ASTM E1835-96(2002)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:E1835–96 (Reapproved 2002)
Standard Test Method for
Analysis of Nickel Alloys by Flame Atomic Absorption
Spectrometry
This standard is issued under the fixed designation E 1835; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope E 1452 Practice for Preparation of Calibration Solutions for
Spectrophotometric and for Spectroscopic Atomic Analy-
1.1 This test method covers analysis of nickel and nickel-
sis
base alloys by flame atomic absorption spectrometric analysis
E 1812 Practice for Optimization of FlameAtomicAbsorp-
for the following elements:
tion Spectrometric Equipment
Element Concentration Range, Section
2.2 ISO Standards:
%
ISO Guide 5725—Accuracy, Trueness, and Precision of
Aluminum 0.2 to 4.0 12
Measurements, Methods and Results
Chromium 0.01 to 4.0 13
ISO 7530 Parts 2 through 9—Flame Atomic Absorption
Cobalt 0.01 to 4.0 14
Copper 0.01 to 4.0 15
Spectrometric Analysis
Iron 0.1 to 4.0 16
Manga- 0.1 to 4.0 17
3. Summary of Test Method
nese
Silicon 0.2 to 1.0 18
3.1 The sample is dissolved in a mixture of hydrochloric
Vanadium 0.05 to 1.0 19
acid and nitric acid. The solution is aspirated into an appropri-
1.2 The concentration range of these elements can be ate flame of an atomic absorption spectrometer. Measurement
expanded by the use of appropriate standards.
of the absorbance of the resonant line energy from the
1.3 This standard does not purport to address all of the spectrum of the analyte is compared with that of calibration
safety concerns, if any, associated with its use. It is the
solutions.
responsibility of the user of this standard to establish appro-
4. Significance and Use
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.Forspecifichazards 4.1 This test method is used for the analysis of nickel and
associated with the use of this test method see Practices E 50 nickel-base alloy samples by flame atomic absorption spec-
and the warning statements included in this test method. trometry to check compliance with compositional specifica-
tions. It is assumed that all who use the procedure will be
2. Referenced Documents
trained analysts capable of performing common laboratory
2.1 ASTM Standards:
procedures skillfully and safely. It is expected that the work
E 50 Practices for Apparatus, Reagents, and Safety Precau- will be performed in a properly equipped laboratory and that
tions for Chemical Analysis of Metals, Ores, and Related
properwastedisposalprocedureswillbefollowed.Appropriate
Materials quality control practices must be followed such as those
E 863 Practice for Describing Flame Atomic Absorption
described in Guide E 882.
Spectroscopy Equipment 4.2 Interlaboratory Studies (ILS) —This test method was
E 882 Guide for Accountability and Quality Control in the
evaluated by a subcommittee within ISO Technical Committee
Chemical Analysis Laboratory 155 (ISO/TC 155/SC 4) on analysis of nickel alloys, in
accordance with ISO Standard 5725. It was published as ISO
Standard 7530, Parts 2 through 9. The ILS test data was not
This test method is under the jurisdiction of ASTM Committee E01 on
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
responsibilityofSubcommitteeE01.08onNiandCoandHigh-TemperatureAlloys.
Current edition approved Oct. 10, 1996. Published December 1996.
2 3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or AvailablefromAmericanNationalStandardsInstitute,25W.43rdSt.,4thFloor,
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM New York, NY 10036.
Standards volume information, refer to the standard’s Document Summary page on Supporting data are available fromASTM International Headquarters. Request
the ASTM website. RR:E01-1018.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E1835–96 (2002)
TABLE 1 Nominal Composition 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 .
available for recalculation. The published ISO statistics are washed several times with water followed by several washes
summarized separately for each analyte. with acetone and air dried.
5. Apparatus 8. General Procedure
5.1 Atomic Absorption Spectrometer, equipped with an 8.1 Sample Dissolution:
appropriate background corrector, a signal output device (such 8.1.1 Transfer a 1.0-g sample, weighed to the nearest 1 mg,
as a video display screen (VDS)), a digital computer, a printer to a 600-mL beaker. Add 15 mL HCl and 5 mL HNO . Apply
or strip chart recorder, and an optional autosampler. sufficient heat to initiate and maintain the reaction until the
5.2 Radiation Source—Hollow cathode lamp or electrode- dissolution is complete. If the sample contains over 0.5 %
less discharge lamp for the analyte(s). silicone, a few drops of HF will considerably speed up the
dissolution.
5.3 For a general discussion of the instrumental require-
ments of flame atomic absorption see Practice E 863.
NOTE 2—Warning: This operation will emit corrosive, noxious, and
5.4 For a general discussion of apparatus requirements see
toxic gases and should only be performed in a fume hood. Proper personal
Practices E 50.
safety equipment shall be worn and used.
8.1.2 If the sample resists dissolution, some adjustment of
6. Reagents
theacidmixturemayberequired.AddHClin1-mLincrements
6.1 Purity and Concentration of Reagents—The purity and
and continue heating to dissolve the sample.
concentration of common chemical reagents shall conform to
NOTE 3—For some alloys a 30-mLHCl—2-mLHNO mixture is more
Practices E 50. The reagents should be free of or contain
effective.Purenickelornickel-copperalloysdissolvebestinHNO (1+1).
minimal amounts (<0.1µ g/g) of the analyte of interest.
NOTE 4—The general method of dissolution can be modified as
6.2 Calibration Solutions—Made up for the individual ana-
specified in the appropriate sections.
lytes as described in Sections 12-19. They should be prepared
NOTE 5—If sample inhomogeneity is suspected, a larger mass of
to meet the guidelines of Practice E 1452.
sample (10 to 50 g) may be taken for analysis. In that case, however, an
6.3 Matrix Modifiers and Ionization Buffers—Made up for aliquot portion corresponding to 1-g sample shall be taken from the
solution and processed in accordance with the procedure given.
the individual analytes, where required, as described in Sec-
tions 12-19.
8.1.3 Using low heat, evaporate the solution just to dryness.
Donotbake.Cooltoabout50°Candadd25mLHClandagain
7. Sampling and Sample Preparation
evaporate just to dryness. Add 25 mL HCl and repeat the
7.1 Sampling and sample preparation is to be performed by
evaporation.
procedures agreed upon between the buyer and the seller.
8.1.4 Cool to about 50°C, add 5 mL hydrochloric acid and
7.2 The sampling procedure shall not involve any steps or
20 mL water and heat to dissolve the salt.
procedures that can result in the loss of any analyte in the
8.1.5 Proceed as directed in Sections 12-19.
sample.
8.2 Reagent Blank—Carry a reagent blank through the
entire procedure using the same amounts of all reagents with
NOTE 1—Arc melting of the sample or induction melting of the sample
the omitted sample.
under vacuum can result in significant loss of several elements that have
8.3 Calibration Solutions—Proceed as directed in Sections
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 12-19.
sample. Induction melting should be performed only in a complete or
8.4 Atomic Absorption Measurements:
partial inert atmosphere.
8.4.1 The wavelength of the spectral lines and the flame
7.3 The laboratory sample is normally in the form of type to be used are listed in Sections 12-19.
turnings, millings, or drillings and no further mechanical 8.4.2 Set the required instrument parameters in accordance
preparation of the sample is necessary. with the manufacturer’s recommendations and Practice
7.4 The laboratory sample shall be cleaned by washing in E 1812. Light the burner and aspirate water until thermal
pure acetone and then air dried. equilibrium is reached. The flame conditions will vary accord-
7.5 If brazed alloy tools are used in the preparation of the ing to the element being determined. Zero the instrument.
sample, the sample shall be further cleaned by pickling in 8.4.3 Ensure that the instrument meets the performance
dilute nitric acid for a few minutes. The sample shall then be requirements given in Practice E 1812. Optimum settings for
E1835–96 (2002)
the operating parameters vary from instrument to instrument. 12.2 Reagents:
Scale expansion may have to be used to obtain the required 12.2.1 Potassium Chloride Ionization Buffer Solution (48
readability. g/L)—Dissolve 48 g potassium chloride (KCl) in 500 mL of
8.4.4 Ensure that the calibration solutions and the test water, transfer to a 1-L volumetric flask, dilute to volume, and
solution(s) are within 1°C of the same temperature. mix.
8.4.5 Aspirate water and zero the instrument. 12.2.2 Aluminum Stock Calibration Solution (1.000 g/L)—
8.4.6 Aspirate the calibration solutions and the test solu- Dissolve 1.000 g of aluminum (purity 99.9 % min) in 30 mL
tion(s) and note the readings to determine the approximate (1:1) of HCl in the presence of 1 drop of mercury. Filter the
concentration of the test solution(s). solution through a rapid filter paper. Wash the filter with 100
8.4.7 Aspirate water until the initial reading is obtained. mL of warm water.Add 85 mL of HCl to the filtrate, cool and
Zero if necessary. transfer to a 1-L volumetric flask, dilute to volume, and mix.
8.4.8 Aspirate the calibration solutions and the test solu- Store in a polyethylene bottle.
tion(s) in the order of increasing instrument response, starting
NOTE 7—Warning: Mercury which acts a catalyst to help the dissolu-
with the calibration solution containing no analyte (S ). When
tion of high-purity aluminum is highly poisonous and has an appreciable
a stable response is obtained record the reading. Flush the
vapor pressure. It must be stored in strong, tightly closed containers.
system by aspirating water between each test and calibration
Liquid mercury must be transferred in such a manner that a spill can be
contained and thoroughly cleaned up at once. Dispose of mercury in
solution.
accordance with applicable regulations.
8.4.9 Repeat the measurement of the full set of calibration
and test solutions two more times and record the data.
12.2.3 Aluminum Calibration Solution (100 mg/L)—
Transfer a 100-mL aliquot of the aluminum stock standard
9. Preparation of Calibration Graphs
solution(12.2.2)intoa1-Lvolumetricflask.Add90mLofHCl
9.1 Plot the average instrument reading against the concen-
and 800 mL water. Cool, dilute to volume, and mix. Store in a
tration of the analyte in the calibration solutions for each of the polyethylene bottle.
measurements.
12.3 Aluminum Calibration Solutions—Transfer to each of
six 100-mL volumetric flasks 0, 5.0, 10, 15, 20, and 25 mL,
NOTE 6—Some instruments may be adjusted to give a readout in
respectively, of the aluminum calibration solution (12.2.3).
concentration of the analyte. A graph of instrument response versus
Add4mLofthepotassiumchloridesolution(12.2.1)and4mL
concentration should be plotted to check the validity of the readings.
of HNO to each volumetric flask.Add 10.0, 9.5, 9.0, 8.5, 8.0,
9.2 Carry out measurements at least in triplicate.
and 7.5 mL of HCl, respectively, to the six volumetric flasks.
Cool, dilute to volume, and mix. The calibration solutions are
10. Calculation
identified as S through S and contain 0, 5.0, 10.0, 15.0, and
0 5
10.1 Determine the concentration of the analyte in the test
20.0 mg/L aluminum, respectively.
solution from the corresponding calibration graphs for each of
NOTE 8—It is important that all calibration solutions contain the same
the three sets of instrument readings recorded.
concentration (10 % v/v) of HCl, including the 10 % HCl contained in the
10.2 Calculate the percentage of the analyte in the test
aluminum calibration solution (12.2.3).
sample using the formula:
12.4 Sample Dissolution and Dilution:
Analyte, % 5 cVF /10 000 m (1)
~ !
12.4.1 Transfer a 1-g sample to a 400-mLPTFE beaker and
where:
add 15 mL of HCl and 5 mL of HNO . Heat to initiate and
c = analyte concentration, mg/L, found in the test solu-
maintain the reaction until dissolution is complete. If any alloy
tion, less the blank;
resists dissolution, add HCl in 1-mL increments and continue
V = volume, mL, of the initial test solution;
to heat to dissolve sample.
F = dilution factor for the secondary dilution; and
12.4.2 Dilute the solution to 50 mL with water and filter
m = mass, g, of the test portion.
through 11-cm low-ash medium-porosity filter paper into a
250-mLbeaker. Wash the filter five times with 10-mLportions
11. Report
of hot water.Add the washings to the filtrate. Reserve the filter
11.1 Report at least the following information:
paper containing any undissolved residue.
11.1.1 Designation of the test method used,
12.4.3 Primary Dilutions for Samples Containing Less Than
11.1.2 Results of the analysis,
0.25 % Aluminum—Evaporate the filtrate reserved from 12.4.2
11.1.3 Number of independent replications,
to approximately 60 mL. Cool and transfer to a 100-mL
11.1.4 Any unusual features noted during the analysis, and
volumetric flask. Add 2.5 mL HCl, 4 mL HNO3, and 4 mL
11.1.5 Any operation not included in this test method or
potassium chloride solution (12.2.1). Cool, dilute to volume,
described as optional.
and mix.
12.4.4 Primary Dilution for Samples Containing Over
12. Determination of Aluminum
0.25 % Aluminum—Evaporate the filtrate reserved from 12.4.2
12.1 Parameters: to approximately 60 mL. Cool and transfer to a 100-mL
12.1.1 Wavelength: volumetric flask. Add 2.5 mL HCl, dilute to volume, and mix.
309.3 nm. 12.4.5 Secondary Dilution for Samples C
...