1、Designation: E2823 11E2823 17Standard Test Method forAnalysis of Nickel Alloys by Inductively Coupled PlasmaMass Spectrometry (Performance-BasedMethod)(Performance-Based)1This standard is issued under the fixed designation E2823; the number immediately following the designation indicates the year of
2、original 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 test method describes the inductively coupled plasma m
3、ass spectrometric analysis of nickel, nickel and nickel allys,as specified by Committee B02, and having chemical compositions within the following limits:Element Application Range (Wt. (MassFraction %)Aluminum 0. 016.00Boron 0. 010.10Carbon 0. 010.15Chromium 0. 0133.00Copper 0.0135.00Cobalt 0. 0120.
4、00Iron 0.0550.00Magnesium 0. 010.020Molybdenum 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 this method.Element Quantification Range (g/g)Antimon
5、y 0.550Bismuth 0.111Gallium 2.954Lead 0.421Silver 135Tin 2.297Thallium 0.53.01.3 This method has only been interlaboratory tested for the elements and ranges specified. It may be possible to extend thismethod to other elements or different composition ranges provided that method validation that incl
6、udes evaluation of methodsensitivity, precision, and bias as described in this document is performed. Additionally, the validation study must evaluate theacceptability of sample preparation methodology using reference materials and/or spike recoveries. The user is cautioned tocarefully evaluate the
7、validation data as to the intended purpose of the analytical results. Guide E2857 provides additional guidanceon method validation.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establ
8、ish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. Specific safety hazard statements are given in Section 9.1 This test method is under the jurisdiction of ASTM Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materia
9、ls and is the direct responsibility ofSubcommittee E01.08 on Ni and Co and High Temperature Alloys.Current edition approved May 1, 2011Jan. 1, 2017. Published July 2011February 2017. Originally approved in 2011. Last previous edition approved in 2011 as E282311.DOI: 10.1520/E2823-11.10.1520/E2823-17
10、.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior ed
11、itions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States12. Referenced Documents2.1 ASTM Standards:2D119
12、3 Specification for Reagent WaterE29 Practice for Using Significant Digits in Test Data to Determine Conformance with SpecificationsE50 Practices forApparatus, Reagents, and Safety Considerations for ChemicalAnalysis of Metals, Ores, and Related MaterialsE55 Practice for Sampling Wrought Nonferrous
13、Metals and Alloys for Determination of Chemical CompositionE88 Practice for Sampling Nonferrous Metals and Alloys in Cast Form for Determination of Chemical CompositionE135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related MaterialsE177 Practice for Use of the Terms Precisio
14、n and Bias in ASTM Test MethodsE691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test MethodE1329 Practice for Verification and Use of Control Charts in Spectrochemical AnalysisE1479 Practice for Describing and Specifying Inductively Coupled Plasma Atomic Emission
15、 SpectrometersE1601 Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical MethodE2027 Practice for Conducting Proficiency Tests in the Chemical Analysis of Metals, Ores, and Related MaterialsE2165 Practice for Establishing an Uncertainty Budget for the Chemica
16、l Analysis of Metals, Ores, and Related Materials(Withdrawn 2007)3E2857 Guide for Validating Analytical MethodsE2972 Guide for Production, Testing, and Value Assignment of In-House Reference Materials for Metals, Ores, and OtherRelated Materials2.2 ISO Standards:4ISOISO/IEC 17025 General Requirement
17、s for the Competence of Calibration and Testing LaboratoriesISO Guide 31 Contents of Certificates of Reference MaterialsISO Guide 34 Quality System Guidelines for the Production of Reference MaterialsISO Guide 98-3 Uncertainty of MeasurementPart 3: Guide to the Expression of Uncertainty in Measureme
18、nt (GUM:1995),First Edition3. Terminology3.1 DefinitionsFor definitions of terms used in this test method, refer to Terminology E135.4. Summary of Test Method4.1 Samples are dissolved in a mixture of mineral acids and the resulting solutions are measured using inductively coupledplasma mass spectrom
19、etry.5. Significance and Use5.1 This test method for the chemical analysis of nickel and nickel alloys is primarily intended to test material for compliancewith specifications such as those under jurisdiction of ASTM committee B02. It may also be used to test compliance with otherspecifications that
20、 are compatible with the test method.5.2 It is assumed that all who use this method will be trained analysts capable of performing common laboratory proceduresskillfully and safely, and that the work will be performed in a properly equipped laboratory.5.3 This is a performance-based method that reli
21、es more on the demonstrated quality of the test result than on strict adherenceto specific procedural steps. It is expected that laboratories using this method will prepare their own work instructions. These workinstructions will include detailed operating instructions for the specific laboratory, t
22、he specific reference materials employed, andperformance acceptance criteria. It is also expected that, when applicable, each laboratory will participate in proficiency testprograms, such as described in Practice E2027, and that the results from the participating laboratory will be satisfactory.6. I
23、nterferences6.1 When possible, analyte isotopes are selected, whichselected that are free from mass overlap interferences. Because isotopechoices are limited, this is not always an option. It is the responsibility of the user to determine run conditions and parameters thatavoid or compensate for int
24、erferences that may bias test results.6.2 The use of an internal standard may compensate for the physical interferences resulting from variations in sample andcalibration solution aerosol transport rates. The user may chose to add the internal standard by spiking each solution with a2 For referenced
25、ASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 The last approved version of this historical standard is referenced on www.
26、astm.org.4 Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http:/www.ansi.org.E2823 172specified amount of an appropriate certified reference material (CRM) solution. Alternatively, on-line addition of a peripheralinternal standard solution
27、 during sample analysis is also possible provided acceptable instrument sensitivity is maintained.6.3 Isobaric and polyatomic mass overlap interferences are best addressed by selecting an alternate atomic mass. Someinstrument manufacturers offer software options for mathematically correcting for com
28、mon interferences, but the user is cautionedto carefully evaluate this approach to mass overlap correction. However, some laboratories participating in the interlaboratorystudy found it necessary to generate a mathematical correction for the effect of the ZrO interference on theAg 107 isotope. In th
29、iscase the Zr 91 isotope was used for zirconium determination.6.4 Modern instruments may have a collision or reaction cell whichthat can use ion-molecule collisions or reactions to removespectral interferences. The user of this method must examine this information to ascertain the need for collision
30、/reaction cells forthe removal of spectral interferences. However, it should be noted that no collision/reaction gases were used by the laboratoriesparticipating in the interlaboratory study of the elements listed in the Scope, thus implying that the use of collision/reaction gasesis not required fo
31、r determination of those elements.6.5 The isotopes listed in Table 1 have been used to analyze the listed elements in nickel alloys and are suggested for the user.The user may choose to use multiple isotopes to help verify that atomic mass selection is optimized for the particular alloy beingdetermi
32、ned. It is recommended that once isotopes and appropriate spectral corrections are determined, the user of this methodspecify this information or reference instrument programs, which include this information in their laboratory analysis procedures.7. Apparatus7.1 Suitability of an Inductively Couple
33、d Plasma Mass Spectrometer for testing of this method will be established using theperformance criteria described in section 12.1. The sample introduction system shall be capable of handling solutions containingtrace amounts of HF. Each instrument shall be installed and operated according to the man
34、ufacturers recommendations.7.2 Sample Preparation EquipmentMachine tools shall be used that are capable of removing surface oxides and othercontamination from the as-received sample and then taking uncontaminated and chemically representative chips suitable foranalysis.7.3 All labware used should be
35、 suitably cleaned for trace level analysis.8. Reagents and Materials8.1 Reagents:8.1.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents conform to the specifications of the Committee on Analytical Reagents of the Americ
36、an Chemical Society where suchspecifications are available.5 However, the purity of acid reagents utilized in this procedure shall be suitable for trace metal analysisand should not contain impurities in any significant amount. amount of the analyte. Other grades may be used, provided it is firstasc
37、ertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination.8.1.2 Reagent Purity of WaterThe purity of reagent water water used in this test method shall conform to the requirementsof Specification D1193 for reagent water, Type I. Th
38、e water purification method used must be capable of removal of all elementsin concentrations that might bias the test results.8.1.3 Internal StandardThe use of an internal standard is recommended. The use of an internal standard may compensate forthe physical interferences resulting from variations
39、in sample and calibration solution aerosol transport rates. Select an internalstandard element of similar atomic mass to the analyte and one that is not commonly found in the samples to be determined. Theexact concentration added is not critical, however, the amount added should yield a significant
40、signal when measured.8.2 Calibration Solutions:5 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. https:/.acs.pubs.org/reagents/index.html. For suggestionson the testing of reagents not listed by the American Chemical Society, see the United Sta
41、tes Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention, Inc.(USPC), Rockville, MD, https:/www.usp.org.TABLE 1 Suggested Isotopes/InterferenceElement Isotope PotentialInterferenceAntimony 121Bismuth 209Gallium 71Lead 208Silver 107 ZrO, FeCrTin 120 MoOThallium 205E2823 1738.2.1 In this
42、 test method, calibration is based on laboratory-prepared, pure nickel matrix- matched solutions. The matrixsolutions are prepared with nickel of known purity. These matrix solutions are then spiked with aliquots of single element certifiedreference material (CRM) solutions which contain the element
43、s of interest. The CRMs shall be compliant with ISO Guides 31 and34.8.2.2 Step 8.2.3 and following describe the preparation of calibration solutions for analysis of sample solutions that contain 1g alloy/L final dilution. It is acceptable to vary final concentrations as long as the users method demo
44、nstrates adequate sensitivityand precision (see section 12.1).8.2.3 Determine the number and composition of calibration solutions needed to cover the concentration range for each element.It is suggested that the calibration solutions have their highest concentration slightly above the highest expect
45、ed sampleconcentration, a concentration in the mid range mid-range of the expected sample concentrations, a concentration at or near thereporting limit, and a blank. In any case, a minimum of three solutions including a blank must be used for calibration.8.2.4 Prepare matrix solutions as follows:8.2
46、.4.1 Weigh 0.5 g of pure nickel into an HF resistant digestion vessel. Use one vessel for each calibration solution to be made.Note that using 0.5 g of nickel approximates the mass fraction of nickel (50 %) found in 1 g of a typical nickel alloy.8.2.4.2 Dissolve the pure nickel in 20 mL of acid mixt
47、ure per gram of sample. Select acid mixtures that will dissolve the alloysto be analyzed using this method.NOTE 1Caution: If powdered nickel is used, add the acid cautiously as powdered metals tend to be very reactive.Caution: If powdered nickel is used, add the acid cautiously as powdered metals te
48、nd 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) will dissolvemany types of nickel alloys . For high Mo-Cr alloys it has been found that concentrated HCl with the addition of concentratedHNO3 dropwise may be necessary to avo
49、id passivation.8.2.4.4 Heat the digestion vessels gently until the nickel dissolves. Remove the beakers from the heat, add 10 drops of 49 %HF, and swirl gently. If HNO3 + HF + H2O (1 + 1 + 1) is used for digestion, it is not necessary to add additional HF. The laboratorymay choose to reduce this solution to wet salts in order to remove excess HF and then re-dissolve by heating the salts inapproximately 20 mL of water.8.2.4.5 If an internal standard is to be used, add the predetermined amount into each solution.8.2.4.6 Cool the nickel solutions
