This methods is part of the book:
Klemm, D., et al. “Comprehensive cellulose chemistry: v. 2: functionalization of cellulose: functionalization of cellulose.” (1998).
A weighed cellulose samples of known water content up to 0.5 g is suspended in 25 ml of aquaeus methylne blue chloride solution (300mg/l) and 25 ml of borate buffer of pH = 8.5 for 1 h at 20 oC in a 100 Erlenmeyer flask and then filtered through a sintered-glass disk. 5 or 10 ml of the filtrate are transferred to a 100 ml calibrated flask. Then 100 of 0.1 N HCl and subsequently water, up to 100 ml, are added. Then the methylene blue content of the liquid is determined photometrically, employing a calibration plot, and from the result the total amount of free, i.e. nonsorbed, methylene blue is calculated. The carboxyl group content of the sample is obtained according to:
Phillip, B., Rehder, W., Lang H. Papier 1965, 1-10