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Thermal-ionization isotope-dilution mass spectrometry is a highly precise and accurate method for the determination of potassium concentrations in serum. Although not suited for routine use because of the time and expense required, the technique provides an extremely valuable tool for the characterization of reference materials and for evaluating other analytical methods. The technique has recently been used to determine the concentration of potassium in a human serum standard, NBS Standard Reference Material 909.