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.
The strain‐promoted azide alkyne cycloaddition (SPAAC) is a powerful tool for forming covalent bonds between molecules even under physiological conditions, and therefore found broad application in fields ranging from biological chemistry and biomedical research to materials sciences. For many applications, knowledge about reaction kinetics of these ligations is of utmost importance. Kinetics are commonly assessed and studied by NMR measurements. However, these experiments are limited in terms of temperature and restricted to deuterated solvents. By using an inline ATR‐IR probe we show that the cycloaddition of azides and alkynes can be monitored in aqueous and even complex biological fluids enabling the investigation of reaction kinetics in various solvents and even human blood plasma under controlled conditions in low reaction volumes.
Off-the-shelf computer cooling hardware was used to construct a closed-loop air cooling system (CLACS) that is distinguished by scalability, low energy, and no tap water consumption. Constructed to be generally used with laboratory condensers, the system was tested with several common low and high boiling solvents and showed a condensation performance equivalent to conventional tap water cooling. Reaction yields were therefore unaffected. Also, long-lasting Soxhlet extractions showed no performance loss relative to conventional cooling. Optionally, the device can be assembled from low-voltage components and be powered from a battery, rendering it independent of the main power. Both investment and running costs are minimal, allowing a lab-wide adoption and elimination of the two major drawbacks of commonly employed tap water cooling: waste of drinking water and the risk of flooding.
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