Study of the Effect of Physical Aging on the Polylactic Acid by Thermal and Optical Techniques

2021 ◽  
Vol 33 ◽  
pp. 73-81
Author(s):  
Amirouche Bouamer ◽  
Nasser Benrekaa ◽  
Abderrahmane Younes
Keyword(s):  
Polylactic Acid ◽  
Aging Time ◽  
Physical Aging ◽  
Attenuated Total Reflection ◽  
Hydroxyl Group ◽  
Scanning Calorimetry ◽  
Absorption Bands ◽  
Depolarization Current ◽  
Optical Techniques ◽  
Aging Period

In this work, we investigated the influence of physical aging on polylactic acid (PLA) films using thermal and optical techniques; Differential Scanning Calorimetry (DSC), Thermally Stimulated Depolarization Current (TSDC), and Attenuated Total Reflection Spectroscopy (ATR). The PLA films were aged for different periods: 60, 90, and 120 minutes at a temperature Ta = 43 °C. The result obtained by DSC showed that the effect of physical aging appeared as an endothermic peak, which increased with increasing aging time and evolved towards higher temperatures. TSDC results showed a thermal current peak located between 30 and 80 ° C, which represented the main relaxation mode (α relaxation) of the dielectric manifestation of the glass transition. The intensity of this peak decreased and was shifted to higher temperatures when aging time increased, this result can be explained by a decrease in the molecular mobility of macromolecular chains due to the decrease in the free volume. The effect of physical aging on the PLA by the ATR technique showed a gradual decrease in all absorption bands during the aging period. In particular, the wide absorption band between 3000 and 3700 cm-1 attributed to the hydroxyl group (OH), which disappeared after two hours of aging

scholarly journals A Study on Physical Aging of Semicrystalline Polyethylene Terephthalate below the Glass Transition Point

2012 ◽  
Vol 10 (5) ◽  
Author(s):  
M. Farhoodi ◽  
S. M. Mousavi ◽  
R. Sotudeh-Gharebagh ◽  
Z. Emam-Djomeh ◽  
A. Oromiehie ◽  
...  
Keyword(s):  
Glass Transition ◽  
Aging Time ◽  
Polyethylene Terephthalate ◽  
Physical Aging ◽  
Degree Of Crystallinity ◽  
Glass Transition Point ◽  
Scanning Calorimetry ◽  
Different Temperatures ◽  
Dsc Method ◽  
Final Degree

Physical aging of semicrystalline polyethylene terephthalate was studied using differential scanning calorimetry(DSC). PET samples with crystallinity content of 0.28 were aged at two different temperatures, 25 and 45°C. Thesamples were stored for several days and periodically tested using DSC method. The glass transition temperature forthe samples aged at 25°C was about 73-74°C, and the position and intensity of endothermic peaks wereapproximately constant. Higher glass transition of the samples aged at 45°C, 73-86°C, was attributed to the enthalpyrelaxation process of amorphous regions of semicrystalline PET. For the samples aged at 45°C, the endothermicpeaks shifted to higher temperatures with increasing aging time. The position of the endothermic peaks determined bythe temperature of the maximum, Tmax, tended to increase with aging time for samples aged at 45°C, and theintensity of the peaks continuously increased with time; however, the results showed that the aging of PET samples at45°C even after 120 days continued the enthalpic relaxation of semicrystalline PET and that the process could bestudied by DSC method. The results also showed that the aging process could affect the final degree of crystallinity ofc-PET samples and the samples stored at 45°C showed higher degree of crystallinity than the samples aged at 25°C.

Nevirapine Pharmaceutical Cocrystal: Design, Development and Formulation

2019 ◽  
Vol 9 (3) ◽  
pp. 240-247
Author(s):  
Prabhakar Panzade ◽  
Priyanka Somani ◽  
Pavan Rathi
Keyword(s):  
Dosage Form ◽  
In Vitro Dissolution ◽  
Soluble Form ◽  
Ir Absorption ◽  
Stoichiometric Ratio ◽  
Design Development ◽  
Formulation Development ◽  
Scanning Calorimetry ◽  
Absorption Bands ◽  
Pharmaceutical Cocrystal

Background and Objective: The top approach to deliver poorly soluble drugs is the use of a highly soluble form. The present study was conducted to enhance the solubility and dissolution of a poorly aqueous soluble drug nevirapine via a pharmaceutical cocrystal. Another objective of the study was to check the potential of the nevirapine cocrystal in the dosage form. Methods: A neat and liquid assisted grinding method was employed to prepare nevirapine cocrystals in a 1:1 and 1:2 stoichiometric ratio of drug:coformer by screening various coformers. The prepared cocrystals were preliminary investigated for melting point and saturation solubility. The selected cocrystal was further confirmed by Infrared Spectroscopy (IR), Differential Scanning Calorimetry (DSC), and Xray Powder Diffraction (XRPD). Further, the cocrystal was subjected to in vitro dissolution study and formulation development. Results: The cocrystal of Nevirapine (NVP) with Para-Amino Benzoic Acid (PABA) coformer prepared by neat grinding in 1:2 ratio exhibited greater solubility. The shifts in IR absorption bands, alterations in DSC thermogram, and distinct XRPD pattern showed the formation of the NVP-PABA cocrystal. Dissolution of NVP-PABA cocrystal enhanced by 38% in 0.1N HCl. Immediate release tablets of NVP-PABA cocrystal exhibited better drug release and less disintegration time. Conclusion: A remarkable increase in the solubility and dissolution of NVP was obtained through the cocrystal with PABA. The cocrystal also showed great potential in the dosage form which may provide future direction for other drugs.

scholarly journals Characterization of Beeswax, Candelilla Wax and Paraffin Wax for Coating Cheeses

Coatings ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 261
Author(s):  
Adolfo Bucio ◽  
Rosario Moreno-Tovar ◽  
Lauro Bucio ◽  
Jessica Espinosa-Dávila ◽  
Francisco Anguebes-Franceschi
Keyword(s):  
Physical And Mechanical Properties ◽  
Tensile Tests ◽  
Paraffin Wax ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Absorption Bands ◽  
Dimensional Changes ◽  
Ductile Behavior ◽  
Candelilla Wax

A study on the physical and mechanical properties of beeswax (BW), candelilla wax (CW), paraffin wax (PW) and blends was carried out with the aim to evaluate their usefulness as coatings for cheeses. Waxes were analyzed by X-ray diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), differential scanning calorimetry (DSC), permeability, viscosity, flexural and tensile tests and scanning electron microscopy. Cheeses were coated with the waxes and stored for 5 weeks at 30 °C. Measured parameters were weight, moisture, occurrence and degree of fractures, and dimensional changes. The crystal phases identified by XRD for the three waxes allowed them to determine the length of alkanes and the nonlinear compounds in crystallizable forms in waxes. FTIR spectra showed absorption bands between 1800 and 800 cm−1 related to carbonyls in BW and CW. In DSC, the onset of melting temperature was 45.5 °C for BW, and >54 °C for CW and PW. Cheeses coated with BW did not show cracks after storage. Cheeses coated with CW and PW showed microcraks, and lost weight, moisture and shrunk. In the flexural and tensile tests, BW was ductile; CW and PW were brittle. BW blends with CW or PW displays a semi ductile behavior. Cheeses coated with BW blends lost less than 5% weight during storage. The best waxes were BW and the blends.

scholarly journals Physical Aging Behavior of a Glassy Polyether

Polymers ◽  
2021 ◽  
Vol 13 (6) ◽  
pp. 954
Author(s):  
Xavier Monnier ◽  
Sara Marina ◽  
Xabier Lopez de Pariza ◽  
Haritz Sardón ◽  
Jaime Martin ◽  
...  
Keyword(s):  
Glass Transition ◽  
Transition Temperature ◽  
Glass Transition Temperature ◽  
Physical Aging ◽  
Glassy State ◽  
Aging Behavior ◽  
Scanning Calorimetry ◽  
Narrow Temperature Range ◽  
Glass Forming ◽  
Fast Scanning Calorimetry

The present work aims to provide insights on recent findings indicating the presence of multiple equilibration mechanisms in physical aging of glasses. To this aim, we have investigated a glass forming polyether, poly(1-4 cyclohexane di-methanol) (PCDM), by following the evolution of the enthalpic state during physical aging by fast scanning calorimetry (FSC). The main results of our study indicate that physical aging persists at temperatures way below the glass transition temperature and, in a narrow temperature range, is characterized by a two steps evolution of the enthalpic state. Altogether, our results indicate that the simple old-standing view of physical aging as triggered by the α relaxation does not hold true when aging is carried out deep in the glassy state.

scholarly journals Recycling Waste Cotton Cloths for the Isolation of Cellulose Nanocrystals: A Sustainable Approach

Polymers ◽  
2021 ◽  
Vol 13 (4) ◽  
pp. 626
Author(s):  
Siti Hajar Mohamed ◽  
Md. Sohrab Hossain ◽  
Mohamad Haafiz Mohamad Kassim ◽  
Mardiana Idayu Ahmad ◽  
Fatehah Mohd Omar ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Cellulose Nanocrystals ◽  
Value Added ◽  
Crystallinity Index ◽  
Attenuated Total Reflection ◽  
Cellulose Content ◽  
Scanning Calorimetry ◽  
Good Thermal Stability ◽  
Alkaline Pulping ◽  
Hydrolysis Of Cellulose

There is an interest in the sustainable utilization of waste cotton cloths because of their enormous volume of generation and high cellulose content. Waste cotton cloths generated are disposed of in a landfill, which causes environmental pollution and leads to the waste of useful resources. In the present study, cellulose nanocrystals (CNCs) were isolated from waste cotton cloths collected from a landfill. The waste cotton cloths collected from the landfill were sterilized and cleaned using supercritical CO2 (scCO2) technology. The cellulose was extracted from scCO2-treated waste cotton cloths using alkaline pulping and bleaching processes. Subsequently, the CNCs were isolated using the H2SO4 hydrolysis of cellulose. The isolated CNCs were analyzed to determine the morphological, chemical, thermal, and physical properties with various analytical methods, including attenuated total reflection-Fourier transform-infrared spectroscopy (ATR-FTIR), field-emission scanning electron microscopy (FE-SEM), energy-filtered transmission electron microscopy (EF-TEM), X-ray diffraction (XRD), thermogravimetric analysis (TGA), and differential scanning calorimetry (DSC). The results showed that the isolated CNCs had a needle-like structure with a length and diameter of 10–30 and 2–6 nm, respectively, and an aspect ratio of 5–15, respectively. Additionally, the isolated CNCs had a high crystallinity index with a good thermal stability. The findings of the present study revealed the potential of recycling waste cotton cloths to produce a value-added product.

scholarly journals A Characteristic Study of Polylactic Acid/Organic Modified Montmorillonite (PLA/OMMT) Nanocomposite Materials after Hydrolyzing

Crystals ◽  
2021 ◽  
Vol 11 (4) ◽  
pp. 376
Author(s):  
Su-Mei Huang ◽  
Jiunn-Jer Hwang ◽  
Hsin-Jiant Liu ◽  
An-Miao Zheng
Keyword(s):  
Thermal Stability ◽  
Polylactic Acid ◽  
Decomposition Temperature ◽  
Material Strength ◽  
Scanning Calorimetry ◽  
Hydrolysis Process ◽  
Twin Screw ◽  
Thermal Pressing ◽  
Organophilic Clay ◽  
Mmt Clay

In this study, the montmorillonite (MMT) clay was modified with NH4Cl, and then the structures were exfoliated or intercalated in a polylactic acid (PLA) matrix by a torque rheometer in the ratio of 0.5, 3.0, 5.0 and 8.0 wt%. X-ray diffraction (XRD) revealed that the organic modified-MMT(OMMT) was distributed successfully in the PLA matrix. After thermal pressing, the thermal stability of the mixed composites was measured by a TGA. The mixed composites were also blended with OMMT by a co-rotating twin screw extruder palletizing system, and then injected for the ASTM-D638 standard specimen by an injection machine for measuring the material strength by MTS. The experimental results showed that the mixture of organophilic clay and PLA would enhance the thermal stability. In the PLA mixed with 3 wt% OMMT nanocomposite, the TGA maximum decomposition temperature (Tmax) rose from 336.84 °C to 339.08 °C. In the PLA mixed with 5 wt% OMMT nanocomposite, the loss of temperature rose from 325.14 °C to 326.48 °C. In addition, the elongation rate increased from 4.46% to 10.19% with the maximum loading of 58 MPa. After the vibrating hydrolysis process, the PLA/OMMT nanocomposite was degraded through the measurement of differential scanning calorimetry (DSC) and its Tg, Tc, and Tm1 declined.

scholarly journals Enhancement of Antioxidant and Hydrophobic Properties of Alginate via Aromatic Derivatization: Preparation, Characterization, and Evaluation

Polymers ◽  
2021 ◽  
Vol 13 (15) ◽  
pp. 2575
Author(s):  
Smaher M. Elbayomi ◽  
Haili Wang ◽  
Tamer M. Tamer ◽  
Yezi You
Keyword(s):  
Radical Scavenging Activity ◽  
Radical Scavenging ◽  
Hydroxyl Group ◽  
Hydroxyl Groups ◽  
Gravimetric Analysis ◽  
Scanning Calorimetry ◽  
Benzoyl Group ◽  
Antioxidant Evaluation ◽  
Thermo Stability

The preparation of bioactive polymeric molecules requires the attention of scientists as it has a potential function in biomedical applications. In the current study, functional substitution of alginate with a benzoyl group was prepared via coupling its hydroxyl group with benzoyl chloride. Fourier transform infrared spectroscopy indicated the characteristic peaks of aromatic C=C in alginate derivative at 1431 cm−1. HNMR analysis demonstrated the aromatic protons at 7.5 ppm assigned to benzoyl groups attached to alginate hydroxyl groups. Wetting analysis showed a decrease in hydrophilicity in the new alginate derivative. Differential scanning calorimetry and thermal gravimetric analysis showed that the designed aromatic alginate derivative demonstrated higher thermo-stability than alginates. The aromatic alginate derivative displayed high anti-inflammatory properties compared to alginate. Finally, the in vitro antioxidant evaluation of the aromatic alginate derivative showed a significant increase in free radical scavenging activity compared to neat alginate against DPPH (2,2-diphenyll-picrylhydrazyl) and ABTS free radicals. The obtained results proposed that the new alginate derivative could be employed for gene and drug delivery applications.

scholarly journals Effect of Glycero-(9,10-trioxolane)-trialeate on the Physicochemical Properties of Non-Woven Polylactic Acid Fiber Materials

Polymers ◽  
2021 ◽  
Vol 13 (15) ◽  
pp. 2517
Author(s):  
Anatoliy Olkhov ◽  
Olga Alexeeva ◽  
Marina Konstantinova ◽  
Vyacheslav Podmasterev ◽  
Polina Tyubaeva ◽  
...  
Keyword(s):  
Specific Surface ◽  
Surface Area ◽  
Polylactic Acid ◽  
Specific Surface Area ◽  
Water Sorption ◽  
Fiber Surface ◽  
High Water ◽  
Scanning Calorimetry ◽  
Fiber Mats ◽  
Fiber Materials

Biocompatible glycero (9,10-trioxolane) trioleate (ozonide of oleic acid triglyceride, OTOA) was incorporated into polylactic acid (PLA) fibers by electrospinning and nonwoven PLA mats with 1%, 3% and 5% OTOA content. The morphological, mechanical, thermal and water sorption properties of electrospun PLA mats after the addition of OTOA were studied. A morphological analysis showed that the addition of OTOA increased the average fiber diameter and induced the formation of pores on the fiber surface, leading to an increase in the specific surface area for OTOA-modified PLA fibrous mats. PLA fiber mats with 3% OTOA content were characterized by a highly porous surface morphology, an increased specific surface area and high-water sorption. Differential scanning calorimetry (DSC) was used to analyze the thermal properties of the fibrous PLA mats. The glass transition temperatures of the fibers from the PLA–OTOA composites decreased as the OTOA content increased, which was attributed to the plasticizing effect of OTOA. DSC results showed that OTOA aided the PLA amorphization process, thus reducing the crystallinity of the obtained nonwoven PLA–OTOA materials. An analysis of the mechanical properties showed that the tensile strength of electrospun PLA mats was improved by the addition of OTOA. Additionally, fibrous PLA mats with 3% OTOA content showed increased elasticity compared to the pristine PLA material. The obtained porous PLA electrospun fibers with the optimal 3% OTOA content have the potential for various biomedical applications such as drug delivery and in tissue engineering.

scholarly journals Preparation, Thermal, and Thermo-Mechanical Characterization of Polymeric Blends Based on Di(meth)acrylate Monomers

Polymers ◽  
2021 ◽  
Vol 13 (6) ◽  
pp. 878
Author(s):  
Krystyna Wnuczek ◽  
Andrzej Puszka ◽  
Łukasz Klapiszewski ◽  
Beata Podkościelna
Keyword(s):  
Mechanical Analysis ◽  
Attenuated Total Reflection ◽  
Scanning Calorimetry ◽  
Force Microscopy ◽  
Chemical Structures ◽  
Atomic Force ◽  
Polymeric Blends ◽  
Ft Ir ◽  
Acrylate Monomers ◽  
Synthesized Materials

This study presents the preparation and the thermo-mechanical characteristics of polymeric blends based on di(meth)acrylates monomers. Bisphenol A glycerolate diacrylate (BPA.GDA) or ethylene glycol dimethacrylate (EGDMA) were used as crosslinking monomers. Methyl methacrylate (MMA) was used as an active solvent in both copolymerization approaches. Commercial polycarbonate (PC) was used as a modifying soluble additive. The preparation of blends and method of polymerization by using UV initiator (Irqacure® 651) was proposed. Two parallel sets of MMA-based materials were obtained. The first included more harmless linear hydrocarbons (EGDMA + MMA), whereas the second included the usually used aromatic copolymers (BPA.GDA + MMA). The influence of different amounts of PC on the physicochemical properties was discussed in detail. Chemical structures of the copolymers were confirmed by attenuated total reflection–Fourier transform infrared (ATR/FT-IR) spectroscopy. Thermo-mechanical properties of the synthesized materials were investigated by means of differential scanning calorimetry (DSC), thermogravimetric (TG/DTG) analyses, and dynamic mechanical analysis (DMA). The hardness of the obtained materials was also tested. In order to evaluate the surface of the materials, their images were obtained with the use of atomic force microscopy (AFM).

scholarly journals Silver Nanoparticles from Oregano Leaves’ Extracts as Antimicrobial Components for Non-Infected Hydrogel Contact Lenses

2021 ◽  
Vol 22 (7) ◽  
pp. 3539
Author(s):  
Anastasia Meretoudi ◽  
Christina N. Banti ◽  
Panagiotis K. Raptis ◽  
Christina Papachristodoulou ◽  
Nikolaos Kourkoumelis ◽  
...  
Keyword(s):  
Silver Nanoparticles ◽  
Contact Lenses ◽  
Attenuated Total Reflection ◽  
Bacterial Strains ◽  
Scanning Calorimetry ◽  
X Ray ◽  
E Coli ◽  
Polymer Hydrogels ◽  
20 Nm ◽  
And Staphylococcus Aureus

The oregano leaves’ extract (ORLE) was used for the formation of silver nanoparticles (AgNPs(ORLE)). ORLE and AgNPs(ORLE) (2 mg/mL) were dispersed in polymer hydrogels to give the pHEMA@ORLE_2 and pHEMA@AgNPs(ORLE)_2 using hydroxyethyl–methacrylate (HEMA). The materials were characterized by X-ray fluorescence (XRF) spectroscopy, X-ray powder diffraction analysis (XRPD), thermogravimetric differential thermal analysis (TG-DTA), derivative thermogravimetry/differential scanning calorimetry (DTG/DSC), ultraviolet (UV-Vis), and attenuated total reflection mode (ATR-FTIR) spectroscopies in solid state and UV–Vis in solution. The crystallite size value, analyzed with XRPD, was determined at 20 nm. The antimicrobial activity of the materials was investigated against Gram-negative bacterial strains Pseudomonas aeruginosa (P. aeruginosa) and Escherichia coli (E. coli). The Gram-positive ones of the genus of Staphylococcus epidermidis (S. epidermidis) and Staphylococcus aureus (S. aureus) are known to be involved in microbial keratitis by the means of inhibitory zone (IZ), minimum inhibitory concentration (MIC), and minimum bactericidal concentration (MBC). The IZs, which developed upon incubation of P. aeruginosa, E. coli, S. epidermidis, and S. aureus with paper discs soaked in 2 mg/mL of AgNPs(ORLE), were 11.7 ± 0.7, 13.5 ± 1.9, 12.7 ± 1.7, and 14.3 ± 1.7 mm. When the same dose of ORLE was administrated, the IZs were 10.2 ± 0.7, 9.2 ± 0.5, 9.0 ± 0.0, and 9.0 ± 0.0 mm. The percent of bacterial viability when they were incubated over the polymeric hydrogel discs of pHEMA@AgNPs(ORLE)_2 was interestingly low (66.5, 88.3, 77.7, and 59.6%, respectively, against of P. aeruginosa, E. coli, S. epidermidis, and S. aureus) and those of pHEMA@ORLE_2 were 89.3, 88.1, 92.8, and 84.6%, respectively. Consequently, pHEMA@AgNPs(ORLE)_2 could be an efficient candidate toward the development of non-infectious contact lenses.

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