Anal. Chem. 1989, 61 , 33 R-45 R (XX10) Zagorodnil. V. V.; Karmanov, V. I. Met@ Rentgenospektr. Anal. 1986, 33-40; CA 706(16):130756~. (XX11) Kadyshman, T. A.; Ioffe, V. N.; Martynov, I. F. Zavod. Lab. 1987, 53(6), 90-1; CA 708(6):48263p. (XX12) Kumakura, K.; Ryuzono, A.; Hosokawa, Y. US. US 4,692,935 A, 8 Sep 1987; CA 707(20):189994u. (XX13) Johnson, N. F. A&. X-Ray Anal. 1988, 29, 539-43; CA 706(12):88449u. (XX14) Taguchi, I.; Tanaka, K. Tebu to Hagane 1986, 72(10), 1629-36; CA 105(26):230468z. (XX15) Tanaka. H.; Tagata, S.; Suzumi, J. Jpn. Kokai Tokkyo Koho JP 61/ 62850 A2. 31 Mar 1986: CA 706(4):27083v. (XX16) Wang, Y.; Chen, Z.'X-Ray Spectrom. i987, 76(3), 131-6; CA 707(8):69869k.
(XX17) Wang, Y.; Chen, 2. X-Ray Spectrom. 1987, 76(3), 137-42; CA 707(8):69670d. (XX18) Smagunova, A. N.; Molchanova, E. 1.; Usova, E. R. Zh. Anal. Khim. 1987, 42(10), 1797-807; CA 708(10):87072~. (XX19) Abe, T.; Narlta, M.; Saeki, M. X-sen Buns&/ no Shinpo 1986, 77, 143-75; CA 706(10):77755q. 1987. (XX20) Bilbrey, D. 6.; Leyden, D. E.; Hardlna A. R. ADD/. . . Snectrosc. . 47(8), 1455-7. (XX21) NI, X.; Zhao, S.; Xu, K.: Zhang, F. Helishu 1986, (lo), 36-8; CA 706(14):112730b. (XX22) Roesslger, V.; Dostal, K. P. Ger. (East) DD 237449 A3, 16 Jul 1986; CA 707i20k189999z. (XX23) Baksubramanlan, T. V.; Rao, A. S. Trans. Indian Inst. Met. 1988, 39(5), 399-405; CA 707(8):69868j.
Coatings Dennis G. Anderson DeSoto, Inc., Box 5030, 1700 S. Mt. Prospect Rd., Des Plaines, Illinois 6001 7
A. INTRODUCTION This review covers analytical techniques applicable to the examination of coatings and coatings raw materials, substrates upon which coating are placed, etc., since the last review in 1987. 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 heavily referenced areas are nuclear magnetic resonance spectroscopy, infrared spectroscopy, gas chromatography, thermal analysis, and gel permeation chromatography. New or unique applications for established analytical techniques appear throughout the review. Several articles and books have appeared that deal with analysis and monitoring during the production of paints and varnishes ( A I ) ,the testing of coatings during service (A2),and practical problems with enamel systems ( A 3 ) . General methods for the characterization of radiation curable systems (A4),thermal barrier coatings (A5),coatings for concrete (A6), and marine antifouling paints ( A 7 ) also appeared. Specific topics of interest included models for assessing the damage of acid deposition on painted surfaces ( A @ ,microbial deterioration of corrosion protection coatings ( A 9 ) ,the migration of species from food contact surfaces (AIO, A l l ) , and new physical and analytical techniques to evaluate surfactant detergency (A12).
B. CHEMICAL AND ELECTROCHEMICAL SECTION Titrimetric methods remain popular for the determination of phosphorus and fluorine in organic compounds (B1)and persulfate in the presence of organic substances (B2). Direct potentiometry was reported as the method of choice for the examination of trace chloride in polymeric materials (B3) and the measurement of nitrates in phosphatizing concentrates (B4). Specific papers dealing with the determination of primary amides (B5, B6), isocyanates, biurets, and allophonates in urethanes (B7), mercaptans and disulfides (B8),epoxides (B9,BIOI and phenolic hydroxyls (B11)appeared. The measurement of residual unsaturation in glass fiber polymer coatings (B12) and polyols (B13) received special attention during this period. Papers continue on improved methods for the determination of elemental composition in organic compounds (B14) and nonionic surfactants (B15). The unique problems associated with the measurement of nonvolatile content in paints and coatings (B16)and natural rubber (BI 7) were also presented. An improved procedure for the measurement of moisture in samples which are difficult to dissolve or alter 0003-2700/89/0361-33R$06.50/0
normal Karl Fischer reagents holds promise (B18). Surfactant selective ion electrodes are becoming more widely available and papers have appeared highlighting applications in anionic (B19, B20) and cationic (B21, B22) surfactant mixtures. Two photometric methods for the determination of cationic surfactants were also reported during this period (€323,B24). Water-soluble polymer characterization received special attention in papers dealing with vinyl acetate grafted cellulose (B25)and N-substituted acrylamide copolymers (B26). References to the use of polarographic techniques continue, with articles on the determination of metals in polymeric materials (B27,B28)and lead in pigment pastes and primers (B29). Electroanalytical methods for the determination of organic functional groups included the detection of residual aromatic amine hydrochlorides in polyurethanes (B30) and the examination of nonionic surfactants (B31).
C. GAS CHROMATOGRAPHY The use of gas chromatography for the analysis of volatiles in coatings continues, with publications highlighting the examination of solvents in automotive paints ( C l , C 2 ) , air monitoring in the paint and varnish industry (C3), and the evolution of solvents from emulsion systems (C4, C5). The unique problems associated with the determination of volatiles in aqueous solutions received special attention (C6) as did the examination of the solvent power of petroleum fractions and waxes (C7-C9). The purity of acrylate and vinyl monomers utilized in the production of coating binders was reported, with particular emphasis on monofunctional acrylates (CIO-C12), diacrylates (C13),and unreacted styrene in polyester resins (C14, C I S ) . Monomers used in condensation polymers were the subject of several gas chromatographic studies. Examples include fatty acid esters ( C I S , C17), hydroperoxides in the presence of hindered amine stabilizers (C18), ethylene glycol (C19),glycerol (C20),and high boiling monomers present in polycarbonates and polysulfones (C21). Several unique studies using gas chromatography were reported, such as the migration of packaging components in food containers (C22),the solubility and polarity parameters of poly(ethy1ene glycols) (C23, C24),examination of hydrocarbon-formaldehyde oligomers (C25), gas sorption in polymeric materials (C26), and the determination of organotin (C27, C28) and bromine containing species in polymers ( C 2 9 4 3 1 ) . The examination of undesirable volatile species in polymers and coatings provides a unique opportunity to use the sensitivity afforded by gas chromatographic techniques. During this period, studies concerning dynamic headspace analysis (C32-C35), purgeable organics in water (C36-C38), and outgassing in polyesters (C39) and silicone rubber (C40)have been
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published. Chemical degradation prior to gas chromatographic analysis continues to be popular, with several papers dealing with siloxane containing polyester resins (C41-C43), polyurethanes (C44-C46), triglycerides ((247, C48), rubber (C49), silanol groups ( G O ) ,amphoteric surfactants (C51),and triaryl phosphates (C52). Thermal degradation provides another convenient mechanism to render polymeric materials amenable to examination via gas chromatography. Many general articles have appeared (C53-C57), as have specific studies considering vinyl and acrylate systems (CSS-CSl), ABS plastics (C62),urea-formaldehyde resins (C63),diallyl is0 hthalate polymers (C64), polyamides (C65), polyurethanes (866-C68), polyimides (C69), alcohol polyethoxylates (C70),silicone polymers (C71, C72), epoxies (C73, C74), phenolics (C75), and lignin derivatives (C76, C77). A newer technique suitable for the examination of oligomeric and polymeric materials is supercritical fluid chromatography. A few articles have appeared with specific applications for the coatings industry (C78, C79);however, general articles related to this technique are also of interest (C80, C81). The determination of solubility parameters (C82, C83),activity coefficients (C84, C85), and miscibility (C86-C88) received special attention. Specific studies worthy of consideration deal with the characterization of polycaprolactones (C89), surfactants (C90), and low molecular weight components in polymers (C91-C93). Mass spectrometry, particularly when coupled with the separating power of gas chromatography, remains an extremely powerful tool for coatings analysis. Papers of particular interest to the coatings analyst include studies on styrene polymerization (C94), coal pyrolysis (C95),acrylic acid oligomer characterization (CSS), urethane analysis (C97-C99), epoxy coating components (CI OO-C102),phenol-formaldehyde condensates (C103),adhesives (C104),surfactants (C105-C108) and plasticizers in poly(viny1 chloride) packaging films (Clog).
D. GEL PERMEATION CHROMATOGRAPHY Several review articles have appeared relative to the use of gel permeation or steric exclusion chromatography for the examination of coatings and polymers (01, 0 2 ) . Special studies relative to the characterization of water-soluble polymers ( 0 3 , 0 4 ) , the use of chemometrics (05), and superspeed gel permeation chromatography for process analysis (D6) were also published. Advanced techniques for the examination and treatment of data generated during gel permeation chromatographic studies have been reviewed ( 0 7 ) and computer programs developed which operate using personal computers (08). Other general studies reported include methods for reduced solvent consumption ( 0 9 ) and an improved sample preparation procedure for synthetic rubber lactices (010). Progress continues in understanding the basic separation mechanism operating in gel permeation chromatography (011, 0 1 2 ) , with particular emphasis on nonsize ( 0 1 3 , 0 1 4 ) and electrostatic and steric factors (015). Along these same lines, publications have appeared studying molecular (016) and stereo association (017). Correction for instrumental peak broadening continues to be studied (018-021) as do concentration effects ( 0 2 2 ) . Attempts a t universal calibration continue, with renewed interest in the use of a modified Mark-Houwink equation ( 0 2 3 ) and chromatographic crossfractionation ( 0 2 4 ) . Papers continue on the use of multiple detectors in size exclusion chromatography ( 0 2 5 ) as well as the more common refractive index (026-028), infrared absorption ( 0 2 9 ) ,and light scattering detectors ( 0 3 0 , 0 3 1 ) . The utilization of viscometric detection systems has shown increased interest during this period ( 0 3 2 - O s ) , particularly in reference to the evaluation of polymer molecular weight and branching (037-039). A unique method, derivatization of amines and polyamines with o- hthalaldehyde (D40), was reported to increase sensitivity Ey 2 orders of magnitude over refractive index and ultraviolet detection. Many gel permeation chromatographic studies were published which dealt with specific sample types. These included the examination of low molecular weight compounds ( 0 4 1 , 0 4 2 ) , acrylated polymers ( 0 4 3 , 0441, alkyd resins (D45), polyurethanes ( 0 4 6 , 0 4 7 ) , poly(viny1 alcohol) (D48),polyamides ( 0 4 9 , 0 5 0 ) , polyolefins (051, 0 5 2 ) , silicones ( 0 5 3 ) , 34R
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phenolics ( 0 5 4 , 055), fluoropolymers ( 0 5 6 ) , and alkylene oxide condensates (057).
E. HIGH PERFORMANCE LIQUID AND THIN LAYER CHROMATOGRAPHY A fundamental study was reported ( E l )which provides an exponential expression for dispersion along a high-performance liquid chromatographic column. Another useful study examined the utility of ion exchange cleanup techniques prior to ion chromatography (E2). An exciting area of development involves the use of field flow fractionation to separate polymeric materials. Among the papers published were a review on the separation of polymers (E3),the effects of overloading (E4),electroviscous and particle swelling (E5,E6), and thermal field flow fractionation to study polymer molecular weights (E7). Hydrodynamic chromatography was also reported recently as a mechanism to separate a series of xanthan polymers and hydrolyzed polyacrylamides (E8). A major use of high-performance liquid chromatographic techniques involves the determination of monomeric or additive species in coatings and polymers. Among the specific studies of interest were the quantitation of acid species in soaps (E9)and ethoxylate surfactants (EIO),the measurement of unreacted isocyanates ( E l l )and solvolysis products (E12, E13) in urethanes, biurets, and allophonates, the examination of formaldehyde and other aldehydes in surfactants as the 2,4-dinitrophenylhydrazonederivative (E14),and the analysis of dicumyl peroxide (E15). Specific measurement of tributyltin oxide in antifouling paints (E16), free amines in polymeric amine hardeners (E17 ) and stabilizers (E18), acrylamide monomer (E19),and fatty acids (E20) were also reported since the last review. Among the more widely used high-performance liquid chromatographic procedures of interest to coatings analysts involves the examination of surfactant systems. Papers continue on the separation of nonionic (E21-E23) as well as anionic (E24-E26) surfactants. Reverse-phase techniques have recently been reported for the characterization of acrylate copolymers (E27-E30), polycaprolactone diols (E31),hydroxyl containing oligoesters (E32),hydroxypropyl cellulose (E33), melamine-formaldehyde adducts (E34), and epoxy resins (E35). References to the use of thin-layer chromatography for the examination of polymers and coatings were few in number during this period. Studies were published, however, on the separation of phthalate esters (E36),phenolic alcohols (E37), amine antioxidants (E38),fatty acid diethanolamides (E39), epoxy resins (E40),and poly(ethy1eneamines) (E41).
F. ATOMIC ABSORPTION AND PLASMA EMISSION SPECTROSCOPY Relatively few references to the use of atomic absorption and plasma emission spectroscopy were found since the last review, which deal with coatings and coatings raw materials. The lead content in household paints continues to be examined using flame and flameless atomic absorption spectroscopy (FI). Other atomic absorption spectroscopic studies of interest include: the evaluation of tributyltin levels in estuaries prior to the introduction of regulations governing the use of tributyltin-based antifouling paints (F2),the determination of nickel and cobalt in brass coatings (F3), the detection of elemental sulfur in rubber (F4),the measurement of sodium and silicon in organosilicone and organofluorosilicone surfactants (F5) and the detection of metallic elements in poly(vinyl chloride) (F6,F7). Inductively coupled argon plasma emission spectroscopy continues to displace atomic absorption spectroscopy in many applications, including: multielement analysis of environmental and biological samples (F8), the detection of trace elements in the oil and fat-processing industry (F9) and the examination of elemental composition in electroless nickel coatings on a variety of substrates (FIO).
G. INFRARED SPECTROSCOPY Infrared spectroscopic techniques remain as the most highly referenced since the last review in-1987. Studies of a general nature include the use of least-squares methods during quantitative analysis ( G I )and quantitative multicomponent analyses of resin films when thickness i$ unknown (G2-G4). Many eeellent references to the use of microscope attach-
COATINGS
Dnn)l G.
Aindenon is a Technical Manager
in Anabiical and Compllter Applications Research DepaRment 01 DeSoto. Inc. Since Pining DeSoto 22 years ago. he ha8 been lnvmed in me analysis and characterration of polymers and coatings using chemical and instrumental techniques. He receked B.S. and M.S. degrees in chemlsby hom RWsevetl University. where he is ais0 B faCUW member. Mr. Anderson has BUk e d o( CoBUtlmed 21 publicationsdealing wsh the analysis of polymers and malings and is Coauthor of An Infrared SpechoscoPY Atlas lor the Caah'ngs Industry. He is also the recipient of three ROO" Foundation awards lor distinguished Sewice to the costlngs induslPI.
I
ments were found; particular articles of interest were special studies of recent developments in the field (G5, G6), use of infrared microspectrophotometry as a failure analysis t w l (G7), novel techniques for microscopic sample preparation (G8), utilization in industrial problem solving (G9, GZO), photometric considerations in the design of microscope accesories ( G l l ) ,limitations of quantiative infrared microscopy (GZ2),and methodology to characterize heterogeneities in polymer films (GZ3). Several rather unique studies were found on the advantages of phase analysis during photoacoustic measurements (GZ4),situations where the vibration of regular polymer segments do not couple with neighboring 'defect" units (G15),and the use of infrared reflectance to examine the thickness of thin polymer films on metallic substrates (GZ6, G l 7 ) . The determination of polymer refractive index using infrared spectroscopic techniques was reported again (GZ8, GZ9) as were the determination of dynamic structural properties of polymers (G20) and the use of a Circle cell to evaluate surfactant-acrylate polymer interactions (G2Z). The popularity of infrared spectroscopy for functional group analysis continues, with publications specific to the determination of isocyanate groups (G22, G23),allophonate, biuret, and isocyanurate (G241, methoxy groups in melamine-formaldehyde oligomers (G25), acrylate (G26) and vinyl (G27) unsaturation. degree of ethoxylation in nonionic surfactants (G28), hydroxyl and carboxyl groups in polyester resins (C29), and water in polyethylene insulated cables (G30). Curing studies are numerous, including the use of infrared spectroscopic monitoring of an epoxy adhesive (G3Z), epoxy-amine systems (G32. G33), epoxy-anhydride polymers (G34),UV/moisture curable methacrylates (G35),UV curable multifunctional acrylates (G36),and acrylated epoxies (G37, G38), polyurethanes (G39-G41), alkyd-melamine coatings (G42),unsaturated polyesters (G43),and urea-formaldehyde oligomers (G44). Publications concerning the examination of polymer systems included the determination of ionic interactions in polymer blends (G45), infrared absorption in stretched polymers (G46), modification of surfaces by photoinduced graft copolymerization (G47), the determination of copolymerization ratios in acrylate copolymers ((248, G49), and cationic photopolymerization of acrylates (G50). Among the specific polymer types examined were poly(viny1 chloride) (G51-G53), polyesters (G54, G55),alkyds (G56),nitrocellulose (G57), epoxy resin containing systems (G58-G60), polysiloxanes (G6Z), urea-formaldehyde oligomers (G62),phenolic resins (G63),poly(ethers) (G64-G66), polyurethanes (G67G69) and polyimides (G70, G7Z). Degradation of polymer systems is ideally studied by using infrared spectroscopic techniques. Interesting publications were found on the study of polymer degradation in general (G72-G74), the degradation of epoxide films in a mildly corrosive environment (G75),aging in polyurethane elastomers (G76), polyamides (G77), photocured acrylated epoxy and urethane acrylates (G78), poly(viny1 acetate) (G79), polypropylenes (C80, G8Z), and aminosilane primers (G82). Studies involving accelerated weathering examined the effects of degradation on polyesterurethane coatings (G83) and automotive finishes (G84, G85). Infrared spectroscopic analysis studies of particular interest to the coatings analyst included a general paper on methodology (G861, the examination of lacquer films (G87),Fourier transform techniques in forensic analysis (G88), the use of a
diamond anvil cell for the examination of paint chips (Gag), reflectance studies of coatings on metal wires (GW), the quantiative determination of organic pigments in coatings (G9Z),the evaluation of triazole compounds as antifouling and anticorrosive agents (G92),the distribution of surfactants in latex films (G93),and carbonate leaching from latex paint films (G94). Few references were noted relative to the use of Raman spectroscopy in coatings related analyses. A general review was presented (G95)as were special studies on thin films ((296, G97), measuring the degree of crystallinity in polyethylene (G98), and the degradation of poly(viny1 chloride) (G99).
H. NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY This section will be divided into the following four topic areas: general papers and newer techniques, the detection of specific species and functional groups, studies related to specific polymer types, and the use of nuclear magnetic resonance spectroscopy to study the curing of epoxy resin systems. A number of excellent general review articles appeared during this period (HI-H3), in addition to specific reviews on the examination of polymer microstructure (H4) and heterogeneous systems ( H 5 ) . Two-dimensional nuclear magnetic resonance studies have been reported for polymer mixtures (H6, H a , with special reference to the examination of diffusion in polymer systems (H8) and polymer networks (H9). Unique studies of interest included combined rotation and multiple pulse spectroscopy (HI01 and NMR spin trapSpectral ping for the examination of primary radicals (HZZ). shifts were correlated with the acid-base chemistry in polymers (HZ2),as was the surface chemistry of adsorbed species using nuclear-spin-polarized atomic beams (HZ3). Specific references to the use of nuclear magnetic resonance to study coatings included the examination of thermosetting alkyd systems (H14),radiation curable coatings (HZ5),polyethoxy silanes (H16),and Chinese lacquer (HZ7). End groups in acrylic polymers were studied by using carbon magnetic resonance spectroscopy (H18, H19), as was the identification of hardeners used with solid epoxy resins (H20). The identification of surfactants in household detergents received special attention (H2Z) as did the determination of linoleic acid mono- and diesters of poly(ethy1ene glycols) (H22) and the hydrolysis and condensation mechanisms of a silane coupling agent (H23). Among the specific polymer types examined by using nuclear magnetic resonance techniques were polyolefins (H24H29), poly(viny1methyl ether) (H30),fluorocarbon polymers (H31, H32), polyacrylates (H33-H38), acrylamide containing polymers (H39, H40), tri-n-butyltin methacrylate/methyl methacrylate copolymers (H4Z), polysiloxanes (H42-H45), polyesters (H46-H48), poly(alkylene oxides) (H49-H52), and urea-formaldehyde condensates (H53-H55). The curing and condensation reactions in epoxy-containing polymer systems produced many papers. Among the most interesting examined: model epoxy amine systems (H56,H57), the glycidyl ether-benzyl amine reaction (H58),and curing via silicon containing aliphatic amines (H59), aminodichlorodipheuylmethane (H60), 1,kdiaminohutane (H6Z), masked hexamethylene diisocyanate (H62), and diphenylsilanediol (H63).
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 on which the coating is placed. During this period, several useful review articles appeared (11-14) which document the advantages of the methodologies involved. Standards and reference procedures were also documented (IS)as was an extensive review of surface Fourier transform infrared spectroscopy for the examination of polymers (16). Other reviews included the evaluation of environmental degradation as it relates to metal-polymer adhesion (17,I.S)and the advantages of chemical derivitization prior to surface analytical studies (19). X-ray photoelectron spectroscopy (XPS) or electron spectroscopy for chemical analysis (ESCA) remains one of the most widely utilized tools for surface characterization. Two exANALYTICAL CHEMISTRY, VOL. 61, NO. 12, JUNE 15. 1989
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cellent review articles were published during this period (110, 111) as was a standard practice for re orting ESCA spectra
(112). The unique problems associatecfwith the examination of coatings received special attention (113-115) as did the examination of X-ray induced changes in polymeric materials ( I l S ) ,passivation of tinplate (117,118),degradation of a polyurethane elastomer (119), acrylic polymer blends (120), cellulosic materials (121),sheet molding compound (1221,and suspensions of glass particles in coatings (123). The factors that influence the accuracy of Auger electron spectrometry were documented in an excellent review paper (124) as were methods of excitation, instrumentation, data acquisition, and handling (125). As was previously reported for ESCA spectra, a standard practice for reporting data in Auger electron spectroscopy was published (126). Also reported were a standard guide for background subtraction techniques (127),identifying chemical and matrix effects (I%), and methods for sample handling (129) in Auger electron spectroscopy. Quantitative analysis by a curve synthesis method based on nonlinear least-squares fitting (130)received special attention as did conversion coatings on aluminum substrates (131),polymer/metal interfaces (132),adhesive bonding systems (133),and depth profiling on anodized aluminum (134). Secondary ion mass spectrometry (SIMS) was reviewed in depth (135)as were the elimination of matrix effects (136), the fragmentation of acrylic and methacrylic homopolymers (137),and the characterization of asbestos fiber surfaces (138). Other studies of interest to the coatings analyst, reported during this period, include the use of low energy electron diffraction (LEED) to study surface structure (139),the use of electron spin resonance (ESR) to examine the UV and electron beam curing properties of poly01 polyacrylates (140), and small angle neutron scattering (SANS) from interfacially polymerized core-shell latices (141).
J. ULTRAVIOLET-VISIBLE SPECTROSCOPY Visible spectroscopy was reported as an excellent means to determine the arsenic content in paint on childrens toys ( J I ) ,the evaluation of phosphate content in detergents (J2), and caprolactam purity permanganate index (J3). The determination of organic species via visible spectroscopy continues, with publications on the reaction of p-(dimethylamino)benzaldehyde with aromatic amines (J4),the determination of polyoxyethylene oligomer-hexamethylene diisocyanate reaction products through a cobalt complex (J5),the detection of cationic surfactants by reaction with bromophenol blue (J6),and several methods to detect formaldehyde in urea-formaldehyde oligomers (J7,J8) and resin coated paper (J9). Ultraviolet and fluorescence spectroscopy were reported as the methods of choice to evaluate the curing (JIO)and photolysis ( J l l )of polyurethanes, the morphology and degree of cure in polyimides (J12, J13), molecular mobility in polystyrene-poly(viny1 methyl ether) blends (J14)and the examination of metal ion binding in a perfluorosulfonate membrane (JI5). General papers of interest in this area include data processing techniques to extract pure component spectra from mixture spectra in polymeric materials ( J l S ) ,time resolved laser spectroscopy of photoinitiators used in acrylic polymerization (JI 7), determining the amount of styrenebutadiene latex on the surface of paper (J18),and the determination of heat and light stabilizers in poly(viny1 butyral) (519). Visible spectroscopy remains the primary tool to measure color uniformity in coatings. Color measurement and computer color matching for metallic paints received special attention (J20)as did the evaluation of pearlescent pigments (J21),optical profilometry (J22),and light scattering as a mechanism to measure the interaction between latex spheres and carboxymethyl cellulose (523).
K. SPECTROSCOPY-MISCELLANEOUS TECHNIQUES This section will be divided into three general categories: dielectric measurements, electron spin resonance, and several lesser used methods, including Moessbauer spectroscopy, photo correlation spectroscopy, Rutherford scattering, positron annihalation spectroscopy, and ellipsometry. Dielectric studies have increased in popularity over the last several years as a complement to dynamic mechanical mea38R *
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surements. Publications have recently appeared on the real time measurement of glass transition temperature ( K I ) ,use as a nondestructive monitor of resin processing properties (K2),testing of adhesive joints (K3),the examination of water absorption in coatings (K4),and general studies on monitoring the curing of thermosetting coatings (K5) and polymers (K6). Of special interest were several excellent studies highlighting the use of dielectric measurements to examine the curing behavior of epoxy resin systems (K7-K9). Electron spin resonance was reported as the method of choice for the evaluation of coating weatherability (KIO,K11) and photodegradation (K12-Kl4). More traditional uses of electron spin resonance techniques include studies of radical polymerization (K15,K16),the efficacy of ultraviolet absorbers in paints (K17),the decay rates of radicals in polymers following irradiation (K18,K19) and the magnetic properties of polymers containing conjugated double bonds (K20). Several lesser known methods yield information of value to the coatings analyst. Metal-polymer interfaces were examined in detail using Moessbauer spectroscopy (K21),as was the fate of tributyl tin toxicants in antifouling coatings (K22). Photon correlation spectroscopy was again reported for the measurement of latex particle size distribution (K23,K24) and the absorption of polyethylene oxide copolymers on polystyrene latices (K25). Rutherford backscattering was the major technique employed in the characterization of phosphate conversion coatings (K26)as was positron annihilation spectroscopy for characterizing pigment dispersion in high solids coatings and latices (K27). Adhesion to substrates and surface characterization were reported via inelastic tunneling spectroscopic (K28) and ellipsometry (K29)studies.
L. MICROSCOPY AND X-RAY TECHNIQUES This section is a combination of two areas covered separately in the last review: microscopy and X-ray analysis. Relatively few pertinent references were found utilizing only X-ray techniques and the extensive use of X-ray analysis in conjunction with scanning electron microscopy prompted the decision to combine the sections. Utilization of microscopic techniques for the characterization of paints in forensic science continues (L1). Several newer techniques also received special attention since the last review, including ultrasound microscopy (L2),fluorescence microscopy (L3), and photoacoustic microscopy (L4). Morphological examination of polymers was also enhanced using elementspecific imaging (L5). Optical microscopy, as used in polymer research, was presented (L6),as was the analysis of coatings on paper (L7) and phosphate coatings as they relate to corrosion resistance (L8). The distribution of particulate materials in coatings was studied in general (L9-LII) and with particular emphasis regarding inks (L12). Transmission electron microscopic studies included the complexities in the examination of thin polymer films (L13, L14), domain morphology in polyurethane block copolymers (L15),and polymer blends (L16). Novel methods of preparing polymers for examination via transmission electron microscopy received special attention (L17)as did staining using ruthenium trichloride/Chlorox (L18) and ruthenium tetroxide (L19). Cryotransmission electron microscopy of latex systems was discussed in detail from the viewpoint of particle size distribution and electron beam damage (L20) as was the characterization of nonionic polystyrene latices in aqueous media (L21) and core/shell latex morphology (L22). The use of scanning electron microscopy to study polymeric materials was the subject of two general reviews (L23,L24). Of special interest was the use of low voltage experiments in the examination of polymers (L25,L%), polymer blends (L27), and low density materials (L28). The advanta es noted in these studies were elimination of specimen cfamage, less coating induced artifact structure, and minimal charging during analysis. Specific sample types of interest to the coatings analyst reported using scanning electron microscopy included polyurethane-vinyl chloride interpenetrating networks (L29),polysulfide sealants (L30),surface analysis of conversion coatings on zinc-coated substrates prior to powder coating (L31),detection of microconstituents in paints (1532, L33),and adhesion at a polymer/metal interface (1534,L35). Reported studies of interest concerning X-ray analysis methods were the examination of structure factors in surface X-ray diffraction (L36),the use of wide angle X-ray diffraction
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to evaluate thermal expansion in polyoxymethylene (L37), X-ray scattering in segmented poly(urethane ureas) (L38),and X-ray fluorescence analysis of aluminum paints (L39).
M. THERMAL ANALYSIS The thermoanalytical techniques discussed in this section include differential thermal analysis, differential scanning calorimetry, thermogravimetric analysis, and flammability testing. References to differential thermal analysis continue, however, the quantitative aspects of differential scanning calorimetry are predominating in the literature. Among the references to differential thermal analysis found since the last review were comparative investigations of emulsion paints ( M I ) ,studies on adhesive strength (M2, M3), evaluation of acrylate (M4,M5), and itaconate (M6)bulk polymerization. Two special studies were the determination of epoxide number (M7) and the crystallization and melting behavior of plasticized poly(viny1 chloride) (M8). A paper highlighting the capabilities of differential scanning calorimetry with X-ray diffraction and mass spectrometry appeared (M9)as did studies on the characterization of adthermosetting powder coatings (MI 1) and hesives (MIO), epoxy prepregs (M12). Bound water in polymers (M13)was measured with a high degree of accuracy via calorimetry. Studies continue on the dependence of glass transition temperature on poly(viny1 chloride) tacticity (M14) and poly(propylene glycol) molecular weight (M15). Factors, such as sample size, were studied in great detail (M16)as was methodology to measure the thermal conductivity of polymers ( M I 7-M19), polymer miscibility (M20-M23) and diffusion (M24). Curing kinetic studies remain as one of the most popular applications of differential scanning calorimetry. Epoxy resin systems were studied extensively, using amine (M25-M31), anhydride (M32-M35) and peroxide (M36) curing agents. Unsaturated polyester (M37-M41), acrylic (M42),polyimide (M43) and phenol-furfural (M44, M45) systems were also reported during this period. A relatively new application for differential scanning calorimetry involves the study of photopolymerization kinetics, particularly relative to potential uses in radiation curable coating systems (M46-M51). Among the nonkinetic polymer applications for differential scanning calorimetry were the evaluation of polysiloxanes (M52),POlyphenylsilsesquioxanes (M53),polyoxyethylenes (M54),POlybutadienes (M55),polyurethanes (M56)and bis(maleimide amines) (M57). Thermogravimetric analyses have been reported for a number of polymer systems of interest to coatings chemists, including: acrylates (M58-M60), ethylene vinyl acetates (M61),polystyrenes (M62),styrene-butadienes (M63),chlorinated polymers (M64, M65), polyurethanes (M66, M67), polyester imides (M68),acetylene terminated polymers (M69), phenolics (M70) and sulfide-formaldehyde systems (M71). Thermal analysis procedures are also applicable for the examination of the flammability (M72-M74) and ignition temperatures (M75)of polymers. In addition, adiabatic calorimetry was, again, reported as a mechanism to evaluate the hazard potential of polymerization mixtures (M76)and isocyanate monomers (M77).
N. ENVIRONMENTAL AND INDUSTRIAL HYGIENE Studies of particular interest to coatings analysts include the examination of painters occupationally exposed to waterand solvent-based paints ( N I )and the interferences caused by lacquer fumes on readings obtained by using the Intoxilyzer (N2). General studies of importance centered on the effects of diffusive sampling on compliance with TLV values (N3) and the principles involved in the Inhalation Hazard Test (N4). The examination of volatile organic species in water continues to be studied in depth, with publications on the development of alternate test methods (N5,N6), distillationextraction (N7), purge-and-trap (N8-NIO), and headspace sampling (N11). Statistical models for the analysis of volatile organic compounds in waste disposal sites were also questioned in some detail (N12,N13). Among the other components of interest examined were surfactants in water (N14) and an
analyzer to measure non-methane organic species using EPA Method 25 (N15). Gases and vapors pose their own unique analytical difficulties, as evidenced by publications on the preparation of low-parts-per-billion gas standards (N16),the examination of organic vapors using diffusive samplers (NI 7-N19), and the use of Tenax cartridges (N20)and thermally desorbable passive samplers (N21). Methods of special interest involved the collection and analysis of airborne hexamethylene diisocyanate (N22),the determination of insoluble chromates in paint aerosols (N23),and the development of air sampling methods for the determination of oxirane content in aerosols from partially cured epoxy resins and curing agents (N24). In addition, a standard test was developed for the examination of volatile migrants from polyester food trays to meet FDA requirements (N25)and a statistical comparison was made to evaluate test protocols used in the assessment of combustion product toxicity (N26).
0. MISCELLANEOUS TECHNIQUES Exterior durability continues to be of primary importance during the evaluation and testing of coating systems. Studies continue on the effects of substrate on coating performance ( O l ) ,and the reliability of durability testing (02). Specific coating applications were also investigated, including architectural (03),construction (04,05),automotive (06, 07)and use of tropical environments (08). The study of coating adhesion continues (09,OlO),as does the evaluation of polymer film permeability (011, 012). Testing of coating physical properties has led to publications on the evaluation of coating hardness (013), impact resistance (014), slime-inhibiting paints (015),fire retardation (016-018), and the measurement of coating thickness (019-021). Corrosion protection of paint and coating systems received special attention, with several review papers (022-026). In addition, studies were reported that used impedance (027032),potentiometry (033),and coulometry (034,035)as the measurement probe. Other properties of polymers and coatings are worthy of note, including the measurement of refractive index (036038), the use of a free volume microprobe to measure pigment dispersion (039), the measurement of particle size using sieving techniques (040),and the determination of interfacial tension (041).
P. MISCELLANEOUS MEASUREMENTS (INCLUDING PHYSICAL TESTS) The physical testing methodology discussed in this section includes methods for measuring the viscoelastic properties of coatings and polymers, measuring adhesion of coatings to substrates, and determination of cured film hardness. Dynamic mechanical measurement of coating viscoelasticity if growing in popularity, as evidenced by two review articles specific to coating characterization (PI,P2). Torsional braid analysis was also further developed during this period to provide less scatter in the data obtained (P3). Cross-linking mechanisms and rates continue as an important area for study using dynamic mechanical analysis. Specific studies were published dealing with: acrylic-melamine systems (P4-P6), high solids alkyds (P7), and epoxy-melamine container coatings (P8). Homo- and copolymer characterization was also investigated, as evidenced by papers on acrylic (P9-P12), urethane (P13-P15), epoxy (P16,P17), polycarbonate (P18), polysulfone (P19),and polyamide (P20) systems. One particularly interesting paper on the rheological evaluation of organoclay additives was published since the last review (P21). Adhesion of coatings to substrates, as well as the adhesion of polymers to metals, continues as a fruitful area of research. A book was recently published on the testing, analysis, and design of adhesive joints (P22). An extensive review of methodology for adhesion measurements (P23) was also of interest. Scratch (P24),impact (P25),and composite (P26) testing continue, as does the development of spectroscopic methods to characterize the adhesion properties of surfaces (P27). One interesting paper also compared the relationship between coating scratch adhesion and hardness (P28). Other hardness tests reported included Vickers indentation (P29), scratch tests (P30,P31), impact hardness (P32),and stone impact strength (P33). Finally, a new instrument was deANALYTICAL CHEMISTRY, VOL. 61,
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veloped to measure orange peel characteristics by the degree of distortion of a reflected image (P34).
ACKNOWLEDGMENT The author acknowledges Chemical Abstracts Service for providing access to STN International to aid in the literature search used in the preparation of this work. LITERATURE CITED A. INTRODUCTION
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NO. 12, JUNE 15, 1989 41 R
COATINGS (H35) Braun, Doetrich; Czerwinskl, Wojciech K., Makromol. Chem ., 1987, 788(lo), 2389-401. (H36) Hradil, J.; Plvcova, H.; Spevacek, J.; Svec, F., React. Polym., Ion Exch. Sorbents, 1988. 9(l), 51-8. (H37) Kobayashi, Minoru, J. Appl. Polym. Sci., 1988, 35(2), 299-309. (H38) Tacx, J. C. J. F.; Van der Velden, G. P. M.; German, A. L., J. Polym. Sci., Part A : Polym. Chem., 1988, 26(5),1439-56. (H39) Cheng, H. N., Polym. Mater. Sci. Eng., 1988, 58, 816-20. (H40) Watterson, A. C.; Olson, C. C.; Salamone, J. C., Polym. Prepr. (Am. Chem. Soc., Div. Polym. Chem.), 1988, 29(1), 164-5. (H41) Manders, William F.; Bellama, Jon M.; Johannesen. Rolf 6.; Parks, Edwin J.: Brinckrnan, Frederick, E., J. Polym. Sci., Part A : Polym. Chem., 1987, 25(12), 3469-77. (H42) Schllllng, F. C.; Bovey, F. A. Polm. Prepr. (Am. Chem. Soc., Div. Polym. Chem.) 1988, 29(1), 72-3. (H43) West, Robert; Maxka, Jim ACS Symp. Ser. 1988, 380(Inorg. Organomet. Polym.), 6-20. (H44) Wolff, Andrew R.; Maxka, Jim; West, Robert J. Polym. Sci., Part A : Polym. Chem. 1988. 26(3), 713-20. (H45) Wolff, Andrew R.; Nozue, Ikuo; Maxka, Jim; West, Robert J. Polym. Sci., Part A : Polym. Chem. 1988, 26(3),701-12. (H48) Carter, R.O., 111, Carduner, K.R.; Glerczak, C.A.; Van Dene, H. Eur. Polym. J. 1988, 24(8), 751-8. (H47) Horta, Arturo; Hernandez-Fuentes, Irmlna; Gargallo, Ligla; Radlc, Deodata Makromd. Chem., RapidCommun. 1987, 8(11), 523-8. (H48) Hvilsted, Soeren Bioi. Synth. Polym. Networks 1988, 243-54. Edited by: Kramer, Ole. Elsevler Appl. Sci.: London, UK. (H49) Carmlnati, G.; Cavalli, L. Anal. Appl. Spectrosc. [Proc. Int. Conf.], 1988, Meeting Data 1987, 344-5. Edited by: Creaser, C. S.; Davies, A. M. C. R. SOC. Chem.: London, UK. (H50) Carrion, Dominguez, J. L.; De la Guardla Cirugeda, M. Quim. Anal (Barcelona) 1987, 6(1), 78-82. (H51) Kretz, M.; Meurer, 8.; Spegt, P.; Weill, G. J. Polym. Sci., Part 6 : Polym. Phys. 1988, 26(8), 1553-68. Kulikov, Yu. M.; Kofanov, V. (H52) Varnavskaya, 0. 2.; Zaidenshteln. I.I.; I.; Orlov, M. S.; Tarvin, A. E. Ukr. Khim. Zh. (Russ. Ed.) 1988, 54(4), 365-8. (H53) Ebdon, John R.; Hunt, Barry, J.; O’Rourke, William T.; Parkin, John Br. Po@. J. 1988. 20(4), 327-34. (H54) Galinier, P.; Luarent, J. L.; Garrigue, F.; Mathieu, J. Analusis 1987, 15(8),404-10. (H55) Korolev, S. V.; Kuchanov, S. I.Vysokomol. Soedin., Ser. A . 1987, 29(1l), 2387-92. (H56) Ancelle, J.; Attias, A. J.; Bloch, 8.; Laupretre, F.; Monnerie, L. Makromol. Chem., Macromol. Symp. 1987, 9 , 123-9. (H57) Francillette, J.; Ma&, P. J.; Hoarau, P. A. Makromol. Chem., Macromol. Symp. 1987, 9 , 131-42. (H58) Borbely, J.; Keien, T., CrosslinkedEpoxies, Pro.,Discuss. Conf., 9th, 1987, Meeting Data 1988, 203-11. Edlted by: Sedacek, Blahoslav; Kahovec, Jaroelav. d&ruyer: Berlin, Fed. Rep. Ger. (H59) Glover, Donald J.; Duffy, James, V.; Hartmann, Bruce J. Polym. Sci., Part A : Polym. Chem. 1988, 26(1), 79-87. (H60) h k o p ’ e v , V. P.;Chrlatyakov, V. A.; Kukushkin. B. A,; Aieksandrov, K. N. Kozh.-Obuvn. Promat. 1988, (5), 58-60. (H61) Fry, Charles 0.; Und, Arthur C. McKKnolecules 1988, 21(5), 1292-7. (H62) Lonikar. S. V.; Sankar, S. S.; Rungslmontakul, N.; Fornes, R. E.; GiIbert, R. D. Polym. Prepr. (Am. Chem. Soc.. Dlv. Polym. Chem.) 1987, 28(2). 337-8. (H83) Schickert, P.; Ruehirnann, K. Acta Polym. 1987, 38(10), 562-8.
I. SURFACE ANALYSIS (11) Briggs, D. Surf. Sci. 1987, 189-190, 801-22. (12) Garbassi, F.; Occhiello, E. Anal. Chim. Acta 1987, 197, 1-42. (13) Harris, P. 0.; Trigg, A. D. Mater. Des. 1988, 9(3). 127-34. (14) Laout, J. C.; Roche, A.; Romand, M. Double Liason-Chim. Peint. 1987, 34 (385), I11-XI1 I,13-24. (15) Powell, C. J. S I A , Surf. Interface Anal. 1988. 11(1-2), 103-9. (16) Ishlda. Hatsuo Rubber Chem. Technol. 1987, 60(3), 447-54. (17) Watts, J. F.; Castle, J. E.; Hall, T. J. J. Mater. Scl. Lett. 1988, 7(2), 176-8. (18) Watts, J. F. S I A . Surf. Interface Anal., 1988 1987, 12(1-12), 497-503. (19) Batich, Christopher D. Appl. Surf. Sci. 1988, 32(1-2). 57-73. (110) Maartensson, Nils Treatise Mater. Sci. Technol. 1988, 27(Anal. Tech. Thin Films), 65-109. (111) Turner, Noel H. Anal. Chem. 1988, 60(12), 377R-387R. (I 12) American Society for Testing and Materials SIA , Surf. Interface Anal. 1988, 11(1-2), 112-13. (113) Nozakl, Massoki Kami. Parupu Gijutsu Taimusu 1987, 30(6), 1-7. (114) Rornand, M.; Charbonnier, M.; Sahakian, E. Congr. FATIPEC 1986, 18th (Vol.2/A), 77-107. (115) Watts, J. F. S w f . Coat. 1987, 1 , 137-87. Edited by Wllson, Alan D.; Nlcholson, John W.; Prosser, Havard J. Elsevier Appl. Sci.: London, UK. (116) Chaney, Robert; Barht, Guenter Fresenlus’ 2. Anal. Chem. 1987, 329(2-3), 143-8. (117) Lauritsen, F. R.; Onsgaard, J.; Vinternes, H. S I A , Surf. Interface Anal., 1988, 1987, 12(1-12), 198-202. (118) Wilcox, G. D.; Gabe, D. R.; Warwick, M. E. Trans. Inst. Met. finish. 1988, 66(3), 89-91. (119) Marchant, R. E.; Zhao, Q.; Anderson, J. M.; Hlltner, A. Polymer 1987, 28(12), 2032-9, (120) Schmldt. James J.; Gardella, Joseph A., Jr.; Sakati. Lawrence, Jr. Polym. Pfepr. (Am. Chem. Soc., Div. Polym. Chem.) 1988, 29(1), 301-2. (121) Ahmed, A.; Adnot, A.; Grandmaison, J. L.; Kaliaguine, S.; Doucet, J. Cellul. Chem. Technol. 1987, 21(5), 483-92.
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ANALYTICAL CHEMISTRY, VOL. 61, NO. 12, JUNE 15, 1989
(122) Dillard, John G.; Burtoff, Chuck Adv. Compos., Proc. Conf., 2nd 1986, 203-12. ASM: Metals Park, Ohio. (123) Laven, J.; Huisman, F. J.; Laliue, L. J.; Stein, H. N. Colloids Swf. 1988, 31, 385-405. (124) Powell, C. J. J. Res. Natl. Bur. Stand. (US.)1988, 93(3), 387-90. (125) Paterson, P. J. K. Mater. Forum 1987, 10(2). 144-53. (126) American Society for Testing and Materials SIA , Surf. Interface Anal. 1988, 77(1-2), 110-11. (127) American Society for Testing and Materials S I A , Swf.Interface Anal. 1988, 11(1-2), 114-15. (128) American Society for Testing and Materials S I A , Surf. Interface Anal. 1988, 71(1-2), 116-18. (129) American Society for Testing and Materials S I A , Surf. Interface Anal. 1988. 11f1-2). 119-24. (130) Kojima, %ao; Kurahashi, Masayasu J. Electron Spectrosc. Rebt. Phenom. 1988. 46131. 185-90. (131) Kumagal. k s a o : Ikeda, Satishi Kinmku Kyomen G#~tsu1987, 38(12), 564-70. (132) Choen, J. M.; Castle, J. E. Polm. Mater. Sci. Eng. 1988, 58, 37-43. (133) Clearfield, H. M.; Cote, G. 0.; Olver, K. A.; Shaffer, D. K.; Ahearn, J. S. S I A , Surf. Interface Anal. 1988, 71(6-7), 347-52. (134) Surganov, V. F.; Jansson, C.; Nielsen, J. G.; Morgen, P.; Gorokh, G.; Larsen, A. N. Electrochim. Acta 1988, 33(4), 517-19. (135) Bernius. Mark T.; Morrison, George H. Rev. Sci. Instrum. 1987, 58(10), 1789-804. (136) Kelly, Nicola; Kaiser, Uirich Res. D e v . 1987, 29(8),58-61. (137) Hearn, M. J.; Briggs, D. S I A , Surf. Interface Anal. 1988, 11(4), 198-213. (138) De Waele, Johan K. E., 1988, 295 pp. Avail. Univ. Microfilms Int., Order No. DA8716568. (139) Heinz. K. Prog. Surf. Sci. 1988, 27(4), 239-326. (140) Jitsumatsu, Tetsuji; Matsubara, HMeki Kobunshi Ronbunshu 1987, 44(10), 753-60. (141) Fisher, L. W.; Melpoider, S. M.; O’Rellly, J. M.; Rarnakrlshnan, V.; Wignail, G. D. J. Colloid Interface Sci. 1988, 123(1), 24-35. J. ULTRAVIOLET-VISIBLE SPECTROSCOPY
(J1) Sans Fonfria, R.; Garcia Raurich, J.; Puig Gasol, M. D.; Vaiero Ruiz, A. Pint. Acabadas I n d . 1987, 29(155). 87-8, 70. Lopata, Vaclav; Kepl, Jiri Prum. Potravin (J2) Bouskova, Olga; Zeman, I.; 1988, 39(3), 141-4. (J3) Stopa, Halina; Daniiczyk, Natalia Przem. Chem. 1987, 66(7), 353-4. (J4) Motorina, M. A.; Metelkina, E. I.; Shmagina, N. N. Plast. Massy 1987, (7), 19-20. (J5) Rodriguez, Marino L.; Fiol. Anolan; Siso, Jose A. Rev. Cubana Quim. 1988, 2(4), 57-64. Kulichenko, S. A. Zh. Anal. Khim. (J8) Pipenko, A. T.; Savaranski, L. I.; 1987, 42(6), 1493-501. (J7) Myers, G. E.; Koutsky, J. A. For. Prcd. J. 1987, 37(9), 56-60. (J8) Yaklakov, M. G.; Yaklakova, G. N.; Bogacheva, E. I.;Kul’chltskii, V. I. Pbsf. Massy 1988, (6), 55-6. (J9) Sovorova, L. A. Soversh. Khim. Tekhnol. Polufabrikatov iBumagi 1988, M. 84-8. (J10) Yu, W. C.; Huang, X. Y.; Sung, C. S. P. Polym. Prepr. (Am. Chem. SoC., Div. Polym. Chem.) 1988. 29(1), 532-3. ( J l l ) Hoyle, Charles E.; Kim, Kyu Jun; No, Y. G.; Nelson, G. L. J. Appi. Polym. Sci. 1987, 34(2), 763-74. (J12) Dickinson, P.; Sung, C. S. Polym. Prepr. (Am. Chem. Soc., Div. Polym. Chem.) 1988, 29(1), 530-1. (J13) Wachsman, Eric D.; Frank, Curtis W. Polymer 1988, 29(7), 1191-7. (J14) Hahry, Jean Louis; Larbl, Fadhel Ben Cheikh; Oudin. Pascal; Monnerie, Luclen Makromol. Chem. 1988. 189(9), 2117-24. (J15) Wong, Eric, K. L.; Richmond, Geraldine L. AIP Conf. Roc. 1987, 760(Adv. Laser Sci.-2). 805-7. (J16) Liu, Juwhan; Koenig, Jack L. Anal. Chem. 1987, 59(21). 2609-15. (J17) Fouassier, J. P. Congr. FATIPEC 1987, fSth(Vol. 3), 505-19. (J18) Fujiwara, H.; Kline, J. E. Tappl J. 1987, 70(12), 97-100. (J19) Karamyan, R. A.; Sarkisyan, V. V.; Markosyan. D. E.; Eritsyan, M. L. Pbst. Massy. 1987, (lo), 40-2. (J20) Schmelzer, H. Congr. F A T I E C 1986, 18th(Vol. VB), 807-21. (J21) Hofmeister, Franz Farbe Lack 1987, 93(10), 799-802. (J22) Adachl, M.; Miki, H.; Nakai, Y.; Kawaguchi, I.Opt. Lett. 1987, 12(10). 792-4. (J23) Brown, Wyn; Rymden, Roger Macromolecules 1987, 20(1 l), 2867-73.
K. SPECTROSCOPY-MISCELLANEOUS TECHNIQUES ( K l ) Day, David R.; Shepard. David D.; Wall, Amy S. I n t . SAMPE Symp. Exhib ., 1988, 33(Mater.-Pathway Future), 603-13. (K2) Hoffman, R. D.; Godfrey, J. J.; Kranbuehl, D. E.; Weller, L.; Hoff, M. J. Reinf. Pbst. Compos. 1987, 6(3). 223-33. (K3) Wuich, Walter Gummi fastern. Kunstst. 1987, 40(8), 434-5. (K4) Bokrenev, Yu. A. Lakokras. Mater. Ikh. Primen. 1988, (2), 33-5. (K5) Sirnpson, L. A. Polym. Paint Colour J. 1987, (Suppl.), 73-4, 76-7, 80, 98. (K6) Kranbuehi, D. E.; Delos, S. E.; Hoff, M. S.; Whitham, M. E.;Weller, L. W. A&. compos. Proc. Conf.. 2nd. 1988, 61-7. ASM: Metals Park, OH. (K7) Bidstrup, S. A.; Sheppard, N. F.; Senturla, S. D. Report, T.R-8; Order NO. AD-A177569/11GAR, 1966, 15 pp. (K8) Bidstrup, S. A.; Sheppard, N. F.; Senturia, S. D. Report, Order No. AD-A177558/4/GAR, 1987, 14 pp. (K9) Wetton, R. E.; Foster, G. M.; Smith, Vivien R.; Rochmond, J. C.; Neill. J. T. I n t . S A M E Symp. Exhib. 1988. 33(Mater.-Pathway Future), 1285-94. (KlO) Bauer, D. R.; Gerlock, J. L.; Dickle, R. A. Prog. Org. Coat. 1987, 15(3), 209-21.
COATINGS IK11) Nakamichi. Toshihko; Sakurai, Fumio; Okamoto, Shingo Shikizai Kyokiishi 1987, 60(10), 519-26. (K12) Croll, S. G. R W . 0fg. Coat. 1987, 15(3), 223-47. (K13) Liang, Ranty H.; Kim, Soon Sam; Yavrouian, Andre; Tsay, Fun Dow folym. Prepr. (Am. Chem. SOC., Div. folym. Chem.) 1988, 29(1), 124-5. -. (K14) Shiryaeva, G. V.; Bydanova, V. V.; Lmomnosova, N. V. f r o c . Tihany Symp. Radiat. Chem. 1987, 6th(2). 557-62. (K15) Kamachi, Mikihara A&. Powm. Sci. 1987, 82, 207-75. (K16) Roth, H. Klaus; Loepold, Detiev Makromol. Chem., Macromol. Symp. 1988, 18, 219-40. (K17) Okamoto. S.; Hikita, H.; Ohya-Nishiauchi, H. Congr. FATIPEC 1988, 18th(Vol. 4), 239-55. (K18) Busfield, K. W.; Garrett, R. W.; Hili, D. J. T.; O'Donnell, J. H.; Pomery, P. J. Polym. Repr. (Am. Chem. SOC.,Div. folym. Chem.) 1988, 29(1), 126-7. .. (Kl9) Kashiwabara, H. Radiat. fhys. Chem. 1988, 32(2), 203-8. (K20) Lyubchenko, L. S.; Kozhushner, M. A. Zh. Flz. Khim. 1988, 62(9), 2308-24. (K21) LeMheiser, Henry, Jr.; Deck, Philip D. Science (Washington, D.C.) 1988, 247(4870), 1176-81. (K22) Alten, David W.; Brooks, John S.; Bailey, Stephen; Taylor, Brian F. Appl. Organomet. Chem 1987, 7 (5),393-401. (K23) Krahn, Werner; Luckas, Michael; Luckas, Klaus fart. Part. Syst. Charact. 1988, 5(2), 72-6. 1988, 60(2), 138-9. (K24) Streib, Juergen Chem .-In..-Tech. (K25) Baker, James A.; Berg, John C. Langmuk 1988, 4(4), 1055-61. (K26) Oki M. Indian J . Chem. Sect. A 1988, 27A(5), 287-9. (K27) Mayo, Bret; Wau, James Int. S A M E Symp. Exhib. 1988, 33(Mater.-Pathway Future), 1751-60. (K28) Henriksen, P. N.; Gent, A. N.; Ramsier, R. D.; Alexander, J. D. SIA, Surf. Interface Anal. 1988, 7 7(6-7), 283-6. (K29) Ferrieu, F.; Stehle, J. L.; Bernoux, F.; Thomas, 0. Mater. Res. Soc. Symp . Roc. 1988, lO(Laser Part.-Beam Chem. Process. Microelectron.), 403-8. '
.
L. MICROSCOPY AND X-RAY TECHNIOUES
(L1) Goebel, R.; Stoecklein, W. Scanning Microsc. 1987, (1(3), 1007-15. (L2) Anon. Piastverarbelter 1988, 39(7), 86-7. (L3) Chewer, G. Dale J. Coat. Techno/. 1988, 60(762), 61-4. (L4) Wei, Lanhua; Xu, Jiansheng; Zhang, Shlyu Utrason. Symp . R o c . 1988, (l), 501-4. (L5) Cantow, Hans Joachim Interg. Fundem. folym. Sci. Technol.-Z [Proc. Int. Meet. Polym. Sci. Technol., Rolduc Polym. Meet.-21, 1988, Meeting Date 1987, 401-4. Edited by Lemstra, P. J.; Klelntjens, L. A. Elsevier: London, UK. (L6) Bartosiewicz, L.; Kelly, C. J. A&. folym. Technol. 1988, 6(2), 185-92. (L7) Quackenbush, Dale Tappi J. 1988, 71(5), 70-5. (LE) Kwlatkowski, Lech; Koziowski, Andrzej, ASTM Spec. Tech. fubl., 1987 1986, 947(Test. Met. Inorg. Coat.), 272-88. (L9) Ito, Kensaku; Nakamura, Hiroshi, Ise, Norio Koenshu Kyoto Daigaku Nlppon Kagaku Sen'i Kenkyusho 1987, 44, 85-93. (L10) Schroeder, Jeorg Farbe Lack 1988, 94(1), 9-14. (L11) Schroeder, Jeorg Rog. Org. Coat. 1988, 75(4), 337-53. (L12) Soboiewski, Wieslaw; Kosmowski, Henryk Biui. Inf.: Barwniki Srodki fomocnicze 1988, 32(1), 5-9. (L13) Slckfaus, K. E.; Berger, S. D.; Donald, A. M. J . Mater. Sci. 1988, 23(4), 1368-78. (L14) Thomas, Edwln L. Roc.-Annu. Meet., Electron Mlcrosc. Soc. Am. 1987, 45th, 422-5. (L15) Wang, Yingang; Huang, Dongyun; Gai, Xluzhen Gaofenzi Xuebao, 1988, (1). 59-62. (L16) Briber, Robert M. Roc.-Annu. Meet. Electron Microsc. SOC. Am. 1987, 45th, 506-9. (L17) Howell, Barbara F.; Reneker, Darrell H. Mater. Res. SOC. Symp. R o c . 1988, 175(Specimen Prep. Transm. Electron Microsc. Mater.), 155-60. (L18) Joseph, Eugene, G.; Aguilera, Jacqueline M.; Houie, Judith R. folym. frepr. (Am. Chem. SOC., Div. folym. Chem.) 1987, 28(2), 345-6. (L19) Schrader, Sigurd; Li, Xuan; Guo, Fanxiu; Liu, Yong; Luo, Jijiang; Xu, Duanfu Makromol. Chem., Rapid Commun. 1988, 9(9), 597-601. (L20) Talmon, Yeshayahu Roc .-Annu. Meet ., Electron Mlcrosc. Soc. - Am. 1987, 45th, 496-9. (L21) Onewill, R. H.; Satgurunathan, R. Col/oid folym. Sci. 1987, 265(9), 845-53 - ._ (L22) Shaffer, 0. L9; El-Asser, M. S.; Vanderhoff, J. W. Roc.-Annu. Meet., Electron Microsc. Soc. Am. 1987, 45th., 502-3. (L23) Murata, Masato Yosetsu Gakkaishi 1988, 57(2), 85-7. (L24) Sawyer, Linda C. f r o c .-Annu. Meet ., Electron Microsc. Soc. Am. 1987, 45th, 426-9. (L25) Berry, V. K. Roc.-Annu. Meet., Electron Microsc. Sac. Am. 1987, 45th. 468-9. (L26) Krause, S. J.; Adams, W. W.; Kumar, S.; Reilly, T.; Suzuki, T. froc.Annu. Meet., E k t r o n Microsc. Am. 1987, 45th, 466-7. (L27) Berry, V. K. Scanning 1988. 70(1), 19-27. (L28) Price, C. W.; McCarthy, P. L. Scanning 1988, 10(1), 29-36. (L29) Xiao, H. X.; Frish, K. C.; AI-Katib, S. ACS Symp. Ser. 1988, 367(Cross-Linked Polym.), 31 1-23. (L30) Mazurek, W.; Silva, V. M. Rep.-Mater. Res. Lab. (Aust.) 1987, MRL-R-1096, 26 pp. (L31) Short, N. R.; Dennis, J. K.; Agbonlahor, S. 0. Trans. Inst. Met. Finish. 1988, 66(3), 107-1 1. (L32) Eckert, Richard Mikrochim. Acta 1987, 1(1-6), 193-200. (L33) Tanaka. Takeyuki Toso to Toryo 1988, (434), 39-47. (L34) Palley, Igor; Signotelli, Anthony, J. J. Adhes. 1988, 25(3), 161-7. (L35) Possart, W. Int. J. Adhes. Adhes. 1988, 8(2), 77-83.
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(L36) Robinson, I . K. Aust. J . fhys. 1988, 41(3), 359-67. (L37) Choy, C. L; Nakafuku, C. J . folym. Sci., Parts: folym. fhys. 1988, 26(4), 921-34. (L38) Takahara, Atsushi; Kajiyama, Titsato; Sato, Mamoru folym. Commun. 1988, 29(7), 194-5. (L39) Lad, Saharsha M9; Kane, P. P., Nucl. Inshum. Methods fhys. Res., Sect. B 1988, 634(1), 113-17. M. THERMAL ANALYSIS
(Ml) Kelm, J.; Neubert, D.; Sickfeld, J. Congr. F A T I E C 1986, lSth(Vol. 2/B), 731-85. (M2) Degterov, P. P. Derevoobrab. from.-st. 1988, (3), 16-17. (M3) Jozavi, Hooshang; Sancaktar, Erol J. Adhes. 25(3), 185-201. (M4) Katlme, Issa; Nuno, Terese; Radic, D. Thermochim. Acta 1988, 724, 263-75. (M5) Nuno, T.; Katime, I.Elhuyar 1987, 13(2), 107-17. (M6) Katime, Issa; Nuno, Teresa Thermochim. Acta 1988, 124, 247-61. (M7) Shablygin, M. V. flast. Massy. 1987, (12), 49-50. (ME) Hinrichsen, G.; Jahr, H. J.; Springer, H. folvm. Bull. (Berlin) 1988, 19(2), 155-9. (M9) Fawcett, Tim CHEMTECH 1987, 17(9), 564-9. (M10) Housh, Riitta Kern.-Kemi 1987, 74(10), 868-72. ( M l l ) Franiau, R. P. faintindia 1987, 37(9), 33-8. (M12) Yue, C. Y. J. Mater. Sci. Lett. 1988, 7(8), 811-13. (M13) Hatakeyama, Tatsuko; Nakamura, Kunio; Hatakeyama, Hyoe Thermchim. Acta 1988. 123. 153-61. (M14) Mijangos, Carmen; Martinez, Gerardo; Millan, Jose Luis Makromol Chem. 1988, 189(3), 567-72. (M15) Johari, G. P.; Heilbrucker, Andreas; Mayer, Erwin J. folym. Scl., f a r t 8 : Polym. fhys. 1988, 26(9), 1623-30. (M16) Liu, H.; Armand, J. Y.; buzon, J.; Vergnaud, J. M. Thermochim. Acta 1988, 126, 81-92. (M17) Gobbe, C.; Bazin, M.; Gounot, J.; Dehay, G. J. fo/ym. Sci., f a r t 6: Po/ym. phys. 1988, 26(4), 857-64. (M18) Khanna, Y. P.; Taylor, T. J.; Chomyn, G. folym. Eng. Sci. 1988, 28(16), 1034-41. (M19) Kobayashi, Kiuoshi HSMf Int. J., Ser. 2 1988, 37(1), 1-8. (M20) Bosma. Martin; Ten Brike, Gerrit; Ellis, Thomas S. Macromolecules 1988, 27(5), 1465-70. (M21) Frushour, B. G.; Sabatelli, D. C. J. Appl. folym. Sci. 1988, 36(6), 1453-65. (M22) Lin. Jen Lien; Roe, Ryong Joon Polymer 1988, 29(7), 1227-32. (M23) Shibasaki, Yoshio; Fukuda, Klyashige, Thermochim. Acta 1988. 123, 191-9. (M24) Bittrich, H. J.; Hoering, S.; Steinau, U. J. Acta folym. 1987, 38(10), 584-5. (M25) Chang, Shu Sing J. Therm. Anal. 1988, 34(1), 135-54. (M26) Heise. M. S.; Martin, G. C. J. folym. Sci., f a r t C: folym. Lett. 1988, 26(3), 153-7. (M27) Patel, Ravji D.; Patel, Ranjan G.; Patel, Vithal S. 81.folym. J. 1987, 19(1), 37-41. (M28) Patel, Rasmika H.; Patel, Ranjan G., Angew. Makromol. Chem., 1988, 167, 89-96. (M29) Schiraldi, Alberto; Pezzati, Elisabetta; Baldini, Primo Thermochim Acta 1987, 120, 315-23. (M30) Simon Soerensen, Helle; Naerum, Lars Congr. F A T I E C 1988. 78th (Vol. 4), 257-70. (M31) Thakkar, J. R.; Patel, R. G.; Patei, V. S. Eur. folym. J. 1987, 23(10), 799-802. (M32) Lee, Sung Nung; Yoo, Wu Bin fo/ym. fng. Sci. 1987, 27(17), 1317-22. (M33) Patel, Rasmika H.; Patel, Ranjan G. Angew. Makromol. Chem. 1988, 161,89-96. (M34) Patel, Ravji D.; Patel, Ranjan G.; Patel, Vithai S. Angew. Makromol. Chem. 1987, 155, 57-66. (M35) Steinmann, B. Crosslinked Epoxies, R o c . Discuss. Conf ., 9th, Meeting Date 1986, 117-30. Edited by Sedlacek, Blahoslav; Kahovec, Jaroslav. de Gruyter: Berlin, Fed. Rep. Ger. (M36) Thakkar, Jatin R.; Patel, Ranjan G.; Patel, Vithal S. Br. Polym. J. 1988, 20(1), 49-51. (M37) Avella, M.; Martuscelli, E.; Volpe, M. G. J. Therm. Anal. 1988, 34(2), 441-50. (M38) Kloosterboer, J. G.; L i p , G. F. C. M. ACS Symp. Ser. 1988, 367 (Cross-Linked Polymers), 409-26. (M39) Ng, Hendra; Manas-Zloczower, Ica folym. Mater. Sci. Eng. 1988, 58, 1092-8. (M40) Salla, J. M.; Martin, J. L. Thermochim. Acta 1988, 126, 339-54. (M41) Van de Werff, A.; Schippers, J. Congr. F A T I E C 1988, 18th (Voi 216). 695-712. (M42) Malavisic, T.; Osredkar, U.; Anrur, I.; Vizovisek, I.J. Macromol. Sci. Chem. 1988, A25(1), 55-64. (M43) Fullerton, Rhonda; Roylance, David; Allred, Ronald; Acton, Adra f o lym. Eng. Sci. 1988, 28(6), 372-6. (M44) Arora, Pavin 6.; Patel, Vithal S.; Patel, Shanti R. Br. folym. J. 1987, 19(5), 429-33. (M45) Patel, Ravji D.; Patel, Ranjan G.; Patel, Vithal S.; Pearce. E. M. J. Appl. Polym. Sci. 1987, 34(7), 2583-9. (M46) Abadie, Marc J. M.; Appelt, Bernd K Bull. SOC. Chim Fr. 1988, 1 , 20-24. (M47) Aiiept. B. K.; Abadie, M. J. M. Polym. Eng. Sci. 1988, 28(6), 367-71. (M48) Cox. Bobert J. Polvm. ReDr. (Am. Chem. Soc.. Dlv. folym. Chem.) ' 1988, 29(1), 122-3. (M49) Hoyle, Charles E. Proc. Water-Borne Higher-Solids Coat. Symp. inaa. 15th. 521-5. . (M50) Theweieitl Elke; Kunze, Wolfgang Kunststoffe 1987, 77(9), 870-3. (M51) Thomas, Loenard C. Res. Dev. 1987, 29(11), 86-90.
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COATINGS (M52) Sawan, Samual P.; Tsai, Yi Guan; Huang, Horng Yih Hsu, Tsun Min Polym. Prepr. (Am. Chem. SOC.. Div. Polym. Chem.) 1988, 29(1), 297-8. (M53) Zhang. Xinsheng; Shi, Lianghe; Li, Shuquing; Lin, Yizhen Polym. D e grad. Stab. 1988, 20(2), 157-72. (M54) Jeon, Seung Ho; Ree, Taikyue J. Polym. Sci., Part A : Polym. Chem. 1988, 26(5), 1419-28. (M55) Siegmann, A.; Cohen, D.; Narkis, M. Polym. Eng. Sci. 1987, 27(15), 1187-94. (M56) Ryan, Anthony J.: Stanford, John L.; Still, Richard H. Br. Poly. J. 1988, 20(1), 77-83. (M57) Khabenko, A. V.; Dlomatov, S. A. Pbst. Massy. 1987, (9), 52-4. (M56) Bhuyan, K.; Dass, N. N. J . Indian Chem. SOC. 1988. 65(5), 342-5. (M59) Cascaval, C. N.; Hurduc, N.: Poinescu I.C. J. Therm. Anal. 1988, 34(1), 311-17. (M60) Haken, J. K.; Tan, L. J. Polym. Sci., Part A : Polym. Chem. 1988, 26(5), 1315-22. (M61) Ichlmura, Katsuhiko; Ohta, Hiroshi; Tajima, Takahiro; Okino, Takayuki Mikrochim. Acta, 1987 1988, l(1-6). 157-61. (M62) Farr, Michael P.; Harrison, Ian R Po/ym. Prepr. (Am. Chem. SOC., Div Polym Chem .) 1987, 28(2), 302-3. (M63) Farling, Michael S.Rubber World 1988, 197(4), 20-3. (M64) Cambon, C.; Loiseau, B. Double Liason Chim. Peint. 1987, 34(385), 33-8. (M65) Wieblodt, Richard C.; Lowry, Steven R.; Rosenthal J. Mikrochim. Acta 1987, l(1-6) 179-82. (M66) Chiang, Wen Yen; Chiang, Wen Chang J. Appl. Po/ym. Sci. 1988, 35(6), 1421-32. (M67) Koscielecka, Alicja: Dzierza. Wieslaw Angew. Makromol. Chem. 1987, 152, 41-53. (M68) Chiang, Wen Yen; Chiang, Wen Chang J . Appl. Polym. Sci. 1988, 35(6), 1433-9. (M69) Jones, E. G.; Pedrick. D. L.; Goldfarb, I.J. Polym. Eng. Sci., 1988, 28(16), 1046-51. (M70) Redfern, John Am. Lab. (Fairfield, Conn .) 1988, 20(3), 26, 28, 30-3. (M71) AI-Jabri, N.; Khalef. Moald N.; Adam, Gerogua A. Poly.-Pbst. Techno/. Eng. 1988, 27(3), 351-64. (M72) Hirschler, M. M.; Smith, G. F. Chem. Phys. Process Combust. 1987, 63/1-63/4. (M73) Parrlsh, D. E.; Petreiia, R. V.; Beal, G. E. Proc. I n t . Conf. Fire Saf. 1988, 13, 312-25. (M74) Paul, K. T. Prog. Rubber Pbst. Technol. 1987, 3(2), 23-43. (M75) Thomson, H. E.; Drysdale, D. D. Fire Mater. 1987, 11(4), 163-72. (M76) Subira, F.; Vairon, J. P.; Sigwalt, P. Macromolecules 1988, 21(8), 2339-46. (M77) Kalos, Alexander N. Polym. Mater. Sci. Eng. 1988, 5 8 , 782-6.
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N. ENVIRONMENTAL AND INDUSTRIAL HYQIENE (Nl) Kristensson, J.; Beving, H. Comm. Eur. Communities, [Rep.] EUR 1987, EUR 10555, Dlffusive Sampling, 71-4. (N2) Glgulere. William; Lewis, David; Baseit, Randall C.; Chang, Randall J. Anal. r ~ x l c d 1988, . 12(3), 168. (N3) Lehmann, E.; Auffarth, J.; Haeger, J. Comm. Eur. Communnies, [Rep.] EUR 1987, EUR 10555, Diffuslve Sampllng, 403-6. (N4) Klimisch, H. J. Arch. Toxicol. 1988, 61(5), 411-16. (N5) Coutant, Robert W.; Keigley, G. William Anal. Chem. 1988, 60(22), 2536-7. (N6) Michael, Larry C.; Pellizzari, Edo D.; Wiseman, Roger W. Environ. Sci. Technol. 1988, 22(5), 565-70. (N7) Bruchet, Auguste; Aiben, Katherine; Ding, Wang Hseln; Aldous, Kenneth Pr0c.-Water Qual. Technol. Conf., 1987 1986, I4(Adv. Water Anal. Treat.), 905-16. (N8) Mosesman, Neil H.; Betz, Wllliam R.; Corman, Scott D. LC-GC 1988, 6(4), 328, 332, 334, 336. (N9) Wylie. Philip L., Proc.-Water Qual. Technol. Conf., 1987 1988, 14(Adv. Water Anal. Treat.), 185-202. (N10) Wylie, Phllip L. J.-Am. Water Works Assoc. 1988, 80(8),65-72. (N11) Gryder-Boutet, Donna E.; Kennish, John M. Proc.-Water Qual. Conf., 1987, 1988, 14(Adv. Water Anal. Treat.), 679-88. (N12) Davis. Charles 6.: McNichols, Roger J. Ground Water 1988. 26(5), 849-50. (N13) Gibbons, Robert D. Ground Water 1988, 26(5), 650-1. (N14) Kunkel, E. Tenside, Surfactants, Deterg. 1987, 24(5), 280-5. (N15) Howe, G. E.; Jayanty, R . K. M.: Jackson, M.; Rlley, C. E.; McAlister, G. D. JAPCA 1988. 38(7), 907-13. (N16) Rhoderlck, George C.; Zielinski, Walter L., Jr. Anal. Chem. 1988, 60(22), 2454-60. (N17) Leinster, P.; Irvlne, D.; Evans, M. J. Comm. Eur. Communities. [Rep .] EUR 1987, EUR 10555, Diffusive Sampling, 209-22. (N18) Samiml, Behzad S. Comm. Eur. Communities, [Rep.] EUR 1987, EUR 10555, Diffusive Sampling, 166-9. (N19) Shields, Helen C.; Weschler, Charles J. Proc. APCA Annu. Meet. 1987, 80th(Vol. 5). 87183.9, 15 pp. (N20) Crist, H. L. Report EPA/6001D-87/327; Order No. PB88-125265, 1987, 18 pp. (N21) Bertonl, G.; Fratarcangeli, R.; Libertl, A,; Rotatori. M. Comm. Eur. Communities, [Rep .I EUR 1987, EUR 10555, 63-6. (N22) Podolak, George E.; Cassidy, Richard A.; Esposito, George G.; Kippenberger, Donald J. ASTM Spec. Tech. Pub/. 1987, 957(Sampling Atmos. Meas.), 203-12. (N23) Molina. Daniel; Abell. Martin T. Am. Ind. Hyg. Assoc. J . 1987, 48(10), 830-5. (N24) Herrick. Robert F.; Smith. T. J. Scand. J . Work, Environ. Heafih 1988, 14(Suppl. 1, Proc. Finn-US Jt. Symp. Occup. Saf. Health Swed. Participation, 4th, 1988). 31-2.
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(N25) Risch, Sara J.; Reineccius, Gary A. ACS Symp. Ser., 1988 1987, 365(Food Packag. Interact.), 170-80. (N26) Debanne, S.M.; Hailer. H. S.; Rowiand, D. Y. J . Fire Sci. 1987, 5(6), 416-34. 0. MISCELLANEOUS TECHNIQUES
(01) Gozdan. Walter J. Surf. Coat. Aust. 1988, 25(4), 6-10. (02) Cutrone, L.; Mouiton, D. V. J . Oil Colour Chem. Assoc. 1987, 70(6). 222-8. (03) Misra, J. P.; Raza Ali, M.; Sivasamban, M. A. Paintindia 1988, 38(4), 15-21. (04) Appieman, Bernard R. Polym. Mater. Sci. 1988, 5 8 , 412-16. (05) Robinson, Alan Surf. Coat. Aust. 1988. 25(3), 15-18. (06) Asawa, Tatsuji; Arakawa, Takashi Zairyo Kagaku 1987, 24(1), 28-35. (07) Wootton, Alan B. Pigm. Resin Technol. 198Sg 17(6). 4-5. (06) Davis, A.; Howse, D.; Yarrow, A. S. Polym. Mater. Sci. Eng. 1988, 58, 60-4. (09) Boiziau, C.; Lecayon, G. S I A , Surf. Interface Anal., 1988 1987, 12(112). 475-85. (010) Doblhofer, Karl; Eiselt, Irmgard Corros. Sci. 1987, 27(9), 947-56. (01 1) Bagda, E. Farbe Lack 1988, 94(1), 15-18. (012) Mazarov, V. G.; Gromov, A. N.; Minina. E. M.; Evlampieva, L. A,; Manin, V. N. Zavod. Lab. 1988, 54(6), 65-7. (013) Riesenberg, Evelin; Maertin, Rolf; Resenberg, Rainer Pbste Kautsch 1987, 34(8), 292-3. (014) Sickfeld, Juergen; Raabe, Hans Joachim Materia@rtwfung 1987, 29(78). 203-9. (015) Cinti, G.; Gombach, M. L.; Renni, L. Congr. FATIPEC 1986, IB?h(Vol. l/B), 441-59. (016) Camino. G.; Costa, L.; Casorati, E.; Bertelli, G.; Locatelli, R. J . Appl. Polym. Sci. 1988, 35(7), 1863-76. (017) Eckhoff, Rolf K.; Pedersen, Geir H.; Arvidsson, Tommy J. Hazard. Mater. 1988, 19(1), 1-16. (018) Roesler, Walfried Hoiztechnologie 1987, 28(5), 230-4. (019) Latukhin, D. V.; Valyus. N. A.; Ryabov. V. M.; Sitnikov, L. L.; Masy78-82. chev, V. I.Defektoskopiya 1988, (l), (020) Louie, Michael; Christy, Ronald Thin Solid Films 1987, 154(1-2), 291-9. (021) Nix, Hans F. Metalloberflaeche 1987. 41(12), 580-2. (022) Bubb, Michael Corros. Australas 1887, 12(2), 5-7. (023) Igetoft, Lars; Pedersen, Helli Faerg Lack Scand. 1987, 33(10), 157-60, 162-3. (024) Martin. Johnathan W.; McKnight, Mary E.; Tinh, Nguyen Polym. Mater. Sci. Eng. 1988, 58, 410-11. (025) Plog, H. Galvanotechnik 1988, 79(3), 755-61. (026) Poster, Horst; Schneider, Andreas Korrosion (Dresden) 1987, 18(2), 104- 10. (027) Benyi, G.; Horkay, R.; Janazik, F. Congr. F A T I E C 1987, 18fh(Vol. 3), 15-39. (026) Camara, J. L.; Margarit, I.C.; Mattos, 0. R. Rev. Iberoam. Corros. Prof. 1987, 18(1), 43-8. (029) Di Sarli, A. R.; Giudice, C. A. Corros. Prev. Confrol 1988, 35(4). 99-107. (030) Hajas, Janos Farbe Lack 1988, 94(3), 190-3. (031) Picaud, T.; Pebere, N.; Duprat, M.: Dabosi, F. Met: Corros.-lnd. 1987, 62(747-748). 345-52. (032) Wang, Yar Ming; Radovic, Dusanka Proc. AESF Annu. Tech. Conf., 75th, 1988, H - 5 , 25 pp. (033) Molera, P.; Arias, C.; Archiaga, P. Pint. Acabados Ind. 1987, 29(160), 54-6. (034) Di Sarli, A. R.; Aldasoro, R. M.; Paus. G. F.; Podesta, J. J. J. Coat. Techno!. 1988. 60(760), 41-6. (035) Panasenko. S.A.; Makarchenko, N. N.; Oleshchenko, N. N.; Bitchenko, 0. A.; Grishchuk, V. I.; Danilov, F. I. Fiz.-Khim. Mekh. Mater. 1988, 24(3). 25-7. (036) Chirica, Ligia; Dorohoi, Dana; Pop, V.; Strat, M. An. Stint. Univ. " A / . I. Cuza." lasi, Sect. I b , 1985, 31, 53-8. (037) Devon, Michael J., Rudin, Alfred J . Appl. Polym. Sci. 1987, 34(2), 469-76. (038) Mills, N. J. Encycl. Po/ym. Sci. Eng. 1987, 10. 493-541. Edited by Kroschwitz, Jacqueline I.Wiley: New York. (039) Mayo, Bret; Pfau, James P.; Sharpe, Robert E. J . Coat. Technol. 1987, 59(750). 23-7. (040) Schnabel, Werner Farbe Lack 1987. 93(12) 1001-3. (041) Yu, Hyuk Polym. Mater. Sci. Eng. 1988, 58, 629-33.
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P. MISCELLANEOUS MEASUREMENTS
(Pl) Di Bari, George A., ASTM Spec. Tech. Publ.. 1987 1988, 947(Test. Met. Inorg. Coat.). 4-10. (P2) Skrovanek, Daniel J.; Schoff, Clifford K. Prog. Org. Coat, 16(2). 135-62. .. .~ (P3) Sakeiiauiou, Panagiotis; White, Eric, F. T.; Rowe, Raymond C. 61.PoIym. J . , 1987, 19(1), 73-82. (P4) Hill, L. W.; Kozlowski, K. Prm. Wat8f-BOf~ High-Sdids Coat. Symp. 1987, 14fh, 175-93. (P5) Hill, L. W.; Kozlowski. K. J . Coat. Technol. 1987, 59(751), 63-71. (P6) Takahashi, Seiichi, Okoshi, Noboru; Matsumoto, Takanwl; Ikeda, Takenori J . Appl. Polym. Sci. 1988. 36(3), 613-33. (P7) Beckmann, K. K.; Green, C. D.; Winters, B. K.; Whlte, L. D.; Lamberton. J. G. Proc. Water-Borne Higher-Solids Coatings Symp ., 1987, 14th, 298-313. (P8) Buehner, R. W.; Cooper, E. J. Proc. Water-Borne Higher-SolMs Coatings Symp. 1988, 15th, 362-72. (P9) Cavaille, J. Y.; Jourdan, Perez J. Makromol. Chem. Macromol. Symp. 1988, I6(Europhys. Conf. Macromol. Phys., 18th. 1987), 341-60.
Anal. Chem. 1989, 61, 45R-84R (PIO) Gandhi, Khushroo; Salovey, R. Polym. Eng. Sci. 1988, 28(14), 877-87. (P11) O.Connor, Kevin M.; Oiler, E. Bruce Proc. Water-Borne Higher-Solids Coat. Symp. 1987, 14ih, 143-54. (P12) Rogler, W.; Markert, H.; Stapp, B.; Zapf, R. Polym. Prepr. (Am. Chem. SOC.,Div Polym. Chem.) 1988, 29(1), 528-9. (P13) Cowie, John M. G.; Wu, Hak H. Polymer 1988, 29(5), 934-7. (P14) Demarest, C.;Moore, R. Polyurethanes World Congr. Proc. FSKISPI 1987, 391-7. Technomic: Lancaster, PA. (P15) Hartmann, Bruce; Duffy, James V.; Lee, Gilbert F.; Balker, Edward J. Appl. Polym. Sci. 1988, 35(7), 1829-52. (P16) Prime, R. B.; Burns, J. M.; Karmin, M. L.; Moy, C. H.; Tu, H. B. J. coat. rechnoi. 1988, 60(761), 55-60, (P17) Shut, N. I.; Bartenev, G. M.; Sichkar, T. G. Acta Polym. 1987, 38(8), 477-82. (PIE) Sichina, W. J. Am. Lab. (Fairfield, Conn.) 1988, 20(1),42, 44-6, 48, 50-2. (P19) Nacho, E.; Alberdi, J. M.; Alegria, A,; Colmenero J. Makromol. Chem. Macromol. Symp. 1988, 20/2(Intl. Symp. Polym. Mater., 1987), 451-60. (P20) Alberola, Nicole J. ADP/. Polym. Sci. 1988, 36(4), 787-804. (P21) Tso, Su C.;Rohn. Charles R o c . Water-Borne Higher-Solids Coat. Symp. 1988, 15th, 244-51.
(P22) Johnson, W. S.,Editor, ASTM Spec. Tech. Publ. 1988, 981(Adhesively Bonded Joints), American Society For Testing and Materials: Philadelphia, PA; 310 pp. (P23) Mittal, K. L. ASTM Spec. Publ., 1987 1986, 947(Test. Metal. Inorg. Coat.), 343-62. (P24) Burnett, P. J.; Rickerby, D. S. Thin Solid films 1988, 157(2), 233-54. (P25) Hirschbuehler, Kevin R., ASTM Spec. Tech. Publ. 1987, 937(Toughened Compos.). 61-73. (P26) Gent, A. N. J . Adhes. 1987, 23(2), 115-22. (P27) Romand, M.; Gailard, F.: Charbonnier, M.; Roche, A. J . Adhes. 1987, 23(1), 1-19. (P28) Burnett, P. J.; Rickerby, D. S. Thin Solid Films 1987, 154(1-2), 403-16. (P29) Trautz. S.; Tutschky, G.; Rathjen, D. Wiss. Tag. Tech. Univ. KarlMarx-Stadt 1987, 8 ,("Anorg. Schutzschichten" Oberflaechenschutz Verschleiss), 136-41. (P30) Behncke, H. H. Materialpruefung 1988, 30(7-8), 239-42. (P31) Steinmann, P. A.; Tardy, Y.; Hlntermann, H. E. Thin Solid Fllms 1987, 154I1 -21. 333-49. (P32) fur&, S., Proc. Rubber Plast. Technol. 1988, 4(2), 34-47. (P33) Harlfinger, Rudolf Farbe Lack 1988, 94(3), 179-83. (P34) Matsuta, Morihiro J. Coat. Technol. 1987, 59(754), 61-4.
Food Albert K. Athnasios,* Anthony F. Gross, and Peter S. Given, Jr. Nabisco Biscuit Company, East Hanouer, New Jersey 07936-1944
A. ADDITIVES Kvasnicka ( A I ) developed a capillary isotachophoresis
technique to analyze aspartame sweetener in beverages, yogurt, and coffee. HPLC for saccharine, and other food additives, in liquid foods was developed by Kobayashi et al. (A2). Klein and Stoya (A3)utilized capillary isotachophoresis to assay for acesulfame K in juices, beverages, and aqueous extracts of semisolid foods. A ternary solvent system that yields low IR background was used by Galensa et al. (A4) to analyze benzoylated saccharides in food extracts by HPLC coupled to FT-IR flow analysis. An extraction scheme and spectrophotometric method (314nm) for cyclamate measurement were described by Greve and Bonifer (A5). Matsunaga et al. (A6) determined aspartame and saccharine simultaneously using HPLC. Aspartame in foods was measured by Kataoka et al. (A7) using GC. Aspartame and saccharine were determined by Williams (A8) using HPLC. Timokhina et al. (A9)utilized a conventional amino acid analyzer to separate aspartame from aspartylphenylalanine with sodium citrate buffer. Mono-, di-, and triisopropyl citrates in butter and milk powder were determined by Tsuji et al. (AIO) by GC. Detection limit for all esters was l wg g. Preservative acids (e.g., sorbic, benzoic, propionic, salicy ic, p-hydroxybenzoic, and undecylenic acid) were determined by TLC by Krull and Matissek (A11 ) . Seven preservatives were simultaneously measured by Shiroma and Oshiro (A12) using HPLC. A sensitive screening method for acidic preservatives in foods was developed by Haensel and Stroemmer (A13). Propionic, sorbic, and benzoic acids were derivatized with dansyl semipiperazide, separated by TLC, and detected by fluorescence scanning; less than 20 ng could be detected. The packagin film plasticizer, di(Zethylhexy1) adipate was detected in fools by Startin et al. (A14) using capillary GC isotope dilution mass spectrometry. Mongeau and Brassard (A15) compared several methods for determining soluble and insoluble dietary fiber, including the AOAC method. Their findings indicate that the NDF and soluble fiber method took less operator time than other methods, and yielded comparable results. The molecular weight distribution of pectins was profiled by Deckers et al. (A16) using size exclusion chromatography; various calibrations were obtained for different pectins (high methoxyl and low methoxyl). Acidic, nonnutritive sweetener, and flavor additives in different foods were analyzed using HPLC by Veerabhadrarao et al. (A17). The use of formaldehyde in
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0003-2700/89/036 1-45R$06.50/0
cheese production was monitored by Restani et al. (A18) by applying [14C]formaldehyde to identify a protein-reaction product resolved by isoelectric focusing, PI6.7. A device for remote measurement and control of C 0 2 in beverage liquids was developed by Seiden et al. (A19). The device operates on isolated sample aliquots using a temperature-pressure algorithm after equilibration, to avoid fluctuating line pressures. Antioxidant activity was measured by Hirayama et al. (A2O)using an oxygen electrode. Initial rates of oxygen uptake after sample extract addition were used to calibrate antioxidant effectiveness. Three methods for determination of antioxidant effectiveness in oils, sesamol dimer, SD method, and POV method, were compared by Kikugawa et al. (A21); the SD method yielded results comparable to the POV method and required significantly less sample (>lo mg). MerinoTeillet and Leon-Gonzalez (A22) improved the picrate method for the spectrophotometric determination of nonionic surfactants. Rosin ester gum emulsifiers in fruit juices were determined by Tonogai et al. (A23) by GC. Detection of polar substances (emulsifiers) in frying oils based on silica gel separation of polar fractions was devised by Dieffenbacher and Martin (A24);TLC analysis of the polar fraction was used to screen column separation efficiency and range of polar additives. Benzoic acid in milk was measured by De la Riva Reyero (A25) using HPLC. Protein addition to mushrooms (ovalbumin) was detected by Breton e t al. (A26) using an ELISA. Immunoblotting showed comparable results to the ELISA test obtained at the 1.0and 5.0% contamination range.
B. ADULTERATION, CONTAMINATION, DECOMPOSITION Mycotoxins in Foods is a recently published book edited by Krogh ( B l ) which features chapters by several well-known mycotoxin researchers. Newsome (B2) reviewed the advantages of immunochemical methods and their application in determining natural constituents and contaminants in food. Muecke (B3) reviewed the detection of potential food contaminants by industrial chemicals and their breakdown products and proposed a monitoring program. Page (B4) published a review with 24 references of pattern recognition methods for the determination of food composition and adulteration. Reviews of mycotoxins are the following: Shepherd (B5) compiled HPLC methods for aflatoxins, ochratoxins, fusarium toxins, patulin, ergot alkaloids; GC methods were reviewed 0 1989 American Chemical Society
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