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  • 1
    ISSN: 1520-6882
    Source: ACS Legacy Archives
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    s.l. : American Chemical Society
    Macromolecules 22 (1989), S. 4286-4291 
    ISSN: 1520-5835
    Source: ACS Legacy Archives
    Topics: Chemistry and Pharmacology , Physics
    Type of Medium: Electronic Resource
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  • 3
    ISSN: 1520-5835
    Source: ACS Legacy Archives
    Topics: Chemistry and Pharmacology , Physics
    Type of Medium: Electronic Resource
    Location Call Number Limitation Availability
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  • 4
    ISSN: 1520-5835
    Source: ACS Legacy Archives
    Topics: Chemistry and Pharmacology , Physics
    Type of Medium: Electronic Resource
    Location Call Number Limitation Availability
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  • 5
    Electronic Resource
    Electronic Resource
    s.l. : American Chemical Society
    Macromolecules 25 (1992), S. 45-52 
    ISSN: 1520-5835
    Source: ACS Legacy Archives
    Topics: Chemistry and Pharmacology , Physics
    Type of Medium: Electronic Resource
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  • 6
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Applied Polymer Science 51 (1994), S. 2087-2102 
    ISSN: 0021-8995
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: It is now theoretically possible to obtain absolute accurate values of number-average molecular weight of complex polymers (e.g., branched polymers or copolymers) using size exclusion chromatography (SEC) with only a detector that measures the difference between the eluting polymer solution viscosity and the viscosity of the pure mobile phase (a differential viscometer [DV] detector). However, both precision and accuracy of these “DV M̄n” values are of concern. In this work, the precision of NBS 706 polystyrene was found to be two to three times worse for the DV M̄n than for the conventionally calculated M̄n. Also, regarding accuracy, the DV M̄n values were affected by the location of the universal calibration curve along the retention volume axis (a problem intimately associated with the problem of specifying the correct interdetector volume), the sensitivity of the DV detector to low molecular weights present in the sample, and axial dispersion. Each of these sources of error are examined in turn and two methods of calculating M̄n values are proposed. © 1994 John Wiley & Sons, Inc.
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
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  • 7
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Applied Polymer Science 54 (1994), S. 1455-1461 
    ISSN: 0021-8995
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: A simple method is proposed for using a size-exclusion chromatograph equipped with both concentration and light-scattering detectors to calibrate other chromatographs having only concentration detectors. The method is developed and demonstrated for poly(ethylene terephthalate) in methylene chloride/dichloroacetic acid. It is shown that, in addition to circumventing the need for a light-scattering instrument on other chromatographs to be used for the analysis of PET, precision and accuracy of results are improved over those obtainable with light-scattering detection. The method uses averaging of the light-scattering detector data to establish a correlation between the molecular weight of the polymer of interest and the molecular weight of polystyrene at each retention volume. This correlation can then be used for other instruments employing the same mobile phase and only a concentration detector. Although the method assumes the validity of the universal calibration curve, the actual curve is not required, nor are Mark-Houwink constants or intrinsic viscosities. © 1994 John Wiley & Sons, Inc.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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  • 8
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Applied Polymer Science 47 (1993), S. 1685-1700 
    ISSN: 0021-8995
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Five different types of calibration curve currently used in size exclusion chromatography-differential viscometer (SEC-DV) systems were identified and their use summarized. A simple method of deriving weighting factors for fitting local intrinsic viscosity calibration curves was shown to greatly improve the precision of calculated molecular weight distributions. The problem of reliably extrapolating the fitted curves to allow for differences in sensitivity among detectors has yet to be examined. With regard to Mark - Houwink constants, a method of fitting data from the SEC-DV system to obtain more statistically sound values was derived. For the data used here, the new method involves fitting a plot of logarithm of the local intrinsic viscosity of the sample vs. logarithm of the universal calibration curve parameter, Ji. Results for the data obtained appeared only slightly more precise than those for the traditional method. However, the new method promises improved reliability. © 1993 John Wiley & Sons, Inc.
    Additional Material: 13 Ill.
    Type of Medium: Electronic Resource
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  • 9
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Applied Polymer Science 49 (1993), S. 1359-1374 
    ISSN: 0021-8995
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: A systematic evaluation of two types of light-scattering detectors for size exclusion chromatography (SEC) was completed. The two detectors were the low-angle laser light scattering photometer (LALLS) and the multiangle laser light-scattering photometer (MALLS). Instrument evaluations were performed at both room (30-40°C) and high (135-145°C) temperatures using the polystyrene standard, NBS 706, at room temperature and the polyethylene standard, SRM 1476, at high temperature. Results of the evaluation showed that when experimental uncertainties were taken into account LALLS and MALLS demonstrated equivalent precision and accuracy for molecular weight determination. The main source of inaccuracy found (particularly for SRM 1476) was the sensitivity difference between the light-scattering and the concentration (DRI) detectors; i.e., the DRI detector was unable to measure very low concentrations of very high molecular weight material present in SRM 1476, whereas the light-scattering detectors respond strongly. It was shown that for LALLS the overall weight-average molecular weight (M̄w) for the whole polymer calculated using an equation that did not require the DRI detector output circumvented this sensitivity problem while assuming that the low angle used was sufficiently close to zero. Use of this equation for MALLS is possible by extrapolating data from all angles used to obtain a light-scattering chromatogram at zero angle. However, this possibility was not examined here. A particular advantage of MALLS over LALLS is that MALLS can provide the z-average root mean square radius (commonly referred to here and in other light-scattering literature as the “radius of gyration”) values from the same data as those used to obtain molecular weight values. Although the radius of gyration values at each retention volume were not as precise as the corresponding weight-average molecular weights, at room temperature, precision was better than 2% for a significant portion of the chromatogram. © 1993 John Wiley & Sons, Inc.
    Additional Material: 23 Ill.
    Type of Medium: Electronic Resource
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  • 10
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Applied Polymer Science 45 (1992), S. 1983-1994 
    ISSN: 0021-8995
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Wholly aromatic polyamides, including poly(1,4-phenyleneisophthalamide) and poly(1,4-phenyleneterephthalamide) are N-methylated to render them soluble in N,N-dimethylformamide, a common size-exclusion chromatography eluent. The procedure N-methylates 50-55% of the total amide linkages in these two examples, permitting reproducible measurement of their absolute molecular weight distributions using differential viscometry detection. There is no observable degradation in molecular weight resulting from the N-methylation, provided the excess methylating reagent is destroyed shortly after completion of the derivatization by quenching with potassium acetate. The validity of the molecular weight data obtained by the method is confirmed by light-scattering measurements on derivatized polymer and by comparison to the molecular weight of underivatized polymer that can be approximated from the intrinsic viscosity in concentrated sulfuric acid. The method is applicable to a variety of wholly aromatic polyamide structures. Examples are given.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
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