Anal. Chem. 1987, 59, 114R-119R
Rubber Anoop Krishen Analytical and Materials Testing, The Goodyear Tire & Rubber Company,’ Akron, Ohio 44305
This review covers methods for identification, characterization, and determination of rubber and material in rubber. Literature that became available to the author between November 1984, the end of the period covered by the last review in the series (I),and December 1986 is reviewed. Abbreviations recommended in ASTM Designation D1418-85 have been used. These are listed in Table I.
GENERAL INFORMATION The American Society for Testing and Materials published their latest annual edition of test methods for rubber in 1985 (2). Determination of surface tension of rubber latex was the subject of International Organization for Standards’ (ISO) International Standard 1409-1982. A recent book by Compton (4) covers various aspects of chemical and physical methods for the analysis of polymers. The techniques discussed include spectroscopy, chromatography, fractionation, X-ray diffraction, autoradiography, differential thermal analysis (DTA), thermogravimetric analysis (TGA), and differential scanning calorimetry (DSC). The review on “Analysis of High Polymers” (5) details literature for various techniques which are equally pertinent in the analysis of rubber. Instrumental chemical analysis of polymers by spectroscopy, chromatography, thermal analysis, and surface study techniques was the subject of a review by Lawson (6)while direct mass spectral analysis of polymers was reviewed by Lattimer (7). Another review entitled “Conformational Statistics of Macromolecules” (8)dealt with the molecular conformation and configuration on polymer properties and the analytical techniques used in the study of molecular structure. Proton and carbon NMR spectra of polymers were classified in two books (9, 10). A review (11)discussed the current status of methods for characterizing the cross-link structure in network polymers using NMR, swelling measurement, and mechanical analysis. Chromatographic techniques-size exclusion, supercritical fluid, and thin layer-were reviewed (12)in a recent book. The basic principles of scattering theory were outlined and the applications of light, neutron, and X-ray scattering techniques to the study of polymer blends were detailed (13). A review (14) of analysis of rubber vulcanizates by advanced chemical techniques dealt with rubber chemicals, carbon black, and inorganic fillers. The methods presented include TGA, chromatography, Fourier transform infrared spectroscopy (FT-IR), nuclear magnetic resonance (NMR) spectroscopy, porosimetry, transmission electron microscopy, X-ray fluorescence, and X-ray diffraction. Microstructural characterization of polymers by high-performance pyrolysis-GC was discussed in a review (15). Possibilities and limitations of phase distribution chromatography for analysis of polymers were discussed by Greschner (16).
Quantitative and qualitative analysis of polymers and additives by chromatographic and spectroscopic techniques was reviewed (17 ) with respect to the advantages of automation and computerization. Other reviews covered the fields of SEC (It?), dynamic properties and compound performance (19), analytical trends in elastomer characterization (20), polymer characterization (21),degradation and pyrolysis mechanisms (ZZ), pyrolysis and GC in polymer analysis (23),microstructure Contribution No. 659 from The Goodyear Tire & Rubber Company, Research Laboratory, Akron, OH 44305. 114 R
0003-2700/87/0359-114R$01.50/0
Table I. Abbreviations Recommended by ASTM ( 2 ) butadiene rubber chloroprene rubber EPDM terpolymer of ethylene, propylene, and a diene with the residual portion of unsaturated synthetic rubber IR isoprene synthetic rubber NR natural rubber SBR stvrene-butadiene rubber BR CR
of synthetic polymers (24), and computer applications in polymer laboratory (25).
NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY (NMR) NR was isomerized by treatment with SOz at 100 “C and the diad structures cis-cis, cis-trans, trans-cis, and trans-trans were quantitated by I3C NMR spectroscopy (26). I3C NMR chemical shift assignments of resorcinol-formaldehyde reaction products were made and nuclear Overhauser enhancement factors were determined for relevant carbons (27). These data were applied to commercial and experimental resins (2%). Epoxidation of N R with peroxyacids was carried out in latex i d in homogeneous soltition and the products were studied bv I3C NMR (29). “I3C NMR techniques were used in a preliminary study on the structure and concentration of cross-links produced in sulfur vulcanization of NR (30). This study showed isomerization of some double bonds and indicated the existence of di- and polysulfidic structures. ‘H NMR spectra of methylfluoropropylsilicon oil and rubber were assi ned by using a series of model compounds (31). PBD and 8BRs with 10-70% vinyl content were synthesized and characterized by NMR (32). NMR in combination with IRS, GPC, and electron microscopy was used to study qualitative phase changes in diblock copolymers and blends (33). NMR along with other techniques was utilized for characterization of homopolymers and copolymers of butadiene and isoprene (34). Chain dynamics of the 13CNMR spectra of EPDM at high field was used to interpret various sequence placements (36). This technique was also applied for quantitative measurement of chain folding in 1,4-trans-polyisoprene crystals (37). Isoprene-ethylene diads of various configurations were examined by ‘H and I3C NMR (38). Sequence distributions, microstructure, and stereoregularaties of 1,2-PBD prepared with different catalysts were characterized by 13C NMR (39). Fluorine NMR was attempted for investigation of the decomposition of accelerators using fluorine homologues of some of the common accelerators (40). Proton spin-spin relaxation time for bound rubber in composites containing silica was used to study higher order structures (41). Pulsed and steady field gradient NMR diffusion measurements in polymers were discussed by von Meerwall (42).
INFRARED AND ULTRAVIOLET SPECTROSCOPY (IR, UV) Direct analysis of heavily loaded carbon-black-filled SBR was reported (43). This procedure used attenuated total reflectance (ATR) sampling technique with FT-IR. Some changes between the sectra of filled and unfilled SBR were observed due to interactions between the polymer and the fillers. ATR technique was also used for identification of inorganic additives in vulcanized NR-SBR blends ( 4 4 ) . 0 1987 American Chemical Society
RUBBER
Punjab. He']aink the Research Division of The Goodyear Tire & Rubber Company. Akron . . ., OH . ., ..in. 1969 . .... .Ha . . rinantlv . . ..., Section. Head in charge 01 lhe Maleriais Characlerization Section in lhe AnaiVtical and Materia1s Testing Division. His &blicalions cover the areas 01 GPC, Gc. pyrolysis-GC. and sobent extraction. He is a member 01 the American Chemical Society and its Anaiyiical Chemistry and Rubber Divisions.
*",
...
.-
Rheo-optical FT-IR was applied to study transient structural changes in cross-linked NR during stress-relaxation (45). Thin latex films from latex were formed on AgCl windows by spinning the windows (46). This gave a more uniform film than hy spreading. Diode array UV spectroscopy, FT-NMR, and mass spectrometry (MS) were used in the study of vulcanization and degradation of rubber (47). Multiple reflectance IR was useful in the study of the surface of EPDM vulcanizates (48). Two bands at 1020 and 1050 cm-' were assigned to the C-0 group in the spectrum of dicumyl peroxide and S-vulcanized EPDM, respectively. Molecular orientation in NR and high cis-1,4-polyisoprene was studied with FT-IR dichroism (49). Attenuated total reflection (ATR)-IR was utilized for identification of components separated by paper chromatography (50)due to its simplicity. Temperature dependence of the intensity of IR absorption bands of block and statistical SBR was studied (51) and special features of the observed transitions were described. IR was used to study the effect of p-phenylenediamine type of antiozonants during oxidation (52). Some synergistic stability effects were identified. Near-infrared reflectance spectroscopy was described for the determination of ruhher in guayule (53).
THERMAL METHODS Differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), and thermomechanical analysis (TMA) were used to measure thermal properties (glass temperature, cold crystallization, melting, vulcanization, and thermal stability of SBR), quantitative composition of NR-EPDM mixtures, and dimensional changes in EPDM when exposed to solvents (54).
The DTA oxidation peak at 200 "C was used for evaluating the effectiveness of antioxidants and vulcanizing agent on the thermal stability of cis-1,4-PBD (poly(hutadiene)) (55). The effect of chemical structure, branching, cross-linking, plasticizers, fillers, and other additives on thermal properties like glass transition (Tg), melting point, heat capacity, specific heat, expansion coefficient, and thermal conductivity was studied (56). DSC was used to study the freezing process in swollen networks like NR in cyclohexane (57). Composition-dependent glass transition was examined in theory and practice for polymers, miscible blends, plasticized polymers and copolymers (58). The Tg of highly elastic ruhhers was determined hy increasing the pressure 5-30 MPa prior to cooling and then determining the discontinuous change in the pressure of the desorbed gas (59). A method was described to measure the entropy change of a rubber strip under tensile strain (60). The principles of a dynamic mechanical thermal analysis method for SBR and ABS were described (61). DSC was employed to identify and calculate the amount of vulcanized and unvulcanized rubber, to calculate the amount of sulfur and accelerators in unvulcanized ruhher stock, and to compare the reactivities of phenolic resins in butyl rubber (62). The solubility parameter and Tg were examined as a function of 1,2 content of 1,2-PBD (63). Heat capacities of cis- and trans-1,4-PBDs were calculated as a function of temperature by DSC (64). Oxidative degradation of EPDM was studied with a thermal stress strain analyzer (65).
Blends of cis-1,2-PBD and emulsion polymerized SBR were examined by DSC and light scattering to show the coexistence of the upper and lower critical solution temperatures (66). DSC was used to study the effectiveness of antioxidants for cis-PBD (67). TGA was utilized for quality control of molded NBR parts where the percentages of plasticizer, polymer, carbon black, and minerals were determined (68). Applications of thermal analysis in the automotive industry were detailed (69). Thermal-mechanical analysis was found useful for examining polyisobutylene-based elastomeric ionomers (70). The vulcanization rate constants of ethyleneisobutylene-propylene rubber were determined by DTA and thermodilatometry (71). The influence of compounding ingredients on thermal degradation of chlorine-containing vulcanizates was examined (72). The polymers studied were polychloroprene, chlorinated P E (polyethene), chlorosulfonated PE, and epichlorohydrin. Tgs of emulsion and solution SBR were examined (73). DSC was used to study the crystallization of NR and its synthetic analogues (74). In this study deproteinized NR and synthetic NR with additives were also compared. Oxidation of NR was studied by DSC (75). Oxidative degradation of polymers was examined by using a TGA/ MS/MS combination (76) while curing studies were performed with TGA/GC/FT-IR/MS (77). Modifications needed to examine rubbers by TGA were reported (78). Broad applicahility of various thermal analytical techniques was described (79).
GEL PERMEATION AND SIZE EXCLUSION CHROMATOGRAPHY (GPC, SEC) Applications of GPC in engine oils, hinders in ferrite powders, novalaks, surfactants, and polymers are described (80, 81). A procedure using combined GPC and low-angle laser light scattering (LALLS) was developed for characterizing block copolymers (82). Real-time spectral acquisitions on SEC were combined to give verification of copolymerization (83). High-performance SEC was applied to the analysis of oligomers and small molecules (84). This technique was also used to study polymer degradation. A pressure transducer coupled with a differential UV detector was used to extend size and shape determination by GPC (85). The use of a LALLS detector with a microcomputer system was shown to provide MWD (molecular weight distribution) data even in the presence of small amounts of microgel (86). GPC was employed to determine the MWD of carbonblack-inpregnated copolymer beads in suspension (87). Online molecular weight and large chain branching measurements were made with a SEC-LALLS system (88). A quality assurance program using SEC, multiple detectors, and regression equations was proposed (89, 90). Dilute solution properties of tramns-l,4-polyisoprene were examined after separation by GPC (91). Semimicro SEC for oligomers was compared with separations obtained with conventional columns (92). Coupling of GPC with an automated capillary viscometer facilitated polymer characterization (93). Quantitative SEC was described for polymer characterization by determining branching frequency, copolymer composition, and gel content (94). MWD of wlvchromonhore oolvmers wine SEC and HPLC was compa;ed'(95). . New parameters to evaluate the performance of SEC columns were proqosed (96). Multiple detectors were used to obtain corrections for various parameters (97). Absolute MWD with SEC were obtained by using a differential pressure transducer detector (98). A similar system was used to nrovide true Mark-Houwink-Sakurada Darameters (99). . Concentration effects in SEC were separated by contrihutions due to viscosity and hydrodynamic volume correction (100). A new theory was proposed to explain these effects (101). Also a new model for the mechanism of GPC and a new calibration method were developed (102). Two independent equations were derived from the intrinsic viscosity to estimate MWD (103). High-performance GPC was used in calibration of broad molecular weight standards .
I
I
ANALYTICAL CHEMISTRY. VOL. 59, NO. 12. JUNE 15. 1987
* 115R
RUBBER
(104). Errors could then be calculated.
A model was presented to describe the experimental shifts in elution volumes caused by concentration effects (105). Peak spreading corrections were obtained by using functions like Wesslan and Tung's (106). Reliability of MWD based on a concentration detector and LALLS was studied (107). Equations were derived to relate the statistical moments of uncorrected and spreading-corrected chromatograms in GPC (108). Mark-Houwink constants were obtained from GPC and intrinsic viscosity data (109).
PYROLYSIS (PY) GAS CHROMATOGRAPHY, (GC) MASS SPECTROMETRY (MS) Instrumentation used in PY-GC was described (110,111). Applications of PY-GC-MS for some new polymers were shown and the pyrolysis products identified (112). Pyrolysis-capillary GC-FTIR as used in the automobile industry was described where NR, NBR, SBR, and EPDM were characterized (113). Determination of polymers by PY-GC was shown in various mixtures (114). This technique was also successfully used to determine rubber in SBR latex (115). Identification and differentiation of synthetic polymers by PY-capillary GC were examined (116, 117). Greater versatility was obtained for PY-GC by using MS, flame ionization, flame photometric, and surface ionization detectors (118). Copolymers were examined by PY-MS with field ionization (119). PY-MS with pattern recognition was used to analyze smoke aerosols to determine fuels involved in fires (120). PY-GC was found to be useful in determining styrene in high styrene SBR latexes and compounds (121). PY-IR was used for analysis of SBR and NR in their covulcanizates (122). PY-GC of acrylic fibers and styrene copolymers was used to determine the monomer composition (123). PY-GC with flame ionization, electron capture, and N- and P-selective detectors was used for identification of PVC, NR, NBR, etc. (124).
The influence of pyrolysis parameters on the results in PY-GC was studied (125). Laser PY-MS was used for direct analysis of vulcanizates (126).
syndio-1,2-PBD was examined by PY-GC and the syndio-1,2content was related to certain GC peak ratios (127). Heart-cutting, cold trapping, and back flushing techniques were applied in PY-GC to cut the analysis time for rapid screening of polymers (128). A method was described for applying polymers and inorganic material to Curie-point wires. In this procedure the sample was pressed to the wire at a pressure of 15 tons (129). Cryogenic focusing with PY-capillary GC provided an added dimension to this technique (130). Applications of the technique to polymers and oil shale were described.
CHROMATOGRAPHIC TECHNIQUES Thermogravimetric analysis and dynamic headspace GCMS with on-column cryogenic focusing were used to characterize complex mixtures generated on heating polymers (131). Distribution of accelerators di(2-benzothiazyl) disulfide and N,"-dithiodimorpholine in EPDM was studied by thin-layer and high-performance liquid chromatography (132). GC combined with MS was used to determine solvent being desorbed from polymers (133). Inversion GC for study of polymers (134) and for determining polymer interaction parameters (135) were described. Thin-layer chromatography was used to check for benzothiazole derivatives and @-sitosterolin leachates from disposable syringes (136). Phenolic antioxidants were determined by HPLC on a C,, reversed-phase column using acetonitrile-water as the mobile phase with detection at 280 nm (137). Hydrodynamic chromatography was used to determine polymer latex particle size (138).
Ion chromatography for the analysis of organic anions in natural rubber latex serum was described (139).
ANALYSIS RELATED TO SAFETY AND HEALTH An estimate of toxic vapors in volatiles from rubber goods was made based on the relative concentration of these to the 116R
ANALYTICAL CHEMISTRY, VOL. 59, NO. 12, JUNE 15, 1987
main components (140). An apparatus for simulating the migration of chemicals from polymeric wastes into the atmosphere was described (141). A GC technique was used for volatiles which can be detected down to the 0.05 pg level. Volatiles like hydrocarbons, alcohols, and thiols released into the atmosphere during polymer manufacture were determined by GC after preconcentration (142). Guidelines for using Tenax GC as an absorbant for volatile organic pollutants were given (143). Traces of organic peroxide vulcanizing agents and their transformation products in rubber were determined by thin-layer chromatography (144). Volatile N-nitrosamines in baby bottle nipples (145) and infant pacifiers (146) were determined by extraction followed by GC-TEA. Special techniques to avoid formation of those materials during analysis were emphasized (147). Residual accelerators like dialkyl dithiocarbamates in baby bottle nipples were extracted with chloroform-acetone, converted to ethyl esters, and analyzed by GC with an N-P detector (148j. Extraction and GC determination of formaldehyde in surgical materials was described (149). Formaldehvde was coGerted to Z74-dinitrophenylhydrazonefor this analysis. GC and photometric methods used to determine formaldehyde in air were compared (150). Aniline content of rubber vulcanizates contacting water, alcohols or milk was determined by thin-layer chromatography (151).
Autogenous temperatures for various polymers were determined by ASTM G72 procedure and pressurized DSC (152). Rubber debris in road dust was qualitated by PY-GC (153). Headspace capillary GC was used to detect residual solvents in food packages (154). Fundamental mechanisms of combustion of rubber, inhibition of combustion, the criteria for testing and performance, smoke, and combustion toxicity were studied (155).
MISCELLANEOUS TECHNIQUES Phase morphology of thick rubber blends was studied after staining the surface with KMn04 followed by examination under a microscope (156). Advances in scanning electron microscopy were reviewed by White and Thomas (157). Blooming caused by accelerators was analyzed by multiple reflectance IR and SEM (158). Polarization microscopy was used to determine failures in ethene-propene rubber cable insulation and SEM was used to identify contaminants and filler agglomerates (159). Methods for testing morphology-property relationships in rubber blends were described (160). Field desorption and fast atom bombardment mass spectrometry were used to examine several rubber extracts (161). Both techniques proved to be effective for the identification of organic additives, the molecular weight data provided by MS was complementary to the information from IR. Determination of sulfur by inductively coupled plasma was compared with other techniques (162). In another procedure sulfur was determined as sulfate ions by isotachophoretic analyzer after the combustion gases were absorbed in hydrogen proxide solution (163). Organo phosphite antioxidant, Polygard, was converted to phosphates by reacting the polymer with sulfuric-nitric acid mixture and hydrogen peroxide. The phosphate was then quantitated photometrically (164). The viscosity of cyclohexane solution of guayule rubber was used as a measure of rubber content (165). Ozone degradation products from rubbers were studied by IR (166). Different grades of carbon black were identified by particle size distribution using a double exponential size distribution equation (167). X-ray fluorescence was used to study the thickness and uniformity of PTFE antifriction coatings (168). The standard Soxhlet procedure for quantitation of resin and rubber in guayule was modified to provide a rapid and reliable analysis (169). A turbidimetric method was presented for similar application (170). Semidilute solutions of polydisperse branched polymers were studied by dynamic light scattering (171). Small-angle X-ray scattering from accidental thermal concentration fluctuations of block polymers was studied for styrene-isoprene copolymers (1 72). Particle size measurement using angular light scattering was described (173). Molecular weight determination by SEC and
RUBBER
by small-angle light diffraction was compared (174). Time-resolved small-angle X-ray scattering was used to analyze transient structural responses (175, 176). Chain conformation in elastomeric multiblock copolymer was measured by small-angle neutron scattering (I77). Small-angle X-ray scattering was applied for characterizing the structure of fillers like silica and carbon black (178). Complex dynamic bulk modulus of elastomers was obtained via inversion of acoustic scattering in water (179). The problem of assessing incoherent neutron scattering intensities from polymer systems was defined and attempts were made to obtain those values (180). The degree of interaction between fillers and polymers was obtained by X-ray structure analysis (181). A photometric method to assess dispersion of carbon black was reported (182). The activity of solvents in a swollen polymer network was determined by vapor pressure osmometry (183). Latex distribution in coated paper was examined by electron probe X-ray analyzer after exposing the sample to osmium tetraoxide (184). Sequence distribution in commercial SBRs using ozonolysis-GPC was reported (185). The concept of a diffusion-averaged molecular weight was presented. This value could be determined rapidly for polydisperse samples (186). An isothermal volatilization apparatus based on GC was used for the study of swollen SBR, PBD, and NR (187). The applicability of chemical analysis for fibers, chemicals, and polymers was described (188). A comparative analysis of epoxidized NR by 'H NMR, 13C NMR, titrimetric, elemental, and DSC techniques was reported (189). Equipment to measure the green strength of rubber mixtures was reported (190). The effect of activators and curative in NR/BR on the physical properties of tire treads was reported (191). Flow field-flow fractionation was adapted to nonaqueous systems for polydisperse samples (192). The response of polymeric materials to intense concentrated thermal radiation was investigated (193). In this report ignition, charring, melting, and surface distortion were examined. Torque and mass temperature in a laboratory mixer were related to the processability and molecular properties of polymers (194). The protein components were separated from NR (195). These were found to contain strongly bound mineral particles which were the main sites for vulcanization. The application of FT-NMR, MS, and diode array UV in combination with computer technology was discussed for studying the vulcanization and degradation of rubber (196). Kinetics of spinodal decomposition in an oligomeric blend of PS and PBD were studied by using- small-angle - light scattering (197). Freeze coagulation of latex was described where the latex was frozen onto an ice film which facilitated easy removal (198). The dynamic mechanical thermal analysis of polymers was reviewed especially for the study of physical aging, curing, and coating properties of polymers (199). UV, lH NMR, 13C NMR, MS, and GPC characteristics of phenylhydrazones of aldehydes and ketones were reported to aid in the identification of oxidation products from NR (200). Tensile retraction measurements were used to determine the effective molecular weight between cross-links of vulcanized SBR (201). An amaratus to measure the tack of elastomers was described'(202). The amount and types of higher fatty acid soaps in NR latexes were determined by GC and MS (203). The chemical composition and heterogeneity of some polymers were determined by thin-layer chromatography on coated quartz rods and flame ionization detector (204). The unperturbed dimensions of 1,4-trans-polyisoprenewere estimated by using viscosity-molecular weight extrapolation methods (205).
ACKNOWLEDGMENT The permission of The Goodyear Tire & Rubber Company to prepare and publish this review is greatly appreciated. I specially thank Goodyear's Technical Information Center, D.
N. Thayer, and M. Hampu for their invaluable help. LITERATURE CITED
( I ) Krishen, A. Anal. Chem., 57, 187R-191R (1985). (2)
Amer SOC for Testing and Materlals, "1985 Annual Book of ASTM Standards, 09.01"; ASTM: Philadelphia, PA, 1985. (3) International Organization for Standardization (Geneva), 1982, International Standard 1409-1982. (4) Crompton, T. R.. "Analysis of Plastics", Pergamon: Oxford, 1984. (5) Smith, C. G.; Matile. N. H.; Park, W. R. R.; Smith, P. 5.; Martin, S. J., Anal. Chem., 5 7 , 254R-67R (1985). (6) Lawson, G., Prog. Rubber Plast. Techno/., 7, 1-17 (1985); Chem. Abstr., 704, 2002w. (7) Lettimer, R. P.; Harris, R. E., Mass Spectrum Rev., 4 , 369-90 (1985); Chem. Abstr., 104, 6462q. (8) Tarazona, M. P.; Saiz, E., Rev. Plast. Mod., 49, 319-31 (1985). (9) Pham, Q. T.; Petiaud, R.; Waton, H., Proton and Carbon NMR Spectra of Polymers; Wiley: Chichester, 1983; Vol. 2, pp 224-445. (IO) Pham, Q. T.; Petiaud, R.; Llauro, M. F.; Waton, H., Proton and Carbon NMR Spectra of Polymers; Wlley: Chichester, 1984; Vol. 3, pp 448-677. (11) Harrison, D. J. P.; Yates, W. R.; Johnson, J. F., J. Macromol. Sci. C , 2 5 , 481-549 (1985). 12) Johnson, J. F., Encycl. Polym. Sci. Eng., 3, 491-531. 13) Higgins, J. S., Polymer Blends and Mixtures; Proceedings of the NATO Advanced Study Institute on Polymer Blends and Mixtures, London, 2- 14 July 1984, pp 69-88. 6125, NATO, Advanced Study Institute, edited by Walsh, D. J.; Higgins, J. S.; Maconnachie, A. 14) Mersch, F.; Zimmer, R., Kautsch. Gummi, Kunstst., 427-32 (1986); Chem. Abstr., 105, 80348~. 15) Tsuge, S.,Eunski Kagaku, 35, 417-38 (1986); Chem. Abstr., 105, 79601g. 16) Greschner. G. S., Adv. Pokm. Sci., 73-74, 1-61 (1985); Chem. Abstr., 104, 130525b. 17) Galii, E., Plast. Compounding, JanlFeb, 22-23 (1985). 18) Mori, S., Eunseki, 86, 483-8 (1986); Chem. Abstr., 705, 134584~. 19) Funt, J. M., Rubber World, 793, 25-8, 32, 34-5 (1986); Chem. Abstr., 10.5 . - - , 61932n - .- - (20) Hays, 0. k, Annu. Meet. Proc.-Int. Ins:. Synth. Rubber Prod. 25th Paper 1-4, 12 pp (1984); Chem. Abstr., 704, 208657t. (21) Liebman, S. A.; Levy, E. J., Chromatogr. Sci. 29 (Pyrolysis GC Polym. Anal.), 1-14 (1985); Chem. Abstr., 702, 149997n. (22) Flynn, J. H.; Florin, R. E., Chromatogr. Sci., 29 (Pyrolysis GC Polym. Analy.), 149-208 (1985); Chem. Abstr., 702, 149814a. (23) Liebman, S. A., Levy, E. J., Eds. Chromatogr. Sci. 29 (Pyrolysis GC Polym. Anal.) Marcel Dekker: New York, 1985; Chem. Abstr., 702, 96334k. (24) Ahlstrom, D. H.. Chromatogr. Sci., 29 (Pyrolysis GC Poiym. Anal.), 209-76 (1985); Chem. Abstr., 702, 150000p. (25) Provder, T., ACSSymp. Ssr. No. 313(1986). (26) Maidunny, 2. A. B.; Dulngali, S. B., J . RRI Malaysia, 33, 48-53 (1985). (27) Werstler, D. D., Polymer, 27, 757-64 (1986). (28) Werstler, D. D., Polymer, 2 7 , 750-6 (1986). (29) Bradbury, J. H.; Perera, M. C. S., J . Appi. Polym. Sci., 30, 3347-64 (1985). (30) Komoroski, R. A.; Shockcor, J. P.; Gregg, E. C.; Savoca, J. L., Rubber Chem. Technl., 5 9 , 328-46 (1986). (31) Yu, H.; Mi, J., Eopuxue Zazhi, 7, 429-36 (1984); Chem. Abstr., 104, 1879201. (32) Aggarwal, S. L.; Fabris, H. J.; Hargis, I. G.; Livigni, R. A,, Polym. Prepr. 26, 3-4 (1985). (33) Hsiue, G. H.; Shih, S. W. F., Polym. Prepr. 2 6 , 243-4 (1985). (34) Hsieh, H. L.; Yeh, H. C., Rubber Chem. Technol., 58, 117-45 (1985). (35) English, A. D., Macromolecules 78,178-81 (1985). (36) Cheng, H. N., Macromolecules, 77, 1950-5 (1984); Chem. Abstr., 707, 172784d. (37) Schilling, F. C.; Bovey, F. A.; Anandakumarant, K.; Woodward, A. E., Macromolecules. 78,2688-95 (1985); Chem. Abstr., 703, 216697a. (38) Myagkova, L. A.; Kropacheva, E. N.; Khachaturov, A. S., Polym. Sci. USSR, 2 6 , 1063-72 (1984). (39) Zhong, C.; Xie, D.; Tang, X., Hecheng Xiangjiao Gongye, 8, 412-14 (1985); Chem. Abstr., 704, 51868n. (40) Kelm, J.; Gross, D., Rubb. Chem. Technol., 58,37-44 (1985). (41) Ito, M.; Nakamura, T.; Tanaka, K., Nippon Gomu Kyokaishi, 58, 468-74 (1985). (42) von Meerwall, E. D., Rubb. Chem. Techno/., 58, 527-60 (1985). (43) Sloan, J. M.; Clements, J. P., Report AMMRC-TR-84-25; Chem. Abstr. 702, 150710~. (44) Jovanovic, D., Polimeri(Zagreb), 6, 275-7 (1985); Chem. Abstr., 704, 1698448. (45) Siesler, H. W., Polvm. Bull. (Berlin). 72, 481-6 (1984): Chem. Absb., 702, 2 6 1 0 6 ~ . (46) Cheesman, G. C. N.,; Gaskin, L. J.. Anal. Cbem., 57, 1167-8 (1985). (47) Aart's, A.; Baker, K. M., German Rubber Conference: DKT'83. Summaries. Wiesbaden. 13-16 June 1983. D. 169-70-013. Deutsche Kautschuk Gesellschafl. (48) Wu, Z.; Yang, W.; Gong, K., Hecheng Xiangjiao Gongye, 9 , 262-5 (1986); Chem. Abstr., 705,989734. (49) Amram, B.; Bokobza, L.; Queslei, J. P.; Monnerie, L.. Polymer, 27, 877-82 (1986); Chem. Abstr., 705,61919q. (50) Sreenivasan, K., Chromatographia, 2 2 , 199-200 (1986); Chem. Abstr., 105, 107687t. (51) Sokolova. L. N.; Nikolayeva, D. A.; Shershnev, V. A,, folym. Sci. USSR, 28, 1730-40 (1984). (52) Giurginea, M.; Ivan, G., I z v . Khim., 78,268-76 (1985); Chem. Abstr., 102, 70074s. ANALYTICAL CHEMISTRY, VOL. 59, NO. 12, JUNE 15, 1987
117R
RUBBER (53) Black, L. T.; Hamerstrand, G. E.; Kwolek, W. F., Rubber Chem. Techno/., 58, 304-13 (1985). (54) Staub, F., Am. Lab. (Fairfield, Conn.), 18, 56, 58, 60, 62-3 (1986); Chem. Abstr., 104, 111150j. (55) Xu, C.; Lin, Y.; Xiang, J.; Wang, Q., Hecheng Xiangjiao Gonguye, 8 , 419-22 (1985); Chem. Abstr., 104, 51873k. (58) Fatou, J. M. G., Rev. Pkst. Mod., 49, 551-64 (1965). (57) Arndt, K. F.; Zander, P., Plaste c Kaut., 32, 155-6 (1985). (58) Couchman. P. R., Polym. Pmpr. 2 6 , 13-4 (1965). (59) Shtitelman, M. I.; Stogova, E. P.; Erkovich, E. D.; Kosenkova. A. S., USSR SU I171710 A I , 7 Aug. 1985; Chem. Abstr., 103, 216734k. Izv. Vyssh. Uchebn. Zaved., Fiz., 28, 113-4 (1985); (60) Petrova, L. I., Chem. Abstr., 103, 222016~. (61) Wetton, R. E.; Gearing, J. W. E.; Stone, M. R., J . Phys., Colloq., (C5), C5/68965/694 (1965); Chem. Absh., 103, 124374q. (62) Rugo, G.; Urbani, M.; Barbattini, D.; Nastasi, C.; Orsi, M.; Poponessi, M., Kautsch. Gummi, Kunstst., 39, 216-19 (1986); Chem. Abstr.. 104, 226 146e. (63) He, T.; Li, 8.; Ren, S.,J . Appl. Polym. Sci. 31, 873-84 (1986). (64) aebowicz, J.; Aycock. W.; Wunderllch, B., Polymer. 27, 575-82 (1986). (65) Oklno, T.; Maruta, M.. Shimadzu Hyoron, 42, 277-81 (1985); Chem. Abstr. 105, 9 8 9 7 2 ~ . (66) Ouglzawa, T.; Inoue, T.; Kammer, H. W., Macromolecules, 18, 2089-92 (1985). (67) Sarasci. 0. T.; Petklm; Baysal, S. M., J. Appl. Polym. Sci., 31, 2157-69 (1986); Chem. Abstr., 105, 7702a. (68) Boissel, J., Rev. Gen. Caoutch. Plast., 659, 159-63 (1986); Chem. Abstr., 105, 4 4 4 6 3 ~ . (69) Haedrich, W.; Kalserberger, E., Thermochlm.Acta, 85, 331-4 (1985); Chem. Abstr., 103, 12316r. (70) Bagrodia, S.R.; Wllkes, G. L.; Kennedy, J. P., J . Appl. Polym. Sci., 30, 2179-93 (1985); Chem. Abstr., 103, 205242b. (71) Seldov, N. M.; Aliguliev, R. M.; Allev, F. A.; Ovanesova, G. S.;Ibragimov, Kh. D.: Guseinov, F. O., Azerb. Khim. Zh.. 4 , 82-6 (1984); Chem. Abstr., 102, 186430t. (72) Jaroszynska, D.; Kleps, T., Rubbercon '81; International Rubber Conference Vol. 1, Harrogate, 8-12 June 1981; pp C5.1-C5.10. (73) Moore, D.; Day, L. G., Elastomerics, 117, 22-8 (1985). (74) Burfield, D. R., Polymer, 25, 1823-6 (1984); Chem. Abstr., 102, 80048j. (75) Lye, P. H.; Toh, H. K., J . Appl. Polym. Sci., 29, 2627-34 (1984). (76) Shushan, B.; Wllliamson, C.; Prime, R. B., Antec '84; Plastics In a World Economy; Proceedings of the 42nd Annual Technical Conference, New Orleans, AprN 30-May 3, 1984; pp 319-22; 011, SPE. (77) Sabatelli, D. C.; Lavigne, G.; Tanaka, J.; Johnson, J. F., Antec '84; Plastics in a World Economy: Proceedngs of the 42nd Annual Technical Conference, New Orleans, April 30-May 3, 1964; pp 311-5; 011, SPE. (78) Rossignol, J.; Alarconlorca, F., Caout. Pkst., 62, 49-52 (1985). (79) Maurer, J. J., Quantitative Characterlzation of Plastlcs and Rubber; Symposium, Hamikon, June 22, 1984; pp 92-100, 91T, Chemical Inst. of Canada, Macromolecular Sci. Div., Edited by Vlachopoulos, J. (80) Heisz, 01, GIT Fachz. Lab., 2 9 , 643-4, 847-8 (1985); Chem. Abstr., 104, 6 1 2 5 0 ~ . (81) Miller, R.; Dalton, G., ASTM Spec. Tech. Publ., 846 (Qual. Assur. Polym. Mater. Prod.), 51-64 (1985); Chem. Absh., 104, 69396s. (82) Dumeiow, T.; Holding, S.R.; Maisey, L. J. Dawkins, J. V.. Polymer, 27. 1170-6 (1986); Chem. Abstr., 105, 134631b. (83) Meister, J. J.; Nicholson, J. C.; Patil. D. R.: Field, L. R., Macromolecules, 19. 803-9 (1986); Chem. Abstr., 104, 110481f. (84) Chiantore, 0.; Guaita, M., J. Liq. Chromatogr., 9 , 1341-65 (1986); Chem. Abstr. 105, 79643e. (85) Trowbridge, D.; Brower, L.; Seeger, R.; McIntyre, D., Polym. Mater. Sci. Eng., 54, 85-7 (1986); Chem. Abstr., 104, 1 6 9 2 8 3 ~ . (86) Devaty, J.; Sangal. S. K.; Bednar, 8.; Krallcek, J., Sb. Vys. Sk. Chem.-Techno/. Praze, Polym.: Chem., Vlasfnosti Zpracov., S12, 205-27 (1985); Chem. Abstr., 105, 7123n. (87) Bakhshaee, M.; Pethrick, R. A.; Rashid, H.; Sherrington, D. C., Polym. Commun., 26, 185-92 (1985). (88) Hamielec, A. E.; Meyer, H.. Dev. Polym. Charact., 5,95-130 (1986); Chem. Abstr., 105. 98228q. (89) McCrary, T. J., Jr., Am. Lab. (Fairfieid, Conn.), 17, 84, 86, 86, 90, 92-3 (1985); Chem. Abstr., 104, 6511e. (90) McCrary, T. J., Jr., Am. Lab. (Fairfield, Conn.), 17, 98, 100-5 (1985); Chem. Abstr., 102, 185778a. (91) Chaturvedi, P. N.; Patel, C. K., J. Polym. Sci. Polym. Phys., 23. 1255-62 (1965). (92) Mori, S.,J . Liq. Chromatogr., 9 , 1329-40 (1986); Chem. Abstr.. 105, 43886~. (93) Jin. C.; Sun, S.; Wang, F.: Sun, W.; Yu. F., Vingyong Huaxue, I , 34-40 (1984): Chem. Abstr., 103, 6964j. (94) Balke, S. T., Ouant. Charact. Plast. Rubber, R o c . Symp., 1-11, Edited by: Vlachopoulos. J., McMaster Univ., Dept of Chem. Eng.: Hamilton, Ont. (95) Lai, S. T.; Sangermano, L., J. Chromatogr., 322, 338-46 (1985): Chem. Abstr., 102, 204595g. (96) Chen, Z . , Xiandai Huagong, 35, 47-9 (1986); Chem. Abstr., 105, 98282~. (97) Benchabane, M., Angew. Makromol. Chem., 183, 121-37 (1966); Chem. Abstr., 104, 149765b. (98) Kuo, C.; Provder, T.; Koehler, M. E.; Kah, A. F. Polym. Mater. Sci. Eng., 54,80-4 (1986); Chem. Abstr., 104. 169190~. (99) Horta. A.; Saiz. E.; Barrales-Rienda, J. M.; Gaiera Gomez, P. A,, Polymer, 2 7 , 139-46 (1986); Chem. Abstr., 104, 169188~.
118R
ANALYTICAL CHEMISTRY, VOL. 59, NO. 12, JUNE 15, 1987
(100) Chlantore, 0.; Guaka, M.; J . Chromatogr., 353, 285-94 (1986); Chem. Abstr., 104, 149773~. (101) Mlngshi, S.;Gulxian, H., J . Li9. Chromafogr., 8 , 2543-56 (1985); Chem. Abstr., 104, 69368n. (102) Su, S. G.; Mou, C. Y., J. Chin. Chem. SOC.(Tal@), 33, 55-9 (1966); Chem. Abstr., 105, 134636g. (103) Zhang. Z., Ylngyong Huaxue, 3 , 5-10 (1986); Chem. Abstr., 105, 7965 I f . (104) Andersson, L., J . Chromatogr., 325, 37-42 (1965); Chem. Abstr., 103, 6961n. (105) Soria. V.; Campos, A.: Tejero, R.; Figuerueio, J. E.; Abad, C., J. Liq. Chromatogr., 9 , 1105-21 (1986); Chem. Abstr., 105, 43748d. (106) Chen, Y.; Ye, M.; Li, X.; Shi. L. J. Li9. Chromatogr., 9 , 1163-74 (1986); Chem. Absfr., 105, 6 1 2 1 1 ~ . (107) Prochazka, 0.; Kratochvii, P., J . Appl. Polym. Sci., 31, 919-28 (1986). (106) Kubln, M., J . Appl. Polym. Sci., 30, 2237-52 (1985); Chem. Abstr., 102, 204782r. (109) Mahabldl, H. K., J . Appl. Polym. Sci., 30, 1535-44 (1985); Chem. Abstr., 702, 221409s. (1 IO) Freed, D. J.; Liebman, S. A., Chromatogr. Sci., 29 (Pyrolysis GC Polym. Anal.), 15-51 (1985); Chem. Abstr., 102, 149998~. (111) Liebman, S. A.; Wampler, T. P., Chromatogr. Scl., 29 (Pyrolysis GC Polym. Anal.), 53-148 (1965); Chem. Absfr., 102, 149999q. (112) Takahashi, S.;Ohnishi, S.,Shlmadzu Hyron, 42, 283-90 (1985); Chem. Abstr., 105, 145435s. (1 13) Reddman. C.; Kurz. H., L P Spec: Chromatogr ., Spektrosk.. 166-73. Vogel-Yerlag: Wuerzburg. Fed. Rep. Ger. (1986); Chem. Abstr., 105, 135199d. (114) Hlrayanagi, S.; %to, M.; Harada, T., Jpn. Kokai Tokkyo Koho, A2(86/758), (1986). Chem. Abstr., 105, 116378~. (115) Wang, J.; Pan, Y.; Fang, Y.; Wang, Y., Sepu, 4 , 5-8 (1986); Chem. Absh. 104, 2261480. (116) Levy, E. J.; Wampler, T. P., J . Chem. Educ., 63, A64-A66, A68 (1986). (117) Goetz, N.; Lasserre, P.; Kaba, G.; Cosmet. Scl. Techno/. Ser., 4 , 81-103 (1965); Chem. Abstr., 104, 174331q. (118) Sotnikov, E. E.; Torosyan, Zh. K., Zh. Anal. Khim., 40, 1887-94 (1985): Chem. Abstr., 104, 110478k. (119) Hummel, D. 0.; Duessel. H. J.; Czybulka. G.;Wenzel, N.; Holl, G., Spectrochim Acta, Part A , 4 1 A , 279-90 (1985); Chem. Abstr., 103, 6977r. (120) Yoorhees, K. J.; Tsao, R., AM/. Chem., 57, 1630-6 (1985). (121) Seiffarth, J.; Solf, I.; Huehn, G.; Hoffman, W., Plaste Kautsch., 31, 371-4 (1984); Chem. Absh., 702, 79522~. (122) Jovanovic, D., Pollmerl, 9-10, 261-3 (1983). (123) Tutas, M.; Saglam, M.; Yuksel, M.. &ga B i / h Derg., Seri A / , 8 , 257-63 (1984); Chem. Abstr., 102, 1507662. (124) Stoer, G., Khim. Ind. (Sotla)),57, 34-5 (1985); Chem. Abstr., 103, 37955m. J. Anal. Appl. pvrolvsis, 8 , 73-86 (1985); Chem. Absh., (125) Ericswn, I., 103, 54667m. (126) McClennen, W. H.; Richards, J. M.; Meuzelaar, H. L. C.; Pausch, J. B.. Polym. Mat. Sci. Engng., 53, 203-7 (1965). (127) Yang, J.; Hu, Z., Fenxi Huaxue, 13, 753-6 (1985); Chem. Abstr., 104, 513178. (128) Wright, D. W.; Mahler, K. 0.; Ballard. L. B.; Dawes, E., J . Chromtcgr. Sci., 24, 13-17 (1986); Chem. Absfr., 704, 6 9 3 7 9 ~ . (129) Venema, A.; Veurlnk, J., J. Anal. Appl. Pyrolysis, 7 , 207-13 (1985); Chem. Abstr., 103. 226668k. (130) Wampler, T. P.; Levy, E. J., J. Appl. Pyrolysis, 8 , 65-71 (1985); Chem. Abstr.. 103. 171194r. (131) Kalman, D: A., Am. Ind. Hyg. Assoc. J., 47, 270-5 (1986); Chem. Abstr.. 105. 48075s. (132) Chalykh,'A. E.; Petrova. T. F.; Rubtsov, A. E.; Lapshova, A. A., Vysokomoi. Soedin., Ser. A , 28, 734-8 (1986); Chem. Abstr., 105, 7713e. (133) Smith, S.B.; Krenceski, M. A.; Hubball. J.; Erickson, E. D.; Johnson, J. H., J. Adhes., 18, 157-65 (1985); Chem. Abstr., 105, 24987q. (134) Hradil, J., Chem. Listy, 80, 506-19 (1986); Chem. Abstr., 105, 61164q. (135) Su, A. C.: Fried, J. R., J . Polym. Sci., Part C : Polym. Lett., 24, 232-52 (1986); Chem. Abstr., 105, 79722e. (136) Airaudo, C. 8.; Gayte-Sorbier, A.; Momburg, R.; Laurent, P., J . Chromatogr., 354, 341-54 (1986); Chem. Abstr., 104, 2304208. (137) Baylocq. D.; Majchercryk, P.: Pellerln, F., Ann. Pharm. F r . , 43, 329-36 (1986); Chem. Abstr., 104, 230583n. (136) Honma, T.; Tazaki, M., Nippon Gomu Kyokalshi, 59, 142-9 (1986); Chem. Abstr., 104, 2254622. (139) Crafts, R. C., Polym. Test.. 5 , 193-207 (1985); Chem. Abstr., 103, 75513. (140) Nudel'man, Z. N.; Gur'ev, M. V.; Balanov, L. A.. Kauch. Rezina, 5 , 38-40 (1986); Chem. Abstr., 105, 138966n. (141) Kirillova, Yu. P.; Chernyak, N. B.; Solov'ev, E. M.. Kauch. Rezina, 9 , 32-3 (1985); Ch8m. Abstr., 104, 55416m. (142) Rudenko, G. I.; Mal'tsev, V. V.; Studenichnik, V. N.; Ustinov, E. P., Zh. Anal. Khim., 40, 119-27 (1985); Chem. Abstr., 103, 186806q. (143) Gutknecht, W. F.; Jayanty, R. K. M.; Bursey, J. T., Research Triangle Park, NC, 1984, mlcroflche. fr. 72. 25/1/85. 12-91T. (144) Novitskaya. L. P., Gig. Sanit., 5 , 45-7 (1985); Chem. Abstr.. 103, 55236. (145) Sen, N. P.; Seaman, S.;Clarkson, S.; Garrod, F.; Lalonde, P., IARC Sci. Publ., 57 (N-Nitroso Compd Occurrence, Bioi. Relevance Hum. Cancer), 51-7 (1984); Chem. Abstr., 103, 103519a. (146) Billedeau, S. M.; Thompson, H. C.; Mlller. B. J.; Wlnd, M. L., J. ASSOC. Off. Anal. Chem., 69, 31-4 (1986); Chem. Abstr., 704, 136051r.
Anal. Chem. 1987, 59, 119R-141R (147) Sen, N. P.;Seaman, S. W.; Kushwaha, S. C., Ane/yst(London), 1 7 7 , 139-44 (1986). (148) Yamazaki, T.; Inoue, T.; Yamada, T.; Tanlmura, A., FoodAWff. Contam., 3 , 145-52 (1986); Chem. Abstr., 705, 12227d. (149) Profumo, A,; Pesavento, M., Analyst (London), 7 7 1 , 241-2 (1986). (150) Davydova, E. A.; Stolyanova, A. G.; Ostrovskaya, E. G.; Kaiashnik, A. A., Gig. Sadt., 3, 56 (1986); Chem. Abstr., 104, 201680m. (151) Novitskaya, L. P.; Dukhovnaya, I. S., G/g. Sanff., 3 , 60-1 (1985); Chem. Abstr., 102, 1 8 6 4 3 3 ~ . (152) Bryan, C. J.; Lowrle, R., ASTM Spec. Tech. fubl., 971 (Flammability Sensitivity Mater. Oxygen-Enriched Atmos.), 106-17 (1986). (153) Sato, F.; Konno, K.; Takahashl, Y.; Seki, T.; Tsunoda, A., Sendai-shi Eisei Shikenshoho, 73, 338-44 (1983); Chem. Abstr., 702, 100057s. (154) Roccheiii, V.; Razzini. A., R o c . Int. Symp. Capillary Chromatogr., 6th, 419-28. Edited by: Sandra P. Heuthlg: Heidelberg, Fed. Rep. Ger. (1985); Chem. Abstr., 704, 1876586. (155) Lawson, D. F., Rubber Chem. Technoi., 5 9 , 455-81 (1986). (156) Wu, X.; Li, H.; Wang, M.; Xie. Q.; Xu, C.; Lin, Y., Huegong Xuebao, 3, 278-82 (1984); Chem. Abstr., 102, 114892~. 1157) White. J. R.: Thomas, E. L., Rubber Chem. Techno/.. 5 7 , 457-506 (1984). (158) Loadman, M. F. R., N. R . Technol., 76, 69-75 (1985); Chem. Abstr., 104, 226157). (159) Groeger, J. H.; Rand, E., R o c . €lectr.I€/ectron. Insul. Conf., 77th, 46-51 (1965); Chem. Abstr., 705, 116315~. (160) Hassander. H.; Toernell, B., folym. Test., 5 , 11-25 (1985); Chem. Abstr., 102, 1333122. (161) Lafflmer, R. P.; Harris, R. E.; Ross, D. B.; Diem, H. E. ACS Rubb. DVn. 725th Meeting-Fall, Indianapolis, Ind., May 8-11, 1984. (162) DIPasquak, G.; Casetta, E., At. Spectrosc., 5 , 209-10 (1984); Chem. Abstr., 102, 63386a. (163) Ota, Y.; Yoshida, H., Jpn. Kokai Tokkyo Koho. JP 601169754 (1985); Chem. Abstr., 104, 35301s. (164) Novikova, E. I.; Flllppova, V. A., flast. Massy, IO, 39-40 (1985); Chem. Abstr., 704, 348256. (165) Smith. M. K.. J . Agrlc. Food Chem., 33, 928-31 (1985); Chem. Abstr.. 103, 179455~. (166) Anachkov, M.; Rakovskl, S.; Razumovskii, S.; Zalkov, G.; Shopov, D., I Z V . Khim., 78, 194-201 (1985); Chem. Abstr., 704, 3 5 2 3 3 ~ . (167) Ushlda, Y.; Sugiura, H., Toy& GoseiGlho, 3 7 , 47-52 (1985); Chem. Abstr., 704, 518621. (168) Uflyand, 1. E.; Kir'yanova, I.A.; Kuzharov, A. S.; Sheinker, V. N., Trenle Iznos, 6,941-4 (1985); Chem. Abstr., 704, 35571e. (169) Nurthen. E. J.; McCieary, B. V.; Milthorpe, P. L.; Whitworth, J. W., Anal. chem.,58, 448-53 (1966). (170) Grinberg, S.; Shaubl. E., Rubber Chem. Technol., 5 9 , 204-7 (1986). (171) Candau, S. J.; Ankrim, M.; Munch, J. P.; HIM, G.. Brit. Polym. J., 77, 210-4 (1985). (172) Mori, K.; Hasegawa, H.; Hashimoto, T.. Polym. J . (Jpn.), 17, 799-806 (1985). (173) Frock, H. N., ACS Polymeric Mat. Sci. Eng., 53, 152-5 (1985). (174) Gusev, S. A.; Tsvetkovskii, I. B.; Vaiuev, V. I., Kauch. Rezina, 3 , 32-3 (1984). (175) Hashlmoto. Y.; Kowsaka, K.; Shibayama, M.; Kawal, H., Macromolec u l e ~ .19. 754-62 (1986). (176) Hashimoto, T.; Kowsaka, K.; Shibayama, M.; Suehlro, S., MacromoksCUles, 19. 750-4 (1986).
(177) Cooper, S. L.; Miller, J. A., Rubber Chem. Techno/, 5 8 , 899-912 (1985). (178) Young, R. J.; AI-Khudhairy, D. H. A.; Thomas, A. G., J . Mater. Sci., 27, 1211-18 (1986); Chem. Abstr., 704, 169884t. (179) Piquette, J. C., J. Acoust. SOC.Am., 7 7 , 1665-73 (1985); Chem. Abstr., 703, 7591x. (180) Maconnachie, A., fo/ymer, 25, 1068-72 (1984). (181) Vnukova, V. G.; Kiseiev, V. Ya.; Bukanov, A. M.; Proyanenkov, V. V.; Tutorskii, I.A... Vysokomol, Sodin., Ser. 8,26. 739-41 (1984); Chem. Abstr., 102, 8028k. (182) Mutagahywa. B. M.; Hemsley, D. A., Piast. Rubb. Process. Apph., 5 , 219-27 (1985). (183) Arndt, K. F.; Schreck, J., Acta Polym., 3 7 , 500-4 (1986); Chem. Abstr., 705, 1157671. (184) Hamada. T.; Kohno, M., KamiPa Gikyoshi, 3 9 , 477-85 (1985); Chem. Abstr., 702, 222387~. (185) Tanaka, Y.; Sato, H.; Adachl, J., Rubber Chem. Technoi., 5 9 , 16-26 (1986). (186) Steuer, W.; Jost, K.; Halasz, I., Chrometographia, 20, 13-19 (1985); Chem. Abstr., 702, 1361 15x. Bischef, G. V., Schuffenhauer, C., Plaste Kautsch., (187) Haeusier, K. 0.; 37,332-4 (1984); Chem. Abstr., 702, 8013b. (188) Grandi, F. 2.; Talamini, G., Chimica Ind., 6 6 , 400-5 (1984). (189) Burfield, D. R.; Llm, K. L.; Law, K. S., Ng, S., Polymer, 2 5 , 995-8 (1984). (190) Wezorke, K.; Weber, K.; Ramsperger, J.; Drescher, R.; Heubner, J.; Haberiand, N.; HeMe, R.; Huebei, R.; Clerniak, M., German Patent (East) DD 214454, 1984, Chem. Abstr., 702, 114967a. (191) Shah. R. D., Rubb. India, 3 6 , 9-19 (1984). (192) Brimhail, S. L.; Myers, M. N.; Caidwell, K. D.; Giddings, J. C., ACS folym. Mat. Sci. Engng., 5 0 , 48-52 (1984 (193) Share, S.; Baba, A., Sampa J . , 27, 7-11 (1985). (194) Markert, J., Kautsch. Gummi, Kunstst., 38, 122-7 (1985); Chem. Abstr., 702, 2052192. (195) Grechanovskii. V. A.; Dmitrieva, I . P.; Zaitsev, N. B., Kauch. Rezina, 3, 15-18 (1985); Chem. Absfr., 702, 205204r. (196) Aarts, A. J.; Baker, K. M., Kautsch, Gummi, Kunstst., 3 7 , 497-500 (1984); Chem. Abstr. 702, 221952~. (197) Hill, R. G., Tomiins, P. E.; Hughes, J. S., Polymer, 26, 1708-12 (1985). (198) Moore, E. R., U.S.Patent US 4591632; Chem. Abstf., 105, 61474r. (199) Wetton, R. E., Dev. folym. Charact., 5 , 179-221 (1986); Chem. Abstr ., 705, 982303. (200) Lobo Fiiho, Eurico de Baros; Reyx, D.; Campistron, I.; Casals, P. F., Makromoi. Chem., 187, 1573-82 (1986); Chem. Absah., 105, 118303s. (201) Hergenrother, W. L., J. Appl. Poly. Sci., 32, 3039-50 (1986); Chem. Abstr., 705, 989760. (202) Barquino, M.; RoquesGarmes, C., Rev. Gen. Caoutch. Piast., 667, 89-93 (1986); Chem. Abstr., 105, 135220d. (203) Jurado, C. W.; Mayhan, K. G., Rubber Chem. Technoi., 5 9 , 84-102 (1986). Edited by: Touchstone, J. C.; Sherma, J., Wiley: New York. (204) Dimonie, V. L.; El-Aasser; M. S.; Vanderhoff, J. W., Tech. Appl. Thin Layer Chromatogr. (Proc.-Bienn. Symp. Thin Layer Chromatogr.), 3rd Meeting 1982, 240-59. Edited by: Touchstone, J. C.; J. C.; Sherma, J., Wiiey: New York. (205) Chaturvedi, Po. N.; Patel, C. K., Makromoi. Chem., 786, 2341-53 (1985).
Analysis of Synthetic Polymers Charles G. Smith,* Richard A. Nyquist, Nels Andrew J. Pasztor, Jr.
H.Mahle, Patrick B. Smith, Steven J. Martin, and
Dow Chemical U.S.A., Analytical Laboratories, 1897 Building, Midland, Michigan 48667 This paper reviews state-of-the-art techniques for the characterization and analysis of synthetic polymers, copolymers, and blends. This review includes techniques for structure determination, separation and quantitation of additives and residual monomers, determination of molecular weight, and the study of thermal properties including degradation mechanisms. A majority of the cited references were obtained from volumes of Chemical Abstracts or CA Selects published between November 1984 and December 1986. For the most part, this review contains references to journals published in English.
chromatogra hy with and without pyrolysis for analysis of plastics. Liegman and Levy (A29) provided an overview of chromatogra hic approaches to polymer analysis while Liebman anb3Wampler (A30) presented an in-depth review of pyrolysis instrumentation, gas chromatography, and coupled techniques such as GC/MS and GC/IR. Aspler (A31) reviewed the theory and applications of inverse gas chromatography. Horna and co-workers (A20, A211 used capillary gas chromatography to separate acrylate and methacrylate monomers. These workers used OV-101,SE-54, and SP-1000phases to determine the retention indices of 38 esters of acrylic and methacrylic acids. Retention behavior of n-alkyl and isoalkyl acrylate esters and their mono- and dihalogen derivatives were examined by Horna et al. ( A 2 3 using several capillary columns.
GAS CHROMATOGRAPHY Denig (A24) reviewed the applications of thin-layer chromatography (TLC), high-pressure liquid chromatography (HPLC), size-exclusion chromatography (SEC), and gas 0003-270018710359-119R$06.5010
0
1987 American Chemical Society
ll9R
