Anal. Chem. 1997, 69, 15R-28R
Coatings Dennis G. Anderson
Witco Corporation, 6200 West 51st Street, Chicago, Illinois 60638 Review Contents Chemical and Electrochemical Methods Gas Chromatography Gel Permeation Chromatography High-Performance Liquid Chromatography Infrared Spectroscopy Nuclear Magnetic Resonance Spectroscopy Surface Analysis Ultraviolet/Visible Spectroscopy Spectroscopy. Miscellaneous Techniques Microscopy and X-ray Techniques Thermal Analysis Environmental and Industrial Hygiene Miscellaneous Measurements Literature Cited
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This review covers analytical techniques applicable to the examination of coatings and coatings’ raw materials, substrates upon which coatings are placed, etc., since the last review in 1995 (A1). The contents are divided into 14 analytical techniques useful in coatings characterization. Readers are encouraged to survey the entire review, since the analysis of specific paints, coatings, or related materials may be found in each section. The five most highly referenced areas are infrared spectroscopy, nuclear magnetic resonance spectroscopy, high-performance liquid chromatography, thermal analysis, and gas chromatography. New or unique applications appear throughout the 705 references cited in this review. Two interesting articles dealt with the role of the analytical laboratory in the paint industry (A2) and the reliability of test laboratories in the coatings industry (A3). The use of supercritical carbon dioxide was reported as a mechanism to reduce solvents in wood coatings (A4) as was the use of an encapsulant to control the hazards associated with lead-based paints (A5) and a study of xenoestrogens released from can coatings (A6). Instrumental techniques useful in analyzing radiation-curable coatings received special attention (A7) as did the general examination of polymers (A8, A9) and detergents (A10) and the utilization of hyphenated techniques (A11). Surfactant analysis was treated in considerable depth through the publication of a series of papers, including an introduction (A12), basic analysis techniques (A13), classification and separation procedures (A14), analysis without prior component separation (A15), chromatographic applications (A16), the study of nonionic (A17) and cationic + amphoteric (A18) systems, and the usefulness of surfactants in various domains within analytical chemistry (A19). CHEMICAL AND ELECTROCHEMICAL METHODS A general review discussing the chemical analysis of poly(oxyalkylene) block copolymers was published during this period (B1) as were German standard methods for the measurement of hydroxyl number in fats, fat products, and surfactants (B2). Solid S0003-2700(97)00001-2 CCC: $14.00
© 1997 American Chemical Society
phase extraction methods were found to be useful for the separation of poly(ethylene glycols) and ethoxylates (B3). The accumulation of peroxides in detergents was reported (B4), as was improved testing for lead in the environment (B5, B6), the iodometric titration of metallic zinc in paints (B7), recent work on the use of two-phase titration for anionic surfactants (B8-B11), and the analysis of cocoamidopropyl betaines (B12) and sulfates based on alcohols and alcohol ethers (B13). Potentiometric titrations reported during this period include a re-examination of acid content in polyesters (B14) and a method for the determination of water content in paint through analysis of the vapors formed during distillation (B15). Potentiometric titration of surfactants was reviewed in general (B16), with specific examination of ionic (B17-B22) and nonionic (B23-B25) surfactants thoroughly treated in a number of excellent studies. GAS CHROMATOGRAPHY Gas chromatography remains a primary tool for the characterization of coatings and coatings-related materials. A new book relates the use of chromatographic techniques to the characterization of polymers (C1). Other useful review articles examined the use of supercritical fluids in polymer analysis (C2), the use of chromatography for the analysis of cationic surfactants (C3), the study of synthetic wax composition (C4), and the on-line control of polymerization reactors (C5). Odor-causing species in coatings received special attention (C6, C7) as did the examination of alkyl polyglucosides (C8), poly(glycerols) (C9), additives in polyolefins (C10), polychlorinated biphenyls in railcar coatings (C11), polyesters (C12, C13), and poly(oxyethylene) condensates (C14C17). Headspace techniques were used to measure partition coefficients and residual solvents in coatings (C18-C20), and inverse chromatography was employed in a number of interesting applications (C21-C25). Many species in coatings lack sufficient volatility for direct examination using gas chromatography. The application of pyrolytic techniques continues, with citations concerning the general examination of polymers (C26) as well as specific studies related to styrene-butadiene (C27), acrylic (C28-C31), epoxy (C32), urethane (C33), polyester (C34-C36), quaternary ammonium hydroxides (C37), and ancient paints and inks (C38, C39). Coupling the separating ability of the gas chromatograph with the qualitative analysis capability of a mass spectrometer provides an excellent mechanism for coatings characterization. Several studies of interest include the analysis of siloxane pyrolysis products (C40, C41), the photoablation of urethanes (C42), and the drying of alkyd resins (C43). A relatively new development for volatilization is matrix-assisted laser desorption/ionization timeof-flight mass spectrometry (MALDI-TOF). Reports of interest to the coatings analyst include a study of polymer molecular weight determination (C44) and the functionalization of poly(ethylene glycol) (C45). The mass spectrometric examination of Analytical Chemistry, Vol. 69, No. 12, June 15, 1997 15R
species in liquid chromatographic effluents was also discussed in articles dealing with acrylic polymer components (C46), surfactants (C47-C52), additives in polyurethanes (C53, C54) and polyester resins (C55). GEL PERMEATION CHROMATOGRAPHY Gel permeation (size exclusion) chromatography provides useful information relative to materials used throughout the coatings industry. A number of excellent review articles have appeared (D1-D5), as have papers concerning the characterization of block polymers using multiple detectors (D6) and a historical examination of the development of the technique (D7). The problems encountered with the use of multiple detectors have been studied in detail (D8-D11) as has the measurement of absolute molecular weights via on-line membrane osmometry (D12). Studies with other desirable detector systems include the evaluation of light scattering (D13-D15), mass spectrometry (D16, D17), Fourier transform infrared spectrometry (D18-D20), UV/visible spectrophotometry (D21), and surface area exclusion chromatography (D22). The characterization of lower molecular weight species continues as a major application of gel permeation chromatography. Of particular interest are studies concerning micelle formation in surfactants (D23) and nonionic surfactants (D24-D27), the effect of surfactants on associative thickeners (D28), the isolation of dark-colored impurities in sulfonated fatty acid methyl esters (D29), and the fate of thioxanthones as photinitiators in acrylate polymerization (D30). Polymeric materials remain as the main area of interest relative to the use of gel permeation chromatography. Among the specific polymer types reported were the following: poly(vinyl alcohol) (D31), poly(vinyl acetate) (D32), polyesters (D33-D36), polyurethanes (D37-D39), acrylic systems (D40-D43), and styrenecontaining copolymers (D44-D-46). HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY The application of high-performance liquid chromatography (HPLC) to the examination of polymeric materials was the subject of a recent general review (E1) and a review of the nonexclusion liquid chromatography of polymers (E2). The use of alternate detector systems received special attention, with a paper concerning coupled density detection (E3). HPLC was also used in the characterization of proteinaceous painting ligands (E4), examining the fate of benzotriazole ultraviolet light absorbers (E5), the online measurement of antioxidants and ultraviolet stabilizers (E6), additives in polyolefins (E7, E8) and the measurement of toluene diisocyanate and diphenylmethane diisocyanate during fire simulation tests (E9). HPLC as part of hyphenated analytical instrumentation continued, with specific references to the use of mass (E10) and nuclear magnetic resonance spectrometers (E11). Capillary zone electrophoresis (CZE) is applicable to many of the same types of samples as high-performance liquid chromatography. Specific papers of interest include the study of polycarboxylic acids (E12) and the examination of ionic and neutral surfactants (E13-E18). Supercritical fluid chromatography (SFC) also continued in popularity, with citations related to oligomer analysis and characterization (E19), the investigation of monomeric acrylates (E20), and the separation of fatty alcohol ethers (E21). Field-flow fractionation was also reported for the separation of core-shell 16R
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carboxylated latexes (E22), polystyrene particles (E23), and acrylic paint species (E24). Finally, hydrodynamic chromatography provided information concerning the flow of paints and coatings (E25) and the separation of high molecular weight polymers (E26). The analysis of surfactants continues as a popular application for high-performance liquid chromatography. A retention index system for surfactant analysis was developed (E27) and a review of ion exchange techniques completed (E28). Specific studies of interest include the examination of nonionic surfactant interactions (E29, E30) and oligomer separation in nonionic systems (E31E36), the evaluation of alkyl polyglucosides (E37, E38), and the assay of volatile acids induced by the autoxidation of nonionic surfactants (E39). Anionic surfactants were studied using highperformance liquid chromatography (E40-E46), as were cationic systems (E47, E48). HPLC at the critical point of absorption has been reported for the measurement of heterogeneity in polymers (E49). Citations were also found concerning a novel method to measure unreacted hydroxyl groups in polyesters (E50), the study of acrylate sequences (E51, E52), condensation nucleation light-scattering detection in the examination of poly(ethylene glycols) (E53, E54), the determination of isocyanates in spray painting operations (E55), and the characterization of methoxymelamines using liquid chromatography/mass spectrometry (E56). Several references were found concerning the use of thin-layer chromatography in coatings-related applications. Among the citations were the following: the analysis of detergents and cleaning aids (E57), the examination of fatty acid sarcosides (E58), alkyl polyglucosides (E59, E60), nonionic surfactant lipophilicity (E61), and gemini-type surface active agents (E62) and the use of enzymes to observe spots on TLC plates (E63). INFRARED SPECTROSCOPY Infrared (IR) spectroscopy remains the most popular analytical technique for the examination of coatings, with the greatest number of citations during this period. Several articles dealt with the analysis of 1974-1986 automobile original top coats (F1, F2), the examination of surfactants (F3-F5), and the evaluation of polymers using mid- (F6) and far- (F7) infrared spectroscopy. The use of multimedia to enhance the information obtained during analysis was reported (F8), as were the use of a diamond anvil in forensic analyses (F9), methods useful in the examination of ionomers (F10), applications of IR spectroscopy in the detergent industry (F11), and the use of an IR card to aid in sample preparation (F12). Group frequency assignments for polymer identification were revisited (F13), and two-dimensional IR spectroscopy (F14) and combined infrared spectroscopy/highperformance liquid chromatography reviewed (F15). A new approach to the quantitative analysis of a two-component polymer system was published (F16), as were typical far-infrared spectra of segmented polyurethanes (F17), the spectra obtained from a number of phenolic resins (F18), and the profiling of aged polymer films (F19). The development of an expert system for polymer characterization (F20), the use of aluminum trihydroxide as an ultraviolet transparent filler in radiation-curable coatings (F21), a study of foam stability and foam fractionation in acrylic polymers (F22), a renewed study of redox couples and adsorbed molecules on electrode surfaces (F23), and the use of a closed cell to
measure consumer exposure to paint stripper solvents (F24) also received special attention. Infrared spectroscopy was used extensively to measure the curing of polymers and coatings, with special reports on the following: extraction/IR spectroscopy applied to radiation-cured systems (F25), epoxy-based aerospace coatings (F26), measurements of chemical change rates to select superior automotive clear coats (F27), cure speed in optical fiber coatings (F28), the curing of powder coatings (F29), and the degradation of a number of coating types (F30-F32). The drying of water-based coatings received detailed attention (F33), as did the effect of surfactants on urethane foam cell structure (F34), the effect of ionic groups on the properties of a polyurethane urea emulsion (F35), and the durability of acrylic emulsion (F36), acrylic solution (F37), and vinyl chloride-vinyl acetate- (F38) based coatings. The characteristics of radiation-curable coatings were the subject of papers using real-time infrared spectroscopy (F39), a study of structureproperty relationships (F40), and curing kinetics (F41). Other polymer types examined included the following: polyesters (F42F46), alkyds (F47, F48), vinyl acetate copolymers (F49), silicones (F50-F52), rubber (F53), and nonionic surfactants containing oxyethylene chains (F54-F56). Photoaccoustic applications during this period included the characterization of polymer structure (F57), a review of polymer thermal and interfacial changes (F58), photaccoustic step-scan IR spectroscopy (F59, F60), the study of isocyanurate and isocyanate conversion (F61, F62), an evaluation of acrylonitrile/ butadiene polymers for automotive interiors (F63), and depth profiling of polyethylene surface sulfonation (F64). Reports documenting the application of IR spectroscopy for the study of surface phenomena continue (F65-F67), with specific citations concerning unique problems during the examination of polymers (F68, F69), fillers (F70), latex-coated paper (F71, F72), and water at the coating/substrate interface (F73). Other unique applications include the evaluation of diffusion through coatings (F74), depth profiling of acrylic/melamine formaldehyde coatings (F75), monitoring acrylate polymerization (F76-F78), the study of carboxylic acid-containing surfaces (F79), the distribution of silicone additives in coatings (F80), and investigations of urethane (F81-F84), latex (F85, F86), and surfactant (F87) systems. Interfacial studies via IR spectroscopy included the use of diffuse reflectance techniques (F88) and the examination of fiber/ matrix interactions (F89) and the liquid/solid interface (F90). Reports concerning latex films received special attention (F91), including the air/film interface (F92, F93), the water/film interface (F94, F95), and the general migration of various species throughout a latex film (F96-F101). Near-infrared (near-IR) spectroscopy continues to be used to monitor the concentration of a number of species of interest to the coatings analyst. Among the more interesting studies were the following: the identification of polymer type (F102, F103), choosing materials as near-IR standards (F104, F105), inhomogeneities in sets of near-IR spectra (F106), the standardization of surface contamination analysis systems (F107, F108), and a method to determine molecular orientation in uniaxially stretched polymers (F109). Among the sample types measured using nearIR techniques were the hydroxyl content of polyols (F110-F114), polyester graft copolymers (F115), ethylene-vinyl acetate copolymers (F116), and polyurethanes (F117).
Raman spectroscopic citations include numerous general review articles related to coatings (F118-F121) and polymers (F122-F125), an examination of surface Raman techniques (F126, F127), and deformation studies with polymers (F128). Specific polymers treated in detail included melamine-formaldehyde resins (F129), epoxy systems (F130, F131), and natural waxes and resins (F132). NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY Excellent articles have appeared concerning the use of nuclear magnetic resonance (NMR) spectroscopy to examine solvents in waterborne paints (G1), to study polymer relaxation (G2), and to evaluate microstructure in rigid polymers (G3-G5). Two articles appeared during this period relative to the on-line analysis of polymeric systems using NMR techniques (G6, G7). Other general articles of interest included an examination of lipid and surfactant applications (G8), the measurement of trace levels of chemical warfare agents in paints (G9), an examination of the reaction of melamine with oxiranes (G10), the measurement of hydroxyl groups using 31P NMR (G11), and applications of 117Sn (G12), 23Na (G13, G14), and xenon (G15) as probes into the structure of polymeric systems. Citations continue relative to the study of fumarate and maleate inhibitors (G16) and the examination of flame retardants (G17), corrosion inhibitors (G18), and aromatic diester-diacid isomers (G19). Fatty acid-based chemicals have received special attention, with references to the study of fat- and oil-based amphoteric surfactants (G20) and the examination of partial glycerides (G21). Poly(ethylene oxide)-related studies have taken many forms, including measurement in poly(ethylene) (G22), analysis of block copolymers (G23), and synthesis of oligomers containing amino (G24), cyano (G25), and olefinic (G26) functionalities. Other surfactant systems that have received special attention include the following: alcohol ethoxylates (G27), cationics (G28), poly(ethoxyalkyl) maleates (G29), sulfobetaines (G30, G31), sulfonates (G32), and carbonates (G33). Phenomenological studies concerning motions of a polymer chain in surfactant solutions (G34), absorption of surfactants to polymers (G35), and the structure and dynamics of polyelectrolyte-surfactant complexes (G36) have also been reported. Two new books dealing with the use of NMR spectroscopy in polymer analysis have been published (G37, G38) as have review articles dealing with polymer systems (G39), solid polymers (G40, G41), and the application of 2-D experiments to polymer characterization (G42). Microemulsions (G43), standard emulsions (G44), polymer reactivity (G45), imaging (G46-G48), and the structure of polymer blends received special attention (G49-G52). Among the specific polymer types examined were acrylics (G53G59), vinyl acetates (G60, G61), poly(acrylonitrile) (G62), urethanes (G63-G66), polyesters (G67-G69), polycarbonates (G70), silicones (G71, G72), and phenol (G73, G74) and melamine (G75-G77) formaldehyde condensates. SURFACE ANALYSIS A number of review articles have appeared dealing with the use of surface analytical techniques (H1, H2), as have specific studies concerning the examination of industrial surfaces (H3), fouling-resistant marine coatings (H4-H6), assuring sheet metal surface quality in coating lines (H7), profilometry, and fractal Analytical Chemistry, Vol. 69, No. 12, June 15, 1997
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analysis for coating surface roughness (H8), and the use of scanning tunneling microscopy (H9). X-ray photoelectron spectroscopy (XPS) or electron spectroscopy for chemical analysis (ESCA) continues as a major technique for the examination of coatings surfaces. Several excellent review articles have appeared (H10-H14) as has an extensive study of quantitation methods (H15). Among the specific coating types examined were melamine-cured acrylics (H16), radiation-cured polymers (H17), model latex particles (H18), thermoplastics used in automobiles (H19), and silicones (H20). A general review of Auger electron spectroscopy was published (H21), as was a special report on the use of this technique to measure adhesive wear (H22) and the use of electrochemical impedance spectroscopy to measure corrosion of a polymer-coated metal (H23). Electron spin resonance (ESR) studies included the examination of polymer degradation mechanisms (H24), the emulsion polymerization of acrylates (H25), the fading mechanisms of paint films (H26), the radical polymerization of dialkyl fumarates (H27), and the hydration dynamics of oxyalkylene block copolymers (H28). Time-offlight secondary ion mass spectrometry (TOF-SIMS) studies were reported for the surface analysis of high-solids coatings (H29, H30), polymers and polymer blends (H31-H34), and polyester transesterification (H35) and the desorption of emulsifiers from polystyrene latexes (H36). ULTRAVIOLET/VISIBLE SPECTROSCOPY Stability studies of paint pigments were performed using ultraviolet/visible spectroscopy (I1), as were cure monitoring of polyimide (I2) and styrene/methyl methacrylate polymerization (I3). The hiding power of powder coatings was again measured using scattering measurements (I4), as was the examination of test methods to evaluate UV durability of polymeric coatings (I5, I6). Colorimetric procedures of note included the determination of trace carbonyl compounds in oxyalkylated products (I7), the analysis of isocyanates in spray-painting operations via a 1-(2methoxyphenyl)piperazine derivative (I8), the detection of cellulolytic enzymes in latex paints (I9), the quantitative analysis of organic pigments in forensic applications (I10), and the detection of alkyl polyglucosodes through reaction with anthrone (I11). Simple methods were developed for the determination of sodium dodecyl sulfate through the formation of an ion pair (I12), the measurement of critical micelle concentration in poly(glycol ethers) (I13), and the preparation of novel metal polymers through the reaction of cobalt and zinc chloride with an acrylamide/acrylic acid copolymer (I14). The control of radiance in ultraviolet exposure meters was reviewed (I15), as was UV absorption as a critical component in fire retardant systems (I16) and the application of UV spectroscopy to measure free-volume distributions during polymerization (I17I19). Studies involving lower molecular weight species included the following: the interaction of surfactants and organic dyes (I20), the hydration of water-soluble polymerization initiators (I21), the examination of polyether solvation mechanisms (I22), and the measurement of UV absorbers in acrylics (I23) and polyolefins (I24). Specific polymer types examined were novolacs (I25) and electron beam-cured acrylates (I26). Spectrophotometric studies of pigment trichromacity continued (I27), as did the measurement of opacity due to titanium dioxide (I28) and the determination of flash rust staining (I29). The utilization of fluorescence spectroscopy included citations of potential on-line 18R
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monitoring of vinyl polymerization (I30), monitoring UV curing operations (I31), characterization of triazine compounds (I32), and fluorescence microscopy for penetration analysis of coatings applied to rusty steel (I33). Atomic spectroscopy applications included the use of atomic absorption spectroscopy for lead contamination in paints (I34), the measurement of trace elements in titanium dioxide (I35), and the determination of zeolite, silicate, and phosphate in laundry detergents using inductively coupled argon plasma spectroscopy (I36). SPECTROSCOPY. MISCELLANEOUS TECHNIQUES Static and dynamic light scattering remain as useful tools, with an excellent review (J1), a study using hollow pigments to enhance the light-scattering ability of coatings (J2), and the examination of reflection phenomena in particle sizing (J3). Studies concerning the use of light scattering for the examination of surfactant properties included the following: the interaction of a nonionic surfactant with poly(ethylene glycol) (J4), the characterization of surfactant micelles (J5-J8), the interaction of surfactants with emulsion polymers (J9-J11), the examination of linear viscoelasticity of polymers in solution (J12), and an investigation of the micellular phase of sodium sulfopropyl octadecyl maleate in solution (J13). Small-angle neutron scattering studies reported during this period included the analysis of polymerizable microemulsions (J14), the dependence of shear rate on the critical dynamics in polymer mixtures (J15), and the study of various additives to the growth of surfactant micelles (J16, J17). Other interesting studies of note included measurement of interfacial properties in a cationic surfactant (J18), the use of refractometry to measure the degree of ethoxylation in a nonionic surfactant (J19), and the use of an Abbe refractometer to measure the dispersion in refractive index measurements on nonlinear optical polymers (J20). Electrochemical impedance measurements are very popular for studying the corrosion potential of polymers and coatings systems. A number of excellent reviews were published (J21J26), as were specific articles concerning acrylic automotive top coats (J27) and the development of a simple electrochemical test to measure the barrier resistance of organic coatings (J28). Other unique applications of electrochemical impedance spectroscopy included the effect of functional silanes on the interphase in painted metal (J29), an examination of wet cathodically deposited paint films (J30), the detection and mapping of coating defects (J31), a study of damaged automotive paint films (J32), and a study of anticorrosive latex paint films (J33, J34). Complementary work included the evaluation of corrosion resistance from fractal analysis of electrochemical noise data (J35, J36), a comparison between electrochemical impedance and salt spray tests in evaluating coating barrier properties (J37), and an evaluation of underpaint corrosion (J38). Dielectric spectroscopy has been reported for the study of relaxation in UV-cured acrylated polysiloxanes (J39), adsorptive stripping tensammetry for the measurement of nonionic surfactant concentration (J40), and an accelerated laboratory test examined for the evaluation of corrosion resistance with water of low conductivity (J41). The adhesion of coatings to a variety of substrates was the subject of several reviews (J42-J44). Specific studies of interest include the examination of clear coating weatherability (J45), the testing of exterior coatings (J46), and the effect of surface
preparation on coating adhesion (J47). The measurement of polymer properties using ultrasonic spectroscopy was discussed (J48), as were photon correlation spectroscopy (J49), core excitation spectroscopy (J50), small-angle neutron scattering (J51, J52), positron annihilation methodology (J53), ultrasonic techniques (J54), and photothermal radiometry (J55). MICROSCOPY AND X-RAY TECHNIQUES Particularly interesting literature citations regarding the use of microscopic techniques for the examination of coatings included the use of atomic force microscopy on polymer latex films (K1), the study of fluid/fluid separation in colloid/polymer mixtures via light microscopy (K2), and the examination of a novel sugarbased surfactant using polarizing light microscopy (K3). The utilization of scanning electrochemical microscopy was also examined in detail (K4), including a book concerning reflection electron microscopy (K5), the use of electron microscopy to investigate liquid surfaces (K6) and the limitations of electron probe microanalysis applied to the characterization of coatings and layered structures (K7). Scanning electron microscopic (SEM) references continued, with a general review article concerning coatings applications (K8), a review of enhanced features in modern instrumentation (K9), and a microstructural examination of layered coatings (K10). Other publications of interest included a book dealing with scanning transmission electron microscopy (K11), the problems associated with the study of surfaces having low electrical conductivity (K12), and experimental conditions for the examination of painting cross sections via an environmental SEM (K13). Specific coatings examined during this period include acrylic maintenance finishes (K14), alkyd-melamine systems (K15), thermosetting polyesters (K16), multilayered automotive composites (K17), and UV-curable wood coatings (K18). Latex films received special attention (K19), as did the use of freeze-fracturing techniques (K20, K21), ellipsometry (K22), monodisperse polymer particles formed through photopolymerization (K23), and acrylicpolyurethane aqueous dispersions (K24) and the characterization of glycoside nonionic surfactants (K25). X-ray techniques have been applied in a variety of applications, including the following: scattering within polymeric materials (K26), the study of polymer interfaces (K27), the use of X-ray fluorescence in the surface finishing industry (K28), and the study of thermal spray vitrification for the removal of lead dioxide contained in paints (K29). Water-borne alkyd emulsions (K30), the X-ray microscopy of polymeric materials (K31), the examination of ultrafine titanium dioxide pigments (K32), and forensic (K33) and related analyses (K34) also received special attention. X-ray fluorescence spectroscopy was found to be particularly useful in the study of inorganic pigments in painted objects (K35) and the determination of trace metals in plastics (K36). The vitrification of lead oxide in red lead containing coatings (K37, K38), the solid state ordering of aromatic copolyesters (K39), lamellar structures in surfactant solutions (K40), and the correlation of thermal history and performance in thermoplastic powder coatings (K41) were examined using X-ray diffraction techniques. Finally, non-chromate pigments in paints were examined using X-ray absorption near-edge spectroscopy (K42) and quantitative surface analysis (K43) and the decorative/protective ability of a cathodic conversion coating on steel (K44) studied through the use of X-ray photoelectron spectroscopy.
THERMAL ANALYSIS Four new books have been published regarding the use of thermoanalytical techniques for the characterization of polymers (L1-L4); in addition, one extensive review article was published (L5). Other interesting applications of thermal analysis include studies related to the use of cone calorimetry to evaluate fire retardent properties (L6-L9), the characterization of polymers using simultaneous thermal analysis techniques (L10), the use of reaction calorimetry data to simulate emulsion polymerization kinetics (L11), an estimation of glass transition temperature at polymer surfaces from the temperature dependence of wetting (L12), and the examination of latex polymer film formation (L13). Coatings and coatings raw materials were examined, in general, through the examination of branched polysiloxanes (L14), an analysis of volatiles from esterified propoxylated glycerols (L15), an evaluation of the effects of structure on the thermal degradation of polyesters (L16), the analysis of phosphate-based pigments which are stable at high temperature (L17), and the study of soap-cobalt complexes (L18). The measurement of glass transition temperature through the use of differential scanning calorimetry (DSC) was the subject of a recent review (L19), as were studies correlating polymer structure with DSC behavior (L20) and the use of modulated DSC for the examination of a series of acrylic polymers (L21). Specific studies of interest to the coatings analyst include the measurement of automotive coating glass transitions (L22), the effect of chemical structure on the heat capacity differences observed at glass transition (L23), mechanisms for improving the observed baseline during heat of fusion measurements (L24), the observation of bound water in physically cross-linked hydrogels (L25), and the examination of divinyl ether cationic photopolymerization (L26). Among the sample types studied using DSC techniques were the following: UV-curable clear coats (L27), polyester resins (L28L30), allyl esters (L31), transesterified wax esters (L32), phenolic resins (L33), poly(oxyalkylene) oligomers (L34-L37), polyurethanes (L38-L42), polyacrylates (L43-L45), styrene copolymers (L46), polyethylene (L47), and melamine-formaldehyde resins (L48). Thermogravimetric analysis (TGA) was used to examine polymer degradation (L49), the volatiles present in primary optical fiber coatings (L50), the thermal degradation of polyurethanes via mathematical simulation (L51), characterization of phosphoruscontaining polyurethanes (L52), and the analysis of weathered sealants (L53), elastomers (L54), and poly[poly(ethylene glycol) phosphates] (L55). Dynamic mechanical analysis studies continue, with reports concerning accelerated clearcoat weathering (L56), the examination of thermosetting powder coatings (L57), the characterization of coil coatings (L58), an evaluation of allyl ester polymers and composites (L59), the stability of urethane/siloxane interpenetrating polymer networks (L60), and the study of urethane (L61) and optical fiber coatings (L62, L63). ENVIRONMENTAL AND INDUSTRIAL HYGIENE Most reported effort stems from the examination of methodology to determine the volatile organic content (VOC) of coatings and coatings-related materials. Specific studies include a comparison of EPA method 24 versus the Cal Poly method (M1), an optimal testing protocol for automotive coatings (M2), an interlaboratory study examining consumer paints (M3), a sorption Analytical Chemistry, Vol. 69, No. 12, June 15, 1997
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transfer secondary sorption procedure for measuring VOC in water (M4), and the measurement of VOC in the environment (M5). Techniques to improve the accuracy and precision of VOC measurements were examined in detail, with citations concerning the preparation of artifact-free sampling cartridges (M6), characterizing a site through an analysis of soil gas (M7), and a comparison of European and American techniques for evaluation of environmental matrices (M8). Specific coating types examined included water-based paints (M9, M10), ultraviolet-cured coatings (M11), alkyd-based paints (M12), and species leading to the formation of photochemical oxidants (M13). Flammability issues were treated in detail, with a recent book dealing with polymeric materials (M14), a handbook of fire retardant coatings and fire testing services (M15), a computer simulation based on molecular dynamics to investigate the flammability of model polymers (M16), an evaluation of the radiant panel test to measure fire retardance (M17), and the influence of covalently bonded phosphorus-containing compounds on polymer flammability (M18). Finally, a life-cycle analysis was performed on a series of alkyd emulsion-based paints (M19), and blood lead levels were measured in a group of house painters to evaluate toxic exposure potential (M20). MISCELLANEOUS MEASUREMENTS The use of dynamic mechanical measurements for the characterization of polymers continues to be popular, with the publication of studies concerning core/shell isomeric latexes (N1), latex films on paper (N2), accelerated clear coat weathering (N3), hydrogels (N4), and the examination of epoxy-based coatings (N5, N6). Ultraviolet-curable polyurethane acrylates received special attention, with citations relating structural properties to composition (N7-N9), special considerations for floor coatings (N10), and applications related to optical fiber coatings (N11) and polyetherbased elastomers (N12). Traditional examination of physical properties through stress/strain measurements included a general review article (N13) and the analysis of ultraviolet-cured fiberoptics coatings (N14, N15) and photosensitive polyurethanes based on castor oil (N16). Other miscellaneous measurements of note include the use of core excitation spectra to study polyurethanes (N17), a re-examination of accelerated weathering tests (N18-N20), the development of a wear/corrosion test (N21), the calculation of relaxation time in polyurethanes using additive group considerations (N22), and the evaluation of creep recovery in urethane acrylate oligomers (N23). Performance characteristics of thermosetting and radiation-cured coatings were reported (N24), as were the measurement of water vapor sorption (N25), an evaluation of the ASTM E662 smoke chamber (N26), the use of evaporative rate analysis for the measurement of cure (N27), and the simultaneous measurement of rheological and thermal properties (N28). Finally, an Ubbelohde viscometer was modified for the study of water-soluble polymers prone to foaming (N29), applications of dynamic light scattering for polymer solutions was reviewed (N30), interfacial toughness was measured using indentation tests (N31), the abrasion resistance of ultraviolet curable coatings was investigated (N32), and methods for measuring the adhesion of coatings to concrete examined (N33, N34). 20R
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ACKNOWLEDGMENT
The Author acknowledges Chemical Abstracts Service for access to STN International, which provided the literature search and to Witco Corp. for permission to publish this work. Dennis G. Anderson is Manager of Analytical Sciences for the Oleochemicals/Surfactants Group of Witco Corp. Prior to assuming this responsibility six years ago, Mr. Anderson was employed for 24 years by DeSoto, Inc., where he was involved in the analysis and characterization of polymers and coatings using chemical and instrumental techniques. He received B.S. and M.S. degrees in chemistry from Roosevelt University, where he is also a faculty member. He has authored or coauthored 32 publications dealing with the analysis of polymers and coatings and is coauthor of An Infrared Spectroscopy Atlas for the Coatings Industry. He is also the recipient of three Roon Foundation Awards for distinguished service to the coatings industry.
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