CLSM and TIRF images from lignocellulosic materials: garlic skin and agave fibers study

ABSTRACTFluorescence techniques have been widely used by scientists to reveal valuable information from biological samples, but in food science, small progress is known due to the complexity of the samples. In this study, two different biological samples, garlic skin (GS) and agave fibers (AF), were used to evaluate the techniques of confocal laser scanning microscopy (CLSM) and total internal reflection fluorescence (TIRF) microscopy, to obtain valuable information on the fiber size of the samples. A compositional characterization with calcofluor white in CLSM was achieved, but a superficial characterization of the samples with TIRF was made, evidencing fiber sizes of 398.67 ± 48.47 nm and 677.38 ± 76.88 nm for GS and AF, respectively. This work reveals that only an untreated sample can be used with the two techniques in the same microscope. In addition, it is possible to characterize the sample only using a spatial field of research and which valuable information about the structure of the material is found. This work provides the opportunity to use advanced fluorescence techniques for elucidation of structures shortly before studied with these techniques.

Mechanical and Physicochemical Properties of 3D-Printed Agave Fibers/Poly(lactic) Acid Biocomposites

In order to provide a second economic life to agave fibers, an important waste material from the production of tequila, filaments based on polylactic acid (PLA) were filled with agave fibers (0, 3, 5, 10 wt%), and further utilized to produce biocomposites by fused deposition modeling (FDM)-based 3D printing at two raster angles (−45°/45° and 0/90°). Differential scanning calorimetry, water uptake, density variation, morphology, and composting of the biocomposites were studied. The mechanical properties of the biocomposites (tensile, flexural, and Charpy impact properties) were determined following ASTM international norms. The addition of agave fibers to the filaments increased the crystallinity value from 23.7 to 44.1%. However, the fibers generated porous structures with a higher content of open cells and lower apparent densities than neat PLA pieces. The printing angle had a low significant effect on flexural and tensile properties, but directly affected the morphology of the printed biocomposites, positively influenced the impact strength, and slightly improved the absorption values for biocomposites printed at −45°/45°. Overall, increasing the concentrations of agave fibers had a detrimental effect on the mechanical properties of the biocomposites. The disintegration of the biocomposites under simulated composting conditions was slowed 1.6-fold with the addition of agave fibers, compared to neat PLA.

Study of Agave Fiber-Reinforced Biocomposite Films

Thermoplastic resins (linear low-density polyethylene (LLDPE), high-density polyethylene (HDPE), and polypropylene (PP)) reinforced by different content ratios of raw agave fibers were prepared and characterized in terms of their mechanical, thermal, and chemical properties as well as their morphology. The morphological properties of agave fibers and films were characterized by scanning electron microscopy and the variations in chemical interactions between the filler and matrix materials were studied using Fourier-transform infrared spectroscopy. No significant chemical interaction between the filler and matrix was observed. Melting point and crystallinity of the composites were evaluated for the effect of agave fiber on thermal properties of the composites, and modulus and yield strength parameters were inspected for mechanical analysis. While addition of natural fillers did not affect the overall thermal properties of the composite materials, elastic modulus and yielding stress exhibited direct correlation to the filler content and increased as the fiber content was increased. The highest elastic moduli were achieved with 20 wt % agave fiber for all the three composites. The values were increased by 319.3%, 69.2%, and 57.2%, for LLDPE, HDPE, and PP, respectively. The optimum yield stresses were achieved with 20 wt % fiber for LLDPE increasing by 84.2% and with 30 wt % for both HDPE and PP, increasing by 52% and 12.3% respectively.

Lignocellulosic Composites Prepared Utilizing Aqueous Alkaline/Urea Solutions with Cold Temperatures

Lignocellulosic composites (LCs) were fabricated by partially dissolving cotton to create a matrix that was reinforced with osage orange wood (OOW) particles and/or blue agave fibers (AF). LCs were composed of 15–35% cotton matrix and 65–85% OWW/AF reinforcement. The matrix was produced by soaking cotton wool in a cold aqueous alkaline/urea solvent and was stirred for 15 minutes at 350 rpm to create a viscous gel. The gel was then reinforced with lignocellulosic components, mixed, and then pressed into a panel mold. LC panels were soaked in water to remove the aqueous solvent and then oven dried to obtain the final LC product. Several factors involved in the preparation of these LCs were examined including reaction temperatures (−5 to −15°C), matrix concentration (15–35% cotton), aqueous solvent volume (45–105 ml/panel), and the effectiveness of employing various aqueous solvent formulations. The mechanical properties of LCs were determined and reported. Conversion of the cotton into a suitable viscous gel was critical in order to obtain LCs that exhibited high mechanical properties. LCs with the highest mechanical properties were obtained when the cotton wools were subjected to a 4.6% LiOH/15% urea solvent at −12.5°C using an aqueous solvent volume of 60 ml/panel. Cotton wool subjected to excessive cold alkaline solvents volumes resulted in irreversible cellulose breakdown and a resultant LC that exhibited poor mechanical properties.

Spectroscopic and Microscopic Study of Peroxyformic Pulping of Agave Waste

The peroxyformic process is based on the action of a carboxylic acid (mainly formic acid) and the corresponding peroxyacid. The influences of processing time (60–180 min), formic acid concentration (80–95%), temperature (60–80°C), and hydrogen peroxide concentration (2–4%) on peroxyformic pulping of agave leaves were studied by surface response methodology using a face-centered factorial design. Empirical models were obtained for the prediction of yield,κnumber (KN) and pulp viscosity as functions of the aforementioned variables. Mathematical optimization enabled us to select a set of operational variables that produced the best fractionation of the material with the following results: pulp yield (26.9%), KN (3.6), and pulp viscosity (777 mL/g). Furthermore, this work allowed the description and evaluation of changes to the agave fibers during the fractionation process using different microscopic and spectroscopic techniques, and provided a comprehensive and qualitative view of the phenomena occurring in the delignification of agave fibers. The use of confocal and scanning electron microscopy provided a detailed understanding of the microstructural changes to the lignin and cellulose in the fibers throughout the process, whereas Raman spectroscopy and X-ray diffraction analysis indicated that cellulose in the pulp after treatment was mainly of type I.