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Granulation was performed with a solution containing carvedilol (CAR) as API in the ultralow dose range (0.05 w/w% in the granule) and the addition of riboflavin (RI) as a coloured tracer. An in-line calibration in the range of 0.047–0.058 w/w% was prepared for the measurement of CAR concentration using colour analysis (CA) and particle size analysis (PSA), and the validation with HPLC resulted in respective relative errors of 2.62% and 2.30% showing great accuracy. To improve the technique, a second in-line calibration was conducted in a broader CAR concentration range of 0.039–0.063 w/w% utilizing only half the amount of RI (0.045 w/w%), while doubling the output of the granulation line to 2 kg/h, producing a relative error of 4.51% and 4.29%, respectively. Finally, it was shown that the CA technique can also be carried on to monitor the CAR content of tablets in the 42–62 μg dose range with a relative error of 5.20%. 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