ASTM E1852-96(2001)
(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
SIGNIFICANCE AND USE
This test method is to be used for the determination of trace levels of antimony in carbon and low-alloy steel. It is assumed that the procedure will be performed by trained analysts capable of performing common laboratory practices skillfully and safely. It is expected that the work will be performed in a properly equipped laboratory and proper waste disposal procedures will be followed.
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.
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Designation:E1852–96(Reapproved 2001)
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 E1852; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber 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 5725 Precision of Test Methods—Determination of
Repeatability and Reproducibility for a Standard Test
1.1 This test method covers the determination of antimony
Method by Inter-Laboratory Tests
in carbon and low-alloy steel in the 0.0005 through 0.010%
ISO 10698 Steel—Determination of Antimony Content—
range.
Electrothermal Atomic Absorption Spectrometric
1.2 If this test method is used to test materials having
Method
contents less than 0.001% antimony, users of different labo-
ratories will experience more than the usual 5% risk that their
3. Summary of Test Method
results will differ by more than 50% relative error.
3.1 The sample is dissolved in hydrochloric and nitric acids
1.3 This standard does not purport to address all of the
and diluted to volume. An appropriate aliquot is injected into
safety concerns, if any, associated with its use. It is the
the electrothermal atomizer of an atomic absorption spectrom-
responsibility of the user of this standard to establish appro-
eter, which is equipped with a background correction. The
priate safety and health practices and determine the applica-
sample is dried, pyrolized, and atomized. The absorbance of
bility of regulatory limitations prior to use.
the radiation from the external light source is measured and
2. Referenced Documents compared to the absorbance of samples to which known
amounts of the sought element were added.
2.1 ASTM Standards:
E50 Practices forApparatus, Reagents, and Safety Consid-
NOTE 1—In general, the deuterium correction system should be able to
erations for Chemical Analysis of Metals, Ores, and correct for the broad-band background absorbance up to 0.5 to 0.6
absorbance units. Zeeman systems should compensate for background
Related Materials
levels as high as 1.0 to 1.5 absorbance units.
E 1184 Practice for Electrothermal (Graphite Furnace)
Atomic Absorption Analysis
4. Significance and Use
E1452 Practice for Preparation of Calibration Solutions for
4.1 This test method is to be used for the determination of
Spectrophotometric and for Spectroscopic Atomic Analy-
trace levels of antimony in carbon and low-alloy steel. It is
ses
assumed that the procedure will be performed by trained
E1601 Practice for Conducting an Interlaboratory Study to
analysts capable of performing common laboratory practices
Evaluate the Performance of an Analytical Method
skillfully and safely. It is expected that the work will be
E1770 Practice for Optimization of ElectrothermalAtomic
performed in a properly equipped laboratory and proper waste
Absorption Spectrometric Equipment
disposal procedures will be followed.
2.2 ISO Standards:
5. Apparatus
5.1 Atomic Absorption Spectrometer with Electrothermal
This test method is under the jurisdiction of ASTM Committee E01 on
Atomizer, equipped with background corrector and appropriate
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
signal output device, such as video display screen, digital
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.
Current edition approved Dec. 10, 1996. Published February 1997. computer, printer or strip chart recorder, and autosampler. It is
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
Standards volume information, refer to the standard’s Document Summary page on Available from American National Standards Institute, 11 West 42nd Street,
the ASTM website. 13th Floor, New York, NY 10036.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E1852–96 (2001)
recommended that the instrument meet the following perfor- 7.3 The laboratory sample is normally in the form of
mance requirements after adjusting the instrument and opti- turnings, millings, or drillings. No further mechanical prepa-
mizing the furnace heating program as described in Practice ration of the sample is necessary.
E1770. 7.4 The laboratory sample shall be cleaned by first washing
in acetone and air drying.
5.1.1 The characteristic mass determined in accordance
7.5 If brazed alloy tools are used in the preparation of the
with Practice E1770 for antimony shall be less than 25 pg or
sample, the sample shall be further cleaned by pickling in
within the manufacturer’s tolerance.
diluted nitric acid for a few minutes. The sample shall then be
5.1.2 The minimum precision of the most concentrated
washed several times with water, then several times with
blank addition solution shall not exceed 10% of the mean
acetone and air dried.
absorbance of the same solution. The minimum precision of
the least concentrated blank addition solution (excluding So-
8. Procedure
lution B ) shall not exceed 4% of the mean absorbance of the
most concentrated blank addition solution when determined in
8.1 Sample Size—For samples containing between 0.0005
accordance with Practice E1770. and 0.0050% antimony, the sample size shall be '1.00 g,
5.1.3 The limit of detection of antimony as described in weighedtothenearest0.1mg.Forsamplescontainingbetween
0.0050 and 0.010% antimony, the sample shall be '0.25 g
Practice E1770 shall be less than 20 pg.
weighed to the nearest 0.1 mg.
5.1.4 Unless the instrument is provided with automatic
8.2 Blank—Simultaneously with the sample, a blank test
curve correction circuitry, the graph linearity shall not be less
using the same quantities of all reagents shall be carried along.
than 0.95 when determined in accordance with Practice
The antimony contents of the blank should be no greater than
E1770.
10 ppb.
5.2 Graphite Tubes, with pyrolytic coating and grooves for
8.3 Test Solution—Transfer the test portion in accordance
graphite platform, suitable for use with the electrothermal
with 8.1 into a 250-mL beaker. Add 5 mL HCl and 50 mL
atomizer used.
HNO . Cover the beaker with a watch glass, heat gently until
5.3 Graphite Platform, pyrolytic graphite, L’vov design, to
the reaction ceases, and boil for 1 min to remove the oxides of
fit graphite tubes specified in 5.2.
nitrogen.
5.4 Labware—To prevent contamination of the sample(s),
8.3.1 If sample contains tungsten or niobium, or both,
allbeakers,lids,volumetricflasks,andfunnelsmustbecleaned
transfertestportion(see9.1)toa100-mLbeakerandadd1mL
with hot HNO (1+1) before use.
orthophosphoric acid, 15 mL hydrochloric acid, and 5 mL
nitricacid.Coverbeakerwithwatchglass,andheatgentlyuntil
6. Reagents
reaction ceases. Evaporate the solution to 2 to 3 mL; then add
6.1 Purity and Concentration of Reagents—The purity and
25 mL nitric acid. Boil for 1 min to remove nitrous oxides.
concentration of common chemical reagents shall conform to
Carry along a separate blank test corresponding to this proce-
PracticesE50. It is important that antimony shall not exceed
dure.
0.01 µg/mL in each of the reagents and 0.001 µg/mL in the
8.3.2 Allow the solution, which may contain carbides, to
water.
cool. Add about 15 mL water, filter through medium texture
6.2 Antimony Stock Solution (1 mL = 1 mg Sb)—Dissolve filter paper, and collect the filtrate in a 200-mL volumetric
0.100 6 0.0001 g high-purity antimony (minimum 99.9% Sb)
flask. Wash the filter paper several times with warm water and
in 30 mL HCl+5 mL HNO in a 100-mL beaker. Boil gently collect the washings in the flask. Dilute to the mark with water
to expel oxides of nitrogen. Cool and transfer the solution into
and mix.
a 100-mL volumetric flask. Dilute to mark with HNO(1+1) 8.4 Test Addition Solutions—Transfer separate 20.0-mLali-
and mix. Store in polypropylene or high density polyethylene
quotofthetestsolutionintoaseriesoffive100-mLvolumetric
bottle. flasks. Using a micropipette, inject the respective volumes of
6.3 Antimony Standard Solution (1 mL = 10 µg Sb)— antimony standard solution indicated in Table 1. Dilute to the
markwithwaterandmix.ThesesolutionsarereferredtoasS ,
Transfer 1.0 mL of the antimony stock solution to a 100-mL
S,S,S , and S , respectively.
volumetric flask, dilute to the mark with HNO (1+1), and
1 2 3 4
mix. Prepare this solution immediately before use.
TABLE 1 Test Addition Solutions
7. Sampling and Sample Preparation
Concentration
Corresponding Mass of
Volume of
7.1 Sampling and sample preparation is to be performed by
of Antimony
Antimony Added, ng
Antimony
procedures agreed on between buyer and seller.
Name of Added in Test
Standard
Volume Volume
Solution Addition
7.2 The sampling procedures shall not involve any steps or Solution
Injected, Injected,
Solutions,
Added, µL
operationsthatcanresultinthelossofantimonyinthesample.
10 µL 50 µL
ng/mL
S 00 0.0 0.0
NOTE 2—Arc melting of the sample or induction melting of the sample
S 100 10 0.1 0.5
under vacuum may result in significant loss of several elements that have
S 200 20 0.2 1.0
a low
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