A method for the indirect detection of light elements, L (L = C, N, 0 or F), by using X-ray emission spectroscopy is described. The technique relies upon the formation of certain low-energy satellite peaks to those X-ray emission peaks which originate from electronic transitions involving the valence shell of an element, A, when A-L bonds are made. The energy difference between the main peak and the satellite peak is characteristic of the ligand (F, 20 f 1 eV; 0, 14 j, 2 eV; N, 9 f 2 eV; and C , about 5 eV). Applications to compounds that contain more than one type of ligand are described and experimental limitations are discussed.X-RAY emission spectroscopy is widely used for both qualitative and quantitative analyses for the elements present in a wide variety of minerals, glasses, ceramics and other materials.l-s Characteristic X-ray emission can be brought about either by irradiation with electrons (e.g., microprobe and betaprobe) or with X-rays (X-ray fluorescence), but in either instance it is found that the efficiency of X-ray emission diminishes with decrease in atomic number.Coupled with the inherent difficulties in the production of characteristic X-ray emission from light elements there are concomitant difficulties in detection. The wavelengths of the Ka lines of the light elements are boron 6-76 nm, carbon 4-47 nm, nitrogen 3.16 nm, oxygen 2.36 nm and fluorine 1.83 nm. Only the last two elements can be detected easily by the use of acid phthalate crystals with 2d spacings of about 2.6 nm. Other crystals and "soap films'' have been developed6 with larger 2d spacings but these are not in universal use. A second difficulty in detecting radiations from light elements is again associated with their low energies. Not only will the sample itself readily absorb them but so also will any gas present in the spectrometer. This difficulty can be overcome by carrying out the operation in a vacuum. Even so, it remains true to say that the light elements cannot readily be detected by X-ray emission spectroscopy. The purpose of this paper is to demonstrate that the presence of such light elements in a sample can, however, easily be established by a detailed investigation of specific low-energy satellite peaks associated with characteristic X-ray emissions of other elements in the sample.
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