This paper describes the various types of samples of activated corrosion products obtained from the high-temperature pressurized water-loop facilities in the NRX reactor and the radiochemical procedures and radioactivity assay methods which are used in analysis of these samples.Typically, in-pile loops are simulated reactor systems, i.e. they consist of a primary flowing coolant system and auxiliary make-up, purification, sampling and cooling systems. Two of the loops in NRX, namely, the carbon steel English Electric Corporation “Leo” loop and the Bettis Atomic Power Laboratory central thimble CR-V Loop, are described with particular attention to their associated sampling facilities: autoclaves and out-pile test sections for corrosion and corrosion product deposition studies, hot and cold corrosion product filters for filtration of insoluble materials, and ion exchange columns for purification of the loop water and the study of the ion-exchange behaviour of activated water-borne corrosion and fission products.The types of samples obtained and the method of attack used to separate and isolate specific fractions of the mixed corrosion products are described. In particular, the separation scheme devised is one which permits the isolation of elements of the first transition series and their associated activated impurities from one another. The separation is basically an anion exchange technique involving the successive elution of carrier-equilibrated species.Resin samples from the loop purification system are attacked in the presence of carriers by either digestion with H2SO4-HNO3 or by alkaline fusion.In some cases, corrosion product deposits are assayed directly for activity distribution by means of gamma-scintillation spectrometry (differential pulse height analysis). Application of composite gamma-ray spectrum resolution to deposition coupons and pipe samples is described.The radionuclides found in loop water and in unfilterable corrosion products are mainly radiative neutron capture products of the corroded in-pile and out-pile materials. The main nuclides analyzed for are 45.1 d Fe59, 5.25 y Co60, 27.8 d Cr51, 12.8 h Cu64, 2.58 h Mn68, 2.56 h Ni65, 245 d Zn65 and 65 d Zr95. Fast neutron reactions have been also observed through the appearance of 300 d Mn54 and 72 d Co58. Two radionuclides observed in the water and in solid corrosion products are 60 d Sb124 and 2.8 d Sb122. The source of these radionuclides has not been positively identified. The corrosion products from the CR-V loop also contain 253 d Ag110m, 43 d Cd114m and 50 d In114m arising from the corrosion of an in-pile specimen of a Ag-In-Cd alloy.Radioactivity assay of the purified fractions from separated samples is mainly by γ-ray scintillation spectrometry. Routine activity assay utilizing comparison with standardized differential pulse height distributions for pure radionuclides has been adopted because of the versatility of its use for both separated and gross samples. Conventional end-window beta-proportional counting techniques are used for those nuclides whose decay modes and energies preclude gamma-ray intensity assay techniques.The complexity of corrosion product mixtures from in-pile loops requires that stringent control be maintained at all phases of the program from the time of sampling to the time radioactivity assay is completed. Several problem areas are discussed. For example, large amounts of Fe59 contaminating Co60 samples and Zr95 contamination of Mn54, are difficult to detect without considerable scrutiny of counting data. Carrier exchange is difficult to effect in some cases: e.g. Zr96-ZrN exchange. The gamma-counting data in particular receive careful scrutiny. The gravimetric assay of carrier yield is in some cases a doubtful and time-consuming operation ; therefore, techniques eliminating gravimetric procedures should be explored.