1、Designation: E3061 17Standard Test Method forAnalysis of Aluminum and Aluminum Alloys by InductivelyCoupled Plasma Atomic Emission Spectrometry(Performance Based Method)1This standard is issued under the fixed designation E3061; the number immediately following the designation indicates the year ofo
2、riginal 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 coupledplasma ato
3、mic emission spectrometric analysis of aluminumand aluminum alloys for the following elements:ElementsApplication Range, %Minimum MaximumSi 0.02 16.8Fe 0.02 3.06Cu 0.005 7.0Mn 0.003 1.41Mg 0.006 8.2Cr 0.004 0.52Ni 0.004 2.71Zn 0.02 9.65Ti 0.009 0.20Ag 0.003 0.4As 0.005 0.012B 0.009 0.027Ba 0.002 0.0
4、3Be 0.002 0.11Bi 0.01 0.59Ca 0.003 0.048Cd 0.002 0.055Co 0.002 0.034Ga 0.01 0.019Li 0.001 2.48Mo 0.02 0.15Na 0.008 0.026P 0.01 0.025Pb 0.009 0.51Sb 0.01 0.28Sc 0.01 0.065Sn 0.008 6.28Sr 0.0008 0.028Ti 0.005 0.20Tl 0.009 0.13V 0.01 0.12Zr 0.004 0.251.2 This test method has only been interlaboratory t
5、ested forthe elements and ranges specified. It may be possible to extendthis test method to other elements or different compositionranges if method validation, which includes evaluation ofmethod sensitivity and precision and bias (as described inSection 14), is performed. Additionally, the validatio
6、n studymust evaluate the acceptability of sample preparation method-ology using reference materials and/or spike recoveries. Theuser should carefully evaluate the validation data against thelaboratorys data quality objectives. Method validation ofscope extensions is also a requirement of ISO/IEC 170
7、25.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.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 a
8、ppro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Safety hazardstatements are given in Section 10 and specific warningstatements are given in Sections 15, 17, 18, 19, 20 and 21.2. Referenced Documents2.1 ASTM Standards:2B985 Practice for
9、 Sampling Aluminum Ingots, Billets, Cast-ings and Finished or Semi-Finished Wrought AluminumProducts for Compositional AnalysisD1193 Specification for Reagent WaterE34 Test Methods for Chemical Analysis of Aluminum andAluminum-Base AlloysE50 Practices for Apparatus, Reagents, and Safety Consid-erati
10、ons for Chemical Analysis of Metals, Ores, andRelated MaterialsE135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE406 Practice for Using Controlled Atmospheres in Spec-trochemical AnalysisE
11、691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method1This test method is under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores, and Related Materials and is the directresponsibility of Subcommittee E01.04 on Aluminum and Magne
12、sium.Current edition approved Jan. 15, 2017. Published March 2017. DOI: 10.1520/E3061172For 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 Summar
13、y 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 internationally recognized principles on standardization established in the Decision on Principles f
14、or theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1E716 Practices for Sampling and Sample Preparation ofAluminum and Aluminum Alloys for Determination ofChemical Composition by Spark Atomic Emis
15、sion Spec-trometryE1329 Practice for Verification and Use of Control Charts inSpectrochemical AnalysisE1452 Practice for Preparation of Calibration Solutions forSpectrophotometric and for Spectroscopic Atomic Analy-sis (Withdrawn 2005)3E1479 Practice for Describing and Specifying InductivelyCoupled
16、Plasma Atomic Emission SpectrometersE2857 Guide for Validating Analytical Methods2.2 ISO Standards4ISO/IEC 17025 General Requirements for the Competenceof Calibration and Testing LaboratoriesISO Guide 98-3 Uncertainty of Measurement Part 3:Guide to the Expression of Uncertainty in Measurement(GUM:19
17、95) - First Edition3. Terminology3.1 DefinitionsFor definitions of terms used in this testmethod, refer to Terminology E135.4. Summary of Test Method4.1 The test specimen, in the form of drillings, chips,millings, turnings, small pieces or powder, is dissolved in acaustic solution or a mixture of di
18、lute mineral acids andhydrogen peroxide or sodium nitrite and the resulting solutionsare measured using inductively coupled plasma atomic emis-sion spectrometry. The spectrometer is calibrated using cali-bration solutions prepared to match the sample matrix, using apure aluminum stock solution prepa
19、red in 15.2 and stocksolutions traceable to an SI unit through a national metrologylaboratory or stock solutions prepared as directed in PracticeE1452.5. Significance and Use5.1 This test method for the analysis of aluminum andaluminum alloys is primarily intended to test material forcompliance with
20、 The Aluminum Association Inc.5registeredcomposition limits or other specified composition limits foraluminum and aluminum alloys.5.2 It is assumed that all who use this test method will betrained analysts capable of performing common laboratoryprocedures skillfully and safely, and that the work wil
21、l beperformed in a properly equipped laboratory.5.3 This is a performance-based test method that relies moreon the demonstrated quality of the test result than on strictadherence to specific procedural steps. It is expected thatlaboratories using this test method will prepare their own workinstructi
22、ons. These work instructions should include detailedoperating instructions for the specific laboratory, the specificreference materials employed, and performance acceptancecriteria.6. Interferences6.1 The effect of potential spectral overlap interferences andbackground will vary based on the wavelen
23、gths selected,instrument design, and may vary from instrument to instrumentof the same design. Variation of excitation conditions oroperating parameters may enhance or minimize these interfer-ences. For these reasons, the effect of the potential interfer-ences must be thoroughly investigated for eac
24、h element andmatrix on the instrument chosen for analysis. Practice E1479describes the typical physical and spectral interferences en-countered during the inductively coupled plasma spectrometricanalysis of metal alloys. Potential spectral interferences forrecommended wavelengths are given in Table
25、1. The user isresponsible for ensuring the absence of, or for compensatingfor, interferences that may bias test results obtained using theirparticular spectrometer.6.2 The use of an internal standard may compensate for thephysical interferences resulting from differences betweensample and calibratio
26、n solutions transport efficiencies.6.3 Shifts in background intensity levels because of, forexample, recombination effects or molecular bandcontributions, or both, may be corrected by the use of anappropriate background correction technique. Direct spectraloverlaps are best addressed by selecting al
27、ternative wave-lengths. If alternate wavelengths are not available, spectralinterference studies should be conducted on all new matrices todetermine the interference correction factor(s) that must beapplied to compositions obtained from certain spectral lineintensities to minimize biases. Some instr
28、ument manufacturersoffer software options that mathematically correct for directspectral overlaps, but the user should carefully evaluate thisapproach to spectral correction.6.4 Modern ICP spectrometers typically have software thatallows comparison of a sample spectrum to the spectrumobtained from a
29、 blank solution. The user of this test methodmust examine this information to ascertain the need forbackground correction and the correct placement of back-ground points.6.5 Table 1 recommends wavelengths from the NISTAtomic Spectra Database6that may be used for the analysis ofaluminum and aluminum
30、alloys. In this database, wavelengthsof less than 200 nm were measured in vacuum and wavelengthsgreater than or equal to 200 nm were measured in air. Softwaretables for individual instruments may list wavelengths some-what differently, as instrument optical path atmospheric con-ditions may vary.6.6
31、Information on potential spectral interfering elementstypically found in aluminum alloys was provided by some ofthe laboratories participating in the interlaboratory study and3The last approved version of this historical standard is referenced onwww.astm.org.4Available from American National Standar
32、ds Institute (ANSI), 25 W. 43rd St.4th Floor, New York, NY 10036, http/www.ansi.org5Available from The Aluminum Association Inc., 1400 Crystal Drive, Arlington,VA 22202, http:/www.aluminum.org/6Available from The National Institute of Standards and Technology 100 BureauDr., Gaithersburg, MD 20899 ht
33、tps:/www.nist.gov/E3061 172TABLE 1 Analytical Lines and Possible InterferencesElement Wavelength, nm Possible InterferencesAntimony 206.833 W, Fe, Ni, Be259.805 FeArsenic 189.042 Cr193.759 Zr197.262 PbBarium 455.403 Zr493.409Beryllium 234.861 Fe, Zr313.042 Ti, V313.107 TiBismuth 222.825 Cr, Cu, Ti22
34、3.061 Cu, Ni, Ti306.772Boron 208.959 Sn, Fe249.678 Sn, Fe, Ni, Ca249.773 Ni, VCadmium 226.502 Co, Ni228.802 AsCalcium 315.887 Cr, Zr317.933 W393.366 ZrChromium 205.552 Be, Cu, Ni267.716283.563357.869 ZrCobalt 228.616 Mo, Ni, Fe238.892 Fe, MoCopper 221.458 Cr221.810 Si223.008 Bi, Mn, Ti, V224.700 Ni3
35、24.754327.396Gallium 294.364 Fe, Ti, Cr417.206 Ni, Fe, CoIndium 410.172 Cr, Ti451.131 MoIron 238.204 V, Zr239.562259.837259.940Lead 182.203220.353 Bi283.306 CrLithium 670.784 Co, Mo, FeMagnesium 257.610 Mn, Ti259.373 Mn260.569 Mn, Ti, V293.306 Fe, Zr293.930 ZrManganese 257.610259.373260.569 Ti293.30
36、6 Cr293.930Molybdenum 202.030 Ni, Co, Mn277.540 AIE3061 173may have originated from sources such as recognized wave-length reference tables, instrument manufacturers softwarewavelength tables, an individual laboratorys wavelength re-search studies, or a combination thereof.6.7 The user must verify t
37、hat the selected wavelengthperforms acceptably in their laboratory, preferably duringmethod validation (see Section 23). Total dissolved solids, pH,and viscosity should be similar between sample solutions andcalibration solutions. The user also may choose to use multiplewavelengths to help verify th
38、at line selection is optimized forthe particular alloy being analyzed. It is recommended thatwhen wavelengths and appropriate spectral corrections aredetermined, the user of this test method should specify thisinformation or reference instrument programs that include thisinformation in their laborat
39、ory analysis procedures.TABLE 1 ContinuedElement Wavelength, nm Possible InterferencesNickel 221.647231.604232.003239.452Phosphorus 177.499 Cu, Be178.287 AIPotassium 404.721 Ba766.490 Mo, CrScandium 361.384 Mo, Zr, Cr363.075 Ca, FeSilicon 212.412 V250.690 V251.612 V, Zn288.158 Cr, ZrSilver 328.068 M
40、n338.289 Cr, SbSodium 330.237589.592 Cr, ZnStrontium 407.771 Fe421.552 Cr, CuTin 189.989 Ti242.949 FeThallium 276.787190.896Titanium 323.452 Ni, Zr323.657 Mn, Zr334.904334.941336.121 Ni337.280 ZrVanadium 290.646 Ti290.882 Cr292.402 Cr310.230 Ni311.838 Cr, TiZinc 202.548 Cr, Cu, Mg, Ni206.200 Bi, Cr,
41、 Ti213.856 Cu, Ni, Ti, V472.216 Bi481.053Zirconium 327.305339.198343.823349.621 MnE3061 1747. Apparatus7.1 Inductively Coupled Plasma Atomic EmissionSpectrometersRefer to Practice E1479 for attributes to con-sider when selecting an appropriate instrument.8. Reagents and Materials8.1 Reagents:8.1.1 P
42、urity and Composition of Reagents7The purity andcomposition of chemical reagents shall conform to the require-ments prescribed in Practices E50. Reagent grade chemicals orbetter shall be used in all tests.8.1.2 Alcohol, ethanol or methanol.8.1.3 Boric Acid (H3BO3).8.1.4 Hydrogen Peroxide (H2O2), 30
43、%.8.1.5 10.5 N Sodium Hydroxide (NaOH) Solution.8.1.6 4 % Sodium Nitrite (NaNO2) Solution.8.1.7 Metals of the highest purity available and havingknown impurity content should be used if preparing stocksolutions as directed in Practice E1452.8.1.8 Purity of WaterReferences to water shall be under-sto
44、od to mean reagent water, Type II grade, as defined bySpecification D1193. The water purification method used mustbe capable of removal of all elements that might bias the testresults.8.1.9 Argon, of 99.998 % purity, has been found satisfac-tory. For information on gas handling, refer to Practice E4
45、06.8.1.10 Stock Solutions, if needed, shall be prepared asdirected in Practice E1452.8.1.11 Certified Reference Materials (CRMs), in chip formare available from some national metrology organizations andcommercial sources.8.1.12 Single Element Certified Reference MaterialSolutionsare available from s
46、ome national metrology orga-nizations and commercial sources.8.1.13 Aluminum Metal (Al), for matrix matching calibra-tion solutions. Aluminum that is at least 99.999 % is recom-mended. Aluminum that is less pure may be used provided theimpurities are not present at levels that affect the measuredamo
47、unt for elements of interest or the internal standard if used.8.2 Internal StandardThe use of an internal standard isnot required but is recommended. The use of an internalstandard may compensate for the physical interferences result-ing from differences in sample and calibration solutionstransport
48、efficiency. Lanthanum, Co, Sc, Be, and Y were usedby participants in the Interlaboratory Study (ILS). Wavelengthsused and potential interferences are given in Table 2.Itisimportant that the element chosen for an internal standard isnot present in the samples at a level that will affect the analysis.
49、9. Control Materials9.1 A laboratory may procure or produce a chip materialwith a composition that is similar to the samples for use as acontrol material. These chips should have low heterogeneityand be well blended. Users of this test method may also usecertified reference materials as control materials.9.2 A laboratory may find it difficult to procure or producethe materials for all of the necessary analytes or alloys. Here,it is acceptable to prepare equivalent reference material solu-tions using the procedure described in Section 15 for use ascontrol solutions.10.
