Optimization of a nitrogen analyser based on the Dumas method

The objectives of this work was to obtain a total nitrogen concentration in milk with the Dumas method for industrial and research applications. This method was faster than the Kjheldal method (5 min against 2 h or 3 h) but less precise. A three factor experimental design was performed to optimize the instrument, a FP-2000 supplied by LECO. The first interpretation of the experimental design was disappointing and no conclusion could be done. It was not a failure of experimental design but a lack of thinking on the physical and chemical aspect of the problem. Selection and construction of composite responses based on chemical and physical consideration were the keys to optimize the Dumas method. This method is now as precise as the Kjheldal method, but considerably faster.     

Determination of nitrogen and carbon in refractory nitrides and carbonitrides by means of Dumas gas chromatography

The applicability of an automated Dumas-GC method for the determination of nitrogen and carbon in refractory materials was investigated. Analyses were carried out to determine nitrogen and carbon in TiN, ZrN and Ti(C,N) using CuO, V₂O₅ and Pb₃O₄ as oxidizing additives. The reproducibility of the analyses obtained with V₂O₅ was better than ± 1 rel% for major constituents. An estimation of the accuracy of the Dumas-GC method shows that this rapid and low-cost method can compete with other methods, at least for the refractory nitrides and carbonitrides of the transition metals.