Judith P.A. Feitosa

Amylose contents, rheological properties and gelatinization kinetics of yam (Dioscorea alata) and cassava (Manihot utilissima) starches

Abstract After defatting yam and cassava starches have amylose contents of 36.2 and 24.2%, respectively. Suspensions of these starches in water were analysed, in an oscillatory rheometer, using a heating rate of 4.0 °C min−1, deformation of 1% and a frequency of 1 Hz, the initial temperatures of gelatinization being 71 and 62 °C for yam and cassava, respectively. A gelatinization study was also carried out by differential scanning calorimetry with different heating rates (2.5, 3.0, 4.0 and 5.0 °C min−1), to give, by the Arrhenius equation, the activation Energy (Ea) of the process. Yam starch showed a more energetic gelatinization process of when compared to cassava starch and also had a lower rate constant (s−1), indicating a relatively slow gelatinization process of at higher temperatures. Yam gels formed by autoclaving a suspension (50 g l−1) showed after 24 h of refrigeration, a stronger structure than for a cassava gel.

Antioxidant activity of cashew nut shell liquid (CNSL) derivatives on the thermal oxidation of synthetic cis-1,4-polyisoprene

CNSL is a mixture of meta-alkylphenols with variable degree of unsaturation attached to the benzene ring. The kinetic study of the thermal degradation at 140 °C of synthetic cis-1,4-polyisoprene film, in the presence of technical CNSL and some derivatives (cardanol, hydrogenated cardanol and alkylated hydrogenated cardanol) was carried out by FTIR. The amount of OH/OOH and C=O formed and also of C=C consumed during the degradation was determined. All materials increase the induction period and decrease the apparent rate constants of thermal-oxidation. Based on kinetic parameters, the order of antioxidant activity was: CNSL >> cardanol @ hydrogenated and alkylated cardanol > hydrogenated cardanol. The effect of CNSL could be attributed to the extra contribution of the other components besides cardanol and to the unsaturation on the long side chain. This greater activity is important because CNSL is much more cost effective than its derivatives.

Improvement of polyvinyl alcohol properties by adding nanocrystalline cellulose isolated from banana pseudostems

Cellulose nanocrystals (CNCs) isolated from banana pseudostems fibers (BPF) of the Pacovan variety were used as fillers in a polyvinyl alcohol (PVOH) matrix to yield a nanocomposite. The fibers from the external fractions of the BPF were alkaline bleached and hydrolyzed under acidic conditions (H2SO4 62% w/w, 70 min, 45 °C) to obtain CNCs with a length (L) of 135.0 ± 12.0 nm and a diameter (D) of 7.2 ± 1.9 nm to yield an aspect ratio (L/D) of 21.2. The CNCs were applied to PVOH films at different concentrations (0%, 1%, 3%, and 5% w/w, dry basis). With higher concentrations of CNCs, the water-vapor barrier of the films increased, while the optical properties changed very little. Increasing the concentration of the CNCs up to 3% significantly improved the mechanical properties of the nanocomposite.

Structural characterization of polysaccharide obtained from red seaweed Gracilaria caudata (J Agardh).

Seaweeds are considered an important source of bioactive molecules. In this work the marine red alga Gracilaria caudata was submitted to aqueous extraction of their polysaccharides for 2 h at 100 °C. The polysaccharide fraction (PGC) presented a recovery of 32.8%. The sulfate content of PGC, calculated by S%, is 1 ± 0.2% and the degree of sulfation accounts for 0.13 ± 0.2. High-Performance Size-Exclusion Chromatography demonstrated that PGC consists of a high molecular weight polysaccharide (2.5 × 10(5)gmol(-1)). Chemical analysis of PGC was performed by microanalysis, infrared (FT-IR) and nuclear magnetic resonance (NMR, 1 and 2D) spectroscopy. The structure of PGC is mainly constituted by the alternating residues 3-linked-β-D-galactopyranose and 4-linked-3,6-α-L-anhydrogalactose; however some hydroxyl groups were substituted by methyl groups and pyruvic acid acetal. The biological precursor of 3,6-α-L-anhydrogalactose (6-sulfate-α-l-galactose) was also detected.

Effect of mono and divalent salts on gelation of native, Na and deacetylated Sterculia striata and Sterculia urens polysaccharide gels

The effects of purification and salt addition on gelation of Sterculia striata and Sterculia urens (karaya) gels were investigated. Both gums form thermoreversible and ‘true’ gels. Melting transition temperature (Tm) of Na-polysaccharide sample was lower than that of the native gum. A gel-like mechanical spectrum is observed for two Sterculia gums with G′>G″ and little frequency dependence. The presence of acetyl groups in both gums seems to stabilize the gel. The Tm decreases and the critical gelation concentration increases after deacetylation. The addition of monovalent salts (LiCl, NaCl, KCl) to native S. striata polysaccharide decreases the Tm. However, the gel becomes stronger when monovalent salts are added to Na- and deacetylated gum. The gel strength of Na- S. striata polysaccharide in the presence of divalent salt follows the order: Mg2+>Ca2+>Sr2+>Ba2+, i.e. inversely proportional to the cationic radius. Addition of divalent salts to S. urens polysaccharide promotes a Tm decrease. A model for the gelation was proposed that includes ionic interactions and hydrogen bonding.

A novel green approach for the preparation of cellulose nanowhiskers from white coir

The aim of this work was to optimize the extraction of cellulose nanowhiskers (CNW) from unripe coconut husk fibers (CHF). The CHF was delignified using organosolv process, followed by alkaline bleaching (5% (w/w) H2O2+4% (w/w) NaOH; 50°C, 90 min). The CHF was subsequently hydrolyzed with 30% (v/v) sulfuric acid (60°C, 360 min). The process yielded a partially delignified acetosolv cellulose pulp and acetic black liquor, from which the lignin was recovered. The CNW from the acetosolv pulp exhibited an average length of 172±88 nm and a diameter of 8±3 nm, (aspect ratio of 22±8). The surface charge of the CNW was -33 mV, indicating a stable aqueous colloidal suspension. The nanocrystals presented physical characteristics close to those extracted from cellulose pulp made by CHF chlorine-pulping. This approach offers the additional advantage of extracting the lignin as an alternative to eradication.

Brazilian gutta-percha points: Part I: chemical composition and X-ray diffraction analysis

Eight nonstandardized gutta-percha points commercially available in Brazil (Konne, Tanari, Endopoint, Odous, Dentsply 0.04, Dentsply 0.06, Dentsply TP and Dentsply FM) were analysed chemically and by X-ray diffraction, and their chemical compositions were compared. The organic fraction (gutta-percha polymer and wax/resin) of the gutta-percha points was separated from the inorganic fraction (ZnO and BaSO4) by dissolving them in chloroform. The gutta-percha polymer was precipitated with acetone. The inorganic fraction was analysed by elemental microanalysis. Energy-dispersive X-ray microanalysis (EDX) and X-ray diffraction were employed to identify the chemical elements and compounds (barium sulfate and zinc oxide). The barium sulfate content was calculated based on the percentage of sulfur found in the elemental microanalysis. All analyses were repeated three times. The means and standard deviations of the percentage by weight of gutta-percha in the points were: Konne (17.6 +/- 0.30), Tanari (15.2 +/- 0.30), Endopoint (16.7 +/- 0.23), Odous (18.8 +/- 0.20), Dentsply 0.04 (15.7 +/- 0.17), Dentsply 0.06 (16.6 +/- 0.17), Dentsply TP (21.6 +/- 0.15) and Dentsply FM (16.3 +/- 0.23). The means and standard deviations of the zinc oxide content were: Konne (79.9 +/- 0.10), Tanari (81.9 +/- 0.07), Endopoint (81.3 +/- 0.40), Odous (79.7 +/- 0.26), Dentsply 0.04 (77.9 +/- 0.03), Dentsply 0.06 (78.2 +/- 0.07), Dentsply TP (69.8 +/- 0.19) and Dentsply FM (72.6 +/- 0.70). The method utilized was appropriate to quantify gutta-percha, wax/resin, zinc oxide and barium sulfate. Cone brands without barium sulfate were found. An unusual high wax/resin percentage was detected in Dentsply FM (p = 0.0003). Dentsply TP showed the highest gutta-percha percentage.

Bacterial cellulose nanocrystals produced under different hydrolysis conditions: properties and morphological features

Bacterial cellulose (BC) is a polymer with interesting physical properties owing to the regular and uniform structure of its nanofibers, which are formed by amorphous (disordered) and crystalline (ordered) regions. Through hydrolysis with strong acids, it is possible to transform BC into a stable suspension of cellulose nanocrystals, adding new functionality to the material. The aim of this work was to evaluate the effects of inorganic acids on the production of BC nanocrystals (BCNCs). Acid hydrolysis was performed using different H2SO4 concentrations and reaction times, and combined hydrolysis with H2SO4 and HCl was also investigated. The obtained cellulose nanostructures were needle-like with lengths ranging between 622 and 1322nm, and diameters ranging between 33.7 and 44.3nm. The nanocrystals had a crystallinity index higher than native BC, and all BCNC suspensions exhibited zeta potential moduli greater than 30mV, indicating good colloidal stability. The mixture of acids resulted in improved thermal stability without decreased crystallinity.

Application of ftir in the determination of acrylate content in poly(sodium acrylate-co-acrylamide) superabsorbent hydrogels

Hydrogels have been prepared by free-radical solution copolymerization of acrylamide and sodium acrylate (NaAc), with molar ratio ranging from 25/75 to 80/20, respectively, using methylene bisacrylamide as the crosslinking agent. A FTIR spectroscopy procedure to determine the acrylate/acrylamide ratio in these hydrogels was proposed based on absorbance at 1410 cm-1 (nCOO-) and 2940 cm-1 (nCH and nCH2). A straight line with a good linear correlation coefficient (0.998) was obtained by plotting the acrylate content (Ac%) versus relative absorbance (Arel = A1410/A2940). Results were confirmed by the amount of sodium cation released in acid medium determined by atomic absorption spectrometry.

Oxidation of cashew tree gum exudate polysaccharide with TEMPO reagent

Cashew gum (CG), an exudate polysaccharide from Anacardium ocidentale trees, was oxidized with TEMPO reagent and the 7product (CGOX) characterized by spectroscopic techniques (FT-IR and NMR), chromatographic analyses (HPLC and GPC), viscosity measurements and thermal analysis (TGA). The yield of the reaction product was 96%. The uronic acid content in starting gum (7.2 m%) was increased to 36 m%. The degree of oxidation based on free galactose and glucose units was 68%. NMR data show that oxidation occurred preferentially at primary carbons of galactose units. High degradation degree after oxidation was estimated by the difference on the expected and observed hCGOX/hCG ratio. The presence of organic and inorganic impurities in the new polyelectrolyte was detected by TGA. A less thermally stable cashew gum is formed after the oxidation with TEMPO based on initial decomposition temperature and IPDT.