Analysis of Synthetic Polymers and Rubbers - ACS Publications

Anal. Chem. 1999, 71, 61R-80R

Analysis of Synthetic Polymers and Rubbers P. B. Smith,* A. J. Pasztor, Jr., M. L. McKelvy, D. M. Meunier, S. W. Froelicher, and F. C.-Y. Wang

Analytical Sciences, The Dow Chemical Company, 1897 Building, Midland, Michigan 48667 Review Contents Pyrolysis Gas Chromatography Liquid Chromatography Mass Spectrometry Nuclear Magnetic Resonance Spectroscopy Thermal Analysis Infrared and Raman Spectroscopy Literature Cited

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This paper reviews techniques for the characterization of rubbers, synthetic polymers, and blends. Chromatographic techniques such as gas chromatography, inverse gas chromatography, pyrolysis gas chromatography, and liquid chromatography, including size exclusion chromatography, are included in this review. Also covered are references to mass spectrometry, nuclear magnetic resonance spectroscopy, and infrared and Raman spectroscopies and thermal techniques such as thermogravimetric analysis and differential scanning calorimetry. Applications include structure determination, structure-property determinations, separation and quantification of residual monomers and additives, determination of molecular weight and branching, and the study of degradation mechanisms and other thermal properties of synthetic polymers and rubbers. A majority of the cited references were obtained from literature searches and volumes of Chemical Abstracts published between October 1996 and October 1998. For the most part, this review contains references to journals published in English and readily available in the United States. PYROLYSIS GAS CHROMATOGRAPHY Pyrolysis is one of the important techniques in the study of synthetic polymers. Current trends in the development of this technique are focused in two major directions. The first is the modification of current instrumentation and analytical methods to improve the quality of analytical results for the existing applications. The second is to explore new experimental setups and different analytical approaches to find more application opportunities. Because of advances in instrumentation, computer technology, and laboratory sample preparation apparatus, several methods were integrated with these new developments to capture these advantages. For the purposes of qualitative and quantitative analysis as well as different experimental approaches, this part of the review has been roughly categorized into sections such as the improvement of instrumentation and analytical methodology for current applications and exploration of experimental setups and analytical approaches for new applications. Sometimes, it is hard to clearly separate an improvement effort from an exploration venture. An exploration venture may turn into an improvement effort once this exploration method has been used routinely. In the same way, 10.1021/a1990004f CCC: $18.00 Published on Web 04/17/1999

© 1999 American Chemical Society

an improvement effort may quickly turn into a exploration venture once new applications can be found from this improvement method. Py-GC techniques were reviewed many times during its developmental years. Within the last two years, one important article appeared which provided an extensive bibliography on the Py-GC of synthetic polymers (A1). This bibliography tabulated all the literature of Py-GC analysis of homopolymers, copolymers, microstructure, and end groups as well as pyrolytic alkylation and reactive degradation. There is another review that focused on the structural characterization of polymeric materials by Py-GC/MS (A2). This review started with the history and scope of analytical pyrolysis and then the instrumental and methodological aspects of Py-GC/ MS. Some applications to the structural characterization of various polymeric materials are discussed in detail. These include the studies of sequence distribution of polyacetals by reactive pyrolysis in the presence of a catalyst, stereoregularity of polystyrene (PS) and poly(methyl methacrylate) (PMMA), and terminal groups of various PS, PMMA, and polycarbonates (PC). Because of the developments in GC instrumentation, computers, and laboratory sample preparation apparatus, several methods have been integrated with these new developments to capture their advantages. There are developments based on pyrolysis hardware such as the utilization of different setups to perform pyrolysis as well as other thermochemical analyses. There is a development in the GC carrier gas flow programming and fast oven heat programming to speed up the GC separation. In the database application area, there is a development in the database creation for Py-GC databases to not only provide the pyrogram information but also allow for textual searches throughout the database. Py-GC/MS remains the most convenient way to qualitatively analyze polymers. The heated filament, Curie-point, and furnace are three major types of pyrolyzers used in the experiments. The standard configuration is the pyrolyzer mounted on top of the GC injection port. The GC, which is exclusively used for pyrolysis, is often equipped with a flame ionization detector (FID) and a massselective detector (MSD). Other commonly used GC detectors include the atomic emission detector (AED), flame photoionization detector (FPD), and nitrogen phosphorus detector (NPD). Besides using different types of detectors, the instrument configuration may be varied or other thermal analysis equipment may be converted to meet specific application needs. Different configurations include utilizing a programmable temperature vaporization (PTV) injector to conduct the multistep thermal desorption and programmed Py-GC experiment. Polymers were studied using a high-temperature PTV injector to thermally treat the polymer sample at different temperatures (A3). The Analytical Chemistry, Vol. 71, No. 12, June 15, 1999 61R

individual chromatograms of the various constituents of the polymeric sample were correlated with those of the final material in order to identify additives (thermal desorption) and degradation products (pyrolysis). The advantage of using the PTV injector for this purpose is that no heated transfer line and switching valves are needed. This eliminates the risk of losses of high-molecularweight components. Other advantages of the technique are simplicity, versatility, and low cost. A second configuration approach is the creation of a dual-inlet (pyrolysis and autosampler) system to flexibly use both kinds of injection systems. In a conventional Py-GC system, the pyrolyzer is interfaced on top of the GC, which blocks off the normal sample injection port. In the former configuration, the pyrolyzer is mounted differently such that it can coexist with traditional sample injection devices such as an autosampler (A4). The advantages of this configuration are that the pyrolyzer attachment does not interfere with sample introduction through the injection port, the GC system can be easily converted to a Py-GC system without mounting or dismounting of the equipment, and when operated as a Py-GC unit, the conventional sample injection port can be used as an auxiliary sample introduction route to greatly enhance the capability of Py-GC data handling in qualitative and quantitative analysis. The third development in instrument configuration is the development of a Py-GC with a movable reaction zone (A5). The device enables the thermal degradation of polymers inside a capillary precolumn and transfer of the reaction zone into a column oven. The pyrolysis procedure described protects thermally sensitive compounds prior to pyrolysis, prevents the process of irreversible condensation of high-boiling pyrolysis products during the chromatographic process, and eliminates extracolumn effects on peak broadening. The use of a thermal extraction unit for a furnace-type pyrolysis interface was studied for the suitability of polymer analysis (A6). Pyrolysis is achieved by accurate temperature programming of the pyrolysis cell from ambient to very high temperatures. The suitability of the thermal extraction unit for use as a pyrolyzer was evaluated by analyzing several model polymers. The results obtained demonstrated that this unit can be used as a pyrolyzer. The main advantages of the technique are good reproducibility, minimum secondary reactions, capability for quantitative analysis, and minimum sample handling. The development of fast-GC has been on going for several years (A7-A11). Recent reports (A12) show that the concept and technology development have reached a mature stage. Py-GC is one type of application that utilizes the GC for separation of pyrolysates. A Py-fast-GC development has also been reported in which the development of fast-GC for pyrolysis applications in synthetic polymers was summarized (A13). Several examples demonstrated the advantages of Py-fast-GC. Derivatization is a well-known and well-developed technique in the chromatographic analysis area. Derivatization is used to enhance chromatographic separation and/or detection for those compounds not suitable for separation/detection originally. The same concept has been adapted to Py-GC and Py-GC/MS for polymer analysis. However, the scope of the derivatization should be expanded from the conventional chromatographic analysis point of view to include the pyrolysis process. The derivatization 62R

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reaction serves not only to enhance the chromatographic separation and/or detection but also to alter the normal thermal degradation pathway to improve the pyrolysis process for qualitative and quantitative analysis. In Py-GC, the derivatization does not have to be limited to the “precolumn” and “postcolumn” situation. The derivatization reaction may be performed selectively during the pyrolysis process such that it may be categorized into “prepyrolysis” and “postpyrolysis”. The postpyrolysis derivatization techniques for the Py-GC analysis of polymers have been developed for a long time. For example, the pyrolysates can be derivatized “simultaneously”, “in situ”, or “on column” to reduce the difficulties of polar pyrolysates being separated in a nonpolar capillary column (A14). In another example, unsaturated aliphatic alkenes can be derivatized by hydrogenation to simplify the number of fragments and enhance structural identification capabilities (A15). In general, these techniques modify the pyrolysates produced by the pyrolysis process. Postpyrolysis derivatization implies that during the course of pyrolysis, there is no intention of altering the thermal degradation through derivatization. The derivatization techniques of the postpyrolysis category have experienced additional development in pyrolysis analysis of polymers. The major portion of the derivatizations involve the methylation of alcohols and acids. The most popular methylation regents are tetramethylammonium hydroxide (TMAH) and trimethyl sulfate (TMS). The purpose of derivatization is to modify the pyrolysates in order to have better separation and detection results. In situ hydrolysis/methylation pyrolysis gas chromatography for the characterization of polymers was studied (A16). Some parameters that influenced in situ methylation by TMAH during pyrolysis were explored. Both pyrolysis temperature and excess TMAH (pH effect) influenced the methylation of carboxy, aromatic, amino, and hydroxyl functional groups. The solvent of TMAH, i.e., methanol or water, significantly affected the methylation for the polyaramids but hardly influenced other model compounds studied. The explanation given assumed a transesterification mechanism rather than hydrolysis/methylation. However, N-methylation prior to the decomposition of polyaramids may not be excluded. The characterization of copolymer-type PC by reactive Py-GC in the presence of TMAH was reported (A17). In this study PyGC in the presence of TMAH was successfully used to the determine the chemical composition and end group content of thermally and light-stabilized PC copolymers. The Py-GC with postderivatization of these PC copolymers enabled almost quantitative detection of the constituents of the polymer sample as their methyl ethers. On the basis of these peak intensities, the compositions as well as the number-average molecular weights were correctly estimated without using any reference polymer. The reagent used in the postpyrolysis does not have to be limited to organic alkali compounds, as other types of reagents have been used for this purpose. The sequence distribution study of polyacetals by postderivatization Py-GC in the presence of cobalt sulfate is an example (A18). In this study, postderivatization of the copolymer of polyacetals in the presence of cobalt sulfate together with Py-GC was applied to the study of sequence

distribution. The ethylene oxide content and the distribution of ethylene oxide sequences up to seven monomer units in the polymer chain were evaluated on the basis of peak intensities of cyclic ethers in the pyrogram. These values were in good agreement with those obtained by hydrolysis. The composition of alternating olefin-carbon monoxide copolymers and their derivatives was studied through derivatization by Py-GC/MS (A19). An alternating copolymer of carbon monoxide and olefins (ethylene, styrene, and norbornadiene) and their modified polymers with primary amines, P2S5, or P2O5 were prepared. In each pyrolysis, hydrocarbons arising from the corresponding olefin comonomer were detected as the volatile products. Py-GC/MS confirmed that these 1,4-arrangements of the ketonic groups in the alternating copolymers were converted into pyrroles, thiophene, and furan-containing chains with primary amines, P2S5, and P2O5, respectively. The oxygen-containing groups, which remained intact during the modification with P2S5, were detected in small amounts in the pyrolysates. Composition (qualitative and quantitative) analysis is based on the relative intensity of monomers or monomer-related pyrolysates which were produced from pyrolysis. This type of analysis has been developed for a long time. Recent developments focused on the enhanced detection for low-level chemical species in the polymers. The low-level comonomer or other additives that were hard to separate from the polymers may be identified by direct pyrolysis. To effectively detected those chemical species, other techniques besides pyrolysis are required. The other techniques are needed mainly for separation and reconcentration purposes. A pyrolysis with trapping scheme was developed in order to determine low-level acrylic acid and methacrylic acid in emulsion polymers (A20). The advantages of the trapping setup are the flexibility of trapping solvent selection, sample accumulation, and the option of choosing the separation technique after trapping. Low levels of acrylic acid and methacrylic acid were qualitatively detected in an emulsion polymer by this method. A similar technique was applied to determine acrylamide monomer in an emulsion polymer (A21). The trapped pyrolysate mixture was separated and identified by a GC/MS system. Because many other low-level fragments elute at the same time, a single ion monitoring technique must be used to clearly catch the peak. It was demonstrated in this study that the trapping technique is an effective means to detect low-level monomers of the acrylamide and methacrylamide in emulsion polymers. The detection of low-level monomers not only can be approached by this trapping technique but also can be achieved by derivatization. The qualitative study of fumaric acid and itaconic acid in emulsion polymers by Py-GC is an example (A22). Fumaric acid and itaconic acid were derivatized by methylamine to form cyclic imide-type functional groups. The derivatized products produced a stable pyrolysate which was detected at relatively low concentration. Most additives are organic molecules which can be analyzed by extraction from polymers followed by GC or LC methods. When an additive is polymeric in nature, an extraction followed by a GC/LC method will not work. For this reason, a Py-GC method was developed to explore low levels of polyacrylamide in poly(vinyl alcohol) (A23). Because of the large number of pyrolysates produced from the poly(vinyl alcohol) matrix, an

atomic emission detector was used to selectively detect the nitrogen-containing fragments from pyrolysis of polyacrylamide. A study of composition analysis of multicomponent acrylic resins by Py-GC was presented (A24). Py-GC was used to analyze the composition of ethyl acrylate-butyl methacrylate copolymers and ethyl acrylate-styrene-ethyl methacrylate terpolymers. The characteristic peaks of the pyrolysis products, up to the pentamers, were almost completely separated on the pyrogram. The quantification of end groups in anionically polymerized PMMA by PyGC was studied (A25). The molecular weight distribution was determined due to the fact that the characteristic fragments reflected the end groups of the PMMA. These end groups were identified by comparison with those of a radically polymerized PMMA together with the mass spectra of the characteristic peaks on the resulting pyrograms. Py-GC/MS was used to investigate the degree of cure of polyimide systems (A26). Pyrolysis products of both initial components and the cured polymer were identified. Changes in the pattern of pyrolysis products could be related to the progress of polymerization. Chromatography databases, such as for GC and LC, based on the retention time have been available for many years. Because chromatography techniques are focused on separation, the peaks in a chromatogram are representative of the number of components in that mixture and relative elution/retention order of that mixture under that experimental conditions. The elution/retention time of peaks can be affected by many factors. These factors include type of mobile phase, type of stationary phase, thickness of stationary phase, mobile-phase flow rate, and elution temperature. Because the retention time is highly dependent on experimental conditions, it may not be suitable as a searchable parameter in a database. To solve this problem, there have been different types of retention indexes developed. The most commonly accepted index is the Kovats retention index. More recently, the concept of retention indexes has been further developed in the chromatography field (especially in GC) to accommodate various experimental conditions. Even with retention indexes, there are still difficulties when comparing chromatograms obtained from different types of stationary and mobile phases. This is one of the major reasons why there is no universal chromatography database widely available. However, there are small chromatography databases for specific groups of compounds for specific purposes. As mentioned above, the chromatography technique is really aimed at the separation of mixtures. The mobile phase, stationary phase, and experimental conditions are optimized to obtain the best separation. These parameters should not be standardized to obtain a consistent retention time. Instead, the reference chromatogram in the database should be used mainly to determine the separation phases and experimental conditions, the elution/ separation order, the components in the mixture, and the relative abundance of components. If these are the most important parameters in the chromatography database, the database design should concentrate on how to find the desired reference chromatograms and the information about those components with minimum effort. The creation and maintenance of a Py-GC database of polymers was previously described. However, these databases are in book form (A27) as a collection of chromatograms (pyrograms), in an Analytical Chemistry, Vol. 71, No. 12, June 15, 1999

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electronic (A28) or hard copy format (A29). The depth of information included is limited, and the search capability is restricted to a polymer index in the database or library. The users have to possess the electronic files or a book to have the database available. To create and maintain a chromatography database in the electronic form, there are issues that have to be addressed. The issues include inputting data from different sources, maintaining (add, delete, and modify the entries) the database, access/ distribution management, compatibility with other similar databases, potential to integrate with other databases, access from different computer platforms, and cost of software. A hypertext markup language (HTML)-based database for distribution on the Web for chromatographic database creation and maintenance was developed (A30). In this development, a Py-GC database was used as an example to demonstrate the structure and the architecture of a chromatographic database. The database program, the users, and database interface as well as the distribution issues of a database were discussed. The development of Py-GC for new applications includes the characteristic study of copolymer structures and another type of derivatization technique. In copolymer structure determination, pyrolysis was able to explore the number-average sequence length of each monomer in the copolymer using a statistical approach. Pyrolysis was also used to study the stereoregularity of the homopolymers by making use of the tetramers or higher oligomers. In the derivatization technique, the polymer of interest was derivatized before the pyrolysis in order to have favored pyrolysates for qualitative and quantitative analysis. Another development in derivatization technology is of the prepyrolysis type. The purpose of this type of derivatization is to convert the functional group in the polymer in a design way to obtain a favorable thermal degradation pathway during pyrolysis. These favorable pathways normally utilize a major monomer or monomer-related fragment to allow for easier qualitative and quantitative analysis. The major difference between the prepyrolysis derivatization and postpyrolysis derivatization is that the polymer backbone should be stable enough to resist the attack from the derivatization reagent in prepyrolysis derivatization. Pyrolysis is merely the mechanism to decompose the polymer to fragments. In the prepyrolysis derivatization, the main considerations of this modification or derivatization are four-fold: (1) Ease and convenience; the derivatization reaction takes place without rigorous conditions such as heating the sample to high temperature or reacting in high pressure. (2) Reduced interference from surrounding materials; most derivatization reagents for primary amines are hydrogen sensitive, which means these reagents cannot be used in aqueous solutions or chemicals with alcohol or acid functional groups. (3) The final product will degrade with a favorable thermal degradation pathway. The derivatization reaction will produce a stable functional group. Under thermal degradation, this derivatized polymer will depolymerize with either an unzipping pathway or a major fragment-producing pathway. (4) The major monomer or fragment produced either by the unzipping reaction or by monomer-related chain cleavage should be suitable for GC separation and detection. For example, the monomer or fragment should be a nonpolar compound when a nonpolar capillary separation column is used. The elution time of 64R

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the fragment should not be so fast as to lose the resolution from other pyrolysates in the separation. At the same time, the elution time should not be too long, which would waste analysis time. A thermal degradation pathway reselection study of poly(methacrylic acid) through derivatization (A31) demonstrated the value of prepyrolysis derivatization in Py-GC qualitative and quantitative analysis. The pyrolysis of poly(methacrylic acid) produced a number of pyrolysates that reflected the unzipping degradation as well as the random chain session and recombination. If the polymer has been derivatized by TMAH to convert the acid functional group to methyl ester, the thermal degradation of PMMA only produces one major fragment which is the methyl methacrylate monomer. In the same study, several copolymers containing low levels of methacrylic acid were successfully identified by this prepyrolysis derivatization technique. There are two major developments in the area of structure determination of polymers by Py-GC. The first one is the structure (the number-average sequence length) determination for copolymers through analysis of trimer fragments. The second is the structure (stereoregularity) determination for homopolymers through analysis of tetramers or high-oligomer fragments. The copolymer structure or the monomer arrangement in the polymer chain can be determined by the triad intensities that have been studied previously, especially with the 13C NMR technique. This concept has been adapted to the Py-GC study of copolymer structures. The study of a styrene-butyl acrylate copolymer system (A32) demonstrated that the statistical distribution of triads can be correlated to the trimers obtained from Py-GC. If all eight trimers are well resolved in the pyrogram and the peak area can be obtained, the number-average sequence length as well as composition can be calculated from these trimer peak intensities. In many other polymer cases, because of the stability of the trimer components, they do not always contain all the trimer peaks in the pyrogram. An example is the styrene-methyl methacrylate copolymer system (A33). The dimers and trimers of methyl methacrylate do not normally exist in the pyrogram under any pyrolysis conditions. However, the structure information still can be obtained by utilizing the monomer peak intensity to generate the composition along with the information obtained from other trimers. The trimers produced from pyrolysis of polymers are not always fragments with the three original monomer units bonded together. Sometimes, the trimers may go through a decomposition to lose certain easy to lose fragments to form more stable compounds. An example is the vinyl chloride-vinylidene chloride copolymer system (A34). The pyrolysis mechanism involves a dehydrohalogenation reaction to form benzene, chlorobenzene, dichlorobenzene, and trichlorobenzene. With the knowledge of monomer reactivities and polymerization kinetics, a correlation can be made between the triad distribution of the polymer to that detected in the pyrogram. The copolymer structure as well as composition can be elucidated. Polymeric structure determination does not have to be limited by the copolymer system. Other polymers that are produced by other methods may be treated as a copolymer system consisting of two different types of monomers. Chlorinated polyethylene is a good example (A35). In some circumstances, a chlorinated

polyethylene system can be considered as a copolymer system of vinyl chloride and 1,2-dichloroethylene. By examining the appropriate fragments that correspond to the trimer combination of vinyl chloride and 1,2-dichloroethylene, one can utilize a statistical formula to calculate the number-average sequence length and composition. One can also explore the chlorine content as well as the arrangement of chlorine atoms in the polyethylene chain. The polymer structure study heavily depends on the production of trimers during pyrolysis. Certain types of monomers do not form stable fragments after pyrolysis. An example is maleic anhydride. To study the structure and composition of a styrenemaleic anhydride copolymer, a derivatization method was developed (A36). The anhydride functional group was derivatized with methylamine to form a cyclic imide functional group, allowing the structure and composition to be studied. In terms of structure (stereoregularity) determinations, the first example is the stereoregularity study of PS (A37). Py-GC/MS was able to detect and identify diastereoisomers such as tetramers and pentamers. The minimum requirement for a diastereoisomer is the inclusion of more than two asymmetric carbons in the molecule. This means that tetramers are the smallest possible candidates. To allow quantitative interpretation of data, the PyGC method was calibrated by a set of standards with known tacticity (by NMR). The second example is the determination of the tacticity of various stereoregular PMMA materials (A38). The experiment was achieved by separating the associated diastereometric tetramers. In this study, stereoisomers at slightly shorter retention time are also detected. Using the combination of two diastereoisomers, in addition to other stereoisomers, the ratio of different tacticities can be calculated. Again, these values are in a very good agreement with NMR data. In recent years, several different configurations of instrumentation were developed to accomplish pyrolysis by several similar thermal analysis devices. In addition to the conventional qualitative and quantitative analysis, which is based on the relative intensity of monomers or monomer-related fragments, structure analysis has been revisited/developed and has become new territory for Py-GC. Structure analysis includes the exploration of monomer arrangement in the copolymer system, such as the numberaverage sequence length and various stereoregular distributions in homopolymers. The development of derivatization techniques continues to grow in order to match the demand of different types of applications. In addition to the traditional postpyrolysis derivatization techniques, prepyrolysis derivatization techniques have been developed in order to effectively reselect degradation pathways to achieve the purpose of the analysis. To perform GC experiments in a more efficient fashion, the development of fast-GC has been ongoing for several years. The experimental time can be decreased from an average of 50 min to approximately 5 min. In addition to the improvements in the GC oven heating speed and programmable flow control, the incorporation of cyrotrapping with fast-GC may further reduce the experimental time to 1-3 min. In a similar manner, if the pyrolysis can be incorporated with fast-GC in every case, Py-GC can be performed exclusively in the fast fashion. This will certainly

encourage more development in instrumentation as well as applications in synthetic polymer analysis. LIQUID CHROMATOGRAPHY A book concerning the topic of high-performance liquid chromatography (HPLC) of polymers was published in 1997 (B1). The book includes chapters covering the topics of thermodynamics of polymer chromatography, equipment and materials, size exclusion chromatography (SEC), liquid adsorption chromatography (LAD), liquid chromatography at the critical point of adsorption, and two-dimensional liquid chromatography. The application of SEC and HPLC to the characterization of synthetic polymers, oligomers, and rubbers was reviewed (B2). The analysis of polymers and biopolymers by SEC was reviewed (B3). Fundamental developments and selected applications of SEC and related separation techniques were reviewed (B4). The Handbook of Instrumental Techniques in Analytical Chemistry included a chapter concerning techniques for determining polymer molecular weight with emphasis on SEC (B5). High osmotic pressure chromatography (HOPC), a technique for preparative- and processscale separations of polymers according to molecular size, was reviewed (B6). On-line coupling of nuclear magnetic resonance spectroscopy to chromatographic separation methods including applications in polymer characterization was reviewed (B7). SEC coupled to a chemiluminescent nitrogen detector for compositional and molecular weight characterization of cationic polyelectrolytes was reviewed (B8). A comprehensive analysis of data reduction in triple detector SEC was published (B9). Industrial, high molar mass, grades of linear low-density polyethylene, high-density polyethylene (HDPE), and polypropylene were characterized by SEC in methylcyclohexane at 90 °C (B10). Commercial HDPE and ultrahigh-molecular-weight polyethylene were characterized by SEC at 160 and 170 °C (B11). Apparent molecular weights (based on PS calibration) of repeatedly extruded poly(ethylene terephthalate) samples were determined by SEC with chloroform as the eluent (B12). Variables affecting the yield in reactions of polymeric organolithium species with chlorosilane coupling agents were studied by SEC (B13). A new SEC method employing an eluent of 8 parts dimethylformamide (DMF), 1 part triethylamine, and 1 part pyridine was developed for characterizing the living anionic homopolymerization and block copolymerization of (tert-butyl methacrylate) with 4-vinylpyridine (B14). The SEC behavior of PMMA containing sulfate terminal end groups and poly(acrylic acid) was investigated in DMF and DMF containing LiBr (B15). Molar mass distributions of poly(vinyl alcohol) were determined by SEC using dimethyl sulfoxide as the eluent (B16). SEC was used to study the degradation kinetics of poly(2-hexyne) (B17). The molecular size distributions of pregel clusters of poly(propylene oxide) were studied by SEC (B18, B19). Phenol-formaldehyde resol resins (B20) and novolac resins were studied by SEC (B21). The molar mass distributions of aliphatic oligoamides were determined by SEC in methylene chloride (B22). The results of an intralaboratory statistical evaluation of a high-temperature SEC technique for polyamides 6, 11, and 12, using benzyl alcohol as the eluent, were presented (B23). Oligo(lactone) macromonomers were characterized by SEC (B24). Analytical Chemistry, Vol. 71, No. 12, June 15, 1999

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Aqueous SEC was used to monitor the interaction between liposomes and anionic polyelectrolytes (B25). The anionic polyelectrolyte poly(N-vinylpyrrolidone-co-maleic acid) was analyzed by SEC (B26). The permeation of small charged colloids into cavities of like charge was investigated by studying the SEC behavior of carboxyl-terminated dendritic polymers on porous glass stationary phases (B27). SEC coupled to infrared spectroscopy was used to study polymer composition as a function of SEC elution volume (B27), short-chain branching in polyolefins (B28), commercial adhesives (B29), preferential solvation effects (B30), and postcure reactions in polyurethanes (B31). Microcolumn SEC was coupled to matrixassisted laser desorption/ionization (MALDI) time-of-flight mass spectrometry for direct determination of molecular weight and end groups in SEC fractions of PC (B32) and PMMA (B33). SEC fractions of PS, poly(butyl acrylate), PC, polyester, and methacrylate-methacrylic acid copolymer (B34), poly(dimethylsiloxane) (B35, B36), epoxy copolymers (B37), and copolyesters of butylene adipate, butylene succinate, and butylene sebacate (B38) were collected and characterized off-line by MALDI. SEC and MALDI were used to determine the molecular weight distributions of lowmolecular-weight surfactants (B39). Macromonomers containing glycidyl and butyl methacrylate were characterized by SEC coupled to Fourier transform mass spectroscopy (B40). The oxidative changes in chemical structure of styrene-butadiene copolymers were studied by SEC coupled to a UV-visible absorbance diode array detector (B41). Ultraviolet absorbance and differential refractive index detectors were used in conjunction with SEC to study the copolymer composition of chlorinated butylrubber/PS comb graft copolymers as a function elution volume (B42). SEC/IR and SEC NMR were used to study OHterminated poly(ether sulfone) oligomers (B43). Quantitation of copolymers and blends using dual concentration detector SEC was discussed (B44). Temperature gradient HPLC was used to separate PS according to molecular weight (B45-B47). Thermal field flow fractionation (TFFF), SEC, and light scattering were used to determine the molecular weight distributions of anionically polymerized p-methoxystyrene, p-methylstyrene, p-chlorostyrene, and p-cyanostyrene (B48). TFFF and SEC/multiangle laser light scattering (MALLS) were used to study the thermal diffusion coefficients of PS, poly(tert-butylstyrene) (PtBS) and PS/PtBS copolymer microgels (B49). The retention behavior of poly(styrene-co-methyl methacrylate) and poly(styrene-b-isoprene) in TFFF and SEC was studied (B50). SEC fractions of blends and copolymers of PS and poly(ethylene oxide) were cross fractionated by TFFF (B51). Electrical field flow fractionation and HPLC were used to characterize polyelectrolytes containing grafted hydrophobic ligands (B52). Enhanced fluidity liquid mobile phases comprising tetrahydrofuran (THF) and CO2 were used in the SEC mode to separate PS (B53, B54). In addition to SEC-based separations, enhanced fluidity THF/CO2 was used with packed capillaries in the critical mode to characterize carboxy-terminated PS and PS/ poly(styrene-co-methyl acrylate) blends (B55). HOPC was performed with controlled-pore glass as the separation medium to fractionate PMMA by molecular size (B56). A technique for detecting local polydispersity (heterogeneity in the types of molecules present at a given elution volume) in 66R

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SEC/light scattering (LS)/differential viscometry (DV) experiments was presented and applied to PS homopolymer and blends of PS with poly(2,4,6,-tribromostyrene) (B57). The interdetector delay (IDD) in SEC/DV experiments was studied as a function of polymer concentration and eluent composition in the analysis of PMMA and PS narrow molecular weight fraction standards (B58). Various techniques for determining the IDD in SEC/LS/ DV experiments were compared in the analysis of a variety of broad molecular weight distribution polymer samples (B59). The effect of IDD on absolute molecular weight calibration in the SEC/ LS analysis of narrow molecular weight distribution samples was discussed (B60). SEC/LS/DV was used to study the dilute solution properties of the polymeric antitumor drug carrier poly[(N-(2-hydroxypropyl)methacrylamide]/Paclitaxel conjugate (B61). SEC/MALLS was used to characterize carboxymethyl methyl cellulose (B62). SEC/MALLS was used to determine branching ratios (g′ and g) for low-density polyethylene samples (B63). An SEC/MALLS procedure for determining polydispersity was applied to narrow-molecular-weight PS standards (B64). SEC/ MALLS was used to determine molecular weights and root-meansquare radii of poly[bis(carboxylatophenoxy)phosphazene] and its reactive precursor polydichlorophosphazene (B65). Conventional SEC with off-line MALLS was used to characterize starbranched poly(styrene-b-butadiene-b-styrene) (B66). SEC/MALLS was used to study molecular conformation, molecular weight, and polydispersity of the photodegradation products of poly(phenylmethylsilane) (B67). Two separate eluents, toluene and THF, were used in SEC/LS experiments to characterize molecular weight and composition of PMMA grafted with poly(dimethylsiloxane) (B68). The degradation of high-molecular-weight PS during SEC separation was investigated by SEC/LS, and the molecular weight results were compared to those determined by LS alone (B69). The micellization behavior of PS-b-PMMA in 1,4-dioxane/cyclohexane was studied by SEC/LS (B70). Polyamide-6 and poly(ethylene terephthalate) were characterized by SEC/LS using 1,1,1,3,3,3,-hexafluoro-2-propanol as the eluent (B71). A sample pretreatment approach for preparing aggregate-free poly(vinyl chloride) solutions in THF was proposed and studied by SEC/LS (B72). SEC and off-line static and dynamic LS were used to characterize the weight-average molecular weights, second virial coefficients, and z-average translational diffusion coefficients of poly(aryleneethynylene)s (B73). A custom-built, single-capillary viscometer (SCV) was compared to a bridge-style viscometer for use as a molecular weight-sensitive detector in SEC and the major sources of error for both detectors were discussed (B74). Fast Fourier transform filtration was used as a means of reducing the pump noise in the SCV traces in multidetector SEC characterization of a variety of organic-soluble and water-soluble polymers (B75). SEC and off-line vapor pressure osmometry were used to determine molecular weights of hydroxy-terminated polybutadiene (B76). Laboratory robotics were developed to automate the sample preparation procedure for high-temperature SEC/LS analyses (B77). Liquid chromatography at the critical point of adsorption was used to separate blends of poly(alkyl methacrylates), and a viscosity detector was used in conjunction with the MarkHouwink--Sakurada constants obtained at the critical eluent composition to determine the molecular weights of the eluting

blend components (B78). A variety of techniques including SEC, liquid chromatography at the critical point of adsorption, and light scattering were used to characterize graft copolymers of PS and poly(ethylene oxide) (B79). Copolymers comprising blocks of polyTHF and PMMA were characterized by liquid chromatography at the critical point of adsorption (B80). The chromatographic behavior of the water-soluble polymers pullulan, polyacrylamide, and poly(ethylene glycol) was studied under limiting conditions of solubility and limiting conditions of adsorption (B81). Blends of poly(styrene-co-acrylonitrile) with poly(ethylene-co-propyleneco-diene) were characterized by SEC with UV and DRI detectors, which allowed for the determination of average blend composition as a function of elution volume, and by precipitation LC, which allowed for complete separation of the blend components (B82). Full adsorption/desorption chromatography (FAD) was used to physically separate binary component blends of PS with PMMA and PS with poly(vinyl acetate) and was coupled to SEC in order to separate the blend components by size (B83). FAD/SEC was also applied to three- and four-component blends comprising combinations of PS, PMMA, poly(vinyl acetate), and poly(ethylene oxide) (B84, B85). A multistep process for separating vinyl chloride oligomers by degree of polymerization and then isomeric purity was developed (B86). HPLC coupled to UV absorbance and mass spectrometric detectors was used to separate and characterize nonylphenylethylene oxide oligomers (B87). Cyclic oligomers of poly(ethylene terephthalate) were characterized by HPLC coupled to mass spectrometry (B88). Gradient HPLC was used to separate polyester oligomers (B89). The retention behavior of low-molecular-weight PS and low-molecular-weight polyester resin in reversed-phase HPLC was studied (B90). The retention behavior of low-molecular-weight, crystalline polyesters was studied by gradient polymer elution chromatography under reversed-phase conditions (B91). Carboxy-terminated oligostyrenes were separated by gradient HPLC and characterized by MALDI-mass spectrometry (B92). The elution behavior of lowmolecular-weight poly(ethylene glycol), its mono and dimethyl ethers, and poly(propylene glycol) was studied by reversed-phase adsorption chromatography (B93). Derivitization with 3,5-dinitrobenzoyl chloride followed by normal-phase HPLC was used to separate ethylene glycol oligomers (B94). Liquid chromatography at the critical point of adsorption and SEC were coupled to MALDImass spectrometry to characterize the thermal degradation products of oligo(L-lactide) (B95). MASS SPECTROMETRY This portion of the review will cover topics pertaining to the application of mass spectrometric techniques to the characterization of polymers and rubbers. The Handbook of Instrumental Techniques For Analytical Chemistry has a series of chapters devoted to mass spectrometry. The handbook includes chapters on the mass spectrometry of volatile analytes (C1), high-resolution MS of volatiles and nonvolatiles (C2), GC/MS (C3), fast atom bombardment (FAB), and liquid secondary ion mass spectrometry (SIMS) (C4), HPLC electrospray ionization MS (C5), and laser mass spectrometry (C6). Each chapter includes a description of the operation and applications of the various mass spectral techniques.

Much of the emphasis in the research area of polymer mass spectrometry over the past two years has been in attempting to optimize MALDI techniques. Two major problems in MALDI are mass discrimination effects and molecular mass distribution inaccuracies. Mass discrimination effects were investigated in MALDI-MS (C7). The molecular mass distribution was found to be extremely sensitive to ionization conditions, such as laser power, and to detector conditions. Criteria were suggested for selecting the ion kinetic energy for minimizing distortion of the spectra. It was noted that the criteria would be different for different types of mass spectrometers. In addition, ionization efficiency differences were observed between low- and higher-mass oligomers, leading to further mass discrimination effects. Mass discrimination and poor reproducibility were addressed in another MALDI-time-of-flight (TOF) study where binary solvent systems were used to analyze PMMA (C8). The use of binary solvent systems helped demonstrate that the presence of a second solvent, such as water, was a major cause of mass discrimination and reproducibility problems. This effect also varied with the matrix used and the main polymer solvent used. The study suggested ways in which the second solvent problem could be addressed. Mass discrimination is more of a problem with high-mass oligomers (C9). MALDI-TOF was used to measure the molecular weight distribution of polydisperse PMMA to help assess this phenomenon. Detector saturation caused by matrix-related ions and low-mass oligomers, which are difficult to remove from a spectrum, was determined to be a major factor. Use of different matrixes also contributed to the mass discrimination problem. Similar studies indicated that sample preparation can have a significant impact on measuring Mn values (C10). Multimer formation and cation inclusion were also listed as contributing factors. Instrumental factors of mass discrimination were also studied (C11). Improved resolution and mass accuracy were demonstrated using time-lag focusing MALDI-TOF MS (C12). The upper mass limit of oligomer resolution was extended using this method. However, the overall resolution of polymer spectra was still found to be dependent on the matrix used and sample preparation methods. Improvements in consistency of sample preparation were achieved with a recent innovation involving the use of a robotic interface for polymer analysis using microscale SEC/MALDI-TOF MS (C13). The MALDI matrix solution is coaxially added to the column effluent and spotted onto MALDI targets in a robotic interface. Each spot corresponded to a 10-s elution window from the SEC. MALDI is usually favored over electrospray ionization (ESI) as a technique for polymer analysis because the spectra obtained from ESI are typically complex because of charge-state complications. However, ion-molecule reactions in a quadrupole ion trap have been used as an effective means of reducing the chargestate distribution complexity of spectra generated using ESI (C14). MALDI-FTICR MS was used to determine the block length distributions of poly(oxypropylene) and poly(oxyethylene) block copolymers (C15). The experimental data showed a distorted molecular weight distribution. A correction algorithm was develAnalytical Chemistry, Vol. 71, No. 12, June 15, 1999

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oped that when applied to the data yielded the correct molecular weight distribution. Because of the importance of obtaining accurate molecular weight distributions using mass spectrometry, various comparisons were made using different techniques. A few examples are discussed here. SEC and MALDI-TOF MS were compared in the analysis of hydroxylated polybutadienes (C16) and SRM 1487, a low-molecular-weight PMMA (C17). Also, low-molecular-weight polymers of polystyrene and poly(ethylene glycol) were analyzed by both API-LC/MS and MALDI-TOF MS (C18). Low-molecular-weight copolymers were analyzed by MALDI MS, and it was determined that detailed structural information could be obtained from a copolymer mass spectrum, provided that the end group masses and repeat units were know in advance or could be determined (C19). MALDI-TOF FTMS has been demonstrated for the analysis of hydrocarbon polymers (C20). Polyisoprene, polystyrene, and polybutadiene were analyzed using an FTMS with a 3-T magnet, an upper mass range of 6000 amu, and a matrix of DHB and silver nitrate (to produce silver-cationized oligomers). Ion trapping discrimination was observed for molecular weight distributions above 2500 amu, but integral reconstruction procedures were demonstrated to reconstruct true polymer profiles. MALDI-collision-induced dissociation (CID) was utilized to determine structural information from poly(alkyl methacrylate)s (C21). A tandem hybrid sector-TOF instrument was used. Useful end group information, which is essential to defining the properties of the polymer, was inferred from the data. The fragmentation patterns of a series of poly(dimethylsiloxane)s (PDMS) were investigated using TOF-SIMS (C22). The lowmass range was characterized by extensive fragmentation, whereas the relative intensity of cyclic fragments increased with increasing molecular weights. Investigations of the distribution of PDMS segment lengths on surfaces of copolymers such as poly(dimethylsiloxane-urethane) (PU-DMS)-segmented copolymers were also performed (C23). Additives analysis is important from the perspective of both distribution in a polymer matrix and determination of the presence in the polymer. MALDI-TOF MS was used in combination with supercritical fluid extraction to analyze UV stabilizer and antioxidant additives (C24). The spectra of the UV stabilizers Tinuvin 622LD and Chimassorb 944LD showed oligomeric components were present. The antioxidants Irganox 1076, Irgapos 168, and Irganox 1010 were all detected in the MALDI-TOF spectrum from an LLDPE extract. A thermal vapor deposition method for sample preparation was used in conjunction with MALDI-MS to determine the molecular weights of insoluble sorbitol derivatives (C25). The sorbitol derivatives, which are nucleating agents, were deposited on ferrulic acid microcrystals prior to MALDI-MS. No thermal decomposition of the derivatives was observed during analysis. UV stabilizers and antioxidants were successfully detected in poly(oxymethylene) and poly(vinyl chloride) (PVC) using spatially resolved in situ analysis by two-step laser MS (C26). Additives analysis from PP and poly(ethylene tetraphthalate) (PET) were not successful because these polymers were weakly absorbing of the laser light and showed only laser melting. Depth profiling was achieved in poly(oxymethylene) and enabled the determina68R

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tion of the spatial distribution of an antioxidant in an injection molded test bar. Glow discharge (GD) mass spectrometry, which is useful for bulk analysis, was demonstrated as a technique for depth-resolved analysis of polymeric paint coatings on an aluminum substrate for the automotive industry (C27). Each ∼15-µm layer of coating was distinguishable using signature ion peaks. A cryogenically cooled sample holder also has been constructed for GDMS (C28). This device allows the direct analysis of low-melting-point polymers such as polyethylene and results in the reduction of undesirable ions (e.g., from residual water or protonated fragment ions). The device can also be used for the analysis of thermally sensitive polymers. A direct current GDMS instrument was set up for the elemental analysis of polymers (C29). The advantages and disadvantages of this technique over the normal rf GDMS technique were discussed. An in-line molding press interfaced to a GC/MS was used to analyze the effluent from the vulcanization of rubber formulations for the purpose of identifying and quantifying organic compounds present in the vulcanization fumes (C30). Analyses were performed on natural, ethylene-propylene-diene monomer, styrenebutadiene, nitrile, chloroprene, silicone, and polyfluorocarbon rubbers. Degradation mechanisms were proposed based on the volatiles observed. Pyrolysis-field ionization-MS (Py-FI-MS) was performed on polybutadiene and polyisoprene (C31). Fragmentation mechanisms were suggested based on the long ion sequences observed from the spectra. Py-FI is performed in the source, enabling the detection of higher mass pyrolysates without condensation. MALDI-TOF MS using trans-retinoic acid as the matrix and copper(II) nitrate as the cationization reagent was used to analyze narrowly polydisperse polybutadiene (up to 300 000 u) and polyisoprene (up to 150 000 u) (C32). NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY Several reviews were written on the characterization of polymers and rubbers by NMR spectroscopy. General reviews were written on polymer characterization (D1, D2) NMR characterization of polymers (D3, D4), solid-state NMR of polymers (D5, D6), multidimensional NMR methods for determining structure and dynamics in solid polymers (D7, D8), conformational analysis (D9-D11), crystalline-phase structure (D12), polymer interfaces (D13), liquid crystals (D14, D15), gels and network polymers (D16-D19), characterization of micellar systems (D20), latex morphology (D21), and NMR imaging (D22, D23). The crystalline morphology of polymers was probed using solid-state NMR. Two different types of all-trans chains were observed in orthorhombic crystalline domains of polyethylene (D24). The phase structure of ethylene-(dimethylamino)ethyl methacrylate (DAM) copolymers was investigated, showing that the DAM unit and the R- and β-methylenes relative to the DAM tertiary carbon were excluded from the crystal (D25). The crystalline morphology of polyethylene was quantitatively determined using time domain proton NMR spectroscopy (D26, D27). The four crystalline forms of poly(4-methyl-1-pentene) were characterized using solid-state 13C NMR spectroscopy (D28). Solidstate 2H NMR was used to investigate the alignment of the chain segments near crystallites of a styrene-dimethylsiloxane block

copolymer through the incorporation of deuterium-labeled octane as a probe (D29). Solid state 13C NMR spectroscopy was used to characterize the dynamics and conformations of polyether liquid crystals (D30). The level of crystallinity of poly(tetrafluoroethylene) was determined by several methods including WAXS, density, DSC, Raman, IR, and 19F NMR (D31). Data from all these techniques correlated well except for the NMR data, and possible reasons this behavior were discussed. Double-quantum NMR was used to study conformational structure in amorphous polymers (D32-D34). This analysis utilized a multiple-pulse technique which gave rise to complete decoupling of directly bonded 13C-labeled sites allowing the determination of their torsion angles. Local orientational order between chain segments of a glassy polycarbonate was probed using a 13C NMR polarization transfer technique (D35) as well as for PET (D36). The preferred orientations were determined from the rate constants for polarization transfer using a 2-D NMR experiment. A rapid solid-state 1H NMR method for quantifying composition, crystallinity, and long spacing in ethylene-vinyl alcohol copolymers was presented (D37). Low-resolution solidstate 1H NMR was used to study the density of chemical crosslinks in ethylene, propylene, diene-modified (EPDM) rubber (D38). The structure of structured latex particle films was probed using solid-state NMR spin diffusion experiments and electron microscopy (D39). The adsorption isotherm for a nonionic surfactant (Triton X-405) on polystyrene latex particles was determined using differences in the 1H NMR chemical shifts for free and bound surfactant (D40). A thermotropic phase transition in a mixed cationic and zwitterionic surfactant micelle exposed to poly(acrylic acid) was detected using 2H NMR spectroscopy of deuterated surfactants (D41). NMR diffusion measurements were used to probe interactions between ethoxylated urethane associating polymers with polystyrene latex particles and surfactants (D42). Several authors utilized solid-state NMR to probe the dynamic heterogeneities that exist in glassy polymers. 2H NMR was used to probe this heterogeneity in polystyrene-d3 near the glass transition temperature (D43). Nonexponential relaxation was observed below Tg, but as the temperature was increased above Tg the relaxation became exponential, indicating that structural relaxation was fast enough to average efficiently over all environments. A new 2-D solid-state NMR pulse sequence combining proton spin diffusion and exchange of polarization between the protons and carbons was used to probe dynamic heterogeneities in poly(vinyl acetate) (D44). Multi-time-correlation functions were used to evaluate nonexponential relaxation in polymer glasses to determine whether the source of the nonexponential behavior was heterogeneous or homogeneous in nature (D45). The effects of antiplasticization on the β-relaxation of an epoxy network based on DGEBPA and hexamethylenediamine was probed by solid-state NMR and dynamic mechanical analysis (DMA) (D46). Antiplasticization caused a dramatic reduction in the β-relaxation, and the solid-state NMR measurements showed a marked reduction in the mobility of the methylenes near the nitrogen cross-link sites. In a similar study, the location of the antiplasticizer in the same epoxy network was probed using 2H, 15N, and 13C rotational-echo double-resonance (REDOR) NMR

(D47). The antiplasticizer was found to be located roughly 5 Å from the amine nitrogen. The local polymer dynamics of plasticized polyether-urethane networks was investigated using solidstate 13C NMR spectroscopy (D48). Solid-state NMR techniques were used to correlate molecular dynamics with mechanical behavior of polymers. In one case, the molecular dynamics associated with sub-Tg relaxations in arylaliphatic polyamides were studied using DMA, dielectric relaxation, and NMR (D49). The molecular origin of the R-relaxation in poly(ethyl methacrylate) and poly(methyl methacrylate) was characterized using 2-D exchange 2H NMR spectroscopy (D50). Solid-state 13C NMR and DMA were used to investigate the molecular motions associated with the β-relaxation for some DGEBA epoxy networks (D51). The molecular dynamics in glassy poly(ethylene-2,6-naphthalene dicarboxylate) were investigated using 2H NMR (D52) as were those of poly(isobutylene) and its block copolymers with poly (p-methylstyrene) using 1- and 2-D solid state 1H, 2H, and 13C NMR spectroscopy (D53), of polyesters using solid-state 13C NMR techniques (D54, D55), of poly(ethylene terephthalate) using solid-state 2H NMR spectroscopy (D56), and of the phenyl ring libration of a styrene-acrylonitrile copolymer doped with oxygen as a contrast agent for a 1H NMR relaxometric study (D57). Solid-state 13C NMR spectroscopy was used to investigate the effect of strain on polymers. In one case, block copolymers of poly(butylene terephthalate) and poly(tetramethylene oxide) were stretched in situ in a MAS rotor and the spectrum was taken (D58). New resonances were observed which were assigned to strain-induced crystallinity. In another case, several different solidstate NMR parameters were determined for partially deuterated polybutadiene networks under deformation (D59). Deuterium line shapes and splittings were used to calculate the molar mass of the network chains. A linear relationship between the elastic modulus of a poly(dimethylsiloxane) network and its 1H NMR transverse relaxation rate was established (D60). Deuterium NMR spectroscopy was used to probe the orientation of a non-flowaligning liquid crystalline polymer in a nematic solvent under shear in the magnetic field (D61). Variable-temperature 2H NMR T1 experiments were performed on backbone deuterated polystyrene in dilute solutions as a function of temperature and field strength (D62). Temperature, frequency superposition was not consistent with their data, indicating that the shape of the correlation function for C-D vector reorientation was temperature dependent. Dynamic filters for 2-D solid-state NMR techniques that allow selection of specific portions of a multi-time-correlation function were described (D63). The experiment was applied to poly(vinyl acetate), which possesses nonexponential, heterogeneous relaxation behavior. The molecular weight dependence of nuclear spin correlations for poly(dimethylsiloxane) and poly(ethylene oxide) melts was modeled in the form of a β-echo (sine correlation) function, which was especially sensitive to slow reorientational motions (D64). A theoretical analysis of the information content of multi-time-correlation functions for polymeric glasses was presented (D65). The morphology of polymer blends was investigated by a number of different solid-state NMR approaches. 1H NMR spin diffusion was used to probe the domain sizes in compatibilized polystyrene, ethylene-propylene rubber blends (D66). Spin diffuAnalytical Chemistry, Vol. 71, No. 12, June 15, 1999

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sion combined with cross polarization magic angle spinning (CP/ MAS) 13C NMR was used to probe the domain structure of poly(γmethyl-L-glutamate), poly(vinylpyrolidone) blends (D67). Techniques for characterizing the morphology of core-shell latexes of poly(butyl acrylate) (PBuA) and PMMA, including the structure of the interphase between the core and shell, were presented (D68). Models for the treatment of spin diffusion data were discussed (D69). Microphase separation in RIM polyureas was studied by advanced solid-state NMR techniques (D70). Incomplete phase separation gave a rather complex morphology whose development upon annealing was characterized. The microphase and interphase structure of PMMA-co-PBuA copolymers was determined (D71) as it was for styrene-co-isoprene block copolymers (D72) and polycarbonate (specifically 13C-labeled), polyfluorostyrene blends (D73). In the latter case, the nearest-neighbor separation and dynamics at the interface of the blends were characterized using 13C-19F REDOR NMR. The blend morphology of poly(styrene-co-acrylonitrile) with poly(styrene-co-maleic anhydride), both of which were specifically 13C-labeled, was characterized using 2-D proton-driven spin diffusion experiments (D74). A method employing rapid MAS at temperatures above Tg was presented for obtaining nearly high-resolution 1H NMR spectra such that solution 2-D spin-exchange experiments could be used to probe polymer morphology (D75). Natural-abundance solid-state 13C NMR using 2-D isotropicanisotropic correlation spectroscopy was used to determine orientational order in Kevlar fibers (D76). Two-dimensional MAS 13C NMR and FT-IR spectroscopy (D77) and solid-state CP/MAS 13C NMR together with X-ray diffraction (D78) were used to determine orientation in uniaxially drawn poly(ethylene terephthalate). Slow MAS DECODER NMR was used to define orientation in poly(4-oxybenzoate-co-1, 4-phenylene isophthalate) (D79) and orientation in poly(dimethylsiloxane) networks was characterized by 2H NMR (D80). Shear-induced orientation in a polystyrene, benzene-d6 solution was probed using 2H NMR (D81). The orientational order of locally parallel chain segments in glassy, carbonate 13C-labeled polycarbonate was probed using a solidstate 13C NMR pulse sequence called dipolar restoration at the magic angle (D82). This experiment determines interchain distances between 13C-labeled pairs or between 13C-labeled atoms and natural-abundance 13C atoms. 129Xenon NMR was used to probe the morphology of blends. In one example, 129X NMR was used to probe the morphology of blends of poly(ethylene oxide) and PMMA of varying concentration (D83). The exchange of xenon between the domains of each component fit well to a simple two-site exchange model and 2-D exchange NMR also demonstrated this phenomenon. The morphology and domain size of a polystyrene, poly(vinyl methyl ether) blend was probed in a similar way (D84). The miscibility of an ionomeric polymer blend was probed by 129Xe NMR (D85). 129Xenon NMR was used to probe polymer sorption sites and transport in semicrystalline polymers (D86). The self-diffusion coefficients of xenon in polypropylene and EPDM rubber and blends thereof were determined using pulse field gradient NMR spectroscopy (D87). Polymer networks of styrene, butadiene rubber (D88) and polybutadiene (D89) were characterized using field cycling NMR relaxometry. The NMR line shapes of strained Gaussian elasto70R

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meric networks were modeled (D90). Solid-state NMR heteronuclear NOE spectroscopy was used to study complexation in swollen networks of poly(methacrylic acid) and deuterated poly(ethylene glycol) due to hydrogen bonding (D91). End-linked poly(propylene oxide) gels of known molecular weight starting materials were used to establish quantitative relationships between 1H NMR relaxation parameters and molecular weight of the precursors (D92). Double-quantum NMR experiments of polybutadiene melts were presented which probed the translational chain dynamics allowing an assessment of the long-term topological constraints (D93). A series of 3-D NMR experiments for the characterization of heteroatom-containing polymer structure were presented for the analysis of chain-end structure for 13C-labeled polystyrene, diphenylphosphinyl radical initiated (D94), for characterization of tacticity for poly(1-phenyl-1-silabutane) (D95) and for poly(1chloro-1-fluoroethylene) (D96). A simple method was described to obtain 13C CP/MAS NMR spectra of samples exposed to up to 7-MPa pressure (D97) as was its application to the study of polystyrene exposed to CO2 (D98). A new NMR device for the characterization of polymer surfaces, the NMR mobile universal surface explorer (MOUSE), was described (D99) as well as its application to the study of the weathering of PVC coatings (D100). Polymerization kinetics and reaction mechanisms were characterized by a variety of NMR techniques. Many applications of NMR to the study of reaction kinetics and mechanisms to specific polymers were reported but are not mentioned here unless special emphasis was paid to the development of NMR techniques. The polymerization kinetics of acrylic acid were determined using in situ 1H NMR, as a function of temperature, percent neutralization, and concentration (D101). The emulsion polymerization of PBuA was determined by on-line solid-state NMR (D102). Chain transfer to polymer in the free-radical polymerization of BuA (D103) and vinyl acetate (D104) was determined. The propagation center in the anionic polymerization of methacrylic monomers by lithium 2-(2-methoxyethoxy) ethoxide was characterized using 1H, 13C, 7Li, and 6Li NMR spectroscopy (D105), as it was for a LiCl initiator (D106) and for the reaction of poly(styryl)lithium with propylene oxide (D107). The curing of (15N-labeled) amine cross-linked epoxy resins was characterized using REDOR 13C NMR and dipolar rotational echo 15N NMR spectroscopies (D108). 15NLabeled analogues were also used to study the curing of bismaleimide polymers by 15N NMR spectroscopy (D109). The gel kinetics for the curing of unsaturated polyester resins with styrene were investigated, comparing low-resolution pulse NMR methods to more conventional methods of measuring gel time (D110). Methods were presented to model the sequence distribution of copolymers at high conversion (D111), for copolymers possessing nonsymmetrical composition distributions (D112), for copolymers with chirality (D113), and for polymers that contain multiple components using factor analysis (D114). High-resolution 1H NMR was used to investigate correlations between the level of hydrogen bonding and phase separation in polyether polyurethane zwitterion systems (D115). The molecular weight and cross-link level of polyethylene networks and star polymers was characterized using 1H NMR FID analysis in the melt (D116). Except for the lowest molecular weight sample, all

FIDs were very similar, this attributed to the dominant effect of chain ends on the FID. Proton NMR relaxation measurements were used to define the existence of polymer solvent complexes in various polymer gel systems (D117). An NMR method for the determination of phase diagrams was described for acrylonitrile, sodium methallylsulfonate copolymer solutions in DMSO as a function of concentration, temperature, and thermal history (D118). Light-scattering and NMR spinlattice relaxation measurements were used to characterize the spinodal decomposition of a polystyrene, poly(vinylmethyl ether) blend (D119). The two techniques were found to be in satisfying agreement for the determination of the apparent diffusion coefficients. High-pressure, high-resolution 1H NMR was utilized to study the solution behavior of poly(1,1-dihydroperfluorooctyl acrylate) and its copolymer with styrene (D120). Discontinuities in the 1H NMR chemical shifts were postulated to originate from transitions between poor and good solvent quality. A new nonacidic solvent system consisting of a binary mixture of a fluorinated alcohol and a chloroalkane solvent was found to greatly improve the NMR analysis of nylons (D121). High-speed magic angle spinning (25-kHz) solid-state 19F NMR was used to obtain highresolution spectra of Kel-F such that the triad sequence distribution could be determined (D122). An application of the cyclic J cross polarization (CYCLCROP) NMR imaging pulse sequence for acquisition of 1H-detected 13C NMR images of elastomeric materials was presented (D123). A T1F filter for the NMR imaging of slow molecular dynamics in solid polymers was described (D124) as was an extension of the solidstate NMR imaging based on magic angle in the rotating frame (MARF) line-narrowing methodology (D125). Deuterium NMR imaging of stress in a strained natural rubber was performed by incorporating deuterated poly(butadiene) oligomers into the network (D126). The spatial variation in self-diffusion coefficients was determined using NMR microscopy (D127) as it was to determine the flow of fluids in a cone-and-plate viscometer (D128). Pore widths of macroporous glass filter systems filled with silicone oil were imaged using a 3-D spin-echo sequence (D129) as were the cells of open-cell polyurethane foams (D130). Hydrogel formation from hydroxypropylmethylcellulose was investigated by NMR and NMR imaging techniques (D131) as was enzymatic degradation of poly(3-hydroxybutyrate) and poly(3-hydroxybutyrate-co-3-hydroxyvalerate) in which degradation was found to be more rapid in the amorphous phase (D132). Aging in polymer networks of natural rubber was investigated by T1F material property NMR imaging (D133) as it was for carbon black-filled natural rubber using spin-echo and parameter-selective NMR imaging (D134). NMR diffusion measurements were used to probe the mobility of trimethoxymethane and water in Nafion membranes (D135). The mobility of a tackifying resin in a pressure-sensitive adhesive was investigated using pulsed field gradient spin-echo NMR (D136). Multivariate curve resolution techniques were used to analyze diffusion ordered spectroscopy (DOSY) experiments of polymer mixtures as well as GPC NMR curves (D137). GPC NMR was used to determine the absolute molecular weight distribution of PMMA from an end group determination as a function of elution time (D138) as it was for poly(ether sulfone) (D139). The molecular weight and tacticity of oligosty-

renes was determined using LC NMR (D140) as was the characterizion of fatty alcohol ethoxylate-based surfactants (D141). THERMAL ANALYSIS The thermal degradation of blends of common commercial polymers for recycling purposes was studied (E1). While the primary products were those observed for the individual polymers, some products were formed that suggested interactions during the degradation process. The degradation products from the decomposition of a phenolic urethane resin were determined over a temperature range of up to 900 °C with different products formed at different temperatures (E2). In an attempt to find ways of stabilizing polyacrylamides, the affect of adding sulfonated polymers to polyacrylamide was studied (E3). The thermal and oxidative degradation of epoxidized natural rubber was studied (E4). During the early stages of oxidation of polyolefins, little or no change in physical properties occurred until embrittlement was reached. The application of differential scanning calorimetry (DSC) and thermogravimetry (TGA) to the early stages of degradation was studied (E5). For isotactic polypropylene, a shift in the degradation mechanism in air at 80 °C was studied (E6). The kinetics for the degradation of epoxy resin in nitrogen/oxygen atmospheres with different oxygen levels was studied using TGA (E7). The onset of degradation was observed to be dependent on the oxygen level of the mixture and two degradation processes were observed, as compared to only one process in the absence of oxygen. TGA and IR were used to study the thermal oxidation of isotactic polypropylene in air (E8). The results suggested that degradation was dependent on hydroperoxide decomposition kinetics. In a study using both DSC and TGA, it was found that the presence of ethylene-acrylic acid copolymer accelerated the degradation of low-density polyethylene, whereas plasticized starch stabilized low-density polyethylene toward degradation (E9). A recent review discussed patterns of polymer degradation including interactions observed in the degradation of polymer blends (E10). In another work, a kinetic model for the thermal degradation of polymers was developed and applied to poly(methyl methacrylate) (E11). Dielectric spectroscopy was used to study the degradation of poly(ethylene glycol terephthalate) (E12). Two relaxation processes were observed, and the changes during degradation and the molecular origins for these changes were discussed. The effect of surface treatments applied to polyethylene films on the oxidation of the film was studied (E13) as were the effects of radiation on the degradation of poly(ethylene tetrafluoroethylene) (E14). Thermally stimulated current was used to study relaxations in poly(ethylene terephthalate) at temperatures above 20 °C, and three relaxation processes are observed (E15). Dielectric spectroscopy was used to study segment mobility in side-chain crystalline comb polymers (E16). It was found that at temperatures below the melting point of the side-chain crystals the mobility of the main chain was entirely suppressed. Thermally stimulated current was used to study the low-temperature relaxations of an epoxy modified with amine-terminated butadiene-acrylonitrile copolymers (E17). Four relaxations were observed. Analytical Chemistry, Vol. 71, No. 12, June 15, 1999

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A comparison of relaxations observed in Ultem 1000 as analyzed by DSC, dynamic mechanical spectroscopy, dielectric relaxation spectroscopy, and thermally stimulated depolarization current was reported (E18, E19). There was good agreement among the techniques reported, with thermally stimulated depolarization current showing two additional relaxations which may be due to spatial charges in the system. Thermally stimulated depolarization current was also used to study relaxations in poly(ethylene terephthalate) (E20). Relaxations involving a dipolar process and space-charge relaxation were reported. The dielectric constant, loss factor, and dielectric strength of polyester films aged between -40 and +120 °C were studied (E21). Only the dielectric strength was found to have been affected with increasing aging temperature causing a decrease in the dielectric strength. Dielectric spectroscopy was used to characterize a series of styrene-butyl methacrylate copolymers (E22). The relaxations observed were primarily attributed to the carbonyl group in the methacrylate and followed the expected temperature dependence as the butyl methacrylate level changed. An instrument was developed that allows for simultaneous dielectric spectroscopy and calorimetry (E23). Application to the reaction of a diepoxide with a monoamine was reported. Dielectric spectroscopy was applied to study the aging of adhesive-bonded structures, and it was suggested that this technique was appropriate for studying the aging process (E24). Dielectric measurements were used to study the reduction in the dielectric constant of polymers with controlled porosity (E25). For films of poly(methyl methacrylate) cast from different solutions, the effect of the solvent the film was cast from was studied and an explanation proposed based on solvent-polymer interactions (E26). The curing of biphenyl epoxy resins with different functional hardeners was studied, and different reaction orders were observed for different hardeners (E27). Dielectric spectroscopy was applied to study the postcuring of diglycidyl ether of bisphenol A and cyclohexylamine (E28). The development and growth of an intermediate relaxation process during curing was discussed. The thermal and thermooxidative degradation of a series of model epoxy resins was studied and related to the epoxy structure and cross-link density (E29). Simultaneous dielectric relaxation measurements and X-ray scattering were used to study the crystallization of poly(ethylene terephthalate) (E30). It was suggested that fluctuations in the electron density in the early stages of crystallization were due to isothermal compressibility. The effect of molecular weight on the crystallization of poly(phenylene sulfide) was reported (E31). DSC was used to study the change in glass transition temperature (Tg) of poly(ethylene terephthalate) at different levels of crystallinity (E32). It was suggested that this could be used to study the crystallization process of PET samples molded under different conditions such as blow molding. The miscibility of poly(vinylpyrrolidone) and poly(styrene-covinylphenol) blends were studied (E33). The miscibility of tetramethyl polycarbonate with syndiotactic polystyrene was studied (E34). A single glass transition for blends indicated that they were miscible and crystallinity was retarded for the syndiotactic polystyrene phase. 72R

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The thermal properties of an ethylene, propylene copolymer grafted with acrylic acid were investigated by DSC (E35). While the peak melting temperature was not changed, the grafting caused changes in overall crystallinity and crystallization kinetics. The melting of isotactic polypropylene that had been isothermally crystallized at different temperatures was reported (E36). At crystallization temperatures above 132 °C, two melting points were observed while only a single broad melting was observed at lower crystallization temperatures. This was related to different crystals being formed. DSC and temperature rising elution fractionation (TREF) were used to study the crystallization and melting of blends of low- and high-density polyethylene (E37). Both techniques showed that with rapid cooling a third melting phase was created and was attributed to a fraction of the two polymers that had cocrystallized. DSC was used to study the crystallization of poly(ethylene terephthalate) for blow-molding applications (E38). The effects of crystal nucleation and growth on the nonisothermal crystallization behavior are discussed. A two-stage crystallization model for the crystallization of poly(butylene terephthalate) blended with other polymers was developed (E39). The crystallization of syndiotactic poly(propene-cooctene) was studied (E40). Octene levels of up to 67% were used, and a wide range of crystallinities and variations in crystallization kinetics were reported. The effect of plane-strain compression on the thermodynamic properties of semicrystalline polymers was studied (E41). When high-density polyethylene and poly(vinylidene fluoride) were studied, a decrease in the crystallinity of the polymer was observed as well as changes in the thermal expansion. The crystallization and crystallinity of polylactides, having optical purities ranging from 43 to 100%, was studied (E42). While all samples studied could crystallize, it was reported that decreasing optical purity lowered the level of crystallinity and decreased the crystallization kinetics. The thermal properties of poly(phenylene sulfide amide) were studied (E43). The melting point was reported as 291-305 °C and Tg as 103.4-104.5 °C. A recent volume on instrumental techniques for analytical chemistry included a section on thermal analysis of polymers and examples of applications for those new to the area (E44). Relaxation processes in nonlinear optical polymers were studied by a variety of techniques (E45). Data were presented for both main-chain and side-chain NLO systems and optimum annealing conditions were discussed. The melting of syndiotactic polystyrene and blends with poly(phenylene oxide) were studied (E46). DSC and X-ray data of the blends showed two lower melting forms that originated during the crystallization process and a third melting form due to recrystallization from the first two melts. DSC combined with nonlinear mathematical models were shown to be well suited to characterize the polymerization of epoxy systems (E47). Modulated differential scanning calorimetry was used to study the reorganization of poly(ethylene terephthalate) in the melting region (E48). The observation of a reversible melting fraction suggested that melting within a few kelvins of the melting point was not complete. DSC and rheology were used to determine the order-order and order-disorder transition temperatures for a styrene-isoprene-styrene triblock copolymer (E49). The noniso-

thermal crystallization kinetics of poly(β-hydroxybutyrate) were studied using DSC, and activation energies were reported (E50). The thermodynamic properties and crystallization kinetics of poly(pentadecanolactone) were reported (E51). Thermodynamic interactions between 1,4- and 1,2-polybutadiene binary blends were studied (E52). Flory-Huggins interaction parameters and PVT properties were inconsistent with a simple random copolymer model. The effects of cross-link density on the volumetric properties of polycyanurate networks were studied by DSC and positron annihilation (E53). Bulky triazine cross-links were believed to be responsible for an increase in free volume holes as cross-linking increased. The use of TGA as an accelerated test method for investigating long-term stability was reported (E54). In particular, the weight loss between 150 and 300 °C was reported to be indicative of the extent of depolymerization. The relationship between physical aging and chemical structure for amorphous linear polyesters was reported (E55). Ellipsometry was used to determine the Tg and linear thermal expansion for poly(methyl methacrylate) films of 10-25 µm coated onto silicon wafers (E56). For very thin samples, optical properties of the substrate are reported to interfere with the measurement. The thermodynamic properties, including the heat capacity and heat of fusion, of an ethylene/carbon monoxide copolymer were reported (E57). The glass transition of highly grafted polystyrene was studied (E58). At low-molecular-weight grafting (∼5000) no effect on Tg was observed. However, for high-molecular-weight grafts (∼30000), Tg was found to broaden and the heat capacity change as Tg decreased. Thermal and mechanical properties for blends of poly(lactic acid) and poly(ethylene/butylene succinate) were studied, and the results indicated that these two polymers are not miscible (E59). The interaction between hydrophilic polymers and water was studied and described in terms of different levels of binding between the water and the polymer (E60). A comparison of relaxation times using mechanical and dielectric measurements on polybutadienes was reported, and good agreement between the two techniques was found (E61). The use of birefringence to measure phase transitions in liquid crystalline polymers was reported (E62). It was reported that transitions and stress relaxations were readily observed and results compared well with DSC and thermomechanical measurements. The study of polymer aging by the thermal step method was proposed (E63). This work used the measurement of space charges in the polymer to determine how the polymer has aged. INFRARED AND RAMAN SPECTROSCOPY The application of infrared and Raman spectroscopies to the characterization of polymeric systems continues to be a prolific area of the literature. General reviews of vibrational spectroscopy for the characterization of polymers are presented first, followed by review of applications to specific polymers. Of special note during the time period covered by this article are the continued evolution of Raman spectroscopy and two-dimensional dynamic infrared spectroscopy. A general review of the application of infrared and Raman spectroscopies to the analysis of polymer orientation was prepared (F1). Two reviews of the application of FT-Raman spectroscopy

to the analysis of polymers were presented (F2, F3). The use of high-pressure step-scan infrared spectroscopy to study several polymer systems was investigated (F4). The application of attenuated total reflectance (ATR) spectroscopy was presented (F5-F7). Specific applications of the ATR technique to paper coatings (F8), adhesives (F9), and to combinatorial chemistry (F10) were detailed. Specular reflectance to study polymer systems was investigated (F11, F12). Raman and infrared techniques for studying polymer/polymer and polymer/substrate interfaces were reviewed (F13). New approaches to quantitative analysis of copolymer systems were discussed (F14). The design and construction of a cell used to monitor copolymerization reactions using Raman spectroscopy was described (F15). Remote monitoring of polymerization processes by mid- and near-IR spectroscopies was discussed (F16). The use of synchrotron radiation in infrared microspectroscopy to identify the layers in a polymer laminate was discussed (F17). Hadamard transform infrared spectroscopy and its application to chemical mapping of polymer systems was reviewed (F18). Raman spectroscopy of biodegradable polymers was investigated (F19). The elastic modulus of polyethylene was measured using Raman spectroscopy (F20). Micro Raman spectroscopy was used to study orientation drawing in polyethylene (F21, F22). The online measurement of crystallization in low-density polyethylene was performed using Raman spectroscopy (F23). Dynamic twodimensional infrared spectroscopy was used to study the crystal/ amorphous interphase region in low-density polyethylene (F24). Short-chain branching in polyethylene was measured using size exclusion chromatography coupled with infrared spectroscopy (F25). Oxidation of ultrahigh-molecular-weight polyethylene was investigated with infrared spectroscopy (F26). Specular reflectance in the mid- and far-IR regions was used to examine adhesion in oxidized polyethylene (F27). Characterization of the structure of propylene-ethylene copolymers by infrared (F28, F29) and Raman (F30) spectroscopies was discussed. Infrared linear dichroic spectra of isotactic polypropylene and high-density polyethylene were acquired and analyzed (F31). Dynamic infrared linear dichroism spectra of isotactic polypropylene were acquired and analyzed (F32). Differences in crystallinity from surface to bulk in compression-molded polypropylene were characterized by ATR spectroscopy (F33). Environmental photooxidation of polypropylene films was followed by infrared spectroscopy (F34). Interactions between a steel surface and a maleic anhydridegrafted ethylene (vinyl acetate) copolymer was investigated using diffuse reflectance infrared spectroscopy (F35). In-line monitoring of vinyl acetate content in ethylene(vinyl acetate) copolymer films was performed using near-IR spectroscopy (F36). Band shifts indicating interactions between comonomers in miscible vinyl polymer blends were characterized (F37). Characterization and quantitation of butadiene in styrenebutadiene copolymers was conducted using FT-Raman spectroscopy (F38). The near-IR spectrum of polybutadiene was recorded and interpreted (F39). Resonance Raman spectroscopy was used to characterize interpenetrating elastomer systems (F40). Interactions between natural rubber and chlorinated natural rubber were Analytical Chemistry, Vol. 71, No. 12, June 15, 1999

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studied using infrared spectroscopy and scanning electron microscopy (F41). Infrared dichroic investigations of orientation in poly(dimethylsiloxane) in the near- and mid-IR were presented (F42). The photo-cross-linking reaction of disiloxanes was studied using infrared spectroscopy (F43). Quantitation of poly(dimethylsiloxane) levels in turbid samples was performed using Raman spectroscopy (F44). Infrared dichroism in linear and branched polystyrene chains was investigated (F45). Phase separation of surfactant in polystyrene/poly(n-butyl acrylate) latexes was studied using ATR spectroscopy (F46-F48). A mid-IR optical fiber probe was used to investigate the polymerization of styrene-acrylate emulsions (F49). Vibrational dynamics of syndiotactic polystyrene were investigated (F50, F51). Internal reflection infrared spectroscopy was used to observe water diffusion in polymer films (F52). Acetylation of polystyrene microspheres was studied with infrared spectroscopy (F53, F54). Interactions of blends of polycaprolactone and poly(styrene-acrylonitrile) copolymers were investigated by infrared spectroscopy (F55). Mechanical relaxation phenomena in styrene-acrylonitrile copolymers was studied with twodimensional infrared spectroscopy (F56-F58). Infrared and Raman spectroscopies were used to follow the UV degradation of styrenic copolymers (F59). Size exclusion chromatography coupled with infrared spectroscopy was used to study solvation effects in styrenic copolymers (F60). Interface segregation in blends of acrylic and fluoropolymer blends was studied using phase-modulated photoacoustic spectroscopy (PAS) (F61). Adhesion of acrylic polymers to polyethylene was examined using rheophotoacoustic spectroscopy (F62). Quantitative analysis of ethylene-acrylate copolymers was performed using infrared spectroscopy (F63). ATR spectroscopy was used to characterize silicone-modified acrylic coatings (F64). The copolymerization of epoxy methacrylates was followed using FTRaman spectroscopy (F65). The nanostructure of poly(methyl methacrylate) glass was investigated with Raman spectroscopy (F66). The water content of coatings on plastic lenses was investigated using near-IR spectroscopy (F67). Temperaturedependent resonance Raman spectroscopy was used to study poly(vinyl alcohol) films (F68). The intermolecular interactions of blends of poly(vinyl alcohol) with poly(acrylic acid) were studied by infrared spectroscopy (F69). Orientation in ethylene(vinyl alcohol) copolymers was investigated using infrared dichroism and birefringence (F70). Quantitation of the concentration of poly(ethylene glycol) in chloroform solution was performed using Raman spectroscopy (F71). Raman longitudinal acoustic mode studies during the isothermal crystallization of poly(ethylene oxide) were characterized (F72). Crystallization of a poly(ether ether ketone)/poly(ether sulfone) blend was studied with Raman spectroscopy (F73). Interactions in poly(ether ether ketone)/poly(ether imide) blends were characterized with infrared spectroscopy (F74). Infrared spectroscopic investigations of cross-linked polyethers after implantation in rats was used to characterize the biodegradation of these materials (F75). Size exclusion chromatography coupled with infrared and NMR spectroscopies was used to characterize poly(ether sulfone) (F76). 74R

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Anhydride intermediates for cross-linking of cotton cellulose were investigated with infrared spectroscopy (F77). The application of two-dimensional near-IR correlation spectroscopy to study premelting behavior in nylon-11 (F78) and nylon12 was reviewed (F79, F80). Orientation and morphology of the surfaces of polyimide films was studied by infrared spectroscopy (F81, F82). Mid-IR optical fibers were used to study the reaction chemistry of polyurethane foams (F83). The correlations between infrared spectra and physical properties of polyurethane foams were investigated (F84). The photodegradation of aliphatic poly(ester urethanes) was characterized with infrared spectroscopy (F85). Interdiffusion at the interface between polyurethanes and epoxy resins was studied with infrared spectroscopy (F86). Rheooptical spectroscopy was used to examine cyclic elongation and recovery of polyurethane-polyolefin blends (F87, F88). Changes in the infrared spectra of hydrogen-bonded polyureas during heating were investigated (F89, F90). Photodegradation of the surface of polycarbonate was investigated with IR reflectance spectroscopy (F91). The correlation between thermal behavior, as studied by DSC, and infrared spectroscopic changes during annealing of PET was presented (F92). Comparisons of crystallization rates for surface and bulk regions of PET were made using reflection-absorption and transmission infrared spectroscopies (F93). Raman spectroscopy (F94), specular reflection infrared spectroscopy (F95), and transmission IR (F96-F99) were used to study orientation and conformation in PET films. Diffusion of water into PET was followed in situ using ATR spectroscopy (F100). Single fibers of PET were characterized by polarization infrared microspectroscopy (F101). Yellowing during thermal degradation of PET was investigated with infrared spectroscopy (F102). Melamine enrichment at the surface of melamine/polyester films was investigated with ATR spectroscopy (F103). This technique was also used to measure surface orientation in PET (F104). End group analysis and melting behavior (F105) of poly(ethylene-naphthalene) films was performed using infrared spectroscopy (F106). Decomposition of poly(vinyl chloride) was studied in situ with a specially designed infrared cell (F107). Decomposition of plastisols in poly(vinyl chloride) was monitored by infrared spectroscopy (F108). Uniaxial orientation changes in poly(vinylidene fluoride) were examined using infrared spectroscopy (F109). The effect of electron beam radiation on the structure and orientation of fluoropolymers was studied using infrared microspectroscopy (F110). Time-resolved IR was used to study the reorientation of liquid crystalline polymers in an electric field (F111, F112). Spatially resolved infrared microspectroscopy enabled the analysis of in situ diffusion of liquid crystalline polymer systems (F113, F114). Liquid crystalline poly(ester amide) was characterized (F115). Hydrogen bonding in liquid crystalline epoxy resins was examined in order to learn about curing mechanisms of this material (F116). The characterization of benzocyclobutene-based polymers by infrared spectroscopy was discussed (F117). The characterization of changes during the transition from the neutral to conducting forms of poly(phenylene-vinylene) was performed with resonance

Raman spectroscopy (F118, F119). Curing reactions of epoxy formulations were studied with near-IR (F120) and Raman (F121, F122) spectroscopies. A Raman sensor was used to measure stress and strain in aramid/epoxy composites (F123-F125). The interdiffusion of polymer coatings with epoxy resin laminates was studied using ATR spectroscopy (F126). Patrick B. Smith is a Technical Leader in the Materials Characterization Group of the Analytical Sciences Laboratory, Dow Chemical U.S.A., Midland, MI. He received his Ph.D. in physical chemistry from Michigan State University in 1978. His research interests are largely concerned with structural characterization of synthetic polymers by NMR spectroscopy, both in solution and in the solid state. Dr. Smith is the coauthor of 56 publications and 1 patent. He is an Adjunct Professor at Central Michigan University and a member of the American Chemical Society. He received the Midland Chapter Sigma Xi award in 1987 and the Midland Chapter ACS award for Outstanding Achievement and Promotion of the Chemical Sciences in 1998. Andrew J. Pasztor, Jr. is a Technical Leader in the Materials Characterization Group of the Analytical Sciences Laboratory, Dow Chemical U.S.A., Midland, MI. He received his Ph.D. in physical chemistry from The University of Miami (Florida) in 1976. He joined Dow and worked in the Halogens Research Laboratory and the Styrene Molding Polymers Laboratory before taking his current assignment. His research interests are centered on applications of thermal analytical techniques to polymer characterization, in particular curing of thermosets, the relationship of crystallinity and crystallization to chemical structure, and applications of dielectric spectroscopy to polymer characterization. He is the author or coauthor of 18 publications and 5 U.S. patents. He is a member of the North American Thermal Analysis Society. Marianne L. McKelvy is a Senior Specialist in the Molecular Spectroscopy Group of the Analytical Sciences Laboratory of the Dow Chemical Co., U.S.A., Midland, MI. She received her B.S. degree from the University of Detroit, Detroit, MI (1979) and the M.S. (1982) and Ph.D. (1985) degrees in polymer chemistry from Polytechnic University, Brooklyn, NY. She joined the Dow Chemical Co. in the Analytical Sciences Laboratory in 1984, where she is involved in solving polymer problems using infrared spectroscopy. Her research interests involve the characterization of polymers using vibrational spectroscopy and infrared microspectroscopy. She is a member of Sigma Xi, the Coblentz Society, the Society for Applied Spectroscopy, and the American Chemical Society. David M. Meunier is a Research Leader in the Materials Characterization Group of the Analytical Sciences Laboratory, Dow Chemical U.S.A., Midland, MI. He received his B.S. degree in chemistry from North Central College, Naperville, IL, in 1984 and his Ph.D. degree in analytical chemistry from the University of Illinois, UrbanasChampaign, in 1988. He joined Dow in 1988 in the Research Assignments Program. In 1990, he became a member of his current group. His research interests lie in characterizing molecular weight and molecular architecture in polymer systems by multidetector liquid chromatographic techniques. He is the author or coauthor of eight publications and is a member of the American Chemical Society. Stephen W. Froelicher is a Senior Specialist in the Reactive Chemical/Thermal Analysis/Physical Property discipline of the Analytical Sciences Laboratory, Dow Chemical, USA, Midland, MI. He received a B. S. degree in chemistry (1980) from Northern Kentucky University and a Ph.D. in analytical chemistry (1985) from Purdue University. He joined Dow that same year and his research interests include the development and application of evolved gas analysis techniques such as thermogravimetry/mass spectrometry for polymer characterization. The emphasis of his research is understanding the thermal and oxidative degradation of synthetic polymers under processing conditions. Frank C.-Y. Wang is a Project Leader in the Materials Characterization Group of the Analytical Sciences Laboratory, Dow Chemical Co., U.S.A., Midland, MI. He received his B.S. in chemistry from the Fu-Jen University in Taiwan (1977) and his Ph.D. in physical chemistry from Michigan State University (1983). He joined the Dow Chemical Co. in the Analytical Sciences Laboratory in 1989 and worked on various analytical projects. His research interests currently include pyrolysis techniques for polymer analysis and applications of gas chromatography to polymeric systems. Frank is a member of the American Chemical Society.

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