ASTM_E_1097_-_12.pdf

Designation:E109712Standard Guide forDetermination of Various Elements by Direct CurrentPlasma Atomic Emission Spectrometry1This standard is issued under the fixed designation E1097;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 guide covers procedures for using a Direct CurrentPlasma atomic emission spectrometer(DCP-AES)to deter-mine the concentration of elements in solution.Recommenda-tions are provided for preparing and calibrating the instrument,assessing instrument performance,diagnosing and correctingfor interferences,measuring test solutions,and calculatingresults.A method to correct for instrument drift is included.1.2 This guide does not specify all the operating conditionsfor a DCP-AES because of the differences between models ofthese instruments.Analysts should follow instructions pro-vided by the manufacturer of the particular instrument.1.3 This guide does not attempt to specify in detail all of thehardware components and computer software of the instru-ment.It is assumed that the instrument,whether commerciallyavailable,modified,or custom built,will be capable of per-forming the analyses for which it is intended,and that theanalyst has verified this before performing the analysis.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.Specific precau-tionary statements are given in Section 7.2.Referenced Documents2.1 ASTM Standards:2E29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE50 Practices for Apparatus,Reagents,and Safety Consid-erations for Chemical Analysis of Metals,Ores,andRelated MaterialsE135 Terminology Relating to Analytical Chemistry forMetals,Ores,and Related MaterialsE882 Guide for Accountability and Quality Control in theChemical Analysis LaboratoryE1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analytical Method3.Terminology3.1 Definitions:For definitions of terms used in this guide,refer to Terminology E135.3.2 Definitions of Terms Specific to This Standard:3.2.1 background equivalent concentration(BEC),ninDCP-AES,the analyte concentration whose signal is equivalentto the signal generated by the plasma and matrix at the analyteline when the actual analyte concentration is zero.3.2.2 detection limit(DL),nin addition to the DL definedin Terminology E135,the following detection limits aredescribed and used in this guide:3.2.2.1 instrumental detection limit(IDL),nin DCP-AES,the analyte concentration corresponding to three times thestandard deviation of the background noise beneath the analyteline on a set of nine consecutive 10-s measurements of thebackground intensity of the blank.3.2.2.2 method detection limit(MDL),n in DCP-AES,thedetection limit measured on the matrix blank.3.2.3 equivalent analyte concentration,nthe apparentconcentration of an interfering element on an anlalyte.3.2.4 linear dynamic range,nthe concentration rangefrom the limit of quantification to the highest concentration thatremains within 610%of linearity based on lower concentra-tions.3.2.5 limit of quantification(LOQ),nthe lowest concen-tration at which the instrument can measure reliably with adefined error and confidence level.3.2.6 sensitivity,nthe slope of the analytical curve,whichis the ratio of the change in emission intensity to the change inconcentration.4.Summary of Guide4.1 Direct Current Plasma atomic emission spectrometers,either simultaneous or sequential,measure the concentration of1This guide is under the jurisdiction of ASTM Committee E01 on AnalyticalChemistry for Metals,Ores,and Related Materials and is the direct responsibility ofSubcommittee E01.20 on Fundamental Practices.Current edition approved June 1,2012.Published June 2012.Originallyapproved in 1986.Last previous edition approved in 2007 as E1097 07.DOI:10.1520/E1097-12.2For 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 elements in solution.Samples,calibration and other solutionsare nebulized and the aerosol is transported to the direct currentplasma jet where excitation occurs and characteristic emissionspectra are produced.The spectra are dispersed by an echellegrating and cross-dispersed by a prism or grating.The spectrathen impinge on photomultiplier tubes,whose outputs