ASTM E222 - 10

    Standard Test Methods for Hydroxyl Groups Using Acetic Anhydride Acetylation

    Active Standard ASTM E222 | Developed by Subcommittee: E15.01

    Book of Standards Volume: 15.05


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    Significance and Use

    Hydroxyl is an important functional group, and knowledge of its content is required in many intermediate and end use applications. The test methods described herein are for the determination of primary and secondary hydroxyl groups and can be used for the assay of compounds containing them.

    1. Scope

    1.1 These test methods cover the determination of hydroxyl groups attached to primary and secondary carbon atoms in aliphatic and alicyclic compounds and phenols.

    1.2 Three test methods are given as follows:

    Sections
    Test Method A (Pressure Bottle Method) 8-14
    Test Method B (Reflux Method) 15-21
    Test Method C (Perchloric Acid Catalyzed Method) 22-28

    1.2.1 Test Method A is recommended for general use. Test Method B is included to give a standard procedure for the method that has been used widely. Test Method C is recommended when the results are required in a minimum period of time or where ambient temperature for the reaction is desired.

    1.2.2 The results obtained using Test Methods A and B will be essentially the same, but the results obtained using Test Method C will be higher (up to approximately 4 % relative) than those obtained using the other two methods.

    1.2.3 Statements on precision are included with each test method. The precision of Test Methods A and C is consistent over a wide range of hydroxyl content (tested over hydroxyl number range of 250 to 1600), whereas Test Method B is less precise at the higher hydroxyl content level than it is at the lower hydroxyl content level. In general, Test Method A is approximately two-fold as precise as Test Method C. Test Method B has approximately the same precision as Test Method C at the lower hydroxyl content level but poorer precision at the higher hydroxyl content level.

    1.2.4 The interferences are essentially the same for the three methods. Some compounds can be analyzed using Test Methods A or B but not using Test Method C because of interfering reactions of the strong acid catalyst with the compound being analyzed or the acetate product formed in the determination. However, because of its increased reactivity, Test Method C is applicable for determination of some compounds, particularly sterically hindered secondary alcohols, which react too slowly or not at all in Test Methods A and B.

    1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.

    1.4 Review the current appropriate Material Safety Data Sheets (MSDS) for detailed information concerning toxicity, first aid procedures, and safety precautions.

    1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazards statements are given in Section 7.

    Note 1—Other methods for determination of hydroxyl groups are given in Test Methods D1957, D2195, E326, E335, and .


    2. Referenced Documents (purchase separately) The documents listed below are referenced within the subject standard but are not provided as part of the standard.

    ASTM Standards

    D1193 Specification for Reagent Water

    D1957 Test Method for Hydroxyl Value of Fatty Oils and Acids

    D2195 Test Methods for Pentaerythritol

    E180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial and Specialty Chemicals

    E200 Practice for Preparation, Standardization, and Storage of Standard and Reagent Solutions for Chemical Analysis

    E203 Test Method for Water Using Volumetric Karl Fischer Titration

    E326 Test Method for Hydroxyl Groups by Phthalic Anhydride Esterification (Discontinued 2001)

    E335 Test Method for Hydroxyl Groups by Pyromellitic Dianhydride Esterification

    E567 Test Method for Tertiary Hydroxyl Groups with Hydrogen Bromide


    ICS Code

    ICS Number Code 71.040.40 (Chemical analysis)

    UNSPSC Code

    UNSPSC Code 12352100(Organic derivatives and substituted compounds)


    DOI: 10.1520/E0222-10

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