Previous Page
TABLE 1. cont'd Method of fractionation
Polymer
Solvent or solvent/nonsolvent mixture
Remarks
Refs.
Ethanol/water 300C Poly(di-n-tetradecyl itaconate) PoIy(I-n-tetradecyloxycarbonylmethyl)-l-(tetradecyloxycarbonyl)ethylene) Fractional precipitation Benzene/methanol Poly(di-«-undecyl itaconate) Turbidimetric titration Benzene/methanol 300C Chloroform/methanol 300C
3348 3374 3368 3368
1.6. POLY(VINYL ETHERS) PolytS-tt^'^'-bis^^-n-alkoxybenzoylloxyjbenzylloxylcarbonyllbicyclotl.l.lJhept-l-enes Fractional precipitation Tetrahydrofuran/hexane Poly (ally loxyethylene) Poly (ally I vinyl ether) Chromatography Tetrahydrofuran Poly(butoxyethylene) Fractional precipitation Benzene/methanol Poly(2-chloro-4-methylpenthyl 4 '[[8-vinyl oxy]octyl]oxy]biphenyl-4-carboxylete) Chromatography Tetrahydrofuran Poly(2-chloroethoxyethylene) Chromatography Chloroform Poly(hexadecyloxyethylene) Fractional precipitation n-Heptane/acetone Poly(isobutoxyethylene) Chromatography Chloroform Tetrahydrofuran Extraction
Acetone, benzene, ethyl ether, methylene chloride Fractional precipitation Toluene-butanone (1: l)/ethanol Poly(isobutyl propenyl ether) [Poly(l-isobutoxy-2-methylethylene)] Chromatography Chloroform Poly(isobutyl vinyl ether) Chromatography Chloroform Toluene, chloroform Poly(isopropyloxyethylene)
Acetone, benzene, ethyl ether, methylene chloride Poly 5-[[[n-[(4/-methoxy-4-biphenyl)oxy]alkyl]-oxy]carbonyl]bicyclo [2.2.1]hept-2-enes Chromatography Tetrahydrofuran Poly(methoxyethylene) Chromatography Tetrahydrofuran Fractional precipitation Benzene/w-hexane, n-heptane or decane Chloroform/heptane Methanol
2676 SEC u-bondagel
2989 2977
SEC, styragel, 4O0C, (r,s) SEC, styragel SEC, styragel SEC u-styragel SEC, styragel Oppanol C Lowering temp.
2865
SEC, styragel SEC, styragel SEC, styragel, analytical and preparative
Extraction
Fractional solution Poly (vinyl isobutyl ether) see Poly(isobutoxyethylene) Poly(vinyl methyl ether) see Poly (methoxyethylene)
Toluene/heptane Water Toluene/petroleum ether
2569 1300 1760 2212 2856 1244,1827 1972
1299 1597,1692 1569 584 1972
SEC, styragel SEC, u-styragel
1744 2857 2025
Lowering temp. 65 to 25°C and to3°C Raising temp. Continous extraction (CPF)
247 3352 246 2025 2587
1.7. POLY(VINYL ALCOHOL), POLY(VINYL KETONES), POLY(VINYL HALIDES), POLY(VINYL NITRILES) Poly(acrylonitrile)
Chromatography
Chloroform Dimethylacetamide Dimethylformamide
Fractional precipitation
Dimethyl sulfoxide-aq. hydrochloric acid/toluene Dimethyl sulfoxide/toluene Dimethylformamide Dimethylformamide/ethanol Dimethylformamide/lauric alcohol Dimethylformamide/ligroin Dimethylformamide/n-heptane
SEC, styragel SEC, styragel SEC SEC, Merck gel SEC, Sephadex SEC, styragel, 700C 35°C 35°C 110-90 0 C pH 6.0, ageing period 50-60 0 C 600C
1781 330,1965 985,1846 1461 1781 1142 1715 946,947,1414, 1554,1558,1716 2888 2173 3071 1111 267,339,383,594, 945,948,1371, 1626,2167
References page VII-438
TABLE 1. cont'd Polymer
Method of fractionation
Solvent or solvent/nonsolvent mixture
Dimethylformamide/n-heptaneether (1/1) Hydroxy acetonitrile ethanol/benzene Hydroxy acetonitrileethanol/toluene Nitric acid 60%/n-butanol Fractional solution Dimethylformamide/rc-butylacetate Dimethylformamide/tt-heptane Sedimentation velocity Dimethylformamide Thermal diffusion Dimethylformamide Turbidimetric titration Dimethylformamide/dioxaneheptane (1/1) Poly(tert-butyl vinyl ketone) Fractional precipitation Acetone/methanol Poly(chlorotrifluoroethylene) Fractional precipitation Dichlorobenzotrifluoride/diethyl phthalate(3/l) Poly(a-chlorovinyl acetic acid) Poly((carboxychloromethyl)ethylene) Fractional precipitation Methanol/water Poly(diketene) Extraction Acetone, dioxane Ethyl ether, acetone benzene, toluene Methanol, ethyl ether, benzene, acetone Poly(isopropenyl methyl ketone) PoIy[I-acetyl-1-methylethylene) Chromatography Tetrahydrofuran Poly(methyl vinyl ketone) Poly(acetylethylene) Extraction Acetone Poly(phenyl vinyl ketone) Poly(benzoylethylene) Chromatography Tetrahydrofuran Extraction Acetone Poly(trifluoroethylene) Chromatography Tetrahydrofuran Poly(vinyl alcohol) Poly(hydroxyethylene) Brownian diffusion Water Chromatography Acetonitrile -f 50 mM lithium chloride Sodium nitrate 0.25 M/sodium phOvSphate (monobasic) 0.01 M Water
Extraction Fractional crystallization Fractional precipitation
Fractional solution
Poly(vinyl chloride)
Thermal diffusion Chromatography
Foam method amorphous-crystalline Water Water/1-propanol Water/acetone Water/acetone-propanol Water/>z-propanol Water/methyl acetate: methanol (3:1) Water/n-propanol Water Benzene/tetrahydrofuran (6/4) Cyclohexanone/methanol Hexamethyl phosphoramide Tetrahydrofuran
Remarks
Refs. 1285,3131 1714
35°C 5°C 900C, film extraction Extraction
Solvent volatilization, 1500C, KeI-F
1714 945 935 1800 2046 1862,1863,1868 2477 1140 1618,2449
Boiling
1719 959,1635 3564
Boiling
3529
SEC
1979
Sol. and insol.
3249
SEC, styragel Sol. and insol. SEC, u-styragel
260,1095,3251 3249 486 924 2409
SEC, aquagel-OH
2121
SEC SEC, aquagel-OH SEC, spheron SEC, TSK gel
1806 2122 150 150,1224 1412,1674
Stirring 25°C
Film extraction 65°C
3535,3536,3537 2430 754,759,1861,3127 3222 2090,2429,2815, 3493,3535 934
295 931,1861,1863 SEC, 25°C 1984 Precipitation chromatogr., 25-600C 671 SEC, styragel, 1030C 2050 SEC 1032 SEC, u-styragel, 25°C 416,2311 SEC, Porous silica gel, 25°C 1742,1885,1974 SEC, styragel, 25°C, 30°C, 5,90,284,540,543, analytical 880,932,1035,1087, 1088,1165,1314,1315, 1641,1745,2389,2474, 2677,2769,2822,2922, 3170,3228,3239,3354
TABLE 1. cont'd Polymer
Method of fractionation
Extraction
Extraction (CPF) Field flow Fractional precipitation
Solvent or solvent/nonsolvent mixture
Acetone, chloroform, tetrahydrofuran Acetone-methanol mixtures Benzene, chloroform, acetone, tetrahydrofuran and cyclohexanone Dioxane, tetrahydrofuran, cyclohexanone Mixtures, ethyl alcohol, butanone, tetrahydrofuran, chloroform Tetrahydrofuran/water Water + 0.1 % FL-70 tensoactive Acetone -f- chlorobenzene -fcyclohexane/methanol Cyclohexanone/ethylene glycol Cyclohexanone/methanol Cyclohexanone/methanol-water Cyclohexanone/rt-butanol Liquid ethylene at 132 bar and 800C Tetrahydrofuran/ethanol Tetrahydrofuran/methanol Tetrahydrofuran/water
Remarks
Refs.
SEC, styragel, 35°C, preparative SEC, ultrastyragel, 35°C Hot and cold
1229 824 2455
Selective extraction
416 1886
At several temp.
2050 1922 1032 1902 2167
Sedimentation, latex beads
981,1886,2132,2308 432,443,1091, 1164,2168 3442,3585 782 3298
Releasing pressure
1316 288,1091,3443 90,170,244,370, 371,921,1035,1317,
1717,1741,1782,1886, 2132,2251,2342,2588, 2591,2592,3133, 3353,3378 Fractional solution
Sedimentation analysis Thermal diffusion Turbidimetric titration Poly(vinyl fluoride) Fractional precipitation Poly(vinyl methyl ketone) Extraction Pcly(vinylidenefluoride)PoIy(1,1-difluoroethylene) Chromatography Fractional precipitation
Fractional solution Freeze-extraction
Cyclohexanone/ethylene glycol Cyclohexanone/methanol Methyl isobutyl ketone Tetrahydrofuran/water Water/acetone Cyclohexanone Cyclohexanone Cyclohexanone/rc-heptane-carbon tetrachloride (9:1) Dimethylformamide/water Acetone Dimethylacetamide Acetophenone/o-dichlorobenzene Dimethylformamide/aq. acetic acid Tetrahydrofuran/petroleum ether Acetophenone Chloroform, petroleum ether, carbon tetrachloride Dioxane
Column extraction Film extraction
981,983 1171 1860 3069 1015 1805 1011,1020,1170
44°C Continous method 2478
3573 3249
Soluble and insoluble SEC, styragel 136 and 158°C
3446 3446 40 1607 2359 418
Separation according degree of crystallinity
3509
1.8. POLY(VINYL ESTERS) Poly(vinyl acetate)
Chromatography
Acetonitrile 4- 50 mM aq. lithium chloride Benzene/isopropanol Dimethylformamide
2409 Activated carbon -f supercel Precipitation chromatogr. large scale, 28-600C SEC, styragel
601 501 2418
References page VII-438
TABLE 1. cont'd Polymer
Method of fractionation
Distribution between immiscible liquids Fractional precipitation
Fractional solution
Selective adsorption Thermal diffusion
Turbidimetric titration Poly(vinyl /7-trimethyl silyl benzoate) Fractional precipitation 1.9.
Solvent or solvent/nonsolvent mixture
Remarks
Methyl ethyl ketone Tetrahydrofuran
SEC, silica gel SEC, styragel
Toluene Trichlorobenzene Benzene-methanol-water
SEC, ultrastyragel SEC, preparative SEC Countercurrent
AcetoneM-heptane Acetone/n-hexane Acetone/rc-pentane Acetone/petroleum ether Acetone/water Acetone/water-methanol (1:1) Benzene/cyclohexane Benzene/isopropanol Butanone/cyclohexane Chlorobenzene/cyclohexane Dioxane/isopropanol Dioxane/n-heptane Ethyl acetate/cyclohexane Methanol/water Methanol/water, chloroform/methanol Methyl acetate/petroleum ether Methyl and ethyl acetate/petroleum ether Methyl isobutyl ketone Tetrahydrofuran/methanolwater (1:1) Water/acetone Acetone Benzene Chloroform Dioxane Ethyl acetate Isoamyl acetate Methanol Toluene Acetone/water
35°C, branched 250C
25°C 25° C 25°C 25°C 35°C, branched
Refs. 1453 284,407,496,681, 826,1087,1088,1910, 2389,2417,2418,2860 2037 149 3401 2754 1322,1323 286,909,2249,2980 1865 2198,2706,3126 315,937,2217,2336, 2418,2468 1148,1149,1576,3405 2535 832 2524 2524 832 2524 1696,2524 310,311,1955 2460 937
Film extraction 25°C Carbon
Benzene/methanol
295,933,935 I860 496 1004 1575 1865 1865 1865 1865 1865 1865 1863,1865 58,2270 1351
POLY(STYRENES)
Poly(p-aminostyrene) Poly(p-bromostyrene)
Chromatography Chromatography
Poly(p-terf-butylstyrene)
Chromatography
Poly(p-chloro-a-methylstyrene) Poly(m-chlorostyrene) Poly(o-chlorostyrene) Poly(p-chlorostyrene)
Chromatography Fractional precipitation Fractional precipitation Chromatography Fractional precipitation
Tetrahydrofuran o-Dichlorobenzene Tetrahydrofuran Tetrahydrofuran Tetrahydrofuran/water Tetrahydrofuran Benzene/methanol Benzene/methanol Butanone o-Dichlorobenzene Tetrahydrofuran Benzene/methanol
Butanone/methanol PolyWAT^'^^-tetraethyl^-isopropenylphenylphosphosnous diamide) Chromatography Tetrahydrofuran + 2% Af-methylpyrrolidine)
SEC SEC, styragel SEC, ^-styragel SEC, styragel, 45°C SEC, styragel SEC, styragel, 25°C 35°C 35°C SEC, styragel SEC, styragel SEC, u-styragel
SEC
3520 1242 2013 1811 989 158,1911 2087 2088 1296 1242 1666,2013 210,354,1282,1459, 1808,2089,2227 3135 1585
TABLE 1. cont'd Method of fractionation
Polymer
Poly(p-fluoromethylstyrene) Chromatography Poly(p-fluorostyrene) Chromatography Poly(4-hydroxystyrene) Chromatography Poly(p-isopropyl-a-methylstyrene) Chromatography
Solvent or solvent/nonsolvent mixture
SEC, styragel SEC, styragel SEC, styragel
138 1242 3566
Tetrahydrofuran
SEC, u-styragel SEC, styragel, 25°C SEC, u-styragel, preparative
2013 1918,2007,2008 2008
Poly((p-methoxyphenyl)ethylene)
Chromatography
Fractional precipitation Turbidimetric titration Poly (methyl 4-vinylbenzoate) Poly(oc-methylstyrene)
Refs.
Tetrahydrofuran o-Dichlorobenzene Tetrahydrofuran
Toluene Poly(p-methoxystyrene)
Remarks
Chromatography
Butanone Chloroform o-Dichlorobenzene Tetrahydrofuran Butanone/ethanol Benzene: butanone (3: l)/ethanol Tetrahydrofuran
SEC, styragel SEC, styragel SEC, styragel SEC, u-styragel Column extraction, 25°C glass beads
1296 1734 1242 2013 524,2619 1152
SEC, styragel, 400C
1309
Benzene/n-hexane Carbon/tetrachloride/heptane (2:1) GPC, modified silica gel 40°C Tetrahydrofuran
Precipitation chromatogr., 10-580C TLC, silical gel
3527 978
[Poly(p-methoxyphenyl)ethylene)]
Chromatography
2667 2108 SEC, n-styragel, 25°C 1661,2013 SEC, modified silica gel 400C 2667 SEC, styragel 558,835,955,1245,
1609,1614,1631,1917, 1918,2420,2767, 3504,3527 Toluene Toluene/methanol Benzene/methanol
SEC, styragel
Coacervation Fractional precipitation
Low temp. 21.4 to 10.40C
Fractional solution
Cyclohexane Methyl ethyl ketone - benzene (6: l)/methanol Toluene/methanol Cyclohexane
Sedimentation velocity Turbidimetric titration Poly(2,4,6-trimethylstyrene) Poly(2,4-dimethylstyrene) Poly(2,6-dimethylstyrene) Poly(m-methylstyrene) Poly(o-methylstyrene) Poly(/?-methylstyrene) Poly((3-methylstyrene) Poly(styrene)
Chromatography Chromatography Fractional precipitation Chromatography Chromatography Fractional precipitation Chromatography Chromatography Chromatography Brownian diffusion Chromatography
Cyclohexane Cyclohexane/«-octanol Methylcyclohexane o-Dichlorobenzene o-Dichlorobenzene Benzene/methanol o-Dichlorobenzene o-Dichlorobenzene Benzene/methanol o-Dichlorobenzene Butanone o-Dichlorobenzene Tetrahydrofuran Benzene, cyclohexane 1,2,4-Trichlorobenzene
Column extraction, increasing temp., glass beads 35°C Lowering temp. SEC, styragel SEC, styragel SEC, styragel SEC, styragel 35.8°C SEC, styragel SEC, styragel SEC, styragel SEC, styragel SEC, styragel, 145°C Syndiotactic, 145°C SEC, 135°C, isotactic ThFFF
1,2-Dichlorobenzene 1,2-Dichloroethylene, perchloroethylene, tetrahydrofuran, ethylbenzene, w-dodecane/tetrahydrofuran, cyclohexane/1,2-dichloroethylene Acetone and acetone/ TLC, gradient elution tetrahydrofuran (7:3) Acetone/chloroform TLC
1042 471 642,655,944, 1613,2810 2407 1139 2405,2810 944,2407,3527 942,2116,3527 2702 634,2660 1242 1242 3392 1242 1242 553 1242 1296 1242 2420 2079 572,2729 1693 1957 3008
2480 2093 References page VII-438
TABLE 1. contd Polymer
Method of fractionation
Solvent or solvent/nonsolvent mixture Acetone/chloroform mixture (8:2) Acetone/methanoi Benzene
Benzene, acetone butanone, ethanol Benzene, carbon tetrachloride, methanol, petroleum ether Benzene/hexane (34.7/65.3)
Remarks
Refs.
TLC, constant elution
2480
TLC 2093 SEC, 2050C Supercritical fluid 1495 chromatogr. 41-62 bar SEC, ethylene dimethacrylate gel 1291 SEC, styragel 984,1263, 1732,1984 TLC, gradient cone. 1571 67 TLC, gradient cone, -2-(Af,iV-dimethylcarbamoyioxy)ethyl methacrylate) Chromatography Tetrahydrofuran SEC, styragel, 28°C Poly(n-butyl acrylate-a/f-propylene) Chromatography Tetrahydrofuran SEC, styragel Poly(di-n-butyl itaconate-staMnono butyl itaconate) Fractional precipitation Acetone/petroleum ether Poly(rc-butyl methacrylate-co-glycidylmethacrylate-co-methacrylic acid Fractional precipitation Dioxane/water Poly(tert-butyl methacrylate-co-methacrylic acid) Chromatography Tetrahydrofuran SEC, styragel Poly(/2-butyl methacrylate-co-1-naphthyl methacrylate) Chromatography Tetrahydrofuran Random, SEC, 400C Poly(n-butyl acrylate-co-2-hydroxyethylmethacrylate) Chromatography Dimethylformamide SEC Poly(n-butyl acrylate-co-vinyl acetate) Chromatography Tetrahydrofuran SEC Poly(butylene adipate-co-succinate) Chromatography Tetrahydrofuran SEC Poly(N-butylmaleimide-a/Msobutene) Chromatography Chloroform SEC, ja-styragel, 38°C Poly(A^-5^c-butylmaleimide-