Measurement of Hydrogen Embrittlement Threshold in Steel by The Incremental Step Loading Technique
Measurement of Hydrogen Embrittlement Threshold in Steel by The Incremental Step Loading Technique
Measurement of Hydrogen Embrittlement Threshold in Steel by The Incremental Step Loading Technique
for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
INTRODUCTION
Hydrogen embrittlement is caused by the introduction of hydrogen into steel that can initiate
fracture as a result of residual stress or in service when external stress is applied (1).2 The hydrogen
can be generated during cleaning or plating processes or the exposure of cathodically protected steel
parts to a service environment including fluids, cleaning treatments, or maintenance chemicals that
may contact the surface of steel components. This method can be used to rapidly determine the effects
of residual hydrogen in a part caused by processing or quantify the relative susceptibility of a material
under a fixed set of hydrogen-charging conditions.
The combined residual and applied stress above which time-delayed fracture will occur (finite life)
or below which fracture will never occur (infinite life) is called the threshold stress or threshold stress
intensity (K) for precracked specimens. Historically, sustained load time-to-failure tests have been
conducted on notched bars to determine the threshold stress for the onset of hydrogen stress cracking.
This technique may require 12 to 14 specimens and several high-load capacity machines. For
precracked specimens, the run-out time can be as long as four to five years per U.S. Navy requirements
for low-strength steels at 33 to 35 HRC. In Test Method E1681, more than 10 000 h (> one year) are
specified for low-strength steel (< 175 ksi) and 5000 h for high-strength steel (> 175 ksi).
This standard provides an accelerated method to measure the threshold stress or threshold stress
intensity as defined in Test Method E1681 for the onset of hydrogen stress cracking in steel within one
week on only one machine. The specific application of this standard to hydrogen embrittlement testing
of fasteners is described in Annex A1.
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1.5 This standard does not purport to address all of the J1237 Metric Thread Rolling Screws
safety concerns, if any, associated with its use. It is the 2.3 ANSI/ASME:6
responsibility of the user of this standard to establish appro- B18.18.2M Inspection and Quality Assurance for High-
priate safety, health, and environmental practices and deter- Volume Machine Assembly Fasteners, 1987
mine the applicability of regulatory limitations prior to use. B18.18.3M Inspection and Quality Assurance for Special
1.6 This international standard was developed in accor- Purpose Fasteners, 1987
dance with internationally recognized principles on standard- B18.18.4M Inspection and Quality Assurance for Fasteners
ization established in the Decision on Principles for the for Highly Specialized Engineering Applications, 1987
Development of International Standards, Guides and Recom- 2.4 Related Publications:7
mendations issued by the World Trade Organization Technical ASTM STP 543, Hydrogen Embrittlement Testing, 1974
Barriers to Trade (TBT) Committee. ASTM STP 962, Hydrogen Embrittlement: Prevention and
Control, 1985
2. Referenced Documents
3. Terminology
2.1 ASTM Standards:3
A490 Specification for Structural Bolts, Alloy Steel, Heat 3.1 Symbols—Terms not defined in this section can be found
Treated, 150 ksi Minimum Tensile Strength (Withdrawn in Terminologies F2078 and E6 and shall be considered as
2016)4 applicable to the terms used in this test method.
A574 Specification for Alloy Steel Socket-Head Cap Screws 3.1.1 P—applied load.
B602 Test Method for Attribute Sampling of Metallic and 3.1.2 Pc—critical load required to rupture a specimen using
Inorganic Coatings a continuous loading rate.
E4 Practices for Force Verification of Testing Machines 3.1.3 Pi—crack initiation load for a given loading and
E6 Terminology Relating to Methods of Mechanical Testing environmental condition using an incrementally increasing
E8 Test Methods for Tension Testing of Metallic Materials load under displacement control.
[Metric] E0008_E0008M
3.1.4 Pth—the invariant threshold load. Pth is the basis for
E29 Practice for Using Significant Digits in Test Data to
calculating the threshold stress or the threshold stress intensity.
Determine Conformance with Specifications
E399 Test Method for Linear-Elastic Plane-Strain Fracture 3.1.5 Pth-n—the threshold load at a specified loading rate.
Toughness KIc of Metallic Materials 3.1.6 EHE—Environmental Hydrogen Embrittlement —
E812 Test Method for Crack Strength of Slow-Bend Pre- test conducted in a specified hydrogen-charging environment.
cracked Charpy Specimens of High-Strength Metallic 3.1.7 IHE—Internal Hydrogen Embrittlement — test con-
Materials (Withdrawn 2005)4 ducted in air.
E1681 Test Method for Determining Threshold Stress Inten- 3.1.8 th—threshold — the lowest load at which subcritical
sity Factor for Environment-Assisted Cracking of Metallic cracking can be detected.
Materials 3.2 Irregular Geometry-Type Specimens—test sample other
F519 Test Method for Mechanical Hydrogen Embrittlement than a fracture mechanics-type specimen; examples include a
Evaluation of Plating/Coating Processes and Service En- notched round bar or fastener.
vironments 3.2.1 σ = applied stress.
F606 Test Methods for Determining the Mechanical Proper- 3.2.2 σnet = net stress based on area at minimum diameter of
ties of Externally and Internally Threaded Fasteners, notched round bar or per Test Method E812 for bend speci-
Washers, and Rivets (Metric) F0606_F0606M mens.
F2078 Terminology Relating to Hydrogen Embrittlement 3.2.3 σi = stress at crack initiation.
Testing 3.2.4 σth = threshold stress.
G5 Reference Test Method for Making Potentiodynamic 3.2.5 σth-EHE = EHE threshold stress — test conducted in a
Anodic Polarization Measurements specified hydrogen charging environment — geometry depen-
G129 Practice for Slow Strain Rate Testing to Evaluate the dent.
Susceptibility of Metallic Materials to Environmentally 3.2.6 σth-IHE = IHE threshold stress — test conducted in air
Assisted Cracking — geometry dependent.
2.2 SAE Standards:5 3.2.7 FFS = Fast Fracture Strength.
J78 Self-Drilling Tapping Screws 3.2.8 Kth-EHE = EHE threshold stress intensity at a specified
J81 Thread Rolling Screws loading rate — test conducted in a specified hydrogen charging
environment — not geometry dependent.
3.2.9 Kth-IHE = IHE threshold stress intensity at a specified
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or loading rate — test conducted in air — not geometry depen-
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM dent.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
4 6
The last approved version of this historical standard is referenced on Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
www.astm.org. 4th Floor, New York, NY 10036.
5 7
Available from Society of Automotive Engineers (SAE), 400 Commonwealth Available from ASTM, 100 Barr Harbor Dr., PO Box C700, West
Dr., Warrendale, PA 15096-0001. Conshohocken, PA 19428.
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3.2.10 KIEHE = invariant value of the EHE threshold stress 5.4 For fasteners, the value of σth-IHE is used to specify
intensity — test conducted in a specified hydrogen charging quantitatively the maximum stress during installation and in
environment — not geometry dependent — equivalent to service to avoid premature failure caused by residual hydrogen
KIEAC. in the steel as a result of processing.
3.2.11 KIIHE = invariant value of the IHE threshold stress 5.5 For fasteners, the value of σth-EHE is used to specify
intensity — test conducted in air — not geometry dependent. quantitatively the maximum stress during installation and in
3.2.12 KISCC = invariant value of the threshold stress inten- service to avoid failure from hydrogen absorbed during expo-
sity for stress corrosion cracking—test conducted under open sure to a specific environment.
circuit corrosion potential or freely corroding conditions—not
geometry dependent. 5.6 To measure the relative susceptibility of steels to hydro-
3.2.13 SCG = Subcritical Crack Growth. gen pickup from various fabrication processes, a single,
selected, discriminating rate is used to rank the resistance of
4. Summary of Test Method various materials to hydrogen embrittlement.
4.1 The test method is based on determining the onset of 5.7 Annex A1 describes the application of this standard test
subcritical crack growth with a step modified, incrementally method to hydrogen embrittlement testing of fasteners.
increasing, slow strain rate test (Practice G129) under displace-
ment control (3), (4), (5). 6. Apparatus
4.2 This test method measures the load necessary to initiate 6.1 Testing Machine—Testing machines shall be within the
a subcritical crack in the steel at progressively decreasing guidelines of calibration, force range, resolution, and verifica-
loading rates, for specimens of different geometry and different tion of Practices E4.
environmental conditions.
6.2 Gripping Devices—Various types of gripping devices
4.2.1 By progressively decreasing the loading rate, the
shall be used in either tension or four-point bending to transmit
threshold stress can be determined.
the measured load applied by the testing machine to the test
4.3 Four-point bending is used to maintain a constant specimen.
moment along the specimen. This condition is used to simplify
the calculation of stress or stress intensity for an irregular cross 6.3 Test Environment—The test shall be conducted in air or
section. any other suitable controlled environment using an appropriate
inert container.
4.4 The minimum or invariant value of the stress intensity 6.3.1 Potentiostatic Control—The corrosion potential of the
(KISCC, KIIHE, or KIEHE) or stress for a given geometry with specimen can be controlled with a reference saturated calomel
regard to the loading rate, is the threshold for the onset of crack electrode (SCE) or equivalent reference electrode such as
growth due to hydrogen embrittlement. Ag/AgCl in accordance with Test Method G5. The imposed
4.5 In tension (T) and bending (B), the onset of SCG as a potential is typically cathodic, ranging from 0.0 to −1.2 V
result of hydrogen in steel is identified by a concave decrease versus SCE (VSCE) in a 3.5 weight percent NaCl solution (9).
in load while holding the displacement constant. At net section 6.4 Equipment, such as RSL (trademarked),8 for determin-
yielding or above, a convex load drop is also observed. ing the onset of SCG with a step modified, incrementally
4.6 The displacement is incrementally increased in tension increasing, slow strain rate test under displacement control.
or four-point bending and the resulting load is monitored.
While the displacement is held constant, the onset of subcriti- 7. Sampling and Test Specimens
cal crack growth is detected when the load decreases. 7.1 Sampling—For research, design, and service evaluation
4.7 The loading rate must be sufficiently slow to permit and development, the sampling size depends on the specific
hydrogen to diffuse and induce cracking that manifests itself as requirements of the investigator. For manufacturing control,
a degradation in strength (see Pollock (6) and (7)). loading rates shall be fixed, but statistically significant sam-
5. Significance and Use pling sizes are used such as Test Methods F606, ANSI/ASME
B18.18.2M, B18.18.3M, or B18.18.4M and Test Method B602
5.1 This test method is used for research, design, service for fasteners. For other quality assurance tests, the sampling
evaluation, manufacturing control, and development. This test size shall be in compliance with the requirements of the
method quantitatively measures stress parameters that are used specification.
in a design or failure analysis that takes into account the effects
of environmental exposure including that which occurs during 7.2 Test Specimens—The test specimen should be classified
processing, such as plating (8) (ASTM STP 962). as either fracture mechanics-type specimens or irregular-
shaped specimens (10).
5.2 For plating processes, the value of σth-IHE is used to
specify quantitatively the maximum operating stress for a
given structure or product. 8
The sole source of supply of the apparatus known to the committee at this time
5.3 For quality control purposes, an accelerated test is is Fracture Diagnostics International, 20261 SW Acacia St., Newport Beach, CA
92660, http://www.fracturediagnostics.net. If you are aware of alternative suppliers,
devised that uses a specified loading rate, which is equal to or please provide this information to ASTM International Headquarters. Your com-
lower than the loading rate necessary to determine the thresh- ments will receive careful consideration at a meeting of the responsible technical
old stress (see 8.1). committee,1 which you may attend.
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7.2.1 Fracture mechanics-type specimens are defined in 8.1.4 The load Pth-n is the threshold load, which is the load
standards such as Test Method E399. corresponding to the step before the onset of crack growth for
NOTE 2—The maximum stress used during fatigue precracking must be
a specific loading rate.
less than 60 % of any measured value of load for crack initiation for the 8.1.5 The invariant threshold load for the onset of hydrogen
data to be valid. induced stress cracking Pth, is used to calculate KIEHE, KISCC,
7.2.2 Irregular geometry-type specimens shall be either or KIIHE. The invariant threshold load is attained when the
specimens as defined in standards such as Test Method F519 or difference between two subsequent threshold loads is less than
specimens from product. The product shall be tested either 5 % of PFFS. The value of Pth-EHE, Pth-SCC, or Pth-IHE is the
substantially full size or as a machined specimen. lowest measured threshold value.
8.1.6 Referencing Fig. 1, the step load testing protocol can
8. Procedure be summarized as follows:
SN(1)–Baseline: fast fracture test of specimen after plating to
8.1 Determination of Threshold Load (Pth): measure PMAX = PFFS. (This ensures that no cracks initiated or
8.1.1 This test protocol requires that a minimum of three softening occurred during the plating process)
samples be tested to establish the threshold load, Pth. Load one
For the hardness range of >54 HRC (see Fig. 1)
sample to rupture at a rate consistent with Test Methods E8 to SN(2)–(20/5/1) @ PMAX = PFFS; → Pth-1
establish the fast fracture strength (FFS) or load, PFFS, for a SN(3)–(20/5/1) @ PMAX = 1.1 × Pth-1; → Pth-2
given specimen geometry, (PFFS = Pc in Fig. 1). This test SN(4)–(20/5/1) @ PMAX = 1.1 × Pth-2; → Pth-3
and if necessary;
provides the baseline reference data. SN(5)–(20/5/1) @PMAX = 1.1 × Pth-3; → Pth-4
8.1.2 The specific load profile depends on the hardness of measures Pth-EHE, Pth-SCC, or Pth-IHE when ∆Pth # 5 % PFFS
the samples within the ranges of ≥33 HRC to 45 HRC; >45
or,
HRC to 54 HRC; and >54 HRC. The notation used for the For the hardness range of >45 HRC to 54 HRC (see Fig. 2)
incremental step load profile is (# / %PMAX/hrs) where # is the SN(2)–(10/5/1,2) @ PMAX = PFFS; → Pth-1
number of steps, % PMAX is the percent of the maximum SN(3)–(10/5/1,2) @ PMAX = 1.1 × Pth-1; → Pth-2
SN(4)–(10/5/1,2) @ PMAX = 1.1 × Pth-2; → Pth-3
anticipated load at each step, and hrs is the hold time for each and if necessary;
step. For the hardness range of ≥33 HRC to 45 HRC, the SN(5)–(10/5/1,2) @ PMAX = 1.1 × Pth-3; → Pth-4
loading profile is (10/5/2,4) or an initial loading profile of 10 measures Pth-EHE, Pth-SCC , or Pth-IHE when ∆Pth # 5 % PFFS
FIG. 1 Schematic of a (20/5/1) Step Loading Profile to Determine FIG. 2 Schematic of a (10/5/1,2) Step Loading Profile to Deter-
Threshold for the Hardness of Steel >54 HRC mine Threshold for the Hardness of Steel >45 HRC to 54 HRC
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FIG. 3 Schematic of a (10/5/2,4) Step Loading Profile to Deter- NOTE 1—*See Fig. 5 for calculation of additional increment.
mine Threshold for the Hardness of Steel $ 33 HRC to 45 HRC FIG. 4 Definition of Crack Initiation Load, PI Load and Threshold
Load, Pth
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9.3 The ultimate tensile strength (UTS) per Test Methods E8 10.2.3 Report the fracture load and any maximum fracture
is given as Pc/Anet. stress or stress intensity parameter that has been calculated
9.4 The threshold stress (σth) is calculated from the same from the rupture load.
mathematical relationship as UTS except that the threshold 10.2.4 Report the threshold load (P th) and any threshold
load (Pth) is used instead of Pc. stress or stress intensity parameter that has been calculated
from the threshold load.
9.5 The threshold stress (σth) is measured in an aqueous
NOTE 3—When testing irregular geometry type specimens, note that the
environment under a cathodic or hydrogen-producing environ- test results are geometric and orientation specific and deviations will occur
ment or in air for electroplated parts. These values are not from one type of sample to another of the same material if identical test
necessarily the same. samples are not used.
9.5.1 A further designation of σth-EHE is used if the test is NOTE 4—Use the loading code of “B” for four-point bending and “T”
for tension.
conducted in a specified environment.
9.5.2 A further designation of σth-IHE is used if the test is 10.2.5 Loading and duration of each increment.
conducted in air. 10.2.6 Method used to determine loading rate.
10.2.7 Environmental conditions.
9.6 Stress intensity parameters per Test Method E399 are
10.3 Test information to be available on request shall
calculated from the load measurements in section 8.1.
include:
9.7 The strain rate in units of in./in./s can be calculated by 10.3.1 Table identifying the loading profile similar to sec-
dividing the slope (see Fig. 5) of the loading rate (∆σ / ∆t) in tion 8.1.2.
units of ksi/second by the elastic modulus in units of ksi. In 10.3.2 Equations used to calculate fracture mechanics prop-
accordance with Practice G129, the loading rate should range erties and estimate stresses on irregularly shaped geometry.
from 10-5 s-1 to 10-8 s-1. 10.3.3 Fixture dimensions pertaining to how irregular test
specimens were loaded and what specific geometry was tested.
10. Report 10.3.4 Use Practice E29 for rounding of test results.
10.1 Test information on materials not covered by a product 11. Precision and Bias
specification shall be reported in accordance with 10.2 or both 11.1 Precision—The precision of the procedure in this test
10.2 and 10.3. method for measuring the susceptibility to hydrogen embrittle-
10.2 Test information to be reported shall include the ment in steel is being determined.
following when applicable: 11.2 Bias—There is no known bias in this test method.
10.2.1 Material and sample identification.
10.2.2 Specimen types can be either fracture mechanics or 12. Keywords
irregular geometry. Fracture mechanics-type specimens with 12.1 decreasing loading rate; delayed brittle failure; dis-
specified geometry shall be reported as described in Test placement control; fasteners; hydrogen embrittlement thresh-
Method E399. Irregular geometry type specimens are classified old; hydrogen induced stress cracking; rising step load; slow
according to their respective standard or specification. strain rate
ANNEX
(Mandatory Information)
INTRODUCTION
This annex addresses the specific use of this standard to determine the threshold stress for the onset
of hydrogen embrittlement of fasteners. The test is performed either in air, to measure the effect if
residual hydrogen is in the steel because of the processing (IHE), or in a controlled environment, to
measure the effect of hydrogen introduced into the steel as a result of the external sources of hydrogen
(EHE) as defined in 1.3. Alloy/Coating systems should be specified. The Open Circuit Potential (OCP)
or Corrosion Potential (ECORR) should be measured in a 3.5 % NaCl solution to characterize the
galvanic corrosion behavior of the coating relative to the specific grade of steel. A scribe mark should
be inserted in the coating at the root of a thread to simulate a damaged coating or “holiday” in the
coating. As a baseline, fasteners are tested in bending in air at Test Methods E8 loading rates to
measure the Fast Fracture Strength, FFS(B) to obtain PMAX. To measure the hydrogen embrittlement
susceptibility (EHE), fasteners are tested in a salt-water environment using the step load procedure of
Section 8 to measure Pth, except as modified herein. A minimum of three tests is required.
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A1.1 Load Requirements
A1.1.1 Tensile fasteners can range from very small screws
to 4-in. diameter (4”D) bolts per ANSI/ASME B18 or Speci-
fication A490, requiring a large load range for tensile testing
from pounds to 1000 tons; therefore, it is wise to use the
mechanical advantage of bending to reduce the testing loads. It
is also more representative of the actual installation, wherein
there is always some component of bending. For 4-point
bending, such as a Test Method F519 Type 1c specimen with
self-loading frame, the tensile loads are reduced by d/8L,
where d = the minimum diameter of the fastener and L = length
of them moment arm; or as an example, with an 8-in. long
moment arm, the load in bending required to reach the tensile
strength for a 1”D bolt would be 1/64 the load required in
tension. Compression loading a bolt in 4-point bending is
shown in Fig. A1.1 and a 4-point bend loading frame for a Type
NOTE 1—For Net Tensile Stress (σt) in bending = σb , Pt = 8M/d ≥
1c specimen that can be adapted to fasteners is shown in Fig. 1.2PUTS-E8, where M = LPc.
A1.2. FIG. A1.2 Four-Point Bend Loading Fixture for Fasteners per
Test Method F519 Type 1c
A1.2 Bare Metal Surfaces
A1.2.1 During processing, hydrogen can be introduced into
the fastener during melting of the steel, as a result of
processing, such as pickling, or during any plating or coating must always be maintained cathodic to the coating and the
operation. Subsequent thermal baking treatments are used to cathode is where the hydrogen is generated in an aqueous
remove the hydrogen. Guidelines of time and temperature are solution. When a cathodic coating is used, or the fastener is
provided under assumed process controls, but to quantitatively anodic, a crack in the coating can cause aggressive pitting
evaluate the level of hydrogen contamination or effectiveness corrosion into the substrate.
of the baking treatment, mechanical testing must be conducted
because any quantitative measurement of hydrogen is insuffi- A1.3.2 The metals involved in making a fastener can vary
cient information, since the amount is alloy and microstructur- from zinc used in making the coating at -1.2 VSCE, (Volts
ally dependent. Testing is conducted in air and the parameter versus Saturated Calomel Electrode) to zero-VSCE for stainless
that must be measured is the threshold stress for the onset of steels under freely corroding, ECORR or OCP conditions. For
hydrogen-induced stress cracking, which is calculated from plain carbon or low alloy steels that have an OCP of about -0.7
Pth. VSCE, the cathodic or hydrogen charging conditions can be as
much as 0.5 V with a zinc coating. For stainless steel fasteners
A1.3 Environmental Effects that are noble or at 0 VSCE when passivated, the cathodic
A1.3.1 The environment and primarily aqueous environ- charging potential with zinc or aluminum can be as much as 1.0
ments are in situ sources of introducing hydrogen into the V. Any damage in the coating, immediately causes a “worst
fastener while in service. This further contamination with case” situation of a very local hydrogen attack. Without any
hydrogen can occur on both bare metal surfaces, and even damage, the hydrogen infusion is controlled by the permeabil-
more aggressively on coated metal surfaces due to galvanic ity of the coating. As a result, to evaluate environmentally
corrosion effects. Although platings or coatings are used to induced hydrogen effects, the actual fastener material should
protect against general corrosion, they can be an aggressive be tested with the coating in the actual environment and again,
source of hydrogen contamination in service. The fastener the parameter that must be measured is the threshold stress for
the onset of hydrogen-induced stress cracking, which is calcu-
lated from the threshold load, Pth.
A1.4 Imposed Galvanic Potential
A1.4.1 To evaluate the general effects of coatings on fas-
teners and the influence of microstructure, bare bolts can be
tested in an aqueous environment with an imposed cathodic
potential to simulate the effects of a coating. These conditions
would represent the “worst case” conditions of a damaged
coating. The testing range of the imposed cathodic potentials
could vary from that of zinc (–1.2 VSCE) to the OCP of the
NOTE 1—For Net Tensile Stress (σt) in bending = σb , Pt = 8M/d ≥
1.2PUTS-E8, where M = Pbλ, and Pc = 2Pb. fastener material. Again, the parameter that must be measured
FIG. A1.1 Compression Four-Point Bend Loading for Tensile is the threshold stress for the onset of hydrogen-induced stress
Fasteners with Adapters cracking, which is calculated from Pth.
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A1.5 Bolt Diameter, Maximum Load in Bending tensile strength, the maximum anticipated or ultimate load
A1.5.1 The larger the diameter, the higher the maximum (PULT) for a given bolt diameter in bending can be calculated.
load. In bending, the ultimate or limiting bend stress is A1.5.2 As a baseline, fasteners are tested in bending in air at
referenced as the Modulus of Rupture (MoR) or Rsb, the Test Methods E8 loading rates to measure the Fast Fracture
specimen strength ratio in bending per Test Method E812 or as Strength, FFS(B), to obtain PMAX ≤PULT (Fig. A1.3). The
defined in Terminology F2078, have a maximum value of initial value of PMAX is taken as the 5 % secant offset. The
about 2 x UTSE8. Therefore, from the hardness conversion to minimum value should be ≥ 1.2 UTS, which corresponds to
NOTE 1—FFS(B) for 1.0”D bolt at 39 HRC with PMAX at 2.0 UTS-E8 and the 1.2 UTS-E8 acceptance level and the 5 % secant offset identified.
FIG. A1.3 Fast Fracture Strength in Bending
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75 % NTS (NTS = 1.6 UTS) in a notched round bar tension test A1.8.3 Fixtures—Various types of adapters may be used for
per Test Method F519, Type 1a. PMAX is used as the initial load the four-point bending to transmit the measured load applied
in the step load test. by the testing equipment to the test specimen. Fig. A1.1
illustrates an example of a four-point bend-loading fixture that
A1.5.3 Testing is to be carried out using tension bolts. The
could be adapted to a Test Method F519, Type 1c loading
bolts shall be of 5D in length. Since all tension bolts are
frame (See Fig. A1.2).
designed to fail in the threads, even in a wedge tensile test, the
head may be removed. The test program requires a minimum of A1.8.4 Test Environment—The test shall be conducted in a
three samples to measure the threshold. hydrogen producing environment by immersion of the fastener
into a 3.5 % NaCl solution under freely corroding or OCP
A1.6 Hardness conditions or under potentiostatic control by imposing a
A1.6.1 The most significant variable for susceptibility to galvanic cathodic potential in salt water contained in an
hydrogen induced cracking in applying this standard to steel appropriate inert container.
fasteners is the hardness. Therefore, for the most efficient A1.8.5 Potentiostatic Control—For testing of the sensitivity
selection of specific loading rates the recommended loading of the fastener to EHE, an inert container and potentiostat can
profiles are grouped according to the hardness, measured per be used to impose a cathodic potential slightly more negative
Test Methods F606. than the OCP of the coated fastener. The cathodic charging
HRC > 54; (20/5/1) profile: Fig. 1 potential of the fastener is measure relative to a reference
HRC > 45 to 54; (10/5/1,2) profile: Fig. 2 Saturated Calomel Electrode (SCE) or equivalent reference
HRC $ 33 to 45; (10/5/2,4) profile: Fig. 3 electrode such as with Ag/AgCl in accordance with Test
Each hardness range has an optimum loading sequence that Method G5.
minimizes the total test time for that hardness range. A1.8.6 OCP Testing—If the fastener can be isolated from all
Obviously, the lower the hardness, the slower the loading rate other metal contacts, the test can be conducted under freely
or the longer the total test time to measure the threshold load. corroding or OCP conditions. Such testing most accurately
An actual (10/5/2,4) test profile is shown in Fig. A1.4. represents the combined effects of general corrosion on the
A1.7 Coating surface of the coating and stress corrosion cracking.
A1.7.1 The coating that is to be evaluated shall be applied to A1.9 Acceptance Criterion
all fastener components used under normal production condi- A1.9.1 Fasteners shall be tested to the same hydrogen
tions. embrittlement acceptance criterion as with Test Method F519,
A1.7.2 Alloy/Coating system should be specified. The OCP Type 1a specimens, which also require a “worst case” scenario
should be measured in a 3.5 % NaCl solution to characterize and a threshold stress greater or equal than 75 % of the notch
the galvanic corrosion behavior of the coating relative to the tensile strength (NTS) of the Type 1a specimen.
specific grade of steel. Insert a scribe mark in the coating at the A1.9.1.1 The worst-case scenario for a coated fastener
root of a thread to simulate a damaged coating or “holiday” in consists of Wedge Tension Testing the coated fastener per Test
the coating. The hardness of the scribe should be less than the Methods F606 to verify that the fastener still meets the
hardness of the specimen in order to avoid scarring the surface specified minimum ultimate tensile load after it has been
of the notch. coated. The coating shall have a Holiday (a scribe mark
through the coating at the root of the thread). For the Type 1a
A1.8 Test Procedures specimen with d/D = 0.7, the threshold tensile stress is 75 %
NTS (where NTS = 1.6 UTSE8 and 75 % NTS = 1.2 UTSE8).
A1.8.1 Hydrogen Embrittlement Tests—The threshold load,
In terms of load, the equivalent acceptance criterion in tension
Pth, is obtained on completion of a minimum of three tests. The
to be used on the coated bolts is Pt-th ≥1.2 Pt-UTS E8.
threshold is the lowest value of two consecutive tests, when the
A1.9.1.2 Bending must be used to attain the tensile load to
difference between them is within 5 % of FFS(B). Once an
produce the equivalent stress, since d/D for fasteners is always
invariant value is obtained, no further tests are required.
greater than 0.8. Pure bending stresses (4-pt) using a rising step
Otherwise, additional tests shall be performed following the
load under displacement control shall be used to determine a
protocol of 8.1.6 until an invariant value within 5 % of FFS(B)
hydrogen embrittlement threshold stress level. Pure bending
is obtained from two consecutive tests. Test results shall be
(4-pt) shall be used so that the stress may be calculated
autographically recorded in terms of load versus time and
anywhere along the length of the fastener.
included as part of the report.
A1.9.1.3 Equivalence between pure tension and pure bend-
A1.8.2 Testing Equipment—A computerized, four-point ing is based on the stress at the root of the thread. A fastener
bend, digital displacement controlled loading frame that is adapter loaded in four-point bending is shown in Fig. A1.1. The
capable of stepping in 0.5 % load steps and is programmed to fastener may be cut to isolate a segment with threads. Four
increase incrementally in steps of load and time to vary the point bend loading may be obtained by applying an axial
effective strain rate at the root of the notch between 10-5 and compression load (Fig. A1.1) or by using leverage in bending
10-8s-1 is required to conduct these tests. Testing machines with a Test Method F519, Type 1c load fixture, Fig. A1.2.
shall be within the guidelines of calibration, force range, A1.9.1.4 To be consistent with a notched round tensile
resolution, and verification of Practice E4. coupon per Test Method F519, Type 1a, the load at threshold in
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NOTE 1—For 1”D bolt at 39 HRC with PMAX(cracked) and Pth identified at 65 % UTS-E8 that failed the acceptance criterion.
FIG. A1.4 ASTM F1624 Fig. 1C (10/5/2,4) RSL Curve
bending should exceed 1.2 Pt-UTS as a measure of sufficient M = applied moment (in-lb).
resistance to environmentally induced hydrogen stress crack-
ing. For equivalent stresses, σb = σt, the load in tension (Pt) is
The tensile stress in bending (σb) and in tension (σt) at the given by:
root of the thread can be computed using the formulas: P t 5 8M/d (A1.2)
3 2
σ b 5 ~ 32M/πd ! ; and σ t 5 ~ 4P t /πd ! (A1.1) A1.9.2 When applying the four-point load (Pb in Fig. A1.1)
where: in an axial load compression fixture, the applied moment, M =
Pbλ and Pc = 2Pb (Fig. A1.1). Therefore solving Pt in terms of
d = minimum thread diameter (in.), and
P c:
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P t 5 ~ 4λ/d ! P c $ 1.2 P t2UTS E8 (A1.3) = 32.4 kips, the acceptable minimum equivalent compressive
or bend threshold load (Pc in Fig. A1.2) is:
Pc $ ~ d/4λ ! 1.2P t2UTS E8 Acceptance level, axial compression P c2th $ 200 lb (A1.8)
(A1.4) A1.9.5 A typical 4-pont bend curve of a coated 1”D A490
A1.9.3 When applying the four-point load (Pb in Fig. A1.1) bolt is shown in Fig. A1.3, with the 5 % secant offset load
in a bend fixture such as the Type F519, Type 1c fixture with shown to be equal to 1.2 UTSE8 and the max load to be equal
L = 8 in. and solving Pt in terms of Pc, where M = 8L (Fig. to 2.0 UTSE8. Fig. A1.4 is an example of the EHE threshold
A1.2): load measured per F1624 for the bolt, equal to 0.9 UTSE8. Per
the criterion set forth in this standard, this coating would have
P t 5 ~ 8L/d ! P c $ 1.2 P t2UTS E8 (A1.5)
or failed to meet the minimum threshold requirements of equal to
≥ 1.2 UTSE8.
P c $ ~ d/8L ! 1.2P t2UTS E8 Acceptance level, compression bend
(A1.6) A1.10 Report
A1.9.4 Example—Per Specification A574, for a nominal 1/2 A1.10.1 A test report shall be produced in accordance with
-1/3 in. alloy steel socket head cap screws, the hardness range Section 10. See Fig. A1.3 and Fig. A1.4. The report shall
is 39–45 HRC, the specified minimum ultimate tensile load = include:
Pt-UTS ≥ 25,500 lb (25.5 kips) and, dt = 0.400 in. The “worst A1.10.1.1 Executive summary,
case” or maximum hardness is 45 HRC, which equals 215 ksi A1.10.1.2 Introduction,
UTSE8 or 27 kips. Therefore, the threshold tensile load Pt-th = A1.10.1.3 Detailed coating process description and coating
1.2 Pt-UTS = 32.4 kips. characteristics (including product name and coating
A1.9.4.1 Using an axial load compression fixture (A1.9.2) applicator),
for dmin = 0.4 in., λ = 1 in., and 1.2 Pt-UTS = 32.4 kips, the A1.10.1.4 Test methodology,
acceptable minimum equivalent compression threshold load is: A1.10.1.5 Detailed results,
A1.10.1.6 Discussion of results, and
P c2th $ 3.2 kips (A1.7)
A1.10.1.7 Conclusion.
A1.9.4.2 Using a bend fixture such as the Type F519, Type A1.10.1.8 All third party certifications and test reports shall
1c fixture (A1.9.3) with L = 8 in., dmin = 0.4in., and 1.2 Pt-UTS be included in the appendixes.
REFERENCES
(1) Interrante, C. G., Raymond, L., “Hydrogen Damage,” in Corrosion NAVSEA Contract No. N00024–89–C-3833, LRA Labs, Final Report
Tests and Standards, MNL 20, Baboian, R., Ed., American Society for No. NAVSEA 80058, Dec. 1989 and Dec. 1993, respectively.
Testing and Materials, West Conshohocken, PA, 1995, p. 272. (6) Pollock, W. J.,“Assessment of the Degree of Hydrogen Embrittlement
(2) Raymond, L., “The Susceptibility of Fasteners to Hydrogen Em- Produced in High-Strength 4340 Steel by Plating and Baking Process
brittlement and Stress Corrosion Cracking,” in Handbook of Bolts and Using Slow Strain Rate Testing,” ASTM STP 962, p. 68.
Bolted Joints, Marcel Decker, Inc., New York, 1998, p. 723. (7) Pollock, W. J.,“Assessment of the Degree of Hydrogen Embrittlement
(3) Raymond, L., “Application of a Small Specimen Test Method to Produced in High-Strength 4340 Steel by Paint Strippers Using Slow
Measure the Subcritical Cracking Resistance in HY-130 Steel Strain Rate Testing,” ASTM STP 962, p. 372.
Weldments,” under Contract No. DTNSRDC-SME-CR-09–82,“High-
(8) Raymond, L., “Plating or Coating Processes Can Be Monitored for
Strength Steel Weldment Subcritical Cracking Program,” under Navy
Control of Hydrogen Embrittlement,” in American Fastener Journal,
Contract N00167–81–C-0100, LRA Labs (formerly named
METTEK), Final Report No. 210123, March 1982. March/April 1998, p. 26.
(4) Raymond, L. and Crumly, W. R., “Accelerated, Low-Cost Test (9) Tyler, P. S., Levy, M., Raymond, L., “Investigation of the Conditions
Method for Measuring the Susceptibility of HY-Steels to Hydrogen for Crack Propagation and Arrest Under Cathodic Polarization by
Embrittlement,” in Proceedings of the First International Conference Rising Step Load Bend Testing,” Corrosion, NACE, Vol. 47, No. 2,
on Current Solutions to Hydrogen Problems in Steel, American Feb. 1991, pp. 82–86.
Society for Metals, Metals Park, OH, Nov. 1982, pp. 477–480. (10) National Materials Advisory Board, “Rapid Inexpensive Tests for
(5) Raymond, L., “Accelerated Stress Corrosion Cracking Screening Test Determining Fracture Toughness,” NMAB 328, National Academy
Method for HY-130 Steel,” under SBIR Phase I and Phase II of Sciences, Washington, DC, 1976 .
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