ASTM E1835-96(2002)e1

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:E1835–96(Reapproved2002)
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 (´) indicates an editorial change since the last revision or reapproval.
´ NOTE—Added research report footnotes and corrected warning notes throughout editorially in October 2008.
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 1601 Practice for Conducting an Interlaboratory Study to
for the following elements:
Evaluate the Performance of an Analytical Method
Element Concentration Range, Section
E 1812 Practice for Optimization of FlameAtomicAbsorp-
%
tion Spectrometric Equipment
Aluminum 0.2 to 4.0 12
2.2 ISO Standards:
Chromium 0.01 to 4.0 13
ISO Guide 5725 Accuracy,Trueness, and Precision of Mea-
Cobalt 0.01 to 4.0 14
Copper 0.01 to 4.0 15
surements, Methods and Results
Iron 0.1 to 4.0 16
ISO 7530 Parts 2 through 9—Flame Atomic Absorption
Manganese 0.1 to 4.0 17
Spectrometric Analysis
Silicon 0.2 to 1.0 18
Vanadium 0.05 to 1.0 19
3. Summary of Test Method
1.2 The concentration range of these elements can be
3.1 The sample is dissolved in a mixture of hydrochloric
expanded by the use of appropriate standards.
acid and nitric acid. The solution is aspirated into an appropri-
1.3 This standard does not purport to address all of the
ate flame of an atomic absorption spectrometer. Measurement
safety concerns, if any, associated with its use. It is the
of the absorbance of the resonant line energy from the
responsibility of the user of this standard to establish appro-
spectrum of the analyte is compared with that of calibration
priate safety and health practices and determine the applica-
solutions.
bilityofregulatorylimitationspriortouse.Forspecifichazards
associated with the use of this test method see PracticesE50
4. Significance and Use
and the warning statements included in this test method.
4.1 This test method is used for the analysis of nickel and
2. Referenced Documents
nickel-base alloy samples by flame atomic absorption spec-
trometry to check compliance with compositional specifica-
2.1 ASTM Standards:
tions. It is assumed that all who use the procedure will be
E50 Practices forApparatus, Reagents, and Safety Consid-
trained analysts capable of performing common laboratory
erations for Chemical Analysis of Metals, Ores, and
procedures skillfully and safely. It is expected that the work
Related Materials
will be performed in a properly equipped laboratory and that
E 863 Practice for Describing Atomic Absorption Spectro-
properwastedisposalprocedureswillbefollowed.Appropriate
metric Equipment
quality control practices must be followed such as those
E 882 Guide for Accountability and Quality Control in the
described in Guide E 882.
Chemical Analysis Laboratory
5, 6
4.2 Interlaboratory Studies (ILS) —This test method was
evaluated by a subcommittee within ISO Technical Committee
This test method is under the jurisdiction of ASTM Committee E01 on
155 (ISO/TC 155/SC 4) on analysis of nickel alloys, in
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
responsibility of Subcommittee E01.08 on Ni and Co and HighTemperatureAlloys.
Current edition approved May 10, 2002. Published May 2002. Originally
approved in 1996. Last previous edition approved in 2002 as E 1835 - 96 (2002). Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 4th Floor, New York, NY 10036, http://www.ansi.org.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Supporting data have been filed at ASTM International Headquarters and may
Standards volume information, refer to the standard’s Document Summary page on be obtained by requesting Research Report RR: E01-1018.
the ASTM website. Supporting data have been filed at ASTM International Headquarters and may
Withdrawn. be obtained by requesting Research Report RR: E01-1019.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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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 .
accordance with ISO Standard 5725. It was published as ISO 7.5 If brazed alloy tools are used in the preparation of the
Standard 7530, Parts 2 through 9. The ILS test data was not sample, the sample shall be further cleaned by pickling in
available for recalculation. The published ISO statistics are dilute nitric acid for a few minutes. The sample shall then be
summarized separately for each analyte. washed several times with water followed by several washes
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
as a video display screen (VDS)), a digital computer, a printer 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
or strip chart recorder, and an optional autosampler.
5.2 Radiation Source—Hollow cathode lamp or electrode- sufficient heat to initiate and maintain the reaction until the
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
5.3 For a general discussion of the instrumental require-
dissolution. (Warning—This operation will emit corrosive,
ments of flame atomic absorption see Practice E 863.
noxious, and toxic gases and should only be performed in a
5.4 For a general discussion of apparatus requirements see
fume hood. Proper personal safety equipment shall be worn
PracticesE50.
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
Practices E50. The reagents should be free of or contain
NOTE 2—For some alloys a 30-mLHCl—2-mLHNO mixture is more
effective. Pure nickel or nickel-copper alloys dissolve best in HNO
minimal amounts (<0.1 µg/g) of the analyte of interest.
(1 + 1).
6.2 Calibration Solutions—Made up for the individual ana-
NOTE 3—The general method of dissolution can be modified as
lytes as described in Sections 12-19. They should be prepared
specified in the appropriate sections.
to meet the guidelines of Practice E 1452.
NOTE 4—If sample inhomogeneity is suspected, a larger mass of
6.3 Matrix Modifiers and Ionization Buffers—Made up for
sample (10 g to 50 g) may be taken for analysis. In that case, however, an
the individual analytes, where required, as described in Sec-
aliquot portion corresponding to 1-g sample shall be taken from the
tions 12-19.
solution and processed in accordance with the procedure given.
8.1.3 Using low heat, evaporate the solution just to dryness.
7. Sampling and Sample Preparation
Do not bake. Cool to about 50 °C and add 25 mL HCl and
7.1 Sampling and sample preparation is to be performed by
again evaporate just to dryness.Add 25 mLHCl and repeat the
procedures agreed upon between the buyer and the seller.
evaporation.
7.2 The sampling procedure shall not involve any steps or
8.1.4 Cool to about 50 °C, add 5 mL hydrochloric acid and
procedures that can result in the loss of any analyte in the
20 mL water and heat to dissolve the salt.
sample.
8.1.5 Proceed as directed in Sections 12-19.
8.2 Reagent Blank—Carry a reagent blank through the
NOTE 1—Arc melting of the sample or induction melting of the sample
entire procedure using the same amounts of all reagents with
under vacuum can result in significant loss of several elements that have
the omitted sample.
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
8.3 Calibration Solutions—Proceed as directed in Sections
sample. Induction melting should be performed only in a complete or
12-19.
partial inert atmosphere.
8.4 Atomic Absorption Measurements:
7.3 The laboratory sample is normally in the form of 8.4.1 The wavelength of the spectral lines and the flame
turnings, millings, or drillings and no further mechanical type to be used are listed in Sections 12-19.
preparation of the sample is necessary. 8.4.2 Set the required instrument parameters in accordance
7.4 The laboratory sample shall be cleaned by washing in with the manufacturer’s recommendations and Practice
pure acetone and then air dried. E 1812. Light the burner and aspirate water until thermal
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E1835–96 (2002)
equilibrium is reached. The flame conditions will vary accord- 12. Determination of Aluminum
ing to the element being determined. Zero the instrument.
12.1 Parameters:
8.4.3 Ensure that the instrument meets the performance
12.1.1 Wavelength: 309.3 nm.
requirements given in Practice E 1812. Optimum settings for
12.1.2 Flame: nitrous oxide—Acetylene.
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)—
Dissolve 1.000 g of aluminum (purity 99.9 % min) in 30 mL
8.4.6 Aspirate the calibration solutions and the test solu-
(1 + 1) of HCl in the presence of 1 drop of mercury. Filter the
tion(s) and note the readings to determine the approximate
solution through a rapid filter paper. Wash the filter with 100
concentration of the test solution(s).
mL of warm water.Add 85 mL of HCl to the filtrate, cool and
8.4.7 Aspirate water until the initial reading is obtained.
transfer to a 1-L volumetric flask, dilute to volume, and mix.
Zero if necessary.
Storeinapolyethylenebottle.(Warning—Mercurywhichacts
8.4.8 Aspirate the calibration solutions and the test solu-
a catalyst to help the dissolution of high-purity aluminum is
tion(s) in the order of increasing instrument response, starting
highly poisonous and has an appreciable vapor pressure. It
with the calibration solution containing no analyte (S ). When
must be stored in strong, tightly closed containers. Liquid
a stable response is obtained record the reading. Flush the
mercury must be transferred in such a manner that a spill can
system by aspirating water between each test and calibration
be contained and thoroughly cleaned up at once. Dispose of
solution.
mercury in accordance with applicable regulations.)
8.4.9 Repeat the measurement of the full set of calibration
12.2.3 Aluminum Calibration Solution (100 mg/L)—
and test solutions two more times and record the data.
Transfer a 100-mL aliquot of the aluminum stock standard
solution(12.2.2)intoa1-Lvolumetricflask.Add90mLofHCl
9. Preparation of Calibration Graphs
and 800 mL water. Cool, dilute to volume, and mix. Store in a
9.1 Plot the average instrument reading against the concen-
polyethylene bottle.
tration of the analyte in the calibration solutions for each of the
12.3 Aluminum Calibration Solutions—Transfer to each of
measurements.
six 100-mL volumetric flasks (0, 5.0, 10, 15, 20, and 25) mL,
respectively, of the aluminum calibration solution (12.2.3).
NOTE 5—Some instruments may be adjusted to give a readout in
Add4mLofthepotassiumchloridesolution(12.2.1)and4mL
concentration of the analyte. A graph of instrument response versus
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,
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 6—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-mLPTFE 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 = 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 = volume, mL, of the initial test solution;
through 11-cm low-ash medium-porosity filter paper into a
F = dilution factor for the secondary dilution; and
250-mLbeaker. Wash the filter five times with 10-mLportions
m = mass, g, of the test portion.
of hot water.Add the washings to the filtrate. Reserve the filter
paper containing any undissolved residue.
11. Report
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
...