1、Designation: E2823 11Standard Test Method forAnalysis of Nickel Alloys by Inductively Coupled PlasmaMass Spectrometry (Performance-Based Method)1This standard is issued under the fixed designation E2823; the number immediately following the designation indicates the year oforiginal adoption or, in t
2、he 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 test method describes the inductively coupledplasma mass spectrometric analysis
3、of nickel, as specified byCommittee B02, and having chemical compositions within thefollowing limits:Element Application Range (Wt. %)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 0. 0130.0Niobium 0.
4、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 0.421Silver 135Tin 2.297Thalli
5、um 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, and bias as described
6、 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 analytical results.1.4 T
7、his 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 safetyhaza
8、rd statements are given in Section 9.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterE50 Practices for Apparatus, Reagents, and Safety Consid-erations for Chemical Analysis of Metals, Ores, andRelated MaterialsE55 Practice for Sampling Wrought Nonferrous Metals andAll
9、oys for Determination of Chemical CompositionE88 Practice for Sampling Nonferrous Metals and Alloys inCast Form for Determination of Chemical CompositionE135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE177 Practice for Use of the Terms Precision and Bias inAST
10、M Test MethodsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test MethodE1329 Practice for Verification and Use of Control Charts inSpectrochemical AnalysisE1479 Practice for Describing and Specifying Inductively-Coupled Plasma Atomic Emission SpectrometersE1601
11、 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analytical MethodE2027 Practice for Conducting Proficiency Tests in theChemical Analysis of Metals, Ores, and Related MaterialsE2165 Practice for Establishing an Uncertainty Budget forthe Chemical Analysis of Metals,
12、Ores, and RelatedMaterials32.2 ISO Standards:41This 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 Temperature Alloys.Current edition approved May
13、1, 2011. Published July 2011. DOI: 10.1520/E2823-11.2For 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.3Withdraw
14、n. The last approved version of this historical standard is referencedon www.astm.org.4Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, P
15、A 19428-2959, United States.ISO 17025 General Requirements for the Competence ofCalibration and Testing LaboratoriesISO Guide 31 Contents of Certificates of Reference Mate-rialsISO Guide 34 Quality System Guidelines for the Productionof Reference MaterialsISO Guide 98-3 Uncertainty of MeasurementPar
16、t 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 E135.4. Summary of Test Method4.1 Samples are dissolved in a mixture of mineral acids andthe resulting solutions are m
17、easured using inductively coupledplasma mass spectrometry.5. Significance and Use5.1 This test method for the chemical analysis of nickelalloys is primarily intended to test material for compliance withspecifications such as those under jurisdiction of ASTMcommittee B02. It may also be used to test
18、compliance withother specifications that are compatible with the test method.5.2 It is assumed that all who use this method will be trainedanalysts capable of performing common laboratory proceduresskillfully and safely, and that the work will be performed in aproperly equipped laboratory.5.3 This i
19、s a performance-based method that relies more onthe demonstrated quality of the test result than on strictadherence to specific procedural steps. It is expected thatlaboratories using this method will prepare their own workinstructions. These work instructions will include detailedoperating instruct
20、ions for the specific laboratory, the specificreference materials employed, and performance acceptancecriteria. It is also expected that, when applicable, each labora-tory will participate in proficiency test programs, such asdescribed in Practice E2027, and that the results from theparticipating la
21、boratory will be satisfactory.6. Interferences6.1 When possible, analyte isotopes are selected, which arefree from mass overlap interferences. Because isotope choicesare limited, this is not always an option. It is the responsibilityof the user to determine run conditions and parameters thatavoid or
22、 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 sample andcalibration solution aerosol transport rates. The user may choseto add the internal standard by spiking each solution with
23、aspecified amount of an appropriate certified reference material(CRM) solution. Alternatively, on-line addition of a peripheralinternal standard solution during sample analysis is alsopossible provided acceptable instrument sensitivity is main-tained.6.3 Isobaric and polyatomic mass overlap interfer
24、ences arebest addressed by selecting an alternate atomic mass. Someinstrument manufacturers offer software options for math-ematically correcting for common interferences, but the user iscautioned to carefully evaluate this approach to mass overlapcorrection. However, some laboratories participating
25、 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 isotope was used forzirconium determination.6.4 Modern instruments may have a collision or reactioncell which can use ion-molecul
26、e collisions or reactions toremove spectral interferences. The user of this method mustexamine this information to ascertain the need for collision/reaction cells for the removal of spectral interferences.6.5 The isotopes listed in Table 1 have been used to analyzethe listed elements in nickel alloy
27、s 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 once isotopesand appropriate spectral corrections are determined, the user ofthis method specify this i
28、nformation or reference instrumentprograms which include this information in their laboratoryanalysis procedures.7. Apparatus7.1 Suitability of an Inductively Coupled Plasma MassSpectrometer for testing of this method will be establishedusing the performance criteria described in section 12.1. Thesa
29、mple introduction system shall be capable of handlingsolutions containing trace amounts of HF. Each instrumentshall be installed and operated according to the manufacturersrecommendations.7.2 Sample Preparation EquipmentMachine tools shallbe used that are capable of removing surface oxides and other
30、contamination from the as-received sample and then takinguncontaminated and chemically representative chips suitablefor 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
31、in all tests. Unless otherwise indicated, it is intended thatall reagents conform to the specifications of the Committee onTABLE 1 Suggested Isotopes/InterferenceElement Isotope Potential InterferenceAntimony 121Bismuth 209Gallium 71Lead 208Silver 107 ZrO, FeCrTin 120 MoOThallium 205E2823 112Analyti
32、cal 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 impurities in anysignificant amount. Other grades may be used, provided it isfirst asc
33、ertained that the reagent is of sufficiently high purity topermit its use without lessening the accuracy of the determi-nation.8.1.2 Reagent WaterThe purity of reagent water shallconform to the requirements of Specification D1193 for re-agent water, Type I. The water purification method used mustbe
34、capable of removal of all elements in concentrations thatmight 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 and calibration solution aeroso
35、l transport rates.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 refe
36、rence material (CRM) solutions which contain theelements of interest. The CRMs shall be compliant with ISOGuides 31 and 34.8.2.2 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
37、 finalconcentrations as long as the users method demonstratesadequate sensitivity and precision (see section 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 theirhigh
38、est concentration slightly above the highest expectedsample concentration, 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
39、Prepare matrix solutions as follows:8.2.4.1 Weigh 0.5 g of pure nickel into an HF resistantdigestion vessel. Use one vessel for each calibration solution tobe made.8.2.4.2 Dissolve the pure nickel in 20 mL of acid mixtureper gram of sample. Select acid mixtures that will dissolve thealloys to be ana
40、lyzed using this method.NOTE 1Caution: 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),orHNO3+HF+H2O (1 + 1 + 1) willdissolve many types of nickel alloys . For high Mo-Cr alloys ithas been fo
41、und 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 HNO3+HF+H2O(1+1+1)is used for digestion it
42、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 to be used, add thepredetermined amount into each solution.8.2.
43、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 into the flasks, making sure to leave one analyte-freefor use as a blank. Maintain the acidity necess
44、ary 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, the quantity of acids used in 8.
45、2.4 will besufficient to hold all analytes in solution.8.3 Other Materials:8.3.1 Argon and Collision/Reaction GasesThe ICP argonsupply and any collision/reaction gas supply shall be specifiedby the instrument manufacturer.8.3.2 Control Materials:8.3.2.1 A laboratory may choose to procure, produce, o
46、rhave 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.8.3.2.2 A laboratory may find it difficult to procure or havemanufactured the materials described in 8.3.2.1
47、for all of thenecessary analytes or alloys. If this is the case, then it isacceptable to prepare equivalent reference material solutionsusing an alternative source of nickel for the matrix solution andspiked with different single element CRM solutions.9. Hazards9.1 This method involves the use of co
48、ncentrated HF. Readand follow label precautions, MSDS information, and refer toPractice E50. For precautions to be observed in the use ofcertain other reagents in this test method, refer to Practice E50.10. Sampling, Test Specimens, and Test Units10.1 Laboratories shall follow written practices for
49、sam-pling and preparation of test samples. These practices shallmeet all customer requirements. Practices E55 and E88 alsoprovide guidance for sampling.10.2 Test specimens should be obtained by milling ordrilling chips that are clean and of sufficient quantity to fulfillthe sample weight required by the procedure.11. Preparation of Apparatus11.1 Analytical instrumentation and sample preparationequipment shall be installed and operated in a manner consis-tent with manufacturers recommendations.5Reagent Chemicals, American Chemical Society Specificat
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