The collaborative evaluation of a procedure for the determination of N-nitroso compounds as a group

Two collaborative studies have been made of the method devized for the determination of N-nitroso compounds as a group, which involves their selective denitrosation with hydrogen bromide in glacial acetic acid, followed by the measurement of the nitric oxide liberated using a chemiluminescence analyzer, such as the TEA. Considerable variation was evident between the results in the first study, most of the values reported being low. This situation undoubtedly arose from the carry-over of traces of hydrogen bromide from one determination to the next, which resulted in premature denitrosation. The precision and consistency of the results were greatly improved in the second study, for which additional precautions had been recommended. All of the six participating laboratories reported reasonably consistent values, the coefficients of variation being 27.9% and 21.1% respectively, at the levels of spiking of N-nitrososarcosine equivalent to 32.9 ng and 146.4 ng of nitric oxide.