Abstract: Highly quantitative methods for determining the concentration of residual phase transfer catalysts (PTCs) in radiotracer or radiopharmaceutical doses are described. The methods comprise mixing aliquots of the doses that can contain residual PTCs with a sodium and/or potassium salt; extracting a residual PTC/salt complex into an organic phase; and detecting the amount of PTC/salt complex in the organic phase. The detecting can involve visual colorimetry or measuring the absorbance or transmittance of the organic phase when the sodium and/or potassium salt comprises a chromophoric ion, or measuring the resistance of the organic phase. Also described are devices for use in performing the methods.