadelphia, PA, 1981; Vol. 1. (11) Smidt, J.; Wlsman, W. H. "Proceedings of the Joint ISMAR-AMPERE International Conference on Magnetic Resonance, Delft, 1980"; Franklin Instltute Press: Philadelphia, PA, 1981. (12) Bertini, I.; Drago, R. S. "ESR and NMR of Paramagnetic Species in Biological and Related Systems"; Kluwer Boston Inc.: Hingham, MA, 1960. (13) Kaplan, J. I.;Fraenkel, G. "NMR of Chemlcally Exchanglng Systems"; Academic Press: New York, 1980. (14) Becker, E. D. "High Resolution NMR: Theory and Chemical Appllcatlons", 2nd edn.; Academic Press: New York, 1980. (15) Levy, G. C., Ed. "Topics In Carbon-I3 NMR Spectroscopy"; Wiley: New York, 1979; Vol. 3. (16) Pregosin, P. S.;Kunz, R. W. "Phosphorus-31 and Carbon-13 NMR of Transition Metal Phosphlne Complexes"; Springer-Veriag: Berlin, 1979. (17) Levy, 0. C.; Lichter, R. L. "Nitrogen-15 Nuclear Magnetic Resonance Spectroscopy"; Wiley: New York, 1979. (18) Beach, L. B., Ed. "Selected Carbon-13 Nuclear Magnetic Resonance Spectral Data, Supplementary Voi. No. G-9"; Texas A&M University, College Station, TX, 1980. (19) Berliner, L. J., Reuben, J., Eds. "Biological Magnetic Resonance"; Plenum Press: New York, 1980; Vol. 2. (20) Levy, G. C.; Lichter, R. L.; Nelson, G. L. "Carbon-I3 Nuclear Magnetic Resonance Spectroscopy", 2nd ed.; Wiley: New York, 1980. (21) Guenther, H. "NMR Spectroscopy: An Introduction"; Wiley: New York, 1980. (22) Shulman, R. G., Ed. "Biological Applications of Magnetic Resonance"; Academic Press: New York, 1979. (23) Fraissard, J. P., Resing, H. A,, Eds. "Magnetic Resonance in Colloid and Interface Sclence", Reidel: Boston, MA, 1980; NATO Adv. Study Inst. Series C, Vol. 61. (24) Woodward, A. E., Bovey, F. A., Eds. "Polymer Characterization by ESR and NMR"; American Chemical Society: Washington, DC, 1980. (25) Cohen, J., Ed. "Magnetic Resonance in Biology"; Wiley: New York, 1980: Vol. 1. (26) Bievard, C.; Granger, P. "Handbook of High Resolution Multinuclear NMR"; Wiley: New York, 1981. (27) Pasika, W. M., Ed. "Carbon-I3 NMR in Polymer Science"; American Chemical Society: Washington, DC, 1979. (28) Opella, S. J., Lu, P., Eds. "NMR and Biochemistry"; Dekker: New York, 1979. (29) Abraham, R. J., Ed. "Specialist Periodical Report: Nuclear Magnetic Resonance"; The Chemical Society: London, 1979; Vol. 8. (30) Webb, G. A,, Ed. "Annual Reports on NMR Spectroscopy"; Academic Press: London, 1980; Vol. IOB. (31) Cooper, J. W. "Spectroscoplc Techniques for Organic Chemists"; WIley: New York, 1980. (32) Mccausiand, M. A. H.; Mackenzie, J. S. "Nuclear Magnetlc Resonance In Rare Earth Metals"; Taylor and Francis Ltd.: London, 1980. (33) "Carbon-I3 NMR of Monomers and Polymers"; Sadtler Research Laboratories: Philadelphia, PA, 1979; Vol. 1. (34) Conti, F., Ed. "Proceedings of European Conference on NMR on Macromolecules, Sassari, Sardinia May 8-1 1, 1978"; Lerici: Rome, 1978. (35) Martin, M. L.; Martin, G.; Deipuech, J. J. "Practlcal NMR Spectroscopy"; Heyden & Son, Inc.: Philadelphia, PA, 1979. (36) Martin, G. J.; Martin, M. L.; Gouesnard, J.-P. "NMR, Basic Principles and Progress. Vol. 18: Nitrogen-I5 NMR Spectroscopy"; Springer-Verlag: New York, 1981. (36a) Mann, B. E.; Taylor, 8. F. "13C NMR Data for Organometallic Compounds"; Academic Press: New York. 1981. (37) Burfield, D. R. J . Chern. Educ. 1979, 56, 486. (38) Orrell, K. G.; Sik, V. Anal. Chem. 1980, 52, 567-9.
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(230) Tayal, V. P.; Srivastava, B. K.; Khandelwal, D. P.; Bist, H. D. Appl. Spectrosc. Retv. 1980, 76, 43-134. LITERATURE FOll TABLE 11
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Molecular Fluorescence, Phosphorescence, and Chemiluminescence Spectrometry E. L. Wehry Department of Chemistry, University of Tennessee, Knoxville, Tennessee 37996
As in the previous review in this series (AI), this survey stresses advances in the techniques of luminescence spectrometry and in instrumentation related to present or potential analytical lumiinescence methods. Applications are cited only when they seem particularly novel to this reviewer. The review, prepared with the assistance of a computer search profile of Chemical Ab:rtracts titles and identifiers prepared locally, covers literature indexed by Chemical Abstracts from December 1979 Wol. 91, issue 23) through October 1981 (Vol. 95, issue 20). Many journals scanned manually by the author are covered up through issues received by November 30,1981. As in the previous review, certain topics are excluded; for example, virtually all publications concerning atomic fluorescence, moleculiilr luminescence in flames, X-ray fluorescence, solid-state phosphor and semiconductor luminescence (both organic and inorganic), radioluminescence, liquid scintillation counting, and photosynthesis and solar energy conversion have been excluded. Papers dealing with 0003-2700/82/ 0354- 13 1 R$OS.OO/O
luminescence detection in liquid, thin-layer, or paper chromatography ai*e cited only when they appear to be of uppreciable spectroscopic interest. The immense literature on fluorescent probing of macromolecular and micellar systems, much of which could quite properly be subsumed in the rubric of‘ “analytical chemistry”, has been excluded almost totally except for citation of a few general reviews. Certain other subject matter areas, noted in the appropriate sections of the review, are covered in a highly arbitrary manner. The literature related to luminescence analysis continues to expand rapidly. For example, I estimate that 14% of the full papers published in Analytical Chemistry in 1981 could have qualified for inclusion in this review on the basis of their subject-matter coverage! Thus, to keep the number of references and length of the review from becoming unduly preposterous, a great deal of arbitrary exclusion of interesting work was necessary. I apologize to those authors whose work has been slighted. 0 1982 Amerlcan Chemical Society
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