Anel. Chem. 1991, 63,87R-99R
Coatings Dennis G. Anderson* 123 N . Forrest, Arlington Heights, Illinois 60004
A. INTRODUCTION This review covers analytical techniques applicable to the examination of coatings and coatings of raw materials, substrates upon which coatings are placed, etc., since the last review in 1989 ( A I ) . The contents are divided into 16 analytical techniques useful in coatings characterization. Readers are advised 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 specific areas are infrared spectroecopy, gas chroma aphy, nuclear magnetic resonance s ectroscopy, thermal an ysis, and high performance li uid c!romat$aphy. New or unique applications for establised analytica techniques appear throu hout this review. General books and reviews on tke analysis of pol appeared (A2, A3), as have papers dealin with ans;: methods to verify the composition of f o o t contact plastics (A4),methods to automate the testing of coatings (A5),diagnostic testing to improve electrostatic powder coatings (A6, A7), the characterization of phosphate conversion coatin s (A@,testing of biocide efficacy in liquid coatings (A9-AI17 testing the adhesion of slimea to silicone marine coat’~ ( A 1 2 ) : and a laboratory investigation of concrete sealers A13).
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B. CHEMICAL AND ELECTROCHEMICAL SECTION Several review articles of interest have a peared relative
to the use of aromatic nitro compounds ( E l f d e extraction methods (E2),and electrochemical methods (B37 for polymer analysis. The s cial problems involved with the hydrolysis of polyester p o h e r s was also studied (E4, E5), as was the measurement of free formaldehyde (E6)in a variety of coating systems. Titrimetric procedures remain popular, with studies related to the determination of nonionic surfactants (E7), fluorine in organic com ounds (Et?), acid value in polymeric systems (E9-E11), hyt8oxyl groups (E12, E13), and epoxy functionality (E141 receiving s ecial attention. Work continues relative to tEe role of chloride ion in corrosion phenomena, with one report on the measurement of chloride in coating blisters (E15) and two papers on measurement at the coating substrate interface (E16,El 7). An extensive review was pu lished on improvements to methodology for the evaluation of polymer nonvolatile content (B18). Several references were also noted relative to the use of polarographic techniques for characterizing coatings, including the determination of nonionic surfactants (E19),fatty acids (EN),e xy resins (E21),and styrene in unsaturated polyester resins ( E 2 ) .
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C. GAS CHROMATOGRAPHY The use of gas chromato aphy for the analysis of volatile5 in coatings continues, wit several general review articles (CI-C3) and more s ecific studies related to the evaporation of solvents from pobmer films (C4),the use of deactivated capillary columns for solvent analysis (C5),and the use of a pro ammed temperature vaporization zone ((26). More tragional uses for gas chromatography continue, with reports on the measurement of solvent components (C7),water in rubber (CS),and the identification of volatile species in phenolic polymers ((29). Two studies of special interest involved the determination of alkyl tin antifouling com ounds as they leached into seawater (C10, C I 1 ) . A new pogmeric pentafluorobenzylating agent was also reported for the gas
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*Current addreea: Witco Corp., 6200 W. 51et St, Chicago, IL 60638. 0003-2700/91/0363-87R~O9.5OlO
chromatographic analysis of inorganic anions (C12). The measurement of residual monomers in polymer systems continues, with reports dealing with measurements in polymer emulsions (C13), glycidyl methacrylate (C14), polyst ene (C15), low molecular weight monomeric epoxides (??IS), ethylene oxide (Cl7),monomeric isocyanates (CIS),amine light stabilizers (C19),and volatile species in vegetable oils and fats ((220423). Chemical degradation rior to gas chromato aphic analysis remains popular, wit reports on assaying &arboxylic acids in silicone- lyester resins (C24), acrylate species in acrylic polymers ( 25), monomeric components in olyamides (C26),and allophonates and biuretes in polyuretRanes ( ~ 2 7 ) . Renewed interest in evolved as analysis has rompted a large general study (C28) as we 1 as several stu ies specific to the coatings industry (C2SC31). Other papers of interest in this area include the generation of aromas from foods (C32), casein containing building materials (C33),paint vapors (C34), polyolefins (C35),and monomers in olystyrene (C36) and during the oxidation of vegetable oils (&7, C38). Basic studies have used as chromatography to assess vapor mobility in polymers (839, C40), solubility arameters (C41-C43), the polarity of nonionic surfactants 6441, and phase separation in polymer blends (C45). Thermal d adation continues as an active area of research, including s t x e s on coatin vehicles (C46),polymer degradation mechanisms (C47, 848),a library of pyrolysis-gas chromatographicdata (C49),and element, functional group, and mass specific detection techniques ( G O , C51). Among the specific pol er types studies via pyrolytic techni ues were acrylates E 2 - C 5 4 ) , amides (C55), vinyls (C56, 257), and ethers (C58). Inverse gas chromatographic studies have grown considerably since the last review, with papers concerning the thermodynamics of polymer blends (C59-C62), solvent diffusion in polymer-solvent systems (C63-C65), interaction parameters relative to the classical lattice model (C66, C67), in polymer blends (C68), vapor absorption on “%YC69) and fillers (C70),epoxy resin curing (C71), ancoly(methy1 methacrylate) characterization (C72). A newer technique suitable for the examination of oligomeric and polymeric materials is supercritical fluid chromatography. Although no studies specific to the coatings industry were found, selected studies of interest include the examination of ethoxylated nonionic surfactants (C73-C77), the use of adient elution techniques (C78),the se aration of phenofformaldehyde prepolymers (C79),and Betermination of monomeric isocyanates in polyurethanes (C80-C82), trilycerides (C83), and UV stabilizers from plastics (C84). bupercritical fluid extraction is growing considerably in popularity with two general review articles appearing recently (C85, C86). Combining the separating power of gas chromatography with the qualitative and quantitative analysis capability of the mass spectrometer makes an analytical tool of great magnitude. Review articles relative to the examination of polymers (C87)and fast atom bombardment (C88)continue, as do papers dealing with sequence analysis in condensation polymers (C89),arson residues (C90),and organic emissions from buildings (C91-C93). Specific studies of interest include the examination of olyglycols (C94),fire retardant and intumescent paints (895),and thermoplastic polymers (C96). The general problems associated with the examination of polymer degradation mechanisms also received special attention (C97, C98),as did the degradation of specific polymer types, such as silicones (C99),urethanes (CIOO),polystyrene (C101,C102),nonionic surfactants (C103,CI04),and polyester based materials (C105-C107).
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0 1991 American Chemical Society
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D. GEL PERMEATION CHROMATOGRAPHY Several review articles have appeared relative to the use of gel permeation or steric exclusion chromato a hy for the examination of polymers and coatings (D1-53f Studies continue relative to obtaining a more thorough understanding of the separation mechanisms operating during el permeation chromato a hy, including papers on numeric optimization methods 6 4 f obtaining universal calibration curves (05,D6), calculating polymer dispersit (D7), and factors influencing peak shape and dispersion (38-DI1). Utilization of viscometric detectors in size exclusion chromatogra h continues as an active area of research, with apers & d n g with the calculation of viscosity aver e moEcular weights (012-015) and the measurement ofxarkHouwink constants ( 0 1 6 ) . Separations in aqueous media continue to be problematic; however, much work has been done on the characterization anionic (0181, cationic (019), and of electrob es (017), nonionic ( 20-023) polymers. Among the specific 01 er t s studies in organic media were polystyrene ( D B f $& 0 2 6 ) , ac lics (027, 0281, epoxies (029), urethanes (030),UV stabxzers (031),cellulosics (032-0341, silicones (035-038polyamides ), ( 0 3 W l 4 1 ) ,and phenolics (042-044).
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E. HIGH PERFORMANCE LIQUID AND THIN LAYER CHROMATOGRAPHY Excellent studies were reported concerning applications of ion chromatographyin corrosion inhibition studies (El),the ap lication of an eva orative light scattering detector in PO ymer analyses (E2fl the use of macro orous polymeric stationary phases in high performance liquii chromatography (E3), multidimensional ap roaches to microcolumn liquid chromatography (E4),and &e use of hi h performance liquid chromatography to estimate the solubibty parameters of impurities in polymer additives (E5). The detection of monomeric species in complex sample matrices remains as an important ap lication of high performance liquid chromatography, witgstudies re orting the determination of benzil in air as an indicator o emissions from polyester powder coatings (E6),the measurement of dicyandiamide in epoxy paints (E7),the examination of low molecular weight epoxy compounds (E8-E10), and the determination of organotin compounds in air ( E l l ) . The evaluation of fatty acids (E12-E14),fatty amides (E15),and monomeric acrylates (E16, E1 7)received special attention, aa did the examination of side reactions during the formation of polyurethanes (818, E19), the detection of monomeric diisocyanates (E20, E21), the measurement of alkylbenzene sulfonates in aqueous environmental matrices (E22, E23), and the characterization of PO* er additives (E24, E25) and antioxidants (E26, E27). e separation of oligomeric species in nonionic surfactants continues to a pear in the literature with great frequency (E28-E34), the determination of hydrophile-lipophile balance (HLB](E35, E36). Some studies of interest also appeared relative to the separation of cationic (837) and anionic (E38, E39) surfactants. Among the other polymeric se arations reported were the examination of acrylates (%O-E&), acrylonitrile/st ene polymers (E&), polystyrene (E47), and epoxy resins (&). References to the use of thin layer chromatography for the examination of coatings and polymers were few in number during this eriod. Among the applications noted were the analysis of fndian stam pad inks (E49),the separation of Surfactants ( E a ,E51),$e determination of free polyethylene glycol in nonionic surfactants (E52), the separation of fatty acid dimers (E531,the study of long chain phenols (E54),and the distribution of monomeric species in styrene containing copolymers (E55, E56).
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F. ATOMIC ABSORPTION AND PLASMA EMISSION SPECTROSCOPY Relatively few references were found relative to the use of atomic absorption or plasma emission spectroscopy for the examination of polymers and coatings. Among the papers of interest noted were an excellent atomic spectroscopy update (FI),the determination of anionic surfactants as their 1,lOphenanthroline copper(I1) complexes (F2),several methods for the determination of total and soluble lead in aints (F3-F6), the analysis of polyvinyl chloride for metal& im88R
ANALYTICAL CHEMISTRY, VOL. 63, NO. 12, JUNE 15, 1991
purities (F7,F8),and the detection of tributyltin antifoulants in shell fish (F9)and in coastal waters (F10).
G. INFRARED SPECTROSCOPY The use of infrared spectroscopy continues as an im rtant analytical tool for the characterization of coatin s. gveral excellent general review articles appeared (GI- 4), as well as two revlews dealing with coatings (C5, G6) and the use of Raman spectroscopy for the examination of lymers (C7-C9). Photoacoustic Fourier transform infrare spectroscopy for coatings analysis also received special attention (GIO, G11) as did the examination of core-shell lattices (G12),evolved gas analysis (G13),the use of diffuse reflectance (C14),and the determination of two dimensional cryatal structures (C15). Improvements in dealing with data from infrared s ectral measurements continues, with studies on the use o curve analysis to analyze overlapping bands (CIG-GIS), a critical comparison of solid sample re aration techniques (G19),an improved sample holder ( 8 2 0 f and special problems associated with the examination of black solid samples (G21). been given to the general use of infrared oscopy to the exammation of f i i (G22), and the rheological properties of materials (C26-GB). Microsampling techniques continue to be refined ((229G31),with special emphasis given to the use of infrared microsco es for the examination of small articles and defects (C32-936). Diffuse and specular relectance accessories continue to be developed (G37, C38),with special studies of note related to the examination of road markings (G39), polymer contaminants (G40),single crystals (C41),polymer microstructures (G42),polymer blends (G43),and minerals (G44). Reflection infrared spectrosco y was reportedly wed to examine historical varnishes (CGf UV curable coatings on plastic substrates (G46), and epoxy glues (G47). Procedyree have aleo appeared for the determination of hydroxyl groups in polyether carbonates (G48, G49) and to determine eth 1 groups in polyethylene (G50). Additional applications incluJe the characterization of lubricants ( C S l ) ,polymer additives (G52),and aliphatic carboxylic acids (G53)and a comparison of polymer spectra obtained using transmission, s ecular reflectance, and attenuated total reflectance (C547, acrylate polymers (G55-G57), silicone coating weights (C58), polyurethanes (G59),rubber (G60-G63), water soluble polymers (G64), and lecithin (G65). Physical property measurements via Fourier transform infrared spectroscopy continue, with specific studies of latices (G66-GSS), solvent absorption into acrylates (G69-G71), functional group imaging (G72),polymerpolymer miscibility (G73, G74),hydrogen bonding (C75), and acid-base interactions (G76). The use of Fourier transform infrared s ectroscopy for studying the kinetics of chemical reactions hafled to extensive studies related to radiation curing processes ( C 7 7 4 8 3 ) . In addition, pers were published on studies concerning hydroxy acrylate Esepoxides (G84), alkyd resins (C85-G87), polyester/styrene systems (G88-C90), polyester/melamine enamels (C91), polyurethanes (G92-G95), vinyl pol erization ((396,G97), olyimides (G98-G103), siloxanes ( G 4 , G105), polyamides pG106), and epoxies (G107-G111). Reports continue relative to the interaction of polymeric coatin s on metallic substrates (G112-G122), painted wood (&23), phosphate coatings on iron (G124), and ionomers (G125). Means for examining coating durability remain an important field of study throughout the coatings indust Fourier transform infrared spectroscopy provides an excegnt mechanism to studyin weathering phenomena (G126-G129), coating inte rity (8130),photostabilization and photode acurable coatings (G131-G135), and sur ace dation for defects in a wide variety of coating systems (C136-13140). The effects of thermal degradation were also studied via infrared spectroscopy (G141-G143), as were the products of pyrolysis from vinyl lymers (13144, G145) and polyurethanes (15146) and the e f g t s of exposure to gases, such as sulfur dioxide (C147), water (G148, G149), and hydrocarbons (G150).
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H. NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY Several excellent general review articles relative to the use of nuclear magnetic resonance (NMR)spectroscopy to char-
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coatings industry on the USB of anatytical chemistry for problem sohrlng. Prbr to this, he was employed for 24 years by DeSoto, Inc., where he was involved in the anatysls and charactefizatbn of p o t y ” and coatings using chemical and instrumental techniques. He received B.S. and M.S. degrees in chemistry from Roosevelt University, where he k also a faculty member. Mr. Anderson has authored or coauthored 29 wblC cations and Is coauthor of AR FTIR A& fur the Cof??/ngsIndustty, to be published shortly. He is also the rectpient of three Roon Foundation awards for distlnguished service to the coatings industry.
acterize polymer systems have appeared (HI, H2),as has a review on the use of nuclear magnetic resonance for coatings analysis (H3). Other helpful articles of general interest to the spectroscopistusing NMR techni ues involve applications to cross-linked polymer systems ( H a and the determination of polymer structure using carbon-13 (H5, H6) and fluorine-19 (H7) magnetic resonance. Two dimensional nuclear magnetic resonance studies appeared with much greater frequency (H8-H11), as did papers on the effects of radiation on polymers (HI2) NMR imaging (HI3,HI4), use of nuclear magnetic resonance to determine pore structure in paper coatings (HI5, H16), the effects of shear on pol er fluids ( H I 7 ) , polyester-solvent interactions (HI8),s o c n t diffusion and drying of coatings (H19),and the determination of microstructure and stereochemical configuration in polymers (H20). Papers dealing with the examination of specific polymer types included the study of acrylated polyols (H21, H22), acrylic acid oligomers (H23),polyacrylates (H24-H30), and organotin containin acrylic polymers (H31). Of special interest were studies fealing with the relative reactivity of the i s y p a t e groups in isophorone diisocyanate (H32),carbon-13 stu ies in model urethane elastomers (H33),and the characterization of phenolic ( H a ,H35), silicone ( H S H 3 9 ) ,vinyl (H40-H44), polyester (H45-H47), and polyether (H48-H50) polymers. Curing mechanisms also have been studied extensively using nuclear magnetic resonance spectroscopic techniques, including drying mechanisms in coatings (H51),the reaction of diisocyanates with polyols (H52),the curing of epoxy resins (H53-H57), phenol-formaldehyde condensation reactions (H58-H62), cross-linking in silicone containing coatings (H63-H65), rubber modified lyester resins (H66),residual unsaturation during cure of ðac lates (H67),the fate the of organotin stabilizersduring thermal ggradation (H68), role of phosphites in polyester blends (H69), and the fire retardance afforded by diammonium pyrophosphate-pentaerythritol in protective coatings for polypropylene (H70).
I. SURFACE ANALYSIS The ultimate performance of a coating in protecting a substrate can, in many cases, be directly linked to the characteristics of the substrate upon which it is placed. During this period, several excellent review articles appeared (11-14), along with standard definitions of terms relating to surface analysis (E),reference materials for surface analysis (16),and special problems associated with the quantitative analysis of surfaces (17, 18). Specific studies related to coatings and polymers include the examination of interfacial chemistry in organic coatings (19),glass and ceramic surfaces and coatings (IIO),the characterization of minerals ( I l l ) , and adhesion phenomena (112). A standard reference material for depth profile has been developed (113),as have procedures for the determination of element distribution in multiphase polymers (114), inorganic elements in paint (115), scanning electrochemical microscopy (116), reflection electron energy loss spectroscopy (117), reflection high-energy electron diffraction [RHEED] (118,119),laser ionization for surface analysis (120), positron annihilation s ectroscopy (121),and ion scattering spectrometry (122,123f X-ray photoelectron spectrosco y [XPS]or electron spectroscopy for chemical analysis [ESEA] remain popular for the examination of organic coatings (124-126),conversion coatings on aluminum (127),titanium dioxide pigments (I%), polymer
latices (129), coalesced acrylic latex films (130), and the printability of surface treated polyethylene (131). Auger electron spectrampy has continued to develop, with published reports on a standard practice for elemental identification (132), standard reference spectra for Auger electron spectroscopy (133), and the influence of diffraction effects on quantitative measurements (134-137). A fracture technique for examining zinc/steel interfaces (138)was recently reported, as was the quantitative analysis of adsorbed hydrocarbons and oxygen on solid surfaces (139). Quantitative aspects of secondary ion mass spectroscopy [SIMS] were reviewed in detail (140,141),as were the errors associated with depth profiling experiments (142,143). The specific problems of high resolution ion probe imaging were discussed in detail (144),as was the study of specific pol types including: polyurethanes (145-147), silicones polystyrene (149, 150), polycarbonates (151), and poly(h droxyalkyl methacrylates) before and after chemical mo& fication (152).
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J. ULTRAVIOLET-VISIBLE SPECTROSCOPY The use of visible and ultraviolet spectroscopy to measure functional group content continues, with studies on the determination of carbonyl content in peroxide-containing oils (JI),the use of 4,4’-dimethoxytrityl chloride to assay amino groups (JZ),and the effect of zinc and calcium ions on the strength of fluorescent pigments (J3). Other colorimetric studies of interest include the determination of nonionic surfactants through the formation of colored complexes (J4, J5), the detection of urea-formaldehyde resins (56),the study of polyamide polymerization kinetics (J7),the identification of blue pigments in paints (J8),assaying the presence of styrene in solution polymers (J9, JIO),studying urethane formation reactions (JI I), and photopolymerization reactions (J12-J15). Higher order reflectance spectrometry was used to study synthetic organic pigments in artists’ paints (JIS),matching colors of metallic paints (J17),assaying the luster of mat finish coatings (J18),and measuring the gloss of automobile lacquers (JI9),black paints (JZO),and metallic topcoats (J21). Cure studies utilizing ultraviolet spectroscopy included the investigation of polyimides (522) and mixtures of naphthalene containing polymers and polyacrylates (J23). The use of chemiluminescence to characterize polymeric materials was reviewed (524) as was the use of UV light scavengers for automotive lacquers (J25). Opacity measurements remain critical in the coatings industry, with recent reviews of igment coating theory (J26),light scattering by titanium dioxife (J27), swelling and dissolution of latex dispersions (J28),the determination of critical micelle concentration (J29), photoyellowing in radiation curable materials (530,531),and the alkaline coloration of acrylonitrile-styrene copolymers (532).
K. SPECTROSCOPY-MISCELLANEOUS TECHNIQUES Translational diffusion in polystyrene solutions was examined by using photon correlation spectroscopy (KI), as were interactions between a nonionic surfactant and a benzenewater mixture (K2),particle interactions in a dispersion (K3), and amorphous regions in polymers when studied near their glass transition temperature (K4). On line coating weight along with the measurements were reported using rays (K5), use of inelastic tunneling spectroscopy to evaluate surfaces (K6),high frequency Lamb waves to study epoxy/phenolic Rutherford back scattering to excoating uniformity (K7), amine the location of lattice impurities in solids (K8),and low energy electron diffraction in surface crystallography (K9). Pressure tunneling spectroscopy was reported for the study of molecular interactions in condensed phases (KIO),as was ultrasonic microscopy to examine coating/substrate bonding ( K I I ) and positron annihilation spectroscopy to investigate pigment dispersion (K12). Electron spin resonance continues as a useful analytical technique to examine coatings, with general reviews of application areas (K13, KI4), the examination of polymer photodegradation (K15, KI6), the examination of the nature of free radicals formed during plasma irradiation (KI7),the diffusion of oxygen into polymers (K18), curing reactions of bismaleimides (K19,K20), and the fading of azo pigment/titanium dioxide mixtures (K21).Finally, Moessbauer spectroscopicstudies have been reported for the ANALYTICAL CHEMISTRY, VOL. 63, NO. 12, JUNE 15, 1991
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study of corrosion on steel substrates (K22-K24) and the degradation of triphenyltin biocides in neoprene-based elastomeric marine antifouling coatings (K25).
L. MICROSCOPY AND X-RAY TECHNIQUES Several newer microscopic techniques have been a plied to the study of organic coatings durin this period, inc uding time resolved acoustic microscopy fluorescence microscopy (L2),a general review on microscopic a n a l r (L3), atom-probe field ion microscopy (L4),electron pro e microanalysis (L5),and scanning tunnelin microscopy (L6,L7). Scanning electron microecopy, with i t s b h magnlfcation and large depth of field, continues to find wde application, particularly for the examination of latex paint infusion into hardwoods (L8),the cryogenic examination of wet coating microstructures (L9),the examination of submicron particles in air and water (LlO), and the study of sucrose fatty acid vesicles ( L I I ) . S ecial studies relative to solid surface characterization (I ! 121, the evaluation of pipeline coatin morphology and performance (L13),the replacement of re lead and m c chromate as corrceion *biting pigments (L14), the examination of chromate conversion coatings (L15),element-specific electron microsco y (L16), the detection of fibrous contaminants in paint fi ms (Ll7),the examination of powder coatings. (L18), ablative antifoulin paints (L19), wear resistant coatings (L20),alkyd surfaces %2l, L22), and zinc rich paints (L23) also appeared since the last review. In addition, several interesting publications have been found using transmission electron microscopy for the examination of coatings, includin the preparation of thin polymeric films (L24),the im ‘n o! surfaces using element s cific electron microscopy ( 25 , the study of large emuEon particles (L26-L28), the investigation of aluminum corrosion beneath organic coatings (L29), and the study of water permeation into epoxy com osites (L30). X-ray dikraction techniques continue as a primary method to examine elemental com ition and distribution throughout coating films, with specifp“ IC studies reportin the use of green copper pigments in old Russian frescoes &31), the examination of crystallinity in poly(amide imides) (L32),and the study of alkyd and ester um resins (L33),ionomers (L34), paint films on rusted sutstrates (L35), and hydrated zinc hosphate incorporated in a paint film (L36). X-ray iuorescence studies reported recently include total reflection techniques for surface analysis (L37-L39), grazing incidence the determination of coating film weight measurements (UO), (L41, L42),and the detection of trace elements in paints and pigments (L43, ,544).
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M. THERMAL ANALYSIS The thermoanalytical technqiues discussed in this section include differential thermal analysis, differential scanning calorimetry, thermo ravimetric analysis, and flammability testing. Several excefient review articles have appeared in the past 2 years (Ml-M4), alon with specific reviews on scanning microcalorimeter history ( h 5 ) ,thermodynamic interactions in mixtures (M6),and combined thermogravimetry-differential scanning calorimet (M7). Specific studies related to coatings include the preyiction of dispersion stability for pigment paste/paint base mixtures (M8),pi ent interactions during dispersion in organic solvents (M9rand the investigation of bindin media in paints usin differential thermal analysis ( M I O ) h. e r m o a n a lytical stusies continue relative to the determination of co olymer composition via thermogravimetry ( M l 1 , M12), tge measurement of carbon black content in rubber (M13),the evaluation of smoke (M14)and wire and cable performance (M15) using a heat release calorimeter, and the investigation of surfactants as stabilizers during the degradation of poly(viny1 chloride) ( y 1 6 ) . The measurement of polymer and coatin physical properties continues as a major use for thermal an&& techniques. Studies continue on the evaluation of glass transition temperatures in eneral (M17-M20) along with specific examination of acry!ics (M21,M22), polystyrene (M23),chlorinated rubber containing paints (M24),polyolefins ( M B ) ,epoxides (M26),and polyamides (M27). A new apparatus was recently described which improved the measurement of polymer thermal conductivity ( M a ) ,as well as the determination of flammabilit in composite materials (M29). Ra id measurement oTpigment content from ink density an volume
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fraction was reported (MM),as was the use of thermal analysis to evaluate the storage stability of radiation curable coatings (M31). Other polymer types of interest studied were epoxy acrylate adhesives (M32), acrylic latex copolymers (M351, polyolefuls (M36),polyurethanes (M37,M B ) ,polyesters (M39, M40). and the evaluation of cross-linking as flame - agents reGdents (M41). Polvmerization reactions are also a fruitful area of study. particdarly relative to the characterization of ed aint f h (M42), acrylate photopol erization ( M 4 3 3 4 5 1 acrylate thermal polymerization g 4 6 - M 4 9 ) , amine cured epoxies (M50-M51), isocyanate cured epoxy resins (M52),phenolic baaed polymers (M53),urethanes (M54),polyimides (M55), and the quality evaluation of fats and oils (M56). Cure characterization studies continue, with several specifically dealing with coatings systems (M57,M58). Other studies of note include the use of an accelerating rate calorimeter to study decomposition kinetics (M59),curing an alk d-melamine resin system (M60),enthalpy relaxation in cured epoxy coatings (M61),and activation ener measurements during the formation of urethane linkagesyM2, M63). Finally, unsaturated polyester resin curing (M64-M70) and a comparison of microwave vs thermal energy curing for a sulfone/epoxy resin system (M71), e oxy amine mixtures (M72-M75), phenolic cured epoxies rM7LM78) and mercaptan cured epoxy resins (M79,M80)were recently reported.
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N. ENVIRONMENTAL AND INDUSTRIAL HYGIENE Concerns with meeting environmental regulations continue, with test methods reported to evaluate leaks from new stationary sources ( N I ) ,establishing a protocol to determine volatile compound emissions from automobile and light duty truck topcoat o rations (N2). Concerns over proper sam ling prompted s t u g s using in situ extraction and analysis &3), field sampling for volatile5 at residential sites (N4),sorting volatile organics into source related groups (N5),evaluating organic s ecies in indoor air (N6-N9), and the examination of grounxwater samples for volatile organic compounds (NIO, M I ) . Evaluation of the Toxic Characteristics Leaching Procedure [TCLP] was completed (N12),as were the examination of coating components as indirect food additives (N13), l,4-dicyanobenzene as an occupational marker compound for the thermal degradation of polyester powder coatings (N14), and new methods to determine alkyltin antifoulants in water (N15) and marine sediments (N16).
0. MISCELLANEOUS TECHNIQUES Several interesting papers were published since the last review on rendering polymeric materials fire retardant (01041, polymer flammability-structure relationships ( 0 5 ) ,the use of critical oxygen index to measure flammabhty (06,07), and the develo ment of a classification system for combustion modified flexibe polyurethane foams (08). Accelerated aging continues as a necessary evaluation method for paints and coatings. Comparisons of accelerated and natural aging tests continue (09, OlO),with specialstudies reported concernin melamine cured acrylic clearcoats (011), alkyd coatings (0127,the examination of color fastneas toward light and weather (0131, weathe% of titanium dioxide (0141, the effect of sulfur dioxide on painted steel surfaces (0151, and the evaluation of a “biomer aint” (016). Further examination of methololo to evaluate particle to several excellent size and particle size distribution has review articles (017, OM),as well as pa ers on the dynamics of light scattering from latex particles (&9-022), particle size measurement in concentrated latex sus ensions using fiber optic photon correlation spectroscopy ( 23), the use of zero angle depolarized light scattering in studying titanium dioxide (024),the use of small angle neutron scattering (Os), and the examination of high s eed dielectric spectroscopy (026). The fractionation of l a t e x - h adhesives and paints received special attention (027), as did article size measurements using a disk centrifuge (028, &9), the evaluation of new hydrodynamic chromatographic techniques (030-034), size exclusion chromatographyto evaluate particle size distribution (035), and field flow fractionation techniques for particle characterization (036-042). The corrmion protection afforded by coatings is continually under evaluation, with papers dealing with the quality as-
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surance of anticorrosive coatings (0431, a general review of corrosion testing methods (044-043, the unique problems associated with the measurement of film thickness for corrosion resistant coatings (OB),the effects of atmospheric salta on corrosion protection (049,050), donor-acceptor properties of solid surfaces (051)and the development of paints with high barrier effects (052). The use of electrochemical impedance measurementa remains the primary tool to redict the corrosion protection afforded by organic coatings. burin this period, several general review articles have appeare! (053-059) as well as studies of the detection of coatin degradation in various atmospheres usin an electrochemic3 monitor (060)and the evaluation of a pEosphate coating on steel (061). The study of nontoxic pigments in anticorrosive primers (062-064), cathodic protection of zinc-rich paints (065), the prediction of long term durability of coated metal containers (066-069), the examination of coated metal panels (070-072), monitoring coating degradation during atmospheric or vapor phase exposure (073), the statistical analysis of coating degradation over time (0741, and the examination of electrochemical noise generated by a zinc-rich paint on mild steel (075) all received special attention.
P. MISCELLANEOUS MEASUREMENTS (INCLUDING PHYSICAL TESTS) Characterization of the physical properties of polymers and coatin s continues, with reviews on nondestructive testing procecfures (PI-P5), the utilization of ultrasonic and eddyInfinitesimal Module Determicurrent measurements (P6), nation (P7),thermal pulse video thermography (I%), radiation transmission measurements (P9), and the use of the Comrehensive Abrasion Tester to simulate rub problems (P10). tudies related to scratch testing continue (P11, P12) as does the examination of coatingaubstrate adhesion (P13-P16), the effects of polymer surface modification on adhesion (PI7),the and the measurement of delamination surface energy (P18), effects of alkox ilane monomers on adhesion to glass (P19), anrpolymer films (P21). The blister testing was steel (RO), also used to evaluate the adhesion of thin films (P22), as was stress analysis (P23) and adhesive bond stren h and durability studies (P24). The development of new ardness tests conhues (PW, P26)as does the use of acoustic emission (P27), mechanical strength (PB), toughness (P29, P30), and ultrasonic (P31,P32) measurements. Mechanical film property measurements continue to be used extensive1 to characterize polymers and coatings, with studies highligiting the measurement of Young's modulus (P33, PM),the characterization of pressure sensitive acrylic the examination of radiation curable coatings adhesives (P35), (P36), the bonding strength of lacquered wood (P33, and the study of polyurethane foams (P38).Paint rheology continues to be studied in detail, including controlled stress measurementa (P39, P40),rheological characterization of paints during film formation (P41), interpreting flow curves of pigmented paper coatings (P42), acrylic coatings (P43,Pa),poly(acry1ic acid) thickeners (P45), problems associated with the measurement of viscosity at low shear rate (P46), and a fresh look at the relationship between polymer molecular weight and solution viscosity (P47). The utilization of thermomechanical measurements continues to row as the potential of this technique is better realized. o,!n the studies of interest were several general review articles (548,P49), the assessment of cure (P50-P53) and chemical heterogeneity in emulsion co olymers (P54). Among the specific polymer types studie in detail were acrylics (P55-P58), melamine-polyol inter enetrating netpolyworks (P59), linseed oil based coatings (g60, HI), urethanes (P62, P63), epoxy based systems (P64-P68), polysulfones (P69), and elastomers (P70).Ceramic coatings were also exhaustively examined (P71) as were structure- roperty relationships in coatin s (P72, P73) and the use of $electric (P74-P78), ultrasonic ( h 9 ) , and Fourier transform mechanical analysis measurements (P80)to characterize a wide variety of polymer and coating types.
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ACKNOWLEDGMENT I acknowledge Chemical Abstracts Service for providin acceea to STN International to aid in the literature search me8 in the preparation of this work.
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E. n1dn PLRFOAMAW LIQUID AND THIN LAYER CHROMAmApHY (€1) Andrew, B. E., Cones, Conf. Ssr., NACE-7 (Ceros. Inhlb.), 185-92 (1988). (€2) S C h h , R.; EWbherdt, H., chrometmphb, 29 (11-12), 517-22 (1990). (€3) pktrzyk, D. J., chem.Anal. (N.Y.). 98 (Hlgh Perform. Uq. Chromatog.), 223-78 (1989). (€4) Cartes, H. J.; Jewett, G. L.: Pfelffer, C. D.; Martin, S.; Smtth, C., Anal. them., 61 (9), 981-5 (1989). (€5) Srmnhraclen, K., J . Llq. chrometogr., 13 (2), 383-90 (1990). (€8) PukkHa, J.; Kokotti, H.; Peltonen, K., J . Chrometog., 479 (2). 389-78 (1989). (€7) Pukklla, J.; Peltonen, K., J . Llq. Chrometog., 13 (2). 409-14 (1990). (€8) Vaqwz, A.; Mateka. L,; Spacek. P.; Dusek, K., J . pdym. Scl., Part A : Pdym. chsm.,28 (9), 2305-19 (1990). (€9) Domeretlus, F.; WaM"r, S.; Fedtke, M.. P e m . Bull. (8ef/ln),22 (5-6), 579-84 (1989). (€10) Sreenkasan, K., J . Indlen Chem. Soc.,87 (2), 180-1 (1990). (€71) W n g , C. W.; Tsal, W. L., J . Chln. Chem. Soc. (Taipei), 38 (3). 179-88 (1989). (€12) Link, W.; Spiteller, G., Fen Wlss. Techno/., 92 (4), 135-8 (1990). (€13) Fatlcla, M. G., JAOCS. J . Am. 011Chem. Soc.. 60 (4), 572-5 (1989). (€14) Schrosder, B.; Mangels, J.; Seke. K.; Wolpers, S.; Danmcker. W., J . chrometogr.. 514 (2). 241-51 (1990). (€15) Jasperse, J. L.. JAOCS. J . Am. 011 Chem. Soc.. 65 (11). 1804-7 (1988). (€18) Neyer, J. M.; Vlgouroux. A.; Vamvakarls, C.; Mandery, H.. ChrometoBrepMe, 25 (10). 915-8 (1988). (€17) Mnd, H.; Hensel, R., Fresenlus' Z . Anal. Chem., 331 (B), 846 (1988). (€18) SpMcova, M.; Kublln, M.; Dusek, K., J. Macromd. Sei. Chem., A27 (4), 509-22 (1990). (€19) Hull, C.; Outhrle. J. L.; McKlnney, R. W.; Taylor, D. C.; Mabud, M. A.; Rescott, S. R., J . Chr4mBtogr.,477 (2). 387-95 (1989). (€20) RaStOgl, S. C., C h r o m e t ~ p / I &28 , (1-2). 15-8 (1989). (€21) Slmon, P.; Moulut, O., J . Llq. chrometogr., 11 (9-lo), 2071-89 (1988). (€22) Castles, M. A.; Moore, B. L.; Ward, S. R. Anal. Chem., 01 (22), 2534-40 (1989). (E231 anden, W. A. A.; Rlemersma, R.. Tens&, Surfactants. Deterg., 27 (l), 48-51 (1990). (€24) Fbyd. T. R. Chfomaroorephle, 25 (9), 791-6 (1988).
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(€47) Van der Beek. 0.P.; Cohen, S. M. A.; Fleer, 0. J.; Hofman. J. E., Lengmuk, 5 (5), 1180-6 (1989). (€48) Fedtke, M.; Domaratlus, F.; Pfitzmann, A., pdvm. Bdl. (m). 23 (4). 381-8 11990). (E49) Jasuia, 0. P.; Singla, A. K.; Seema, B. L., Fwenslc Scl. Int.. 42 (3), 255-62 (1989). (E50) kt" G., seilen, oele, Fette, Wachse, 116 (7), 273-80 (1990). (€51) Saky, P.; Farkas, L.; Rusznak, I.. Acta Chlm. Hung., 127 (l), 95-8 (1990). (€52) Zhang, P., RivOng Huexue Gongye (3). 138-9 (1988). (€53) Chrlstopoulou, C. N.; Perklns, E. G., JAOCS, J . Am. OIIChem. Soc. 66 (9), 1353-9 (1989). (€54) Tyman, J. H. P.; Tychopoulos, V.. J . Plenar chromatogr.-Mod. n C ,1 (31, 227-30 (1988). (E55) Yamagucchl, S.; Hhano, J.; I d a . Y.. J . Anal. Appl. pvrorL&, 18 (2), 159-84 (1989). (€58) Podesva. J.; Kratochvll. P.; Oloeckner, G., Acta Po/ym., 40 (8), 414-8 (1989). F. ATOMIC ABSORPTION AND PLASMA EMISSION SPECTROSCOPY
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ANALYTICAL CHEMISTRY, VOL. 63,NO. 12, JUNE 15, 1991
OSR
COATINGS ( H 9 ) Cardum, K. R.; Carter, R. O., 111; Cheng, M. F.; Gdovoy. A.; Van Dene, H., J . A M . polLm. Sd., 40 (5-8), 983-75 (1990). (H70) Ddobd, R.; Le Bras, M.; Quassou. N.; Decressaln, R., polLm. Depad. Stab., 30 (I), 41-58 (1990).
1. 8URFACCANALYSIS (11) Singer, P. H.. semlcond. Int., 11 (12), 59-81 (1988). (12) D., EncyC. pdLm. Scl. Eng.; Wky: New York, 1989 Vol. 18, pp 399-442. (13) TW’W, N., Anal. chem.,62 (12), 113R-25R (1990). (14) SkPOrd, A. J.; L m , E. A.; Chin, R. L., cwds Mew. Charact. chem. AM/.; SIMwa, J. P., Ed.; VCH New York, 1988; pp 187-204. (15) Anon., S I A , Swf. Interfaw Anal., 14 (8-7). 423-9 (1989). (18) POW4 C. J., Ekclrm. Mter. F ” s , Int. SAW€€ktron. Conf., fst; K&mekr, N. H.. Jr., Harper, C. A., Lee, S. M., Eds.; SAMPE: Cordova, CA, 1987; pp 252-83. (17) Rutton, M.; El (kmatl. M. M., Inst. Fhys. Conf. Ser., 93 (Eurem 88, Vd. I), 255-60 (1988). (18) Flschmelster, H. F., Fresenlus’ 2. Anal. Chem.. 332 (5), 421-32 (1988). (19) Schuetrle, D.; Carter, R. 0.. 111; De Vries, J. E.; Dickb, R. A., A&. W .Coat. Sd. Tsdmd. Ser. 11, 229-45 (1989). (110) Bach, H.. F f 0 ~ 8 n k 2. ’ Anal. chem.,333 (4-9, 373-82 (1989). (I11) Coyne, L. M.; McKeever, S. W. S., ACS Symp. Ser., 415 (Spectrosc. Charact. Miner. Their Surf.), 1-29 (1989). (112) Ferrante. J.. S I A , S u l . Interface Anal., 14 (12), 809-22 (1989). (113) Fine, J.; Navlnskl, B., S I A , Surf. Interface Anal.. 11 (lo), 542-3 (1988. (114) Centow, H. J.; Kunr, M.; Klotz, 6.; Moeller, M., M e k m l . Chem. Mecmrol. svmp., 26, 191-8 (1989). (115) Fmukawa, K., K8WkU K&tSU Ksnkyusho HokokU HokegakU Hen, 42 (I), 1-3 (1989). (118) E n ~ ~ t r o m R., C.: Pharr, C. M., Anal. Chem., 81 (19), 1099A-l100A, 1102A, 1104A (1989). (117) Wang, 2. L.. J . €&ctron. Mcrosc. ~ e c h .1 , 1 (I), 70-5 (1989). (118) Im, S., MITO AS1 Ser., 8 , 168 (ReRectkn HlgMnergy Electron M . Refkctkn Electron Imaglng Surf.), 3-28 (1988). (119) Beeby, J. L., NATO AS1 Ser., Ser. 8 , 168 (Reflection HlgMnergy Electron Dlth. RefkcWon Electron Imaging Surf.), 29-42 (1988). (120) Palllx. J. 6.; Schuhle, U.; Becker, C. H.; Huestls, D. L., Anal. Chem., 61 (e), 805-11 (1989). (121) Chena. K. L.: Jean. Y. C.: Luo. X. H.. Crtt. Rev. Anal. Chem.. 21 (3). . . 209-24 (1989). (122) Gardelle. J. A., Jr.; Plreaux, J. J., Anal. Chem., 82 (11). 845A-846A, 848A, 8SOA-858A9 858A-881A (1990). (123) T w , T. T.; Chen, C. L.: Llu, K., J. Meter. Res., 4 (a), 1549-59 I, l-9-8- -9,l . (124) Watts, J. F.. J. Ass., 31 (l), 73-85 (1989). (125) HduMca, J. W., A&. W . Coat. Scl. T & M . Ser.,10 (Int. Conf. Org. Coat. SCL T M n d . , 12Ul, 1988), 158-63 (1988). (126) Aral, T.; Tomknesu, H. K e d Pa OkyOsM, 43 (2), 213-25 (1989). (127) Crompton, J. S.; Andnws, P. R.; McAiplne, E., S I A , Surf. Interface Anal., 13 (2-3), 180-8 (1988). (128) Losd, T., J. Coat. Tsdmd., 61 (776), 57-63 (1989). (129) Lynn, R. A. P.; Davls, S.S.;Davles, M. C.; Hearn, J., Potym. Meter. Scl. Eng., 62, 889-94 (1990). (130) -0. C. L.; Dobkr, F.; Plth, T.; Holl. Y.: Lamble, M., J . C O W Interfece &/., 128 (2), 437-49 (1989). (131) Eekr, G. E.; Samuels, S. 6.; Harris, W. C., Tappi, J . , 73 (I), 145-50 (1990). (132) Anon., S I A , Surf. Inrerlece Anal.. 14 (6-7), 419-20 (1989). (133) Sm)th, G. C.; %ah, M. P.. S I A , Surf. Interface Anal., 16 (1-12), 144-8 (1990). (134) Blshop, H. E., SIA Surf. Interface Anal., 18 (1-12), 118-28 (1990). (135) Seah, M. P.; Smlh, G. C., S I A , Surf. Interface Anal., 18 (1-12), 188-72 (1990). (138) Nebesny, K. W.; Maschhoff, 6. L.; Armstrong, N. R., Anal. Chem., 61 (7), 489A-472AB 474A, 476A, 478A, 480A-481A (1989). (137) Powell, C. H.; Seah, M. P., J. v 8 C . SCi. Techno/., A , 8 (2), 735-83 (1990). (138) Eberle, W. J., S I A , Surf. Interface Anal., 15 (2), 135-8 (1990). (139) Mlllo, 0.; Many, A.; GoMsteln, Y., J. v 8 C . SCl. Technol., A , 7 (4), 2888-94 (1989). (140) (3rasserbaw, M.; Stlngeder. G.; Frledbechw, 0.; Vlrag, A,, S I A , S u l . Interface Anel., 14 (lo), 823-34 (1989). (141) Kin$”, D. R.; Rlchardson, C. H.; Walls, J. M., Res. Dev., 30 (9), 120-2, 124 (1988). (142) Hws. S. M.: Colon. R. J.. S I A , Surf. Inleftace Anal., 14 (3), 101-8 (1989). (143) Anon., S I A , Surf. Intetface Anal., 14 (8-7), 421-2 (1989). (144) LevbSettl, R.; Chabaia, J. M.; Wang, Y. L.; Hallegot, P., Microbeam Anal., 23rd, 93-101 (1988). (145) Bletsos. I.V.; i+afcules. D. M.: VanLeyen, D.; Bennlnghoven. A,; KaraRleck. J. N., Mecromokcules, 23 (le), 4157-63 (1990). katclanls, C. 0.; (148) Wtsos, 1. V.; Hercules, D. M.; VanLeyen. D.; Bennlnghoven, A.; Karakataanls, C. G.; Rleck, J. N.. Anal. Chem., 81 (lg), 2142-9 (1989). (147) Hercules, D. M., fob“. Meter. Scl. Eng., 59, 724-8 (1988). (148) Van Wj, W. J.; Mlchad. R. S.,Po&m. Mater. Scl. Eng., 59, 734-8 (1988). (149) Jones, R. A. L.; Kramar, E. J.; Rafallovlch, M. H.; Sokobv, J.; Schwartr, S. A.. Mew.Res. Soc. Symp. Roc., 153 (Interfaces Poiym., Met. Ceram.). 133-41 (1989). (150) Van Leyden. D.; Hagenhoff, 6.; Nlehuls, E.; Benninghoven, A.; Bietss, I.V.: Hercules, D. M., J. Vac. Sci. Techno/., A , 7 ( 3 , Part 2). 1790-4 (1989). (151) Lub, J.; Buning, 0. H. W. Polymer, 31 (e), 1009-17 (1990).
m,
e.
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I
@OR ANALYTICAL CHEMISTRY, VOL. 63,NO. 12, JUNE 15, 1991
(152) Lub. J.; Van der Wel, H.; Van Vroonhoven, F. C. E. M.; Bennlnghown, A., RWl. Tf8V. chhn.PeyS-68S. 109 (8), 387-74 (1990). J. ULTRAVIOLET-VISIIKE SPECTRo8copY
(J1) CMba. T.; Tokazawa, M.; Fujlmoto, K., J A W S , J. Am. Oichem. Soc., 88 ( l l ) , 1588-92 (1989). (J2) Gaur, R. K.; Sharma, P.; Gupta, K. C., Analyst (London), 114 (g), 1147-50 (1989). (J3) cook,J., f i s t . Compd., 11 (7), 38-7, 40-1 (1988). (J4) Kautzer, 6.; Laby. R. H., GITFaclu. Leb., 32 (5), 527, 529-32 (1988). (J5) Kuban, V.; Jurasova, J., Scr. Fac. Scl. Net. Unlv. Pukynknae Bnm., 18 (3-4). 159-86 (2988). (J6) Oneeve, V. I.; Besov. V. N. Zavod. Lab., 54 (lo), 28-7 (1988). (J7) Yw, J. K.; Sung,C. S. P.. pd)lm. Meter. Scl. Ew.,60, 429-33 (1989). (J8) Wakeford. C. M.; Wardman. R. H., J. Oll cdow Chem. Assoc.. 72 (11, .. 22-8, 34 (1989). (J9) Kress, A. 0.; Mathias, L. J.; Cei. G., ~ e c r m k & ~ 22, (21, 537-48 11989l. s.---,(JIO) Soares. 6. G.; Gomes, A. de S., Polym. Bull. ( W i n ) , 20 (e), 543-8 (1988). (J11) Hung. X. Y.; Yu, W.; Sung, C. S. P.; Mecromokuks, 23 (2), 390-8 (1990). (J12) Yamashlta. H.; Ito, D.; Murakami. K.: Ito. H., J. Photmobm. Scl. .~ Technci., 2 (2), 225-30 (1989). (J13) Davidson. R. S.; Lowe. C.. fw.Polym. J . , 25 (2), 159-85 (1989). (J14) Miller, R. D.; RaboR, J. F.; Soorlyakumaran, R.; Flemmlng, W.; Flckles, G. N., Report TR-14; Order No. AD-A187889 (1987). (J15) Devaux, J.; Sledz, J.; Schue, F.; oiral. L; Naarman, H., Mek“/. Chem., 10 (I), 139-46 (1990). (J16) Taisky, G.; Ristlc-SolaJlc, M., Anal. Chim. Acta, 226 (2), 293-304 (1989). ( J l i ) h k ,H.; Rappel, T., Farbe Lack, 95 (ll), 804-5 (1989). (J18) Boekmair. G., Farbe Lack, 95 (I), 13-15 (1989). (J19) BrueckmK, F., MetaWWfkeche, 44 (e), 402-4 (1990). (J20) Fernandez, R.; Seashob, R. G.; Oberle, L. 0.;Kadambl, J. R., Roc. SPIE-Int. Soc.Opt. Eng., 967 (Stray Llght Contam. Opt. Syst.), 292-305 (1989). (J21) TChhI, K.; Okuda, C.; SUZUki, S.. J. Coet. Technd., 62 (782), 43-50 (1990). (J22) Martin, P. S.; Wachsman. E. D.; Frank, C. W., Po&lm&s: Meter. Chem. *act., Roc. Int. Cont. Pc$4tnhs, 3rd; Feger, C., Khojasteh, M. M.. McOlath. J. E., Eds.; Elsevier: Amsterdam, 1989 pp 371-8. (J23) Holden. D. A.; Strauss, J., Polym. Eng. Sci., 28 (21), 1373-80. (J24) Mendenhall, G. D., Angew Chem., 102 (4), 380-91 (1990). 1 (lgth), 317-34 (J25) Avar, L.; Boehnke, H.; Hess, E., FATIFfC-K-., (1988). (J26) Slmpson, L. A., P w m . Paint cdwr J . (Feb 22). 108, 110-1, 114. 117-9 (1989). (J27) Craft. R. W., Mod. Paint C o d . , 79 (lo), 158-80 (1989). (J28) Quadrat, 0.; Mrkvlckova, L.; Jasna, E.; Snuparek, J., Cdbhl Po&m. SCi., 288 (e), 493-9 (1990). (J29) Goheen, S . C.; Matson, R. S., J A W S , J . Am. OIIChem. Scc., 66 (7). 994-7 (1989). (J30) Allen, N. S.; Lo, D.;Salim, M. S.; Jennings, P.. Po/ym. Depad. Stab., 28 (l), 105-14 (1990). (J31) A h , N. S.; Robinson, P. J.; Ciancy, R.; WhRe, N. J.. ACS Symp. Sw.. 417 (Radiat. Curing Polym. Mater.), 348-60 (1990). (J32) Kopic, M.; Beer, D., Vestn. Slov. Kem l)rus., 38 (4), 433-44 (1989). K. SPECTROSCOPY-MISCELLANEM TECHNIWES
(K1) VanCSO, G. J.; Forer. M., Mecromoh3c&s, 23 (4), 1220-2 (1990). (K2) Hwang, J. S.; Lln, C. L.; GI, H. J.; Chen, S. N., Chin. J . Fhp. (T8@3/), 27 (5), 371-8 (1989). (K3) F W . R., Part. Part. Syst. Charact., 7 (2), 74-9 (1990). (K4) Yu, T. L., Avali. Univ. Microfilms Int.; Order No. DAB917216 (1988). (K5) R W g e , W. C., Pub. Pap. Can., 90 (9), 102-4, 108-7 (1989). (K6) Brown, N. M. D., Adv. Spectrosc. (Chichester, U . K . ) , 18 (Spectrosc. Surf.).215-81 (1988). (K7) Bridge, 6.; Ramli, A., J. Meter. Sci., 25 (3), 1794-802 (1990). (K8) Pretorius, R., S.Afr. J . Fhys., 12 (I), 24c-29c (1989). (K9) Pendry, J. 6.; Helnz, K., Swf. Scl., 230 (1-3), 137-49 (1990). (K10) Drlckamer, H. G., Chemtracts: Anal. Phys. Chem., 1 (5), 271-87 (1989). (KIT) Tsukahara, Y.; Ohira, K., Ulbasonlcs, 27 (I), 3-7 (1989). (K12) Pfau, J. P.; Mayo, 6. A., Potym. Meter. Scl. Eng., 59, 273-7 (1988). (K13) Martini, G.. Colloids Surf., 45, 83-133 (1990). (K14) Sohma, J., Prog. Potym. Sei.. 14 (4), 451-596 (1989). (K15) Okamoto, S., ShklzaiKyakeiSM, 62 (7), 404-10 (1989). (K16) Bauer. D. R.; Cierlock, J. L.; Mlelewski, D. F.; Peck, M. C. P.; Carter, R. o., 111. Potym. w a d . Stab., 27 (3). 271-84 (1990). (K17) Kuzuya, M.; KoMe, A.; Ito, A.; Noguchl, A., Chem. Lett. (4), 355-8 (1989). (K18) Kaptan, Y.; Pekcen, 0.; Arka, E.; Gwen, O., J . Appl. pdym. Scl., 37 (9), 2577-85 (1989). (K19) Brown, I.M.; Sandreczkl, T. C., Potym. Meter. Sei. Eng., 59, 612-5 (1988). 2821-31 (K20) A M , H.; Takese, 1.: Noxl, T.. Mekromol. Chem., 190 (ll), (1989). (K21) Okamoto, S.; Ohya-Nishlguchl, H., Bull. Chem. Soc. Jpn., 63 (a), 2348-51 (1990). (K22) Vertes, C.; Czako-Nagy, I.; Kolonlts, M.; Tabs, E.;Suba, M.; Vertes, A., J. Radlaanal. Nucl. Chem., 144 (3), 189-94 (1990). (K23) Brooks, J. S.; Thorpe. S., Hyperfine Interact., 47-48 (1-4), 159-78 (1989). (K24) Vertex, A., Hyperfine Interact., 45 (1-4), 105-25 (1989).
COATINGS A b , D. W.; books, J. S.; Balky, S., 343-7 (1989). L.
&.
Opmonwt. m., 3 (4),
MICROSCOPY Am X-RAY TECHNIQUES
(LI) Shton, A. M.; %rlggs, G. A. D.; Twkahara. Y., Awusf. Im&, 17, 87-95 (1989). (L2) K W . D. A.. -, 38 (l), 51-9 (ISSO). (L3) W e , P. M., Anal. Chem., 82 (12), 423R-41R (1990). (L4) T W , T. T., J. h C . Scl. T s c h d . , A , 8 (4), 3397-404 (1990). (L5) WMlCh, P.; obertw, D., J . Pnp. (C5 Roc. E v . Conf. Chem. Vap. DwosMon, 7th. 1989). C5-2851C5-294 (1989). (L8) T-, J., m.-Ekcb.odnm,. Soc., 90-11 (Anal. Tech. Semlcond. Mater. Rocsss Charact.). 327-32 (1990). (L7) cmflth,J. E.; Kochanskl, G. P., Annu. Rev. Mater. Scl., 20, 219-44 ( 1990). (La) MlddktM, T. M., W w d Sd. T m . , 23 (4). 299-302 (1989). (LS) Sh@ehan,J. C.; Whakn-shew, M., TapplJ. 73 (5), 171-8 (1990). (L10) S t d , E. B., Mcrot” Anal., 23rd, 466-8 (1988). (L11) IshlMml. Y.: Machlda. H.. JAOCS. J . Am. 011 Chem. Soc..55 (4). .. . 599-603 (1989). (L12) IcMnokawa, T., Dmus. D s k t . Data, Ft. B. 5 (Appl. Electron MC WOSC Mater. Scl.), 31-57 (1989). (L13) Charkoudlan, J. C.; DOITIpSter, W. A., 111; Duputs, C. W.; Schonhorn, H., pdym. Mater. Scl. Eng., 62, 858-62 (ISSO). (LW M , P.; Mayfarth, H., Krwroskn (l)resden), 20 (l), 17-30 (1989). R15) Trevsrton, J. A,; A m , M. P., J . M a w . scl., 23 (lo), 3706-10 (1988). (L16) Kunx, M.; Helnrlch, U. R.; Moeller, M.; Cantow, H. J.. Rog. cdldd Pdym. Scl., 77 (Dispersed SySt.), 238-41 (1988). (L17) Falla. N. A. R., Fa* Le&. 94 (12), 983-4 (1988). (L18) Clarldge, M. A.; Stratton. J. L.; Watson, J. G., A&. Ckg. Coat. Scl. Techno/. Ser., 10 (Int. Conf. Org. Coat. Scl. Technd., 12th. 1986), 145-51 (1988). (Ll9) Rend. L.; Qombach, M. L.; Cintl. G., A&. Org. Coat. Scl. Techno/. Ser.. 10 (Int. Conf. Org. Coat. Scl. Technd., 12th, l986), 209-14 (1988). (L20) V-, S.; skogwno, J., Swf. W f . Techno/., Roc. I n f . Conf. Surf. Modw. Tedmol., lst, Sudershen, T. S., Bhat, D. G., Eds.; Metall. Soc.: Wansndale, PA, 1988 pp 143-68. (L21) Van C)erreshelm, W.; Van Rossum, C. A. J. L.; Cremers, J.; Van der PbW, A. F. M. J., F A T I K C - K w . , loth, 287-302 (1988). (L22) -8, N. L., R o c . - € L s c t ” . Soc.,89-13 (Roc. Symp. Adv. COrrOS. Rot. Org. a t . ) , 451-87 (1989). (L23) Morcllk, M.; Barajas, R.; Fellu, S.; Bastidas, J. M., J . Mater. Scl., 25 (5), 2441-6 (ISSO). R24) Porte, M. L.; bncwrt, J. D.; Taybr, L. T., Am. l a b . (FaM8k9, ann.), 21 ( l l ) , 92-3 (1989). (US) Kktt, S.; Von %ggem, J.; Kunz, M.; Cantow, H. J., polvm. corn".. 31 (a), 322-5 (1990). (L26) Chen, S. A.; Lee, S. T., Mekronwl. Chem.. Rapkl Commun., 11 (9). 443-50 (1990). (L27) Sl)versteR, M. S.; Talmon, Y.; Markls, M., Polymer, 30 (3), 418-24 (1989). (L28) IehhRtawa, S.; Fukutoml, T.. J . Appl. M y m . Scl., 40 (9-lo), 1547-55 (1990). (L29) Kobeyashl, K.; Shlmlzu, K.; Tsuda, Y.. Kelknzdru, 39 (6), 457-9 ( 1989). (L30) HoweW, B. F., pdym. Mater. Scl. Eng., 60, 797-800 (1989). (L31) Nawnova, M. M.; plsereva, S. A.; Nechlporenko, G. D.. stud. Conm.,3s (2), 81-8 (ISSO). (L32) H e m .S. J.; Wgenrother, P. M., J . pdvm. Scl., Part A : M y m . them., 28 (S), 2427-36 (1990). (L33) Swaw, S.; Chandre, A., Acta M y m . 40 (7), 473-5 (1989). (LW) R W , R. A.; Dlng, Y. S.; Foucart, M.; Jerome, R.; Hubbard. S. R., m n , K. 0.:Coopet, S. L., ACS Symp. Ser., 395 (Muklphase Polym.: Bbnds t o n o ” ) , 420-38 (1989). (L35) DOkbU, A,, Mater. Tech. (Pa&), 77 (1-2). 25-30 (1989). (L36) QrdnOf, P. J.; McArn, 1. W.; Barton, V.; Seydt, G. M., J . 011 Cdow ChOt??. A m . . 73 (I), 16-17, 34 (ISSO). (L37) Kn~th.J.; Schwenke, H.; Welsbrod, U., SpectrocMm. Acta, Part B , 448 (5), 477-81 (1989). (L38) Schwenke, H.; Bernelke, W.; Knoth, J.; Welsbrod, U., A&. x-R8y AM/., 32, 105-14 (1989). (L39) Lengeler, B., Feslkoerperproblme, 29, 53-73 (1989). (L40) Brunel, M.; ales,B., J . Pnp.,colyoq. (C7, X-Ray Neutron Scatterlng Suf. Thh FHms), C7-851C7-96 (1989). (L41) Matsuura, N.; Aral, T., A&. X-Ray Anal., 32, 21-30 (1989). (L42) Pdyakov, V. N., EMWon &ab. Mater. (S), 78 (1988). (L43) NoniS, J. D., Pdym. Paht ColovJ., 178 (4225), 816-17, 836 (1988). (L44) Wlllams, R. S.; Kuster, T. A.; Spence, J., J . Coat. Techno/., 81 (769). 19-24 (1989).
m.
Y. THERMAL ANALYSIS
(Ml) Ddllmore, D., Anal. Chem.,62 (12), 44R-50R (ISSO). (M2) Flynn, J. H., E m y d . Pdym. Scl. Eng., Kroschwttz, J. I., Ed.; Wlley: NOW YWk, I990 SUppl. VOl. 690-723. (m) Halnes8P. J., 7b”Mn.Acta, 148, 365-73 (1989). (M4)MlbStW, N. 8.. Chem. N . 2..52 (3), 55-8 (1988). (M5) Rhrabv, P. L.; Pktnkov, V. V., 77”xhh.Acta, 13s. 257-77 (1989). (w) Munk. p.; Hattam. P.; Du. O., J. Appl. Pdym. Scl.: Appl. Po(Lm. Synp., 43 (Potym. Anal. Charact.). 373-99 (1989). (M7) Le Parbwr, P., J . 7bm.Anal.. 33 (4), 1085-90 (1988). (M8) WMbW, J. E., A&. Org. a t . S d . Techno/. Ser., 11. 97-103
m am. .----,.
uphard, M.; Von Ryblnskl, W.. Rug. CoWl Pdym. Sd., 77 (Dispersed SySt.), 158-64 (1988).
(Mg)
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COATINGS (M85) Lam, P. W. K., porVm. Comp~.,10 (6). 439-48 (1989). (W) H.; M~MSZ~CZOWW, I.. porVm. Eng. Sei., 28 (16), 1097-102
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P. MISCELLANEOUS MEASUREMENTS (INCLUDINa PHYSICAL TESTS) (Pl) Cawley, P.; Adams, R. D., Meter. Scl. Technol., 5 (5), 413-25 (1989). (P2) Crostack. H. A.; Pohl, K. J., VDI-Ber., 702 (Reuf. Bewerten Oberflaechenschutzschichten), 139-84 (1988).
Anal. Chem. 1991, 63,99R-118R (p3) I-, F., E m . M .Sd. EW.; Kroschwtk, J. I., Ed.; Wlley: New Yolk, 1990 Suppl. Vol. 542-53. (P4) POWW. J. K., A M / . Specbosc., 12 (5), 453-508 (1989). (P5) Rsyndds, W. N e . Rev. Rep.. 3 (2), 3011-30/95 (1990). (w) Smlth, R. L., Inst. PhyS. Conf. Ser., 69 (New Mater. Their Appl. 1967), 251-4 (1988). (P7) OOSt&, K. M., Pmve Vemlcl, 63 (3), 34-42 (1987). (Pa) smith, R. L., VrrsVnp.. 93 (AngkFlnn. Jt. Symp. Adv. Nondestr. Test. I988), 28-32 (1988). (Pg) Afsharl, S.; VerWnden, M., Plest. a m @ . , 12 (3), 31-2, 34, 37 (1989). (PlO) V a n d t m m w b , G., Am. InkMektv, 66 (Io). 18-20, 22,24 (1988). (P11) Sekler, J.; Stelnmann, P. A.; Hlntermann. H. E., Surf. Coat. Techno/., . 36 (1-2), 519-29 (1988). (P12) Peny, A. J.; Valll, J.; Stehmann, P. A.. Surf. Coat. Techno., 36 (1-2). 559-75 . _iigaai. (P13) RlCkerby, D. S., Surf. Coat. Tech&., 36 (1-2), 541-57 (1988). (P14) DunStan, I., Surf. Coat. AIM., 26 (9,6-7, 9-10 (1988). (P15) Roche, A.; Le&, J. C.; Job, A. M.; Romend, M., m b Lleson-Chkn. Pdnt.9 35 (398), IX-XVII, 30-40 (1988). (P18) Stelnmann. P. A.; Hlntermann. H. E., J . Vac. Scl. Techno/.,A . 7 (3. Par! 2), 2287-72 (1989). (P17) Meter, W.; Van de Ven. L., Coatlng, 21 (12), 459-83 (1988). (P18) Harris, R. J.; Beuer, C. L., J. Adhes., 26 (4), 293-300 (1988). (Pl9) Rlde, A.; Gozzelho, G.; Ferrero. F., Int. J. Aches., 10 (2), 77-80 119901. (P20) dayless, R. A.; Perry, D. L.. J . Aches., 26 (2-3), 113-30 (1988). (P21) Allen. M. G.; Senturia, S. D.. pdym. Scl. Tech&., 37 (Adhes. Sealants Coat. Space Harsh Envlron.), 501-8 (1988). (P22) Lewandowskl, L. H., Avail. Unlv. Mlcrofllms Int.; Order No. DA8818754. (P23) Korobov, Y.; Salem, L., Mater. Perfcfm., 29 (4), 30-5 (1990). (P24) at-, J.; Rosty, R.; Bodner, M. K., S A M E J . , 25 (4). 15-19 (1989). (P25) Weller, W., Br. J . NonDestr. Test., 31 (5), 253-8 (1989). (P28) NOUmakr, P.:MkbnWMbeChe, 43 (2), 59-84 (1989). (P27) Bardeflheler, R., IW.J . Tech/)O/.,24 (3-4), 805-13 (1988). (P28) R W , R. P., Roc. Annu. Tech. Conf.-Soc. Vac. Coaters, 31st, 29 1-300 (1988). (P29) htolC, P.; McPherson, R., Mater. Sd. F c " , 34-38 (Int. Ceram. Conf.. AUSTCERAM 88, Part I), 451-5 (1988). (P30) COX, L. C.. Surf. Coat. Technol., 36 (3-4), 807-15 (1988). (P31) V~gel,K., Ind. LackkKbetr., 57 ( I l ) , 403-7 (1989). (P32) Nk, H. F., MatWh@fMtUng, 31 (3), 83-8 (1989). (P33) Hond, S. Y.; Kertesz, M., Phys. Rev. B : condens. Mater., 41 (ls), 11388-78 (1990). (P34) Hulsman, H. F.; Plgmans, H. J. M.; Schaake, R. C. F., A&. Org, Caet. Scl. Tschncf. Ser., 11, 75-81 (1989). (P35) Dale, W. C.; Paster, M. D.; Haynes, J. K., J . Adhes., 31 (I), 1-20 (1989). (P38) Twlsu, S.; Ueno, K., Polym. Palnt cdow J . , 179 (4242), 521, 523 (1989). (P37) Swletllczny, M., M W c h n o b g k , 31 (2), 89-91 (1990). (P38) A s k , W. A.; &ace, 0. M.. Roc. SPIEAnnu. Tech.lMark. Conf., 31sl (Polyurethanes 88). 209-18 (1988). (P39) Bell, D., Palnt Resin. 56 (4), 11-2, 15 (1988). ( ~ 4 0 1Bohtin, L., A&. 09. coat. sci. Tech&. w.,11, 118-26 (1989). (P41) buecker, M.; Brands, A.; Dlesel. H. D.; Lenhard. W.; Bentzen, A. C., Farbe Lack, 96 (2), 103-7 (1990). (P42) Lepoutre, P.; Engstroem, G.; Rlgdahl, M.. Nord. pulp Pap. Res. J . , 4 (I), 48-50 (1989). (P43) Stelkel, W., Kunstherz-Nachr.. 47 (25), 4-10 (1988). ( p u ) Schbnd, B.; GUM,J.; Pichot. C.; cluz,A., &bmef, 30 (IO). 1883-94 (1989). (P45) Lochhead, R. Y.; DavMson, J. A.; Thomas, 0. M., A&. Chem. Ser..
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223 (Polym. Aqueoue Media), 113-47 (1989). (P48) PhllHp, M.; WmVW. J. C., J. Coat. Technd., 61 (774), 41-50 (1989). (P47) Kotilar, A. M.; McDonnd, M. E.; Walsh, E. K., Gt& kbter. CYwract. them. AM/.; Sibilia, J. P., Ed.; VCH: New Yolk, 1988 pp 229-49. (p48) m, P., ADD/. pdhn. AM/. cheracl.; Mltchd. J., Jr., Ed.; H a w : Munlch, FRG, 1987; pp 297-312. (P49) Thompson, E. V., Encycl. Pdym. Sci. Eng.; Wley: New Yolk, 1989 Val. 18. DO 711-47. (P50) S k r o v k k , D. J., h g . Org. Coat., 16 (I), 89-101 (1990). (P51) Wolfe, S. V.; Tod, D. A., J. MacromdScl. Chem., A25 (I), 249-72 (1989). (P52) Zumbrun, M. A.; Ward, T. C., Polym. Mater. Scl. Eng., 60, 381-5 (1989). (P53) Kojlma, Y.; Hlrayam, T.; Sato, T.; Tanamura, T., A&. t3g. Coat. Sci. Techno/. Ser., 11, 112-7 (1989). (P54) Zosel, A.; Heckmann, W.; Ley, G.; Maechtle, W., A&. Org. Coat. Techno/. Ser.,11, 15-22 (1989). (P55) Nakamura, Y.; Yamaguchl, M.; Iko, K.; Okubo, M.; Matsumoto, T.. J. Mater. Scl., 25 (6), 2711-6 (1990). (P56) ReM, C. G.; Qleenberg, A. R., J . Appl. polym. 4Scl., 39 (4), 995-1014 (1990). (P57) Hill, L. W.; Kozbwskl, K., A&. Org. Coat. Scl. Technol. Ser., 10 (Int. Conf. Org. Coat. Scl. Technol., 12th, 1986), 31-9 (1988). (P58) Zosel, A.. Farbe Lack, 94 (lo), 809-15 (1988). (P59) sdlmeno, R. D.; Moren. M. S.; Jones, F. N., Pdym. Mater. Sd. Eng., 80, 700-4 (1989). (P60) odlyhe, M.; Hedley, 0.; Fllnt. C. D.; Slmpson, C. F., Anal. Roc. (London), 26 ( l l ) , 399-401 (1989). (P61) Takahashi. S.; Tashlro, N., KobunsM Ronbunshu, 46 ( I l ) , 873-81 (1988). (P62) Duffy, J.; Hartmann, S.; Lee. G.; Lee, J., Po&". Mater. Scl. Eng.,60, 817-21 (1989). (P63) Dlubec, J. J.; Lee, 0. F.; Duffy, J. V.; W i n , R. J.; Lee, J. D.,pdym. Mater. SCl. EW., 60, 579-83 (1989). (P64) a n . (%ban. J. K.: Prime. R. B... J . ADD/. ,. pdvm. &/.. 37 (3). . .. ' 803-18 (1969). (P65) Wlsanrakklt, G.; Glllhan. J. K.. W m . Mater. Scl. €no., 62. 786-72 (1990). (P86) Bayer, H.; Lehner, B., pdym. Mater. Sci. Eng.. 80, 372-81 (1989). (P67) Wngard, S.; WHliams, W.; Wolkhg, K.; batty, C. L., ACS Symp. Ser., 367 (Crosslinked Polym.), 199-220 (1988). (P68) Dlcksteln, H. L.; Prlme, R. B.; Dlcksteln, W. H., Pdym. Mater. Sd. Eng., 59, 985-9 (1988). (P89) Adams, G. W.; Farrls, R. J., Polymer, 30 (IO), 1829-35 (1989). (P70) Mazich, K. A.; Kllloger, P. C., Jr.; Ingram, J. A., Rubberchem. Techn d . , 62 (2), 305-14 (1989). (P71) Leroy, J. M.; Floquet, A.; Vellechalse. B., J . Trfbol., 111 (3), 538-44 ( 1989). (P72) Bratton, 0. J.; Wasson, E. A.; Nicholson, J. W.; Wllson, A. D., J . OM Cdour Chem. Assoc., 72 (l), 10-4 (1989). (P73) Steinhaus, R.; Baumgarten, G., Roc. E/ectr.l€lectron Insul. Conf., 19th, 164-8 (1989). (P74) Day, D. R., J. Relnf. Plest. Compos., 7 (5), 475-84 (1988). (P75) Gotro. J.; Yandrastis, M., Pdym. Eng. Scl., 29 (5), 278-84 (1989). (P78) WaPWIan, K. E. D., A&. Org. Coat. Techno/. Ser., I O (Int. Conf. Org. Coat. Scl. Technol., 12th. 1986), 40-5 (1988). (P77) Mopslk, F. I.; Chang, S. S.; Hunston, D. L.. Mater. Eva/.. 47 (4), 448-53, 465 (1989). (P78) Schlosser, E.; Schoenhals, A., ColkM pdym. Scl., 267 (1 1). 963-9 ll989l. ---, (P79) Tsukahara. Y.: ohira, K.; Sako, M.; Brlggs, G. A. D., Acoust. Imaghg, 17. 257-64 (1989). (P80) (1989). Generiwala. S. N.; Hartung. H. A., Polym. Mater. Scl. Eng.. 80, 800-4
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Surface Characterization M. A. Ray, G. E. McGuire,* I. € Musselman, I. R. J. Nemanich, and D. R. Chopra Microelectronics Center of North Carolina, 3021 Cornwallis Road, P.O. Box 12889, Research Triangle Park, North Carolina 27709
INTRODUCTION Reviews of surface characterization have appeared in Analytical Chemistry every 2 years since 1977 (1-7). During this time. the field has erown sienificantlv in the volume of papers published as wefl as the iumber d ap lications and diversity of surface characterization tools. $his review is similar to the last one on this series, bein written by multiple authors with s cialties in one or more ofthe broad categories of surface anarsis in an attempt to highlight important advances in each of these areas. This review begins with lit0003-2700/91/0363-99R$09.50/0
erature from Jan 1989 and ends with literature from Dec 1990.
A. ION SPECTROSCOPY Secondan Ion Mass SDoctromdn
Considerable pro e'ss has been made over thb past several years in understangng the basis of secondary ion formation and in developing new techniques for studying sputtered ions. Since 1988, three books reviewing various SIMS methods and techniques have been published. The volumes include a technical handbook primarily for depth profiling and impurity 0 1991 American Chemical Society
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