Selective Detection of Volatile Organics in a Mixture Using a Photoionization Detector and Thermal Desorption from a Nanoporous Preconcentrator.

The selective detection of individual hazardous volatile organic compounds (VOCs) within a mixture is of great importance in industrial contexts due to environmental and health concerns. Achieving this with inexpensive, portable detectors continues to be a significant challenge. Here, a novel thermal separator system coupled with a photoionization detector has been developed, and its ability to selectively detect the VOCs isopropanol and 1-octene from a mixture of the two has been studied. The system includes a nanoporous silica preconcentrator in conjunction with a commercially available photoionization detector (PID). The PID is a broadband total VOC sensor with little selectivity; however, when used in conjunction with our thermal desorption approach, selective VOC detection within a mixture can be achieved. VOCs are adsorbed in the nanoporous silica over a 5 min period at 5 °C before being desorbed by heating at a fixed rate to 70 °C and detected by the PID. Different VOCs desorb at different times/temperatures, and mathematical analysis of the set of PID responses over time enabled the contributions from isopropanol and 1-octene to be separated. The concentrations of each compound individually could be measured in a mixture with limits of detection less than 10 ppbv and linearity errors less than 1%. Demonstration of a separation of a mixture of chemically similar compounds, benzene and o-xylene, is also provided.

Alpha-chitin nanocrystals prepared from shrimp shells and their specific surface area measurement.

Alpha-chitin was isolated from shrimp shells. The chitin was subjected to extensive treatments of acid hydrolysis and mechanical disruption to yield nanocrystals. The goal of this article is to characterize alpha-chitin nanocrystals produced from shrimp shells in regard to crystallite properties and the specific surface area of the chitin nanoparticles. X-ray diffraction data indicate an increase in chitin crystallinity after hydrolysis, as less-ordered chitin domains are digested. Line broadening data were used to measure crystallite size and particle size in the hydrolyzed chitin nanocrystals. Dye adsorption with Congo red was used to measure the specific surface area of the particles, indicating values near 350 m2/g. This value was supported with calculations derived from X-ray crystallite size measurements. Particle surface area measurements were compared with similarly prepared cellulose nanocrystals.

Effect of sulfate groups from sulfuric acid hydrolysis on the thermal degradation behavior of bacterial cellulose.

When used as fillers in polymer composites, the thermostability of cellulose crystals is important. Sulfate groups, introduced during hydrolysis with sulfuric acid, are suspected to diminish the thermostability. To elucidate the relationship between the hydrolysis conditions, the number of sulfate groups introduced, and the thermal degradation behavior of cellulose crystals, bacterial cellulose was hydrolyzed with sulfuric acid under different hydrolysis conditions. The number of sulfate groups in the crystals was determined by potentiometric titration. The thermal degradation behavior was investigated by thermogravimetric analysis. The sulfate group content increased with acid concentration, acid-to-cellulose ratio, and hydrolysis time. Even at low levels, the sulfate groups caused a significant decrease in degradation temperatures and an increase in char fraction confirming that the sulfate groups act as flame retardants. Profile analysis of the derivative thermogravimetric curves indicated thermal separation of the degradation reactions by the sulfate groups into low- and high-temperature processes. The Broido method was used to determine activation energies for the degradation processes. The activation energies were lower at larger amounts of sulfate groups suggesting a catalytic effect on the degradation reactions. For high thermostability in the crystals, low acid concentrations, small acid-to-cellulose ratios, and short hydrolysis times should be used.