Porcine pepsin was immobilized inside the SBA-15 mesoporous silica system through physical adsorption. A grafting step with 3-aminopropryltriethoxysilane (APTES) was performed to reduce the pore openings of the host material, in order to minimize the enzyme leaching. A detailed physical chemical characterization of hybrid materials was performed. The catalytic activity of the hybrid bioinorganic material, tested with two different substrates (hemoglobin and Z-l-glutamyl-l-tyrosine dipeptide), confirmed that pepsin was located inside the pore/channels of the silica material and that the grafting process did not affect the enzyme structure. The immobilized pepsin has maintained the necessary degree of freedom to fulfill its catalytic activity. The reusability of the so-called bioreactor was also investigated.

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The aim of the study was to analyse BTEX compounds (benzene, toluene, ethylbenzene, xylenes) in air by solid phase micro-extraction/gas chromatography/mass spectrometry (SPME/GC/MS), and this article presents the features of the calibration method proposed. Examples of real-world air analysis are given. Standard gaseous mixtures of BTEX in air were generated by dynamic dilution. SPME sampling was carried out under non-equilibrium conditions using a Carboxen/PDMS fibre exposed for 30 min to standard gas mixtures or to ambient air. The behaviour of the analytical response was studied from 0 to 65 microg/m3 by adding increasing amounts of BTEX to the air matrix. Detection limits range from 0.05 to 0.1 microg/m3 for benzene, depending on the fibre. Inter-fibre relative standard deviations (reproducibility) are larger than 18%, although the repeatability for an individual fibre is better than 10%. Therefore, each fibre should be considered to be a particular sampling device, and characterised individually depending on the required accuracy. Sampling indoor and outdoor air by SPME appears to be a suitable short-delay diagnostic method for volatile organic compounds, taking advantage of short sampling time and simplicity.

Sources of VOC (Volatile Organic Compounds) reference-materials at ppm and ppb levels are needed for calibration of air monitoring instruments. The permeation-tube technique is considered effective for the preparation of low concentration standards of high accuracy and stability. In this work, purpose-built PTFE permeation tubes, containing benzene, toluene, ethylbenzene, o-xylene or m-xylene (BTEX) were accurately and rapidly calibrated. Using the sensitive thermo-balance of a thermogravimetric apparatus, very low permeation rates were determined by the continuous monitoring of the tube weight loss as a function of time. Permeation rates in the range from 25 to 350 ng min(-1) were determined with precision. Thermogravimetry appears to be a rapid method for the measurement of weight loss at constant temperature, allowing rapid characterization and recalibration of permeation tubes. A detailed study on toluene, chosen as a typical case, showed that there are variations of the permeation rate in the long term. The temperature dependence of the permeation coefficient was also explored and permeation rates were shown to display an Arrhenius behavior in the temperature range 304-324 K. Thermodynamic parameters influencing the permeation were discussed.

Permeation tubes are convenient analyte sources for generating standard gas mixtures (containing, in particular, volatile organic compounds) used in the calibration of analytical instruments. For small permeation rates, corresponding to trace levels of analytes, the calibration of permeation tubes is time-consuming. The use of thermogravimetry as a means to measure rapidly the weight loss at constant temperature was investigated. An attempt to apply this technique to calibrating a permeation tube filled with benzene is described. In the 20 ng/min range of permeation rate, day-to-day variations of <5% were observed. The continuous weight loss monitoring of permeation tubes by thermogravimetry allows their rapid characterization.