ASTM E1852-19

Standard Test Method for Determination of Low Levels of Antimony in Carbon and Low-Alloy Steel by Graphite Furnace Atomic Absorption Spectrometry

SIGNIFICANCE AND USE
5.1 This test method is utilized 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 than 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Published
• Publication Date: 14-Jun-2019
• ICS: 71.040.50 - Physicochemical methods of analysis
• Technical Committee: E01 - Analytical Chemistry for Metals, Ores, and Related Materials
• Drafting Committee: E01.01 - Iron, Steel, and Ferroalloys

Relations

• Replaces: ASTM E1852-13 - Standard Test Method for Determination of Low Levels of Antimony in Carbon and Low-Alloy Steel by Graphite Furnace Atomic Absorption Spectrometry
• Effective Date: 15-Jun-2019
• Refers: ASTM E135-20 - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 01-Jan-2020
• Refers: ASTM E1601-19 - Standard Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical Method
• Effective Date: 01-Nov-2019
• Refers: ASTM E135-19 - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 15-May-2019
• Refers: ASTM E1770-19 - Standard Practice for Optimization of Instrumentation for Graphite Furnace Atomic Absorption Spectrometry
• Effective Date: 15-Apr-2019
• Refers: ASTM E50-17 - Standard Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
• Effective Date: 01-Sep-2017
• Refers: ASTM E50-11(2016) - Standard Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
• Effective Date: 01-Aug-2016
• Refers: ASTM E135-16 - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 15-May-2016
• Refers: ASTM E135-15a - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 01-Jul-2015
• Refers: ASTM E135-15 - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 15-May-2015
• Refers: ASTM E1770-14 - Standard Practice for Optimization of Electrothermal Atomic Absorption Spectrometric Equipment
• Effective Date: 01-Dec-2014
• Refers: ASTM E135-14b - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 15-Aug-2014
• Refers: ASTM E135-14a - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 01-Apr-2014
• Refers: ASTM E135-14 - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 15-Feb-2014
• Refers: ASTM E135-13a - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 01-Dec-2013

Overview

ASTM E1852-19 is the internationally recognized standard test method for the determination of low levels of antimony in carbon and low-alloy steel using graphite furnace atomic absorption spectrometry (GFAAS). This method is essential for laboratories analyzing trace element concentrations in metals, supporting quality control, material certification, and regulatory compliance in the steel industry. It enables precise detection of antimony within the 0.0005% to 0.010% range, ensuring the integrity and performance of steel products.

Key Topics

• Trace Analysis of Antimony: This method provides clear procedures for detecting extremely low antimony concentrations, helping manufacturers maintain safety, quality, and compliance in steel production.
• Sample Preparation: Detailed steps include dissolving steel samples in hydrochloric and nitric acids, filtering and diluting, and ensuring contamination-free labware and reagents.
• Instrument Requirements: The test requires a graphite furnace atomic absorption spectrometer equipped with background correction and accurate signal output. Optimal use relies on adherence to best practices for instrument calibration and performance verification.
• Precision and Reproducibility: The standard provides information on expected repeatability and reproducibility via interlaboratory testing and statistical evaluation.
• Health, Safety, and Environmental Practices: The standard emphasizes the importance of proper laboratory procedures and waste disposal, highlighting user responsibility for compliance with safety regulations.
• Interference and Quality Control: Recommendations address matrix effects, background correction, and the potential need for blanks and standards to ensure accurate results.

Applications

Adhering to ASTM E1852-19 enables:

• Quality Assurance in Steel Manufacturing: Manufacturers can ensure that steel products meet strict specifications regarding trace element composition, vital for applications in construction, automotive, and heavy industry.
• Material Certification: Accredited laboratories use this method to provide certified test reports on steel composition, essential for customer assurance and contractual compliance.
• Regulatory Compliance: Many national and international regulations require verification of trace elements in metals; following this standard supports compliance with these requirements.
• Research and Development: R&D labs employ this method to develop new steel grades or refine existing ones by monitoring trace antimony levels.
• Environmental Monitoring: Facilities concerned with environmental impact assessments utilize this test for precise tracking of antimony content in process streams and waste products.

Related Standards

ASTM E1852-19 references a suite of related standards to provide a complete analytical framework:

• ASTM E29: Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
• ASTM E50: Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
• ASTM E135: Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• ASTM E1184: Practice for Determination of Elements by Graphite Furnace Atomic Absorption Spectrometry
• ASTM E1601: Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical Method
• ASTM E1770: Practice for Optimization of Instrumentation for Graphite Furnace Atomic Absorption Spectrometry
• ASTM E1806: Practice for Sampling Steel and Iron for Determination of Chemical Composition
• ISO 5725: Precision of Test Methods-Determination of Repeatability and Reproducibility for a Standard Test Method by Inter-Laboratory Tests
• ISO 10698: Steel-Determination of Antimony Content-Electrothermal Atomic Absorption Spectrometric Method

Practical Value

Implementing ASTM E1852-19 ensures high-quality, reproducible results when analyzing low-level antimony in steel. This test method underpins robust steel manufacturing processes, supports reliable material characterization, and helps organizations demonstrate compliance with international standards and industry best practices for atomic absorption spectrometry.

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: E1852 − 19
Standard Test Method for
Determination of Low Levels of Antimony in Carbon and
Low-Alloy Steel by Graphite Furnace 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope E1601Practice for Conducting an Interlaboratory Study to
Evaluate the Performance of an Analytical Method
1.1 This test method covers the determination of antimony
E1770Practice for Optimization of Instrumentation for
incarbonandlow-alloysteelinthe0.0005%through0.010%
Graphite Furnace Atomic Absorption Spectrometry
range.
E1806Practice for Sampling Steel and Iron for Determina-
1.2 If this test method is used to test materials having
tion of Chemical Composition
contents less than 0.001% antimony, users of different labo- 3
2.2 ISO Standards:
ratories will experience more than the usual 5% risk that their
ISO 5725Precision of Test Methods—Determination of
results will differ by more than 50% relative error.
Repeatability and Reproducibility for a Standard Test
1.3 This standard does not purport to address all of the
Method by Inter-Laboratory Tests
safety concerns, if any, associated with its use. It is the
ISO 10698Steel—Determination of Antimony Content—
responsibility of the user of this standard to establish appro-
ElectrothermalAtomicAbsorption Spectrometric Method
priate safety, health, and environmental practices and deter-
3. Terminology
mine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accor-
3.1 Fordefinitionsoftermsusedinthistestmethod,referto
dance with internationally recognized principles on standard-
Terminology E135.
ization established in the Decision on Principles for the
4. Summary of Test Method
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
4.1 ThesampleisdissolvedinHClandHNO anddilutedto
Barriers to Trade (TBT) Committee.
volume. An appropriate aliquot is injected into the graphite
furnace atomizer of an atomic absorption spectrometer, which
2. Referenced Documents
isequippedwithabackgroundcorrection.Thesampleisdried,
2.1 ASTM Standards:
pyrolized, and atomized.The absorbance of the radiation from
E29Practice for Using Significant Digits in Test Data to
the external light source is measured and compared to the
Determine Conformance with Specifications
absorbance of samples of known composition.
E50Practices for Apparatus, 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
Related Materials
absorbance units. Zeeman systems should compensate for background
E135Terminology Relating to Analytical Chemistry for
levels as high as 1.0 to 1.5 absorbance units.
Metals, Ores, and Related Materials
5. Significance and Use
E1184Practice for Determination of Elements by Graphite
Furnace Atomic Absorption Spectrometry
5.1 This test method is utilized 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
This test method is under the jurisdiction of ASTM Committee E01 on
analysts capable of performing common laboratory practices
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.
skillfully and safely. It is expected that the work will be
Current edition approved June 15, 2019. Published August 2019. Originally
performed in a properly equipped laboratory and proper waste
approved in 1996. Last previous edition approved in 2013 as E1852–13. DOI:
disposal procedures will be followed.
10.1520/E1852-19.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
the ASTM website. 4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E1852 − 19
6. Hazards 9. Sampling and Sample Preparation
9.1 Refer to Practice E1806 for devices and practices to
6.1 For precautions to be observed in the use of certain
sample liquid and solid steel.
reagents and equipment in this test method, refer to Practices
E50.
9.2 The sampling procedures shall not involve any steps or
operationsthatcanresultinthelossofantimonyinthesample.
7. Apparatus
NOTE 2—Arc melting of the sample or induction melting of the sample
7.1 AtomicAbsorptionSpectrometerwithGraphiteFurnace
under vacuum may result in significant loss of several elements that have
a low vapor pressure. Arc melting of the sample should be avoided and
Atomizer, equipped with background corrector and appropriate
induction melting should be performed only in an at least partial inert
signal output device, such as video display screen, digital
atmosphere.
computer, printer or strip chart recorder, and autosampler. It is
9.3 The laboratory sample shall be cleaned by first washing
recommended that the instrument meet the following perfor-
in acetone and air drying.
mance requirements after adjusting the instrument and opti-
mizing the furnace heating program as described in Practice
9.4 If brazed alloy tools are used in the preparation of the
E1770.
sample, the sample shall be further cleaned by pickling in
7.1.1 The characteristic mass determined as directed in
diluted HNO for a few minutes. The sample shall then be
Practice E1770 for antimony shall be less than 25 pg or within washed several times with water, then several times with
the manufacturer’s tolerance.
acetone and air dried.
7.1.2 The precision of the most concentrated blank addition
solution shall not exceed 10% of the mean absorbance of the 10. Procedure
same solution. The precision of the least concentrated blank
10.1 Sample Mass—For samples containing between
addition solution (excluding Solution B ) shall not exceed 4%
0.0005% and 0.0050% antimony, the sample mass shall be
of the mean absorbance of the most concentrated blank
≈1.00g,weighedtothenearest0.1mg.Forsamplescontaining
addition solution when determined as directed in Practice
between 0.0050% and 0.010% antimony, the sample shall be
E1770.
≈0.25 g weighed to the nearest 0.1 mg.
7.1.3 The limit of detection of antimony as described in
10.2 Blank—Simultaneously with the sample, a blank test
Practice E1770 shall be less than 20 pg.
using the same quantities of all reagents shall be performed.
7.1.4 Unless the instrument is provided with automatic
The antimony contents of the blank should be no greater than
curve correction circuitry, the graph linearity shall not be less
10 ng/mL.
than 0.95 when determined as directed in Practice E1770.
10.3 Test Solution—Transfer the test portion as directed in
7.2 Graphite Tubes, with pyrolytic coating and grooves for
10.1 into a 250-mL beaker.Add 5 mL HCl and 50 mL HNO .
graphite platform, suitable for use with the graphite furnace
Cover the beaker with a watch glass, heat gently until the
unit.
reaction ceases, and boil for 1 min to remove the oxides of
7.3 Graphite Platform, pyrolytic graphite, L’vov design, to
nitrogen.
fit graphite tubes specified in 7.2. 10.3.1 If sample contains tungsten or niobium, or both,
transfer the test portion to a 100-mL beaker and add 1 mL
7.4 Labware—To prevent contamination of the sample(s),
H PO ,15mLHCl,and5mLHNO .Coverbeakerwithwatch
3 4 3
allbeakers,lids,volumetricflasks,andfunnelsmustbecleaned
glass, and heat gently until reaction ceases. Evaporate the
with hot HNO (1+1) before use.
solution to 2 mL to 3 mL; then add 25 mL HNO . Boil for 1
min to remove oxides of nitrogen. Conduct a separate blank
8. Reagents
test corresponding to this procedure.
8.1 Purity and Concentration of Reagents—The purity and
10.3.2 Allow the solution, which may contain carbides, to
concentration of common chemical reagents shall conform to
cool. Add about 15 mL water, filter through medium texture
Practices E50. It is important that antimony shall not exceed
filter paper, and collect the filtrate in a 200-mL volumetric
0.01 µg/mL in each of the reagents and 0.001 µg/mL in the
flask. Wash the filter paper several times with warm water and
water.
collect the washings in the flask. Dilute to the mark with water
and mix.
8.2 Antimony Stock Solution (1 mL = 1 mg Sb)—Dissolve
0.1000 g 6 0.0001 g high-purity antimony (minimum 99.9%
10.4 Test Addition Solutions—Transfer separate 20.0-mL
Sb) in 30 mL HCl+5 mL HNO in a 100-mL beaker. Boil
aliquots of the test solution into a series of five 100-mL
gently to expel oxides of nitrogen. Cool and transfer the
volumetric flasks. Using a micropipette, inject the respective
solution into a 100-mL volumetric flask. Dilute to mark with
volumes of antimony standard solution indicated in Table 1.
HNO (1+1) and mix. Store in polypropylene or high density
Dilute to the mark with water and mix. These solutions are
polyethylene bottle.
referred to as S,S,S,S , and S , respectively.
0 1 2 3 4
8.3 Antimony Standard Solut
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: E1852 − 13 E1852 − 19
Standard Test Method for
Determination of Low Levels of Antimony in Carbon and
Low-Alloy Steel by Graphite Furnace 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. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. 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 than 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
E50 Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
E135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
E1184 Practice for Determination of Elements by Graphite Furnace Atomic Absorption Spectrometry
E1601 Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical Method
E1770 Practice for Optimization of Instrumentation for Graphite Furnace Atomic Absorption Spectrometry
E1806 Practice for Sampling Steel and Iron for Determination of Chemical Composition
2.2 ISO Standards:
ISO 5725 Precision of Test Methods—Determination of Repeatability and Reproducibility for a Standard Test Method by
Inter-Laboratory Tests
ISO 10698 Steel—Determination of Antimony Content—Electrothermal Atomic Absorption Spectrometric Method
3. Terminology
3.1 For definitions of terms used in this test method, refer to Terminology E135.
4. Summary of Test Method
4.1 The sample is dissolved in hydrochloricHCl and nitricHNO acids and diluted to volume. An appropriate aliquot is injected
into the graphite furnace atomizer of an atomic absorption spectrometer, which is equipped with a background correction. The
sample is dried, pyrolized, and atomized. The absorbance of the radiation from the external light source is measured and compared
to the absorbance of samples of known composition.
This test method is under the jurisdiction of ASTM Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials and is the direct responsibility of
Subcommittee E01.01 on Iron, Steel, and Ferroalloys.
Current edition approved Nov. 15, 2013June 15, 2019. Published January 2014August 2019. Originally approved in 1996. Last previous edition approved in 20082013
as E1852 – 08.E1852 – 13. DOI: 10.1520/E1852-13.10.1520/E1852-19.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E1852 − 19
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 absorbance
units. Zeeman systems should compensate for background levels as high as 1.0 to 1.5 absorbance units.
5. Significance and Use
5.1 This test method is utilized 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.
6. Hazards
6.1 For precautions to be observed in the use of certain reagents and equipment in this test method, refer to Practices E50.
7. Apparatus
7.1 Atomic Absorption Spectrometer with Graphite Furnace Atomizer, equipped with background corrector and appropriate
signal output device, such as video display screen, digital computer, printer or strip chart recorder, and autosampler. It is
recommended that the instrument meet the following performance requirements after adjusting the instrument and optimizing the
furnace heating program as described in Practice E1770.
7.1.1 The characteristic mass determined in accordance withas directed in Practice E1770 for antimony shall be less than 25
pg or within the manufacturer’s tolerance.
7.1.2 The precision of the most concentrated blank addition solution shall not exceed 10 % of the mean absorbance of the same
solution. The precision of the least concentrated blank addition solution (excluding Solution B ) shall not exceed 4 % of the mean
absorbance of the most concentrated blank addition solution when determined in accordance withas directed in Practice E1770.
7.1.3 The limit of detection of antimony as described in Practice E1770 shall be less than 20 pg.
7.1.4 Unless the instrument is provided with automatic curve correction circuitry, the graph linearity shall not be less than 0.95
when determined in accordance withas directed in Practice E1770.
7.2 Graphite Tubes, with pyrolytic coating and grooves for graphite platform, suitable for use with the graphite furnace unit.
7.3 Graphite Platform, pyrolytic graphite, L’vov design, to fit graphite tubes specified in 7.2.
7.4 Labware—To prevent contamination of the sample(s), all beakers, lids, volumetric flasks, and funnels must be cleaned with
hot HNO (1 + 1) before use.
8. Reagents
8.1 Purity and Concentration of Reagents—The purity and concentration of common chemical reagents shall conform to
Practices E50. It is important that antimony shall not exceed 0.01 μg/mL in each of the reagents and 0.001 μg/mL in the water.
8.2 Antimony Stock Solution (1 mL = 1 mg Sb)—Dissolve 0.1000 g 6 0.0001 g high-purity antimony (minimum 99.9 % Sb) in
30 mL HCl + 5 mL HNO in a 100-mL beaker. Boil gently to expel oxides of nitrogen. Cool and transfer the solution into a 100-mL
volumetric flask. Dilute to mark with HNO (1 + 1) and mix. Store in polypropylene or high density polyethylene bottle.
8.3 Antimony Standard Solution (1 mL = 10 μg Sb)—Transfer 1.0 mL of the antimony stock solution to a 100-mL volumetric
flask, dilute to the mark with HNO (1 + 1), and mix. Prepare this solution immediately before use.
9. Sampling and Sample Preparation
9.1 Refer to Practice E1806 for devices and practices to sample liquid and solid steel.
9.2 The sampling procedures shall not involve any steps or operations that can result in the loss of antimony in the sample.
NOTE 2—Arc melting of the sample or induction melting of the sample under vacuum may result in significant loss of several elements that have 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 atmosphere.
9.3 The laboratory sample shall be cleaned by first washing in acetone and air drying.
9.4 If brazed alloy tools are used in the preparation of the sample, the sample shall be further cleaned by pickling in diluted
nitricHNO acid for a few minutes. The sample shall then be washed several times with water, then several times with acetone and
air dried.
10. Procedure
10.1 Sample Mass—For samples containing between 0.0005 % and 0.0050 % antimony, the sample mass shall be ≈1.00 g,
weighed to the nearest 0.1 mg. For samples containing between 0.0050 % and 0.010 % antimony, the sample shall be ≈0.25 g
weighed to the nearest 0.1 mg.
10.2 Blank—Simultaneously with the sample, a blank test using the same quantities of all reagents shall be performed. The
antimony contents of the blank should be no greater than 10 ng/mL.
E1852 − 19
10.3 Test Solution—Transfer the test portion in accordance withas directed in 10.1 into a 250-mL beaker. Add 5 mL HCl and
50 mL HNO . Cover the beaker with a watch glass, heat gently until the reaction ceases, and boil for 1 min to remove the oxides
of nitrogen.
10.3.1 If sample contains tungsten or niobium, or both, transfer the test portion to a 100-mL beaker and add 1 mL H PO , 15
3 4
mL HCl, and 5 mL HNO . Cover beaker with watch glass, and heat gently until reaction ceases. Evaporate the solution to 2 mL
to 3 mL; then add 25 mL nitricHNO acid. . Boil for 1 min to remove oxides of nitrogen. Conduct a separate blank test
corresponding to this procedure.
10.3.2 Allow the solution, which may contain carbides, to cool. Add about 15 mL water, filter through medium texture filter
paper, and collect the filtrate in a 200-mL volumetric flask. Wash the filter paper several times with warm water and collect the
washings in the flask. Dilute to the mark with water and mix.
10.4 Test Addition Solutions—Transfer separate 20.0-mL aliquots of the test solution into a series of five 100-mL
...