ASTM D4273 Determination of Primary Hydroxyl Content of Polyether Polyols

ASTM D4273 is used to determine the primary hydroxyl content of ethylene oxide (EO)-propylene oxide (PO) polyether polyols used to form flexible polyurethane foams. This method is highly efficient for polyether polyols with primary hydroxyl contents of 10 to 90%. The values are considered as a standard when expressed in SI units.

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    Scope:

    ASTM D4273 delivers information about the relative reactivities of polyols. It also provides a good balance between hydrophobicity and reactivity. Sometimes, poor reactivity ethylene oxide is added to the tail of the polyether polyols.

    Procedure:

    For ASTM D4273, a solution of the polyol sample in deuterated acetone having tetramethyl silane (TMS) as an internal standard is prepared. Then transfer a suitable amount of the sample solution to an NMR tube. The NMR tube is then placed in a spinner and the optimized field-homogeneity is acquired from the NMR data. Apply a spectral weighting function (apodization) to the Free Induction Decay and Fourier Transform (FID). Internal TMS reference is set to around 0 ppm. The primary hydroxyl peaks usually resonate between 61.0 and 62.5 ppm, while the secondary hydroxyl peaks generally resonate between 65.5 and 67.5 ppm.

    Specimen size:

    The suggested broadening line value is 1 per acquisition time.

    Data:

    The following equation is used in ASTM D4273 to calculate the primary hydroxyl content of polyether polyols

    Primary hydroxyl, % 5 = A* 100/A+B

    A= primary hydroxyl peak

    B= secondary hydroxyl peak

    Conclusion:

    ASTM D4273 delivers information about the relative reactivities of polyols.

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