RESUMEN
Although acoustic-emission (AE) piezoelectric transducers have distinctive variations in sensitivity, depending on frequency, propagation medium, and coupling, the vast majority of AE research is conducted by utilizing uncalibrated AE transducers. As a consequence, most results obtained by different groups are not comparable among each other. In this work, primary calibration by the method of reciprocity is shown. Rayleigh and longitudinal wave calibration curves are presented for piezoelectric high-frequency broadband transducer, mounted on steel and aluminium, in the frequency range 300 kHz-4 MHz. Influences on primary calibration of AE transducers, namely, by coupling medium, contact pressure, and propagation medium, are investigated.
RESUMEN
Two highly phenylated tetramethyl-p-silphenylene-diphenylsiloxane copolymers were coated on fused silica capillary columns and used as stationary phases in GC. The copolymers offered new insights into the coating process and column preparation due to their physicochemical properties. The fused silica capillary surface had to be pretreated in various ways to achieve a homogeneous film and a well deactivated surface: etching with ammonium bifluoride; leaching with sodium hydroxide and hydrochloric acid; silylation with tetraphenyldimethyldisilazane and triphenylsilylamine. Droplet formation was observed on tetraphenyldimethyldisilazane silylated surfaces leading to capillary columns with low separation efficiency. The topology of inhomogeneous films was investigated by light microscopy, scanning electron microscopy, and Auger electron spectroscopy. It became apparent that the stationary phase did not form droplets but islands, which are connected by a wetting layer according to the Stranski-Krastanov growth mode. Both copolymers are potential stationary phases for high-temperature GC with promising properties. They offer a higher overall polarity than 75% phenyl, 25% methyl-polysiloxanes in combination with increased thermal stability and reduced bleed levels.
