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In this paper, a new approach to the torrefaction process is proposed. The approach consists of obtaining a single torrefied product with an energy value and standardized physicochemical properties in the range of sub-bituminous coal from two types of waste: the cotton stalk and vine pruning. A multifactorial design was used to investigate the effect of temperature, time, and reaction atmosphere on the properties of the torrefied product (char). The process was optimized according to the mass and energy yield and the increase in the higher heating value (HHV). A series of physicochemical, kinetic, and microscopic analyses were carried out on the raw and torrefied biomass to evaluate the combustible properties. Char was obtained with an energy value in the range of sub-bituminous coal and with more uniform fuel properties concerning raw biomass. The optimal torrefaction conditions for cotton stalk were 6% O2–257.8°C–60 min and 0% O2–275°C–20 min for vine pruning. The HHV of the cotton stalk and vine pruning increased from 16.88 to 22.21 MJ kg−1 and from 17.01 to 22.43 MJ kg−1, respectively. The char from both residues presented similar O/C and H/C atomic ratios, and its value decreased compared with the raw biomass. Char is hydrophobic and easy to grind. Oxygen concentration played an essential role in reducing the time and temperature of torrefaction.

Electrodes fouling associated with the electroenzymatic phenols determination was characterized in this work, applying various techniques such as cyclic voltammetry, amperometry, EQCM, and optical microscopy. An approach to overcome the fouling effects and hence to improve the precision of the phenolic compounds determination was suggested and tested. This approach consists of pulsed potential waveform application with a cleaning potential step of + 1.4 V vs. Ag, AgCl/KCl sat with a duration of 166.66 ms, while the determination was carried out at 0.0 V vs. Ag, AgCl/KCl sat applied for 66.64 ms. As a result a RSD of 2.97% for 0.6 mmol L −1 o-catechol determination was achieved, compared with 6.53% without the cleaning step application. The method was successfully used for the precise phenolic and triazine pollutants determination.

Public health and environmental protection concerns provoked by phenolic compounds pollution impose the development of sensitive, rapid and cost effective methods for in situ phenols monitoring. Given that biosensors based techniques could face these challenges, a variety of such devices was suggested and applied for phenolic compounds quantification. Their majority are based on the polyphenol oxidase (PPO) catalyzed phenols oxidation to catechol and then, to quinones, coupled with the registration of the quinones reduction current. Nevertheless, quinoid products polymerization involving electrode passivation corrupts the biosensors operational stability. Thus, to avoid this drawback, in this work is proposed another approach for phenolic compounds quantification based on the electrochemical detection of the oxygen depletion during PPO catalyzed catechol oxidation using a Clark type electrode with a disposable active enzyme membrane. The oxygen probe was modified in comparison to the commercial ones: its flat front allowed ensuring a good contact with the active enzyme membrane and the gold multicathode uniformly dislocated on the surface of the flat front permitted eliminating O2 diffusional constraints. The active enzyme membrane was prepared by drop-coating of a mixture of PPO and gelatin onto a gelatin-saturated cellulose filter. A linear calibration graph for catechol determination was obtained in the range up to 0.7 mM with a slope of 0.902 μA/mM, at pH 6.5 and ambient temperature. The steady-state response to catechol of the biosensor was reached in 120 s. The biosensor had an excellent reproducibility (RSD2 reduction. Another biosensor advantage is associated with the use of disposable prefabricated active enzyme membranes.

In this work is suggested a Clark type electrode with disposable enzyme membrane for phe- nols determination. This approach allows avoiding the electrode fouling by recording the oxygen re- duction current, and obtaining a stable and reproducible sensor response. An appropriate method for enzyme membrane fabrication by cellulose acetate filters coating with tyrosinase through the use of biocompatible hydrogels was proposed and tested. The sensitivity of the catechol determination, as an example, was found to be 0.89 ∝A mmol -1 L. The detection limit equaled 1 ∝mol L -1 . The achieved RSD was 1.22%.