ASTM_E_1086-14.pdf

Designation:E1086-14INTERNATIONALStandard Test Method forAnalysis of Austenitic Stainless Steel by Spark AtomicEmission SpectrometryThis standard is issued under the fixed designation E1086;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(8)indicates an editorial change since the last revision or reapproval.1.Scope2.Referenced Documents1.1 This test method2 covers the analysis of austenitic2.1 ASTM Standards:3stainless steel by spark atomic emission vacuum spectrometryE135 Terminology Relating to Analytical Chemistry forfor the following elements in the ranges shownMetals,Ores,and Related MaterialsElementComposition Range,%E305 Practice for Establishing and Controlling AtomicChromium17.0to23.0Emission Spectrochemical Analytical CurvesNickel7.5to13.0E406 Practice for Using Controlled Atmospheres in Spec-Molybdenum0.01to3.0Manganese0.01to 2.0trochemical AnalysisSilicon0.01to0.90E1060 Practice for Interlaboratory Testing of Spectrochemi-Copper0.01to0.30cal Methods of AnalysisCarbon0.005to0.25Phosphorus0.003to0.15E1329 Practice for Verification and Use of Control Charts inSulfur0.003to0.065Spectrochemical Analysis1.2 This test method is designed for the routine analysis ofE1806 Practice for Sampling Steel and Iron for Determina-chill-cast disks or inspection testing of stainless steel samplestion of Chemical Composition2.2 Other ASTM Documents:that have a flat surface of at least 13 mm(0.5 in.)in diameter.ASTM MNL 7 Manual on Presentation of Data and ControlThe samples must be sufficiently massive to prevent overheat-ing during the discharge and of a similar metallurgical condi-Chart Analysistion and composition as the reference materials.3.Terminology1.3 One or more of the reference materials must closely3.1 Definitions-For definitions of terms used in this testapproximate the composition of the specimen.The techniquemethod,refer to Terminology E135.of analyzing reference materials with unknowns and perform-ing the indicated mathematical corrections may also be used to4.Summary of Test Methodcorrect for interference effects and to compensate for errors4.1 A controlled discharge is produced between the flatresulting from instrument drift.A variety of such systems aresurface of the specimen and the counter electrode.The radiantcommonly used.Any of these that will achieve analyticalenergy of selected analytical lines are converted into electricalaccuracy equivalent to that reported for this test method areenergies by photomultiplier tubes and stored on capacitors.Theacceptable.discharge is terminated at a predetermined level of accumu-1.4 This standard does not purport to address all of thelated radiant energy from the internal standard iron line or aftera fixed integration time.At the end of the integration period,safety concerns,if any,associated with its use.It is thethe charge on each capacitor is measured,and displayed orresponsibility of the user of this standard to establish appro-recorded as a relative energy or mass fraction%.priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.5.Significance and Use5.1 The chemical composition of stainless steels must bedetermined accurately to ensure the desired metallurgicalThis test method is under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals,Ores,and Related Materials and is the directresponsibility of Subcommittee E01.01 on Iron,Steel,and Ferroalloys.For referenced ASTM standards,visit the ASTM website,www.astm.org,orCurrent edition approved March 1,2014.Published April 2014.Originallycontact ASTM Customer Service at serviceastm.org.For Annual Book of ASTMapproved in 1985.Last previous edition approved in 2008 as E1086-08.DOI:Standards volume information,refer to the standards Document Summary page on10.1520/E1086-14.the ASTM website.2 Supporting data have been filed at ASTM International Headquarters and may Withdrawn 1997.be obtained by requesting Research Report RR:E02-1023.5 ASTM Manual Series,ASTM International,8th edition,2010.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United StatesE1086-1410.Preparation of Apparatuswill be done anytime verification indicates that readings have10.1 Follow the manufacturers instructions for verifyinggone out of statistical control.the optical alignment of the entrance slit and programming the12.3 Verification-Analyze verifiers in replicate to confirmappropriate wavelengths(Table 1).that they read within expected confidence interval,in accor-dance with 12.4.11.Excitation and Integration12.3.1 Each laboratory should determine the frequency of11.1 Electrical Parameters-Two different types of sourcesverification necessary based on statistical analysis.Typically,every 4 h to 8 h is practical and adequate(or if the instrumentwere employed in the testing of this test method.has been idle for more than 1 hour).If the results are not within11.1.1 Directional Self-Initiating Capacitor Dischargethe control limits established in 12.4,perform a standardizationSource:and then repeat verification.Repeat standardization as neces-Capacitance,uF0.015sary so verifications are within control limits or investigateInductance,L1,pH310Inductance,L2,pH20further for instrument problems.Resistance.residual12.4 The confidence interval will be established from ob-Potential,V13500Peak Current.A90servations of the repeatability of the verifiers by utilizing theFirst Valley Current,A60upper and lower limit of a control chart in accordance withCurrent pulse duration,us120Practice E1329 or ASTM Manual MNL 7.Number of discharges/s24011.1.1.1 Excitation Conditions:13.Procedure for Excitation and Radiation MeasurementFlush,s7Argon Flow 0.42 m/h13.1 Produce and record the spectra using the conditions inPrebum,s20Argon Flow 0.42 m3/hIntegration,s2011.1.Argon Flow 0.42 m/h11.1.2 Triggered Capacitor Discharge Source:13.2 Replicate Excitation-Make duplicate excitations ofeach specimen and report the average.Place the freshlyPrebumIntegrationPulse Output:surfaced specimen on the excitation stand in a manner to effectCapacitance,uF(d-c charged)7.52.5a gas-tight seal and adequate argon flushing.Position theInductance,uH5050residualresidualspecimen so there will be a uniform pattern of excitationsResistance.Potential,V950950around its face.For example,a disk-shaped specimen shouldPeak Current,A275100have a ring of excitation marks around its outer edge andCurrent pulse duration,us250130Number of discharges/s120120approximately 6 mm(0.25 in.)from the edge.Avoid the centerTrigger:of cast specimens because of possible quench cracks andCapacitance(d-c charged).uF1.2Inductance.uHresidualsegregation.Make a good electrical ground.If required,coolResistance,residualthe specimen after two excitations to prevent overheating.Potential.V425Examine the specimen after each excitation to evaluate the11.1.2.1 Excitation Conditions:quality of excitation.Cracks,voids,pits,moisture,or inclu-sions will limit the sampling and the accuracy of a determina-Flush,s2Argon Flow 0.56 m3/hPreburn,s10Argon Flow 0.56 m3/htion.Successive excitations shall be sufficiently separated soIntegration,s10 or15Argon Flow 0.56 m3/hthat the discharge patterns do not overlap.12.Calibration,Standardization,and Verification14.Calculation of Results12.1 Calibration-Using the conditions given in 11.1,excite14.1 Average the readings obtained for each specimen.Ifthe readout is not in direct mass fraction%units,use this valueeach calibrant and drift correction sample two to four times andbracket these with similar excitations of any verifiers.A verifierto obtain the mass fraction%from the curves,or related scalevalues and mass fraction%by reference to a table that has beenmay be used as a calibrant even though it is burned only as averifier.There shall be at least three calibrants for eachpreviously prepared.element,spanning the required concentration range.If the15.Precision and Bias2spectrometer system and software permits,perform random15.1 Precision-The precision of this test method wasexcitations of each calibrant and drift correction sample anddetermined by submitting three stainless alloy samples to fiverepeat with different random sequences at least four times.different laboratories.The interlaboratory testing was con-Follow the spectrometer manufacturers software procedures toducted in accordance with Practice E1060.Instrument calibra-convert sample intensities into mass fraction%.Using thetions were performed utilizing(1)reference materials suppliedaverages of the data for each point,determine analytical curveswith the unknowns,(2)in-house reference materials,and(3)in accordance with Practice E305.NIST and British Certified reference materials.The unknowns12.2 Standardization-Following the manufacturersand in-house reference materials were run on three separaterecommendations,standardize on an initial setup or anytimedays.The precision data for the three unknowns are shown inthat it is known or suspected that readings have shifted.MakeTable 2.the necessary corrections either by adjusting the controls on the15.1.1 Accuracy-The three unknowns were analyzed byreadout or by applying arithmetic corrections.Standardizationalternate chemical methods by two laboratories independent of3E1086-14TABLE 3 Accuracy DataMass Fraction%Accuracy.%(95%Confidence)ElementSampleAssumedDeterminedTrue ValueA7.SBE1060,Sw)E1060,S(SR)CarbonCT-3040.0620.0630.00250.00110.0033CT-3050.0670.0670.00520.00150.0052CT-3160.0610.0610.00260.00130.0015ManganeseCT-3040.7650.780.0250.00380.0212CT-3051.841.850.0270.0160.037CT-3161.661.670.0220.0120.022PhosphorusCT-3040.0250.0260.00150.00040.0025CT-3050.0250.0250.00090.00040.0010CT-3160.0310.0290.00210.00040.0012SulfurCT-3040.0220.0230.00210.00070.0017CT-3050.0220.0220.00170.00070.0018CT-3160.0240.0230.00180.00060.0011SiliconCT-3040.550.560.0130.0050.006CT-3050.560.550.0140.0040.008CT-3160.720.690.0130.0080.016CopperCT-3040.330.340.0230.0050.022CT-3050.290.290.0070.0050.006CT-3160.240.250.0170.0030.012NickelCT-3049.639.600.2230.0550.237CT-30511.9711.950.1810.1050.191CT-31612.5412.610.780.0730.242ChromiumCT-30418.6518.570.1650.0750.148CT-30518.5518.580.1140.1070.108CT-31617.4817.600.1840.0530.150MolybdenumCT-3040.3160.330.0170.00350.0082CT-3050.4700.450.0190.00200.0116CT-3162.442.450.0200.0160.019 All mass fractions consist of a 15-determination average,the apparent outiers were leftin because a statistical evaluation of the diata is not a satisfactory reason foreliminating the data values.The results for each individual laboratory are on file at ASTM Intenational Headquarters.Estimate of the overall accuracy for a single analysis from any laboratory.Estimate of the standard deviation of any single random analysis within laboratories.PVariable use to calculate R in Table2 and comprised of the/of the sum of(1)estimate of variance between laboratories and(2)S,2 divided by the number of analysesthat are averaged to obtain the reported value.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard.Users of this standard are expressly advised that determination of the validity of any such patent rights,and the riskof infringement of such rights,are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised,either reapproved or withdrawn.Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters.Your comments will receive careful consideration at a meeting of theresponsible technical committee,which you may attend.If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards,at the address shown below.This standard is copyrighted by ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United States.Individual reprints(single or multiple copies)of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585(phone),610-832-9555(fax),or serviceastm.org(e-mail);or through the ASTM website(www.astm.org).Permission rights to photocopy the standard may also be secured from the ASTM 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