Quantitative evaluation of the lactate signal loss and its spatial dependence in press localized (1)H NMR spectroscopy

Localized (1)H NMR spectroscopy using the 90 degrees -t(1)-180 degrees -t(1)+t(2)-180 degrees -t(2)-Acq. PRESS sequence can lead to a signal loss for the lactate doublet compared with signals from uncoupled nuclei which is dependent on the choice of t(1) and t(2). The most striking signal loss of up to 78% of the total signal occurs with the symmetrical PRESS sequence (t(1)=t(2)) at an echo time of 2/J (approximately 290 ms). Calculations have shown that this signal loss is related to the pulse angle distributions produced by the two refocusing pulses which leads to the creation of single quantum polarization transfer (PT) as well as to not directly observable states (NDOS) of the lactate AX(3) spin system: zero- and multiple-quantum coherences, and longitudinal spin orders. In addition, the chemical shift dependent voxel displacement (VOD) leads to further signal loss. By calculating the density operator for various of the echo times TE=n/J, n=1, 2, 3,..., we calculated quantitatively the contributions of these effects to the signal loss as well as their spatial distribution. A maximum signal loss of 75% can be expected from theory for the symmetrical PRESS sequence and TE=2/J for Hamming filtered sinc pulses, whereby 47% are due to the creation of NDOS and up to 28% arise from PT. Taking also the VOD effect into account (2 mT/m slice selection gradients, 20-mm slices) leads to 54% signal loss from NDOS and up to 24% from PT, leading to a maximum signal loss of 78%. Using RE-BURP pulses with their more rectangular pulse angle distributions reduces the maximum signal loss to 44%. Experiments at 1.5 T using a lactate solution demonstrated a maximum lactate signal loss for sinc pulses of 82% (52% NDOS, 30% PT) at TE=290 ms using the symmetrical PRESS sequence. The great signal loss and its spatial distribution is of importance for investigations using a symmetrical PRESS sequence at TE=2/J.     

NMR at very low fields

Although nuclear magnetic resonance in low fields around or below the Earth's magnetic field is almost as old as nuclear magnetic resonance itself, the recent years have experienced a revival of this technique that is opposed to the common trend towards higher and higher fields. The background of this development is the expectation that the low-field domain may open a new window for the study of molecular structure and dynamics. Here, we will give an overview on the specific features in the low-field domain, both from the technical and from the physical point of view. In addition, we present a short passage on the option of magnetic resonance imaging in fields of the micro-Tesla range.     

Fabrication of ridge waveguides in zinc-substituted lithium niobate by means of ion-beam enhanced etching

We present results on the fabrication and characterization of ridge waveguides in zinc-substituted lithium niobate. High-quality waveguides were fabricated by a combination of liquid-phase epitaxy and multiple applications of ion-beam enhanced etching. The two major demands on ridge waveguides, a very low side-wall roughness and a rectangle shape with side-wall angles close to 90 degrees , were realized simultaneously by using this technique. Single-mode waveguiding at a wavelength of 1064 nm was demonstrated with attenuation values of 0.9 dB/cm.     

Application of multi-channel analysis techniques to beam-foil spectroscopy of neutral cobalt in the region 3000 Å to 3950 Å

A new experimental arrangement is described which is designed for measuring lifetimes of levels of low ionization states of heavy elements using the beam-foil technique. The method is applied to obtain lifetimes of 14 CoI transitions in the spectral range 3000 Å to 3950 Å. Our results are found to be in excellent agreement with the lifetime of the levels which have been measured previously using dye-laser excitation. Thef-values derived from our results indicate that the temperature correction proposed by Degenkolb and Griffiths greatly improves the accuracy of the Corliss and Bozman data, and also show remarkable consistency with the semi-empirical values tabulated by Kurucz and Peytremann. Finally, our newf-values are used to obtain a cobalt photospheric abundance given by logN(Co)=4.75±0.05.     

Perfluoralkyljod-verbindungen: Darstellungen und eigenschaften von CF3JO,CF3JOF2 und CF3JO2

Perfluoroalkyl iodine compounds: preparations and properties of CF₃IO, CF₃IOF₂, and CF₃IO₂. The trifluoromethyl iodine compounds CF₃IO, CF₃IOF₂, and CF₃IO₂ are formed from the reactions of CF₃I, CF₃IF₂ or CF₃IF₄ with ozone or silicon dioxide respectively. Their preparartions, properties, ¹⁹F-nmr spectra, and ir spectra are described.     

Novel 6-(trifiuoromethyl)cytosines and 6-(trifluoromethyl)uracils

Ethyl 3-amino-4,4,4-trifluorocrotonate ( 3 ) has been converted by a one step reaction with alkyl and aryl isocyanates to novel 3-substituted-6-(trifluoromethyI)uracils. Also several 3-amino-4,4,4-trifluorocrotonitriles ( 11a-c ) have been cyclized to novel 6-(trifluoromethyI)cytosines ( 13a-c ) and then hydrolyzed to the corresponding uracils ( 4, 14b-c ). Alkylation studies with isopropyl bromide of three 6-(trifluoromethyl)uracils ( 1, 4, 5 ) are described.     

Beitr?ge zur Chemie des Schwefels. 84

Zusammenfassung Durch Zonenschmelzen konnte hochreiner Schwefel dargestellt werden, dessen Verunreinigungsgehalt (Kohlenstoff: weniger als 2,4 · 10^–4%, Silicium 1,3 · 10^–6%, Magnesium: 4,0 · 10^–6%) wesentlich kleiner war als bei allen nach anderen Verfahren gereinigten Schwefelproben. Ein Verfahren zur Bestimmung von Silicium, Eisen und Magnesium in kleinen Schwefeleinwaagen durch Spektralanalyse ohne vorherige Anreicherung wurde ausgearbeitet.

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Summary High-purity sulphur was prepared by zone melting. The percentage of impurities (carbon < 2.4×10^–4%, silicon 1.3×10^–6%, magnesium 4.0×10^–6%) was considerably smaller than in sulphur purified by other procedures. A method is described for the determination of silicon, iron and magnesium in sulphur samples by direct spectroscopic analysis without enrichment of the elements to be analysed.

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83. Mitteilung: Lutz, H. D., u. Lj. Kosti: Z. Naturforsch. 21b, 892 (1966).

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Der Deutschen Forschungsgemeinschaft danken wir für die Förderung dieser Arbeit.     

Die sterischen Bedingungen der Fragmentierungsreaktion III. Teil. Stereoisomere 4-, 5- und 7-Decahydrochinolyl-toluolsulfonate Fragmentierungsreaktionen, 16. Mitteilung

In a heterolytic fragmentation reaction of the type a-b-c-d-X → a - b + c = d + : X the geometry of the d - X bond and that of the electron-donating group a relative to the b - c bond are critical. This follows from a study of solvolysis rates and products of stereoisomeric 1-methyl-4-, -5- and -7-decahydroquinolyl p-toluenesulphonates in 80 Vol.% ethanol.     

Novel halogenated imidazoles. Chloroimidazoles

With one exception chloroimidazoles containing an unalkylated ring nitrogen have been ignored. Procedures are described using hypochlorite solution that permit the synthesis of 4,5-dichloroimidazole and 2,4,5-trichloroimidazole. Various bromoimidazoles are also converted to chloroimidazoles in refluxing hydrochloric acid.