ASTM International - ASTM E222-00(2005)e1
Standard Test Methods for Hydroxyl Groups Using Acetic Anhydride Acetylation
|Publication Date:||1 March 2005|
|ICS Code (Chemical analysis):||71.040.40|
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... View More
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.View Less
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:
|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 the 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 E567.