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The thyroidal uptake of ³⁶ClO₄^– and the effect of stable perchlorate ion and functional state of the thyroid, such as after long-term administration of propylthiouracil (PTU) or after hypophysectomy, on the uptake of ³⁶ClO₄^– were studied in rats and guinea-pigs. Based on the analysis of uptake curves, radioactive inulin and sulphate spaces, and histological measurements of compartmental sizes of the thyroid, the relative concentrations of ³⁶ClO₄^– in the various compartments were calculated and compared with those of ³⁶Cl^-. The passage of ³⁶ClO₄^– and ³⁶Cl^– across both the basal and the apical membranes of the follicular cells in the different conditions were analysed. The results suggest that ³⁶ClO₄^– is concentrated in the lumen of the thyroid by a two-step process. It is actively transported across the basal cell membrane from the interstitial fluid into follicular cells, and is further concentrated in passage across the apical membrane into the lumen. The evidence suggests that the latter process is also an active one.