ASTM_C_1301_-_95_2014.pdf

Designation:C130195(Reapproved 2014)Standard Test Method forMajor and Trace Elements in Limestone and Lime byInductively Coupled Plasma-Atomic Emission Spectroscopy(ICP)and Atomic Absorption(AA)1This standard is issued under the fixed designation C1301;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 The following test method covers the use of inductivelycoupled plasma-atomic emission spectroscopy(ICP)andatomic absorption spectroscopy(AA)in the analysis of majorand trace elements in limestone and lime(calcined limestone).1.2 Table 1 lists some of the elements that can be analyzedby this test method and the preferred wavelengths.Also seeU.S.EPA Methods 200.7 and 200.9.1.3 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:2C51 Terminology Relating to Lime and Limestone(as usedby the Industry)D1193 Specification for Reagent WaterE135 Terminology Relating to Analytical Chemistry forMetals,Ores,and Related MaterialsE863 Practice for Describing Atomic Absorption Spectro-metric Equipment(Withdrawn 2004)3E1479 Practice for Describing and Specifying Inductively-Coupled Plasma Atomic Emission Spectrometers2.2 U.S.EPA Standards:Methods for the Determination of Metals in EnvironmentalSamples;U.S.EPAMethods200.2,200.7,and200.9;Smoley,C.K.,19924Method 6010 Inductively Coupled Plasma Method,SW-846,Test Methods for Evaluating Solid Waste53.Terminology3.1 DefinitionsDefinitions for terms used in this testmethod can be found in Terminologies C51 and E135.3.2 Additional Definitions:3.2.1 total recoverable,ntrace element concentration inan unfiltered sample after heating in acid.3.2.2 total digestion,ncomplete digestion of a sample,including silica and silicate minerals,using the fusion-fluxmethod.4.Summary of Test Method4.1 A sample,digested by either fusion or acid,is atomizedand passed into an excitation medium(a plasma in the case ofICP;a flame in the case ofAA).The resulting ions are analyzedby atomic spectroscopy.Elemental concentrations are deter-mined by graphically relating the emission/absorption at spe-cific wavelengths for an unknown sample to analytical curvesmade from reference standards of known composition.5.Significance and Use5.1 The presence and concentration of elements in lime andlimestone is important in determining product quality and itssuitability for various uses.This test method provides a meansof measuring the major and trace element concentration in limeand limestone.6.Interferences6.1 ChemicalChemical interferences,most common inAA,arise from the formation of molecular compounds that1This test method is under the jurisdiction of ASTM Committee C07 on Limeand Limestone and is the direct responsibility of Subcommittee C07.05 on ChemicalTests.Current edition approved July 1,2014.Published July 2014.Originally approvedin 1995.Last previous edition approved in 2009 as C1301 95(2009).DOI:10.1520/C1301-95R14.2For 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.3The last approved version of this historical standard is referenced onwww.astm.org.4Available from CRC Press,2000 Corporate Blvd.,N.W.,Boca Raton,FL33431.5Available from U.S.Government Printing Office Superintendent of Documents,732 N.Capitol St.,NW,Mail Stop:SDE,Washington,DC 20401,http:/www.access.gpo.gov.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 cause absorbances at the wavelength of interest.This molecu-lar band spectral overlap can be minimized by buffering thesample with matrix modifiers(a Lanthanum additive,forexample),using standard additions techniques,matrix match-ing or by careful selection of operating conditions(forexample,using a hotter nitrous oxide/acetylene flame,selectingan alternate wavelength).6.2 PhysicalPhysical interferences are the result of theinconsistencies in the introduction of the sample into theinstrument,namely the transport and atomization/nebulizationof the sample.These inconsistencies are a function of changingviscosity and surface tension,and are found primarily insamples of high-dissolved solids or high-acid concentrations.Physical interferences can be reduced by diluting the sampleand by the use of a peristaltic pump.6.3 SpectralSp