ASTM E2575-19

Standard Test Method for Determination of Oxygen in Copper and Copper Alloys by Inert Gas Fusion

SIGNIFICANCE AND USE
5.1 This test method is primarily intended as a referee test for compliance with compositional specifications. It is assumed that all who use this test method will be trained analysts, capable of performing common laboratory procedures skillfully and safely. It is expected that work will be performed in a properly equipped laboratory.
SCOPE
1.1 This test method covers the determination of oxygen in copper and copper alloys from 0.00035 % to 0.090 %.  
1.2 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.  
1.3 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: 77.120.30 - Copper and copper alloys
• Technical Committee: E01 - Analytical Chemistry for Metals, Ores, and Related Materials
• Drafting Committee: E01.05 - Cu, Pb, Zn, Cd, Sn, Be, Precious Metals, their Alloys, and Related Metals

Relations

• Replaces: ASTM E2575-08 - Standard Test Method for Determination of Oxygen in Copper and Copper Alloys (Withdrawn 2017)
• 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 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 E882-10(2016)e1 - Standard Guide for Accountability and Quality Control in the Chemical Analysis Laboratory
• Effective Date: 01-Dec-2016
• Refers: ASTM E882-10(2016) - Standard Guide for Accountability and Quality Control in the Chemical Analysis Laboratory
• Effective Date: 01-Dec-2016
• 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 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 E2575-19 - Standard Test Method for Determination of Oxygen in Copper and Copper Alloys by Inert Gas Fusion outlines procedures for accurately measuring oxygen content in copper and copper alloys. This method is essential for assessing compliance with compositional specifications and is recognized internationally for analytical accuracy. The standard defines the test’s scope, which applies to oxygen determination in the range of 0.00035% to 0.090%. ASTM E2575-19 is primarily intended as a referee method and should be performed by trained analysts within a properly equipped laboratory environment.

Key Topics

• Test Method and Principle: The test utilizes inert gas fusion, where the copper sample is heated in a graphite crucible under a stream of inert gas (argon, helium, or nitrogen) to release oxygen. The released oxygen reacts with carbon to form carbon monoxide, which is then detected, typically by infrared measurement.
• Sample Preparation: Accurate results depend on careful sample handling, consistent surface cleaning, and preparation to avoid contamination and oxidation artifacts. Only solid samples are suitable, and recommended procedures include successive rinses in distilled water and methanol, acid etching, and drying.
• Calibration and Quality Control: The method requires calibration against certified copper or copper alloy reference materials. Regular calibration, blank correction, and drift checks are specified for maintaining accuracy.
• Apparatus and Reagents: High-purity graphite crucibles, inert gases, moisture traps, and analytical balances are essential components, together with reagent-grade chemicals for sample cleaning.
• Precision and Bias: Data from interlaboratory studies indicate satisfactory levels of repeatability and accuracy when the method is followed precisely.
• Safety Considerations: The standard emphasizes laboratory safety, handling of hot equipment, and chemical hazards, mandating that users establish appropriate safety and environmental protocols.

Applications

ASTM E2575-19 is widely adopted in quality control, research, and compliance testing for industries working with copper and copper alloys. Typical users include:

• Copper Refiners and Producers: Ensures product meets oxygen content specifications, which is critical for electrical conductivity, mechanical properties, and corrosion resistance.
• Metallurgical Laboratories: Allows comparative and referee testing to resolve disputes or confirm results from routine oxygen analysis methods.
• Research and Development: Provides a standardized approach for material characterization, processing studies, and new alloy development.

By providing a clear, reliable method for measuring oxygen, this standard underpins high-quality production and rigorous specification adherence in products where copper’s purity and performance are vital.

Related Standards

For organizations seeking broader guidance or complementary methods, the following referenced standards are relevant when applying ASTM E2575-19:

• ASTM E1019: Test Methods for Determination of Carbon, Sulfur, Nitrogen, and Oxygen in Steel, Iron, Nickel, and Cobalt Alloys.
• ASTM E50: Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals.
• ASTM E135: Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials.
• ASTM E882: Guide for Accountability and Quality Control in the Chemical Analysis Laboratory.
• IEEE/ASTM SI 10: American National Standard for Use of the International System of Units (SI): The Modern Metric System.

These standards bolster laboratory practices, improve analytical consistency, and facilitate international trade by aligning with World Trade Organization (WTO) recommendations on standardization.

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Keywords: ASTM E2575-19, oxygen determination, copper alloys, inert gas fusion, analytical chemistry, quality control, calibration, laboratory standard, compositional analysis, metallurgical testing

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: E2575 − 19
Standard Test Method for
Determination of Oxygen in Copper and Copper Alloys by
Inert Gas Fusion
This standard is issued under the fixed designation E2575; 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 2.2 IEEE/ASTM Standard:
IEEE/ASTM SI 10 American National Standard for Use of
1.1 This test method covers the determination of oxygen in
theInternationalSystemofUnits(SI):TheModernMetric
copper and copper alloys from 0.00035 % to 0.090 %.
System
1.2 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
3. Terminology
responsibility of the user of this standard to establish appro-
3.1 Definitions—For definitions of terms used in this test
priate safety, health, and environmental practices and deter-
method, refer to Terminology E135.
mine the applicability of regulatory limitations prior to use.
1.3 This international standard was developed in accor-
4. Summary of Test Method
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the 4.1 This test method is intended for use with commercially
Development of International Standards, Guides and Recom- available inert gas fusion determinators.
mendations issued by the World Trade Organization Technical
4.2 The test specimen is fused in a graphite crucible under
Barriers to Trade (TBT) Committee.
a flowing inert gas stream of argon (Ar), helium (He), or
nitrogen (N ) at a temperature sufficient to release oxygen.
2. Referenced Documents
Oxygen from the specimen combines with carbon from the
2.1 ASTM Standards:
crucible to form carbon monoxide (CO).The detector output is
E29 Practice for Using Significant Digits in Test Data to
converted to the mass fraction of oxygen in the specimen using
Determine Conformance with Specifications
a previously established calibration. Depending on the instru-
E50 Practices for Apparatus, Reagents, and Safety Consid-
ment design, CO is oxidized to carbon dioxide (CO ) or left as
erations for Chemical Analysis of Metals, Ores, and
CO and swept by the inert gas stream into an infrared detector.
Related Materials
4.3 In a typical instrument based on infrared detection the
E135 Terminology Relating to Analytical Chemistry for
evolved gases are swept into an infrared cell through which
Metals, Ores, and Related Materials
infrared energy is transmitted. The CO in the gas stream
E882 Guide for Accountability and Quality Control in the
absorbs some of the transmitted infrared energy and the
Chemical Analysis Laboratory
decrease in the energy reaching the detector is processed and
E1019 Test Methods for Determination of Carbon, Sulfur,
displayed directly as percent oxygen. Some instruments oxi-
Nitrogen, and Oxygen in Steel, Iron, Nickel, and Cobalt
dize the CO to CO , which is subsequently measured by an
Alloys by Various Combustion and Inert Gas Fusion
infrared cell designed to measure CO .
Techniques
E1601 Practice for Conducting an Interlaboratory Study to
5. Significance and Use
Evaluate the Performance of an Analytical Method
5.1 This test method is primarily intended as a referee test
forcompliancewithcompositionalspecifications.Itisassumed
This test method is under the jurisdiction of ASTM Committee E01 on
that all who use this test method will be trained analysts,
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
responsibility of Subcommittee E01.05 on Cu, Pb, Zn, Cd, Sn, Be, Precious Metals, capable of performing common laboratory procedures skill-
their Alloys, and Related Metals.
fully and safely. It is expected that work will be performed in
Current edition approved June 15, 2019. Published August 2019. Originally
a properly equipped laboratory.
approved in 2008. Last previous edition approved in 2008 as E2575–08, which was
withdrawn January 2017 and reinstated in June 2019. DOI: 10.1520/E2575-19.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 6. Interferences
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
6.1 The elements usually present in copper and its alloys do
Standards volume information, refer to the standard’s Document Summary page on
theASTM website. not interfere.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E2575 − 19
7. Apparatus 9. Hazards
7.1 Instrument—Fusion and measurement apparatus con- 9.1 For hazards to be observed in the use of certain reagents
sisting of an electrode furnace, provision for scrubbing impu-
in this test method refer to Practice E50.
ritiesfromanalyticalgasstream,infraredmeasurementsystem,
9.2 Use care when handling hot crucibles and operating
and auxiliary gas purification systems (see Note 1).
furnaces to avoid injury by either burn or electrical shock.
NOTE 1—Several models of commercial oxygen determinators are
available and presently in use by industry. Each has its own unique design
10. Sampling and Sample Preparation
characteristics and operational requirements. Consult the instrument
manufacturer’s manual for operational details.
10.1 Use only solid samples to minimize the potential for
7.2 Graphite Crucibles—The crucibles must be made of
errors due to surface oxidation. Samples must be of the proper
high-purity graphite as recommended by the instrument manu-
size to permit free introduction into the sample-loading device
facturer and be of the dimensions recommended by the
of the instrument. Sample mass range should be 0.5 g to 2.0 g.
instrument manufacturer.
Refer to instrument manufacturer’s recommendations.
7.3 Tweezers—, used to handle samples during the prepara-
10.2 Cut the sample to an appropriate size using a silicon
tion process.
carbide, water-cooled cut-off wheel or by other means that will
avoid overheating. Avoid oxide cutting or abrading materials.
7.4 Balance—Measurement apparatus with capacity up to
10 g capable of weighing 60.1 mg accurately or as specified
10.3 Etch sample with concentrated HCl at 20 °C for three
by the instrument manufacturer.
minutes.
10.4 Etch sample in the copper pickle solution at 70 °C for
8. Reagents and Materials
one minute.
8.1 Purity of Reagents—Reagent grade chemicals shall be
10.5 Rinse sample in three successive distilled water rinses.
used in all tests. Unless otherwise indicated, it is intended that
10.6 Rinse sample in three successive methanol rinses.
all reagents shall conform to the specifications of the Commit-
tee onAnalytical Reagents of theAmerican Chemical Society,
10.7 Dry in a stream of hot air (hair dryer).
where such specifications are available. Other grades may be
10.8 Do not touch sample with fingers during and following
used, provided it is first ascertained that the reagent is of
the final stages of cleaning. Store the prepared sample in a
sufficiently high purity to permit its use without lessening the
desiccator. If samples are not analyzed within four hours of
accuracy of the determination.
preparation, repeat 10.3 – 10.7 prior to analysis.
8.2 Graphite Powder/Carbon Black—High-purity graphite
10.9 Careful adherence to the sample preparation procedure
powder or carbon black specified by the instrument manufac-
described above is critical to obtaining accurate and unbiased
turer.
results. The use of small and irregular shaped samples requires
8.3 Inert Gas—Use the purity and type (Ar, He, or N )
a diligent effort to ensure that all surface contamination has
specified by the instrument manufacturer.
been removed.
8.4 Magnesium Perchlorate (Mg(ClO ) )—Anhydrous—
4 2
Used as a moisture trap. Use purity specified by the instrument 11. Preparation of Apparatus
manufacturer.
11.1 Assemble the apparatus as recommended by the manu-
8.5 Rare Earth/Copper Oxide—Reagent used in some in- facturer. Make the required power, gas, and water connections.
struments to oxidize CO to CO . Use purity specified by the Turnontheinstrumentandallowsufficienttimetostabilizethe
instrument manufacturer. system.
8.6 Sodium Hydroxide Impregnated Clay—Used to absorb
11.2 Change the chemical reagents and filters as required.
CO in the inert gas stream. Use purity specified by the Testthefurnaceandtheanalyzertoinsuretheabsenceofleaks.
instrument manufacturer.
Make a minimum of two determinations using a sample as
directed in Section 13 to condition the instrument before
8.7 Methanol—Used in sample preparation, see Section 10.
attempting to calibrate the system or to determine the value of
8.8 Copper Pickle Solution—Prepare a fresh solution of
the blank.
equalpartsofconcentratedHNO ,concentratedCH OOH,and
3 3
11.3 Calibrate the balance as recommended by the manu-
concentrated H PO . Used in sample preparation, see Section
3 4
facturerusinginternalorexternalcalibrationtraceabletotheSI
10.
(see IEEE/ASTM SI 10).
8.9 Hydrochloric Acid (HCl)—Used in sample preparation,
see Section 10.
12. Calibration
12.1 Calibration Reference Materials Use only copper or
copper alloy reference materials. Select four reference materi-
“Reagent Chemicals, American Chemical Society Specifications,” American
als containing approximately 0.0004 %, 0.01 %, 0.03 %, and
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
0.06 % oxygen and designate them as A, B, C, and D
listed by the American Chemical Society, see the United States Pharmacopeia and
National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD. respectively.
E2575 − 19
12.1.1 The oxygen content of the materials selected must
t.975 = student’s t chosen for
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