ASTM E1835-14(2022)
(Test Method)Standard Test Method for Analysis of Nickel Alloys by Flame Atomic Absorption Spectrometry
Standard Test Method for Analysis of Nickel Alloys by Flame Atomic Absorption Spectrometry
SIGNIFICANCE AND USE
5.1 This test method is used for the analysis of nickel alloy samples by FAAS to check compliance with compositional specifications. It is assumed that all who use the procedure will be trained analysts capable of performing common laboratory procedures skillfully and safely. It is expected that the work will be performed in a properly equipped laboratory and that proper waste disposal procedures will be followed. Appropriate quality control practices must be followed such as those described in Guide E882.
5.2 Interlaboratory Studies (ILS)5, 6—International interlaboratory studies were conducted by ISO/TC 155/SC4, Analysis of nickel alloys. Results were evaluated in accordance with ISO 5725:1986 and restated to conform to Practice E1601. The method was published as ISO 7530, Parts 1 through 9. The published ISO statistics are summarized separately for each analyte to correspond with Practice E1601.
5.3 In this test method, some matrix modifiers are specified. However, other additives have come into common use since the original publication of this test method. These may be equally or more effective but have not been tested. It is the responsibility of the user to validate the use of such additives or the use of different dilutions, or both.
SCOPE
1.1 This test method covers analysis of nickel alloys by flame atomic absorption spectrometry (FAAS) for the following elements:
Element
Compostiton Range, %
Aluminum
0.2 to 4.0
Chromium
0.01 to 4.0
Cobalt
0.01 to 4.0
Copper
0.01 to 4.0
Iron
0.1 to 4.0
Manganese
0.1 to 4.0
Silicon
0.2 to 1.0
Vanadium
0.05 to 1.0
1.2 The composition ranges of these elements 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 responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazards associated with the use of this test method, see Practices E50 and the warning statements included in this test method.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
Relations
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: E1835 − 14 (Reapproved 2022)
Standard Test Method for
Analysis of Nickel Alloys by Flame Atomic Absorption
Spectrometry
This standard is issued under the fixed designation E1835; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
1.1 This test method covers analysis of nickel alloys by 2.1 ASTM Standards:
flame atomic absorption spectrometry (FAAS) for the follow- D1193 Specification for Reagent Water
ing elements: E29 Practice for Using Significant Digits in Test Data to
Determine Conformance with Specifications
Compostiton Range,
Element %
E50 Practices for Apparatus, Reagents, and Safety Consid-
erations for Chemical Analysis of Metals, Ores, and
Aluminum 0.2 to 4.0
Related Materials
Chromium 0.01 to 4.0
Cobalt 0.01 to 4.0
E135 Terminology Relating to Analytical Chemistry for
Copper 0.01 to 4.0
Metals, Ores, and Related Materials
Iron 0.1 to 4.0
E882 Guide for Accountability and Quality Control in the
Manganese 0.1 to 4.0
Silicon 0.2 to 1.0
Chemical Analysis Laboratory
Vanadium 0.05 to 1.0
E1601 Practice for Conducting an Interlaboratory Study to
1.2 The composition ranges of these elements can be
Evaluate the Performance of an Analytical Method
expanded by the use of appropriate standards.
E1812 Practice for Optimization of Flame Atomic Absorp-
tion Spectrometric Equipment (Withdrawn 2004)
1.3 The values stated in SI units are to be regarded as
2.2 ISO Standards:
standard. No other units of measurement are included in this
ISO 5725:1986 Precision of Test Methods—Determination
standard.
of Repeatability and Reproducibility for a Standard Test
1.4 This standard does not purport to address all of the
Method by Inter-laboratory Tests
safety concerns, if any, associated with its use. It is the
ISO 7530 Parts 1 through 9—NickelAlloys—FlameAtomic
responsibility of the user of this standard to establish appro-
Absorption Spectrometric Analysis
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
3. Terminology
Forspecifichazardsassociatedwiththeuseofthistestmethod,
3.1 Definitions—For definitions of terms used in this test
see Practices E50 and the warning statements included in this
method, refer to Terminology E135.
test method.
1.5 This international standard was developed in accor-
4. Summary of Test Method
dance with internationally recognized principles on standard-
4.1 The sample is dissolved in a mixture of HCl and HNO .
ization established in the Decision on Principles for the
Thesolutionisaspiratedintoanappropriateflameofanatomic
Development of International Standards, Guides and Recom-
absorption spectrometer. The absorbance of the resonant line
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
This test method is under the jurisdiction of ASTM Committee E01 on Standards volume information, refer to the standard’s Document Summary page on
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct the ASTM website.
responsibility of Subcommittee E01.08 on Ni and Co and HighTemperatureAlloys. The last approved version of this historical standard is referenced on
Current edition approved Aug. 15, 2022. Published August 2022. Originally www.astm.org.
approved in 1996. Last previous edition approved in 2014 as E1835 – 14. DOI: Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
10.1520/E1835-14R22. 4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E1835 − 14 (2022)
TABLE 1 Nominal Compositions of Test Samples, %
Test Material Al Co Cr Cu Fe Mn Mo Nb Ni Si Ti V Zr
825 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 0.1 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 0.05
NPK31 0.5 14 20 . 1 . 4.5 5 Bal . 2 0.3 .
IN100 5.5 15 10 . <0.5 . 3 . Bal . 5 1 .
energy from the spectrum of the analyte is measured and such specifications are available. Other grades may be used,
compared with that of calibration solutions. provided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of
5. Significance and Use
the determination. The reagents should be free of or contain
minimal amounts (<0.1 µg⁄g) of the analyte of interest.
5.1 This test method is used for the analysis of nickel alloy
samples by FAAS to check compliance with compositional
7.2 Purity of Water—Unless otherwise indicated, references
specifications. It is assumed that all who use the procedure will
towatershallbeunderstoodtomeanreagentwaterconforming
be trained analysts capable of performing common laboratory
to Type I or II of Specification D1193. Type III or IV may be
procedures skillfully and safely. It is expected that the work
used if they effect no measurable change in the blank or
will be performed in a properly equipped laboratory and that
sample.
properwastedisposalprocedureswillbefollowed.Appropriate
7.3 Calibration Solutions—Prepared for the individual ana-
quality control practices must be followed such as those
lytes.
described in Guide E882.
7.4 Matrix Modifiers and Ionization Buffers—Prepared for
5, 6
5.2 Interlaboratory Studies (ILS) —International inter-
the individual analytes, where required.
laboratorystudieswereconductedbyISO/TC155/SC4,Analy-
sis of nickel alloys. Results were evaluated in accordance with
8. Sampling and Sample Preparation
ISO 5725:1986 and restated to conform to Practice E1601.The
8.1 Sampling and sample preparation shall be performed by
method was published as ISO 7530, Parts 1 through 9. The
normal procedures agreed upon between the parties, or, in the
published ISO statistics are summarized separately for each
event of a dispute, in accordance with the relevant standard if
analyte to correspond with Practice E1601.
one is available.
5.3 In this test method, some matrix modifiers are specified.
8.2 The sampling procedure shall not involve any steps or
However, other additives have come into common use since
procedures that can result in the loss of any analyte in the
the original publication of this test method. These may be
sample.
equally or more effective but have not been tested. It is the
responsibility of the user to validate the use of such additives
NOTE 1—Arc melting of the sample or induction melting of the sample
or the use of different dilutions, or both.
under vacuum can result in significant loss of several elements that have
a low vapor pressure.Arc melting of the sample should be performed only
after careful consideration of all elements to be determined on the melted
6. Apparatus
sample. Induction melting should be performed only in a complete or
6.1 Flame Atomic Absorption Spectrometer, equipped with
partial inert atmosphere.
an appropriate background corrector, a signal output device
8.3 The laboratory sample is normally in the form of
(such as a video display screen (VDS), a digital computer, a
turnings, millings, or drillings and no further mechanical
printer or strip chart recorder, and an optional autosampler.
preparation is necessary.
6.2 Radiation Source—Hollow cathode lamp or electrode-
8.4 If it is suspected that the laboratory sample is contami-
less discharge lamp for the analyte(s).
nated with oil or grease from the milling or drilling operation,
it shall be cleaned by washing it with high purity acetone, or
7. Reagents
other appropriate solvent, and dried in air.
7.1 Purity of Reagents—Reagent grade chemicals shall be
8.5 Ifbrazedalloytoolshavebeenusedinthepreparationof
used in all tests. Unless otherwise indicated, it is intended that
the sample, it shall be further cleaned by pickling in dilute
all reagents conform to the specifications of the Committee on
HNO for a few minutes. The sample shall then be washed
Analytical Reagents of the American Chemical Society where
5 7
Supporting data have been filed at ASTM International Headquarters and may Reagent Chemicals, American Chemical Society Specifications, American
be obtained by requesting Research Report : RR:E01-1018. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Supporting data have been filed at ASTM International Headquarters and may listed by the American Chemical Society, see the United States Pharmacopeia and
be obtained by requesting Research Report : RR:E01-1019. National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
E1835 − 14 (2022)
several times with water followed by several washes with high 9.4.8 Aspirate the calibration solutions and the test solu-
purity acetone, or other appropriate solvent, and dried in air. tion(s) in the order of increasing instrument response, starting
with the calibration solution containing no analyte (S ). When
9. General Procedure
a stable response is obtained record the reading. Flush the
system by aspirating water between each test and calibration
9.1 Sample Dissolution:
solution.
9.1.1 Transfer a 1.0-g sample, weighed to the nearest 1 mg,
9.4.9 Repeat the measurement of the full set of calibration
to a 600-mL beaker. Add 15 mL HCl and 5 mL HNO . Apply
and test solutions two more times and record the data.
sufficient heat to initiate and maintain the reaction until the
dissolution is complete. If the sample contains over 0.5 %
10. Preparation of Calibration Graphs
silicon, a few drops of HF will speed up the dissolution
10.1 For each calibration solution, calculate the average of
considerably. (Warning—This operation will emit corrosive,
the replicate absorbance measurements made in 9.4.9. Then,
noxious, and toxic gases and should only be performed in a
plottheaverageabsorbancevaluesversustheconcentrationsof
fume hood. Proper personal safety equipment shall be worn
the analyte in the calibration solutions.
and used.)
9.1.2 If the sample resists dissolution, some adjustment of
NOTE 5—Since the testing of these methods, there have been many
theacidmixturemayberequired.AddHClin1-mLincrements
advances in instrument technology for FAAS and the procedures for
calibration, making the manual plotting of calibration graphs redundant.
and continue heating to dissolve the sample.
10.2 Conduct measurements at least in triplicate.
NOTE 2—For some alloys a 30-mLHCl—2-mLHNO mixture is more
effective. Nickel alloys dissolve best in HNO (1 + 1).
NOTE 3—The general method of dissolution may be modified as 11. Calculation
specified in the appropriate sections.
11.1 Determine the concentration of the analyte in the test
NOTE4—Ifsampleinhomogeneityissuspected,alargermassofsample
solution from the corresponding calibration graphs for each of
(10 g to 50 g) may be taken for analysis. However, an aliquot portion
corresponding to 1-g sample shall be taken from the solution and
the three sets of instrument readings recorded.
processed in accordance with the procedure given.
11.2 Calculate the percentage of the analyte in the test
9.1.3 Using low heat, evaporate the solution just to dryness.
sample using the formula:
Do not bake. Cool to about 50 °C and add 25 mL HCl and
Analyte, % 5 ~cVF!/10000 m (1)
again evaporate just to dryness.Add 25 mLHCl and repeat the
evaporation.
where:
9.1.4 Cool to about 50 °C, add 5 mL HCl and 20 mL water
c = analyte concentration, mg/L, found in the test solution,
and heat to dissolve the salt.
less the blank;
9.1.5 Proceed as directed in Sections 12 through 19.
V = volume, mL, of the initial test solution;
F = dilution factor for the secondary dilution; and
9.2 Reagent Blank—Carry a reagent blank through the
m = mass, g, of the test portion.
entire procedure using the same amounts of all reagents with
the sample omitted.
11.3 Roundingoftestresultsobtainedusingthistestmethod
shall be performed in accordance with Practice E29, Rounding
9.3 Calibration Solutions—Proceed as directed in Sections
Method, unless an alternative rounding method is specified by
12 through 19.
the customer or applicable material specification.
9.4 Atomic Absorption Measurements:
9.4.1 The wavelengths of the spectral lines and the flame
12. Determination of Aluminum
types to be used are listed in Sections 12 through 19.
12.1 Parameters:
9.4.2 Set the required instrument parameters in accordance
12.1.1 Wavelength: 309.3 nm.
with the manufacturer’s recommendations or Practice E1812.
12.1.2 Flame: nitrous oxide—Acetylene.
Light the burner and aspirate water until thermal equilibrium is
reached. The flame conditions will vary according to the 12.2 Reagents:
element being determined. Zero the instrument. 12.2.1 Potassium Chloride Ionization Buffer Solution (48
9.4.3 Ensure that the instrument meets the performance g/L)—Dissolve 48 g potassium chloride (KCl) in 500 mL of
requirements given in Practice E1812. Optimum settings for water, transfer to a 1-L volumetric flask, dilute to volume, and
the operating parameters vary from instrument to instrument. mix.
Scale expansion may have to be used to obtain the required 12.2.2 Aluminum Stock Calibration Solution (1.00 g/L)—
readability. Dissolve 1.00 g of aluminum (purity 99.99 % min) in 30 mLof
9.4.4 Ensure that the calibration solutions and the test HCl (1 + 1). (Warning—If powdered aluminum is used, add
solution(s) are within 1 °C of the same temperature. the acid cautiously because powdered aluminum tends to be
9.4.5 Aspirate water and zero the instrument. very reactive). Place the beaker on a hot plate and heat the
9.4.6 Aspirate the calibration solutions and the test solu- solution to approximately 90 °C to start the reaction. Remove
tion(s) and note the readings to determine the approximate the beaker from the hotplate when the reaction starts and cover
concentration of the test solution(s). withawatchglass.PurealuminumdissolvesslowlyinHCland
9.4.7 Aspirate water until the initial reading is obtained. complete dissol
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