Anal. Chem. 1993, 65, 1R-11R
Coatings Dennis G. Anderson Witco Corporation, 6200 West 51st Street, Chicago, Illinois 60638
Review Contents Introduction Chemical and Electrochemical Techniques Gas Chromatography Gel Permeation Chromatography High-PerformanceLiquid Chromatography Atomic Absorption and Plasma Emission Spectroscopy 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 (Including Physical Tests)
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Dennis G. Anderson is Manager of Analytical R&D for the Oleochemicals/Surfactants Division of Witco Corp. Prior to assuming this position two 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. Mr. Anderson has authored or coauthored 29 publications dealing with the analysis of polymers and coatings and is coauthor of A n Infrared SpectroscopyAtlas for the Coatings Industry. He is also the recipient of three Roon Foundation Awards for distinguished service to the coatings industry.
the polarographic determination of acrylic monomers (B9), potential-time measurements for optimization of surfactants in phosphating additives (BIO),and electrochemicalmethods for laboratory corrosion testing (BII).
GAS CHROMATOGRAPHY INTRODUCTION 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 1991 ( A I ) . The contents are divided into 15 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, spectroscopy-miscellaneous techniques, gas chromatography, and thermal analysis. New or unique applications for established analytical techniques appear throughout this review. Severalgeneral articles of interest have appeared, including the evaluation of paints to protect concrete (AZ),examination of the Rausch method for converting subjective evaluations into quantitative measurements (A3),methods to evaluate the service life of coatings (A4),examination of the efficacy of nonmercurial preservatives (A5) and structure-property relationships in automotive clear coats (A6). A review examining the changing face of paint analysis was published ( A n ,as were reviews of powder coatings analysis (A&, testing UV-curable coatings for wood (A9), two books (AIO, A l l ) and two reviews (AI2, AI3) examining general polymer analysis (AI4),reviews of analytical techniques useful for the analysis and characterization of silicones (AI5-AI 7), rubber testing (AI8, AI9), and the analysis of surfactants (AZO).
CHEMICAL AND ELECTROCHEMICAL TECHNIQUES The use of instrumental analysis techniques for the characterization of coatings remains on the increase;however, chemical and electrochemicaltechniques continue to provide useful information. Publications concerning the analysis of red pigments and mercury red ( B I ) ,a review of elemental analysis for the characterization of polymers (BZ),and the determination of sulfur in polystyrene emulsion polymers (B3)were noted during this period. Specificfunctional group analyses included the measurement of hydroxyl functionality in phenol formaldehyde oligomers (B4),residual isocyanate groups in polyurethanes (B5),oxirane content in epoxy resins (B6),and carboxyland sulfate groups in polyelectrolytes (B7). Other studies of interest include the examination of surface acidity using the contact angles of seven probe liquids (B8),
Gas chromatography remains the primary analytical technique for the examination of volatile species in coatings and volatile species generated following chemical and thermal degradation. Solvent analysis continues, with publications on the effect of organic solvent exposure on liver function (CI), the composition of solvents in inks (C2),the determination of residual styrene in unsaturated polyesters (C3),the examination of cured polyurethane floor coatings for unreacted toluene diisocyanate (C4), and the determination of paint odor components (C5). The uptake of oxygen during the oxidation of acrylic and alkyd coatings was examined using gas chromatographic analysis (CS), as were the measurement of nonionic surfactant polarity index (C7), polymer solubility (C8) and interaction (C9) parameters, the thermodynamics of alkane-silicone polymer interactions (CIO), and the determination of oxygen in anaerobic sealant formulations ( C I I ) . Headspace techniques continue for the concentration of volatile species, with studies concerning volatiles from pine (CI2), the solubilization behavior of solvents in surfactant solutions ( C I 3 ) , the examination of volatile species in aerosol products (CI4),and the study of thermal desorption cold trap analysis of air volatiles (CIS). Two studies were also published relative to the measurement of leaching rates for organotin compounds used in antifouling paints (CI6, CI7). Chemical degradation of polymers is frequently necessary to produce species suitable for gas chromatographic analysis. Among the specific studies reported during this period were the following: the examination of fine art using gas chromatographic analysis techniques (CI8),new techniques for the analysis of fatty acids (CI9, CZO), intermediate identification during oleic acid dimerization ( C Z I ) , a review of polyester and alkyd resin analysis (C22),the degradation of polysulfones through alkali fusion (C23),the selective degradation of siloxane-capped polyimides (C24),and the characterization of ethoxylated fatty alcohols (C25). Controlled pyrolysis also remains popular, with publications concerning the determination of vulcanization accelerators (C26) and the use of a purge and trap sampler to concentrate pyrolysis products (C27). Specific polymer types examined by controlled thermal degradation include acrylates (C28-C30), alkyds (C31),styrene copolymers (C32),polycyclohexanone (C33),silicones(C34),varnishes (C35),polyamides (C36),and epoxies (C37, C38). Coupling a mass spectrometer to the gas chromatograph dramatically increases the qualitative analysis capability of @ 1993 American Chemical Society
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the combined system (C39). The following studies were of interest to the coatings analyst: the use of l19Sn as a tracer to examine tributyltin degradation (C40),new techniques for the examination of volatile trace impurities in environmental matrices (C41),the examination of fatty tertiary amines (C421, the sequencing of copolymer structures (C43),the location of double bonds in fatty acids (C44),maleate plasticizer analysis (C45),the examination of organosilicones ('2461, and epoxy resins (C47-C49). An emerging technology for the analysis of polymers and coatings is supercriticalfluid extraction and chromatography. A review has been presented documenting the use of supercritical fluids for the spray application of low-pollution coatings ((250). Analytical studies of interest include techniques for large-volume injection in capillary systems (C51), techniques for analytical parameter optimization (C52,C53), and the use of a Fourier transform infrared detector (C54). Specific polymer and coatin types reported were as follows: antioxidants, lubricants, an antistatic agents in polyolefins (C55-C58), polymeric surfactant characterization (C59),the examination of automobile coatings (C60), alcohol ethoxylates (C61), the evolution of formaldehyde, and methanol during the cure of high-performance coatings (C62).
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GEL PERMEATION CHROMATOGRAPHY Gel permeation (size exclusion) chromatography was the subject of two excellent review articles (01,0 2 ) and a review of techniques for the determination of coating resin molecular weights ( 0 3 ) . Other general articles of interest during this period include the performance characteristics of a highefficiency chromatographic system ( 0 4 ) , an evaluation of deconvolution techniques to correct for peak broadening (05, 0 6 ) ,an experimental evaluation of conflicting models for gel permeation chromatography (on,and special techniques for the examination of water-soluble ( 0 8 )and emulsion polymers ( 0 9 ,010). Examination of specific polymer types has led to the publication of studies concerning the characterization of acrylates (011-014), poly(vinylpyrro1idone) (0151, polystyrene (016-019), polyesters (020, 021), alkyd resins (022, 0 2 3 ) ,vegetable oils ( 0 2 4 ) ,polyethers (025,026),urethanes ( 0 2 7 , 0 2 8 ) ,polycarbonates ( 0 2 9 ) ,and silicones ( 0 3 0 , 0 3 1 ) . Three special studies of interest during this period were the examination of sodium polyacrylates ( 0 3 2 , 0 3 3 )and hydrolyzed poly(viny1 acetate) ( 0 3 4 ) .
HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY High-performance liquid chromatography remains a popular tool for the examination of coatings and coating-related materials. Several general reviews have appeared during this period ( E l ,EZ), as has a review dealing with the analysis of dyes and chemicals for leather ( E 3 ) . Solute-polymer interaction constants were measured in a number of systems (E41 as was the evaluation of amino acid separation efficiency in capillary zone electrophoresis (E5). High- erformance liquid chromatography continues to be reportex for the determination of inhibitors in monomers (E6,E n , additives and antioxidants in polymers (E8-E12), and optical brighteners in detergents (E13). The analysis of polymeric materials included published reports concerning catalyzed isocyanate reactions (E14,E15),the stereospecific separation of species in triacylglycerols ( E l 6 ) ,the hydrolysis of methoxylated melamine resins (Eli'), and the characterization of acrylate (E18, E19), styrene (EZO), acrylonitrile (E21),ethylene propylene dimethacrylate (E22),and stereoisomeric (E23),silicone (E24),and epoxy (E25) polymers. Surfactants received special attention, with several studies concerning the separation of anionic species using thin-layer chromatography (E26)and reversed-phase (E27-E29) and ion-exchange (E30-E32) columns. Thin-layer chromatography was reported for the characterization of impurities in nonionic surfactants (E33)as was the separation of quaternary ammonium surfactants with the use of a normal-phase system and an evaporative light scattering detector (E34). Papers dealing with the use of field flow fractionation for the examination of polymers continue,with two general review articles (E35,E36), and the use of thermal (E37-E39), flow 2R
ANALYTICAL CHEMISTRY, VOL. 65, NO. 12, JUNE 15, 1993
(E40,E41 ), and sedimentation (E42,E43) as the driving forces for separation.
ATOMIC ABSORPTION A N D PLASMA EMISSION SPECTROSCOPY Several useful studies have been published utilizing atomic absorption and plasma emission spectroscopy for the examination of polymers and coatings. The atomic spectroscopy of silicones has been exhaustively reviewed ( F I , FZ), as has the use of flow injection to improve the accuracy of the standard additions technique (F3)and the effects of etching pretreatment on electrodeposit adhesion (F4). Studies relative to the leaching of metals from antifoulingpaint continue, with published reports on copper leaching from triphenyltin systems (F5),the examination of antifouling paints based on calcium resinate (F6),the characterization of leaching rates from organotin-free coatings systems (F7),and the use of a graphite furnace for the measurement of total tin leached from ship paints (F8). Other unique studies of interest to the coatin s analyst include the examination of lead in poly(viny1 chloridie) (F9),the measurement of mercury emission from latex paint films (FIO),the determination of barium, cadmium, zinc, and phosphorous in vinyl stabilizers ( F I I ) ,the automatic dissolution of trace metals from epoxy laminates with acid (F12),and the determination of isotope ratios via plasma mass spectrometry (F13).
INFRARED SPECTROSCOPY Several books using infrared spectroscopy for the characterization of polymers have appeared ( G I , G2) as have publications concerning recent advances in the Fourier transform infrared spectroscopy (FTIR) of polymeric systems (G3, G4), practical applications of FTIR microscopy (G5G7), the examination of coating defects through infrared imaging (G8),and FTIR surface analysis studies ( G S G 1 2 ) . Photoacoustic infrared spectroscopy was reported for the study of thermosetting coating cross-linking ( G I 3 ) ,as were the use of image analysis for the study of pigment dispersion (G14,G15),FTIRdichroismforpolymersurface studies (GI@, new techniques for preparing paint samples for microscopic examination (G17, G18), and the use of FTIR for the examinationof coil (G19),automotive (G20),andalkyd (G21) coatings. Special analytical studies of general interest included the construction of a automated in-plant analytical system to monitor epoxy resin production (G22),the determination of film thickness using a low-energy infrared sensor (G23),and the study of mutual diffusion in polymers (G24). The use of infrared spectroscopy for the detection and quantitation of specific species continues, with reports concerning the use of near-infrared techniques (G25),the analysis of paint solvents (G26),the estimation of flexural modulus in reaction-injection molded polyurethanes (G27), the determination of hydroxyl (G28, G29),epoxy (G30),and residual unsaturation (G31),water absorption in UV-curable fiber optic coatings (G32),and coating moisture determination (G33). The Curtis rearrangement during diisocyanate monomer preparation was studied (G34),as were the determination of ethylbenzene hydroperoxide (G35), the composition of ethylene oxide-propylene oxide surfactants (G36, G37), the mobility of surfactants in acrylate latexes (G38, G39) and coatings (G40),pH effects on amine oxide surfactants (G41), and the determination of light stabilizers in polyolefins (G42, G43). Fourier transform Raman spectroscopy was the subject of four review articles (G44-G47), and studies specific to the examination of coatin s (G48), autoxidation in some fatty acid methyl esters ( d 9 ) , acrylate homopolymers (G50), conversion coated aluminum (G51),and the in situ identification of thin-layer chromatography fractions (G52). Studies of many polymer types were reported, including acrylic latexes (G53, G54), styrene-containingacrylate polymers (G55-G57), blocked isocyanatoethyl methacrylate polymers (G58),and ethylene-containing polymers (G59, G60). The characterization of radiation-curable coatings has received special attention, with a review (G61),the examination of photopolymerization kinetics (G62-G66), the real-time monitoring of polymerization quantum yields (G67), and structure-property correlations (G68, G69). Other polymer
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t es receivin attention durin this period were polyuret%es (G70-8741,polyesters (875-G79)ipolyimides (G80), epoxies (G81-G84), and siloxanes (G85, 86). The measurement of physical properties through the use of FTIR spectroscopy resulted in the publication of mechanical and surface ropert studies (G87), sulfur mustard percolation thro paint h m s (G88),correlatingaccelerated with natural weaxermg (G89-G91), hydrogen bond formation in polyurethanes (G92-G94), the study of epoxy-coated aluminum alloys (G95), and the role of metal catalysts in Bisphenol A cyanate ester curing (G96). Other special studies of interest to the coatings analyst include the examination of oxidative degradation (G97), additives to increase the anticorrosiveproperties of poly(viny1acetate) coatings (G98),the thermal (G99-G102), radiative (G103), and oxidative (104) degradation of polymers, the kinetics of polyurethane reactions (G105), the study of water-based inor anic adhesive primers (GI(%), and the measurement of PO ymer ignition temperatures in oxygen-rich atmospheres (G107).
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NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY One general review of nuclear magnetic resonance (NMR) spectroscopy appeared durin this period (H1) as did more specific renews concerning t e examination of etroleum products (H2) araffinicFischer-Tropsch waxes (&3),model printing inks (841, conductingpolymers (H5),ionomers (H6), and heterogenous ~ o l (H7). r Other general studies included the use of 2 Si MR to examine siliconeresins (H8), twedimensional13CINADEQUATE studies of cycloaliphatic epoxy monomers (H9), the evaluation of acrylic monomersulfur dioxide copolymers (HIO), the direct observation of residual monomers in cross-linkedpolyesters using solid-state 1% techni ues (H11), and the examination of adhesivejoints using NMIt imaging (H12, H13). Studies of monomeric and oligomeric species related to coatings analysis included a review of aqueous surfactantphase science (H14),the examination of anionic surfactants with divalent counterions of separate electricalcharge (H151, poly(ethy1ene oxide) ionic association (H16, H17),and the desulfonation of 0-sultones during the synthesis of a-olefin sulfonates (H18).The electronic pro erties of polymers formed from vinyl isocyanate and m eic anhydride were studied (H19),as well as the characterization of degradation groducts of hosphorus-containing polymer additives usin 1P NMR (d20) and the examination of stabilizers for v i n j polymers (H21). Polymers received special attention, with the publication of three general review articles (H22-H24), the applications of high-resolution solid-state 1% NMR to 01 era (H25H27), a review of two-dimensionalNMR app 'e to the study of polymers (HB), reviews concerning the determination of monomer sequence distribution on copol era (H29, H30), and a review of macromolecular morpho!? (H31). Many condensation polymer types were examineencluding polymer electrolytes (H32),cis-trans isomerization in long-chain aliphatic quaternary ammonium salts (H33), polyester sequence distribution (H24-H38), and the s t r u ~ ~ u ranalysis al of an alkyd resin (H39). Other typical addition polymers studied were as follows: polyurethanes (H40-H44), isocyanurates (H45),the reaction roduct of gl cero1 2-phosphoric acid and diphenylmethane d?imcyanate (f;46), cycloaliphatic epox resins (H47), epoxy resin cross-hnlung (H48-H51), Bispgenol A cyanates (H52), Bisphenol A olycarbonates (H53),e ichloroh drin polyethers (H54) m$ pol siloxanes (H55, d 6 ) . AdJtion polymer t e8 examinezin detail included the following: structural c anges during the environmental de adation of coatingscontaining emulsion acrylic copolymers methacrylate copolymer sequencing ( ~ 5 8 H62), acrylonitrile-containing systems (H63-H67), methacrylic acid-poly(oxyethy1ene)co lymers (H68), acrylic acid copolymer microstructure (H69, vinyl acetate-containing systems (H71-H73), polyolefims (H74-H76), maleic anhydride copolymers (H77), and the study of acetal ring conformations in poly(viny1 acetal) resins (H78).
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SURFACE ANALYSIS Many of the ultimate pro erties of coatings are determined by the integrity of the s J a c e upon which they are placed;
therefore the characterization of surfaces is extreme1 important to the coatings analyst. During this period: the activities of ASTM Committee E-42 on surface analysis were reviewed (11).The eneral field of surface analysis was also reviewed (12,13), afong with specific reviews dealing with ion-scatterin s ectrometry (14), techniques for examining the surface of siicones (IS), surface structure through laser desorption (16),and the use of probe molecule chemisorption in the characterization of catalyst surfaces (17). X-ray photoelectron s ectroscopy or electron s ectroscopy for chemical analysis (EgCA)continues to be withy used for the characterization of surfaces. Standard practices for checking spectrometer operation (18)and determining 8 ecimen area contributing to detected signal (191, stantard practice for reporting spectra (110),and methods for ensuring quantitative accuracy (111)have been reported. Amon? the specific studies of interest were the followin the selectivity of surface hydroxyl derivitization using trifuoroacetic acid (1121, the investigation of lacquer failure on tinplate (1131, the evaluation of adhesion promoters for alkyd paints (1141, the study of acrylic coating degradation (115),the evaluation of water-based inor anic rimers (116, 117), and polymer studies involvin po!yuretkane (1181, polypro ylene (1191, polyimide (120),!atex (121), and polyacrylate (f22) systems. Publications continue reportin use of Auger electron spectroscopy, with reviews consi ering the interaction of surfaces with the environment (1231, the development of materials with im roved properties (124,1251,corrosion of phosphatized steef(126) and standard methodolo relating to surface analysis (127), the reporting of Auger %a (1281, and background subtraction techniques (129). Second mass spectroscopy (SIMS) has been reported aa an exce ent tool for the analysis of advanced materials (130,131) and the examination of metal phthalocyanines (1321, oxygen-containing olymer structures (1331, polymer interfaces (134) polymeta! crylates (135),and silicone release coatings (136).
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ULTRAVIOLET-VISIBLE SPECTROSCOPY Ultraviolet-visible spectroscopycontinues as a useful tool for the Characterizationof coatings. A useful book concerning polymer spectroscopy has a peared (JI),as have extensive reviews of metallic aint co orimetry (J2) and surfacg color analysis (J3). Visibpe spectroscopy has been reported for the examination of turbidity during latex film formation (J4), the determination of latex coating hidin power (J5, J61, acrylic polymer coating dry hiding (J7),an scattering within paper coatings (J8),the evaluation of emulsion polymer particle size wa turbidity (J9),and the examination of normal and hemispherical emittance from black silicone paints for space applications (JIO). Ultraviolet spectroscopy has been reported for the study of acrylate copolymer composition (J1l ) ,acylation kinetics (J12), diisocyanate determination jJ13),amino groups .in polyimides (J14), carbonyl determination (J15),potential paint oils from,central India (J16), UV absorbers within automotive coatings (JI7), surfactant com osition (J18,J19) and siloxane characterization (J20). PubEcations of special interest include a comparison of radiometers for the examination of UV coat' cure speed (F21), the photodegradation of polyurethaneacry tes (F22)and poly(viny1chloride) (F23), and the efficac of polymers containing ultraviolet stabilizer moieties laceialong the polymer cham (~24).our papers appeared) using fluorescence spectrosco y, including the determination of resin particles in aper ( 25),the evaluation of block polymer aggre ation ( 26), the study of epoxy polymer cross-linkin (#27), and methods to characteree energy migration an excimer formation in vinyl aromatic polymers (F28).
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SPECTROSCOPY-MISCELLANEOUS TECHNIQUES Time-resolved infrared radiometry was reported for the examination of multilayer organic systems using subsurface heating (KI), as waa the utilization of ultrasonic waves (K2), luminescence spectroscopy (K3), Fourier transform photon echo spectroscopy (K4), and ion beam analysis (K5) for the examination of coatings and pigments. Other s ecific tests developed for the examination of coatings inclufe the use of ANALYTICAL CHEMISTRY, VOL. 65, NO. 12, JUNE 15, 1003
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objective parameters (K6), the examination of optimum pigment volume concentrationin epoxy coatings (K7),contact angle measurements on latex paints (K8),the examination of car wash resistance for automotive coatings ( K 9 ) , the modification of flame retardants useful in UV-curable coatings (KIO), the study of wear properties in electrodeposits ( K I I ) , and the nondestructive gauging of coatings using backscattered @ particles (K12). Electron energy loss spectroscopy continues to be used in material science (K13) as does the evaluation of artificial weathering devices for the prediction of coating durability (K14-KZO). Improvements in adhesion for automotive coatings was studied following corona discharge (K21)and exposure to water (K2.2). Other studies of interest to the coatings analyst include electrokinetic measurements (K23),microwave spectrometry (K24), and the use of solubility parameters (K25). The protection of substrates from corrosion continues to be studied extensively, with several new review articles published (K26-K28),as well as specific papers dealing with exposure to Arctic waters (K29), the use of electrokinetic potential measurements (K30), and electrochemical noise analysis (K31). Other electrochemical techniques which continue to be used include dielectric analysis (K32-K36) and conductometry (K37-K40). Of special interest were general studies incorporating electrical impedance measurements (K41-K47) and special studies of epoxy (K48, K49), polyester melamine (K50), styrene acrylate (K51), alkyd (K52),and polyurethane (K53,K54) coatings systems. Impedance spectroscopy also continues to be reported for the study of substrate corrosion, particularly when sodium chloride electrolyte solutions are used (K55-K57) Spectroscopic determination of latex and pigment particle size continues to be studied using photon correlation spectroscopy (K5B-K60),quasielasticlight scattering (K61-K63), dynamic li ht scattering (K64),angle-resolved light scattering (K65), disf centrifugation (K66, K67) and mercury porosimetry (K68). Other techniques of interest include the examination of coated surfaces with Moessbauer spectroscopy (K67-K72) and free-radical-containing systems via electron spin resonance spectroscopy (K73-76) and electron paramagnetic resonance spectroscopy (K77, K78).
MICROSCOPY AND X-RAY TECHNIQUES Light microscopy continues to provide useful information for the characterization of polymers ( L I ) ,particularly during the study of fracture mechanics (L2). Transmission electron microscopy was reported for the examination of polymer deformation (L3),poly(buty1 methacrylate) latex film morphology (L4,L5),styrene acrylate core-shell emulsion polymer morphology (L6),and polystyrene particle size (L7). Reports utilizing scanning electron microscopy continue to appear, with a review on the examination of coatings (L8), the evaluation of coating buildup during electrodeposition (L9), the adhesion of latex coatings on weathered substrates (LIO), electrostatic interactions in paper coatings ( L I I ) , coating surface topography (L12),coating microstructure following scratch testing (L13),and the evaluation of galvanized steel corrosion under automobile coatings (L14,L15). Among the specific polymer types studied were hydrogenated styrene butadiene block copolymers (LI6),polyolefins (LI 7), poly(vinyl chloride) (LIB),and thermally sprayed coatings (L19). Other microscopic techniques of interest to the coatings analyst include the use of scanning tunneling microscopy (LZO),field ion microscopy (L211, ion beam analysis (L.221, surface secondary ion microanalysis (L23),image analysis for the study of electrophoretic thermal barrier coatings (~5,241, waveguide microscopy (L25),and thermal wave microscopy for the examination of steel corrosion (L26). Coupling X-ray techniques to a scanning electron microscope greatly increases the utility of the information enerated. Studies of interest in this regard include the ciaracterization of particulate emissions from dye pigments (L27), the examination of pigments in coated paper (L28,L29),the examination of coatings for rusty steel (L30), and failure analysis following scratch testing (L31). Analysis of coatings and polymers using X-ray techniques alone included a general review (L32),the use of X-ray fluorescence in the plastics industry (L33),polymerization catalyst analysis (L34,L35), the detection of lead in paint (L36-L38),the examination of 4R
ANALYTICAL CHEMISTRY, VOL. 65, NO. 12, JUNE 15, 1993
silicone (L39),urethane (L40),and propylene (L41)polymers, and testing material wear resistance (L42).
THERMAL ANALYSIS Four excellent general review articles have appeared (MIM4) detailing the use of thermoanalytical analysis, as well as publications regarding the examination of polymer flammability (M5),the thermal analysis of thin films (M6),poly(viny1 ether)-polystyrene interpenetrating networks (M7), and polyurethane block deformation (M8). Studies relating the use of dynamic mechanical analysis to measure automotive coating glass transition temperature (M9),the relationship of coating parameters to hot dip-coating performance (MIO), and the determination of optimum cure times for encapsulation (MI1) have also appeared. Thermal volatilization analysis was reported for the study of a styrene-methacrylic acid copolymer (M12),and the cone calorimeter for examining poly(pheny1ene oxide) (M13),polymer fire parameters (M14), the thermal conductivity of polymers (M15), the ambient cross-linking of epoxy resins (M16),heat and smoke release during the combustion of plastics (M17), and heat generated during the peeling of polymeric films from metal substrates
(M18). Differential scanning calorimetry continues as a popular technique for the examination of polymers and coatings. Two review articles have appeared (M19,MZO), as have publications dealing with the examination of paint media (M21), mature oil paint films (MZZ),crystallinity density in polyolefins (M23),modeling of cross-linking kinetics (M24),effects of y irradiation on polyketones (M25),and examination of polymer blend miscibility (M26). Among the specific studies using differential scanning calorimetry during this period were the cross-linking of acrylic-polyurethane fiber optics coatings (M27-M29), oxyethylene methacrylate polymerization dynamics (M30), alkylphenyl methacrylate kinetics (M31), ethylene polymer irradiation (M32),polyester cross-linking (M33),and the use of amines to cross-link functionalized polystyrene (M34). Cross-linking of epoxy resin systems has received special attention, with publications studying photinitiation of the curing reaction (M35), the use of an autocatalytic kinetic model 04361, the deconvolution of multikinetic events (M37),the use of dynamic mechanical measurements (M38),and cure via sulfones (M39, M40), amines (M41),and anhydrides (M42). Other specific polymer types reported on were alkyd resins (M43),cyanate ester polymerization (M44), vinyl ester resins (M45), phenolformaldehyde curing (M46),polyurethanes (M47),polyimides (M48), polyesters (M49), and evaluation of antioxidant efficacy (M50-M52). Thermogravimetry is also highly utilized for the examination of coatings and coating-related materials, with pa ers dealing with the examination of vinyl ester resins (&3), poly(ethy1ene terephthalate) (M54), polyester plasticizer analysis (M55), ethylene acrylic copolymers (M56), poly(methyl methacrylate) (M57, M58),melamine (M59), and phenol formaldehyde condensates (M60) a pearing during this period. Other specific polymer stu8es include the thermal degradation kinetics for polyimides (M61, M62), polywethaneisocyanuates (M6>M65), polyperoxidea (M66), and nonionic surfactant ethoxylates (M67).
ENVIRONMENTAL AND INDUSTRIAL HYGIENE The systematic evaluation of biodegradable solvents for the removal of grease and masking wax from aircraft prior to painting was reported ( N I ) as , were the use of passive samplers for the determination of volatile organic solvents (N2),food contamination by solvents released from plastics (N3),toluene absorption in an epoxy coating system (N4),indirect fertility analysis in painters exposed to ethylene glycol ethers ( N 5 ) , evaluation of an automated apparatus for the determination of solvent permeability through elastomer gloves (N6),and investigation of coating industry solids as a fuel source (N7). Other interesting publications involved measurement of petroleum resin thermal properties (N8),development of an analytical scheme for the determination of visiblity reducing carbonaceous aerosols ( N 9 ) ,dynamic headspace analysis of polyolefins by correlation chromatography (N10)and eval-
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uation of an apparatus to determine the permeability of coatings to carbon dioxide (Nll, N12). Several reports were issued relative to coatings flammability, with blowin agents W 3 ) ,flame propagation thro h organic vapors (1$14),the effect of coatings on the f l a " 3 i l i t y of engineeringplastics (N15),the use of oxygen index for screening fire retardant fillers (N16), and the examination of smoke suppressant agents (Nl7)receiving special attention.
MISCELLANEOUS MEASUREMENTS (INCLUDING PHYSICAL TESTS) Characterization of physical properties continues, with general apers on the testing of coatings for concrete (Ol), the stu& of coated sphere suspension theory through light scattering (02),and the influence of surfactants on the viscoelastic behavior of zwitterionic solutions (03).Studies of coating rheology continue,with coating flow (04,051,paint thixotropy (061,and architecturalpaint sagging (07) receiving special attention. Rheometric characterization of polymer systems included publications documenting the examination of epoxy curing (081, sheet molding compounds (091, and energy-impulse nondestructive testing of coatings (010). Special publications of interest during this period were a review of polymer flammability and fireproofing (0111laser , diffraction for characterizing smoke formed during polymer degradation (0121,dynamic surface tension measurements for the characterization of surfactant solutions (0131,coating adhesion testing (014-017),surfacetribology and lubrication (OB), and Taber abrasionof anodicoxidation coatings (019). Two recent books appeared concerning the measurement of polymer physical properties (020,021)as well as a book onmeasuring polymer impact fracture (022).Specificstudies of polymer and coating physical roperties include the examination of pull-off tests (023, 241,ramp.ed stram for a better understanding of polymer stress-stram ro erties (0251and , the use of a vibrating reed to measure t e oungs modulus of thin films (026). Thermomechanical analysis of coatings was the subject of a thorough review (027),as was the examinationof structureproperty relationships of thermoset coatings (028) and the characterization of artificially weathered acrylic clear coats with and without stabilizers (029). Specific dynamic mechanical studies of interest include the examination of butadiene styrene latex films (030),phenolic resin curing (0311, cross-linkedpolyesters (032,033), siliconecopolymers (034), poly(ether sulfones) (0351, and the elation of UVcurable urethanes (0361,polyurethanes ( 37, 0381, and epoxies (03s042).
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ANALYTICAL CHEMISTRY, VOL. 65, NO. 12, JUNE 15, 1993
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