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ASTM C816-15(2020)e1

(Test Method)

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

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, 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.

General Information

Status
Published
Publication Date
30-Nov-2020
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

Refers
ASTM E50-17 - Standard Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
Effective Date
01-Sep-2017
Refers
ASTM E50-11(2016) - Standard Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
Effective Date
01-Aug-2016
Refers
ASTM E50-11 - Standard Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
Effective Date
15-Oct-2011
Refers
ASTM E50-00(2005) - Standard Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
Effective Date
01-May-2005
Refers
ASTM D3177-02 - Standard Test Methods for Total Sulfur in the Analysis Sample of Coal and Coke
Effective Date
10-Sep-2002
Refers
ASTM E50-00 - Standard Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
Effective Date
10-Nov-2000
Refers
ASTM D3177-89(2002) - Standard Test Methods for Total Sulfur in the Analysis Sample of Coal and Coke
Effective Date
29-Sep-1989

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ASTM C816-15(2020)e1 - Standard Test Method for Sulfur Content in Graphite by Combustion-Iodometric Titration MethodASTM C816-15(2020)e1 - Standard Test Method for Sulfur Content in Graphite by Combustion-Iodometric Titration Method
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ASTM C816-15(2020)e1 - Standard Test Method for Sulfur Content in Graphite by Combustion-Iodometric Titration Method
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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.
´1
Designation: C816 − 15 (Reapproved 2020)
Standard Test Method for
Sulfur Content 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 U.S. Department of Defense.
ε NOTE—Editorially corrected 10.1 in December 2020.
1. Scope 3. Terminology
3.1 Definitions:
1.1 This test method covers the determination of sulfur in
3.1.1 combustion, n—chemical reaction by which graphite
graphite in the concentration range from 1 µg⁄g to 1000 µg⁄g
is combined in a controlled manner with pure oxygen in a high
(ppm).
temperature furnace for analytical purposes.
1.2 The values stated in SI units are to be regarded as
3.1.2 sulfur content, n—percentage content by weight of
standard. No other units of measurement are included in this
elemental sulfur present in graphite.
standard.
3.1.3 titration, n—quantitative chemical analysis method
1.3 This standard does not purport to address all of the
used to determine the unknown concentration of a specified
safety concerns, if any, associated with its use. It is the
element by reacting a solution prepared from the sample to be
responsibility of the user of this standard to establish appro-
analyzed with a known concentration and volume of specific
priate safety, health, and environmental practices and deter-
reagent.
mine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accor-
4. Summary of Test Method
dance with internationally recognized principles on standard-
4.1 The sample is combusted with pure oxygen in a high-
ization established in the Decision on Principles for the
temperature furnace and a major portion of the sulfur is
Development of International Standards, Guides and Recom-
converted to sulfur dioxide. The sulfur dioxide is passed
mendations issued by the World Trade Organization Technical
through a potassium iodide-starch solution where it is titrated
Barriers to Trade (TBT) Committee.
with potassium iodate solution. The potassium iodate solution
is standardized against samples of known sulfur content.
2. Referenced Documents
2.1 ASTM Standards:
5. Significance and Use
D3177 Test Methods forTotal Sulfur in theAnalysis Sample
5.1 Sulfur, even in very low concentrations, is of concern in
of Coal and Coke (Withdrawn 2012)
a nuclear reactor because of potential corrosion of metallic
E50 Practices for Apparatus, Reagents, and Safety Consid-
components. This test method has the sensitivity to analyze
erations for Chemical Analysis of Metals, Ores, and
very low sulfur contents in graphite using very small samples.
Related Materials
5.2 This test method can be used to characterize graphite for
design purposes.
This test method is under the jurisdiction of ASTM Committee D02 on
6. Interferences
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.F0 on Manufactured Carbon and Graphite Products.
6.1 Any substance that releases volatile material, which
Current edition approved Dec. 1, 2020. Published December 2020. Originally
tends to enhance or to bleach the starch-iodine complex, will
approved in 1977. Last previous edition approved in 2015 as C816 – 15. DOI:
interfere. Halogens and oxides of nitrogen interfere through
10.1520/C0816-15R20E01.
darkening the color of the starch-iodine complex. Ultraviolet
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
light will also darken the solution. A tube packed with either
Standards volume information, refer to the standard’s Document Summary page on
silver wool or antimony filings placed in the line between the
the ASTM website.
furnace and titration assembly will remove halogens from the
The last approved version of this historical standard is referenced on
www.astm.org. gas stream.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
´1
C816 − 15 (2020)
6.2 If the solution in the titration vessel becomes colorless 9.8 Remove the stopper from the mouth of the combustion
during the titration, some SO will be lost and a low res
...

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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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5.1 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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ASTM D8091-21(Guide)
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:  
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.  
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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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