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: E1019 − 24

Standard Test Methods for

Determination of Carbon, Sulfur, Nitrogen, and Oxygen in
Steel, Iron, Nickel, and Cobalt Alloys by Combustion and
Inert Gas Fusion Techniques1
This standard is issued under the fixed designation E1019; 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.

This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope Sections
Carbon and Sulfur by Combustion 10 – 19
1.1 These test methods cover the determination of carbon,
sulfur, nitrogen, and oxygen, in steel, iron, nickel, and cobalt Nitrogen by the Inert Gas Fusion and Thermal Conduc- 20 – 30
alloys having chemical compositions within the following tivity Detection Test Method

limits: Oxygen by the Inert Gas Fusion and Infrared Absorp- 31 – 42

Element Mass Fraction Range, % tion or Thermal Conductivity Detection Test Method
Aluminum 0.001 to 18.00 1.3 The values stated in SI units are to be regarded as
Antimony 0.002 to 0.03
Arsenic 0.0005 to 0.10 standard. No other units of measurement are included in this
Beryllium 0.001 to 0.05 standard.
Bismuth 0.001 to 0.50
Boron 0.0005 to 1.00 1.4 This standard does not purport to address all of the
Cadmium 0.001 to 0.005 safety concerns, if any, associated with its use. It is the
Calcium 0.001 to 0.05 responsibility of the user of this standard to establish appro-
Carbon 0.001 to 9.50
Cerium 0.005 to 0.05 priate safety, health, and environmental practices and deter-
Chromium 0.005 to 35.00 mine the applicability of regulatory limitations prior to use.
Cobalt 0.01 to 75.0 Specific hazards statements are given in Section 6.
Niobium 0.002 to 6.00
Copper 0.005 to 10.00 1.5 This international standard was developed in accor-
Hydrogen 0.0001 to 0.0030 dance with internationally recognized principles on standard-
Iron 0.01 to 100.0 ization established in the Decision on Principles for the
Lead 0.001 to 0.50
Magnesium 0.001 to 0.05 Development of International Standards, Guides and Recom-
Manganese 0.01 to 20.0 mendations issued by the World Trade Organization Technical
Molybdenum 0.002 to 30.00
Barriers to Trade (TBT) Committee.
Nickel 0.005 to 84.00
Nitrogen 0.0005 to 0.50
Oxygen 0.0005 to 0.03 2. Referenced Documents
Phosphorus 0.001 to 0.90
Selenium 0.001 to 0.50 2.1 ASTM Standards:2
Silicon 0.001 to 6.00 D1193 Specification for Reagent Water
Sulfur 0.001 to 0.45
E29 Practice for Using Significant Digits in Test Data to
Tantalum 0.001 to 10.00
Tellurium 0.001 to 0.35 Determine Conformance with Specifications
Tin 0.002 to 0.35 E50 Practices for Apparatus, Reagents, and Safety Consid-
Titanium 0.002 to 5.00
Tungsten 0.005 to 21.00
erations for Chemical Analysis of Metals, Ores, and
Vanadium 0.005 to 5.50 Related Materials
Zinc 0.005 to 0.20 E55 Practice for Sampling Wrought Nonferrous Metals and
Zirconium 0.005 to 2.500
Alloys for Determination of Chemical Composition
1.2 The test methods appear in the following order: E88 Practice for Sampling Nonferrous Metals and Alloys in
Cast Form for Determination of Chemical Composition
1
These test methods are under the jurisdiction of ASTM Committee E01 on
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct
2
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved July 1, 2024. Published August 2024. Originally contact ASTM Customer Service at www.astm.org/contact. For Annual Book of
approved in 1984. Last previous edition approved in 2018 as E1019 – 18. DOI: ASTM Standards volume information, refer to the standard’s Document Summary
10.1520/E1019-24. page on the ASTM website.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

1
 E1019 − 24
E135 Terminology Relating to Analytical Chemistry for 6.2 Use care when handling hot crucibles and operating
Metals, Ores, and Related Materials electrical equipment to avoid personal injury by either burn or
E173 Practice for Conducting Interlaboratory Studies of electrical shock.
Methods for Chemical Analysis of Metals (Withdrawn
1997)3 7. Sampling
E177 Practice for Use of the Terms Precision and Bias in 7.1 Refer to Practices E55, E88 or E1806 for suggested
ASTM Test Methods sampling procedures.
E691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method 8. Rounding Calculated Values
E1806 Practice for Sampling Steel and Iron for Determina- 8.1 Rounding of test results obtained using these test meth-
tion of Chemical Composition ods shall be performed as directed in Practice E29, Rounding
E2857 Guide for Validating Analytical Methods Method, unless an alternative rounding method is specified by
2.2 ASTM Manuals:2 the customer or applicable material specification.
MNL7 Presentation of Data and Control Chart Analysis, 9th
Edition 9. Interlaboratory Studies
9.1 The test methods for carbon and sulfur have been
3. Terminology
evaluated in accordance with Practice E691. The test methods
3.1 For definition of terms used in this test method, refer to for nitrogen and oxygen have been evaluated in accordance
Terminology E135. with Practice E173. The Reproducibility R2 of Practice E173
corresponds to the Reproducibility Index R of Practice E691.
4. Significance and Use
The Repeatability R1 of Practice E173 corresponds to the
4.1 This test method is intended for the testing of iron, steel, Repeatability Index r of Practice E691.
cobalt, and nickel alloys to verify compliance with composi-
tional specifications such as those issued by Committees A01
and B02. It is assumed that all who use this test method will be CARBON AND SULFUR BY COMBUSTION
trained analysts capable of performing common laboratory
10. Scope
procedures skillfully and safely. It is expected that the work
will be performed in a properly equipped laboratory. 10.1 This test method applies to the determination of carbon
and sulfur in iron, steel, nickel, and cobalt alloys in mass
4.2 Laboratories using this method shall prepare work
fractions from 0.002 % to 9.50 % for carbon and 0.001 % to
procedures documenting how the test method is to be imple-
0.45 % for sulfur.
mented in their specific laboratory operation.
10.2 This method has been interlaboratory tested for the
4.3 This test method contains numerous references to
quantification ranges specified in 10.1. The ranges in 10.1
“manufacturer’s recommendations”. When this statement is
indicate intervals within which results have been demonstrated
used, the user of this method is expected to refer to the
by interlaboratory study to be quantitative. It may be possible
instrument operation manual for the specific instrument being
to extend this method to different ranges provided that a
used or consult directly with the manufacturer to determine
method validation study is performed and that the results of
recommendations.
this study show that the method extension is meeting labora-
5. Apparatus and Reagents tory data quality objectives. Guide E2857 provides information
on how to perform method validation studies. The laboratory
5.1 Apparatus and reagents required for each determination may use other documented validation methods.
are listed in separate sections preceding the procedure.
10.3 This standard does not purport to address all of the
5.2 The methods for nitrogen and oxygen were originally safety concerns, if any, associated with its use. It is the
developed for older technology, using manual instrumentation, responsibility of the user of this standard to establish appro-
with the flow schematics indicated. Current commercially priate safety, health, and environmental practices and deter-
available instruments are more automated and may have mine the applicability of regulatory limitations prior to use.
slightly different flow schematics and should be capable of For specific precautionary statements, see Section 6.
producing data meeting or exceeding the precision and bias
requirements. 11. Interferences
5.3 The method for carbon and sulfur was developed using 11.1 The elements ordinarily present in iron, steel, nickel,
current commercially available instruments. and cobalt alloys do not interfere.
6. Hazards 12. Apparatus
6.1 For hazards to be observed in the use of certain reagents 12.1 Combustion and Measurement Apparatus—Automatic
in this test method, refer to Practices E50. elemental analyzer, capable of determining carbon only or
carbon and sulfur, combined.
3
The last approved version of this historical standard is referenced on 12.1.1 The analyzer will consist of an induction furnace,
www.astm.org. analytical gas stream impurity removal, catalyzing systems,

2
 E1019 − 24
auxiliary purification systems (if required by the for carbon or sulfur or both, containing analyte mass fractions
manufacturer), and an infrared absorption detection system. adequate to calibrate for the expected range of carbon or sulfur
Several models of commercial elemental analyzers are avail- or both in the laboratory’s expected analytical range.
able and presently used in industry. Each has its own unique 13.4 Gas Purification Reagents—Composition, form and
design characteristics and operational requirements. Consult purity are typically specified by the instrument manufacturer.
the instrument manufacturer’s instructions for operational The reagents used may vary somewhat from analyzer to
details. analyzer.
12.2 Ceramic Crucibles—Use the crucible design(s) recom- 13.4.1 Sulfur Trioxide Absorber—Cellulose has been used
mended by the instrument manufacturer. Some crucible de- for this purpose.
signs may have lids fitted to the crucible which help minimize 13.4.2 Water Absorber—Magnesium perchlorate or phos-
or prevent spattering associated with vigorous combustion. The phorous pentoxide have been used for this purpose.
most commonly analyzed iron, steel, cobalt, or nickel- based 13.4.3 CO2 Absorber—Sodium hydroxide on clay has been
materials will not require the use of lids. The lab should used for this purpose.
evaluate the necessity of lid use during the method develop- 13.5 Gas Conversion Reagents—Composition, form and
ment trials described in Section 14. purity are typically specified by the instrument manufacturer.
12.2.1 New crucibles may be contaminated with small The reagents used may vary somewhat from analyzer to
amounts of carbon or sulfur or both and should be conditioned analyzer.
prior to use by heating in a suitable furnace for not less than 13.5.1 CO to CO2 Converter—Platinum or platinized silica
40 min at 1000 °C or not less than 15 min at 1250 °C and have been used for this purpose.
allowed to safely cool. Exact timing of the crucible heating 13.5.2 Hydrogen/Hydrocarbon Contaminant Converter—
cycle is not required. The conditioned crucibles shall only be Rare earth copper oxide has been used for this purpose.
handled with tongs and may be stored in a covered container
for up to four hours prior to use. Crucibles not used within four 13.6 Combustion/Carrier Gas-Oxygen—Purity as specified
hours may be re-conditioned and used for analysis. Exact by the instrument manufacturer.
timing of the crucible standing time is not required.
Alternatively, the laboratory may use a different combination 14. Preparation of Apparatus
of time and temperature parameters for conditioning provided 14.1 Analytical instrumentation shall be installed following
the precision and bias demonstrated meet the laboratory’s the manufacturer’s recommendations.
quality objectives. If lids are used these should be conditioned 14.1.1 For implementation of this test method on existing
using the same heating conditions used for crucibles. equipment that is currently producing analyses which meet
12.2.2 Conditioning may not be necessary if the carbon and laboratory data quality objectives, the performance of steps
sulfur contents of the unconditioned crucibles are insignificant 14.2 – 14.5 may be unnecessary and is, therefore, non-
to the required measurement quality. It is incumbent upon mandatory. For newly installed equipment, steps 14.2 – 14.5
laboratories choosing not to condition crucibles to assess the shall be performed.
impact to laboratory measurement quality objectives. Compar-
14.2 Using the instrument software, set up an analytical
ing results obtained using unconditioned crucibles to the data
protocol with measurement parameters. Instrument manufac-
presented in the Precision and Bias tables of this method may
turers typically provide application notes with suggested pa-
provide an objective evaluation of the impact to the measure-
rameters. Refer to these application notes as a starting point for
ment results. This method was tested using conditioned cru-
method development. Parameters that are typically specified
cibles; therefore, laboratories that do not condition crucibles
are as follows:
may not be able to demonstrate repeatability and bias similar to
14.2.1 Instrument Measurement Parameters:
that presented in the Precision and Bias tables.
14.2.1.1 Gas Flow—This may be fixed by the design of the
12.2.3 Crucibles should be stored in a dry environment.
equipment.
12.3 Crucible Tongs—Capable of handling recommended 14.2.1.2 Purge Time—Use of inadequate purge time may
crucibles. adversely affect the analysis precision of low mass fraction
13. Reagents and Materials content specimens.
14.2.1.3 Measurement times (integration time(s), delay
13.1 Accelerators—These will typically be copper,
time(s)).
tungsten, iron, tin, or a mixture of these metals. Composition,
14.2.1.4 Furnace parameters (furnace power, power ramp
form and purity are typically recommended by the instrument
protocol).
manufacturer. The exact composition to be used will be
14.2.1.5 Calibration and specimen analysis may only be
determined per Section 14.
made on materials with analyte mass fractions falling into the
13.2 Acetone—Used for sample drying and decontamina- instrument manufacturer defined linear range of the equipment.
tion. The laboratory should determine the quality of acetone Therefore, only calibration protocols using first order line fits
necessary to meet data quality objectives. A.C.S. reagent grade may be used with this test method. Select a calibration protocol
acetone has been found to produce acceptable results. from either (1) or (2) while giving consideration to (3) and (4).
13.3 Calibration Reference Materials—Iron, steel, nickel or (1) Single Point Calibration—A calibration line is deter-
cobalt alloys with reference values and uncertainty estimates mined using a blank or blank adjusted origin and a high content