ASTM_E_1770_-_14.pdf

Designation:E177014Standard Practice forOptimization of Electrothermal Atomic AbsorptionSpectrometric Equipment1This standard is issued under the fixed designation E1770;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 practice covers the optimization of electrothermalatomic absorption spectrometers and the checking of spectrom-eter performance criteria.1.2 The values stated in SI units are to be regarded as thestandard.1.3 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:2E50 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forMetals,Ores,and Related MaterialsE876 Practice for Use of Statistics in the Evaluation ofSpectrometric Data(Withdrawn 2003)3E1184 Practice for Determination of Elements by GraphiteFurnace Atomic Absorption SpectrometryE1452 Practice for Preparation of Calibration Solutions forSpectrophotometric and for Spectroscopic Atomic Analy-sis(Withdrawn 2005)33.Terminology3.1 For definitions of terms used in this test method,refer toTerminology E135.4.Significance and Use4.1 This practice is for optimizing the parameters used inthe determination of trace elements in metals and alloys by theelectrothermal atomic absorption spectrometric method.It alsodescribes the practice for checking the spectrometer perfor-mance.The work is expected to be performed in a properlyequipped laboratory by trained operators and appropriatedisposal procedures are to be followed.5.Apparatus5.1 Atomic Absorption Spectrometer with ElectrothermalAtomizer,equipped with an appropriate background corrector,a signal output device such as a video display screen(VDS),adigital computer,a printer,and an autosampler.5.2 Pyrolytic Graphite-Coated Graphite Tubes,conformingto the instrument manufacturers specifications.5.3 Pyrolytic Graphite Platforms,Lvov design,fitted to thetubes specified in 5.2.5.4 PyrolyticGraphite-CoatedGraphiteTubes,platformless,conforming to the instrument manufacturersspecifications.5.5 Radiation Source for the AnalyteA hollow cathodelamp or electrodeless discharge lamp is suitable.NOTE1Theuseofmulti-elementlampsisnotgenerallyrecommended,since they may be subject to spectral line overlaps.5.6 For general discussion of the theory and instrumentalrequirements of electrothermal atomic absorption spectromet-ric analysis,see Practice E1184.6.Reagents6.1 Purity and Concentration of ReagentsThe purity andconcentration of common chemical reagents shall conform toPractices E50.The reagents should be free of or containminimal amounts(0.01 g/g)of the analyte of interest.6.2 Magnesium Nitrate Solution 2 g/L Mg(NO3)2Dissolve 0.36 6 0.01 g high-purity Mg(NO3)26H2O in about50 mL of water,in a 100-mL beaker,and transfer the solutioninto a 100-mL volumetric flask.Dilute to mark with water and1This practice 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 Dec.1,2014.Published February 2015.Originallyapproved in 1995.Last previous edition approved in 2006 as E1770 95(2006).DOI:10.1520/E1770-14.2For 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 mix.Store in polypropylene or high-density polyethylenebottle.Alternatively,this solution may be purchased from acommercial supplier.6.3 Calibration SolutionsRefer to the preparation of cali-bration solutions in the relevant analytical method for thedetermination of trace elements in the specific matrix.Calibra-tion solution S0represents the calibration solution containingno analyte;S1the least concentrated calibration solution;S2thecalibration solution with the next highest concentration;through Sk,the most concentrated calibration solution.Alsorefer to Practice E1452.6.4 Matrix ModifiersRefer to the relevant analyticalmethod for the determination of trace elements in the specificmatrix.7.Initial Checks and Adjustments7.1 Turn on power,cooling water,gas supplies,and fumeexhaust system as required for the instrument be