ASTM_D_464_-_05_2010.pdf

Designation:D46405(Reapproved 2010)Standard Test Methods forSaponification Number of Naval Store Products IncludingTall Oil and Other Related Products1This standard is issued under the fixed designation D464;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.1.Scope1.1 These test methods cover the determination of thesaponification number of tall oil and products obtained by thefractionation of tall oil such as rosin,fatty acids and distilledtall oil as defined in Terminology D804.These test methods arealso applicable to gum and wood rosin.Two test methods arecovered as follows:1.1.1 Test method using a potentiometric method,and1.1.2 Test method using an internal indicator method.1.2 The potentiometric method is suitable for use with bothlight-and dark-colored test samples.It should be consideredthe referee method.The internal indicator method is suitablefor use only with light-and medium-colored test samples.Itshould be considered the alternate method.1.3 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.4 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.2.Referenced Documents2.1 ASTM Standards:2D803 Test Methods for Testing Tall OilD804 Terminology Relating to Pine Chemicals,IncludingTall Oil and Related ProductsE70 Test Method for pH of Aqueous Solutions With theGlass Electrode3.Significance and Use3.1 These test methods are designed to broaden the scope ofthe earlier editions of the test method by the inclusion of tall oiland tall oil derived products as test materials and is referencedin Test Methods D803.3.2 The saponification number is an important property oftall oil and the products obtained by the fractionation of tall oil.It is the test method widely used to determine the total acidcontent,both free and combined,of these products.3.3 The potentiometric test method should be used when themost reproducible results are required.4.Preparation of Sample4.1 If the sample for analysis is rosin,it shall consist ofsmall pieces of rosin chipped from a freshly exposed part of alump or lumps,and thereafter crushed to facilitate weighingand dissolution.Prepare the sample the same day on which thetest is begun in order to avoid changes in properties due tosurface oxidation.Changes are very pronounced on groundrosin that has a large surface area exposed to air.Existing rosindust and powdered rosin must not be used.4.2 If the sample is a nonhomogeneous liquid,heat theentire sample in a closed container fitted with a capillary ventor the equivalent.Some kind of agitation,even if doneoccasionally by hand,saves much time.Heat by immersion inopen steam or hot water bath to avoid overheating.Whendealing with crystallized rosin,a higher temperature of ap-proximately 160C may be needed.Remove samples fortesting only when the entire sample is homogeneous and hasbeen well stirred.5.Purity of Reagents and Water5.1 Unless otherwise indicated,it is intended that all re-agents shall conform to the specifications established by the1These test methods are under the jurisdiction of ASTM Committee D01 onPaint and Related Coatings,Materials,and Applications and are the directresponsibility of Subcommittee D01.34 on Pine Chemicals and HydrocarbonResins.Current edition approved June 1,2010.Published June 2010.Originallyapproved in 1937.Last previous edition approved in 2005 as D464 05.DOI:10.1520/D0464-05R10.2For 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 Committee on Analytical Reagents of the American ChemicalSociety,3where such specifications are available.References towater shall be understood to mean distilled or deionized water.POTENTIOMETRIC TEST METHOD(Referee Method)6.Apparatus6.1 Erlenmeyer Flask,250-mL,of chemically resistantglass4with standard-taper glass joint.6.2 Hot Plates.6.3 Water-Cooled Reflux Condenser,with standard-taperjoint to fit the Erlenmeyer flask.6.4 Buret,with 0.1 mL divisions.6.5 Stirrer,variable-speed,with a polytetrafluoroethylene(PTFE)coated magnetic stir bar.6.6 Delivery or Volumetric Pipet,50-mL constant.6.7 PTFE Boiling Stones,or glass beads.6.8 Beaker,400-mL tall-form.6.9 Glass Electrode pH Meter,conforming to the require-ments of Test Method E70.Use either standard or alkal