ASTM E1835-96

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
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Designation: E 1835 – 96
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 ISO Guide 5725—Accuracy, Trueness, and Precision of
Measurements, Methods and Results
1.1 This test method covers analysis of nickel and nickel-
ISO 7530 Parts 2 through 9—Flame Atomic Absorption
base alloys by flame atomic absorption spectrometric analysis
Spectrometric Analysis
for the following elements:
Element Concentration Range, Section
3. Summary of Test Method
%
3.1 The sample is dissolved in a mixture of hydrochloric
Aluminum 0.2 to 4.0 12
acid and nitric acid. The solution is aspirated into an appropri-
Chromium 0.01 to 4.0 13
ate flame of an atomic absorption spectrometer. Measurement
Cobalt 0.01 to 4.0 14
Copper 0.01 to 4.0 15
of the absorbance of the resonant line energy from the
Iron 0.1 to 4.0 16
spectrum of the analyte is compared with that of calibration
Manga- 0.1 to 4.0 17
solutions.
nese
Silicon 0.2 to 1.0 18
Vanadium 0.05 to 1.0 19
4. Significance and Use
1.2 The concentration range of these elements can be 4.1 This test method is used for the analysis of nickel and
expanded by the use of appropriate standards. nickel-base alloy samples by flame atomic absorption spec-
1.3 This standard does not purport to address all of the trometry to check compliance with compositional specifica-
safety concerns, if any, associated with its use. It is the tions. It is assumed that all who use the procedure will be
responsibility of the user of this standard to establish appro- trained analysts capable of performing common laboratory
priate safety and health practices and determine the applica- procedures skillfully and safely. It is expected that the work
bility of regulatory limitations prior to use. For specific hazards will be performed in a properly equipped laboratory and that
associated with the use of this test method see Practices E 50 proper waste disposal procedures will be followed. Appropriate
and the warning statements included in this test method. quality control practices must be followed such as those
described in Guide E 882.
2. Referenced Documents 5
4.2 Interlaboratory Studies (ILS) —This test method was
2.1 ASTM Standards: evaluated by a subcommittee within ISO Technical Committee
E 50 Practices for Apparatus, Reagents, and Safety Precau-
155 (ISO/TC 155/SC 4) on analysis of nickel alloys, in
tions for Chemical Analysis of Metals
accordance with ISO Standard 5725. It was published as ISO
E 863 Practice for Describing Flame Atomic Absorption Standard 7530, Parts 2 through 9. The ILS test data was not
Spectroscopy Equipment
available for recalculation. The published ISO statistics are
E 882 Guide for Accountability and Quality Control in the summarized separately for each analyte.
Chemical Analysis Laboratory
5. Apparatus
E 1452 Practice for Preparation of Calibration Solutions for
Spectrophotometric and for Spectroscopic Atomic Analy- 5.1 Atomic Absorption Spectrometer, equipped with an
sis appropriate background corrector, a signal output device (such
E 1812 Practice for Optimization of Flame Atomic Absorp- as a video display screen (VDS)), a digital computer, a printer
tion Spectrophotometric Equipment or strip chart recorder, and an optional autosampler.
2.2 ISO Standards: 5.2 Radiation Source—Hollow cathode lamp or electrode-
less discharge lamp for the analyte(s).
This test method is under the jurisdiction of ASTM Committee E-1 on
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
responsibility of Subcommittee E01.08 on Ni and Co and High-Temperature Alloys. Available from American National Standards Institute, 11 W. 42nd St., 13th
Current edition approved Oct. 10, 1996. Published December 1996. Floor, New York, NY 10036.
2 5
Annual Book of ASTM Standards, Vol 03.05. Supporting data are available from ASTM Headquarters. Request RR:E01-
Annual Book of ASTM Standards, Vol 03.06. 1018.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
E 1835
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 .
NOTE 2—Warning: This operation will emit corrosive, noxious, and
5.3 For a general discussion of the instrumental require-
toxic gases and should only be performed in a fume hood. Proper personal
ments of flame atomic absorption see Practice E 863.
safety equipment shall be worn and used.
5.4 For a general discussion of apparatus requirements see
Practices E 50.
8.1.2 If the sample resists dissolution, some adjustment of
the acid mixture may be required. Add HCl in 1-mL increments
6. Reagents
and continue heating to dissolve the sample.
6.1 Purity and Concentration of Reagents—The purity and
NOTE 3—For some alloys a 30-mL HCl—2-mL HNO mixture is more
concentration of common chemical reagents shall conform to
effective. Pure nickel or nickel-copper alloys dissolve best in HNO (1+1).
Practices E 50. The reagents should be free of or contain
NOTE 4—The general method of dissolution can be modified as
minimal amounts (<0.1μ g/g) of the analyte of interest.
specified in the appropriate sections.
6.2 Calibration Solutions—Made up for the individual ana-
NOTE 5—If sample inhomogeneity is suspected, a larger mass of
lytes as described in Sections 12-19. They should be prepared
sample (10 to 50 g) may be taken for analysis. In that case, however, an
to meet the guidelines of Practice E 1452.
aliquot portion corresponding to 1-g sample shall be taken from the
solution and processed in accordance with the procedure given.
6.3 Matrix Modifiers and Ionization Buffers—Made up for
the individual analytes, where required, as described in Sec-
8.1.3 Using low heat, evaporate the solution just to dryness.
tions 12-19.
Do not bake. Cool to about 50°C and add 25 mL HCl and again
evaporate just to dryness. Add 25 mL HCl and repeat the
7. Sampling and Sample Preparation
evaporation.
7.1 Sampling and sample preparation is to be performed by
8.1.4 Cool to about 50°C, add 5 mL hydrochloric acid and
procedures agreed upon between the buyer and the seller.
20 mL water and heat to dissolve the salt.
7.2 The sampling procedure shall not involve any steps or
8.1.5 Proceed as directed in Sections 12-19.
procedures that can result in the loss of any analyte in the
8.2 Reagent Blank—Carry a reagent blank through the
sample.
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
12-19.
after careful consideration of all elements to be determined on the melted
8.4 Atomic Absorption Measurements:
sample. Induction melting should be performed only in a complete or
8.4.1 The wavelength of the spectral lines and the flame
partial inert atmosphere.
type to be used are listed in Sections 12-19.
7.3 The laboratory sample is normally in the form of
8.4.2 Set the required instrument parameters in accordance
turnings, millings, or drillings and no further mechanical
with the manufacturer’s recommendations and Practice
preparation of the sample is necessary.
E 1812. Light the burner and aspirate water until thermal
7.4 The laboratory sample shall be cleaned by washing in
equilibrium is reached. The flame conditions will vary accord-
pure acetone and then air dried.
ing to the element being determined. Zero the instrument.
7.5 If brazed alloy tools are used in the preparation of the
8.4.3 Ensure that the instrument meets the performance
sample, the sample shall be further cleaned by pickling in
requirements given in Practice E 1812. Optimum settings for
dilute nitric acid for a few minutes. The sample shall then be
the operating parameters vary from instrument to instrument.
washed several times with water followed by several washes
Scale expansion may have to be used to obtain the required
with acetone and air dried.
readability.
8. General Procedure
8.4.4 Ensure that the calibration solutions and the test
solution(s) are within 1°C of the same temperature.
8.1 Sample Dissolution:
8.4.5 Aspirate water and zero the instrument.
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 HNO . Apply 8.4.6 Aspirate the calibration solutions and the test solu-
tion(s) and note the readings to determine the approximate
sufficient heat to initiate and maintain the reaction until the
dissolution is complete. If the sample contains over 0.5 % concentration of the test solution(s).
silicone, a few drops of HF will considerably speed up the 8.4.7 Aspirate water until the initial reading is obtained.
dissolution. Zero if necessary.
E 1835
NOTE 7—Warning: Mercury which acts a catalyst to help the dissolu-
8.4.8 Aspirate the calibration solutions and the test solu-
tion of high-purity aluminum is highly poisonous and has an appreciable
tion(s) in the order of increasing instrument response, starting
vapor pressure. It must be stored in strong, tightly closed containers.
with the calibration solution containing no analyte (S ). When
Liquid mercury must be transferred in such a manner that a spill can be
a stable response is obtained record the reading. Flush the
contained and thoroughly cleaned up at once. Dispose of mercury in
system by aspirating water between each test and calibration
accordance with applicable regulations.
solution.
12.2.3 Aluminum Calibration Solution (100 mg/L)—
8.4.9 Repeat the measurement of the full set of calibration
Transfer a 100-mL aliquot of the aluminum stock standard
and test solutions two more times and record the data.
solution (12.2.2) into a 1-L volumetric flask. Add 90 mL of HCl
and 800 mL water. Cool, dilute to volume, and mix. Store in a
9. Preparation of Calibration Graphs
polyethylene bottle.
9.1 Plot the average instrument reading against the concen-
12.3 Aluminum Calibration Solutions—Transfer to each of
tration of the analyte in the calibration solutions for each of the
six 100-mL volumetric flasks 0, 5.0, 10, 15, 20, and 25 mL,
measurements.
respectively, of the aluminum calibration solution (12.2.3).
NOTE 6—Some instruments may be adjusted to give a readout in
Add 4 mL of the potassium chloride solution (12.2.1) and 4 mL
concentration of the analyte. A graph of instrument response versus
of HNO to each volumetric flask. Add 10.0, 9.5, 9.0, 8.5, 8.0,
concentration should be plotted to check the validity of the readings.
and 7.5 mL of HCl, respectively, to the six volumetric flasks.
9.2 Carry out measurements at least in triplicate. Cool, dilute to volume, and mix. The calibration solutions are
identified as S through S and contain 0, 5.0, 10.0, 15.0, and
0 5
10. Calculation
20.0 mg/L aluminum, respectively.
10.1 Determine the concentration of the analyte in the test
NOTE 8—It is important that all calibration solutions contain the same
solution from the corresponding calibration graphs for each of
concentration (10 % v/v) of HCl, including the 10 % HCl contained in the
the three sets of instrument readings recorded.
aluminum calibration solution (12.2.3).
10.2 Calculate the percentage of the analyte in the test
12.4 Sample Dissolution and Dilution:
sample using the formula:
12.4.1 Transfer a 1-g sample to a 400-mL PTFE beaker and
Analyte, % 5 ~cVF!/10 000 m (1)
add 15 mL of HCl and 5 mL of HNO . Heat to initiate and
maintain the reaction until dissolution is complete. If any alloy
where:
resists dissolution, add HCl in 1-mL increments and continue
c 5 analyte concentration, mg/L, found in the test solu-
to heat to dissolve sample.
tion, less the blank;
12.4.2 Dilute the solution to 50 mL with water and filter
V 5 volume, mL, of the initial test solution;
through 11-cm low-ash medium-porosity filter paper into a
F 5 dilution factor for the secondary dilution; and
250-mL beaker. Wash the filter five times with 10-mL portions
m 5 mass, g, of the test portion.
of hot water. Add the washings to the filtrate. Reserve the filter
11. Report
paper containing any undissolved residue.
12.4.3 Primary Dilutions for Samples Containing Less Than
11.1 Report at least the following information:
0.25 % Aluminum—Evaporate the filtrate reserved from 12.4.2
11.1.1 Designation of the test method used,
to approximately 60 mL. Cool and transfer to a 100-mL
11.1.2 Results of the analysis,
volumetric flask. Add 2.5 mL HCl, 4 mL HNO3, and 4 mL
11.1.3 Number of independent replications,
potassium chloride solution (12.2.1). Cool, dilute to volume,
11.1.4 Any unusual features noted during the analysis, and
and mix.
11.1.5 Any operation not included in this test method or
12.4.4 Primary Dilution for Samples Containing Over
described as optional.
0.25 % Aluminum—Evaporate the filtrate reserved from 12.4.2
12. Determination of Aluminum
to approximately 60 mL. Cool and transfer to a 100-mL
12.1 Parameters: volumetric flask. Add 2.5 mL HCl, dilute to volume, and mix.
12.1.1 Wavelength: 12.4.5 Secondary Dilution for Samples Containing Between
309.3 nm. 0.25 and 1.0 % Aluminum—Transfer 20 mL of the primary
12.1.2 Flame: nitrous oxide—Acetylene. dilution solution (12.4.4) into a 100-mL volumetric flask, and
12.2 Reagents: add8mL ofHCl,4mL ofHNO , and 4 mL of potassium
12.2.1 Potassium Chloride Ionization Buffer Solution (48 chloride solution (12.2.1). Cool, dilute to mark and mix. The
g/L)—Dissolve 48 g potassium chloride (KCl) in 500 mL of dilution factor F 5 5.
water, transfer to a 1-L volumetric flask, dilute to volume, and 12.4.6 Secondary Dilution for Samples Containing Between
mix. 1.0 and 2.0 % Aluminum—Transfer 10 mL of the primary
12.2.2 Aluminum Stock Calibration Solution (1.000 g/L)— dilution solution (12.4.4) into a 100-mL volumetric flask, and
Diss
...