Polymer blends analysis

Kadla, J.F. Kubo, S. Lignin-based polymer blends analysis of intermolecular interactions in lignin-synthetic polymer blends. Composites, Part A Appl. Sci. Manuf. 2004, 35 (3), 395-400. 

There are tests for physical properties such as deasity and hardness (qv) of plastics. Microscopy (qv) is important ia fracture analysis as well as ia analysis of the morphology of polymer systems for an understanding of polymer blend performance. 

Another example of static SIMS used in a more quantitative role is in the analysis of extmded polymer blends. The morphology of blended polymers processed by extrusion or molding can be affected by the melt temperature, and pressure, etc. The surface morphology can have an effect on the properties of the molded polymer. Adhesion, mechanical properties, and physical appearance are just a few properties affected by processing conditions. 

In a molded polymer blend, the surface morphology results from variations in composition between the surface and the bulk. Static SIMS was used to semiquan-titatively provide information on the surface chemistry on a polycarbonate (PC)/polybutylene terephthalate (PBT) blend. Samples of pure PC, pure PBT, and PC/PBT blends of known composition were prepared and analyzed using static SIMS. Fn ment peaks characteristic of the PC and PBT materials were identified. By measuring the SIMS intensities of these characteristic peaks from the PC/PBT blends, a typical working curve between secondary ion intensity and polymer blend composition was determined. A static SIMS analysis of the extruded surface of a blended polymer was performed. The peak intensities could then be compared with the known samples in the working curve to provide information about the relative amounts of PC and PBT on the actual surface. 

Characterization and control of interfaces in the incompatible polymer blends were reported by Fayt et al. [23]. They used techniques such as electron microscopy, thermal transition analysis, and nonradiative energy transfer (NRET), etc. They have illustrated the exciting potentialities offered by diblock copolymers in high-performance polymer blends. 

Thus, for the investigation of buried polymer interfaces, several techniques with molecular resolution are also available. Recently NMR spin diffusion experiments [92] have also been applied to the analysis of a transition zone in polymer blends or crystals and even the diffusion and mobility of chains within this layer may be analyzed. There are still several other techniques used, such as radioactive tracer detection, forced Rayleigh scattering or fluorescence quenching, which also yield valuable information on specific aspects of buried interfaces. They all depend very critically on sample preparation and quality, and we will discuss this important aspect in the next section. 

This second group of tests is designed to measure the mechanical response of a substance to applied vibrational loads or strains. Both temperature and frequency can be varied, and thus contribute to the information that these tests can provide. There are a number of such tests, of which the major ones are probably the torsion pendulum and dynamic mechanical thermal analysis (DMTA). The underlying principles of these dynamic tests have been covered earlier. Such tests are used as relatively rapid methods of characterisation and evaluation of viscoelastic polymers, including the measurement of T, the study of the curing characteristics of thermosets, and the study of polymer blends and their compatibility. They can be used in essentially non-destructive modes and, unlike the majority of measurements made in non-dynamic tests, they yield data on continuous properties of polymeric materials, rather than discontinuous ones, as are any of the types of strength which are measured routinely. 

Polymer/additive analysis then usually proceeds by separation of polymer and additives (cf. Scheme 2.12) using one out of many solvent extraction techniques (cf. Chapter 3). After extraction the residue is pressed into a thin film to verify that all extractables have been removed. UV spectroscopy is used for verification of the presence of components with a chromophoric moiety (phenolic antioxidants and/or UV absorbers) and IR spectroscopy to verify the absence of IR bands extraneous to the polymer. The XRF results before and after extraction are compared, especially when the elemental analysis does not comply with the preliminary indications of the nature of the additive package. This may occur for example in PA6/PA6.6 blends where... 

For polymer/additive analysis complete dissolution is not a prerequisite. Rather, the solvent should at least swell the polymer by diffusion, which allows the physically blended additives to dissolve. True dissolution occurs predominantly when polymer chain lengths are small, on the order of 5000-10 000 Da. Solvent choice for dissolution or extraction should take into account restrictions imposed by further analysis steps (compatibility with chromatographic and/or spectroscopic requirements). When microwave extraction of additives from a polymer is followed by HPLC analysis, the solvent must be compatible with the HPLC mobile phase so that solvent exchange is not required before analysis. 

On the whole, GPEC remains a technique in search for polymer/additive applications with real added value [835]. Practical applications of GPEC may be found in the analysis of polymer blends [836], laminates and packaging materials. For example, the technique can be used for determination of the impact modifier content in PS packaging material, which contains a soluble transparent rubber for transparent applications,... 

This topic has been mentioned in Section V, Failure, Defect and Contaminant Analysis, in Chapter 15, where a number of typical practical problem invetsigations were presented. Obviously the potential list of examples exhibiting different characteristics and requiring a different type of analysis is lengthy. When the sample is heterogeneous, e.g., a polymer blend or a composite, the study of the surface of a failed piece of material may reveal whether the problem is the interface of the components or that failure occurred within one of these. In particular in the case of crazing or necking orientation may have been induced, the way this can be analysed is discussed in Chapter 8. 

Multiplex CARS microspectroscopy, in conjunction with appropriate spectral analysis tools, was successfully applied to the study of phospholipid bilayer model systems [120, 121, 142, 70, 143], lipids within cells [144, 127, 145-147, 141], a single pollen grain [148], a single bacterial endophore [140], a molecular J-aggregate microcrystal [149], silicon components on a wafer [130], separated phases in polymer blends [123, 135], and concentration profiles in a microreactor [150]. 

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