Preparation and characterization of poly(lactic acid)/poly(methyl methacrylate) blend tablets for application in quantitative analysis by micro Raman spectroscopy

Poly(lactic acid) (PLA) is a biodegradable polymer that has a variety of applications, one of which is as biomaterial in surgery or as functional layers on implants, due to its compatibility with living tissue. This paper reports the possibilities of quantification of poly(lactic acid) (PLA) in a polymer matrix such as poly(methyl methacrylate) (PMMA) by micro Raman spectroscopy (MRS). Blends of amorphous poly(DL‐lactic acid) with poly(methyl methacrylate) were prepared by the procedure of dissolution/precipitation. Thermal properties of the blends such as the glass transition temperature (Tg) were characterized by differential scanning calorimetry (DSC). The PLA/PMMA blends exhibited only a single glass transition region, indicating that this system is miscible. The PLA/PMMA system obeys the Gordon–Taylor equation (Tg versus PLA content). Various concentration ratios of PLA blends were prepared to use as a basis for quantitative analysis by MRS. Intensities of the characteristic bands at 813 cm⁻¹ (νCOC of PMMA) and 873 cm⁻¹ (νC―COO of PLA) were used for the calculation. The calibration graph showed a good linear correlation with an R² value of 0.9985. On the basis of the calibration curve obtained, the determined content of several PLA/PMMA blends was in good agreement when compared with nominal contents. The limit of detection (LOD) and quantification (LOQ) were calculated by the calibration data set as signal‐to‐noise method. The relative standard deviation of this method was lower than 10% and the accuracy better than 4%. This study demonstrated that Raman spectroscopy provides an alternative non destructive method for quantitative analysis of PLA in a PMMA matrix. Copyright © 2015 John Wiley & Sons, Ltd.     

Biomineralization of electrospun poly(l-lactic acid)/gelatin composite fibrous scaffold by using a supersaturated simulated body fluid with continuous CO2 bubbling

To promote the biomineralization, supersaturated simulated body fluids (SBFs), e.g. five times SBF (5 × SBF), were usually applied. In these SBFs, however, homogeneous nucleation of Ca-P mineralites and deposition unavoidably took place owing to the HCO₃⁻ decomposition and the pH value increment, which made the prediction of bone bioactivity of substrates controversial. In this study, the classically prepared 5 × SBF was continuously bubbled with CO₂ to keep the pH value stable at 6.4 and the solution transparent, and a kind of electrospun poly(l-lactic acid)/gelatin composite fibers was used for the biomineralization study. In such a modified 5 × SBF, heterogenenous nucleation occurred dominantly and thermodynamical unstable brushites (dicalcium phosphate dihydrate, DCPD) were detected shortly on both electrospun PLLA fibers and PLLA/gelatin (1:1 in weight) composite fibers. In comparison with electrospun PLLA fibers, the sheet-like DCPD mineralites transformed into flaky carbonated calcium-deficient hydroxyapatite (CDHA) within 24 h on the PLLA/gelatin composite fibers due to the accelerating effect of gelatin component. The formed apatite coating contained much less Mg²⁺ ions than that deposited in the classical 5 × SBF. The results of this study showed that supersaturated SBFs buffered with gassy CO₂ were expected good choices for the accelerated biomineralization, and for the prediction of the bone bonding bioactivity of substrates.     

Damping,thermal, and mechanical properties of polyurethane based on poly(tetramethylene glycol)/epoxy interpenetrating polymer networks: effects of composition and isocyanate index

A series of polyurethane (PU) samples based on poly(tetramethylene glycol)/epoxy resin (EP) graft interpenetrating polymer networks (IPNs) were prepared and their damping, thermal, and mechanical properties were systematically studied in terms of composition and the value of the PU isocyanate index (R). The damping properties and thermal stability measurements revealed that the formation of PU/EP IPN could improve not only the damping capacity but also the thermal stability. Meanwhile, mechanical tests showed that the tensile strengths of the IPNs decreased while their impact strengths increased with increasing PU content. The value of R also had significant impacts on the properties of the IPNs when the PU and EP ratio was fixed, which could be an effective means for manipulating the fabrication of PU/EP IPNs. The morphologies of the PU/EP IPNs were observed by SEM and AFM characterization and the relationship between the morphologies and properties is discussed. With the results in hand, the PU/EP IPNs hold promise for use in structural damping materials.