ASTM E222-17 Standard Test Methods for Hydroxyl Groups Using Acetic Anhydride Acetylation.pdf
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1、Designation: E222 17Standard Test Methods forHydroxyl Groups Using Acetic Anhydride Acetylation1This standard is issued under the fixed designation E222; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A
2、number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 These test methods cover the determination of hydroxylgroups attached to primary and secondary carbon atoms inaliphatic and alicyclic
3、compounds and phenols.1.2 Three test methods are given as follows:SectionsTest Method A (Pressure Bottle Method) 814Test Method B (Reflux Method) 1622Test Method C (Perchloric Acid Catalyzed Method) 24301.2.1 Test Method A is recommended for general use. TestMethod B is included to give a standard p
4、rocedure for themethod that has been used widely. Test Method C is recom-mended when the results are required in a minimum period oftime or where ambient temperature for the reaction is desired.1.2.2 The results obtained using Test Methods A and B willbe essentially the same, but the results obtaine
5、d using TestMethod 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 testmethod. The precision of Test Methods A and C is consistentover a wide range of hydroxyl content (tested over hydroxylnumber
6、range of 250 to 1600), whereas Test Method B is lessprecise at the higher hydroxyl content level than it is at thelower hydroxyl content level. In general, Test Method A isapproximately two-fold as precise as Test Method C. TestMethod B has approximately the same precision as TestMethod C at the low
7、er hydroxyl content level but poorerprecision at the higher hydroxyl content level.1.2.4 The interferences are essentially the same for the threemethods. Some compounds can be analyzed using Test Meth-ods A or B but not using Test Method C because of interferingreactions of the strong acid catalyst
8、with the compound beinganalyzed or the acetate product formed in the determination.However, because of its increased reactivity, Test Method C isapplicable for determination of some compounds, particularlysterically hindered secondary alcohols, which react too slowlyor not at all in Test Methods A a
9、nd B.NOTE 1Other methods for determination of hydroxyl groups are givenin Test Methods D1957, D2195, E326, E335, and E567.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 Review the current appropriate Safety Data Sheets(
10、SDS) for detailed information concerning toxicity, first aidprocedures, and safety precautions.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health pr
11、actices and determine the applica-bility of regulatory limitations prior to use. Specific hazardsstatements are given in Section 7.1.6 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for
12、 theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD1957 Test Method for Hydroxyl Value of Fatty Oils andAcids (Withd
13、rawn 2007)3D2195 Test Methods for Pentaerythritol (Withdrawn 2011)3D6809 Guide for Quality Control and Quality AssuranceProcedures for Aromatic Hydrocarbons and Related Ma-terialsE180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemical
14、s (Withdrawn 2009)3E200 Practice for Preparation, Standardization, and Storageof Standard and Reagent Solutions for Chemical AnalysisE203 Test Method for Water Using Volumetric Karl FischerTitration1These test methods are under the jurisdiction of ASTM Committee D16 onAromatic, Industrial, Specialty
15、 and Related Chemicals and are the direct responsi-bility of Subcommittee D16.15 on Industrial and Specialty General Standards.Current edition approved June 1, 2017. Published July 2017. Originally approvedin 1963. Last previous edition approved in 2010 as E222 10. DOI: 10.1520/E0222-17.2For referen
16、ced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onww
17、w.astm.org.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardi
18、zation established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1E326 Test Method for Hydroxyl Groups by Phthalic Anhy-dride Esterification (Withdrawn 2001)3E
19、335 Test Method for Hydroxyl Groups by PyromelliticDianhydride Esterification (Withdrawn 2002)3E567 Test Method for Tertiary Hydroxyl Groups with Hy-drogen Bromide (Withdrawn 1996)33. Terminology3.1 Definitions:3.1.1 hydroxyl numberthe milligrams of potassium hy-droxide equivalent to the hydroxyl co
20、ntent of1gofmaterial.In the case of a pure compound, the hydroxyl number isinversely proportional to the hydroxyl equivalent weight:equivalent weight g/equivalent! 556100hydroxyl number(1)4. Significance and Use4.1 Hydroxyl is an important functional group, and knowl-edge of its content is required
21、in many intermediate and enduse applications. The test methods described herein are for thedetermination of primary and secondary hydroxyl groups andcan be used for the assay of compounds containing them.5. Interferences5.1 Unless stated otherwise, the following interferencesapply to all three test
22、methods:5.1.1 Pentavalent nitrogen compounds, amides, someethers, and some carbonyl compounds may interfere with theaccuracy of the test method.5.1.2 Tertiary alcohols, cyanohydrins, some hydroxylatedfatty acids, certain substituted phenols, and some polyhydroxylcompounds will react in a nonstoichio
23、metric manner.5.1.3 Primary and secondary amines and mercaptans usu-ally will react quantitatively along with the hydroxyl group.5.1.4 Excessive amounts of water in the sample will inter-fere by consuming the reagent. Provisions are made to accom-modate a small amount of water by adjustment of the s
24、amplesize used for the analysis.5.1.5 Free acids interfere by consuming the standard alkalisolution, and strong bases interfere by consuming an equiva-lent amount of acetic acid; provisions for determining andapplying corrections for these interferences are included in thetest methods. Some of the h
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