Abstract
A sample preparation unit was developed for use in emission spectrometric analysis of 15N, and the unit and the NOI-4 spectroscope were evaluated. The sample preparation unit was designed to permit use of reusable discharge tubes, monitoring of pressure in the tube, and flushing with and addition of an inert gas to the tube. It utilizes the hypobromite oxidation approach for production of nitrogen gas. Instrument problems and sources of error included nonlinear gain settings, baseline determination, overlapping bandheads and nonlinearity of the standard curve. Problems in the sample preparation method adopted were limited to memory in the discharge tube ; this was reduced by prolonged baking of the tubes at 700°. Minimum sample size is about 10 μg N. In the normal to 5 atom% 15N range, the overall method (sample preparation and analysis) gave 0.01 confidence intervals of ±0.03 atom% 15N.
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