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ASTM C816-85(2010)e1

(Test Method)

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

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

SIGNIFICANCE AND USE
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.  
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 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-Apr-2010
ICS
71.060.10 - Chemical elements
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.F0 - Manufactured Carbon and Graphite Products
Current Stage
Ref Project

Relations

Replaces
ASTM C816-85(2005) - Standard Test Method for Sulfur in Graphite by Combustion-Iodometric Titration Method
Effective Date
01-May-2010
Referred By
ASTM C781-20 - Standard Practice for Testing Graphite Materials for Gas-Cooled Nuclear Reactor Components
Effective Date
01-May-2010
Referred By
ASTM F2191/F2191M-13(2020)e1 - Standard Specification for Packing Material, Graphitic or Carbon Braided Yarn
Effective Date
01-May-2010
Referred By
ASTM C1783-15 - Standard Guide for Development of Specifications for Fiber Reinforced Carbon-Carbon Composite Structures for Nuclear Applications
Effective Date
01-May-2010
Referred By
ASTM F2168-13(2019) - Standard Specification for Packing Material, Graphitic, Corrugated Ribbon or Textured Tape, and Die-Formed Ring
Effective Date
01-May-2010
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-May-2010

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ASTM C816-85(2010)e1 - Standard Test Method for Sulfur in Graphite by Combustion-Iodometric Titration MethodASTM C816-85(2010)e1 - Standard Test Method for Sulfur in Graphite by Combustion-Iodometric Titration Method
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ASTM C816-85(2010)e1 - Standard Test Method for Sulfur in Graphite by Combustion-Iodometric Titration Method
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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
´1
Designation: C816 − 85(Reapproved 2010) An American National Standard
Standard Test Method for
Sulfur in Graphite by Combustion-Iodometric 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 Department of Defense.
´ NOTE—Removed source of supply footnote and updated units of measurement throughout the standard editorially in
May 2010.
1. Scope 4. Significance and Use
1.1 This test method covers the determination of sulfur in 4.1 Sulfur, even in very low concentrations, is of concern in
graphite in the concentration range from 1 to 1000 µg/g (ppm). a nuclear reactor because of potential corrosion of metallic
components. This test method has the sensitivity to analyze
1.2 The values stated in SI units are to be regarded as
very low sulfur contents in graphite using very small samples.
standard. No other units of measurement are included in this
standard. 4.2 Thistestmethodcanbeusedtocharacterizegraphitefor
design purposes.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
5. Interferences
responsibility of the user of this standard to establish appro-
5.1 Any substance that releases volatile material, which
priate safety and health practices and determine the applica-
tends to enhance or to bleach the starch-iodine complex, will
bility of regulatory limitations prior to use.
interfere. Halogens and oxides of nitrogen interfere through
darkening the color of the starch-iodine complex. Ultraviolet
2. Referenced Documents
light will also darken the solution. A tube packed with either
2.1 ASTM Standards:
silver wool or antimony filings placed in the line between the
D3177 Test Methods forTotal Sulfur in theAnalysis Sample
furnace and titration assembly will remove halogens from the
of Coal and Coke
gas stream.
E50 Practices for Apparatus, Reagents, and Safety Consid-
5.2 If the solution in the titration vessel becomes colorless
erations for Chemical Analysis of Metals, Ores, and
during the titration, some SO will be lost and a low result will
Related Materials
be obtained for the sulfur content.
3. Summary of Test Method
6. Apparatus
3.1 The sample is burned in oxygen and a major portion of
6.1 Apparatus for the determination of sulfur by direct
the sulfur is converted to sulfur dioxide. The sulfur dioxide is
combustion shall be in accordance with No. 13 in Fig. 13 of
passed through a potassium iodide-starch solution where it is
Practices E50.
titrated with potassium iodate solution. The potassium iodate
solution is standardized against samples of known sulfur
7. Reagents and Materials
content.
7.1 Potassium Iodate Solution (0.2 mM)——Dissolve 44.4
mg of potassium iodate (KIO ) in water and dilute to 1 L.
1 NOTE 1—The sulfur equivalent for the KIO solution is based on the
This test method is under the jurisdiction of ASTM Committee D02 on 3
following reactions:
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.F0 on Manufactured Carbon and Graphite Products.
KIO 15KI16HCl 53I 16KCl13H O
3 2 2
Current edition approved May 1, 2010. Published May 2010. Originally
SO 1I 12H O 5 H SO 12HI
approved in 1977. Last previous edition approved in 2005 as C816 – 85 (2005).
2 2 2 2 4
DOI: 10.1520/C0816-85R10E01. On the basis of 100 % conversion of sulfur to SO , 1 mL of this solu-
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
tion is equivalent to 20 µg of sulfur.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
7.2 Hydrochloric Acid—Dilute 15 mL of concentrated hy-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. drochloric acid (HCl, sp gr 1.19) to 1 L with water.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, We
...

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5.1 The Molten Salt Reactor is a nuclear reactor which uses graphite as reflector and structural material, and molten salt as coolant. The graphite components will be submerged in the molten salt during the lifetime of the reactor. The porous structure of graphite may lead to molten salt permeation, which can affect the thermal and mechanical properties of graphite. Consequently, it may be necessary to measure the various strengths of the manufactured graphite materials after impregnation with molten salt and before exposure to the reactor environment in a range of test configurations in order for designers or operators to assess their performance.
Note 1: Depending upon the salt selected for the reactor, there may be some chemical reaction between the salt and the graphite that could affect properties. The user should establish, prior to following this guide, that any interactions between the molten salt and graphite are understood and any implications for the validity of the strength tests have been assessed.  
5.2 For gas-cooled reactors, the strength of a graphite specimen is usually measured at room temperature. However, for molten salt reactors, the operating temperature of the reactor must be higher than the melting temperature of the salt, and so the salt will be in solid state at room temperature. Consequently, room temperature measurements may not be representative of the performance of the material at its true operating conditions. It is therefore necessary to measure the strength at an elevated temperature where the salt is in liquid form.
Note 2: Users should be aware that a small increase in graphite strength is expected with increasing temperature. Testing at the plant operating temperature will eliminate this small uncertainty.  
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5.4 For the test results to be meaningful, the...
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Standard Guide for Impregnation of Graphite with Molten Salt

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5.1 The molten salt reactor is a nuclear reactor which uses graphite as reflector and structural material and fluoride molten salt as coolant. The graphite components will be submerged in the molten salt during the lifetime of the reactor. The porous structure of graphite may lead to molten salt permeation, which can affect the thermal and mechanical properties of graphite. Consequently, it is important to assess the effect of impregnation of molten salt on the properties of the as-manufactured graphite material.  
5.2 The purpose of this guide is to report considerations that should be included in the preparation of graphite specimens representative of that after exposure to a molten salt environment. The degree to which the molten salt will infiltrate the graphite will depend upon a number of factors, including the type of graphite and the type and extent of porosity, the properties of the molten salt, the impregnation pressure and temperature, and the duration of the exposure of the graphite to the molten salt.  
5.3 The user of this guide will need to select impregnation parameters sufficiently representative of those in a molten salt reactor based on parameters provided by the designer. Alternatively, the user may select a standard set of impregnation conditions to allow comparisons across a range of graphites.  
5.4 This guide is not intended to be prescriptive. A typical apparatus and associated procedure are described. Some indication of the sensitivity of the procedure to graphite type and impregnation conditions is given in He, et al.5  
5.5 There are four major practical issues that must be addressed during the impregnation process:  
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1.1 This guide covers procedures for the impregnation of graphite with molten salt under a consistent pressure and temperature. Such procedures are necessary if the user wishes to prepare graphite specimens for testing that represent material that has been exposed to a molten salt environment in a molten salt nuclear reactor. The user will need to ensure that impregnation temperature and pressure conditions reflect those pertaining to the molten salt environment, noting that the properties of the material will change once it becomes irradiated.
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Standard Test Method for Compressive Strength of Carbon and Graphite

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4.1 Carbon and graphite can usually support higher loads in compression than in any other mode of stress. This test, therefore, provides a measure of the maximum load-bearing capability of carbon and graphite objects.
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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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
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