ASTM D4274 Standard Test Methods for Testing Polyurethane Raw Materials: Determination of Hydroxyl Numbers of Polyols

ASTM D4274 test method is used to determine the amount of primary and secondary hydroxyl groups present in polyester and polyether polyols. They also apply to numerous other things that include hydroxyl. This test method determines several associated procedures which are appropriate to polyester and polyether polyols.

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 Introduction to ASTM D4274

ASTM D4274 generally applies to those substances that contain hydroxyl groups but mainly it aims to analyze hydroxyl groups present in polyester and polyether polyols. Several procedures that are used in compliance with D4274 include Acetic Anhydride Pressure Bottle method, Phthalic Anhydride Pressure Bottle method, Phthalic Anhydride Reflux method, Imidazole–Catalyzed Phthalic Anhydride Pressure Bottle method  and Imidazole-Catalyzed Pyromellitic Dianhydride Esterification.

The applicability of ASTM D4274 is significant in industries involved in the production and quality control of polyurethane materials. This includes manufacturers of foams, coatings, adhesives, sealants, elastomers, and other polyurethane-based products.

ASTM D4274 Test Procedure 

SamplingPolymers and polyethers have mixed molecular weight compounds that fractionate during solidification. Resins are melted and mixed  before sample removal, as many polyols are hygroscopic, requiring minimal atmospheric moisture exposure. The standard specifies that the sample quantity of polyol to be used for the test should be 10.0 ± 0.1 grams. 
Test Setup and ExecutionThe ASTM D4274 test procedure involves weighing a polyol sample, dissolving it in a solvent, adding acetic anhydride, titrating with a standardized sodium hydroxide solution, using phenolphthalein as an indicator. The titration process requires reagents, equipment, and a phenolphthalein indicator. Repeat the procedure with replicate samples for accuracy. The hydroxyl number is calculated using the ASTM D4274 equation.

ASTM D4274 Test Results 

The hydroxyl numbers present in polyols are determined by performing this test method successfully. The number of hydroxyl groups, which in turn measures the average functionality of the polyol, is expressed in milligrams of potassium hydroxide (KOH). The equivalent weight of the polyol is calculated using the hydroxyl number, which represents the molecular weight of the polyol per hydroxyl group. These results help determine the stoichiometry and balance of polyurethane systems, ensuring desired properties and performance.

Tests Related to ASTM D4274

The test methods relevant to ASTM D4274 include ASTM D1638 for acid value of organic coating materials, ASTM D1957 for hydroxyl value of fatty oils and acids, ASTM D4273 for primary hydroxyl content of polyether polyols, and ASTM D4671 for unsaturation of polyols. These methods provide additional characterization and analysis of polyurethane raw materials, including polyols, and can be useful in evaluating their properties and suitability for polyurethane applications.

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