1、Designation: E2823 17Standard Test Method forAnalysis of Nickel Alloys by Inductively Coupled PlasmaMass Spectrometry (Performance-Based)1This standard is issued under the fixed designation E2823; the number immediately following the designation indicates the year oforiginal adoption or, in the case
2、 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 describes the inductively coupledplasma mass spectrometric analysis of nick
3、el and nickel allys,as specified by Committee B02, and having chemical compo-sitions within the following limits:Element Application Range (MassFraction %)Aluminum 0. 016.00Boron 0. 010.10Carbon 0. 010.15Chromium 0. 0133.00Copper 0.0135.00Cobalt 0. 0120.00Iron 0.0550.00Magnesium 0. 010.020Molybdenum
4、 0. 0130.0Niobium 0. 016.0Nickel 25.00100.0Phosphorous 0.0010.025Silicon 0.011.50Sulfur 0.00010.01Titanium 0.00016.0Tungsten 0.015.0Vanadium 0.00051.01.2 The following elements may be determined using thismethod.Element Quantification Range (g/g)Antimony 0.550Bismuth 0.111Gallium 2.954Lead 0.421Silv
5、er 135Tin 2.297Thallium 0.53.01.3 This method has only been interlaboratory tested for theelements and ranges specified. It may be possible to extend thismethod to other elements or different composition rangesprovided that method validation that includes evaluation ofmethod sensitivity, precision,
6、and bias as described in thisdocument is performed.Additionally, the validation study mustevaluate the acceptability of sample preparation methodologyusing reference materials and/or spike recoveries. The user iscautioned to carefully evaluate the validation data as to theintended purpose of the ana
7、lytical results. Guide E2857 pro-vides additional guidance on method validation.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 det
8、ermine the applica-bility of regulatory limitations prior to use. Specific safetyhazard statements are given in Section 9.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with Specifications
9、E50 Practices for Apparatus, Reagents, and Safety Consid-erations for Chemical Analysis of Metals, Ores, andRelated MaterialsE55 Practice for Sampling Wrought Nonferrous Metals andAlloys for Determination of Chemical CompositionE88 Practice for Sampling Nonferrous Metals and Alloys inCast Form for D
10、etermination of Chemical CompositionE135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test MethodE1329 P
11、ractice for Verification and Use of Control Charts inSpectrochemical AnalysisE1479 Practice for Describing and Specifying InductivelyCoupled Plasma Atomic Emission SpectrometersE1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analytical MethodE2027 Practice for
12、 Conducting Proficiency Tests in theChemical Analysis of Metals, Ores, and Related Materials1This test method is under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores, and Related Materials and is the directresponsibility of Subcommittee E01.08 on Ni and Co and High Te
13、mperature Alloys.Current edition approved Jan. 1, 2017. Published February 2017. Originallyapproved in 2011. Last previous edition approved in 2011 as E282311. DOI:10.1520/E2823-17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.or
14、g. 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 StatesThis international standard was developed in accordance with intern
15、ationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1E2165 Practice for Establishing an Uncertainty Bu
16、dget forthe Chemical Analysis of Metals, Ores, and RelatedMaterials (Withdrawn 2007)3E2857 Guide for Validating Analytical MethodsE2972 Guide for Production, Testing, and Value Assignmentof In-House Reference Materials for Metals, Ores, andOther Related Materials2.2 ISO Standards:4ISO/IEC 17025 Gene
17、ral Requirements for the Competenceof Calibration and Testing LaboratoriesISO Guide 98-3 Uncertainty of MeasurementPart 3:Guide to the Expression of Uncertainty in Measurement(GUM:1995), First Edition3. Terminology3.1 DefinitionsFor definitions of terms used in this testmethod, refer to Terminology
18、E135.4. Summary of Test Method4.1 Samples are dissolved in a mixture of mineral acids andthe resulting solutions are measured using inductively coupledplasma mass spectrometry.5. Significance and Use5.1 This test method for the chemical analysis of nickel andnickel alloys is primarily intended to te
19、st material for compli-ance with specifications such as those under jurisdiction ofASTM committee B02. It may also be used to test compliancewith other specifications that are compatible with the testmethod.5.2 It is assumed that all who use this method will be trainedanalysts capable of performing
20、common laboratory proceduresskillfully and safely, and that the work will be performed in aproperly equipped laboratory.5.3 This is a performance-based method that relies more onthe demonstrated quality of the test result than on strictadherence to specific procedural steps. It is expected thatlabor
21、atories using this method will prepare their own workinstructions. These work instructions will include detailedoperating instructions for the specific laboratory, the specificreference materials employed, and performance acceptancecriteria. It is also expected that, when applicable, each labora-tor
22、y will participate in proficiency test programs, such asdescribed in Practice E2027, and that the results from theparticipating laboratory will be satisfactory.6. Interferences6.1 When possible, analyte isotopes are selected that arefree from mass overlap interferences. Because isotope choicesare li
23、mited, this is not always an option. It is the responsibilityof the user to determine run conditions and parameters thatavoid or compensate for interferences that may bias test results.6.2 The use of an internal standard may compensate for thephysical interferences resulting from variations in sampl
24、e andcalibration solution aerosol transport rates. The user may choseto add the internal standard by spiking each solution with aspecified amount of an appropriate certified reference material(CRM) solution. Alternatively, on-line addition of a peripheralinternal standard solution during sample anal
25、ysis is alsopossible provided acceptable instrument sensitivity is main-tained.6.3 Isobaric and polyatomic mass overlap interferences arebest addressed by selecting an alternate atomic mass. Someinstrument manufacturers offer software options for math-ematically correcting for common interferences,
26、but the user iscautioned to carefully evaluate this approach to mass overlapcorrection. However, some laboratories participating in theinterlaboratory study found it necessary to generate a math-ematical correction for the effect of the ZrO interference on theAg 107 isotope. In this case the Zr 91 i
27、sotope was used forzirconium determination.6.4 Modern instruments may have a collision or reactioncell that can use ion-molecule collisions or reactions to removespectral interferences. The user of this method must examinethis information to ascertain the need for collision/reactioncells for the rem
28、oval of spectral interferences. However, itshould be noted that no collision/reaction gases were used bythe laboratories participating in the interlaboratory study of theelements listed in the Scope, thus implying that the use ofcollision/reaction gases is not required for determination ofthose elem
29、ents.6.5 The isotopes listed in Table 1 have been used to analyzethe listed elements in nickel alloys and are suggested for theuser. The user may choose to use multiple isotopes to helpverify that atomic mass selection is optimized for the particularalloy being determined. It is recommended that onc
30、e isotopesand appropriate spectral corrections are determined, the user ofthis method specify this information or reference instrumentprograms, which include this information in their laboratoryanalysis procedures.7. Apparatus7.1 Suitability of an Inductively Coupled Plasma MassSpectrometer for test
31、ing of this method will be establishedusing the performance criteria described in section 12.1. Thesample introduction system shall be capable of handlingsolutions containing trace amounts of HF. Each instrumentshall be installed and operated according to the manufacturersrecommendations.3The last a
32、pproved version of this historical standard is referenced onwww.astm.org.4Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.TABLE 1 Suggested Isotopes/InterferenceElement IsotopePotentialInterferenceAntimony 121Bismuth 209Ga
33、llium 71Lead 208Silver 107 ZrO, FeCrTin 120 MoOThallium 205E2823 1727.2 Sample Preparation EquipmentMachine tools shall beused that are capable of removing surface oxides and othercontamination from the as-received sample and then takinguncontaminated and chemically representative chips suitablefor
34、analysis.7.3 All labware used should be suitably cleaned for tracelevel analysis.8. Reagents and Materials8.1 Reagents:8.1.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents conform to the specifications of the Committee
35、 onAnalytical Reagents of the American Chemical Society wheresuch specifications are available.5However, the purity of acidreagents utilized in this procedure shall be suitable for tracemetal analysis and should not contain any significant amount ofthe analyte. Other grades may be used, provided it
36、is firstascertained that the reagent is of sufficiently high purity topermit its use without lessening the accuracy of the determi-nation.8.1.2 Purity of WaterThe purity of water used in this testmethod shall conform to the requirements of SpecificationD1193 for reagent water, Type I. The water puri
37、fication methodused must be capable of removal of all elements in concentra-tions that might bias the test results.8.1.3 Internal StandardThe use of an internal standard isrecommended. The use of an internal standard may compen-sate for the physical interferences resulting from variations insample a
38、nd calibration solution aerosol transport rates. Selectan internal standard element of similar atomic mass to theanalyte and one that is not commonly found in the samples tobe determined. The exact concentration added is not critical,however, the amount added should yield a significant signalwhen me
39、asured.8.2 Calibration Solutions:8.2.1 In this test method, calibration is based on laboratory-prepared, pure nickel matrix- matched solutions. The matrixsolutions are prepared with nickel of known purity. Thesematrix solutions are then spiked with aliquots of single elementcertified reference mater
40、ial (CRM) solutions which contain theelements of interest.8.2.2 Step 8.2.3 and following describe the preparation ofcalibration solutions for analysis of sample solutions thatcontain 1 g alloy/L final dilution. It is acceptable to vary finalconcentrations as long as the users method demonstratesadeq
41、uate sensitivity and precision (see 12.1).8.2.3 Determine the number and composition of calibrationsolutions needed to cover the concentration range for eachelement. It is suggested that the calibration solutions have theirhighest concentration slightly above the highest expectedsample concentration
42、, a concentration in the mid-range of theexpected sample concentrations, a concentration at or near thereporting limit, and a blank. In any case, a minimum of threesolutions including a blank must be used for calibration.8.2.4 Prepare matrix solutions as follows:8.2.4.1 Weigh 0.5 g of pure nickel in
43、to an HF resistantdigestion vessel. Use one vessel for each calibration solution tobe made. Note that using 0.5 g of nickel approximates the massfraction of nickel (50 %) found in1gofatypical nickel alloy.8.2.4.2 Dissolve the pure nickel in 20 mL of acid mixtureper gram of sample. Select acid mixtur
44、es that will dissolve thealloys to be analyzed using this method.Caution: If powdered nickel is used, add the acid cautiouslyas powdered metals tend to be very reactive.8.2.4.3 A mixture of HCl + HNO3(9 + 1), HCl + H2O+HNO3(3 + 2 + 1), or HNO3+HF+H2O (1 + 1 + 1) willdissolve many types of nickel all
45、oys . For high Mo-Cr alloys ithas been found that concentrated HCl with the addition ofconcentrated HNO3dropwise may be necessary to avoidpassivation.8.2.4.4 Heat the digestion vessels gently until the nickeldissolves. Remove the beakers from the heat, add 10 drops of49 % HF, and swirl gently. If HN
46、O3+HF+H2O(1+1+1)is used for digestion, it is not necessary to add additional HF.The laboratory may choose to reduce this solution to wet saltsin order to remove excess HF and then re-dissolve by heatingthe salts in approximately 20 mL of water.8.2.4.5 If an internal standard is used, add the predete
47、rminedamount into each solution.8.2.4.6 Cool the nickel solutions and transfer into 1-Lplastic flasks. Polypropylene or polymethylpentene flasks areacceptable for this purpose.8.2.5 Add the needed amount of single element CRMsolutions to the flasks, ensuring to leave one analyte-free foruse as a bla
48、nk. Maintain the acidity necessary to assuresolution stability. The acidity given on the solution CRMcertificate of analysis will provide guidance on the necessaryacid concentrations needed to do this. Typically, if thesesolutions are to match samples prepared using one gram ofalloy diluted to1-L, t
49、he quantity of acids used in 8.2.4 will besufficient to hold all analytes in solution.8.3 Other Materials:8.3.1 ArgonThe ICP-MS argon supply should be in accor-dance with the recommendations of the instrument manufac-turer.8.3.2 Control Materials:8.3.2.1 A laboratory may choose to procure, produce, orhave manufactured a chip material containing analyte contentsin the range of typical samples to be used as a control material.These chips should be well blended and checked for homoge-neity. Additional guidance on the production of these contr
