Optical emission spectroscopy of lead sulfide films plasma deposition.

In-situ Optical Emission Spectroscopy (OES) combined with quantum chemical calculations was used as a powerful tool to find out the exited reactive species existing in plasma discharge during the process of lead sulfide chalcogenide materials deposition. Low temperature nonequilibrium RF (40.68 MHz) plasma at low pressure (0.1 Torr) was employed for initiation of chemical interaction between precursors in the gas phase. Only high-pure elements were utilized as the initial substances. The ration between starting materials in the gas phase and power included into the plasma discharge were the variables. The mechanism of the plasma-chemical reaction was assumed and discussed. The stoichiometry and morphology of the surface of the as-deposited materials were studied by different analytical techniques.

Towards the interaction between calcium carbide and water during gas-chromatographic determination of trace moisture in ultra-high purity ammonia.

The current study focuses on the processes involved during the flow conversion of water into acetylene in a calcium carbide reaction cell for the trace moisture analysis of ammonia by reaction gas chromatography. The factors negatively affecting the reproducibility and the accuracy of the measurements are suggested and discussed. The intramolecular reaction of the HOCaCCH intermediate was found to be a side reaction producing background acetylene during the contact of wet ammonia gas with calcium carbide. The presence of the HOCaCCH intermediate among the reaction products is confirmed by an FTIR spectral study of calcium carbide powder exposed to wet gas. The side reaction kinetics is evaluated experimentally and its influence on the results of the gas chromatographic measurements is discussed in relation to the determination of the optimal operating parameters for ammonia analysis. The reaction gas chromatography method for the trace moisture measurements in an ammonia matrix was experimentally compared to an FTIR long-path length gas cell technique to evaluate the accuracy limitations and the resource intensity.

An improved back-flush-to-vent gas chromatographic method for determination of trace permanent gases and carbon dioxide in ultra-high purity ammonia.

A novel method for rapid, quantitative determination of trace permanent gases and carbon dioxide in ultra-high purity ammonia by dual-channel two-dimensional GC-PDHID is presented. An improved matrix back-flush-to-vent approach combining back-flush column switching technique with auxiliary NaHSO4 ammonia trap is described. The NaHSO4 trap prevents traces of ammonia from entering the analytical column and is shown not to affect the impurity content of the sample. The approach allows shortening the analysis time and increasing the amount of measurements without extensive maintenance of the GC-system. The performance of the configuration has been evaluated utilizing ammonia- and helium-based calibration standards. The method has been applied for the analysis of 99.9999+% ammonia purified by high-pressure distillation at the production site.