1、Designation: E 1835 09Standard 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 revision, the year of
2、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 covers analysis of nickel alloys byflame atomic absorption spectrometric analysis (FAAS) for thefollo
3、wing elements:ElementConcentration Range,%Aluminum 0.2 to 4.0Chromium 0.01 to 4.0Cobalt 0.01 to 4.0Copper 0.01 to 4.0Iron 0.1 to 4.0Manganese 0.1 to 4.0Silicon 0.2 to 1.0Vanadium 0.05 to 1.01.2 The concentration range of these elements can beexpanded by the use of appropriate standards.1.3 The value
4、s 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 appro-priate safe
5、ty 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 Documents2.1 ASTM Standards:2E50 Practices for Appa
6、ratus, Reagents, and Safety Consid-erations for Chemical Analysis of Metals, Ores, andRelated MaterialsE 135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE 882 Guide for Accountability and Quality Control in theChemical Analysis LaboratoryE 1601 Practice for Con
7、ducting an Interlaboratory Study toEvaluate the Performance of an Analytical MethodE 1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analytical MethodE 1812 Practice for Optimization of Flame Atomic Absorp-tion Spectrometric Equipment32.2 ISO Standards:4ISO 572
8、5:1986 Precision of Test MethodsDeterminationof Repeatability and Reproducibility for a Standard TestMethod by Inter-laboratory TestsISO 7530 Parts 1 through 9Nickel AlloysFlameAtomic Absorption Spectrometric Analysis3. Terminology3.1 DefinitionsFor definitions of terms used in this testmethod, refe
9、r to Terminology E 135.4. Summary of Test Method4.1 The sample is dissolved in a mixture of HCl and HNO3.The solution is aspirated into an appropriate flame of an atomicabsorption spectrometer. The absorbance of the resonant lineenergy from the spectrum of the analyte is measured andcompared with th
10、at of calibration solutions.5. Significance and Use5.1 This test method is used for the analysis of nickel alloysamples by FAAS to check compliance with compositionalspecifications. It is assumed that all who use the procedure willbe trained analysts capable of performing common laboratoryprocedures
11、 skillfully and safely. It is expected that the workwill be performed in a properly equipped laboratory and thatproper waste disposal procedures will be followed.Appropriate1This test method is under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores, and Related Material
12、s and is the directresponsibility of Subcommittee E01.08 on Ni and Co and High Temperature Alloys.Current edition approved Aug. 1, 2009. Published September 2009. Originallyapproved in 1996. Last previous edition approved in 2002 as E 1835 96 (2002)1.2For referenced ASTM standards, visit the ASTM we
13、bsite, 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.3Withdrawn. The last approved version of this historical standard is referencedon www.astm.org.4Available from
14、 American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.quality control practices must be followed such as thosedescribed in Guid
15、e E 882.5.2 Interlaboratory Studies (ILS)5, 6International inter-laboratory studies were conducted by ISO/TC 155/SC4,Analy-sis of nickel alloys. Results were evaluated in accordance withISO 5725:1986 and restated to conform to Practice E 1601.The method was published as ISO 7530, Parts 1 through 9.
16、Thepublished ISO statistics are summarized separately for eachanalyte to correspond with Practice E 1601.5.3 In this test method, some matrix modifiers are specified.However, other additives have come into common use sincethe original publication of this test method. These may beequally or more effe
17、ctive but have not been tested. It is theresponsibility of the user to validate the use of such additivesor the use of different dilutions, or both.6. Apparatus6.1 Flame Atomic Absorption Spectrometer, equipped withan appropriate background corrector, a signal output device(such as a video display s
18、creen (VDS), a digital computer, aprinter or strip chart recorder, and an optional autosampler.6.2 Radiation SourceHollow cathode lamp or electrode-less discharge lamp for the analyte(s).7. Reagents7.1 Purity and Concentration of ReagentsThe purity andconcentration of common chemical reagents and wa
19、ter shallconform to Practices E50. The reagents should be free of orcontain minimal amounts (0.1 g/g) of the analyte of interest.7.2 Calibration SolutionsPrepared for the individual ana-lytes.7.3 Matrix Modifiers and Ionization BuffersPrepared forthe individual analytes, where required.8. Sampling a
20、nd Sample Preparation8.1 Sampling and sample preparation shall be performed bynormal procedures agreed upon between the parties, or, in theevent of a dispute, in accordance with the relevant standard ifone is available.8.2 The sampling procedure shall not involve any steps orprocedures that can resu
21、lt 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 onlyafter careful consideration of all elements to
22、be determined on the meltedsample. Induction melting should be performed only in a complete orpartial inert atmosphere.8.3 The laboratory sample is normally in the form ofturnings, millings, or drillings and no further mechanicalpreparation is necessary.8.4 If it is suspected that the laboratory sam
23、ple is contami-nated with oil or grease from the milling or drilling operation,it shall be cleaned by washing it with high purity acetone, orother appropriate solvent, and dried in air.8.5 If brazed alloy tools have been used in the preparation ofthe sample, it shall be further cleaned by pickling i
24、n diluteHNO3for a few minutes. The sample shall then be washedseveral times with water followed by several washes with highpurity acetone, or other appropriate solvent, and dried in air.9. General Procedure9.1 Sample Dissolution:9.1.1 Transfer a 1.0-g sample, weighed to the nearest 1 mg,to a 600-mL
25、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 speed up the dissolutionconsiderably. (WarningThis operation will emit corrosive,noxious, and toxic gase
26、s and should only be performed in afume hood. Proper personal safety equipment shall be wornand used.)9.1.2 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 2For some alloys a 30-mL HCl2-mL
27、 HNO3mixture is moreeffective. Nickel alloys dissolve best in HNO3(1 + 1).NOTE 3The general method of dissolution may be modified asspecified in the appropriate sections.NOTE 4If sample inhomogeneity is suspected, a larger mass ofsample (10 g to 50 g) may be taken for analysis. However, an aliquotpo
28、rtion corresponding to 1-g sample shall be taken from the solution andprocessed in accordance with the procedure given.9.1.3 Using low heat, evaporate the solution just 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 theevapor
29、ation.9.1.4 Cool to about 50 C, add 5 mL HCl and 20 mL waterand heat to dissolve the salt.9.1.5 Proceed as directed in Sections 12-19.5Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: E01-1018.6Supporting data have been filed at
30、ASTM International Headquarters and maybe obtained by requesting Research Report RR: E01-1019.TABLE 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 . . 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
31、.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 14 20 . 1 . 4.5 5 Bal . 2 0.3 .IN100 5.5 15 10 . 0.5 . 3 . Bal . 5 1 .E18350929.
32、2 Reagent BlankCarry a reagent blank through theentire procedure using the same amounts of all reagents withthe sample omitted.9.3 Calibration SolutionsProceed as directed in Sections12-19.9.4 Atomic Absorption Measurements:9.4.1 The wavelength of the spectral lines and the flametype to be used are
33、listed in Sections 12-19.9.4.2 Set the required instrument parameters in accordancewith the manufacturers recommendations or Practice E 1812.Light the burner and aspirate water until thermal equilibrium isreached. The flame conditions will vary according to theelement being determined. Zero the inst
34、rument.9.4.3 Ensure that the instrument meets the performancerequirements given in Practice E 1812. Optimum settings forthe operating parameters vary from instrument to instrument.Scale expansion may have to be used to obtain the requiredreadability.9.4.4 Ensure that the calibration solutions and th
35、e testsolution(s) are within 1 C of the same temperature.9.4.5 Aspirate water and zero the instrument.9.4.6 Aspirate the calibration solutions and the test solu-tion(s) and note the readings to determine the approximateconcentration of the test solution(s).9.4.7 Aspirate water until the initial read
36、ing is obtained.Zero if necessary.9.4.8 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 w
37、ater between each test and calibrationsolution.9.4.9 Repeat the measurement of the full set of calibrationand test solutions two more times and record the data.10. Preparation of Calibration Graphs10.1 Plot the average instrument reading against the con-centration of the analyte in the calibration s
38、olutions for each ofthe measurements.NOTE 5Since the testing of these methods, there have been manyadvances in instrument technology for FAAS and the procedures forcalibration, making the plotting of calibration graphs redundant.10.2 Conduct measurements at least in triplicate.11. Calculation11.1 De
39、termine the concentration of the analyte in the testsolution from the corresponding calibration graphs for each ofthe three sets of instrument readings recorded.11.2 Calculate the percentage of the analyte in the testsample using the formula:Analyte, % 5 cVF!/10 000 m (1)where:c = analyte concentrat
40、ion, mg/L, 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.12. Determination of Aluminum12.1 Parameters:12.1.1 Wavelength: 309.3 nm.12.1.2 Flame: nitrous oxideAcetylene.12.2 R
41、eagents: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 mLHC
42、l (1 + 1) 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. (WarningMercury which act
43、sa catalyst to help the dissolution of high-purity aluminum ishighly poisonous and has 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 ofme
44、rcury in accordance 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.12.3 Al
45、uminum Calibration SolutionsTransfer to each ofsix 100-mL volumetric flasks (0, 5.0, 10.0, 15.0, 20.0, and25.0) mL, respectively, of the aluminum calibration solution(12.2.3). Add 4 mL of the KCl solution and 4 mL of HNO3toeach volumetric flask.Add (10.0, 9.5, 9.0, 8.5, 8.0, and 7.5) mLof HCl, respe
46、ctively, to the six volumetric flasks. Cool, diluteto volume, and mix. The calibration solutions are identified asS0through S5and contain (0, 5.0, 10.0, 15.0, 20.0, and 25.0)mg/L Al, respectively.NOTE 6It is important that all calibration solutions contain the sameconcentration (10 % v/v) of HCl, in
47、cluding 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, weighed to the nearest 1 mg,to a 400-mL PTFE beaker and add 15 mL of HCl and 5 mL ofHNO3. Heat to initiate and maintain the reaction until disso-lution is co
48、mplete. If any alloy resists dissolution, add HCl in1-mL increments and continue to 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
49、 the washings 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 toapproximately 60 mL. Cool and transfer to a 100-mL volumet-ric flask. Add 2.5 mL HCl, 4 mL HNO3, and 4 mL KClsolution. Cool, dilute to volume, and mix.12.4.4 Primary Dilution for Samples Containing Over0.25 % AluminumEvaporate the filtrate reserved from toE1835093approximately 60 mL. Cool and transfer to a 100-mL volumet-ric flask. Add 2.5 mL HCl, di
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