Hydrogen-powered fuel-cell cars nowadays provide a huge potential for reducing pollutant and greenhouse gas emissions caused by the transport sector. They manage to combine most benefits from both combustion engine-powered and battery-powered electric cars into a single vehicle, and under certain circumstances can provide a climate-neutral drive concept. The necessary hydrogen can be provided in ever increasing amounts and better economic efficiency than ever before through the ever more common use of power-to-gas applications. Electrolysis in the context of power-to-gas offers a sustainable and eco-friendly basis for hydrogen production via wind and solar energy. Thus, the biggest challenge for a widespread usage and acceptance of hydrogen-fuelled cars lies in providing a sufficiently developed infrastructure of adapted gas stations. The HylyPure®-Process, which was developed at the Technical University of Vienna, tries to address this issue with its concept of feeding hydrogen to the existing gas grid for storage and distribution, therefore being able to provide hydrogen in fuel cell quality of at least 99,97 Vol.-% purity in any place that has access to the natural gas grid. Over the course of the work in hand the design, dimensioning, automation and initial operation of a lab-scale pressure swing adsorption unit were conducted. Whilst the applications main focus was on the context of HylyPure®, there was an emphasis on high flexibility in view of usage for different gas separation tasks and possible subsequent usage for high-pressure applications of up to 90 bar(g). The executed design consists of four packed-bed adsorbers using activated carbon as the adsorbent and an identically constructed buffer tank. In these, the breakthrough curves of a binary mixture made from equal volume fractions of methane and hydrogen were obtained at 8 bar(g) and compared to literature-based computational results. Qualitative experiments were performed in succession through the cyclical pressure swing adsorption process containing 12 individual steps. For those experiments a gas mixture reflecting the conditions of the HylyPure®-process containing 70 Vol.-% methane and 30 Vol.-% hydrogen was used. The variation of operational parameters led to a detailed discussion on the three different runs. Based on the results obtained, subsequent optimization and possibilities for a profound quantitative analysis, including the examination of the hydrogen yield under the implementation of the designated analytical possibilities, was determined.