ASTM E1835-1996(2002)e1 Standard Test Method for Analysis of Nickel Alloys by Flame Atomic Absorption Spectrometry.pdf

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1、Designation: E 1835 96 (Reapproved 2002)1Standard 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 rev

2、ision, 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.1NOTEAdded research report footnotes and corrected warning notes throughout editorially in October 2008.1. Scop

3、e1.1 This test method covers analysis of nickel and nickel-base alloys by flame atomic absorption spectrometric 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 16Manganese 0.

4、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 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 thi

5、s standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For specific hazardsassociated with the use of this test method see Practices E50and the warning statements included in this test method.2. Referenced Documents2.

6、1 ASTM Standards:2E50 Practices for Apparatus, Reagents, and Safety Consid-erations for Chemical Analysis of Metals, Ores, andRelated MaterialsE 863 Practice for Describing Atomic Absorption Spectro-metric Equipment3E 882 Guide for Accountability and Quality Control in theChemical Analysis Laborator

7、yE 1452 Practice for Preparation of Calibration Solutions forSpectrophotometric and for Spectroscopic Atomic Analy-sis3E 1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analytical MethodE 1812 Practice for Optimization of Flame Atomic Absorp-tion Spectrometric

8、Equipment32.2 ISO Standards:4ISO Guide 5725 Accuracy, Trueness, and Precision of Mea-surements, Methods and ResultsISO 7530 Parts 2 through 9Flame Atomic AbsorptionSpectrometric Analysis3. Summary of Test Method3.1 The sample is dissolved in a mixture of hydrochloricacid and nitric acid. The solutio

9、n 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 calibrationsolutions.4. Significance and Use4.1 This test method is used for the analysis of nickel andnic

10、kel-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 common laboratoryprocedures skillfully and safely. It is expected that the workwill be pe

11、rformed 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 Studies (ILS)5, 6This test method wasevaluated by a subcommittee within ISO Technical Co

12、mmittee155 (ISO/TC 155/SC 4) on analysis of nickel alloys, in1This 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 editio

13、n approved May 10, 2002. Published May 2002. Originallyapproved in 1996. Last previous edition approved in 2002 as E 1835 - 96 (2002).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume info

14、rmation, refer to the standards Document Summary page onthe ASTM website.3Withdrawn.4Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.5Supporting data have been filed at ASTM International Headquarters and maybe obtained by

15、 requesting Research Report RR: E01-1018.6Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: E01-1019.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.accordance wit

16、h ISO Standard 5725. It was published as ISOStandard 7530, Parts 2 through 9. The ILS test data was notavailable for recalculation. The published ISO statistics aresummarized separately for each analyte.5. Apparatus5.1 Atomic Absorption Spectrometer, equipped with anappropriate background corrector,

17、 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 lamp for the analyte(s).5.3 For a general discussion of the instrumental require-ments o

18、f flame atomic absorption see Practice E 863.5.4 For a general discussion of apparatus requirements seePractices E50.6. Reagents6.1 Purity and Concentration of ReagentsThe purity andconcentration of common chemical reagents shall conform toPractices E50. The reagents should be free of or containmini

19、mal 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 Matrix Modifiers and Ionization BuffersMade up forthe individual analytes, where require

20、d, 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 shall not involve any steps orprocedures that can result in the loss of any analyte in thes

21、ample.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 onlyafter careful consideration of all elements to be determined on the meltedsample. In

22、duction 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 sample is necessary.7.4 The laboratory sample shall be cleaned by washing inpure acetone

23、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 several times with water followed by several washeswith acetone and air dried.8. General Proce

24、dure8.1 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 thedissolution is complete. If the sample contains over 0.5 %silicone, a few drops of HF will consid

25、erably speed up thedissolution. (WarningThis operation will emit corrosive,noxious, and toxic gases and should only be performed in afume hood. Proper personal safety equipment shall be wornand used.)8.1.2 If the sample resists dissolution, some adjustment ofthe acid mixture may be required.Add HCl

26、in 1-mLincrementsand continue heating to dissolve the sample.NOTE 2For some alloys a 30-mL HCl2-mL HNO3mixture is moreeffective. Pure nickel or nickel-copper alloys dissolve best in HNO3(1 + 1).NOTE 3The general method of dissolution can be modified asspecified in the appropriate sections.NOTE 4If s

27、ample inhomogeneity is suspected, a larger mass ofsample (10 g 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 processed in accordance with the procedure given.8.1.3 Using low heat, evaporate the solution ju

28、st to dryness.Do not bake. Cool to about 50 C and add 25 mL HCl andagain evaporate just to dryness. Add 25 mL HCl and repeat theevaporation.8.1.4 Cool to about 50 C, add 5 mL hydrochloric acid and20 mL water and heat to dissolve the salt.8.1.5 Proceed as directed in Sections 12-19.8.2 Reagent BlankC

29、arry 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:8.4.1 The wavelength of the spectral lines and the flametype to be used are listed in Sectio

30、ns 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 thermalTABLE 1 Nominal Composition of Test Samples, %Test Material Al Co Cr Cu Fe Mn Mo Nb Ni Si Ti V Zr825 0.2 0.07 21 1.6 30 0.7 .

31、 . 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 . 2 0.05 0.05NPK31 0.5

32、 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)12equilibrium is reached. The flame conditions 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.

33、 Optimum settings forthe 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 testsolution(s) are within 1 C of the same temperature.8.4.5 Aspirate water and zero the instrume

34、nt.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 obtained.Zero if necessary.8.4.8 Aspirate the calibration solutions and the test solu-tion(s

35、) 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 each test and calibrationsolution.8.4.9 Repeat the measurement of the full set of cali

36、brationand 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 each of themeasurements.NOTE 5Some instruments may be adjusted to give a readout inconce

37、ntration 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 the concentration of the analyte in the testsolution from the corresponding calibration

38、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, found in the test solu-tion, less the blank;V = volume, mL, of the initial test solut

39、ion;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 analysis,11.1.3 Number of independent replications,11.1.4 Any unusual features noted durin

40、g 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 Reagents:12.2.1 Potassium Chloride Ionization Buffer Solution (48g/L)Dissolve 48 g potas

41、sium 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 + 1) of HCl in the presence of 1 drop of mercury. Filter thesolution through a rapid f

42、ilter 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. (WarningMercury which actsa catalyst to help the dissolution of high-purity aluminum ishighly poisonous and h

43、as an appreciable vapor pressure. Itmust be stored in strong, tightly closed containers. Liquidmercury must be transferred in such a manner that a spill canbe contained and thoroughly cleaned up at once. Dispose ofmercury in accordance with applicable regulations.)12.2.3 Aluminum Calibration Solutio

44、n (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.12.3 Aluminum Calibration SolutionsTransfer to each ofsix 100-mL volumetric flasks (0, 5.0,

45、 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)and4mLof HNO3to each volumetric flask. Add (10.0, 9.5, 9.0, 8.5, 8.0,and 7.5) mL of HCl, respectively, to the six volumetric flasks.Cool, dilute to volume, and mix.

46、The calibration solutions areidentified as S0through S5and contain (0, 5.0, 10.0, 15.0, and20.0) mg/L aluminum, respectively.NOTE 6It is important that all calibration solutions contain the sameconcentration (10 % v/v) of HCl, including the 10 % HCl contained in thealuminum calibration solution (12.

47、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 any alloyresists dissolution, add HCl in 1-mL increments and continueto heat to dissolve sa

48、mple.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 to the filtrate. Reserve the filterpaper containing any undissolved residue.12.4.3 Primar

49、y 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 mLpotassium 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 12.4.2E 1835 96 (2002)13to approximately 60 mL. Cool and transfer to a 100-mLvolumetric flask. Add 2.5 mL HCl, dilute to volume, and mix.12.4.5 Secondary Dilution for Sampl