Reproducibility of preparation of cellulose-based cryogels characterised by TG–MS

Abstract

A TG-MS analysis was applied to reveal the reproducibility of preparation of cellulose-based cryogels. The cellulose materials were obtained by dissolution of cellulose in melted Ca(SCN) 2 , followed by gelation and regeneration in an ethanol bath and dried by lyophilisation. The whole preparation process was repeated 14 times. The pyrolysis of the prepared samples was investigated by TG-MS. A number of parameters were determined from the obtained TG, DSC and MS curves and statistically analysed. TG and MS data together with estimated reactions which occurred during sample decomposition enable the calculation of the composition of cryogels and pyrolysed material. An unexpected amount of calcium thiocyanate was found in cellulose cryogels (about 31 %) and after pyrolysis, a high content of calcium oxide (about 58 %) as a product of calcium thiocyanate decomposition was calculated for the final material. The total yield of carbon from cellulose decomposition was about 12 %. From the obtained data, it could be concluded that the preparation of cellulose cryogels is well reproducible if the amounts of the initial substances are kept constant.