Nitrogen content and isotopic composition of carbonaceous-rich metasediments were determined by on-line and sealed-tube combustion using ultra-high vacuum line and static mass spectrometer adapted to analyse nitrogen nanomoles. Accurate measurements showed that nitrogen amount released by on-line combustion technique was underestimated to various extents. As a result, the nitrogen isotopic composition was not correctly determined. In contrast, sealed-tube combustion appeared to yield the most reproducible and accurate measurements, except for nitrogen depleted carbonaceous matter (semi-graphite to graphite transition) containing less than around 60 ppm of nitrogen, which were contaminated during their extraction from the rock. In view of that, a preliminary sealed-tube investigation of the organic nitrogen content and isotopic composition in a homogenous series of low-grade metasediments was undertaken: in spite of an important nitrogen loss, the carbonaceous matter nitrogen isotopic composition remains about the same during the meta-anthracite and semi-graphitisation stages. Inferences on the process of organic nitrogen mineralization during carbonaceous matter metamorphism can be drawn and several paleo-biogeochemical implications envisaged.