overview of astm international - ingsm-2019

© ASTM International

Overview of ASTM

International

September 2019

Nassia Tzelepi

Tjark van Staveren

Derek Tsang

www.astm.org

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Agenda

Role of ASTM International

How standards are created, approved and maintained

New standards for Molten Salts Reactors

Graphite specific standards: Recent developments

Open discussion (30 min, all):

- Additional requirements for standards

- Future ASTM meetings during INGSM

- Q&A for prospective participants

AOB


What is ASTM International

One of the largest voluntary standards developing organizations in the world.

A not-for-profit organization that provides a forum for the development and publication of international voluntary consensus standards for materials, products, systems and services.

From its inception, the ASTM method of developing standards has been based on consensus without borders. The ASTM process ensures that interested individuals and organizations representing academia, industry, product users and governments alike all have an equal vote in determining a standard’s content.

ASTM volunteer members belong to one or more committees, each of which covers a subject area such as steel, petroleum, medical devices, nanotechnology and many more. These committees develop the more than 12,000 ASTM standards found on the website and in the 80-volume Annual Book of ASTM Standards.

Anyone interested in the field covered by a committee’s scope is eligible to become a committee member.


How are standards developed

A standard is a document that has been developed and established through

ASTM's consensus principles and which meets the requirements of the

ASTM procedures and regulations. Full consensus standards are developed

with the participation of stakeholders with an interest in their development

and use.

The sub-committee and main committee have 2meetings/year in the USA.

The next meeting is in New Orleans (9-12 Dec 2019).


Types of standards


Types of standards

All standards have to be reviewed every 5 years.

If not reviewed, the standards will be withdrawn.


Standard Test Method

For test methods, once a draft is written, it is evaluated by a series of interlaboratory test programs (ILS) which are designed to show the method’s precision and bias and general suitability as a laboratory test.

According to ASTM E691:

Under no circumstances should the final statement of precision of a test method be based on acceptable test results for each material from fewer than 6 laboratories. This would require that the ILS begin with 8 or more laboratories in order to allow for attrition.

An ILS of a test method should include at least three materialsrepresenting different test levels, and for development of broadly applicable precision statements, six or more materials should be included in the study.

When cooperative testing shows the test method to be satisfactory, the Task Group that developed it recommends that the Subcommittee ballot the draft as a new standard.


ILS Process

Registration - register the ILS through the MyASTM area of the website.

Samples

Lab Solicitation

Lab Instructions

Data Report Forms - ASTM will collect the study data using an online data report form or an excel data report form (depending on the amount/complexity of the data). The data report form will be sent to the technical contact for review before the labs receive it.

Sample Distribution

Data Submission - ASTM will track data submitted by the lab participants.

Statistical Summary - once all of the data has been received from the labs, ASTM will then compute the repeatability and reproducibility using ASTM Statistical Software. A draft precision and bias statement will be written and sent to the TC for review.

Research Report (RR) - to generate the RR, ASTM will utilize information collected during the ILS, including information in the online registration, study instructions, data analysis and the precision and bias statement. The draft research report will be sent to the TC for review.

Precision and Bias Statement - the precision and bias statement (along with any other revisions to the standard) should be placed on the next ballot.

Approval - after the ballot is approved and the research report is complete, ASTM will assign a RR#, and send out copies of the RR to the TC and the participating labs.


Risk of not maintaining sub-committee D02.F on

Manufactured Carbons and Graphite Products

ASTM standards are referenced in the ASME design codes for new reactors.

ASTM standards provide reassurance to regulators.

ASTM Standards no longer reflect new developments, understanding and new

testing methods for graphite.

ASTM standards are withdrawn if there is not sufficient expertise in the

committee to re-approve them.

Lost opportunity to engage with manufacturers, users, regulators to reach

common understanding










AOB


Graphite for Molten Salt reactors (TMSR)

• Molten salt reactor has a graphite core.

• Graphite working conditions:

In direct contact with molten salt.

High does irradiation damage.

• Molten salt

Introduce uncertainty in neutron spectra,

hazard the reactor control.

Change in graphite material properties

• Mechanical strength, Young’s modulus

• Thermal conductivity and CTE

Combine effect of irradiation and molten salt

• UNKNOWN

11


Graphite for Molten Salt reactors (TMSR)

12

• TMSR project requires superfine grain graphite for reactor core to prevent molten salt impregnation.

• New graphite => requires new graphite testing standard!

• Several new graphite standards/guides for ASTM have been proposed from SINAP.

High temperature strength measurement for graphite with molten salt.

Tensile test for small graphite samples.

Guide for impregnation of graphite with molten salt.

Liquid permeability for graphite

Gas permeability for graphite


Tensile test for small graphite samples

13


Introduction

• Tensile test is not included in irradiation programs due to the sample size.

NGNP

• Tensile strength is smallest in graphite.

• Little irradiation data for Chinese graphite.


Tensile test for small graphite samples

Aims:

Develop a tensile strength method for small graphite

samples used in irradiation programs

Measure tensile strength at high temperature for molten salt

graphite sample

Objections:

Experimental study fixture shapes and sizes

Finite element analysis of fixture and graphite sample


Different diameters

D10x5, D15x7.5, D20x10

Different sample sizes give consistent results

D10×5 D15×7.5 D20×10

No. of samples 43 4 5

Average (MPa) 23.1 23.9 23.3

Maximum (MPa) 25.41 24.5 24.7

Minimum (MPa) 18.45 22.8 21.4

D15x7.5


Results from Round robin test (inter laboratory test)

17


Guide for impregnation of graphite with molten salt

18


Introduction

19

• A new standard is required to impregnate graphite with molten salt.

• So the results from different graphite at different impregnation pressures and temperatures can be compared/studied.

• How to measure of the extent of penetration of different graphite porosities by different molten salts?


FLiBe Salt

20


Autoclave and graphite crucible

21


High temperature strength measurement for graphite with molten salt

22


Background

• Graphite is a moderator and structural components in the molten salt

reactors in China.

• Molten salt in graphite has a big influence on material properties at high

temperature.

• Existing standards: ASTM C749-08, ASTM C695, ASTM C651, ASTM

D7779 can be used in room temperature;

• Measuring material properties at high temperature are required for

graphite to be used in molten salt reactors.

23


Aim 1: Measure High Temperature Tensile Strength for

Graphite with Molten Salt

ASTM C749-08 Standard Test

Method for Tensile Stress-Strain

of Carbon and Graphite

Existing standard:


Aim 2: Measure High Temperature Compressive Strength

for Graphite with Molten Salt

ASTM C695 Standard Test

Method for Compressive

Strength of Carbon and

Graphite

Existing standard:


Aim 3: Measure High Temperature Flexural Strength for

Graphite with Molten Salt

ASTM C651-91(2010) Standard test method

for flexural strength of manufactured carbon

and graphite articles using four point loading

at room temperature

Existing standard:


Aim 4: Measure High Temperature Fracture Toughness

for Graphite with Molten Salt

ASTM D7779-11 Standard Test

Method for Determination of

Fracture Toughness of Graphite at

Ambient Temperature

Existing standard:


Things to consider

• Graphite is easy to oxidize

at high temperature;

• Some molten salts are

harmful on human body;

• The clamp behavior at high

temperature.

• Testing graphite samples

in an inert environment;

• Gas treatment before

emission;

• The clamp is manufactured

by high temperature alloy.

28










AOB


List of ASTM graphite standards

C559-16 Standard Test Method for Bulk Density by Physical Measurements of Manufactured Carbon and Graphite Articles

C560-15e1 Standard Test Methods for Chemical Analysis of Graphite

C561-16 Standard Test Method for Ash in a Graphite Sample

C562-15 Standard Test Method for Moisture in a Graphite Sample

C565-15 Standard Test Methods for Tension Testing of Carbon and Graphite Mechanical Materials

C611-98(2016) Standard Test Method for Electrical Resistivity of Manufactured Carbon and Graphite Articles at Room Temperature

C625-15 Standard Practice for Reporting Irradiation Results on Graphite

C651-15 Standard Test Method for Flexural Strength of Manufactured Carbon and Graphite Articles Using Four-Point Loading at Room Temperature

C662-16 Standard Specification for Impervious Graphite Pipe and Threading

C695-15 Standard Test Method for Compressive Strength of Carbon and Graphite

C714-17 Standard Test Method for Thermal Diffusivity of Carbon and Graphite by Thermal Pulse Method

C747-16 Standard Test Method for Moduli of Elasticity and Fundamental Frequencies of Carbon and Graphite Materials by Sonic Resonance

C748-98(2015) Standard Test Method for Rockwell Hardness of Graphite Materials

C749-15 Standard Test Method for Tensile Stress-Strain of Carbon and Graphite

D7779-11(2015) Standard Test Method for Determination of Fracture Toughness of Graphite at Ambient Temperature

C769-15 Standard Test Method for Sonic Velocity in Manufactured Carbon and Graphite Materials for Use in Obtaining an Approximate Value of Young's Modulus

C781-18 Standard Practice for Testing Graphite Materials for Gas-Cooled Nuclear Reactor Components

C783-85(2015) Standard Practice for Core Sampling of Graphite Electrodes

C808-75(2016) Standard Guide for Reporting Friction and Wear Test Results of Manufactured Carbon and Graphite Bearing and Seal Materials

C816-15 Standard Test Method for Sulfur Content in Graphite by Combustion-Iodometric Titration Method

C838-16 Standard Test Method for Bulk Density of As-Manufactured Carbon and Graphite Shapes

C886-98(2015) Standard Test Method for Scleroscope Hardness Testing of Carbon and Graphite Materials

C1025-15 Standard Test Method for Modulus of Rupture in Bending of Electrode Graphite

C1039-85(2015) Standard Test Methods for Apparent Porosity, Apparent Specific Gravity, and Bulk Density of Graphite Electrodes

C1179-15 Standard Test Method for Oxidation Mass Loss of Manufactured Carbon and Graphite Materials in Air

D7219-08(2014) Standard Specification for Isotropic and Near-isotropic Nuclear Graphites

D7301-11(2015) Standard Specification for Nuclear Graphite Suitable for Components Subjected to Low Neutron Irradiation Dose

D7542-15 Standard Test Method for Air Oxidation of Carbon and Graphite in the Kinetic Regime

D7775-16 Standard Guide for Measurements on Small Graphite Specimens


The following standards are under preparation, and are all related to nuclear

graphite:

WK52152 High Temperature Testing of Graphites Exposed to Molten Salt

Environments

WK56273 Measurement of Molten Salt Permeability in Nuclear-Grade Graphite

WK56275 the Measurement of Gas Permeability in Nuclear-Grade Graphite

WK61462 Tensile Strength Estimate by Disk Compression of Manufactured Graphite

WK66174 Work of Fracture Measurements on Small Nuclear Graphite Specimens

WK66450 Sonic Velocity in Manufacture Carbon and Graphite Materials for use in

obtaining Approximate Elastic Constants: Youngs Modulus, Shear Modulus and

Poissons Ratio

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Standards in preparation


ASTM standards typically specify requirements on test specimen size. However, in some applications, available test material or experiment design constraints on test specimen sizes may result in noncompliance.

Testing of irradiated graphite is restricted to small specimen sizesfor practical reasons, e.g. due to the volume in irradiation facilities, sampling from reactors, radioactivity)

Different techniques have succesfully been used for small specimens by different companies / institutes, and good practicesare collected in D7775 Standard Guide for Measurements on Small Graphite Specimens:


D7775 Standard Guide for

Measurements on Small Graphite Specimens


The nomenclature used for microstructural features in graphite often leads

to confusion and debate.

Guide D8075 provides guidance on:

Performing microscopy on graphite, i.e. specimen preparation and obtaining

micrographs

Categorization of features


D8075 Standard Guide for

Categorization of Microstructural and Microtextural Features

Observed in Optical Micrographs of Graphite










AOB


Have you hear about ASTM before this presentation?

Are you a user of ASTM graphite standards?

Would you like to be involved in the development of graphite

standards?

Do you have a need for a specific standard?

Would you attend a dedicated ASTM session at an INGSM

conference to discuss ongoing developments on graphite

standards?


Poll


www.astm.org

Thank you

overview of astm international - ingsm-2019

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