1、Designation: E 1835 96 (Reapproved 2002)Standard Test Method forAnalysis of Nickel Alloys by Flame Atomic AbsorptionSpectrometry1This standard is issued under the fixed designation E 1835; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revi
2、sion, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers analysis of nickel and nickel-base alloys by flame atomic absorption spectr
3、ometric analysisfor the following elements:Element Concentration Range,%SectionAluminum 0.2 to 4.0 12Chromium 0.01 to 4.0 13Cobalt 0.01 to 4.0 14Copper 0.01 to 4.0 15Iron 0.1 to 4.0 16Manga-nese0.1 to 4.0 17Silicon 0.2 to 1.0 18Vanadium 0.05 to 1.0 191.2 The concentration range of these elements can
4、 beexpanded by the use of appropriate standards.1.3 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 determine the applica-bility of reg
5、ulatory limitations prior to use. For specific hazardsassociated with the use of this test method see Practices E 50and the warning statements included in this test method.2. Referenced Documents2.1 ASTM Standards:2E 50 Practices for Apparatus, Reagents, and Safety Precau-tions for Chemical Analysis
6、 of Metals, Ores, and RelatedMaterialsE 863 Practice for Describing Flame Atomic AbsorptionSpectroscopy EquipmentE 882 Guide for Accountability and Quality Control in theChemical Analysis LaboratoryE 1452 Practice for Preparation of Calibration Solutions forSpectrophotometric and for Spectroscopic A
7、tomic Analy-sisE 1812 Practice for Optimization of Flame Atomic Absorp-tion Spectrometric Equipment2.2 ISO Standards:ISO Guide 5725Accuracy, Trueness, and Precision ofMeasurements, Methods and Results3ISO 7530 Parts 2 through 9Flame Atomic AbsorptionSpectrometric Analysis33. Summary of Test Method3.
8、1 The sample is dissolved in a mixture of hydrochloricacid and nitric acid. The solution is aspirated into an appropri-ate flame of an atomic absorption spectrometer. Measurementof the absorbance of the resonant line energy from thespectrum of the analyte is compared with that of calibrationsolution
9、s.4. Significance and Use4.1 This test method is used for the analysis of nickel andnickel-base alloy samples by flame atomic absorption spec-trometry to check compliance with compositional specifica-tions. It is assumed that all who use the procedure will betrained analysts capable of performing co
10、mmon laboratoryprocedures skillfully and safely. It is expected that the workwill be performed in a properly equipped laboratory and thatproper waste disposal procedures will be followed.Appropriatequality control practices must be followed such as thosedescribed in Guide E 882.4.2 Interlaboratory S
11、tudies (ILS)4This test method wasevaluated by a subcommittee within ISO Technical Committee155 (ISO/TC 155/SC 4) on analysis of nickel alloys, inaccordance with ISO Standard 5725. It was published as ISOStandard 7530, Parts 2 through 9. The ILS test data was not1This test method is under the jurisdi
12、ction 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-TemperatureAlloys.Current edition approved Oct. 10, 1996. Published December 1996.2For referenced ASTM standards, visit the ASTM web
13、site, 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.3Available fromAmerican National Standards Institute, 25W. 43rd St., 4th Floor,New York, NY 10036.4Supporting d
14、ata are available from ASTM International Headquarters. RequestRR:E01-1018.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.available for recalculation. The published ISO statistics aresummarized separately for each analyte.5. Apparat
15、us5.1 Atomic Absorption Spectrometer, equipped with anappropriate background corrector, a signal output device (suchas a video display screen (VDS), a digital computer, a printeror strip chart recorder, and an optional autosampler.5.2 Radiation SourceHollow cathode lamp or electrode-less discharge l
16、amp for the analyte(s).5.3 For a general discussion of the instrumental require-ments of flame atomic absorption see Practice E 863.5.4 For a general discussion of apparatus requirements seePractices E 50.6. Reagents6.1 Purity and Concentration of ReagentsThe purity andconcentration of common chemic
17、al reagents shall conform toPractices E 50. The reagents should be free of or containminimal amounts (0.1 g/g) of the analyte of interest.6.2 Calibration SolutionsMade up for the individual ana-lytes as described in Sections 12-19. They should be preparedto meet the guidelines of Practice E 1452.6.3
18、 Matrix Modifiers and Ionization BuffersMade up forthe individual analytes, where required, as described in Sec-tions 12-19.7. Sampling and Sample Preparation7.1 Sampling and sample preparation is to be performed byprocedures agreed upon between the buyer and the seller.7.2 The sampling procedure sh
19、all not involve any steps orprocedures that can result in the loss of any analyte in thesample.NOTE 1Arc melting of the sample or induction melting of the sampleunder vacuum can result in significant loss of several elements that havea low vapor pressure.Arc melting of the sample should be performed
20、 onlyafter careful consideration of all elements to be determined on the meltedsample. Induction melting should be performed only in a complete orpartial inert atmosphere.7.3 The laboratory sample is normally in the form ofturnings, millings, or drillings and no further mechanicalpreparation of the
21、sample is necessary.7.4 The laboratory sample shall be cleaned by washing inpure acetone and then air dried.7.5 If brazed alloy tools are used in the preparation of thesample, the sample shall be further cleaned by pickling indilute nitric acid for a few minutes. The sample shall then bewashed sever
22、al times with water followed by several washeswith acetone and air dried.8. General Procedure8.1 Sample Dissolution:8.1.1 Transfer a 1.0-g sample, weighed to the nearest 1 mg,to a 600-mL beaker. Add 15 mL HCl and 5 mL HNO3. Applysufficient heat to initiate and maintain the reaction until thedissolut
23、ion is complete. If the sample contains over 0.5 %silicone, a few drops of HF will considerably speed up thedissolution.NOTE 2Warning: This operation will emit corrosive, noxious, andtoxic gases and should only be performed in a fume hood. Proper personalsafety equipment shall be worn and used.8.1.2
24、 If the sample resists dissolution, some adjustment ofthe acid mixture may be required.Add HCl in 1-mLincrementsand continue heating to dissolve the sample.NOTE 3For some alloys a 30-mL HCl2-mL HNO3mixture is moreeffective. Pure nickel or nickel-copper alloys dissolve best in HNO3(1+1).NOTE 4The gen
25、eral method of dissolution can be modified asspecified in the appropriate sections.NOTE 5If sample inhomogeneity is suspected, a larger mass ofsample (10 to 50 g) may be taken for analysis. In that case, however, analiquot portion corresponding to 1-g sample shall be taken from thesolution and proce
26、ssed in accordance with the procedure given.8.1.3 Using low heat, evaporate the solution just to dryness.Do not bake. Cool to about 50C and add 25 mL HCl and againevaporate just to dryness. Add 25 mL HCl and repeat theevaporation.8.1.4 Cool to about 50C, add 5 mL hydrochloric acid and20 mL water and
27、 heat to dissolve the salt.8.1.5 Proceed as directed in Sections 12-19.8.2 Reagent BlankCarry a reagent blank through theentire procedure using the same amounts of all reagents withthe omitted sample.8.3 Calibration SolutionsProceed as directed in Sections12-19.8.4 Atomic Absorption Measurements:8.4
28、.1 The wavelength of the spectral lines and the flametype to be used are listed in Sections 12-19.8.4.2 Set the required instrument parameters in accordancewith the manufacturers recommendations and PracticeE 1812. Light the burner and aspirate water until thermalequilibrium is reached. The flame co
29、nditions will vary accord-ing to the element being determined. Zero the instrument.8.4.3 Ensure that the instrument meets the performancerequirements given in Practice E 1812. Optimum settings forTABLE 1 Nominal Composition of Test Samples, %Test Material Al Co Cr Cu Fe Mn Mo Nb Ni Si Ti V Zr825 0.2
30、 0.07 21 1.6 30 0.7 . . Bal 0.4 1.1 . .902 0.4 0.05 5 0.04 48 0.4 . . Bal 0.35 2.5 . .3920 0.15 2 19 0.1 3 0.3 . . Bal 0.6 2.3 . .3927 0.1 1 20 0.05 44 0.4 . . Bal 0.8 0.6 . .7013 1.5 17 20 0.2 0.2 0.05 . . Bal 0.7 2.4 . .7049 1 0.01 15 0.15 7 0.8 . . Bal 0.3 2.3 . .925 0.3 0.2 21 . 27 . 3 0.4 Bal .
31、 2 0.05 0.05NPK31 0.5 14 20 . 1 . 4.5 5 Bal . 2 0.3 .IN100 5.5 15 10 . 0.5 . 3 . Bal . 5 1 .E 1835 96 (2002)2the operating parameters vary from instrument to instrument.Scale expansion may have to be used to obtain the requiredreadability.8.4.4 Ensure that the calibration solutions and the testsolut
32、ion(s) are within 1C of the same temperature.8.4.5 Aspirate water and zero the instrument.8.4.6 Aspirate the calibration solutions and the test solu-tion(s) and note the readings to determine the approximateconcentration of the test solution(s).8.4.7 Aspirate water until the initial reading is obtai
33、ned.Zero if necessary.8.4.8 Aspirate the calibration solutions and the test solu-tion(s) in the order of increasing instrument response, startingwith the calibration solution containing no analyte (S0). Whena stable response is obtained record the reading. Flush thesystem by aspirating water between
34、 each test and calibrationsolution.8.4.9 Repeat the measurement of the full set of calibrationand test solutions two more times and record the data.9. Preparation of Calibration Graphs9.1 Plot the average instrument reading against the concen-tration of the analyte in the calibration solutions for e
35、ach of themeasurements.NOTE 6Some instruments may be adjusted to give a readout inconcentration of the analyte. A graph of instrument response versusconcentration should be plotted to check the validity of the readings.9.2 Carry out measurements at least in triplicate.10. Calculation10.1 Determine t
36、he concentration of the analyte in the testsolution from the corresponding calibration graphs for each ofthe three sets of instrument readings recorded.10.2 Calculate the percentage of the analyte in the testsample using the formula:Analyte, % 5 cVF!/10 000 m (1)where:c = analyte concentration, mg/L
37、, found in the test solu-tion, less the blank;V = volume, mL, of the initial test solution;F = dilution factor for the secondary dilution; andm = mass, g, of the test portion.11. Report11.1 Report at least the following information:11.1.1 Designation of the test method used,11.1.2 Results of the ana
38、lysis,11.1.3 Number of independent replications,11.1.4 Any unusual features noted during the analysis, and11.1.5 Any operation not included in this test method ordescribed as optional.12. Determination of Aluminum12.1 Parameters:12.1.1 Wavelength:309.3 nm.12.1.2 Flame: nitrous oxideAcetylene.12.2 Re
39、agents:12.2.1 Potassium Chloride Ionization Buffer Solution (48g/L)Dissolve 48 g potassium chloride (KCl) in 500 mL ofwater, transfer to a 1-L volumetric flask, dilute to volume, andmix.12.2.2 Aluminum Stock Calibration Solution (1.000 g/L)Dissolve 1.000 g of aluminum (purity 99.9 % min) in 30 mL(1:
40、1) of HCl in the presence of 1 drop of mercury. Filter thesolution through a rapid filter paper. Wash the filter with 100mL of warm water. Add 85 mL of HCl to the filtrate, cool andtransfer to a 1-L volumetric flask, dilute to volume, and mix.Store in a polyethylene bottle.NOTE 7Warning: Mercury whi
41、ch acts a catalyst to help the dissolu-tion of high-purity aluminum is highly poisonous and has an appreciablevapor pressure. It must be stored in strong, tightly closed containers.Liquid mercury must be transferred in such a manner that a spill can becontained and thoroughly cleaned up at once. Dis
42、pose of mercury inaccordance with applicable regulations.12.2.3 Aluminum Calibration Solution (100 mg/L)Transfer a 100-mL aliquot of the aluminum stock standardsolution (12.2.2) into a 1-Lvolumetric flask.Add 90 mLof HCland 800 mL water. Cool, dilute to volume, and mix. Store in apolyethylene bottle
43、.12.3 Aluminum Calibration SolutionsTransfer to each ofsix 100-mL volumetric flasks 0, 5.0, 10, 15, 20, and 25 mL,respectively, of the aluminum calibration solution (12.2.3).Add 4 mLof the potassium chloride solution (12.2.1) and 4 mLof HNO3to each volumetric flask. Add 10.0, 9.5, 9.0, 8.5, 8.0,and
44、7.5 mL of HCl, respectively, to the six volumetric flasks.Cool, dilute to volume, and mix. The calibration solutions areidentified as S0through S5and contain 0, 5.0, 10.0, 15.0, and20.0 mg/L aluminum, respectively.NOTE 8It is important that all calibration solutions contain the sameconcentration (10
45、 % v/v) of HCl, including the 10 % HCl contained in thealuminum calibration solution (12.2.3).12.4 Sample Dissolution and Dilution:12.4.1 Transfer a 1-g sample to a 400-mL PTFE beaker andadd 15 mL of HCl and 5 mL of HNO3. Heat to initiate andmaintain the reaction until dissolution is complete. If an
46、y alloyresists dissolution, add HCl in 1-mL increments and continueto heat to dissolve sample.12.4.2 Dilute the solution to 50 mL with water and filterthrough 11-cm low-ash medium-porosity filter paper into a250-mL beaker. Wash the filter five times with 10-mL portionsof hot water. Add the washings
47、to the filtrate. Reserve the filterpaper containing any undissolved residue.12.4.3 Primary Dilutions for Samples Containing Less Than0.25 % AluminumEvaporate the filtrate reserved from 12.4.2to approximately 60 mL. Cool and transfer to a 100-mLvolumetric flask. Add 2.5 mL HCl, 4 mL HNO3, and 4 mLpot
48、assium chloride solution (12.2.1). Cool, dilute to volume,and mix.12.4.4 Primary Dilution for Samples Containing Over0.25 % AluminumEvaporate the filtrate reserved from 12.4.2to approximately 60 mL. Cool and transfer to a 100-mLvolumetric flask. Add 2.5 mL HCl, dilute to volume, and mix.12.4.5 Secon
49、dary Dilution for Samples Containing Between0.25 and 1.0 % AluminumTransfer 20 mL of the primaryE 1835 96 (2002)3dilution solution (12.4.4) into a 100-mL volumetric flask, andadd8mLofHCl,4mLofHNO3, and 4 mL of potassiumchloride solution (12.2.1). Cool, dilute to mark and mix. Thedilution factor F = 5.12.4.6 Secondary Dilution for Samples Containing Between1.0 and 2.0 % AluminumTransfer 10 mL of the primarydilution solution (12.4.4) into a 100-mL volumetric flask, andadd9mLofHCl,4mLofHNO3, and 4 mL of potassiumchloride solution (12.2.1). Cool, dilute
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