Coatings - Analytical Chemistry (ACS Publications)

Anal. Chem. 1999, 71, 21R-32R

Coatings Dennis G. Anderson

Witco Corporation, 5777 Frantz Road, Dublin, Ohio 43017

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Volatile organic compound (VOC) testing remains a critical factor in coatings formulation. This period saw a comparison of EPA method 24 versus the Cal Poly Pomona method (A21) as well as the use of a hollow fiber membrane and carrier gas stripping (A22), an improvement in ASTM D5403-93 for VOC in radiation curable coatings (A23), and a reexamination of the two methods cited by the California Air Resources Board for water content (A24). In terms of trace element analysis, a new paint reference material was proposed for the validation of test methods for metal migration in toys (A25); an interlaboratory collaborative study for the quality control of trace elements in paints was completed (A26), and an on-site extraction and anodic stripping voltametric determination for lead was recommended (A27).

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 1997 (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, miscellaneous measurements, gas chromatography, thermal analysis, and highperformance liquid chromatography. New or unique applications appear throughout the 508 references cited in this review. New books or extensive review articles appearing during this period include the analysis of lipids in fats and oils (A2), the examination of anionic fluorinated surfactants (A3), and the analysis of detergent formulations (A4). Compounds that change color with pH have been incorporated into coatings to detect underfilm corrosion (A5), and imbedded sensors have been used to monitor the extent of cure (A6). A novel method to determine degree of ethoxylation in poly(ethylene glycols) involved the use of microwave irradiation (A7). Other novel methods included the determination of anionic surfactants without the use of chlorinated solvents (A8), the removal of additives from polymers using supercritical fluid extraction (A9), improved methods to measure the wetting of titanium dioxide (A10), and the measurement of degradation index using intrinsic viscosity measurements (A11). The determination of hydroxyl value received special attention with publications dealing with the use of p-toluenesulfonyl isocyanate (A12), a revised German standard method (A13), and a simple Karl Fischer titration procedure useful for silanolterminated polysiloxanes (A14). Methods for the titration of surfactants continue with a general review (A15) and specific studies concerning anionic (A16, A17), nonionic (A18, A19) and amphoteric (A20) systems.

GAS CHROMATOGRAPHY Gas chromatography remains a powerful tool for the characterization of volatile species in coatings and coatings’ raw materials. Nonvolatile species in coatings can also be studied following degradation or derivitization to enhance volatility. Specific studies of interest to the coatings analyst include the characterization of poly(ethylene glycol) ethers (B1), the examination of volatiles and odors in radiation curable coatings (B2), the analysis of alkyl polyglucosides (B3), the direct measure of VOC in water-based coatings (B4), and the measurement of USP Organic Volatile Impurities by static headspace analysis (B5). Studies designed to improve gas chromatographic sensitivity also received special attention with an interesting study examining large-volume sample injections (B6). The determination of acrylate monomer species was published (B7), as was the determination of ethylene oxide in oxylated surfactants (B8, B9) and the characterization of coatings emissions during cure (B10). The species producing a fishy odor in soybean oil received special attention (B11), as did materials formed during the microbial degradation of alkyd resins and coating dispersions (B12). Inverse gas chromatography received special attention with the publication of several review articles (B13, B14) and specific studies relative to adsorption onto polymer surfaces (B15, B16) and the determination of acid-base properties for solid (B17) and pigment surfaces (B18, B19). Also of considerable interest were the examination of candidate coatings for chemical microsensors (B20) and the analysis of nonionic surfactants using capillary supercritical fluid chromatography (B21). Derivitization to produce volatile species amenable to gas chromatographic analysis continues, with the publication of studies concerning alkylbenzene sulfonates (B22) and the measurement of alkyl iodides from alcohol ethoxylates (B23). Pyrolysis studies of interest include several excellent review articles (B24-B27), an in-depth comparison of filament and Curie-point pyrolyzers

Review Contents 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 Acknowledgment Literature Cited

10.1021/a1990002v CCC: $18.00 Published on Web 03/09/1999

© 1999 American Chemical Society

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(B28), and chemometrics related to the quality control of paints (B29). Specific polymer types studied during this period included acrylate homo- and copolymers (B30-B33), varnish binders (B34), and polyurethanes (B35). Combining the separating power of gas chromatography with the qualitative analysis capability of mass spectrometry remains popular. Particular studies of interest include the examination of fatty acid isomers in dehydrated castor oil (B36), the evaluation of species in antifouling paints (B37, B38), the study of alkyl polyglucosides (B39), and the reaction of arylamines with acrylic monomers (B40). A number of excellent review articles have appeared, highlighting the use of mass spectroscopy in general (B41) and for the analysis of anionic surfactants (B42). The use of soft ionization techniques received special attention with the publication of papers dealing with coatings (B43, B44), polymers (B45), isocyanate-containing oligomers (B46), antioxidants (B47), poly(ethylene glycols) (B48), alcohol ethoxylate nonionic surfactants (B49), and the measurement of end groups in poly(methyl methacrylate peroxides) (B50). The use of matrix-assisted laser desorption time-of-flight (MALDI-TOF) mass spectroscopy is growing in importance for the examination of polymeric systems (B51-B56), ethoxylated oligomers (B57-B59), and poly(ethylene glycols) (B60, B61). GEL PERMEATION CHROMATOGRAPHY Gel permeation (GPC) or size exclusion (SEC) chromatography continues to have important applications for the separation of oligomeric and polymeric materials used in coatings. An extensive review concerning the use of GPC for the determination of polymer molecular weights was recently published (C1). Other interesting studies include the characterization of segmented polyurethanes (C2) and the use of GPC and Fourier transform infrared spectroscopy for polymer deformulation (C3) and determination of compositional heterogeneity (C4). The use of unique detectors also received special attention, with publications concerning the use of multiple detector systems (C5), laser desorption matrix-assisted time-of-flight mass spectroscopy (C6, C7), and gradient polymer elution chromatography (C8). Specific coatings systems studied included the following: polymers and oligomers used in coating applications (C9), waterborne epoxy coatings (C10), phenolic resins used in can coatings (C11), acrylic copolymers (C12, C13), cyclic oxyethylene succinate ether-esters (C14), polyester-acrylic polymers (C15), and polyurethane polyols (C16). HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY The determination of low-molecular-weight or monomeric species continues as a major use of high-performance liquid chromatography (HPLC) in coatings analysis. Of special interest were the quantitation of triglycerides and related species (D1), the determination of microbiocide retention during weathering (D2), and the examination of polymer additives (D3). Surfactants continue as key coating raw materials analyzed using HPLC, with specific papers dealing with anionic (D4) and cationic (D5) systems. Nonionic surfactants received special attention, including the study of nonionics as pesticide additives (D6), recent advances in the analysis of alkylphenol-based products (D7), measurement of surfactant polarity (D8), and coupling HPLC with advanced detector systems (D9-D11). Important applications noted in the 22R

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literature during this period include the analysis of oligomer systems using an evaporative light-scattering detector (D12), the examination of detergents and cleaning agents using thin-layer chromatography (D13), the use of temperature gradient interaction chromatography (D14), the use of two-dimensional liquid chromatography (D15), the determination of aerobic carboxylic metabolites of aliphatic alcohol ethoxylates (D16), the evaluation of airborne isocyanates as dibutylamine derivatives (D17), and the determination of 1-octanol-water partition coefficients and aqueous solubilities of fatty acid esters (D18). The utilization of HPLC for polymer characterization was the subject of a recent book (D19). Literature references in this area also highlight the examination of (methoxymethyl)melamine resins (D20, D21), phenolic resols (D22), surfactants in cleaning agents (D23, D24), alkyl polyglucosides (D25-D27), and alkanesulfonates (D28). Six papers were found concerning the analysis of polyether-containing oligomers, including the following: arylalkyl-substituted derivatives (D29), the effect of particle size (D30) and eluant composition (D31) on peak resolution, the determination of relative flame ionization detector response factors for oligomers of alkyl and aryl ether polyethoxylates (D32), the use of evaporative light scattering as a universal detector (D33), and the use of a dinitrobenzoate derivative for enhanced sensitivity (D34). References were located that cite the use of thin-layer chromatography for the characterization of ethoxylated fatty alcohols (D35) and ethoxylated methylbutylphenol (D36). Capillary electrophoresis offers another separation mechanism for coating constituents and raw materials. Among the more interesting applications reported were the separation of oligomeric nonionic surfactant components (D37, D38), the examination of Turkey Red Oil (D39), quaternary ammonium salts (D40), a compilation of general methods for polymer analysis (D41), and the analysis of polyethoxylates (D42, D43). INFRARED SPECTROSCOPY Infrared spectroscopy (IR) remains an extremely popular analytical tool for the examination of coatings and coatings’ raw materials. Several spectral compilations were published during this period, including automotive original top coats (E1), polymers, additives, surfactants, and their mixtures (E2), surfactants and surfactant mixtures (E3), and inorganic fillers (E4). The quantitative determination of polymer and filler content in paper coatings received special attention (E5), as did modeling of automotive coatings during drying (E6), applications of microspectral mapping on vinyl siding (E7), a critical evaluation of accelerated weathering tests (E8), degradation of acrylic-based coatings (E9, E10), radiation curable powder (E11), and intumescent (E12) coatings. The use of infrared spectroscopy to examine surface composition led to the publication of a book on attenuated total reflection spectroscopy (E13), one general review article (E14), two papers dealing with microscopic applications of Fourier transform (FT) techniques (E15, E16) and mirage-FT-IR (E17). Photoacoustic FTIR was reviewed relative to spectral depth profiling (E18), the examination of various reactions on polymer surfaces (E19, E20), and the unique information possible using measurements at high pressure (E21). Other unique surface measurements reported during this period include the prediction of automotive coating

service life (E22), the determination of surfactant concentration in multilayer films (E23), stratification with polysiloxanes (E24), the relationship between wood surface energy and surface composition (E25), and a review of methodology to measure phosphate coating weight on galvanized steel (E26). The determination of residual solvents in coatings was the subject of several studies (E27-E30) as was the measurement of consumer exposure to paint stripper solvents (E31) and the estimation of volatiles released during curing reactions (E32). The measurement of specific species and functional groups led to the publication of studies concerning acid and hydroxyl value determination (E33), the role of amine synergists and photoinitiators (E34) in radiation-curable coatings, the role of surfactants in latex formation (E35-E37), and the identification of minor products formed during linear alkylbenzene sulfonation (E38). Microemulsification polymerization of styrene stabilized by a nonionic surfactant and reactive cosurfactant (E39), the measurement of ethoxylation in nonionic systems (E40), and the study of anionic polyurethane ionomer dispersants in water-soluble baking enamels (E41) were also reported during this period. Numerous studies were also cited with emphasis on the characterization of polymeric materials. The use of high-pressure photoacoustic FT-IR spectroscopy was of special interest (E42), as was a rapid-scan version of 2D-IR spectroscopy (E43). Among the specific UV-curable polymer types studied were acrylates (E44-E47) and thiol-ene systems (E48). Melamine-containing clear coats received special attention (E49), as did polyglycolides (E50), the use of evanescent waves to study water diffusion through coatings (E51), and the use of a midrange infrared optical fiber probe for on-line monitoring of acrylate polymerization (E52). Acrylate-based polymers were the subject of numerous studies (E53-E57), as were vinyl esters (E58, E59), polyamides (E60), polyurethanes (E61-E66), and polyepoxides (E67-E70). Near-infrared (NIR) spectroscopic applications related to coatings continue to appear, with studies related to polymer reaction monitoring (E71), the quality control of polymer dispersions (E72), the measurement of hydroxyl number in polyols (E73, E74), monitoring polyurethane production through the loss of isocyanate functionality (E75), in-process analysis of multifunctional esters (E76, E77), and in situ curing of epoxy systems (E78-E80). Increasing numbers of applications employing Raman spectroscopy appear in the literature. Of specific interest to the coatings analyst are a handbook of polymer Raman spectra (E81), analysis of a number of clear coats (E82), the characterization of multilayer automotive paint systems (E83), the examination of polymer dispersions (E84), and polymerization reactions (E85). Also of special interest were reports dealing with the characterization of radiation-curable coatings (E86), vinyl acetate polymerization (E87), and a vibrational analysis of important group frequencies of melamine derivatives (E88). NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY Water-based coatings containing acetoacetoxy-functional polymers were recently studied by 13C nuclear magnetic resonance spectroscopy (F1), as were a chemoenzymatic transesterification of castor oil (F2) and oil-modified acrylic monomers (F3), the determination of glycerides in polyester-based coatings (F4), the

oligomer distribution in ethoxylated alcohols (F5), and the synthesis of cycloaliphatic UV coating diluents (F6, F7). The deblocking of blocked isocyanate adducts was studied in detail (F8) as was the regioselectivity of isocyanate-polyol reactions (F9), catalytic effects in urethane reactions (F10), the effects of antioxidants on acrylate polymerization (F11), and the measurement of end group concentrations in free-radical polymerization (F12). Also of interest in this period was the surface characterization of amine-containing latexes (F13), diffusion studies between surfactants and latex particles (F14), and the characterization of titanium dioxide using 27Al techniques (F15). The hydrolytic stability of phosphate ester surfactants was thoroughly examined using 31P methods (F16), as were anionic surfactants (F17), betaines (F18), and 23Na probes to study sodium ion dynamics in a mixture of latex and nonionic surfactant (F19). Two excellent books dealing with the use of nuclear magnetic resonance spectroscopy for polymer analysis were published during this period (F20, F21). In addition, distortionless enhancement polarization transfer was used to examine polymer microstructure (F22) and the influence of spacer groups on grafting ability in radiation-curable latexes (F23) was reviewed. Among specific polymer types of interest to coatings analysts were the following: analyses of alkyd resins (F24-F26), copolyesters (F27-F31), vinyl acetate copolymers (F32, F33), acrylate systems (F34-F39), ethoxy/propoxy copolymers (F40), poly(urethanes) (F41), and novolak-type phenolic resins (F42). SURFACE ANALYSIS The longevity and surface protection afforded by coatings are intimately related to the characteristics and properties of the surfaces over which they are applied. Characterization of these surfaces is of great interest to the coatings analyst. A critical review of surface analytical techniques (G1) and an excellent new book (G2) appeared during this period. Specific studies of interest included the use of electron spin resonance spectroscopy to characterize urethane clearcoats (G3) and surface characterization using Auger photoelectron coincidence spectroscopy (G4). X-ray photoelectron spectroscopy (XPS) or electron spectroscopy for chemical analysis (ESCA) continues to be the most popular technique for surface characterization. An excellent review on this topic recently appeared (G5) as did specific papers concerning the role of chromate phosphating of steel on paint adhesion (G6), the selective enrichment of reactive additives at the surface of UV-cured coatings (G7, G8), the changes in surface chemistry during the weathering of coil coatings (G9), the evaluation of environmentally friendly wood protection systems (G10), the examination of core-shell latexes (G11), and the evaluation of unsaturated monoethanolamide ethoxylates as paint surfactants (G12). Finally, an excellent review appeared during this period concerning the use of time-of-flight secondary ion mass spectroscopy (G13) and its application to the characterization of additives incorporated into weathered multilayer automotive coatings (G14). ULTRAVIOLET-VISIBLE SPECTROSCOPY Only four citations concerning the use of ultraviolet-visible spectroscopy were observed during the present review period. These included the binding of antioxidants and photostabilizers in polyurethane macromolecules (H1), the use of ultraviolet Analytical Chemistry, Vol. 71, No. 12, June 15, 1999

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photoacoustic spectroscopy to determine ultraviolet absorber distribution in clear paint layers (H2), the use of spectroscopic absorbance measurements to estimate critical micelle concentrations for ethoxylated alkylphenol surfactants (H3) and a review of luminescence spectroscopy as applied to the study of polymers (H4). SPECTROSCOPY. MISCELLANEOUS TECHNIQUES Compacting that occurs during drying was measured interferometrically (I1) as was film formation using dynamic light scattering (I2). Particle size characterization remains popular, with publications dealing with the examination of polymer latexes using centrifugation plus quasi-elastic light scattering (I3), measuring the optical behavior of organic pigments (I4), the study of coreshell pigments (I5), and the use of classical theory to design a pigment with improved optical properties (I6). Laser diffraction techniques were used to improve the characterization of organic pigments (I7); infrared ellipsometry was found to be useful for the analysis of chromate conversion coatings on aluminum (I8) and the diffusion of solvents from films during the curing process (I9). The quantification of coating adhesion using laser-induced decohesion spectroscopy (I10), dielectric spectroscopy as applied to styrene-butadiene latex dispersions (I11), and the evaluation of in situ cure characterization using thermally stimulated current spectroscopy (I12) were also reported. Glow discharge optical emission spectroscopy was noted for the measurement of elemental composition in a number of coatings systems (I13, I14), with special emphasis on in-depth profile analysis (I15) and the examination of curing mechanisms in water-borne isocyanate-free acrylic coatings (I16). Electron spin resonance spectroscopy was used to examine emulsion polymerization with cross-linking (I17), hydrogen transfer in adhesives containing phenolic antioxidants (I18), the change in can coating structure when in contact with food simulants (I19), and the direct measurement of oligomer entry into latex particles during emulsion polymerization (I20). Moessbauer spectroscopy was reported for the study of corrosion products beneath a primer containing anticorrosive pigments (I21), and neutron activation was employed for studying corrosion processes and the protective ability of paints and coatings (I22). MICROSCOPY AND X-RAY TECHNIQUES A recent review demonstrated how modern microscopic techniques can provide deep insights into films formed from aqueous latex dispersions (J1). Platelet-type pigments in automotive coatings were also studied (J2), as was the use of a scanning probe microscope to measure microhardness (J3) and atomic force microscopy to examine polymers (J4), latex films (J5), and chromate/phosphate conversion coatings (J6). Scanning electron microscopy (SEM) was used to examine film formation from acrylic emulsions (J7, J8), the effects of particle size in hard/soft latex blends (J9), and the migration of water through latex paint films (J10). Other applications of SEM included the characterization of paper coatings (J11), the degradation of epoxy aerosol can linings when exposed to fluorocarbon propellants (J12), the use of stainless steel as a protective pigment for steel structures (J13), the adhesion of an acrylic primer to pine (J14), and the wear behavior of coatings applied using accelerated electrospark deposition (J15). Three references were found during this period 24R


dealing with the use of transmission electron microscopy for coatings characterization. These include the study of organic pigments (J16) and water-based radiation-curable latexes (J17) and the interactions between thickener and latex particles in waterborne automotive coatings (J18). The use of X-ray fluorescence spectroscopy has, again, been reported for the determination of lead in paint (J19, J20). Other important references to the use of X-ray techniques include a review of small-angle scattering on latexes (J21), the study of conversion coatings for rubber bonding and paint adhesion (J22), variations in the orientation of kaolin particles depending upon application technique (J23), the penetration of acrylate coatings into concrete (J24), and a wide-angle diffraction study of copolyesters containing polyether polyols (J25). THERMAL ANALYSIS The use of a cone calorimeter has continued, with two general review articles (K1, K2) and studies of fire-resistant materials for aircraft applications (K3). Adiabatic reaction calorimetry was used to study free-radical polymerization (K4), microscale combustion calorimetry examined flammability (K5), a mathematical model was reported to calculate char formation and kinetic parameters of thermal degradation (K6), and a thermally stimulated current technique was used to study polymer aging (K7). Common thermal analysis techniques for characterizing polymeric systems were reviewed (K8). Specific publications dealing with the use of differential scanning calorimetry (DSC) included the study of intumescent coatings (K9), the measurement of glass transition temperature (K10, K11), the deconvolution of isothermal DSC data (K12), and the effect of glass transition region on the anticorrosive properties of coatings (K13). Modulated DSC was used for measuring thermal conductivity (K14), heat capacity (K15), polyurethane melting points (K16), interfacial macromolecular diffusion in core-shell latex particles (K17), and polymerization processes taking place on the surface of inorganic fillers (K18). Kinetic studies of thermosetting coating reactions were the subject of an excellent review (K19), as were the characterization of powder coatings (K20), methacrylate polymer syntheses (K21), the cure of vinyl ester (K22), and polyester (K23, K24) and alkyd (K25, K26) resins. Ultraviolet-curable epoxidized oils (K27) and cycloaliphatic epoxides (K28) were examined using differential photocalorimetry, along with the thermal curing of melamineformaldehyde (K29), urethane (K30), and epoxy (K31, K32) resins. Oxidative induction time measurements continue, with a review of experimental effects affecting reproducibility and repeatability (K33), a comparison of different testing methodologies (K34), possible modifications of ASTM D-3895-92 (K35), bias in pressure DSC measurements (K36), and a newly proposed polyethylene reference material (K37). The use of high-resolution thermogravimetric analysis for the study of polymers was the subject of an interesting paper (K38) as was the simultaneous use of thermogravimetry-mass spectroscopy for polymer analysis (K39). Other studies using thermogravimetric analysis include an evaluation of thermal decomposition and toxic products from intumescent coatings (K40), measurement of flammability in chlorinated polyurethanes (K41), an evaluation of the thermal properties of radiation-curable

coatings (K42, K43), and the characterization of several curing mechanisms for epoxy systems (K44-K46). Dynamic mechanical property measurements of particular note included the effect of anticorrosive pigments on the adhesion of waterborne acrylic paints (K47), the examination of particleparticle interfaces in reactive latex films (K48, K49), the characterization of two-stage latexes (K50), and the influence of microstructure in emulsion blends containing heterocoagulated composite particles (K51). Dynamic mechanical measurements were also used to study the cross-link density in thermoset coatings (K52), as well as amino-curable automotive refinishing paints (K53), solvent-free organic coatings (K54), and the cure of secondary carbamate groups by melamine-formaldehyde condensates (K55). Etch-resistant clear coats received special attention (K56), as did tricarbamate cross-linkers (K57), the viscoelastic properties of paper coatings (K58), structure-property relationships in polyester-urethane coatings (K59), and the enhancement of tensile strength and modulus in ultraviolet-curable urethane acrylates (K60). ENVIRONMENTAL AND INDUSTRIAL HYGIENE The examination of methodology for the measurement of volatile organic compounds (VOC) continues, with an evaluation of performance criteria for EPA method TO-17 (L1), a general review of test methods to determine VOC (L2), a reconsideration of ASTM D5403-93 for radiation-curable flexographic printing inks (L3), and a laboratory method for the measurement of VOC based on EPA method 24 (L4). Among the specific articles published relative to VOC determination were the determination of water content through reaction with calcium carbide to produce acetylene (L5), a study of substrate effects on VOC emissions from latex paints (L6), the rapid determination of VOC using solidphase extraction techniques (L7), and the measurement of solvent (L8) and fatty acid ester (L9) boiling points. The determination of formaldehyde in latex paints was examined (L10) as was the emission of formaldehyde during the curing of varnishes containing amino resins (L11). The exposure of workers to solvents in Chinese paint factories received special attention (L12), as did an evaluation of source reduction methods during the batch production of coatings (L13), the determination of isocyanates in spray painting operations (L14), the exposure of painters to solvent vapors (L15-L17) and the optimization of a new method for the detection of taste and odor causing compounds in water (L18). Sampling coating matrixes prior to lead determination was the subject of an ASTM special publication (L19). Other interesting articles related to the determination of lead in paint include a method for the analysis of soil (L20) and two critical performance evaluations for lead measurement in paint chips (L21, L22). Studies related to the flammability of water-based paints were reported (L23) along with the examination of fire test methods for fire-retardant polymers (L24). MISCELLANEOUS MEASUREMENTS This section deals with a number of techniques and measurements useful for the characterization of coatings and coatings’ raw materials that do not fit into the other subjects discussed. The use of electrochemical techniques was reviewed in detail (M1, M2) as was the use of cyclic corrosion and weathering test

methods (M3) and the use of dielectric spectroscopy (M4). An excellent series of papers was published on factors related to corrosion protection (M5-M8) and coating adhesion/disbondment (M9). The use of electrochemical impedance spectroscopy (EIS) to study the corrosion protection afforded by coatings was reviewed (M10, M11) as were measurements to determine service lifetime (M12), cathodic disbonding (M13), and an estimation of defect area under a coating (M14) and methods to evaluate how surface treatment affects coating corrosion performance (M15). Other interesting studies published during this period included an examination of mixed metal oxide inorganic/organic systems (M16), high-resolution studies capable of studying localized corrosion (M17, M18), and the advantages of a flowing versus a static electrolyte (M19, M20). The durability of coatings following thermal shock received special attention (M21) as did analysis following exposure to marine environments (M22), pickling effect corrosion (M23), and corrosion on steel (M24, M25). Among the specific coatings systems studied during this period were the following: latex paints (M26-M28), epoxy-based coatings systems (M29-M33), aircraft coatings (M34, M35), electrodeposited coatings (M36, M37) low-toxicity paints (M38), thermoplastic powder coatings (M39), zinc-rich coatings (M40M43), environmentally friendly systems (M44-M46), and petroleum sulfonates as additives in wax coatings (M47). Service life assessment using accelerated test methods received special attention (M48, M49), as did the evaluation of blister tests (M50) and accelerated natural and synthetic weathering (M51-M56). Salt fog erosion of organic coatings was studied in depth (M57, M58), as was the corrosion behavior of coated steel (M59) and silicone rubber (M60). Mechanical property testing was reviewed as it related to structure-property relationships in coatings (M61-M63). Also studied was the effect of surface functional groups on tensile strength (M64), the development of physical properties in thermosetting and radiation-cured coatings (M65), factors leading to improved abrasion resistance in floor coatings (M66), uncertainties in adhesion measurements on a number of substrates (M67-M69), and quantitative evaluation of coating texture (M70). Dielectric measurements were used to assess micellular configuration in emulsions (M71) as well as sedimentation in suspensions of polymer-coated silica (M72). The measurement of coating adhesion was reviewed (M73) as was the examination of crosslinked acrylic latexes (M74) and the depth profiling of multilayered automotive coatings (M75). Dynamic surface tension measurements were reported for radiation cure coatings (M76) and for mixed-surfactant systems contaminated with alcohols and esters (M77). A crater grinder test was reported for the measurement of abrasion resistance (M78), a mathematical model was developed for drying paint (M79), and a new test to measure wet scrub/ cleanability was proposed (M80). Evaporative rate analysis continues as a technique to evaluate coating cure (M81), a microwave scorch test was proposed to evaluate antioxidant synergists for urethane foams (M82), a graphical osmometric procedure was developed to measure viral coefficients for polymers (M83), and the addition of pH indicators to coatings was found to provide an indication of underfilm corrosion (M84). Analytical Chemistry, Vol. 71, No. 12, June 15, 1999

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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 Performance Chemicals Group of Witco Corp. Prior to assuming this responsibility eight years ago, Mr. Anderson was employed for 24 years by DeSoto Inc., where he was involved with 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 was also a faculty member. He has authored 34 publications dealing with the analysis of polymers and coatings and was 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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(M78) Gahlin, R.; Larsson, M.; Hedenqvist, P.; Jacobson, S.; Hogmark, S. Surf. Coat. Technol. 1997, 90(1-2), 107-114. (M79) Wilson, S. K. Surf. Coat. Int. 1997, 80(4), 162-167. (M80) Grochal, P. Farbe Lack 1998, 104(7), 83-86, 89-90. (M81) Sharp, K.; Mattson, G.; Jonsson, S. J. Coat. Technol. 1998, 70(877), 97-100. (M82) Andrews, S. M. 60 Years Polyurethanes, [Int. Symp. Exhib.]; Kresta, J. E., Eldred, E. W., Eds.; Technomic: Lancaster, PA, 1998; pp 101-119. (M83) Amur, K. S.; Harlapur, S. E.; Aminabhavi, T. M. Polymer 1997, 38(26), 6417-6420. (M84) Zhang, J.; Frankel, G. S. Tri-Serv. Conf. Corros. Proc.; National Technical Information Service: Springfield, VA, 1997, Vol. 1, pp 8/1-8/16.

A1990002V

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