1、Designation: E1835 09E1835 14Standard Test Method forAnalysis of Nickel Alloys by Flame Atomic AbsorptionSpectrometry1This standard is issued under the fixed designation E1835; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the ye
2、ar 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 covers analysis of nickel alloys by flame atomic absorption spectrometric analysis spectrometry
3、 (FAAS)for the following elements:ElementConcentration Range,%ElementCompostiton 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 rangecomposition ranges of these elements
4、can be expanded by the use of appropriate standards.1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the respo
5、nsibilityof the user of 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 and thewarningstatements included in this test method.
6、2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterE29 Practice for Using Significant Digits in Test Data to Determine Conformance with SpecificationsE50 Practices forApparatus, Reagents, and Safety Considerations for ChemicalAnalysis of Metals, Ores, and Related Materia
7、lsE135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related MaterialsE882 Guide for Accountability and Quality Control in the Chemical Analysis LaboratoryE1601 Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical MethodE1601 Practice for
8、 Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical MethodE1812 Practice for Optimization of Flame Atomic Absorption Spectrometric Equipment (Withdrawn 2004)32.2 ISO Standards:4ISO 5725:1986 Precision of Test MethodsDetermination of Repeatability and Reproducibility for
9、 a Standard Test Method byInter-laboratory TestsISO 7530 Parts 1 through 9Nickel AlloysFlame Atomic Absorption Spectrometric Analysis1 This test method is under the jurisdiction of ASTM Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials and is the direct responsibility ofS
10、ubcommittee E01.08 on Ni and Co and High Temperature Alloys.Current edition approved Aug. 1, 2009Oct. 1, 2014. Published September 2009December 2014. Originally approved in 1996. Last previous edition approved in 20022009as E1835 96 (2002)E1835 09.1. DOI: 10.1520/E1835-09.10.1520/E1835-14.2 For refe
11、rencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 The last approved version of this historical standard is referenced o
12、n www.astm.org.4 Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http:/www.ansi.org.This 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 previ
13、ous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM Int
14、ernational, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13. Terminology3.1 DefinitionsFor definitions of terms used in this test method, refer to Terminology E135.4. Summary of Test Method4.1 The sample is dissolved in a mixture of HCl and HNO3. The solution is
15、 aspirated into an appropriate flame of an atomicabsorption spectrometer. The absorbance of the resonant line energy from the spectrum of the analyte is measured and comparedwith that of calibration solutions.5. Significance and Use5.1 This test method is used for the analysis of nickel alloy sample
16、s by FAAS to check compliance with compositionalspecifications. It is assumed that all who use the procedure will be trained analysts capable of performing common laboratoryprocedures skillfully and safely. It is expected that the work will be performed in a properly equipped laboratory and that pro
17、perwaste disposal procedures will be followed. Appropriate quality control practices must be followed such as those described inGuide E882.5.2 Interlaboratory Studies (ILS)5, 6International interlaboratory studies were conducted by ISO/TC 155/SC4, Analysis ofnickel alloys. Results were evaluated in
18、accordance with ISO 5725:1986 and restated to conform to Practice E1601. The methodwas published as ISO 7530, Parts 1 through 9. The published ISO statistics are summarized separately for each analyte tocorrespond with Practice E1601.5.3 In this test method, some matrix modifiers are specified. Howe
19、ver, other additives have come into common use since theoriginal publication of this test method. These may be equally or more effective but have not been tested. It is the responsibilityof the user to validate the use of such additives or the use of different dilutions, or both.6. Apparatus6.1 Flam
20、e Atomic Absorption Spectrometer, equipped with an appropriate background corrector, a signal output device (suchas a video display screen (VDS),(VDS), a digital computer, a printer or strip chart recorder, and an optional autosampler.6.2 Radiation SourceHollow cathode lamp or electrodeless discharg
21、e lamp for the analyte(s).7. Reagents7.1 Purity and Concentration of ReagentsThe purity and concentration of common chemical reagents and water shall conformto PracticesReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents conformto the E50.
22、 specifications of the Committee on Analytical Reagents of the American Chemical Society where such specificationsare available.7 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit itsuse without lessening the accuracy of the determin
23、ation. The reagents should be free of or contain minimal amounts (0.1 gg)of the analyte of interest.7.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean reagent water conforming toType I or II of Specification D1193. Type III or IV may be used if they effect
24、 no measurable change in the blank or sample.7.3 Calibration SolutionsPrepared for the individual analytes.7.4 Matrix Modifiers and Ionization BuffersPrepared for the individual analytes, where required.5 Supporting data have been filed at ASTM International Headquarters and may be obtained by reque
25、sting Research Report : RR:E01-1018.6 Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report : RR:E01-1019.7 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the te
26、sting of reagents not listed bythe American Chemical Society, see the United States Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.TABLE 1 Nominal CompositionCompositions of Test Samples, %Test Material Al Co Cr Cu Fe Mn Mo Nb Ni Si Ti V Zr825 0.2 0.07
27、 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 . 2 0.
28、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 .E1835 1428. Sampling and Sample Preparation8.1 Sampling and sample preparation shall be performed by normal procedures agreed upon between the parties, or, in the eventof a dispute, in accordance with the relevant
29、 standard if one is available.8.2 The sampling procedure shall not involve any steps or procedures that can result in the loss of any analyte in the sample.NOTE 1Arc melting of the sample or induction melting of the sample under vacuum can result in significant loss of several elements that have a l
30、owvapor pressure. Arc melting of the sample should be performed only after careful consideration of all elements to be determined on the melted sample.Induction melting should be performed only in a complete or partial inert atmosphere.8.3 The laboratory sample is normally in the form of turnings, m
31、illings, or drillings and no further mechanical preparation isnecessary.8.4 If it is suspected that the laboratory sample is contaminated with oil or grease from the milling or drilling operation, it shallbe cleaned by washing it with high purity acetone, or other appropriate solvent, and dried in a
32、ir.8.5 If brazed alloy tools have been used in the preparation of the sample, it shall be further cleaned by pickling in dilute HNO3for a few minutes. The sample shall then be washed several times with water followed by several washes with high purity acetone,or other appropriate solvent, and dried
33、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 beaker. Add 15 mL HCl and 5 mL HNO3. Applysufficient heat to initiate and maintain the reaction until the dissolution is complete. If the sample contains over 0.5 %silicone,silic
34、on, a few drops of HF will speed up the dissolution considerably. (WarningThis operation will emit corrosive,noxious, and toxic gases and should only be performed in a fume hood. Proper personal safety equipment shall be worn and used.)9.1.2 If the sample resists dissolution, some adjustment of the
35、acid mixture may be required. Add HCl in 1-mL increments andcontinue heating to dissolve the sample.NOTE 2For some alloys a 30-mL HCl2-mL HNO3 mixture is more effective. Nickel alloys dissolve best in HNO3 (1 + 1).NOTE 3The general method of dissolution may be modified as specified in the appropriat
36、e sections.NOTE 4If sample inhomogeneity is suspected, a larger mass of sample (10 g to 50 g) may be taken for analysis. However, an aliquot portioncorresponding to 1-g sample shall be taken from the solution and processed in accordance with the procedure given.9.1.3 Using low heat, evaporate the so
37、lution just to dryness. Do not bake. Cool to about 50 C and add 25 mL HCl and againevaporate just to dryness. Add 25 mL HCl and repeat the evaporation.9.1.4 Cool to about 50 C, add 5 mL HCl and 20 mL water and heat to dissolve the salt.9.1.5 Proceed as directed in Sections 12 1912 through 19.9.2 Rea
38、gent BlankCarry a reagent blank through the entire procedure using the same amounts of all reagents with the sampleomitted.9.3 Calibration SolutionsProceed as directed in Sections 12 1912 through 19.9.4 Atomic Absorption Measurements:9.4.1 The wavelengthwavelengths of the spectral lines and the flam
39、e typetypes to be used are listed in Sections 12 1912through 19.9.4.2 Set the required instrument parameters in accordance with the manufacturers recommendations or Practice E1812. Lightthe burner and aspirate water until thermal equilibrium is reached. The flame conditions will vary according to th
40、e element beingdetermined. Zero the instrument.9.4.3 Ensure that the instrument meets the performance requirements given in Practice E1812. Optimum settings for theoperating parameters vary from instrument to instrument. Scale expansion may have to be used to obtain the required readability.9.4.4 En
41、sure that the calibration solutions and the test solution(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 solution(s) and note the readings to determine the approximate concentrationof the test solution(s).9
42、.4.7 Aspirate water until the initial reading is obtained. Zero if necessary.9.4.8 Aspirate the calibration solutions and the test solution(s) in the order of increasing instrument response, starting with thecalibration solution containing no analyte (S0). When a stable response is obtained record t
43、he reading. Flush the system byaspirating water between each test and calibration solution.9.4.9 Repeat the measurement of the full set of calibration and test solutions two more times and record the data.10. Preparation of Calibration Graphs10.1 Plot the average instrument reading against the conce
44、ntration For each calibration solution, calculate the average of thereplicate absorbance measurements made in 9.4.9. Then, plot the average absorbance values versus the concentrations of theanalyte in the calibration solutions for each of the measurements.solutions.E1835 143NOTE 5Since the testing o
45、f these methods, there have been many advances in instrument technology for FAAS and the procedures for calibration,making the manual plotting of calibration graphs redundant.10.2 Conduct measurements at least in triplicate.11. Calculation11.1 Determine the concentration of the analyte in the test s
46、olution from the corresponding calibration graphs for each of thethree sets of instrument readings recorded.11.2 Calculate the percentage of the analyte in the test sample using the formula:Analyte,%5c V F!/10000 m (1)where:c = analyte concentration, mg/L, found in the test solution, less the blank;
47、V = volume, mL, of the initial test solution;F = dilution factor for the secondary dilution; andm = mass, g, of the test portion.11.3 Rounding of test results obtained using this test method shall be performed in accordance with Practice E29, RoundingMethod, unless an alternative rounding method is
48、specified by the customer or applicable material specification.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 (48 g/L)Dissolve 48 g potassium chloride (KCl) in 500 mL of
49、water,transfer to a 1-L volumetric flask, dilute to volume, and mix.12.2.2 Aluminum Stock Calibration Solution (1.000 g/L)(1.00 g/L)Dissolve 1.0001.00 g of aluminum (purity 99.9 % 99.99% min) in 30 mL HCl (1 + 1) in of HCl (1 + 1). (WarningIf powdered aluminum is used, add the acid cautiously becausepowdered aluminum tends to be very reactivethe presence of 1 drop of mercury. Filter the solution through a rapid filter paper.Wash the filter with 100 mL of warm water. ). Place the beaker on a hot plate and heat the solution to approximatel
