Designation:D6443−14StandardTestMethodforDeterminationofCalcium,Chlorine,Copper,Magnesium,Phosphorus,Sulfur,andZincinUnusedLubricatingOilsandAdditivesbyWavelengthDispersiveX-rayFluorescenceSpectrometry(MathematicalCorrectionProcedure)1ThisstandardisissuedunderthefixeddesignationD6443;thenumberimmediatelyfollowingthedesignationindicatestheyearoforiginaladoptionor,inthecaseofrevision,theyearoflastrevision.Anumberinparenthesesindicatestheyearoflastreapproval.Asuperscriptepsilon(´)indicatesaneditorialchangesincethelastrevisionorreapproval.1.Scope*1.1Thistestmethodcoversthedeterminationofcalcium,chlorine,copper,magnesium,phosphorus,sulfur,andzincinunusedlubricatingoils,additives,andadditivepackagesbywavelengthdispersiveX-rayfluorescencespectrometry.Ma-trixeffectsarehandledwithmathematicalcorrections.1.2Foreachelement,theupperlimitoftheconcentrationrangecoveredbythistestmethodisdefinedbythehighestconcentrationlistedinTable1.Samplescontaininghigherconcentrationscanbeanalyzedfollowingdilution.1.3Foreachelement,thelowerlimitoftheconcentrationrangecoveredbythistestmethodcanbeestimatedbythelimitofdetection(LOD)2(seealso40CFR136AppendixB)orlimitofquantification(LOQ),2bothofwhichcanbeestimatedfromSr,therepeatabilitystandarddeviation.LODandLOQvalues,determinedfromresultsobtainedintheinterlaboratorystudyonprecision,arelistedinTable2.1.3.1LODandLOQarenotintrinsicconstantsofthistestmethod.LODandLOQdependupontheprecisionattainablebyalaboratorywhenusingthistestmethod.1.4Thistestmethodusesregressionsoftwaretodeterminecalibrationparameters,whichcanincludeinfluencecoeffi-cients(thatis,interelementeffectcoefficients)(GuideE1361),hereinreferencedasalphas.Alphascanalsobedeterminedfromtheoryusingrelevantsoftware.1.5SetupofthistestmethodisintendedforpersonstrainedinthepracticeofX-rayspectrometry.Followingsetup,thistestmethodcanbeusedroutinely.1.6ThevaluesstatedineitherSIunitsorangstromunitsaretoberegardedseparatelyasstandard.1.7Thisstandarddoesnotpurporttoaddressallofthesafetyconcerns,if...
