ASTM_D_1631_-_10.pdf

Designation:D163110Standard Test Method forWater in Phenol and Related Materials by the IodineReagent Method1This standard is issued under the fixed designation D1631;the number immediately following the designation indicates the year oforiginal adoption or,in the case of revision,the year of last revision.A number in parentheses indicates the year of last reapproval.Asuperscript epsilon()indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1.Scope*1.1 This test method covers the determination of water inphenol and related materials such as cresols,xylenols,naph-thalene,pyridine,and quinoline.1.2 This test method has been found applicable to a varietyof materials varying in water content from 100 mg/kg tosolutions containing a relatively high percent of water.1.3 In determining the conformance of the test results usingthis method to applicable specifications,results shall berounded off in accordance with the rounding-off method ofPractice E29.1.4 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.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 practices and determine the applica-bility of regulatory limitations prior to use.For specific hazardstatements,see Section 9.2.Referenced Documents2.1 ASTM Standards:2D1364 Test Method for Water in Volatile Solvents(KarlFischer Reagent Titration Method)D3437 Practice for Sampling and Handling Liquid CyclicProductsD3852 Practice for Sampling and Handling Phenol,Cresols,and Cresylic AcidD4790 Terminology of Aromatic Hydrocarbons and RelatedChemicalsD6809 Guide for Quality Control and Quality AssuranceProcedures for Aromatic Hydrocarbons and Related Ma-terialsE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with Specifications2.2 Other Document:3OSHA Regulations,29 CFR paragraphs 1910.1000 and1910.12003.Terminology3.1 See Terminology D4790 for definition of terms used inthis test method.4.Summary of Test Method4.1 When solutions of iodine in methanol and of sulfurdioxide in pyridine are mixed in the presence of water,thefollowing reaction occurs:I21SO21H2O2HI1SO3(1)4.1.1 Sufficient pyridine is present in the reagent to consumethe hydriodic acid and sulfur trioxide:4.1.2 The pyridine sulfur trioxide salt reacts with the metha-nol,this preventing a second mole of water from beingconsumed:4.2 When the pyridine solution contains water and the sulfurdioxide is titrated with iodine in methanol solution,the1This test method is under the jurisdiction of ASTM Committee D16 onAromatic Hydrocarbons and Related Chemicals and is the direct responsibility ofSubcommittee D16.02 on Oxygenated Aromatics.Current edition approved Jan.1,2010.Published January 2010.Originallyapproved in 1959.Last previous edition approved in 2004 as D1631 99(2004).DOI:10.1520/D1631-10.2For referenced 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.3Available from U.S.Government Printing Office Superintendent of Documents,732 N.Capitol St.,NW,Mail Stop:SDE,Washington,DC 20401.*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 States1 platinum electrodes remain polarized until all the water reacts.A slight excess of iodine depolarizes the electrodes,allowingcurrent to flow through the microammeter which indicates theend point.5.Significance and Use5.1 This test method is particularly useful for determiningsmall amounts of water in hygroscopic materials.This testmethod is suitable for setting specifications on materialsreferenced in the scope.It may also be used as an internalquality control tool and in development or research work.6.Interferences6.1 This test method is not applicable in the presence ofmercaptans,peroxides,or appreciable quantities of aldehydesor amines.6.2 If ketones are present in the sample,interference fromthem can be avoided by employing the glycol-pyridine samplesolvent specified in Test Method D1364.7.Apparatus7.1 The apparatus shall be assembled as shown in Fig.1.Any suitable modification permitting equal facility and accu-racy may be used.Automatic titration equipment is commer-cially available and may be used.8.Reagents8.1 Reagent grade chemicals shall be used in all tests.Unless otherwise indicated,it is intended that all reagents shallconform to the specifications of the Committee on AnalyticalReagents of the American Chemical Society,where suchspecifications are available.4Other grades may be used,pro-vided it is first ascertained that the reagent is of suffici