ASTM C816-15

Standard Test Method for Sulfur Content in Graphite by Combustion-Iodometric Titration Method

SIGNIFICANCE AND USE
5.1 Sulfur, even in very low concentrations, is of concern in a nuclear reactor because of potential corrosion of metallic components. This test method has the sensitivity to analyze very low sulfur contents in graphite using very small samples.  
5.2 This test method can be used to characterize graphite for design purposes.
SCOPE
1.1 This test method covers the determination of sulfur in graphite in the concentration range from 1 μg/g to 1000 μg/g (ppm).  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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.

General Information

• Status: Historical
• Publication Date: 30-Nov-2015
• ICS: 71.060.10 - Chemical elements
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.F0 - Manufactured Carbon and Graphite Products

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: C816 − 15
Standard Test Method for
Sulfur Content in Graphite by Combustion-Iodometric
1
Titration Method
This standard is issued under the fixed designation C816; 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* 3.1.3 titration, n—quantitative chemical analysis method
used to determine the unknown concentration of a specified
1.1 This test method covers the determination of sulfur in
element by reacting a solution prepared from the sample to be
graphite in the concentration range from 1 µg⁄g to 1000 µg⁄g
analyzed with a known concentration and volume of specific
(ppm).
reagent.
1.2 The values stated in SI units are to be regarded as
4. Summary of Test Method
standard. No other units of measurement are included in this
standard.
4.1 The sample is combusted with pure oxygen in a high-
temperature furnace and a major portion of the sulfur is
1.3 This standard does not purport to address all of the
converted to sulfur dioxide. The sulfur dioxide is passed
safety concerns, if any, associated with its use. It is the
through a potassium iodide-starch solution where it is titrated
responsibility of the user of this standard to establish appro-
with potassium iodate solution. The potassium iodate solution
priate safety and health practices and determine the applica-
is standardized against samples of known sulfur content.
bility of regulatory limitations prior to use.
5. Significance and Use
2. Referenced Documents
5.1 Sulfur, even in very low concentrations, is of concern in
2
2.1 ASTM Standards:
a nuclear reactor because of potential corrosion of metallic
D3177 Test Methods forTotal Sulfur in theAnalysis Sample
components. This test method has the sensitivity to analyze
3
of Coal and Coke (Withdrawn 2012)
very low sulfur contents in graphite using very small samples.
E50 Practices for Apparatus, Reagents, and Safety Consid-
5.2 This test method can be used to characterize graphite for
erations for Chemical Analysis of Metals, Ores, and
design purposes.
Related Materials
6. Interferences
3. Terminology
6.1 Any substance that releases volatile material, which
3.1 Definitions:
tends to enhance or to bleach the starch-iodine complex, will
3.1.1 combustion, n—chemical reaction by which graphite
interfere. Halogens and oxides of nitrogen interfere through
is combined in a controlled manner with pure oxygen in a high
darkening the color of the starch-iodine complex. Ultraviolet
temperature furnace for analytical purposes.
light will also darken the solution. A tube packed with either
silver wool or antimony filings placed in the line between the
3.1.2 sulfur content, n—percentage content by weight of
furnace and titration assembly will remove halogens from the
elemental sulfur present in graphite.
gas stream.
6.2 If the solution in the titration vessel becomes colorless
1
This test method is under the jurisdiction of ASTM Committee D02 on during the titration, some SO will be lost and a low result will
2
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
be obtained for the sulfur content.
Subcommittee D02.F0 on Manufactured Carbon and Graphite Products.
Current edition approved Dec. 1, 2015. Published January 2016. Originally
7. Apparatus
ɛ1
approved in 1977. Last previous edition approved in 2010 as C816 – 85 (2010) .
7.1 Apparatus for the determination of sulfur by direct
DOI: 10.1520/C0816-15.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
combustion shall be in accordance with Practices E50.
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
8. Reagents and Materials
the ASTM website.
3
8.1 Potassium Iodate Solution (0.2 mM)—Dissolve 44.4 mg
The last approved version of this historical standard is referenced on
www.astm.org. of potassium iodate (KIO ) in water and dilute to 1 L.
3
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
C816 − 15
NOTE 1—The sulfur equivalent for the KIO solution is based on the
9.9 Replace the stopper sending the flow of oxygen through
3
following reactions:
the combustion tube.
KIO 15KI16HCl 53I 16KCl13H O
3 2 2 9.10 Titrate the solution with the KIO solution to maintain
3
SO 1I 12H O 5 H SO 12HI
2 2 2 2 4
the blue color develop
...

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.
´1
Designation: C816 − 85 (Reapproved 2010) C816 − 15 An American National Standard
Standard Test Method for
Sulfur Content in Graphite by Combustion-Iodometric
1
Titration Method
This standard is issued under the fixed designation C816; 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
ε NOTE—Removed source of supply footnote and updated units of measurement throughout the standard editorially in
May 2010.
1. Scope Scope*
1.1 This test method covers the determination of sulfur in graphite in the concentration range from 11 μg ⁄g to 10001000 μg ⁄
μg/g g (ppm).
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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.
2. Referenced Documents
2
2.1 ASTM Standards:
3
D3177 Test Methods for Total Sulfur in the Analysis Sample of Coal and Coke (Withdrawn 2012)
E50 Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
3. Terminology
3.1 Definitions:
3.1.1 combustion, n—chemical reaction by which graphite is combined in a controlled manner with pure oxygen in a high
temperature furnace for analytical purposes.
3.1.2 sulfur content, n—percentage content by weight of elemental sulfur present in graphite.
3.1.3 titration, n—quantitative chemical analysis method used to determine the unknown concentration of a specified element
by reacting a solution prepared from the sample to be analyzed with a known concentration and volume of specific reagent.
4. Summary of Test Method
4.1 The sample is burned in oxygen combusted with pure oxygen in a high-temperature furnace and a major portion of the sulfur
is converted to sulfur dioxide. The sulfur dioxide is passed through a potassium iodide-starch solution where it is titrated with
potassium iodate solution. The potassium iodate solution is standardized against samples of known sulfur content.
5. Significance and Use
5.1 Sulfur, even in very low concentrations, is of concern in a nuclear reactor because of potential corrosion of metallic
components. This test method has the sensitivity to analyze very low sulfur contents in graphite using very small samples.
5.2 This test method can be used to characterize graphite for design purposes.
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.F0 on Manufactured Carbon and Graphite Products.
Current edition approved May 1, 2010Dec. 1, 2015. Published May 2010January 2016. Originally approved in 1977. Last previous edition approved in 20052010 as
ɛ1
C816 – 85 (2005).(2010) . DOI: 10.1520/C0816-85R10E01.10.1520/C0816-15.
2
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.
3
The last approved version of this historical standard is referenced on www.astm.org.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
C816 − 15
6. Interferences
6.1 Any substance that releases volatile material, which tends to enhance or to bleach the starch-iodine complex, will interfere.
Halogens and oxides of nitrogen interfere through darkening the color of the starch-iodine complex. Ultraviolet light will also
darken the solution. A tube packed with either silver wool or antimony filings placed in the line between the furnace and titration
assembly will remove halogens from the gas stream.
6.2 If the solution in the titration vessel becomes colorless during the titration, some SO will be lost and a low result will be
2
obtained for the sulfur content.
7. Apparatus
7.1 Apparatu
...