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ASTM F1459-06(2012)

(Test Method)

Standard Test Method for Determination of the Susceptibility of Metallic Materials to Hydrogen Gas Embrittlement (HGE)

Standard Test Method for Determination of the Susceptibility of Metallic Materials to Hydrogen Gas Embrittlement (HGE)

SIGNIFICANCE AND USE
This test method will provide a guide for the choice of metallic materials for applications in high pressure hydrogen gas.
The value of the PHe/PH2 ratio will be a relative indication of the severity of degradation of the mechanical properties to be expected in hydrogen.
SCOPE
1.1 This test method covers the quantitative determination of the susceptibility of metallic materials to hydrogen embrittlement, when exposed to high pressure gaseous hydrogen.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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
31-May-2012
ICS
77.040.99 - Other methods of testing of metals
Technical Committee
F07 - Aerospace and Aircraft
Drafting Committee
F07.04 - Hydrogen Embrittlement
Current Stage
Ref Project

Relations

Replaces
ASTM F1459-06 - Standard Test Method for Determination of the Susceptibility of Metallic Materials to Hydrogen Gas Embrittlement (HGE)
Effective Date
01-Jun-2012
Replaced By
ASTM F1459-06(2017) - Standard Test Method for Determination of the Susceptibility of Metallic Materials to Hydrogen Gas Embrittlement (HGE)
Effective Date
01-Dec-2017
Referred By
ASTM B650-95(2023) - Standard Specification for Electrodeposited Engineering Chromium Coatings on Ferrous Substrates
Effective Date
01-Jun-2012
Referred By
ASTM F519-18 - Standard Test Method for Mechanical Hydrogen Embrittlement Evaluation of Plating/Coating Processes and Service Environments
Effective Date
01-Jun-2012

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ASTM F1459-06(2012) - Standard Test Method for Determination of the Susceptibility of Metallic Materials to Hydrogen Gas Embrittlement (HGE)ASTM F1459-06(2012) - Standard Test Method for Determination of the Susceptibility of Metallic Materials to Hydrogen Gas Embrittlement (HGE)
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ASTM F1459-06(2012) - Standard Test Method for Determination of the Susceptibility of Metallic Materials to Hydrogen Gas Embrittlement (HGE)
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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
Designation: F1459 − 06 (Reapproved 2012)
Standard Test Method for
Determination of the Susceptibility of Metallic Materials to
Hydrogen Gas Embrittlement (HGE)
This standard is issued under the fixed designation F1459; 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.
1. Scope 4. Significance and Use
1.1 This test method covers the quantitative determination 4.1 This test method will provide a guide for the choice of
of the susceptibility of metallic materials to hydrogen metallic materials for applications in high pressure hydrogen
embrittlement, when exposed to high pressure gaseous hydro- gas.
gen.
4.2 The value of the P /P ratio will be a relative
He H2
1.2 The values stated in SI units are to be regarded as the indication of the severity of degradation of the mechanical
standard. The values given in parentheses are for information properties to be expected in hydrogen.
only.
5. Apparatus
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
5.1 A basic test system shall consist of the following items:
responsibility of the user of this standard to establish appro- 5.1.1 Test Cell, consists of two flanges as shown schemati-
priate safety and health practices and determine the applica-
cally in Fig. 1.
bility of regulatory limitations prior to use. 5.1.1.1 The test cell shall befabricated from materials such
as 316 stainless steel in the annealed condition that are not
2. Referenced Documents
susceptible to HGE (3, 4).
5.1.1.2 The seals shall be elastomer O-rings for helium
2.1 ASTM Standards:
testing and hydrogen testing at rates of 10 bar/min (145
E384 Test Method for Knoop and Vickers Hardness of
psig/min) or higher. For hydrogen tests at a lower rate, indium
Materials
O-rings shall be used.
3. Summary of Test Method 5.1.1.3 An evaluation port (Item 1 in Fig. 1) on the lower
flangeisusedtocheckgaspurityandadjustpressurizationrate.
3.1 Athin disk metallic specimen is subjected to an increas-
5.1.2 The test cell is pressurized with hydrogen or helium
ing gas pressure at constant rate until failure (bursting or
throughapneumaticsystem.Fig.2schematicallyillustratesthe
cracking of the disk). The embrittlement of the material can be
pneumatic system.
evaluated by comparing the rupture pressures of identical disk
5.1.2.1 The pressurization rate shall be adjustable in the
specimens in hydrogen (P ) and in a reference inert gas such
H2
2 system.Athrottle valve is used to adjust the pressurization rate
as helium (P ) (1, 2).
He
in Fig. 2.
3.2 The ratio P /P can be used to evaluate the suscepti-
He H2
bility of the metallic material to gaseous hydrogen embrittle-
6. Gases
ment. The ratio is dependent on the pressurization rate.Aratio
6.1 Helium, purity 99.995 minimum, 6000-psig (41 400-
of 1 or less indicates the material is not susceptible to hydrogen
kPa) or higher pressure source.
embrittlement.Aratio greater than 1 indicates that the material
6.2 Hydrogen, purity 99.995 minimum, 6000-psig (41 400-
is susceptible to hydrogen embrittlement and the susceptibility
increases as the ratio increases. kPa) or higher pressure source.
7. Specimen Preparation
This test method is under the jurisdiction of ASTM Committee F07 on
7.1 Fifteen (15) specimens with identical dimensions and
Aerospace and Aircraft and is the direct responsibility of Subcommittee F07.04 on
temper conditions shall be prepared for each test program. Six
Hydrogen Embrittlement.
Current edition approved June 1, 2012. Published August 2012. Originally
(6) specimens are to be tested in helium and nine (9) specimens
approved in 1993. Last previous edition approved in 2006 as F1459 –06. DOI:
are to be tested in hydrogen. One specimen is to be tested at the
10.1520/F1459-06R12.
predetermined pressurization rate in helium or hydrogen as
The boldface numbers in parentheses refer to the list of references at the end of
this standard. prescribed in 8.2.3.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
F1459 − 06 (2012)
7.4 The surface of the disk specimen shall be free of oxides.
The surface roughness Ra shall be 0.001 mm (40 µin.) or less.
7.5 The disk specimen shall be prepared by a method that
does not alter mechanical properties of the material at the edge
of the specimen. Microhardness testing should be conducted
per Test Method E384 at the outer edge of the specimen
(outside the tested area) to ensure it is as a means of confirming
that the mechanical properties were not altered.
7.6 The specimens shall be cleaned, free of grease and dried
before test.
8. Procedure
8.1 Pressurization Procedure:
8.1.1 Install a disk specimen in the test cell.
-2 -3
8.1.2 Evacuate the system to 10 to 10 torr for 3 min to
eliminate air, moisture, and residual test gases from the system.
8.1.3 Purge the system with the gas to be tested, check gas
purity from the evacuation port on a per batch basis.
8.1.4 Repeat 8.1.2 and 8.1.3 if necessary.
8.1.5 Adjust the pressurization rate to the desired level.
8.1.6 Pressurize the system. The pressure versus time data
shall be recorded.
8.1.7 Stop the test when the disk has burst. Record the burst
1. Port for evacuation and flow
...

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ABSTRACT
This guide presents the simulation procedure which would provide advice for conducting experiments to investigate the effects of helium on the properties of irradiated metals where the technique for introducing the helium differs in someway from the actual mechanism of introduction of helium in service. Simulation techniques considered for introducing helium shall include charged particle implantation, exposure to α-emitting radioisotopes, and tritium decay techniques. Procedures for the analysis of helium content and helium distribution within the specimen are also recommended. The two other methods for introducing helium into irradiated materials namely, the enhancement of helium production in nickel-bearing alloys by spectral tailoring in mixed-spectrum fission reactors, and the isotopic tailoring in both fast and mixed-spectrum fission reactors, are not covered in this guide. Dual ion beam techniques for simultaneously implanting helium and generating displacement damage are also not included here.
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4.1 Helium is introduced into metals as a consequence of nuclear reactions, such as (n, α), or by the injection of helium into metals from the plasma in fusion reactors. The characterization of the effect of helium on the properties of metals using direct irradiation methods may be impractical because of the time required to perform the irradiation or the lack of a radiation facility, as in the case of the fusion reactor. Simulation techniques can accelerate the research by identifying and isolating major effects caused by the presence of helium. The word ‘simulation’ is used here in a broad sense to imply an approximation of the relevant irradiation environment. There are many complex interactions between the helium produced during irradiation and other irradiation effects, so care must be exercised to ensure that the effects being studied are a suitable approximation of the real effect. By way of illustration, details of helium introduction, especially the implantation temperature, may determine the subsequent distribution of the helium (that is, dispersed atomistically, in small clusters in bubbles, etc.).
SCOPE
1.1 This guide provides advice for conducting experiments to investigate the effects of helium on the properties of metals where the technique for introducing the helium differs in some way from the actual mechanism of introduction of helium in service. Techniques considered for introducing helium may include charged particle implantation, exposure to α-emitting radioisotopes, and tritium decay techniques. Procedures for the analysis of helium content and helium distribution within the specimen are also recommended.  
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SCOPE
1.1 The purpose of these test methods is to allow detection of the presence of intermetallic phases in certain duplex stainless steels as listed in Table 1, Table 2, and Table 3 to the extent that toughness or corrosion resistance is affected significantly. These test methods will not necessarily detect losses of toughness or corrosion resistance attributable to other causes. Similar test methods for other duplex stainless steels are described in Test Method A1084, but the procedures described in this standard differ significantly from Test Methods A, B, and C in A1084.  
1.2 Duplex (austenitic-ferritic) stainless steels are susceptible to the formation of intermetallic compounds during exposures in the temperature range from approximately 600 to 1750 °F (320 to 955 °C). The speed of these precipitation reactions is a function of composition and thermal or thermomechanical history of each individual piece. The presence of these phases is detrimental to toughness and corrosion resistance.  
1.3 Correct heat treatment of duplex stainless steels can eliminate these detrimental phases. Rapid cooling of the product provides the maximum resistance to formation of detrimental phases by subsequent thermal exposures.  
1.4 Compliance with the chemical and mechanical requirements for the applicable product specification does not necessarily indicate the absence of detrimental phases in the product.  
1.5 These test methods include the following:  
1.5.1 Test Method A—Sodium Hydroxide Etch Test for Classification of Etch Structures of Duplex Stainless Steels (Sections 3 – 7).  
1.5.2 Test Method B—Charpy Impact Test for Classification of Structures of Duplex Stainless Steels (Sections 8 – 13).  
1.5.3 Test Method C—Ferric Chloride Corrosion Test for Classification of Structures of Duplex Stainless Steels (Sections 14 – 20).  
1.6 The presence of detrimental intermetallic phases is readily detected in all three tests, provided that a sample of appropriate location and orientation is selected. Because the occurrence of intermetallic phases is a function of temperature and cooling rate, it is essential that the tests be applied to the region of the material experiencing the conditions most likely to promote the formation of an intermetallic phase. In the case of common heat treatment, this region will be that which cooled most slowly. Except for rapidly cooled material, it may be necessary to sample from a location determined to be the most slowly cooled for the material piece to be characterized.  
1.7 The tests do not determine the precise nature of the detrimental phase but rather the presence or absence of an intermetallic phase to the extent that it is detrimental to the toughness and corrosion resistance of the material.  
1.8 Examples of the correlation of thermal exposures, the occurrence of intermetallic phases, and the degradation of toughness and corrosion resistance are given in Appendix X1 and Appendix X2.  
1.9 The values stated in either inch-pound or SI units are to be regarded as the standard. The values given in parentheses are for information only.  
1.10 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.  
1.11 This internat...

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ASTM
ASTM E1181-02(2023)(Test Method)
Standard Test Methods for Characterizing Duplex Grain Sizes

SIGNIFICANCE AND USE
5.1 Duplex grain size may occur in some metals and alloys as a result of their thermomechanical processing history. For comparison of mechanical properties with metallurgical features, or for specification purposes, it may be important to be able to characterize grain size in such materials. Assigning an average grain size value to a duplex grain size specimen does not adequately characterize the appearance of that specimen, and may even misrepresent its appearance. For example, averaging two distinctly different grain sizes may result in reporting a size that does not actually exist anywhere in the specimen.  
5.2 These test methods may be applied to specimens or products containing randomly intermingled grains of two or more significantly different sizes (henceforth referred to as random duplex grain size). Examples of random duplex grain sizes include: isolated coarse grains in a matrix of much finer grains, extremely wide distributions of grain sizes, and bimodal distributions of grain size.  
5.3 These test methods may also be applied to specimens or products containing grains of two or more significantly different sizes, but distributed in topologically varying patterns (henceforth referred to as topological duplex grain sizes). Examples of topological duplex grain sizes include: systematic variation of grain size across the section of a product, necklace structures, banded structures, and germinative grain growth in selected areas of critical strain.  
5.4 These test methods may be applied to specimens or products regardless of their state of recrystallization.  
5.5 Because these test methods describe deviations from a single, log-normal distribution of grain sizes, and characterize patterns of variation in grain size, the total specimen cross-section must be evaluated.  
5.6 These test methods are limited to duplex grain sizes as identifiable within a single polished and etched metallurgical specimen. If duplex grain size is suspected in a product too ...
SCOPE
1.1 These test methods provide simple guidelines for deciding whether a duplex grain size exists. The test methods separate duplex grain sizes into one of two distinct classes, then into specific types within those classes, and provide systems for grain size characterization of each type.  
1.2 Units—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 may involve hazardous materials, operations, and equipment. 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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