State-of-the-art in analytical characterization of high purity solid samples by different spectroscopic methods

Facilities and some results of several spectroscopic methods which have potential applications in the field of analysis of solid high purity substances and which have been elaborated in Russia, will be discussed in this paper. Laser nondispersive atomic fluorescence method with glow discharge cathode sputtering atomiser, may be used for trace element determination as well as a tool for the investigation of technological processes, viz. deposition of thin films. Investigations on reduction of a background level in the new hollow cathode ion source for mass-spectrometry have been carried out. Laser mass spectrometry with tandem laser mass reflectron is successfully designed and applied for gaseous impurities determination in high pure silicon with limit of detection of 10−3–10−5 ppm wt. Several results of the layer-by-layer and bulk trace analysis of solids by high resolution mass spectrometry with radio frequency powered glow discharge ion source with the limits of detection at 10−1–10−3 ppm wt will be presented here. The traditional arc and spark emission technique still finds considerable use. One of the examples considered in the paper is the analysis of metalfullerenes. To overcome the calibration problem the fluorination process inside the electrode crater using zinc fluoride has been investigated.