Rf values of different width filter paper chromatograms using 75 per cent methanol in an ascending system are presented for iodide and iodate. The chemical identity of the spots is determined by the use of carrier iodide and iodate. The iodide spot was developed by spraying the dry chromatogram with starch hydrogen peroxide solution. The iodate spot was developed with a spray of ascorbic acid‐starch solution. Description of the equipment is given. The relationship of the chart drive speed and the optimal slit width to the time constant of the counting rate meter is discussed and the minimal slit width calculated for the instrument used. Integration of the curves gave areas representing the total activity at each spot. The ratio of the iodide‐iodate activities thus determined differed from the relative readings of the counting rate meter.