A simple derivatization methodology is shown to extend the application of surface-enhanced Raman spectroscopy (SERS) to the detection of trace concentration of contaminants in liquid form. Normally in SERS the target analyte species is already present in the molecular form in which it is to be detected and is extracted from solution to occupy sites of enhanced electromagnetic field on the substrate by means of chemisorption or drop-casting and subsequent evaporation of the solvent. However, these methods are very ineffective for the detection of low concentrations of contaminant in liquid form because the target (ionic) species (a) exhibits extremely low occupancy of enhancing surface sites in the bulk liquid environment and (b) coevaporates with the solvent. In this study, the target analyte species (acid) is detected via its solid derivative (salt) offering very significant enhancement of the SERS signal because of preferential deposition of the salt at the enhancing surface but without loss of chemical discrimination. The detection of nitric acid and sulfuric acid is demonstrated down to 100 ppb via reaction with ammonium hydroxide to produce the corresponding ammonium salt. This yields an improvement of ~4 orders of magnitude in the low-concentration detection limit compared with liquid phase detection.
In an almost cubical reactor 90 l in volume which is intended to deposit organic polymers by plasma-enhanced chemical vapor deposition (PECVD), microwave power is coupled into the volume via a quartz window which extends to approximately 1/10 of the sidewall area. Since the plasma is excited locally, plasma parameters like electron temperature and plasma density are expected to exhibit a spatial variation. The compilation of these plasma quantities has been accomplished with a bendable single Langmuir probe. To isolate the tungsten wire against its grounded housing tube, it was coated with polyparylene. After having compared this construction with our Langmuir probe, which has been now in use for more than a decade, we have taken data of more than half the volume of the reactor with argon and have found a definitive radial inhomogenity for all plasma parameters. To investigate whether this conduct can be determined applying optical emission spectroscopy, we improved our spectrometer which had been used for endpoint detection purposes and plasma diagnostics in chlorine-containing ambients where we could detect also a spatial dependence. This behavior is discussed in terms of Lieberman's global model.
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