ASTM_D_6130_-_11.pdf

Designation:D613011Standard Test Method forDetermination of Silicon and Other Elements in EngineCoolant by Inductively Coupled Plasma-Atomic EmissionSpectroscopy1This standard is issued under the fixed designation D6130;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 silicon inengine coolant by inductively coupled plasma-atomic emissionspectroscopy(ICP-AES).Silicon can be determined as low asthe range of 5 ppm by this test method.Other elements alsofound in engine coolant can be determined by this method.This test method is applicable to the determination of dissolvedor dispersed elements.1.2 This test method is applicable to both new and usedengine coolant.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:2D1193 Specification for Reagent WaterD1176 Practice for Sampling and Preparing Aqueous Solu-tions of Engine Coolants orAntirusts for Testing PurposesE177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method2.2 US EPA Standards:Method 6010,Inductively Coupled Plasma Method,SW-846,Test Methods for Evaluating Solid Waste3Method 200.7,Inductively Coupled Plasma-Atomic Emis-sion Spectrometric Method for Trace Element Analysis ofWater And Wastes,EPA-600/4-79-020,revised 198433.Summary of Test Method3.1 Elements in solution are determined,either sequentiallyor simultaneously,by ICP-AES.New or used engine coolantsare prepared by dilution.Samples and standards are introducedto the nebulizer using a peristaltic pump and the aerosol isinjected into an argon-supported inductively coupled plasma.The high temperature of the plasma atomizes the sample andproduces atomic emission intensities at wavelengths associatedwith the desired elements.Emission intensity is proportional toconcentration.Elemental determinations are made by compar-ing standard and sample emission intensities.4.Significance and Use4.1 Some engine coolants are formulated with silicon con-taining additives.This test method provides a means ofdetermining the concentration of dissolved or dispersed ele-ments which give an indication of this additive content in theengine coolant.5.Interferences5.1 Interferences may be categorized as follows:5.1.1 SpectralLight emission from spectral sources otherthan the element of interest may contribute to apparent netsignal intensity.Sources of spectral interference include directspectral line overlaps,broadened wings of intense spectrallines,ion-atom recombination continuum emission,molecularband emission and stray(scattered)light from the emission ofelements at high concentrations.Avoid overlaps by selectingalternate analytical wavelengths.5.1.2 PhysicalPhysical interferences are effects associatedwith sample nebulization and transport processes such asviscosity and particulate contamination.1This test method is under the jurisdiction of ASTM Committee D15 on EngineCoolants and Related Fluids and is the direct responsibility of SubcommitteeD15.04 on Chemical Properties.Current edition approved Nov.1,2011.Published January 2012.Originallyapproved in 1997.Last previous edition approved in 2009 as D613097a(2009).DOI:10.1520/D6130-11.2For 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 U.S.Environmental Protection Agency,Environmental Moni-toring and Support Laboratory,Cincinnati,OH 45268.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 5.1.3 BackgroundHigh background effects from scatteredlight,etc.,can be compensated for by background correctionadjacent to the analyte line.5.1.4 ChemicalChemical interferences are caused by mo-lecular compound formation,ionization effects,and thermo-chemical effects associated with sample vaporization andatomization in the plasma.Normally these effects are notpronounced and can be minimized by careful selection ofoperating conditions(incident power,plasma observationposition,etc.).6.Apparatus6.1 SpectrometerAn inductively coupled plasma emissionspectrometer of the simultaneous or sequential type includingRF generator,torch,nebulizer,spray c