ASTM_D_5439_-_95_2012.pdf

Designation:D543995(Reapproved 2012)Standard Test Method forDetermination of Sediment in Moellon1This standard is issued under the fixed designation D5439;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 This test method covers the determination of the tolueneinsoluble sediment contained in Moellon.This test method wasderived from Test Method D473.1.2 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.3 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:2D473 Test Method for Sediment in Crude Oils and Fuel Oilsby the Extraction MethodD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum Products2.2 ISO Standard:3ISO 5272 Toluene for Industrial Use-Specifications3.Significance and Use3.1 This test method is intended for use in determining thetoluene insoluble sediment contained in Moellon.4.Apparatus4.1 Extraction Apparatus(see Fig.1 and Fig.2),consistingof the parts described in 4.1.1 4.1.6.4.1.1 Extraction Flask,a wide-neck Erlenmeyer flask of 1-Lcapacity.4.1.2 Condenser,a condenser in the form of a metal coilapproximately 25 mm in diameter and 50 mm in lengthattached to,and with the ends projecting through a lid ofsufficient diameter to cover the neck of the flask as shown inFig.1.The coil should be made from stainless steel,tin,tin-plated copper,or tin-plated brass tubing having an outsidediameter of 5 to 8 mm and a wall thickness of 1.5 mm.Ifconstructed of tin-plated copper or brass,the tin coating shallhave a minimum thickness of 0.075 mm.The exposed surfaceof the coil for cooling purposes is about 115 cm2.4.1.3 Extraction ThimbleThe extraction thimble should beof a refractory porous material,pore size index P15,25 mm indiameter by 70 mm in height,weighing not less than 15 g andnot more than 17 g.The thimble shall be suspended from thecondenser coil by means of a basket so that it hangs approxi-mately midway between the surface of the extracting solventand the bottom of the condenser coil.4.1.4 Thimble BasketThe thimble basket shall becorrosion-resistant,shall be made of platinum,stainless steel,nickel-chromium alloy,or similar material,and shall meet therequirements of Fig.2.4.1.5 Water CupA water cup shall be used when testing asample having a high-water content(see Fig.1b).The cup shallbe made of glass,shall be conical in shape,shall be approxi-mately 20 mm in diameter and 25 mm deep,and shall have acapacity of approximately 3 mL.Aglass hook fused on the rimat one side is so shaped that when hung on the condenser thecup hangs with its rim reasonably level.In this procedure,thethimble basket is suspended either as shown in Fig.1a bymeans of the corrosion-resistant wire looped over the bottom ofthe condenser coil and attached to the basket supports or as inFig.1b where the wire supports of the basket are attached tohooks soldered to the underside of the condenser lid.4.1.6 Source of Heat,a source of heat,preferably a hot plate,suitable for vaporizing toluene.5.Solvent5.1 Toluene,conformingtoISO5272,Grade2.(WarningFlammable.)5.1.1 The typical characteristics for the reagent are:1This test method is under the jurisdiction of ASTM Committee D31 on Leatherand is the direct responsibility of Subcommittee D31.08 on Fats and Oils.This testmethod was developed in cooperation with the American Leather Chemists Assn.(Method H 231957).Current edition approved April 1,2012.Published April 2012.Originallyapproved in 1993.Last previous edition approved in 2006 as D5439 95(2006).DOI:10.1520/D5439-95R12.2For 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 American National Standards Institute,11 West 42nd St.,13thFloor,New York,NY 10036.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 Color(APHA)10Boiling range(initial to dry point)A2.0CResidue after evaporation0.001%Substances darkened by H2SO4passes ACS testSulfur compounds(as S)0.003%Water(H2O)(by Karl Fischer titration)0.03%ARecorded boiling point 110.6C.6.Sampling6.1 Sampling is defined as all steps required to obtain analiquot of the contents of any pipe,tank,or other system and toplace the sample into the laboratory test container.6.2 Only represen