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  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 39 (1994), S. 557-563 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Copoly(styrene/methyl methacrylate) ; Gradient elution ; Precipitation chromatography of polymers ; Solubility of polymers
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Copolymers from styrene and methyl methacrylate (MMA) were separated by both normal and reversedphase gradient chromatography. Both modes could be performed by sudden-transition gradients where the polymers were injected into a non-solvent whose polarity was either rather low (e.g.,n-heptane) or high (e.g., acetonitrile). Then the solvent strength of the starting eluent was rapidly increased to a given level by addition of dichloromethane. Under properly defined conditions, the sample components still remained on the column. Elution could be triggered off by the steady addition of another non-solvent whose polarity was opposite of that of the starting non-solvent. Thus, the mixture of five copolymers with MMA content ranging from 14 to 84% could be separated on a polar cyanopropyl column by injection inton-heptane and elution through acetonitrile (normal phase mode) and on a RP C18 column by injection into acetonitrile and elution throughn-heptane (reversed-phase mode), provided that in both modes about 30% dichloromethane was added to the starting non-solvent. The elution sequence in the reversed-phase mode was opposite to that in the normal-phase mode, obeying the approved polarity rules of chromatography in both cases.
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  • 2
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Copoly(styrene/ethyl methacrylate) ; Gradient elution ; Precipitation chromatography of polymers ; Solubility of polymers
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Copolymers from styrene and ethyl methacrylate have been separated according to composition byn-heptane gradients on a C18 bonded phase after injection into acetonitrile and subsequent sudden transition to a concentration of either dichloromethane or tetrahydrofuran between 30 and 50% or 20 and 50%, respectively. Acetonitrile is a polar non-solvent for the copolymers under investigation and ensures proper retention of the samples on a non-polar stationary phase. Dichloromethane and tetrahydrofuran are good solvents of moderate polarity. The addition of, e.g., 30 vol% of one of these solvents increased the dissolution power of the starting eluent but not to the extent necessary for elution. The latter was achieved by the addition ofn-heptane, which is a non-solvent for the polymers investigated. Thus, its eluting power must be understood as the consequence of its modifying effect on the polarity of the eluent mixture. The higher the content of copolymer in ethyl methacrylate the earlier it was eluted. Since acetonitrile andn-heptane are only partly miscible, phase diagrams were measured after the addition of either tetrahydrofuran or dichloromethane as a third component. Homogeneous mixtures were obtained on addition of about 30% solvent (one of both of the latter).
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  • 3
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Copoly(styrene/ethyl methacrylate) ; Gradient elution, sudden transition ; Precipitation chromatography of polymers ; Solubility of polymers
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Copolymers from styrene and ethyl methacrylate have been separated according to composition by methanol gradients on a cyanopropyl column after injection inton-heptane and a subsequent rapid increase of dichloromethane (DCM) concentration from zero to a constant value in the range from 10 to 40%. Retention and resolution in sudden-transition gradients increased with decreasing DCM concentration. The gradient rate was varied between 2.5 and 7.5%/min with optimum resolution at 2.5% min. At a level of 20% DCM and a gradient rate of 5%/min, the separation of a mixture of five copolymers in a sudden-transition gradient was the same as with the corresponding common gradient, i.e., with injection into a mixture ofn-heptane and 20% DCM. Elution was also achieved at a level of 20% DCM by continuous addition of tetrahydrofuran (THF) instead of methanol. With THF, the peaks appeared later than with methanol in spite of the fact that methanol is a non-solvent and THF a good solvent for the polymers investigated. This indicates that elution was, in the first instance, caused by the polarity of the eluent. The elution characteristics of the copolymers in the system heptane/methanol at constant DCM concentration were basically similar to the already known characteristics iniso-octane/methanol at constant THF concentrations.
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  • 4
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Copoly(styrene/acrylonitrile) ; Gradient elution ; Precipitation chromatography of polymers ; Solubility of polymers
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Copolymers from styrene and acrylonitrile could be separated according to composition by gradient elution through methanol after injection inton-heptane and sudden addition of 50, 60, or 70 vol% tetrahydrofuran. The peak sequence was the same as with a common binary gradientn-heptane/tetrahydrofuran, i.e., retention increased with acrylonitrile content of the samples. With copolymers containing 37, 31, or 26% acrylonitrile, the elution characteristics in the ternary systems could be logically extrapolated towards the points measured in the corresponding binary gradient system.
    Type of Medium: Electronic Resource
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