ASTM E1852-96e1
(Test Method)Standard Test Method for Determination of Low Levels of Antimony in Carbon and Low-Alloy Steel by Electrothermal Atomic Absorption Spectrometry
Standard Test Method for Determination of Low Levels of Antimony in Carbon and Low-Alloy Steel by Electrothermal Atomic Absorption Spectrometry
SCOPE
1.1 This test method covers the determination of antimony in carbon and low-alloy steel in the 0.0005 through 0,010% range.
1.2 If this test method is used to test materials having contents less than 0.001% antimony, users of different laboratories will experience more than the usual 5% risk that their results will differ by more 50% relative error.
1.3 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 and health practices and determine the applicability of regulatory limitations prior to use.
General Information
Relations
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
e1
Designation: E 1852 – 96
Standard Test Method for
Determination of Low Levels of Antimony in Carbon and
Low-Alloy Steel by Electrothermal Atomic Absorption
Spectrometry
This standard is issued under the fixed designation E 1852; 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.
e NOTE—An Editorial correction was made in June 1997.
1. Scope Electrothermal Atomic Absorption Spectrometric
Method
1.1 This test method covers the determination of antimony
in carbon and low-alloy steel in the 0.0005 through 0.010 %
3. Summary of Test Method
range.
3.1 The sample is dissolved in hydrochloric and nitric acids
1.2 If this test method is used to test materials having
and diluted to volume. An appropriate aliquot is injected into
contents less than 0.001 % antimony, users of different labo-
the electrothermal atomizer of an atomic absorption spectrom-
ratories will experience more than the usual 5 % risk that their
eter, which is equipped with a background correction. The
results will differ by more than 50 % relative error.
sample is dried, pyrolized, and atomized. The absorbance of
1.3 This standard does not purport to address all of the
the radiation from the external light source is measured and
safety concerns, if any, associated with its use. It is the
compared to the absorbance of samples to which known
responsibility of the user of this standard to establish appro-
amounts of the sought element were added.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
NOTE 1—In general, the deuterium correction system should be able to
correct for the broad-band background absorbance up to 0.5 to 0.6
2. Referenced Documents
absorbance units. Zeeman systems should compensate for background
levels as high as 1.0 to 1.5 absorbance units.
2.1 ASTM Standards:
E 50 Practices for Apparatus, Reagents, and Safety Precau-
4. Significance and Use
tions for Chemical Analysis of Metals
4.1 This test method is to be used for the determination of
E 1184 Practice for Electrothermal (Graphite Furnace)
3 trace levels of antimony in carbon and low-alloy steel. It is
Atomic Absorption Analysis
assumed that the procedure will be performed by trained
E 1452 Practice for Preparation of Calibration Solutions for
analysts capable of performing common laboratory practices
Spectrophotometric and for Spectroscopic Atomic Analy-
skillfully and safely. It is expected that the work will be
ses
performed in a properly equipped laboratory and proper waste
E 1601 Practice for Conducting an Interlaboratory Study to
3 disposal procedures will be followed.
Evaluate the Performance of an Analytical Method
E 1770 Practice for Optimization of Electrothermal Atomic
5. Apparatus
Absorption Spectrometric Equipment
5.1 Atomic Absorption Spectrometer with Electrothermal
2.2 ISO Standards:
Atomizer, equipped with background corrector and appropriate
ISO 5725 Precision of Test Methods—Determination of
signal output device, such as video display screen, digital
Repeatability and Reproducibility for a Standard Test
4 computer, printer or strip chart recorder, and autosampler. It is
Method by Inter-Laboratory Tests
recommended that the instrument meet the following perfor-
ISO 10698 Steel—Determination of Antimony Content—
mance requirements after adjusting the instrument and opti-
mizing the furnace heating program as described in Practice
This test method is under the jurisdiction of ASTM Committee E-1 on
E 1770.
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
5.1.1 The characteristic mass determined in accordance
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.
with Practice E 1770 for antimony shall be less than 25 pg or
Current edition approved Dec. 10, 1996. Published February 1997.
Annual Book of ASTM Standards, Vol 03.05.
within the manufacturer’s tolerance.
Annual Book of ASTM Standards, Vol 03.06.
5.1.2 The minimum precision of the most concentrated
Available from American National Standards Institute, 11 West 42nd Street,
blank addition solution shall not exceed 10 % of the mean
13th Floor, New York, NY 10036.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
E 1852
absorbance of the same solution. The minimum precision of 8. Procedure
the least concentrated blank addition solution (excluding So-
8.1 Sample Size—For samples containing between 0.0005
lution B ) shall not exceed 4 % of the mean absorbance of the
0 and 0.0050 % antimony, the sample size shall be ’1.00 g,
most concentrated blank addition solution when determined in
weighed to the nearest 0.1 mg. For samples containing between
accordance with Practice E 1770.
0.0050 and 0.010 % antimony, the sample shall be ’0.25 g
5.1.3 The limit of detection of antimony as described in
weighed to the nearest 0.1 mg.
Practice E 1770 shall be less than 20 pg.
8.2 Blank—Simultaneously with the sample, a blank test
5.1.4 Unless the instrument is provided with automatic
using the same quantities of all reagents shall be carried along.
curve correction circuitry, the graph linearity shall not be less
The antimony contents of the blank should be no greater than
than 0.95 when determined in accordance with Practice
10 ppb.
E 1770.
8.3 Test Solution—Transfer the test portion in accordance
5.2 Graphite Tubes, with pyrolytic coating and grooves for
with 8.1 into a 250-mL beaker. Add 5 mL HCl and 50 mL
graphite platform, suitable for use with the electrothermal
HNO . Cover the beaker with a watch glass, heat gently until
atomizer used.
the reaction ceases, and boil for 1 min to remove the oxides of
5.3 Graphite Platform, pyrolytic graphite, L’vov design, to
nitrogen.
fit graphite tubes specified in 5.2.
8.3.1 If sample contains tungsten or niobium, or both,
5.4 Labware—To prevent contamination of the sample(s),
transfer test portion (see 9.1) to a 100-mL beaker and add 1 mL
all beakers, lids, volumetric flasks, and funnels must be cleaned
orthophosphoric acid, 15 mL hydrochloric acid, and 5 mL
with hot HNO (1 + 1) before use.
nitric acid. Cover beaker with watch glass, and heat gently until
reaction ceases. Evaporate the solution to 2 to 3 mL; then add
6. Reagents
25 mL nitric acid. Boil for 1 min to remove nitrous oxides.
6.1 Purity and Concentration of Reagents—The purity and Carry along a separate blank test corresponding to this proce-
concentration of common chemical reagents shall conform to
dure.
Practices E 50. It is important that antimony shall not exceed 8.3.2 Allow the solution, which may contain carbides, to
0.01 μg/mL in each of the reagents and 0.001 μg/mL in the
cool. Add about 15 mL water, filter through medium texture
water. filter paper, and collect the filtrate in a 200-mL volumetric
6.2 Antimony Stock Solution (1 mL 51mgSb)—Dissolve
flask. Wash the filter paper several times with warm water and
0.100 6 0.0001 g high-purity antimony (minimum 99.9 % Sb) collect the washings in the flask. Dilute to the mark with water
in 30 mL HCl + 5 mL HNO in a 100-mL beaker. Boil gently
and mix.
to expel oxides of nitrogen. Cool and transfer the solution into 8.4 Test Addition Solutions—Transfer separate 20.0-mL ali-
a 100-mL volumetric flask. Dilute to mark with HNO (1+1)
quot of the test solution into a series of five 100-mL volumetric
and mix. Store in polypropylene or high density polyethylene flasks. Using a micropipette, inject the respective volumes of
bottle.
antimony standard solution indicated in Table 1. Dilute to the
6.3 Antimony Standard Solution (1 mL 5 10 μg Sb)— mark with water and mix. These solutions are referred to as S ,
Transfer 1.0 mL of the antimony stock solution to a 100-mL
S ,S ,S , and S , respectively.
1 2 3 4
volumetric flask, dilute to the mark with HNO (1 + 1), and 8.5 Blank Addition Solutions—Transfer separate 20.0-mL
mix. Prepare this solution immediately before use.
aliquot of the blank solution into a series of five 100-mL
volumetric flasks. Using a micropipette, add the respective
7. Sampling and Sample Preparation
volumes of antimony standard solution indicated in Table 2.
Dilute to the mark with water and mix. These solutions are
7.1 Sampling and sample preparation is to be performed by
referred to as B ,B ,B ,B , and B , respectively.
procedures agreed on between buyer and seller. 0 1 2 3 4
8.6 Optical parameters used for the determination of anti-
7.2 The sampling procedures shall not involve any steps or
mony are given in Table 3.
operations that can result in the loss of antimony in the sample.
8.7 The atomic absorption spectrometer and the electrother-
NOTE 2—Arc melting of the sample or induction melting of the sample
mal atomizer should be adjusted and optimized as described in
under vacuum may result in significant loss of several elements that have
Practice E 1770.
a low vapor pressure. Arc melting of the sample should be avoided and
induction melting should be performed only in an at least partial inert
NOTE 3—The volume injected into the atomizer should be between 10
atmosphere.
TABLE 1 Test Addition Solutions
7.3 The laboratory
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.