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ASTM C816-85(2005)

(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 200 g/g in a 1-g sample or 5 to 1000 g/g in a 0.2-g sample.
1.2 The values stated in SI units are to be regarded as the 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-2005
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(1998)e1 - Standard Test Method for Sulfur in Graphite by Combustion-Iodometric Titration Method
Effective Date
01-May-2005
Replaced By
ASTM C816-85(2010)e1 - Standard Test Method for Sulfur in Graphite by Combustion-Iodometric Titration Method
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-2005
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-2005
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-2005
Referred By
ASTM C781-20 - Standard Practice for Testing Graphite Materials for Gas-Cooled Nuclear Reactor Components
Effective Date
01-May-2005
Referred By
ASTM F2191/F2191M-13(2020)e1 - Standard Specification for Packing Material, Graphitic or Carbon Braided Yarn
Effective Date
01-May-2005

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ASTM C816-85(2005) - Standard Test Method for Sulfur in Graphite by Combustion-Iodometric Titration MethodASTM C816-85(2005) - Standard Test Method for Sulfur in Graphite by Combustion-Iodometric Titration Method
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ASTM C816-85(2005) - 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.
An American National Standard
Designation:C816–85 (Reapproved 2005)
Standard Test Method for
Sulfur in Graphite by Combustion-Iodometric Titration
1
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.
1. Scope components. This test method has the sensitivity to analyze
very low sulfur contents in graphite using very small samples.
1.1 This test method covers the determination of sulfur in
4.2 Thistestmethodcanbeusedtocharacterizegraphitefor
graphite in the concentration range from 1 to 200 µg/g in a 1-g
design purposes.
sample or 5 to 1000 µg/g in a 0.2-g sample.
1.2 The values stated in SI units are to be regarded as the
5. Interferences
standard.
5.1 Any substance that releases volatile material, which
1.3 This standard does not purport to address all of the
tends to enhance or to bleach the starch-iodine complex, will
safety concerns, if any, associated with its use. It is the
interfere. Halogens and oxides of nitrogen interfere through
responsibility of the user of this standard to establish appro-
darkening the color of the starch-iodine complex. Ultraviolet
priate safety and health practices and determine the applica-
light will also darken the solution. A tube packed with either
bility of regulatory limitations prior to use.
silver wool or antimony filings placed in the line between the
2. Referenced Documents furnace and titration assembly will remove halogens from the
2
gas stream.
2.1 ASTM Standards:
5.2 If the solution in the titration vessel becomes colorless
D3177 Test Methods for Total Sulfur in the Analysis
during the titration, some SO will be lost and a low result will
2
Sample of Coal and Coke
be obtained for the sulfur content.
E50 Practices for Apparatus, Reagents, and Safety Consid-
erations for Chemical Analysis of Metals, Ores, and
6. Apparatus
Related Materials
6.1 Apparatus for the determination of sulfur by direct
3. Summary of Test Method combustion shall be in accordance with No. 13 in Fig. 13 of
3
Practices E50.
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. Reagents and Materials
passed through a potassium iodide-starch solution where it is
7.1 Potassium Iodate Solution (0.0444 g/L)—Dissolve
titrated with potassium iodate solution. The potassium iodate
0.0444 g of potassium iodate (KIO ) in water and dilute to 1 L.
3
solution is standardized against samples of known sulfur
content.
NOTE 1—The sulfur equivalent for the KIO solution is based on the
3
following reactions:
4. Significance and Use
KIO 1 5KI 1 6HCl 5 3I 1 6KCl 1 3H O
3 2 2
4.1 Sulfur, even in very low concentrations, is of concern in
SO 1 I 1 2H O 5 H SO 1 2HI
2 2 2 2 4
a nuclear reactor because of potential corrosion of metallic
On the basis of 100 % conversion of sulfur to SO , 1 mL of this solution
2
is equivalent to 20 µg of sulfur.
1
This test method is under the jurisdiction of ASTM Committee D02 on
7.2 Hydrochloric Acid—Dilute 15 mL of concentrated hy-
PetroleumProductsandLubricants andisthedirectresponsibilityofSubcommittee
D02.F0 on Manufactured Carbon and Graphite Products.
drochloric acid (HCl, sp gr 1.19) to 1 L with water.
Current edition approved May 1, 2005. Published May 2005. Originally
´1
approved in 1977. Last previous edition approved in 1998 as C816 – 85 (1998) .
3
DOI: 10.1520/C0816-85R05. The sole source of supply of the apparatus known to the committee at this time
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or is available from Laboratory Equipment Co., St. Joseph, MI. If you are aware of
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM alternative suppliers, please provide this information to ASTM International
Standards volume information, refer to the standard’s Document Summary page on Headquarters.Your comments will receive careful consideration at a meeting of the
1
the ASTM website. responsible technical committee , which you may attend.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
C816–85 (2005)
7.3 Starch-Potassium Iodide Solution—Add2gof arrow- 8.12 Make a blank run on an empty prefired boat, igniting
root starch to 50 mLof water. Separately boil 150 mLof water for the same length of time as the sample.
and slowly add the starch solution, stirring constantly. Cool, 8.13 Run st
...

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5.1 Two- and three-parameter formulations exist for the Weibull distribution. This practice is restricted to the two-parameter formulation. An objective of this practice is to obtain point estimates of the unknown Weibull distribution parameters by using well-defined functions that incorporate the failure data. These functions are referred to as estimators. It is desirable that an estimator be consistent and efficient. In addition, the estimator should produce unique, unbiased estimates of the distribution parameters (6). Different types of estimators exist, such as moment estimators, least-squares estimators, and maximum likelihood estimators. This practice details the use of maximum likelihood estimators.  
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5.4 Accurately determined kinetic parameters, like activation energy and logarithm of pre-exponential factor, can be used for prediction of oxidation rates in air as a function of temperature in conditions similar to those of this test method. However, extrapolation of such predictions outside the temperature range where Arrhenius plots are linear (outside the kinetic or chemically controlled regime of oxidation) should be made with extreme caution. In conditions where (1) oxidation rates become controlled by a mechanism other than chemical reactions (such as in-pore diffusion or boundary transport of the oxidant gas), or (2) the oxidant supply rate is no...
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1.6 This international s...

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Standard Test Method for Oxidation Mass Loss of Manufactured Carbon and Graphite Materials in Air

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3.1 This test method is primarily concerned with the oxidation mass loss of manufactured carbon and graphite materials in air at temperatures from 371 °C to 677 °C.  
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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:  
5.5.1 The density of molten salt is greater than that of graphite. A specially designed tool is required to submerge graphite samples in the molten salt during the impregnation process.  
5.5.2 Some molten salts (for example, FLiBe) are poisonous and it is therefore necessary to provide containment by performing proced...
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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.
Note 1: The term impregnation is used throughout this guide as this is the correct term for the described process. Other terms such as infiltration and intrusion may be encountered by the user in other texts and the term intrusion is commonly used to describe penetration of open porosity in graphite in a molten salt reactor environment.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this guide.  
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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ASTM D8377-21a(Guide)
Standard Guide for High Temperature Strength Measurements of Graphite Impregnated with Molten Salt

SIGNIFICANCE AND USE
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.  
5.3 The purpose of this guide is to provide considerations, which should be included in testing graphite specimens impregnated with molten salt at elevated temperature.  
5.4 For the test results to be meaningful, the...
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1.1 This guide covers the best practice for strength measurements at elevated temperature of graphite impregnated with molten salt.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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Standard Test Method for Compressive Strength of Carbon and Graphite

SIGNIFICANCE AND USE
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.
SCOPE
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1.2 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions to SI units that are provided for information only and are not considered 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 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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