The Multi-Analytical Characterization of Calcium Oxalate Phytolith Crystals from Grapevine after Treatment with Calcination

Abstract

Calcium oxalate phytoliths are one of the most prominent types of Ca speciation in the plant kingdom, and they store extensive amounts of carbon in crystalline form. Ca phytoliths were investigated in the root, trunk, and bark of Vitis vinifera Chasselas from a vineyard in Alsace, France. A multi-analytical approach was used, which included SEM coupled with EDX spectroscopy, XRD, XRF, TGA, and 13C-NMR spectroscopy. These techniques revealed that phytoliths are composed of crystalline calcium oxalate monohydrate (whewellite). The whewellite crystals exhibited mostly equant or short-prismatic habits in all of the three studied grapevine parts, but bipyramidal crystals also occurred. Raphide crystals were only observed in the root, where they were abundant. Instead of using wet chemical procedures to extract the mineral components from the organic parts of the biomass, a thermal treatment via calcination was chosen. The suitable temperature of calcination was determined through TGA experiments. The calcination of the biomass samples at 250 °C enhanced the amounts of Ca phytoliths in the residual chars. The thermal treatment, however, affected the appearance of the Ca oxalate crystals by producing surfaces that displayed macroporosity and by creating fractures. For calcination at both 300 °C and 350 °C, Ca oxalate lost a molecule of carbon monoxide to form Ca carbonate, and the modifications of the original crystal surfaces were more pronounced than those observed after thermal treatment at 250 °C.

Cellulose Nanocrystals and Lignin Nanoparticles Extraction from Lemna minor L.: Acid Hydrolysis of Bleached and Ionic Liquid-Treated Biomass

“…The three dominant peaks at 13 • , 30 • , and 42 • can be associated with the crystalline structure of cellulose type II (polymorphic transition from cellulose type I to II in acid-treated cellulose) (Figure 2d) [53]. The signals of calcium oxalate could also be detected in the CNC AH spectrum [54], specifically at 8.3 • , 24.2 • , and 29 • , characteristic of this material [55].…”