Determination of the carbonyl group content of cellulose samples by oximation

This methods is part of the book:
Klemm, D., et al. “Comprehensive cellulose chemistry: v. 2: functionalization of cellulose: functionalization of cellulose.” (1998).

2 g of an air dry sample of known moisture content is suspeded in 100ml 0f 0.02 N aquaeous zinc acetate solution in a 300 ml Erlenmeyer flask under vigorous stirring. After a residence of 2-6 h at room temperature in the covered flask the liquid is sucked off and the moist sample is immediately and quantitatively returned to the flask and subsequently suspended in 100 ml of the oximation reagen (35 g hydroxilamine hydrochoride, 55 g zink acetate, 160 ml 1 N NaOH and 1.6 ml glacial acetic acid/l aquaeous solution) appliying a gentle shaking. After a residence time of 20 h at 20oC, the liquid is again sucked off through the same sintered-glass disk and twice washed with water. Subsequently the sample is suspended again in the same flask in 100 of 0.02 N zinc acetate solution. After 2 h the liquid is again sucked off and the sample is washed with aqueous zinc acetate solution of the same concentration. The moist oximated sample is then immadiately subjected to a determination of the nitrogen content by Kjeldahl method, employing finally a calorimetric determination of the NH4+ formed with Nesslers reagent. I umol of nitrogen correspond to 1 umol of carbonyl groups in the sample.

Laboratory procedure of Fraunhofer Institute of Applied Polymer Research.

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