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Contenido archivado el 2024-04-19

Novel combined on-line and kinetic measurement techniques for the chiral detection of compounds by optical spectroscopy

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The HPLC CD photodiode array (PDA) detector permits the simultaneous measurement of absorption and circular dichroism at all wavelengths in the range 200 - 410 nm. The light source is a highly stable deuterium arc lamp which can be operated in two modes (intensity doubling). The instrument is designed to carry out measurements on samples in standard cuvettes with optical path lengths of 0.01 to 10 mm at fixed temperature in the range 15-100o C using the effective Hewlett Packard Peltier temperature controller, or on samples in an 11 micro flow cell with optical path length 10 mm. The spectral resolution in the steady-state measurements is 3 nm, that in the flow measurements becomes about 5 nm. With a fixed sampling time of 20 ms for the half-cycles with left and right circularly polarized light, taking into account the processing of the data from the PDA detector, the minimum CD measurement time amounts to 80 ms. In highly accumulated CD measurements, e.g. 4 s = ? 100 * 80 ms samplings, a sensitivity better than 1*10-5 can be attained, whereas in flow measurements with only one sampling the detection limit amounts to 5*10-5. The simultaneous detection of absorption and CD permits the direct determination of enantiomeric purity in flowing samples (of which the molecular effects are known).

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