ASTM C816-85(1998)e1

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

SCOPE
1.1 This test method covers the determination of sulfur in graphite in the concentration range from 1 to 200 [mu]g/g in a 1-g sample or 5 to 1000 [mu]g/g in a 0.2-g sample.  
1.2 This standard may involve hazardous materials, operations, and equipment. This standard does not purport to address all of the safety problems 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: 31-Dec-1997
• ICS: 71.060.10 - Chemical elements
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.F0 - Manufactured Carbon and Graphite Products

Relations

• Replaced By: ASTM C816-85(2005) - Standard Test Method for Sulfur in Graphite by Combustion-Iodometric Titration Method
• Effective Date: 01-May-2005
• Referred By: ASTM C1783-15 - Standard Guide for Development of Specifications for Fiber Reinforced Carbon-Carbon Composite Structures for Nuclear Applications
• Effective Date: 01-Jan-1998
• Referred By: ASTM C1793-15 - Standard Guide for Development of Specifications for Fiber Reinforced Silicon Carbide-Silicon Carbide Composite Structures for Nuclear Applications
• Effective Date: 01-Jan-1998
• Referred By: ASTM F2191/F2191M-13(2020)e1 - Standard Specification for Packing Material, Graphitic or Carbon Braided Yarn
• Effective Date: 01-Jan-1998
• Referred By: ASTM F2168-13(2019) - Standard Specification for Packing Material, Graphitic, Corrugated Ribbon or Textured Tape, and Die-Formed Ring
• Effective Date: 01-Jan-1998
• Referred By: ASTM C781-20 - Standard Practice for Testing Graphite Materials for Gas-Cooled Nuclear Reactor Components
• Effective Date: 01-Jan-1998

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
An American National Standard
e1
Designation:C 816–85 (Reapproved 1998)
Standard Test Method for
Sulfur in Graphite by Combustion-Iodometric Titration
Method
This standard is issued under the fixed designation C 816; 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 (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
e NOTE—Section 11 was added editorially in April 1998.
1. Scope 5. Interferences
1.1 This test method covers the determination of sulfur in 5.1 Any substance that releases volatile material, which
graphite in the concentration range from 1 to 200 µg/g in a 1-g tends to enhance or to bleach the starch-iodine complex, will
sample or 5 to 1000 µg/g in a 0.2-g sample. interfere. Halogens and oxides of nitrogen interfere through
1.2 This standard does not purport to address all of the darkening the color of the starch-iodine complex. Ultraviolet
safety concerns, if any, associated with its use. It is the light will also darken the solution. A tube packed with either
responsibility of the user of this standard to establish appro- silver wool or antimony filings placed in the line between the
priate safety and health practices and determine the applica- furnace and titration assembly will remove halogens from the
bility of regulatory limitations prior to use. gas stream.
5.2 If the solution in the titration vessel becomes colorless
2. Referenced Documents
during the titration, some SO will be lost and a low result will
2.1 ASTM Standards: be obtained for the sulfur content.
D 3177 TestMethodforTotalSulfurintheAnalysisSample
6. Apparatus
of Coal and Coke
E50 Practices for Apparatus, Reagents, and Safety Precau- 6.1 Apparatus for the determination of sulfur by direct
tions for Chemical Analysis of Metals combustion shall be in accordance with No. 13 in Fig. 13 of
PracticesE50 .
3. Summary of Test Method
7. Reagents and Materials
3.1 The sample is burned in oxygen and a major portion of
the sulfur is converted to sulfur dioxide. The sulfur dioxide is 7.1 Potassium Iodate Solution (0.0444 g/L)—Dissolve
passed through a potassium iodide-starch solution where it is 0.0444 g of potassium iodate (KIO ) in water and dilute to 1
titrated with potassium iodate solution. The potassium iodate L.
solution is standardized against samples of known sulfur
NOTE 1—The sulfur equivalent for the KIO solution is based on the
content.
following reactions:
KIO 1 5KI 1 6HCl 5 3I 1 6KCl 1 3H O
4. Significance and Use 3 2 2
SO 1 I 1 2H O 5 H SO 1 2HI
2 2 2 2 4
4.1 Sulfur, even in very low concentrations, is of concern in
a nuclear reactor because of potential corrosion of metallic
On the basis of 100 % conversion of sulfur to SO , 1 mL of this solution
components. This test method has the sensitivity to analyze is equivalent to 20 µg of sulfur.
very low sulfur contents in graphite using very small samples.
7.2 Hydrochloric Acid—Dilute 15 mL of concentrated hy-
4.2 This test method can be used to characterize graphite for
drochloric acid (HCl, sp gr 1.19) to 1 L with water.
design purposes.
7.3 Starch-Potassium Iodide Solution—Add2gof arrow-
root starch to 50 mLof water. Separately boil 150 mLof water
and slowly add the starch solution, stirring constantly. Cool,
1 add6gof potassium iodide (KI), and pour the resulting
This test method is under the jurisdiction of ASTM Committee D02 on
solution into a flask. Store in a refrigerator.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.F on Manufactured Carbon and Graphite Products.
Current edition approved July 26, 1985. Published September 1985. Originally
published as C 816 – 77. Last previous edition C 816 – 77.
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