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Radiation crosslinking of carboxymethylcellulose (CMC) with a degree of substitution (DS) from 0.7 to 2.2 was the subject of the current investigation. CMC was irradiated in solid‐state and aqueous solutions at various irradiation doses. The DS and the concentration of the aqueous solution had a remarkable affect on the crosslinking of CMC. Irradiation of CMC, even with a high DS, 2.2 in solid state, and a low DS, 0.7 in 10% aqueous solution, resulted in degradation. However, it was found that irradiation of CMC with a relatively high DS, 1.32, led to crosslinking in a 5% aqueous solution, and 20% CMC gave the highest gel fraction. CMC with a DS of 2.2 induced higher crosslinking than that with a DS of 1.32 at lower doses with the same concentration. Hence, it was apparent that a high DS and a high concentration in an aqueous solution were favorable for high crosslinking of CMC. It is assumed that high radiation crosslinking of CMC was induced by the increased mobility of its molecules in water and by the formation of CMC radicals from the abstraction of H atoms from macromolecules in the intermediate products of water radiolysis. A preliminary biodegradation study confirmed that crosslinked CMC hydrogel can be digested by a cellulase enzyme. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 78: 278–283, 2000

The objective of this study is to investigate the possibility of enhancing mechanical properties of poly(lactic acid) (PLA) samples processed by a rapid manufacturing (RM) technique by increasing PLA crystallinity degree via thermal annealing. The samples are manufactured by fused deposition modeling (FDM) at different temperatures and subsequently evaluated by three‐point bending flexural and tensile tests. The polymer processed at 215 °C is thermally annealed over its glass transition temperature in order to increase the degree of crystallinity to the maximum attainable level as measured by the differential scanning calorimetry and confirmed by X‐ray diffraction. The increase in the degree of crystallinity of FDM‐PLA enhances flexural stress of the samples by 11–17%. The study also demonstrates applicability of radiation sterilization for FDM‐PLA parts. Therefore, thermal annealing might be introduced into a standard RM technology of PLA, particularly for sterilizable customized implants, to efficiently improve their mechanical properties.

ABSTRACT:The effects of high-energy radiation on sodium carboxymethylcellulose (CMC) with a degree of substitution of 2.2 were investigated. Moderate CMC concentrations formed hydrogels by intermolecular crosslinking. Significant influences on the results of irradiation, in addition to the concentration, were the dose and dose rate and the presence of oxygen in the surrounding atmosphere. Up to a 95% gel fraction was obtained from 50 and 60% CMC solutions irradiated by an electron beam. CMC hydrogels swelled by absorbing more than 800 g of water per gram of dry gel at a low applied dose. Swelling tests of CMC hydrogels in salt solutions and in media of various pHs showed that the swelling decreased with the salt concentration and was lower at acidic pH values. Radiation yields of crosslinking and scission were calculated on the basis of gel-sol analysis. Crosslinked CMC, in the form of the hydrogel, was degraded by the action of cellulase enzyme, thereby entering the class of environmentally friendly polymers.

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This work reports on the impact of tetrakis(hydroxymethyl)phosphonium chloride (THPC) on the properties of a VIC gel dosimeter (VIC is an abbreviated acronym of VIPARCT). THPC was used as a substitute oxygen scavenger in VIC (17% N-vinylpyrrolidone, 8% N,N′-methylenebisacrylamide, 12% tert-butyl alcohol, 7.5% gelatine, 0.02% hydroquinone and an oxygen scavenger of 0.007% ascorbic acid and 0.0008% CuSO4  ×  5H2O). THPC reduced the gelation time of VIC from hours to minutes. The best composition (VIC-T) contained 14 mM THPC and a reduced gelatine concentration (5%) with respect to VIC, which allowed for gelation in about 3 min. VIC-T was characterised by the same dose sensitivity (0.176  ±  0.003 Gy−1 s−1 for VIC-T and 0.171  ±  0.002 Gy−1 s−1 for VIC), dose threshold (0.5 Gy) and dynamic dose range (0.5‒50 Gy) as VIC, and a lower linear dose range (20 Gy for VIC-T, 30 Gy for VIC) (0.47 T NMR measurements). VIC-T was stable for at least 10 days after irradiation, and 3D dose distribution was stable for over 4 months after irradiation. The dose response of VIC-T was independent of the radiation dose rate, type and energy of radiation for 6 and 15 MV photons and 12 MeV electrons. This is an improvement with respect to VIC which showed a different dose response for 6 MV photons than for 12 MeV electrons and 15 MV photons. Raman spectroscopy showed similarity in the rate of radiation-induced conversion of monomers in VIC and VIC-T, indicating interaction of THPC with gelatine in VIC-T, and showed ageing of gelatine in both dosimeters. Differential scanning calorimetry showed VIC-T stability at 0 °C–80 °C (VIC: 0 °C‒29.5 °C). The chemical polymerisation and crosslinking of gelatine with THPC is reported, the mechanism of which was analysed in detail. A comparison of N-vinylpyrrolidone-containing dosimeters is presented in this work.