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1992[X]
41Author    Li Pang, E.A C Lucken, P. TissotRequires cookie*
 Title    An NQR and Calorimetric Study of a Phase Transition in tetrakis (a-Phenylethylamine)-bis (isothiocyanato) nickel (II) / örf/ftf-Dichlorobenzene Clathrate  
 Abstract    The 35 C1 NQR spectrum of ortho-dichlorobenzene as a guest molecule in tetrakis(x-phQny\ethy\-amine)-6i's(isothiocyanato)nickel(II), has been studied in the temperature range of 77 K to 250 K. At 77 K the clathrate has two resonances of equal intensity at 35.840 and 36.080 MHz, to be compared with those of pure orr/io-dichlorobenzene, where there are three lines at 35.580, 35.775 and 35.824 MHz. At 230 K there occurs an irreversible phase change which results in the expulsion of the ortho-dichlorobenzene from the host crystal, and the NQR signals thereafter correspond to the three lines of the unclathrated guest molecule. These events were also followed and confirmed by a calorimetric study in the range 210-300 K. The phase change is thought to be due to a transformation of the host molecule, where the thiocyanato groups are in the trans configuration in the clathrate, to the eis configuration, which is known not to form a clathrate. 
  Reference    Z. Naturforsch. 47a, 251—253 (1992); received July 27 1991 
  Published    1992 
  Keywords    Order-disorder effects, Phase transition Potential energy, Host-guest interaction 
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 Identifier    ZNA-1992-47a-0251 
 Volume    47 
42Author    Piotr KoziolRequires cookie*
 Title    High Pressure Studies of Tetrachloro-o-benzoquinone by NQR Spectroscopy  
 Abstract    Tetrachloro-o-benzoquione (TOB) crystallizes in two different forms. The two forms, Sample I and Sample II, show different phases and NQR spectra. When subjected to pressures higher than about 40 MPa the a phase is converted to the y phase. X-ray powder patterns studies as well as DTA measurements have confirmed this result. Heating the y phase above 310 K reverses this process. 
  Reference    Z. Naturforsch. 47a, 254—256 (1992); received November 28 1991 
  Published    1992 
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 Identifier    ZNA-1992-47a-0254 
 Volume    47 
43Author    M. Gourdji, L. Guibé, A. Péneau, J. Gallier, B. Toudic, H. CailleauRequires cookie*
 Title    NQR Investigation of the Temperature-Induced Neutral-to-Ionic Phase Transition in the Mixed-Stack Charge-Transfer Complex TTF-CA  
 Abstract    The chlorine-35 NQR has been investigated in the mixed-stack charge-transfer complex tetrathia-fluvalene-chloranil. The neutral-to-ionic (N-I) phase transition is clearly seen on the NQR spectrum. Among several features of the spectra recorded and their counterpart in the sample behaviour, the evidence for the change in the crystal symmetry and the quite likely existence of neutral domains in the ionic phase below the N-I transition temperature are the most striking ones. 
  Reference    Z. Naturforsch. 47a, 257—260 (1992); received August 3 1991 
  Published    1992 
  Keywords    TTF-CA, TINIT, Neutral-to-ionic phase transition, Mixed-stack charge transfer com-plex, NQR, 35 C1 
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 TEI-XML for    default:Reihe_A/47/ZNA-1992-47a-0257.pdf 
 Identifier    ZNA-1992-47a-0257 
 Volume    47 
44Author    C. Dimitropoulos, F. Borsa, J. PelzlRequires cookie*
 Title    Chlorine-NQR Relaxation Near the Structural Transitions of Natural and Deuterated (NH 4 ) 2 TeCl 6  
 Abstract    The temperature and isotope dependence of the 35,37 C1-NQR spin-lattice relaxation rate near the cubic to trigonal phase transition at TCl = 87 K has been investigated in both (NH4)2TeCl6 and (ND4)2TeCl6 salts. In the temperature range of ~20 K above and ~ 10 K below TCl, the relaxation obeys the relation (Tj • T) 2 cc(T—T Cl). This behaviour corresponds to a direct relaxation mechanism in presence of a strongly damped rotational soft mode of the TeCl^ -tetrahedra and is discussed on the basis of cation-anion coupling near the critical region. Below T Cl we observe an extra contribu-tion to the 35,37 C1 relaxation rate which is tentatively ascribed to the dynamics of the NH4 tetrahedra. 
  Reference    Z. Naturforsch. 47a, 261—26460 (1992); received July 27 1991 
  Published    1992 
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 Identifier    ZNA-1992-47a-0261 
 Volume    47 
45Author    Silvia Wigand, Tetsuo Asaji, Ryuichi Ikeda, Daiyu NakamuraRequires cookie*
 Title    Reorientational Motion of Trihalogenomethyl Groups in Organic Compounds as Studied by 35 C1 NQR and 19 F NMR Spectroscopy  
 Abstract    Trihalogenomethyl derivatives of 4-chloroacetanilide, 4-ClC6HfNHCOCCl3,4-ClC6H4NHCOCF2Cl, and 4-ClC6H4NHCOCF3 were prepared. The 35 C1 NQR and 79 F NMR spin-lattice relaxation times T1Q and T1F, respectively, of these compounds were measured at various temperatures. On heating, T1Q of the CC13 and CF2C1 groups decreased rapidly above ca. 110 and 150 K, respectively, showing the onset of reorientation of the trihalogenomethyl group about the pseudo-triad axis. The activa-tion energies were determined to be 27 and 13kJmol _1 for the CC13 and CF2C1 reorientation, respectively. The temperature dependences of the 19 F NMR T1F of the CF2C1 and CF3 groups lead to activation energies of 13 and 4.3 kJ mol~ 1 , respectively, for the same reorientations. T1F of the CF3 group observed above ca. 200 K was attributed to the spin-rotational interaction. The TIQ 1 of ring-chlorine in 4-ClC6H4NHCOCCl3 and 4-ClC6H4NHCOCF3 can be interpreted by the T" law with « = 2.2 and 1.1, respectively, whereas that of 4-ClC6H4NHCOCF2Cl by the sum of two contributions: T" law (n = 2.0) and the modulation mechanism due to the CF2C1 reorientation. 
  Reference    Z. Naturforsch. 47a, 265—273 (1992); received July 19 1991 
  Published    1992 
  Keywords    Spin-lattice relaxation, NQR, NMR, Reorientational motion 
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 Identifier    ZNA-1992-47a-0265 
 Volume    47 
46Author    Makoto Kaga, Tetsuo Asaji, Ryuichi Ikeda, Daiyu NakamuraRequires cookie*
 Title    Chlorine Nuclear Quadrupole Relaxation and Cationic Motion in Trimethylsulfonium Hexachloroselenate(IV): [(CH 3 ) 3 Sl 2 SeCl^  
 Abstract    The 35 C1 NQR spin-lattice and spin-spin relaxation times, 7^ and T2Q, respectively, and the 'H NMR spin-lattice relaxation time T1H at 32 and 60 MHz were determined for [(CH3j3S]2SeCl6 as functions of temperature. The rapid decrease of observed above ca. 250 K with increasing temperature was attributed to the onset of reorientation of the [SeCl6] 2 " complex anion with the activation energy £a = 42 + 5 kJ mol -1 . When cooled from ca. 250 K, T1Q showed an anomalous decrease. This 7"1Q decrease was explained by electric field gradient modulation related to some cationic motion. Possible origins of the cationic motion are discussed. 
  Reference    Z. Naturforsch. 47a, 274—276 (1992); received July 19 1991 
  Published    1992 
  Keywords    Spin-lattice relaxation, NQR, NMR, EFG modulation, Molecular motion 
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 Identifier    ZNA-1992-47a-0274 
 Volume    47 
47Author    Keizo Horiuchi, Daiyu NakamuraRequires cookie*
 Title    Chlorine Nuclear Spin-Spin Relaxation Mechanism in Mg(H 2 0) 6 SnCl 6 as Studied by NQR and NMR Techniques  
 Abstract    The 35 C1 NQR spin-lattice relaxation time T1Q, spin-spin-relaxation time T2Q, and J H NMR spin-lattice relaxation time in the rotating frame T le in Mg(H20)6SnCl6 were measured as functions of temperature. Above room temperature T2q increased rapidly with increasing temperature, which can be explained by fluctuations of the local magnetic field at the chlorine nuclei due to cationic motions. From the T le experiments, these motions are found to be attributable to uniaxial and overall reorientations of [Mg(H20)6] 2+ ions with activation energies of 95 and 116 kJ mol -1 , respectively. Above ca. 350 K, T1Q decreased rapidly with increasing temperature, which indicates a reorientational motion of [SnCl6] 2-ions with an activation energy of 115 kJ mol -1 . 
  Reference    Z. Naturforsch. 47a, 277—282 (1992); received October 29 1991 
  Published    1992 
  Keywords    Complex compounds, Molecular dynamics, Nuclear relaxation, Nuclear quadrupole resonance, Nuclear magnetic resonance 
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 Identifier    ZNA-1992-47a-0277 
 Volume    47 
48Author    Takashige Shimizu, Tetsuo Asaji, Daiyu Nakamura, Ryuichi IkedaRequires cookie*
 Title    Uniaxial Reorientation of Octahedral Complex Anions Excited in Triethylammonium Hexachlorostannate (IV) Crystals  
 Abstract    The temperature dependence of the 35 C1 NQR spin-latticew relaxation time T1Q has been deter-mined for the three resonance lines observed in [(C2H5)3NH]2SnCl6. The higher frequency lines fade out around 150 K upon heating, whereas the lowest line shows up to room temperature no anomaly, although these three lines are assigned to chlorines belonging to the same complex anion. The T1Q values of the higher two lines decrease exponentially around the fade-out temperature, where T iq of the lowest line shows no such behavior. These results are explained by the onset of uniaxial reorientations of the octahedral complex ions by 90° about the Cl-Sn-Cl axis containing the lowest frequency chlorines. The activation energy (£J of this reorientation (22-24 kJ moP 1) is the lowest so far reportd for [SnCl6] 2-ions. £a about the other axes is 67 kJ mop 1 , indicating a remarkable anisotropic reorientation. 
  Reference    Z. Naturforsch. 47a, 283—287 (1992); received July 19 1991 
  Published    1992 
  Keywords    Spin-Lattice Relaxation, NQR, NMR, Reorientational Motion, Hydrogen Bond 
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 TEI-XML for    default:Reihe_A/47/ZNA-1992-47a-0283.pdf 
 Identifier    ZNA-1992-47a-0283 
 Volume    47 
49Author    Yoshio Kume, Maki Tokoro, Tetsuo Asaji, Ryuichi Ikeda, Daiyu NakamuraRequires cookie*
 Title    Reorientational Motion of Hydrogen Bonded Octahedral Complex Anions in Hydrazinium Hexachlorostannate(IV), (N 2 H 5 ) 2 SnCl 6 , as Studied by 35 C1 NQR Spin-Lattice Relaxation Measurements  
 Abstract    The temperature dependences of NQR frequencies and spin-lattice relaxation times, T1Q, of 35 C1 in (N2H5)2SnCl6 were measured. Four NQR signals distributed in a fairly wide frequency range were observed, the lowest-frequency line exhibiting an anomalous positive temperature coefficient. The highest-frequency line showed a steep temperature dependence. These results could be interpreted by considering the intermolecular interaction between CI and -NH2 in N2H^. Below ca. 250 K, T1Q of the upper three signals exhibited a gradual decrease upon heating, explainable by lattice vibra-tions, while a shallow Tig minimum, ascribable to the modulation of electric quadrupole interaction, was observed at ca. 11ÖK for the lowest-frequency signal. The reorientation of [SnCl6] 2 ~ was elucidated to be highly anisotropic, in that it reorients about one of the CI-Sn-Cl axes much more frequently than about the other two axes. The activation energies were determined to be 62 and 94 kj mol -1 for the respective reorientations. 
  Reference    Z. Naturforsch. 47a, 288—292 (1992); received July 17 1991 
  Published    1992 
  Keywords    Key word: Spin-Lattice Relaxation, NQR, NMR, Reorientational Motion, Hydrogen Bond 
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 Identifier    ZNA-1992-47a-0288 
 Volume    47 
50Author    Masao Hashimoto, Takahiro Isono, Noriko Yomesaka, Haruo Niki, Hiroshi Kyan, Takeshi HamagawaRequires cookie*
 Title    Reorientation of the CC1 3 Group in Chloral 4-Chlorobenzyl- hemiacetal. A Pulsed 35 C1 NQR and X-ray Study  
 Abstract    The crystal structure of the title compound was determined at 291 K: monoclinic, space group C^h-P21/n, Z = 4, a = 1693.2(1), 6 = 579.3(1), c = 1232.5(1) pm, and ß = 107.21 (1)°, R = 0.0415. A sharp decrease of of Cl NQR found at T> 270 K for the CC13 group is attributed to the reorientation of the group over a potential barrier of ca. 50 kJ/mol. Intermolecular interactions between the CC13 and the neighboring atoms seem to dominate the magnitude of the potential barrier. T{~ 1 of the 35 C1 NQR of the Cl atom on the benzene ring obeyed the T 2 law well in the range 80 < T/K <270, while at T>280 K it deviated from the T 2 law. 
  Reference    Z. Naturforsch. 47a, 293—298 (1992); received July 25 1991 
  Published    1992 
  Keywords    Crystal structure, Hydrogen bond, Chlorine NQR, Spin lattice relaxation, Atom-atom potential method 
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 Identifier    ZNA-1992-47a-0293 
 Volume    47 
51Author    Takeshi Kyan, Hamagawa, Takahiro Isono, Masao HashimotoRequires cookie*
 Title    Hiroshi  
 Abstract    The crystal structure of cyclohexylhemiacetal (cycHx-CH) was determined at 296 K: monoclinic, space group P2 Jc, a =1028.7 (9), b = 609.5 (1), c = 1811.9 (4) pm, and ß = 99.79 (3)°, Z -4, R = 0.0552. The three 5s Cl NQR lines in cycHx-CH, T., T2, and T2*, were measured by a pulsed method at 80-300 K. Below 200 K Tf 1 obeyed the T law well, indicating that the spin lattice relaxation is governed by lattice vibrations. The reorientation of CC13 seems to be responsible for the sharp T: drop observed above 250 K. Shoulders in the T { vs. 1/T curves indicate the presence of Ti minima at about 240 K. A fluctuation of the EFG due to a dynamic disorder of hydrogen atoms in the OH groups is assumed to explain the T x minima. 
  Reference    Z. Naturforsch. 47a, 299 (1992); received July 25 1991 
  Published    1992 
  Keywords    Chlorine NQR, Spin-lattice relaxation, Hydrogen bond, Crystal structure 
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 Identifier    ZNA-1992-47a-0299 
 Volume    47 
52Author    AlexanderA. Koukoulas, M. A. WhiteheadRequires cookie*
 Title      
 Abstract    The 35 C1 NQR temperature dependence in (PNC12)3 and (PNC12)4 was measured between 77 K and 293 K. The dependence in both compounds was smoothly varying. A sudden decrease in T* near 112 K indicated the presence of a strong broadening mechanism in (PNC12)3. The nature of this mechanism is interpreted in terms of the Cl spin-lattice relaxation. 
  Reference    Z. Naturforsch. 47a, 305—307 (1992); received August 10 1991 
  Published    1992 
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 Identifier    ZNA-1992-47a-0305 
 Volume    47 
53Author    R. Julian, C. Brown, MeganE. Shortreed, AndrewJ. Szabo, BrianM. Powell, StephenN. StuartRequires cookie*
 Title    NQR and Neutron Diffraction in Scheelites  
 Abstract    Measurements of the spin-lattice relaxation time for rhenium in KRe04 and NH4Re04 are reported; relaxation rates are extremely fast due to the large quadrupole moment of Re. Calculations of the electric field gradient in KRe04 show that the EFG is a very sensitive function of the orientation of the anion in the unit cell as well as of the unit cell dimensions, and that geometrical effects make a major contribution to the temperature dependence. Neutron diffraction in these two salts has been employed to determine the temperature dependence of structural parameters over a wide range of temperature, and preliminary results are reported. 
  Reference    Z. Naturforsch. 47a, 308—312 (1992); received August 4 1991 
  Published    1992 
  Keywords    NQR, Relaxation, Electric field gradient, Neutron diffraction 
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 Identifier    ZNA-1992-47a-0308 
 Volume    47 
54Author    M. Igarashi, H. Kitagawa, S. Takahashi, R. Yoshizaki, Y. AbeRequires cookie*
 Title    Temperature dependence of the Spin-Lattice Relaxation Time of the 23 Na-NMR Line in NaN0 2  
 Abstract    The spin-lattice relaxation time, TX, of the 23 Na-NMR line in NaN02 is measured between 25 K and 160 K at two magnetic field strengths, 1.1 T and 6.9 T. The temperature dependence of TX for the center line, observed on a polycrystalline sample prepared by precipitation from aqueous solution, is given by a monotonous curve. Tx increases gradually as the temperature decreases. On the other hand for a single crystal, which is made by a modified Bridgman method, the temperature dependence of TX shows two deep dips below 150 K and a frequency dependence which cannot be explained by ordinary BPP theory. The dominant relaxation mechanism above and below 150 K is also investigated. 
  Reference    Z. Naturforsch. 47a, 313—318 (1992); received November 6 1991 
  Published    1992 
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 Identifier    ZNA-1992-47a-0313 
 Volume    47 
55Author    Hiroshi Ohki, Nobuo NakamuraRequires cookie*
 Title    Sodium Ion Exchange in Na 1+x Zr 2 Si x P 3 _ ;c 0 1 2 as Studied by 23 Na Nutation NMR  
 Abstract    23 Na two-dimensional nutation NMR was applied to Nat + *Zr2SivP3_vO,2 with x = 0, 1, and 2. The nutation spectrum in each compound consists of two clearly separated peaks corresponding to the two crystallographically inequivalent sodium sites. In the compound with x = 2 the nuclear quadrupole coupling constants (e Qq/h) and the asymmetry parameters (rj) were by spectral simu-lation estimated to be 1.0 MHz and 0 for one site, and 1.5 MHz and 0.8 for the other site. The spectrum varies considerably on heating; the two peaks merge into a single peak at high tempera-tures due to fast ion exchange between the two different sites. For x = 0 and x = 1 the nutation spectra did not show any significant temperature dependence, suggesting that the rates of the sodium ion exchange are negligibly low. 
  Reference    Z. Naturforsch. 47a, 319—324 (1992); received August 10 1991 
  Published    1992 
  Keywords    Nutation NMR, Quadrupole effect, Superionic conductor, Chemical exchange 
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 Identifier    ZNA-1992-47a-0319 
 Volume    47 
56Author    V. P. Tarasov, G. A. Kirakosyan, K. E. German, Acad Sei, UssrRequires cookie*
 Title    Anomalous Temperature Dependence of the "Tc Quadrupole Coupling and Disordering of Cesium Positions in CsTc0 4  
 Abstract    A "Tc and 133 Cs solid-state NMR study of polycrystalline CsTc04 at a field of 7.04 T and temperatures from 90 to 430 K revealed first-order quadrupole effects. "Tc quadrupole coupling constant, Cq, shows anomalous positive temperature coefficients and decreases from 2.0 MHz at 430 K to 0.45 MHz at 90 K. The asymmetry parameter, rj ("Tc), is zero at 430 K and at 210 K. The high-temperature minimum of rj is associated with a phase transition from orthorhombic to tetrag-onal and the second minimum reflects an orientational change of the principal axes q xx and q yy of the EFG-tensor. The 133 Cs NMR spectra are characterised by a superposition of the two powder multiplets from the first-order couplings which arise from magnetically and crystallographically nonequivalent cesium sites, Cs (1) and Cs (2); the population ratio of Cs (2) and Cs (1), p2/p1, varies from 2.0 at 120 K to 6.5 at 373 K. The nonequivalence and population changes are attributed to the temperature change of the crystal field potential in the vicinity of the cations. 
  Reference    Z. Naturforsch. 47a, 325—329 (1992); received July 26 1991 
  Published    1992 
  Keywords    Technetium, Cesium, Solid State NMR, Quadrupole Effects, Phase Transitions 
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 Identifier    ZNA-1992-47a-0325 
 Volume    47 
57Author    A. D. Gordeev, G. B. Soifer, A. P. ZhukovRequires cookie*
 Title    C1 NQR and Molecular Motion in Solid C 6 X 5 C1 (X = H, F)  
 Abstract    The 35 C1 NQR frequency and spin-lattice relaxation time of solid chlorobenzene and chloro-pentafluorobenzene at temperatures from 77 K to the melting points have been measured and explained by thermoactivated librations and reorientations of the molecules around the normal to their plane. The activation energies of these motions have been estimated. 
  Reference    Z. Naturforsch. 47a, 330—332 (1992); received July 18 1991 
  Published    1992 
  Keywords    NQR spectroscopy, Molecular motion, Benzene derivatives 
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 Identifier    ZNA-1992-47a-0330 
 Volume    47 
58Author    R. Blinc, J. SeligerRequires cookie*
 Title    2 D Methods in NQR Spectroscopy  
 Abstract    The application of two-dimensional spectroscopy to nuclear quadrupole resonance (NQR) is reviewed with special emphasys on spin 3/2 nuclei. A new two-dimensional level crossing double resonance NQR nutation technique based on magnetic field cycling is described. This technique allows for a determination of both the electric quadrupole coupling constant and the asymmetry parameter for spin 3/2 nuclei in powdered samples even in cases where the quadrupolar signals are too weak to be observed directly. It works if the usual double resonance conditions are met, i.e. if the spin-lattice relaxation times are not too short if the quadrupolar nuclei are dipolarly coupled to "strong" nuclei. Variations of this techique can be also used for 2 D "exchange" NQR spectroscopy and NQR imaging. 
  Reference    Z. Naturforsch. 47a, 333—341 (1992); received July 27 1991 
  Published    1992 
  Keywords    2D methods, NQR spectroscopy, Double resonance 
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 Identifier    ZNA-1992-47a-0333 
 Volume    47 
59Author    Helmut DreizlerRequires cookie*
 Title    Contribution of Microwave Fourier Transform Spectroscopy to the Investigation of Nuclear Quadrupole Coupling  
 Abstract    Dedicated to Prof. Dr. Yuichi Kamura, Tokyo, on occasion of his seventy fifth Birthday By simple examples it is shown how fine structures in rotational spectra of free molecules can be used to analyse nuclear quadrupole coupling. It is demonstrated that microwave Fourier transform spectroscopy is an adequate tool for these studies. Examples for different nuclei illustrate the present possibilities. 
  Reference    Z. Naturforsch. 47a, 342—352 (1992); received August 5 1991 
  Published    1992 
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 Identifier    ZNA-1992-47a-0342 
 Volume    47 
60Author    W. S. VeemanRequires cookie*
 Title    Quadrupole Nutation NMR in Solids  
 Abstract    The nutation frequency of a quadrupolar spin I depends on the quadrupole interaction. From nutation spectra, therefore, one obtains information about the direct surrounding of the atom. The theory of the straightforward and of more complicated nutation NMR experiments is outlined. Two applications of nutation NMR, to 23 Na in zeolites and 27 A1 in alumina, are shown. In this way in CaO • 6 A1203 penta-coordinated aluminum has been detected. 
  Reference    Z. Naturforsch. 47a, 353—360 (1992); received July 18 1991 
  Published    1992 
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 Identifier    ZNA-1992-47a-0353 
 Volume    47 
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