By Prof. Dr. Koichi Hatada, Prof. Dr. Tatsuki Kitayama (auth.)

ISBN-10: 3642072933

ISBN-13: 9783642072932

ISBN-10: 3662089823

ISBN-13: 9783662089828

NMR Spectroscopy of Polymers locations emphasis at the useful use of NMR spectroscopy in polymer chemistry instead of the theoretical remedies. in response to the authors' vast experimental adventure, subject matters lined comprise (1) experimental difficulties comparable to guidance of pattern answer, collection of solvent, inner commonplace and tube, and contaminants in pattern answer, (2) accuracy and precision of NMR measurements required within the research of polymer constitution resembling tacticity, copolymer composition and chain finish constructions, (3) quantity magnetic susceptibility by way of NMR, (4) stereochemistry of polymer chains, chemical composition and comonomer series distribution in copolymers, and finish teams and abnormal linkages, (5) online coupled measurement exclusion chromatography(SEC) and NMR spectroscopy(SEC/NMR) during which an NMR spectrometer is decided within the SEC approach as a detector.

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So in the measurement of the 13C NMR spectrum of the polymer the flip angle of 90° is recommended to obtain the signals with high SIN ratios. 17 s) 400 300 200 Pulse repetition time I s 0 Fig. 3. 5/N ratios of the signals against pulse repetition times and number of accumulations for 125 MHz 13C NMR spectra of radically prepared PMMA measured with a 90° pulse during a certain period of time (30 min) [2]. 10 wt/vol% CDCI 3 solution, 55 oc under the COM at higher magnetic fields, for example, at 125 MHz, the signal intensities usually deviate from the theoretical value owing to the different NOE values for each carbon.

Although the boiling point of TMS is low (27 °C), it can be used in measurements up to about 100 °C. For higher-temperature measurement, hexamethyldisiloxane (HMDS) or octamethylcyclotetrasiloxane (OMTS) is used, the signal of which appears slightly downfield from that of TMS. For aqueous sample solutions, sodium 4,4-dimethyl-4-silapentane sulfonate (DSS) or sodium [2,2,3,3-d4 ]3-trimethylsilylpropanoate (TSP-d4 )can be used. It should be noted that DSS shows weak signals due to the three methylene groups as well as a strong peak due to three methyl groups.

29. 125 MHz 13( NMR spectra of carbonyl carbon of radically prepared PMMA (10 wt/vol%) in toluene-d8 at 90 •c a with and b without sample spinning. 45• pulse, pulse repetition time 5 s, 12,000 scans After readjusting the probe for the sample of interest, the following operation conditions should be set up before starting the accumulation of the FIDs; RF power (flip angle), pulse repetition, spectral width, data points, and number of accumulations. The effects of these elements of the operating conditions on the spectrum are described in Sect.

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NMR Spectroscopy of Polymers by Prof. Dr. Koichi Hatada, Prof. Dr. Tatsuki Kitayama (auth.)


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