Chuiko Institute of Surface Chemistry, 17 General Naumov Street, Kiev 03164, Ukraine.
Adv Colloid Interface Sci. 2013 Jan;187-188:1-46. doi: 10.1016/j.cis.2012.11.001. Epub 2012 Nov 15.
Experimental results on polymer, protein, and composite cryogels and data treatment methods used for morphological, textural, structural, adsorption and diffusion characterisation of the materials are analysed and compared. Treatment of microscopic images with specific software gives quantitative structural information on both native cryogels and freeze-dried materials that is useful to analyse the drying effects on their structure. A combination of cryoporometry, relaxometry, thermoporometry, small angle X-ray scattering (SAXS), equilibrium and kinetic adsorption of low and high-molecular weight compounds, diffusion breakthrough of macromolecules within macroporous cryogel membranes, studying interactions of cells with cryogels provides a consistent and comprehensive picture of textural, structural and adsorption properties of a variety of cryogels. This analysis allows us to establish certain regularities in the cryogel properties related to narrow (diameter 0.4<d<2 nm), middle (2<d<50 nm) and broad (50<d<100 nm) nanopores, micropores (100 nm<d<100 μm) and macropores (d>100 μm) with boundary sizes within modified life science pore classification. Particular attention is paid to water bound in cryogels in native superhydrated or freeze-dried states. At least, five states of water - free unbound, weakly bound (changes in the Gibbs free energy-ΔG<0.5-0.8 kJ/mol) and strongly bound (-ΔG>0.8 kJ/mol), and weakly associated (chemical shift of the proton resonance δ(H)=1-2 ppm) and strongly associated (δ(H)=3-6 ppm) waters can be distinguished in hydrated cryogels using (1)H NMR, DSC, TSDC, TG and other methods. Different software for image treatment or developed to analyse the data obtained with the adsorption, diffusion, SAXS, cryoporometry and thermoporometry methods and based on regularisation algorithms is analysed and used for the quantitative morphological, structural and adsorption characterisation of individual and composite cryogels, including polymers filled with solid nano- or microparticles.
对聚合物、蛋白质和复合材料的冷冻凝胶进行实验,并对用于材料形态、结构、吸附和扩散特性的数据分析处理方法进行了分析和比较。使用特定软件处理微观图像,可以为天然冷冻凝胶和冷冻干燥材料提供定量结构信息,这些信息对于分析干燥对其结构的影响很有用。冷冻多孔率法、弛豫率法、热孔率法、小角 X 射线散射(SAXS)、低分子量和高分子量化合物的平衡和动力学吸附、大分子在大孔冷冻凝胶膜内的扩散突破、细胞与冷冻凝胶的相互作用的研究,为各种冷冻凝胶的结构、吸附和形态特性提供了一致而全面的图像。通过这种分析,可以确定与窄孔(直径 0.4<d<2nm)、中孔(2<d<50nm)和宽孔(50<d<100nm)、微孔(100nm<d<100μm)和大孔(d>100μm)相关的冷冻凝胶特性的某些规律,这些孔的边界尺寸在经过修正的生命科学孔径分类内。特别关注天然超水合状态或冷冻干燥状态下冷冻凝胶中结合的水。在水合的冷冻凝胶中,至少可以区分五种状态的水:无束缚的自由水、弱束缚水(吉布斯自由能变化-ΔG<0.5-0.8kJ/mol)和强束缚水(-ΔG>0.8kJ/mol)、弱缔合水(质子共振的化学位移 δ(H)=1-2ppm)和强缔合水(δ(H)=3-6ppm)。可以使用 (1)H NMR、DSC、TSD、TG 和其他方法来区分,如(1)H NMR、DSC、TSD、TG 和其他方法。为了分析吸附、扩散、SAXS、冷冻多孔率法和热孔率法等方法获得的数据,开发了不同的图像处理软件,并基于正则化算法,用于对单个和复合冷冻凝胶进行定量形态、结构和吸附特性分析,包括填充有固体纳米或微粒子的聚合物。