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ASTM E3346-22

(Guide)

Standard Guide for Combustion, Inert Gas Fusion and Hot Extraction Instruments for use in Analyzing Metals, Ores, and Related Materials

Standard Guide for Combustion, Inert Gas Fusion and Hot Extraction Instruments for use in Analyzing Metals, Ores, and Related Materials

SIGNIFICANCE AND USE
5.1 The chemical measurement processes covered by this guide are used for determination of Carbon, Sulfur, Nitrogen, Oxygen and Hydrogen in metals, ores and related materials. A test method utilizing this guidance is used to test such materials, and also form the basis for quality assurance of these materials. Thus, it is economically and scientifically critical that these instruments be understood by the laboratories that use them.  
5.2 It is assumed that all who use this guide will be trained analysts, capable of performing common laboratory procedures skillfully, and safely. It is expected that any work will be performed in a properly equipped laboratory.  
5.3 It is expected that the laboratory will prepare their own work procedures for any of the information described in this guide.  
5.4 This guide contains numerous references to “manufacturer’s recommendations”. The user of this guide is expected to refer to the instrument operation manual for the specific instrument being used or consult directly with the manufacturer to obtain instructions or recommendations.  
5.5 This guide stresses the conservation of certified reference materials (CRMs). CRMs should not be used for drift checks or conditioning measurments. Other materials should be developed and used for these operations.
SCOPE
1.1 This guide covers information for using Combustion, Inert Gas Fusion and Hot Extraction instruments to determine the mass fraction of the non-metallic elements Carbon, Sulfur, Nitrogen, Oxygen and Hydrogen in metals, ores and related materials.  
1.2 This guide does not specify all the operating conditions because of the differences among different manufacturer’s instruments. Laboratories should follow instructions provided by the manufacturer of the instrument.  
1.3 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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.  
1.5 The information in this guide is contained in the sections indicated as follows:    
Sections  
Carbon/Sulfur by Combustion/Infrared Detection  
14 – 19  
Nitrogen/Oxygen by Inert Gas Fusion/Thermal Conductivity and Infrared Detection  
20 – 25  
Hydrogen by Inert Gas Fusion Instrumental Measurement and Hot Extraction/Various Detection Cell Technology  
26 – 31  
1.6 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
30-Nov-2022
ICS
77.040.30 - Chemical analysis of metals
Technical Committee
E01 - Analytical Chemistry for Metals, Ores, and Related Materials
Drafting Committee
E01.20 - Fundamental Practices
Current Stage
Ref Project

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ASTM E3346-22 - Standard Guide for Combustion, Inert Gas Fusion and Hot Extraction Instruments for use in Analyzing Metals, Ores, and Related MaterialsASTM E3346-22 - Standard Guide for Combustion, Inert Gas Fusion and Hot Extraction Instruments for use in Analyzing Metals, Ores, and Related Materials
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ASTM E3346-22 - Standard Guide for Combustion, Inert Gas Fusion and Hot Extraction Instruments for use in Analyzing Metals, Ores, and Related Materials
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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: E3346 − 22
Standard Guide for
Combustion, Inert Gas Fusion and Hot Extraction
Instruments for use in Analyzing Metals, Ores, and Related
1
Materials
This standard is issued under the fixed designation E3346; 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 mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
1.1 This guide covers information for using Combustion,
Inert Gas Fusion and Hot Extraction instruments to determine
2. Referenced Documents
the mass fraction of the non-metallic elements Carbon, Sulfur,
2
2.1 ASTM Standards:
Nitrogen, Oxygen and Hydrogen in metals, ores and related
E50 Practices for Apparatus, Reagents, and Safety Consid-
materials.
erations for Chemical Analysis of Metals, Ores, and
1.2 This guide does not specify all the operating conditions
Related Materials
because of the differences among different manufacturer’s
E55 Practice for Sampling Wrought Nonferrous Metals and
instruments. Laboratories should follow instructions provided
Alloys for Determination of Chemical Composition
by the manufacturer of the instrument.
E88 Practice for Sampling Nonferrous Metals andAlloys in
Cast Form for Determination of Chemical Composition
1.3 Units—The values stated in SI units are to be regarded
E135 Terminology Relating to Analytical Chemistry for
as standard. No other units of measurement are included in this
Metals, Ores, and Related Materials
standard.
E882 Guide for Accountability and Quality Control in the
1.4 This standard does not purport to address all of the
Chemical Analysis Laboratory
safety concerns, if any, associated with its use. It is the
E1329 Practice for Verification and Use of Control Charts in
responsibility of the user of this standard to establish appro-
3
Spectrochemical Analysis (Withdrawn 2019)
priate safety, health, and environmental practices and deter-
E1806 Practice for Sampling Steel and Iron for Determina-
mine the applicability of regulatory limitations prior to use.
tion of Chemical Composition
1.5 Theinformationinthisguideiscontainedinthesections
E2857 Guide for Validating Analytical Methods
indicated as follows:
E2972 Guide for Production, Testing, and ValueAssignment
Sections
of In-House Reference Materials for Metals, Ores, and
Carbon/Sulfur by Combustion/Infrared Detection 14–19
Other Related Materials
Nitrogen/Oxygen by Inert Gas Fusion/Thermal Conductivity and Infra- 20–25
red Detection
G93 GuideforCleanlinessLevelsandCleaningMethodsfor
Hydrogen by Inert Gas Fusion Instrumental Measurement and Hot 26–31
Materials and Equipment Used in Oxygen-Enriched En-
Extraction/Various Detection Cell Technology
vironments
1.6 This international standard was developed in accor-
dance with internationally recognized principles on standard-
3. Terminology
ization established in the Decision on Principles for the
3.1 Definitions: For definition of terms used in this guide,
Development of International Standards, Guides and Recom-
refer to Terminology E135.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
1
This test method is under the jurisdiction of ASTM Committee E01 on contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct Standards volume information, refer to the standard’s Document Summary page on
responsibility of Subcommittee E01.20 on Fundamental Practices. the ASTM website.
3
Current edition approved Dec. 1, 2022. Published January 2023. DOI: 10.1520/ The last approved version of this historical standard is referenced on
E3346-22. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
E3346 − 22
4. Summary of Guide the specifications of the Committee on Analytical Reagents of
the American Chemical Society where such specifications are
4.1 This guide provides information assisting users to prop-
4
available. Other grades may be used, provided it is first
erly understand and utilize the various specimen decomposi-
ascertained that the reagent is of sufficiently high purity to
tion and element detection techniques to determine the non-
permit its use without lessening the accuracy of the determi-
metallic elements Carbon, Sulfur, Nitrogen, Oxygen, and
nation.
Hydrogen. The instruments descri
...

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4.1 These test methods for the chemical analysis of beryllium metal are primarily intended as referee methods to test such materials for compliance with compositional specifications. It is assumed that all who use these test methods 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.
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1.1 These test methods cover the chemical analysis of beryllium having chemical compositions within the following limits:    
Element  
Range, %  
Aluminum  
0.05 to 0.30  
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97.5 to 100    
Beryllium Oxide  
0.3 to 3    
Carbon  
0.05 to 0.30  
Copper  
0.005 to 0.10  
Chromium  
0.005 to 0.10  
Iron  
0.05 to 0.30  
Magnesium  
0.02 to 0.15  
Nickel  
0.005 to 0.10  
Silicon  
0.02 to 0.15  
1.2 The test methods in this standard are contained in the sections as follows.    
Sections  
Chromium by the Diphenylcarbazide Spectrophotometric Test Method
[0.004 % to 0.04 %]  
10 – 19  
Iron by the 1,10-Phenanthroline Spectrophotometric Test Method
[0.05 % to 0.25 %]  
20 – 29  
Manganese by the Periodate Spectrophotometric Test Method
[0.008 % to 0.04 %]  
30 – 39  
Nickel by the Dimethylglyoxime Spectrophotometric Test Method
[0.001 % to 0.04 %]  
40 – 49  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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.  
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ASTM E363-23(Test Method)
Standard Test Methods for Chemical Analysis of Chromium and Ferrochromium

SIGNIFICANCE AND USE
4.1 These test methods for the chemical analysis of chromium metal and ferrochromium alloy are primarily intended to test such materials for compliance with compositional specifications such as Specifications A101 and A481. It is assumed that all who use these test methods 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.
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1.1 These test methods cover the chemical analysis of chromium and ferrochromium having chemical compositions within the following limits:    
Element  
Composition, %  
Aluminum  
0.25 max  
Antimony  
0.005 max  
Arsenic  
0.005 max  
Bismuth  
0.005 max  
Boron  
0.005 max  
Carbon  
9.00 max  
Chromium  
51.0 to 99.5  
Cobalt  
0.10 max  
Columbium  
0.05 max  
Copper  
0.05 max  
Lead  
0.005 max  
Manganese  
0.75 max  
Molybdenum  
0.05 max  
Nickel  
0.50 max  
Nitrogen  
6.00 max  
Phosphorus  
0.03 max  
Silicon  
12.00 max  
Silver  
0.005 max  
Sulfur  
0.07 max  
Tantalum  
0.05 max  
Tin  
0.005 max  
Titanium  
0.50 max  
Vanadium  
0.50 max  
Zinc  
0.005 max  
Zirconium  
0.05 max  
1.2 The analytical procedures appear in the following order:    
Sections  
Arsenic by the Molybdenum Blue Spectrophotometric Test Method
[0.001 % to 0.005 %]  
10 – 20  
Lead by the Dithizone Spectrophotometric Test Method
[0.001 % to 0.05 %]  
21 – 31  
Chromium by the Sodium Peroxide Fusion-Titrimetric Test Method
[50.0 % to 99.5 %]  
32 – 38  
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ASTM E2824-23(Test Method)
Standard Test Method for Determination of Beryllium in Copper-Beryllium Alloys by Phosphate Gravimetry

SIGNIFICANCE AND USE
5.1 This test method for the chemical analysis of metals and alloys is primarily intended to test such materials for compliance with compositional specifications. It is assumed that all who use these test methods 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 describes the determination of beryllium in copper-beryllium alloys in percentages from 0.1 % to 3.0 % by phosphate gravimetry.  
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ASTM E55-23(Practice)
Standard Practice for Sampling Wrought Nonferrous Metals and Alloys for Determination of Chemical Composition

ABSTRACT
This practice covers the sampling, for the determination of chemical composition of nonferrous metals and alloys that have been reduced to their final form by mechanical working; that is, by such means as rolling, drawing, and extruding. The portion selection, sample preparation, sampling details, sample size and storage, and resampling are also detailed.
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1.1.1 Refer to Practice E255 for copper and copper alloys.  
Note 1: The selection of correct portions of material and the preparation of a representative sample from such portions are necessary prerequisites to every analysis, the analysis being of no value unless the sample actually represents the average composition of the material from which it was selected.  
1.2 In special cases, when agreed upon by the purchaser and the manufacturer, the heat analysis may be accepted as representative of the composition of the finished product. In such cases, the identity of each heat of metal should be maintained through each stage of the manufacturing process to the final form. This method of sampling is not intended to apply under these conditions.  
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.  
1.4 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.  
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ASTM E255-23(Practice)
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4.1 This practice is intended primarily for the sampling of copper and copper alloys for compliance with compositional specification requirements.  
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1.4 This practice is not intended to supersede or replace existing specification requirements for the sampling of a particular material.  
1.5 The values stated in SI units are to be regarded as standard. The values in parentheses are given for information only.  
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5.1 This test method for the chemical analysis of metals and alloys is primarily intended to test such materials for compliance with compositional specifications. It is assumed that all those 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.
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Element  
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3.0–8.0  
Antimony  
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0.05 max  
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0.015 max  
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0.002 max  
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0.02 max  
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0.02 max  
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1.3 Included are procedures for elements in the following composition ranges:    
Element  
Composition Range, %  
Aluminum  
3.0–8.0  
Cadmium  
0.0016–0.025  
Cerium  
0.005–0.10  
Iron  
0.0015–0.10  
Lanthanum  
0.009–0.10  
Lead  
0.002–0.026  
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ASTM E1085-22(Test Method)
Standard Test Method for Analysis of Low-Alloy Steels by Wavelength Dispersive X-Ray Fluorescence Spectrometry

SIGNIFICANCE AND USE
5.1 This test method is suitable for manufacturing control and for verifying that a product meets specifications. This test method provides rapid, multi-element determinations with sufficient accuracy to ensure product quality and to minimize production delays. The analytical performance data may be used as a benchmark to determine if similar X-ray spectrometers provide equivalent precision and accuracy, or if the performance of a particular X-ray spectrometer has changed.  
5.2 Calcium is sometimes added to steel to affect inclusion shape which enhances certain mechanical properties of steel. This test method is useful for determining the residual calcium in the steel after such treatment.  
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1.1 This test method covers the wavelength dispersive X-ray fluorescence analysis of low-alloy steels for the following elements:    
Element  
Mass Fraction
Range, %  
Calcium  
0.001 to 0.007  
Chromium  
0.04 to 2.5  
Cobalt  
0.03 to 0.2  
Copper  
0.03 to 0.6  
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0.04 to 2.5  
Molybdenum  
0.005 to 1.5  
Nickel  
0.04 to 3.0  
Niobium  
0.002 to 0.1  
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0.010 to 0.08  
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0.06 to 1.5  
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0.009 to 0.1  
Vanadium  
0.012 to 0.6  
1.1.1 Unless exceptions are noted, mass fraction ranges can be extended and additional elements can be included by the use of suitable reference materials and measurement conditions. Deviations from the published scope must be validated by experimental means. See Guide E2857 for information on validation options.  
1.2 The values stated in the International System of Units (SI) are to be regarded as standard. The values given in parentheses are mathematical conversions to other units that are provided for information only, because they may be used in older software and laboratory procedures.  
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ASTM E2209-22(Test Method)
Standard Test Method for Analysis of High Manganese Steel by Spark Atomic Emission Spectrometry

SIGNIFICANCE AND USE
5.1 The chemical composition of high manganese steel alloys must be determined accurately to ensure the desired metallurgical properties. This procedure is suitable for manufacturing control and inspection testing.
SCOPE
1.1 This test method covers the analysis of high manganese steel by spark atomic emission spectrometry for the following elements in the ranges shown:    
Elements  
Composition Range, %  
Aluminum (Al)  
0.02 to 0.15  
Carbon (C)  
0.3 to 1.4  
Chromium (Cr)  
0.25 to 2.00  
Manganese (Mn)  
8.0 to 16.2  
Molybdenum (Mo)  
0.03 to 2.0  
Nickel (Ni)  
0.05 to 4.0  
Phosphorus (P)  
0.025 to 0.06  
Silicon (Si)  
0.25 to 1.5
Note 1: The ranges represent the actual levels at which this method was tested.2 These composition ranges can be extended by the use of suitable reference materials. Validation of these extensions may be conducted by following Practice E2587. Sulfur is not included because differences in results between laboratories exceeded acceptable limits at all sulfur levels.  
1.2 This test method may involve hazardous materials, operations, and equipment. 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.

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ASTM E1086-22(Test Method)
Standard Test Method for Analysis of Austenitic Stainless Steel by Spark Atomic Emission Spectrometry

SIGNIFICANCE AND USE
5.1 The chemical composition of stainless steels must be determined accurately to ensure the desired metallurgical properties. This test method is suitable for manufacturing control and inspection testing.
SCOPE
1.1 This test method2 covers the analysis of austenitic stainless steel by spark atomic emission spectrometry for the following elements in the ranges shown    
Element  
Composition Range, %  
Chromium  
17.0 to 23.0  
Nickel  
7.5 to 13.0  
Molybdenum  
0.01 to 3.0    
Manganese  
0.01 to 2.0    
Silicon  
0.01 to 0.90  
Copper  
0.01 to 0.30  
Carbon  
0.005 to 0.25  
Phosphorus  
0.003 to 0.15  
Sulfur  
0.003 to 0.065  
1.2 This test method is designed for the analysis of chill-cast disks or inspection testing of stainless steel samples that have a flat surface of at least 13 mm (0.5 in.) in diameter. The samples must be sufficiently massive to prevent overheating during the discharge and of a similar metallurgical condition and composition as the reference materials.  
1.3 One or more of the reference materials must closely approximate the composition of the specimen. The technique of analyzing reference materials with unknowns and performing the indicated mathematical corrections (typically referred to as type standardization) may also be used to correct for interference effects and to compensate for errors resulting from instrument drift. A variety of such systems are commonly used. Any of these that will achieve analytical accuracy equivalent to that reported for this test method are acceptable.  
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ASTM E581-17A(2022)e1(Test Method)
Standard Test Methods for Chemical Analysis of Manganese-Copper Alloys

SIGNIFICANCE AND USE
4.1 These test methods for the chemical analysis of metals and alloys are primarily intended to test such materials for compliance with compositional specifications. It is assumed that all who use these test methods 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 These test methods cover the chemical analysis of manganese-copper alloys having chemical compositions within the following limits:    
Element  
Range, %  
Copper  
68.0 to 72.0  
Manganese  
28.0 to 32.0  
Carbon  
0.03 max  
Iron  
0.01 max  
Phosphorus  
0.01 max  
Silicon  
0.05 max  
Sulfur  
0.01 max  
1.2 The test methods appear in the following order:    
Sections  
Iron by the 1,10-Phenanthroline
Spectrophotometric Method
[0.003 % to 0.02 %]  
11 – 20  
Manganese by the (Ethylenedinitrilo)
Tetraacetic Acid (EDTA)—
Back-Titrimetric Method [28 % to 32 %]  
21 – 27  
Phosphorus by the
Molybdivanadophosphoric Acid
Extraction Spectrophotometric Method
[0.002 % to 0.014 %]  
28 – 38  
1.3 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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.  
1.5 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.

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