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Hydrogen due to its high incoherent cross section is a good candidate both for internal source or internal detector nucleus for atomic-resolution holographic measurements. Metal-hydrides are promising materials for the technology of hydrogen storage and the understanding of their structure is crucial. In the present work the solution of problems appearing at preparation of samples for the investigation of YH and PdH systems with the composition of YHx x<0.2 and PdHy at y∼0.7 is described.