ASTM_D_1966_-_69_1998.pdf

Designation:D 1966 69(Reapproved 1998)Standard Test Method forFoots in Raw Linseed Oil(Gravimetric Method)1This standard is issued under the fixed designation D 1966;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(e)indicates an editorial change since the last revision or reapproval.1.Scope1.1 This method covers the determination of foots in rawlinseed oil by the gravimetric method.The procedure iscommonly known in Europe as the PAT foots method.1.2This 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:D 1193 Specification for Reagent Water23.Terminology3.1 Definition:3.1.1 footsthose solid impurities that precipitate from rawlinseed oil during storage and which then settle to the bottomor“foot”of a storage tank.3.2 Definition of Term Specific to This Standard:3.2.1 footsin this method,the material that is precipitatedfrom the oil by phosphoric acid and which is insoluble inacetone under the specific conditions of the test.4.Summary of Test Method4.1 The oil to be tested is refined with 85%phosphoricacid.The precipitated material is settled by centrifuging and iswashed free of oil with acetone.It is dried and weighed todetermine the foots content gravimetrically.5.Apparatus5.1 Fritted Glass Filtering Crucibles,having a mediumporosity(10 to 15 m)and a capacity of 30 mL.5.2 AgitatorThe agitator shall consist of a horizontal shaftsuitably supported and fitted with clamps or a clamping devicefor holding pear-shaped centrifuge tubes.The tubes shall beheld in such fashion that when the shaft rotates,the tubes willbe tipped end over end,thus allowing the liquid content of thetube to mix as it flows from one end of tube to the other.Theshaft shall be rotated mechanically by any means desired thatallows one to choose either of two fixed speeds;a slow speedof 16 6 2 rpm and a fast speed of 32 6 2 rpm.5.3 Centrifuge Tube,pear-shaped conforming to dimensionsgiven in Fig.1,and made of thoroughly annealed glass.Thegraduations,numbered as shown in Fig.1,shall be clear anddistinct and the mouth shall be constricted in shape for closurewith a stopper.5.4 CentrifugeCapable of whirling two or more filledtubes at a speed that can be controlled to give a relativecentrifugal force of between 500 to 800 g at the tip of the tubes.Calculate the speed of the rotating head as follows:rpm 5 265=rcf/d(1)where:rcf5 relative centrifugal force,g,andd5 diameter of swing,in.,measured between tips ofopposite tubes when in rotating position.5.4.1 If d is given in millimetres,use the following equa-tion:rpm 5 1346=rcf/d(2)NOTE1A list of applicable rotational speeds is given in Table 1.5.5 Pipet,1-mL measuring type graduated in 0.01-mLsubdivisions.5.6 Desiccator,containing an efficient desiccant.Anhydrouscalcium sulfate is satisfactory.6.Reagents6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.3Other grades may beused,provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.6.2 Purity of WaterUnless otherwise indicated,referencesto water shall be understood to mean reagent water conformingto Type II of Specification D 1193.1This test method is under the jurisdiction of ASTM Committee D-1 on Paintand Related Coatings,Materials,andApplications,and is the direct responsibility ofD01.32 on Drying Oils.Current edition effective Oct.3,1969.Originally issued 1964.ReplacesD 1966 64 T.2Annual Book of ASTM Standards,Vol 11.01.3Reagent Chemicals,American Chemical Society Specifications,AmericanChemical Society,Washington,DC.For suggestions on the testing of reagents notlisted by the American Chemical Society,see Analar Standards for LaboratoryChemicals,BDH Ltd.,Poole,Dorset,U.K.,and the United States Pharmacopeiaand National Formulary,U.S.Pharmacopeial Convention,Inc.(USPC),Rockville,MD.1AMERICAN SOCIETY FOR TESTING AND MATERIALS100 Barr Harbor Dr.,West Conshohocken,PA 19428Reprinted from the Annual Book of ASTM Standards.Copyright ASTM6.3 Acetone.6.4 Filter Aid,diatomaceous silica.46.5 Phosphoric Acid(85%)(H3PO4).7.Hazard7.1 This standard may involve the use of hazardous mate-rials,operations,and equipment.It is the responsibility ofwhoever uses this standard to establish appropriate safetypractices to determine the applicability of regulatory limita-tions prior to use.8.Preparation of Sample8.1 Allow the