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Analysis of degradation products in rayon spinning baths

Abstract An analytical method for the determination and quantification of the main organic degradation products of viscose spinning baths was outlined herein and successfully applied. Samples were ethoximated and silylated for GC-MS analysis. The main challenge in the analysis was the quantification of the degradation products because standard compounds are often not commercially available. Analyte recovery was optimized with regard to pH and lyophilization conditions. Given that the spinning bath analytes showed a very broad range of volatility, internal standardization by the degradation product of uniformly 13C-labeled glucose in alkaline media was used. This approach allowed for the first time for the accounting of a major part of the organic components in the viscose spinning baths. On average, 57% of total organic carbon was characterized by quantifying 21 individual substances. The methodology opens new perspectives of keeping track of the formation and origin of organic degradation products. It is a prerequisite to all further efforts to avoid contamination of the spinning bath and achieve a higher product quality and a better closure of process cycles. Furthermore, it can be easily applied to other highly complex industrial process streams involving polysaccharide degradation products as they are emerging, for instance, in biorefineries.