ASTM_D_811_-_82_scan.pdf

41 Deelgnatlon:D 811-82 An Amerlc1n NltoNI Slandard Standard Method of CHEMICAL ANALYSIS FOR METALS IN NEW AND USED LUBRICATING OILS1 I.Scope l.l Thae methods of ch analyail cover the determination of barium,tin,silica,zinc,aluminum,calcium,magnesium,and llO-dium and potassium in new and U1Cd lubricat-ing oils.Other metallic ta.sulfur,phoa-phorua,and chlorine i:Ji ountl commonly found in lubricating oilii do not interfere in this method.NOTE 1-Tbeie methodl do not cover the deter-mination of lead,copper.and iron.2.Smnawy of Metbod1 2.1 The analytical procedures follow the well-known scheme of separating the metall into groups for more venient detiqn,u ah.own in Fig.1.Thia K;heme provida a rapid and accuzate mod for the dc;teimma-tion of all,ICVelal,or any one of the metals u may be aeen mCelu_ry from an initial qualita-tive of the oil aamplo.2.2 To avoid it interrmnce throughout the cedure,bariUJJI.ii 1ep1.1ated along with the metala of the hydrogen mlfide grqup.The 8-bydroxyquU:loline lerYOI 81 an c:cllent mew for removiiig iron,aluminum,and Ziu from pboapba.te interference:Phosphate and Bwrate ion&u,remo after e alcium determina-tUm to P.rovide fo a moi:e a.Ccurate determi-nation of sodium.and._fOtusi.Um.3.Prep111a ors.3.1 Heat tbeaamplc of oil to 60 10c and agitate it in the original container until all aedim.e.n1 is homogeneously suapended in the oil.If the original container is of opaque ma-teria1,or if it is more than three quartcn fUll,tramfer the cm.tin:aample to a doar glua bottle having a capacity at lcut one third greater than the volume of the sample.Tranafer all traces of sediment from the containct to the bottle by iple.nt agitatum of portions of the sample Uie original container.After com-plete llilpension of all aedinient,strain the wn-ple or a convenient Aliquot through a 100.mesh ScrcCn for the removal of large contaminating particles.3.2 Heat and thorousMy mix the strained oil or aliquot befOre taking each portion of the sample for test.Homogeneity will be indicated by the preciaion of the inalyses.Purity of R.Mpntt.Matertai.4.1 Purity of kopnt.r-Reagent gnide chemicall ahall be med in all teats.Unl.eu otherwile indieated,it ii intended that all re-agent.s lhall conform to the specificatiomofthe Committee on Analytical Reagents o the.American Cbeinical Society,where auc:h,pee.ificatiom are available.Other gra4e1 may be used.provided it ii tint aacertained that the reagent is of IU.fliciently high plirity to permit ita uae without leue.ning the accuracy of the determination.I n-medaoda wider the jllrildk:lioA of ASTM=:uOo-1111*IH2.Origiully pablilbad,111-44 T.Lut prmmi.edi1icm D 111-41(197).t Ch,Adierlcan Cbcmk:Q Sodcty Spec-il!catiolll,Am.Chemial Soc.,Wulllqtoa.D.C.Jfor 1111-pt!Ons Olll the!mtiliaof rup11 not Jifkld by the Amcrimn themiCaJ Slc:idY.Jl.cUant Chemicall aa4 Studardl,by IOMJih llllaiJI,D.Vu ROltrUll Co.,1De.,New York,N.Y.,ud tlleKUllitedStata 359 NOTICE:This standard has either been superseded and replaced by a new version or discontinued.Contact ASTM International(www.astm.org)for the latest information.4.2 Purity of Water-Unless otherwise indi-cated references to water shall be undcntood to mean distilled waterorwaterofequal purity.PllELIMINARY SEPARATIONS 5.Reapnts 5.1 Alco/lol(95 or Fomwla.U tlenatauwi).2 Acollollc Metllylkd Indicator.Solutn(l g/LDiuolvc 0.5 g of methyl red in 300 m.L of alcohol and dilute with water to SOO mL.5.3 Ammonium Hydroxirk 1 N)(NH,OH).S.4.Ammonbpn SUifate(NlL)tSO,).5.5 Hydiocll/orlc Acid(0.3 N,6 N,12 N)(HCl).5.6 HydlOpn Sulfide(ga.s)(HtS).5.7 Hydropn Sulfrde Waali Solution-Satu-rate 0.3 N HCl with HtS.6.Procedure.6.1.Removl of Organic Mateial-:-Tranafer to a clean 3-in.16-mm.)platinum.dish approx-imately 10 g of the hoiJlogcneous sample wr.ighed to the nearat 0.01 g.Heat thC dish w,th a bunaen burner until the contcJits ignite and bum readily.Move the diah and flamiJl8 contents to a hot plate and maintain them at such a tcnipcrature that only ash and carbon mnain after burning s.If any liq1id or tarry material heat eYer a burner.lJ.Dtil&moking ceaaes.Ipite.over a bu.mer,or in a.furnace at not over 550 to 600C.Cool,add to the residue 1 to 2 drops of 18 N HaSO.,evap-orate the add and ignite at 650 to 700C,until the oxidation of carbon is complete._ 6.2 Separation of Bflrlum.Lad,Copper,Cadmium,Silica,arul Tin from.Zinc,Iron,Alu-minum,Caldtun,Magnalwn,Sodium,an4 Po-ta.utwn-Treat the residue(6.1)with.20 mL of 6 N HCl and evaporate tomoilt dryne8.Add 25 to 30.JbL of water to tie raidue,tranJfer quantitatively to a 400-m.L beaker,and dilute to 100 mL with water.!odd 7 N N80H p l?Y drop until.the iolution is just neutral to methyl red,and then add 6 to 8 mL of l N HCl and 1 g of(N8)sSO Heat to boiling and pass in a vigorous stream Qf H,S until the eolution hu c;ooled to room temperature,add.200 mL of water,and again saturate with fftS.Filter through an ashles.clOtextumd paper into a 600-mL beaker,and wash with H2S wash soluti911.Reserve the preciphite fo