The global demand on highly purified gases provided by energy-efficient separation processes grows steadily since decades. An example of particular industrial relevance is nitrogen generated by pressure swing adsorption from compressed air. A kinetically based separation of oxygen from nitrogen is possible by means of carbon molecular sieves (CMS) since oxygen adsorbs remarkably faster in CMS than nitrogen. Even high product purities (5-1000 ppm O 2) are easily achievable in commercial generators. However, only a few studies present experimental findings in this purity range. That comes as no surprise, since experimental conditions are not standardised and the determination of N 2-PSA performance indicators still creates an experimental challenge. Moreover, the design of the setup remarkably influences the experimental results. Thus it is the motivation of this study to develop a multi-step strategy, comprising the definition of a reference process, the derivation of explicit and implicit performance indicators based on either flow meter readings or macroscopic material balances, a verification strategy for experimentally obtained data, and an error consideration, which advices accuracy requirements for analysers and flow meters. The effect of cycle time and operating temperature on the performance indicators is exemplarily studied at high purities by means of the proposed strategy.