Abstract: This paper dealt with a method to analyse bile bilirubins established in this laboratory, which were first, seperated into four types by thin-layer chromatography, and identified as UCB （unconjugated bilirubin）. MCB （monoconjugated bilirubin）. DCB₁ （diconjugated bilirubin. non-glucuronide type） and DCB₂ （diconjugated bilirubin, glucuronide type） by di-pyrrol azopigment chromatography.The seperated bilirubins were then diazonised and quantitified by photometric method. Using this method. we are able to study the changes of bile bilirubin and of their composition in cholelithiasis and other liver diseases.