1、Designation:E183409 Designation: E1834 11Standard Test Method forDeterminationAnalysis of Lead in Nickel Alloys by GraphiteFurnace Atomic Absorption Spectrometry1This standard is issued under the fixed designation E1834; the number immediately following the designation indicates the year oforiginal
2、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. Scope1.1This test method covers the determination of lead in nickel alloys in
3、 the concentration range 0.00005% to 0.001% by graphitefurnace atomic absorption spectrometry (GF-AAS).NOTE1If this test method is used to test materials having contents less than 0.0001% lead, users in different laboratories may experience more thanthe usual 5% risk that their results will differ b
4、y more than 50% relative error.1.2The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.3This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of
5、 this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. For specific hazards associated with the use of this test method, see Practices E50.1.1 This test method describes the graphite furnace atomic absorption spectro
6、metric analysis of nickel, such as specified byASTM Committee B02, and having chemical compositions within the following limits:Element Application Range (Wt. %)Aluminum 0. 01 - 6.00Boron 0. 01 - 0.10Carbon 0. 01 - 0.15Chromium 0. 01 - 33.00Copper 0.01 - 35.00Cobalt 0. 01 - 20.00Iron 0.05 - 50.00Mag
7、nesium 0. 01 - 0.020Molybdenum 0. 01 - 30.0Niobium 0. 01 - 6.0Nickel 25.00 - 100.0Phosphorous 0.001 - 0.025Silicon 0.01 - 1.50Sulfur 0.0001 - 0.01Titanium 0.0001 - 6.0Tungsten 0.01 - 5.0Vanadium 0.0005 - 1.01.2 The following elements may be determined using this test method:Element Quantification Ra
8、nge (g/g)Bismuth 0.2 - 3Lead 0.6 - 12Selenium 0.7 - 10Tellurium 0.4 - 61.3 This test method has only been interlaboratory-tested for the elements and ranges specified. It may be possible to extendthis test method to other elements or different concentration ranges provided that a test method validat
9、ion study that includes aninstrument performance evaluation as described in Practice E1770 is performed. Additionally, the validation study shall evaluatethe acceptability of sample preparation methodology using reference materials or spike recoveries, or both. The user is cautionedto carefully eval
10、uate the validation data as to the intended purpose of the analytical results.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 establish appropriate safety and health practices and deter
11、mine the applicability of regulatory1This test method is under the jurisdiction of ASTM Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials and is the direct responsibility ofSubcommittee E01.08 on Ni and Co and High Temperature Alloys.Current edition approved July 15, 2009
12、. Published August 2009. Originally approved in 1996. Last previous edition approved in 2002 as E183496(2002). DOI:10.1520/E1834-09.Current edition approved Dec. 1, 2011. Published February 2012. Originally approved in 1996. Last previous edition approved in 2009 as E1834 09. DOI:10.1520/E1834-11.1T
13、his 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 edit
14、ions 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 States.limitations prior to use. For specific hazards st
15、atements see Note 2 and Section 9.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterE50 Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related MaterialsE135Terminology Relating to Analytical Chemistry for Metals,
16、Ores, and Related MaterialsE882Guide for Accountability and Quality Control in the Chemical Analysis Laboratory 55 Practice for Sampling WroughtNonferrous Metals and Alloys for Determination of Chemical CompositionE1184Practice for Determination of Elements by Graphite Furnace Atomic Absorption Spec
17、trometry 88 Practice for SamplingNonferrous Metals and Alloys in Cast Form for Determination of Chemical CompositionE1601Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical Method 135 TerminologyRelating to Analytical Chemistry for Metals, Ores, and Related
18、MaterialsE177 Practice for Use of the Terms Precision 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 AnalysisE1770 Practice for Optimization of
19、Electrothermal Atomic Absorption Spectrometric Equipment Practice for Optimization ofElectrothermal Atomic Absorption Spectrometric EquipmentE2027 Practice for Conducting Proficiency Tests in the Chemical Analysis of Metals, Ores, and Related Materials2.2 ISO Standards:3ISO5725:1986Precision of Test
20、 Methods Determination of Repeatability and Reproducibility for aStandard Test Method by Inter-Laboratory TestsISO11437:1994Nickel Alloys Determination of Trace-Element Content Electrothermal Atomic Absorption SpectrometricMethodPart 2: Determination of Lead Content ISO Guide 31 Contents of certific
21、ates of reference materialsISO Guide 34 Quality system guidelines for the production of reference materialsISO Guide 98-3 Uncertainty of measurement Part 3: Guide to the expression of uncertainty in measurement (GUM:1995) 1st Ed.3. Terminology3.1 DefinitionsFor definitions of terms used in this test
22、 method, refer to Terminology E135.4. Summary of Test Method4.1The sample is dissolved in a mixture of HNO3, HF, and water and diluted to a known volume. A nickel-ammonium phosphatematrix modifier is added to an appropriate aliquot and a portion is injected into the graphite furnace atomizer of an a
23、tomicabsorption spectrometer, which is provided with a background corrector. The sample is dried, pyrolized, and atomized. Theabsorbance of the resonance spectral line of lead is measured at 283.3 nm and compared with that from matrix-matched calibrationsolutions.4.1 Samples are dissolved in a mixtu
24、re of mineral acids and the resulting solutions are measured using graphite furnace atomicabsorption spectrometry.5. Significance and Use5.1This test method is used for the determination of trace levels of lead in nickel alloys by GF-AAS to check compliance withcompositional specifications. It is as
25、sumed that the procedure will be performed by trained analysts capable of performing commonlaboratory practices skillfully and safely. It is expected that the work will be performed in a properly equipped laboratory andproper waste disposal procedures will be followed. Appropriate quality control pr
26、actices must be followed such as those describedin Guide E882.5.1 This test method is primarily intended to test material for compliance with specifications such as those under the jurisdictionof ASTM Technical Committee B02 on Nonferrous Metals and Alloys. It may also be used to test compliance wit
27、h otherspecifications that are compatible with the test method.5.2 It is assumed that users of this test method shall be trained analysts capable of performing common laboratory proceduresskillfully and safely, and that the work shall be performed in a properly equipped laboratory.5.3 This is a perf
28、ormance-based method that relies more on the demonstrated quality of the test result than on strict adherenceto specific procedural steps. It is expected that laboratories using this test method shall prepare their own work instructions. Thesework instructions shall include detailed operating instru
29、ctions for the specific laboratory, the specific reference materials employed,and the performance acceptance criteria. It is also expected that, when applicable, each laboratory shall participate in proficiencytest programs, such as described in Practice E2027, and that the results from the particip
30、ating laboratory shall be satisfactory.2For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3Available from Amer
31、ican National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http:/www.ansi.org.E1834 1126. Apparatus6.1Atomic Absorption Spectrometer , with graphite furnace atomizer, and equipped with an appropriate background corrector,a signal output device, such as a video display s
32、creen, a digital computer, a printer or strip chart recorder, and an autosampler.6.2Pyrolytically Coated Graphite Tubes, grooved, conforming to the instrument manufacturers specifications.6.3Pyrolytic Graphite Platforms, Lvov design, fitted to the tubes specified in 6.2.6.4Radiation Source, lead hol
33、low cathode lamp, or electrodeless discharge lamp with an appropriate power supply.7.Instrument Parameters and Criteria7.1The atomic absorption spectrometer and graphite furnace atomizer are satisfactory if, after adjustment of the instrument andoptimization of the furnace heating program as describ
34、ed in Practice E1770, they meet the criteria given in 7.4-7.7. For generaldiscussion of the theory and instrumental requirements of GF-AAS, see Practice E1184.7.2Calibration solutions S0through S5prepared in accordance with 8.9 and summarized in Interferences6.1 The narrow bandwidth emitted by the s
35、ource lamp makes spectral overlaps rare. However, molecular absorption bands aremore likely to overlap the atomic absorption line. This problem is commonly encountered in complex nickel alloys and abackground correction technique shall be employed. The use of the Zeeman background correction techniq
36、ue should be used inperformance of this test method.6.2 When Zeeman background correction is used for nickel alloy analysis, background absorbance up to approximately 1.5absorbance units is adequately corrected for. The user is cautioned to examine calibration and sample solution background levelsdu
37、ring method validation to verify that background absorbance is less than 1.5 absorbance units.6.3 One significant problem may be encountered for determination of bismuth in alloys with iron in excess of 10 %. It ispossible that use of Zeeman background correction will cause over-correction for backg
38、round, resulting in erroneously low results.This potential problem results from reading the shifted pi (p) absorption components of the iron 222.9 nm line during thebackground read cycle. All modern spectrometers and those with chart recorders allow inspection of absorption profiles obtainedduring a
39、nalysis. During initial instrument optimization and method validation, the user of this test method shall assess the effectof this possible issue on the results to be reported. Adjustment of char time and temperatures may help minimize this problem.Bismuth determinations made using the peak height m
40、easurement mode may also help minimize the error associated with thisissue.6.4 The atomic lines in Table 1 shall be used for testing criteria.7.3The parameters for the determination of lead and the establishing of the instrument criteria are as follows:7.3.1The injection volume is 20 L.7.3.2The peak
41、 area absorbance integration measurements shall be at a wavelength of 283.3 nm.7.4Characteristic MassThe characteristic mass determined in accordance with Practice E1770 shall be within 20% of thatgiven in the manufacturers literature.7.5PrecisionThe variability obtained from calibration solution S3
42、shall not exceed 10% of the mean absorbance of the samesolution, and the variability of calibration solution S1shall not exceed 4% of the mean absorbance of solution S3when determinedin accordance with Practice E1770have been used to analyze the listed elements in nickel alloys and are suggested for
43、 the user.The user may choose to use different atomic lines provided that sensitivity is adequate. It is recommended that once atomic linesare determined, the user of this test method specify this information or reference instrument programs that include this informationin their laboratory analysis
44、procedures.7. Apparatus7.1 Graphite Furnace Atomic Absorption Spectrometer, preferably equipped with a Zeeman background correction accessory.Suitability of the spectrometer shall be established using the performance criteria described in 12.7.TABLE 1 LSuggeasted C Atonmicent Absoraption of CAnalyti
45、brcatl Lion Solues/Intioerference/ModifiersCalibrationSolutiong/L ng/mL g/gElement Wavelength (nm) g/gS00 0 0S00 0 0Potential InterferenceS110 10 2Bismuth 10 10 2S220 20 4223.1 20 20 4FeLead S330 30 6Lead 283.3 30 30 6Selenium S440 40 8Selenium 196.0 40 40 8Tellurium S560 60 12Tellurium 214.3 60 60
46、12ABased 0.500 g sample/100 mL sample solution (10.1).E1834 1137.6Limit of DetectionThe limit of detection of lead as described in Practice E1770 shall be less than 20 pg (equivalent to 1.0g/L lead in the test solution or 0.2 g/g in the original sample).7.7LinearityThe linearity of the calibration a
47、s determined in Practice E1770 shall be not less than 0.7.7.2 Graphite Tubes used in this test method shall utilize a Lvov type platform.7.3 Sample Preparation EquipmentMachine tools used in this test method shall be capable of removing surface oxides andother contamination from the as-received samp
48、le and then taking uncontaminated and chemically representative chips suitable foranalysis.7.4 All labware used in this test method shall be suitably cleaned for trace level analysis.8. Reagents Reagents and Materials8.1 Purity and Concentration of ReagentsThe purity and concentration of common chem
49、ical reagents and water shallconform to Practices E50. The reagents should be free of, or contain minimal amounts (0.01 g/g) of, lead.8.2Dissolution Acid MixtureTo 150 mL water carefully add 150 mL HNOReagents: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 American Chemical Society where suchspecifications are available.4However, the purity of acid reagents utilized in this procedure s
