December 31, 2018 Aim: To develop radiochemical strategies for the analysis of radionuclides in materials. Accurate measurement of radioactivity in waste materials has an important role to play in the decommissioning of nuclear sites, as it enables site operators to dispose of waste in compliance with the regulations. The determination of alpha- and beta-particle emitting radionuclides in decommissioning materials is one of the critical points of material characterisation, because they need to be radiochemically separated before measurement and the materials are difficult to process from the chemical point of view. Work has started towards the development of methods for analysis of the radionuclides 41Ca and 93Zr stainless steel and concrete as materials relevant to nuclear decommissioning. Sample dissolution techniques including acid leaching of stainless steel samples and lithium borate fusion of concrete samples have been tested and scaled up for the dissolution of up to 3g of the two matrices. Method optimisation work was carried out to identify efficient sample to flux ratio. The efficiency of the dissolution procedure was monitored by ICP-MS measurements of the elemental composition of the supernatant. Maximum dissolution efficiency for the automated lithium borate fusion of concrete has been achieved for 2.5 g of sample however the dissolution of 3g concrete was also achieved.