ASTM F519-97e2
(Test Method)Standard Test Method for Mechanical Hydrogen Embrittlement Evaluation of Plating Processes and Service Environments
Standard Test Method for Mechanical Hydrogen Embrittlement Evaluation of Plating Processes and Service Environments
SCOPE
1.1 This test method covers mechanical tests for the evaluation and control of the potential for hydrogen embrittlement that may arise from various sources of hydrogen as in plating processes, from fluids, cleaning treatments, maintenance chemicals, and gaseous environments that may contact the surface of steels.
1.2 The procedures and requirements are specified for five types of test specimens using a heat of AISI E4340 steel with demonstrated sensitivity. This test method is not intended to measure the relative susceptibility of other steels.
1.3 This test method assumes that AISI E4340 steel at 51HRC-54HRC, determined to be sensitive as specified in Table 1, is the worst case; that is, all other heat treated, high-hardness steels are less susceptible to hydrogen embrittlement.
1.4 For testing maintenance chemicals, the containment chamber must be isolated around the test specimen, as shown in Fig. 1 for Type 1a. If the test specimen and self-loading frame are to be immersed into the maintenance chemical, then the test fixture must be made from AISI E4340 steel except that it can be vacuum melted and heat treated to a lower hardness by tempering at 482 + 14°C (900 + 25°F) to a hardness of 40HRC-43HRC. This is done in order to minimize any polarization effects of galvanic coupling that would influence the test results.
1.5 Specimen geometries, equivalent loading conditions, and the pass/fail requirements for each type are also specified.
1.6 Classification -Hydrogen embrittlement tests can be performed with specimens as specified in the following:
1.6.1 Type 1-Notched:
1.6.1.1 Type 1a -Round bar, loaded in tension, under constant load.
1.6.1.2 Type 1b -Round bar, loaded in tension, with self-loading ring.
1.6.1.3 Type 1c -Round bar loaded in bending with self-loading frame.
1.6.1.4 Type 1d -C-rings loaded in bending with self-loading bolt.
1.6.2 Type 2 -Smooth (Unnotched).
1.6.2.1 Type 2a -Ring specimens loaded in bending with displacement bars.
1.7 This standard does not purport to address all of the safety problems, 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.
1.8 This test method is limited to hydrogen embrittlement testing of steels that are exposed to the following:
1.8.1 An electrochemical plating process.
1.8.2 Maintenance chemicals, subsequent to cadmium plate.
1.9 The values stated in acceptable metric units shall be regarded as the standard.
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e2
Designation: F 519 – 97
Standard Test Method for
Mechanical Hydrogen Embrittlement Evaluation of Plating
Processes and Service Environments
This standard is issued under the fixed designation F519; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
e NOTE—Fig. A3.2 was editorially changed to Fig. A4.2 in December 1997.
e NOTE—Note 3 was deleted in Fig. A2.1 and Footnote 11 has been added to Note A3.1 in July 2000.
1. Scope 1.5.1 Annex A1 details notched tensile specimens under
constant load; Annex A2 details notched round bars tensile,
1.1 This test method covers mechanical tests for the evalu-
bend,andC-ringspecimensusingaself-loadingfixture;Annex
ation and control of the potential for hydrogen embrittlement
A3 details a notched four point bend specimen that combines
that may arise from various sources of hydrogen in plating
sustained load and slow strain rate testing for hydrogen
processes, or from subsequent service environments that in-
embrittlementbyusingincrementalloadsandholdtimesunder
clude fluids, cleaning treatments, maintenance chemicals or
displacement control to measure a threshold stress in an
gaseous environments that may contact the surface of steels.
accelerated manner. The test is described as an accelerated
1.2 This test method is intended for process control of
(#24 h) incrementally increasing or rising step load test
hydrogenproducedbydifferentplatingprocessesandexposure
method that measures the threshold for hydrogen stress crack-
to different chemicals encountered in a service environment
ing that is used to quantify the amount of residual hydrogen in
andnottomeasuretherelativesusceptibilityofdifferentsteels.
the specimen. Annex A4 details a smooth O-ring under
1.3 ThistestmethodassumesthatairmeltedAISI4340steel
displacement control; Annex A5 details testing in a service
per MIL-S-5000 at 51 to 53 HRC is the worst case; that is, all
environment.
other heat-treated, high-hardness steels are less susceptible to
1.6 Specificrequirementsforthetwotypesofspecimenand
hydrogenembrittlement.Thesensitivitytohydrogenembrittle-
the seven specific loading and geometrical configurations are
ment shall be demonstrated for each heat of AISI 4340 steel
as listed:
used in the manufacture of test specimens.
1.6.1 Type 1—Notched Specimens
1.4 Test procedures and acceptance requirements are speci-
1.6.2 Type 1a: Round Bar Tension—Constant Load
fied for seven specimens of different sizes, geometries, and
1.6.3 Type 1a.1—Standard Size Annex A1
loading configurations. For plating processes, notched speci-
1.6.4 Type 1a.2—Oversized Annex A1
mens must exceed 200 h at a sustained load of 75% of the
1.6.5 Type 1b: Round Bar Tension—Self Loading Fixture-
fracture stress or exceed a threshold of 75% of the fracture
Annex A2
stress for a quantitative, accelerated (#24 h) incrementally
1.6.6 Type 1c: Round Bar Bend—Self Loading Fixture-
increasing or rising step load (RSL) test. For service environ-
Annex A2
ments, equivalent loading conditions and pass/fail require-
1.6.7 Type 1d: C-ring Bend—Self Loading Fixture-
ments for each specimen are specified.
Annex A2
1.5 Thistestmethodisdividedintotwomainparts.Thefirst
1.6.8 Type 1e: Square Bar Bend—Displacement
part gives general information concerning requirements for
Annex A3
hydrogen embrittlement testing. The second part is composed
1.6.9 Type 2—Smooth Specimens
of annexes that give specific requirements for the seven
1.6.10 Type 2a: O-ring—Displacement Control
specimens covered by this test method.
Annex A4
1.7 The values stated are in American Standard units.
1.8 This standard does not purport to address all of the
This specification is under the jurisdiction of ASTM Committee F07 on
safety concerns, if any, associated with its use. It is the
Aerospace andAircraft and is the direct responsibility of Subcommittee F07.04 on
responsibility of the user of this standard to establish appro-
Hydrogen Embrittlement.
priate safety and health practices and determine the applica-
Current edition approved May 10, 1997. Published August 1997. Originally
published as F519–77. Last previous edition F519–93. bility of regulatory limitations prior to use.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
F 519
2. Referenced Documents plating. It is intended to be used as a qualification test for new
plating processes and as a periodic inspection audit for the
2.1 ASTM Standards:
control of a plating process.
B851 SpecificationforAutomatedControlledShotPeening
4.2 Service Environment—This test method establishes a
of Metallic Articles Prior to Nickel, Autocatalytic Nickel,
2 means to determine the hydrogen embrittlement potential of
or Chromium Plating, or Final Finish
chemicals that may contact plated steel parts during manufac-
D1193 Specification for Reagent Water
turing, overhaul, and service life. The details of testing in a
E4 Practices for Force Verification of Testing Machines
service environment are found in Annex A5.
E8 TestMethodsforTensionTestingofMetallicMaterials
E18 Test Methods for Rockwell Hardness and Rockwell
5. Apparatus
Superficial Hardness of Metallic Materials
5.1 Testing Machine—Testing machines shall be within the
E29 Practice for Using Significant Digits in Test Data to
5 guidelines of calibration, force range, resolution, and verifica-
Determine Conformance with Specifications
tion of Practices E4.
E616 Terminology Relating to Fracture Testing
6 5.2 Gripping Devices—Various types of gripping devices
E709 Guide for Magnetic Particle Examination
shall be used in either tension or bending to transmit the
F1624 Test Method for Measurement of Hydrogen Em-
measured load applied by the testing machine or self-loading
brittlement Threshold in Steel by the Incremental Step
frame to the test specimen.
Loading Technique
5.3 Environmental Testing—For testing in service environ-
G5 Reference Test Method for Making Potentiodynamic
ments, an inert container and fixture arrangement that is
Anodic Polarization Measurements
suitably electrically isolated from the specimen or compen-
2.2 AMS Standards:
sated to prevent galvanic coupling shall be use for testing in
AMS 2430 Shot Peening
aqueousenvironments.Thecorrosionpotentialofthespecimen
2.3 Military and Federal Standards:
canbecontrolledwithareferenceSaturatedCalomelElectrode
MIL-S-5000 Steel, Chrome-Nickel-Molybdenum (E4340)
10 (SCE) or equivalent reference electrode such as withAg/AgCl
Bars and Reforging Stock
in accordance with Test Method G5.
MIL-H-6875 Heat Treatment of Steels, Process for
MIL-C-16173 Corrosion Preventive Compound, Solvent
6. Materials and Reagents
Cutback, Cold-Application
6.1 Materials:
Federal Specification QQ-P-416 Plating, Cadmium (Elec-
10 6.1.1 AISI E 4340 per MIL-S-5000.
trodeposited)
6.1.2 Aluminum oxide (150 grit or finer), and 180-grit
silicon carbide paper.
3. Summary of Test Methods
6.1.3 Clean shot, size in accordance with Specification
3.1 Plating Processes—Unstressed test specimens are
B851.
cleaned, plated, and baked in accordance with the plating
6.2 Reagents:
specificationtowhichtheprocessistobequalified.Specimens
6.2.1 Corrosion—Preventive compound, meeting require-
arethenmaintainedunderasustainedloadinairtomeasurethe
ments of MIL-C-16173, Grade 2.
time to rupture or under a rising step load to measure the
6.2.2 Cadmium—Cyanide electroplating bath (Federal
threshold stress.
Specification QQ-P-416). (Table 1).
3.2 Service Environments—Plated test specimens must first
be certified by the requirements stated herein for the plating
TABLE 1 Electroplating Bath Compositions and Operating
process. They are then tested under load in the service
Conditions for Sensitivity Test of Heats of AISI 4340 Steel
environment. The sequence of exposure to the environment
Item Treatment A Treatment B
and loading shall be as defined in Annex A5.
Bath composition:
Cadmium (as CdO) 4.5 oz/gal (33.7 g/L) 4.5 oz/gal (33.7 g/L)
4. Significance and Use
Sodium cyanide 14 oz/gal (104 g/L) 14 oz/gal (104 g/L)
(NaCN)
4.1 Plating Processes—This test method establishes a
Ratio NaCN to CdO 3 3
means to prevent hydrogen embrittlement of steel parts during
pH 12 12
manufacture by maintaining strict controls during production
Temperature 70–90°F (21–32°C) 70–90°F (21–32°C)
Sodium hydroxide 2.5 oz/gal (18.7 g/L) 2.5 oz/gal (18.7 g/L)
operations such as surface preparation, pretreatments, and
(NaOH)
Brightener such as 2.0 oz/gal (15.0 g/L) .
Rohco 20 3Lor
equivalent
Annual Book of ASTM Standards, Vol 02.05.
2 2 2 2
Electroplating current 10 A/ft (108 A/m ) 60 A/ft (645 A/m )
Annual Book of ASTM Standards, Vol 11.01.
Electroplating time 30 min 6 min
Annual Book of ASTM Standards, Vol 03.01.
Baking:
Annual Book of ASTM Standards, Vol 14.02.
Baking temperature 375 6 25°F (190 6 375 6 25°F (190 6
Annual Book of ASTM Standards, Vol 03.03.
14°C) 14°C)
Annual Book of ASTM Standards, Vol 15.03.
Baking time: Type 1 Do Not Bake 23 h
Annual Book of ASTM Standards, Vol 03.02.
Specimens
Available from AMS, 400 Commonwealth Dr., Warrendale, PA 15096.
Baking time: Type 2a 8h 23 h
Available from Standardization Documents Order Desk, Bldg. 4 Section D, Specimen
700 Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.
F 519
6.2.3 Maintenance chemicals, cleaners, paint strippers, and 7.2.7 After grinding, all specimens shall receive a stress
aqueous environments. relief bake at 375 6 25°F (190 6 14°C) for 4 h. A suitable
6.2.4 Chromic acid. protection from heat treating discoloration should be used.
6.2.5 Water—Specification D1193 Type IV. 7.2.8 Acid or cathodic electrolytic cleaning is prohibited.
7.2.9 Straightening after final heat treatment is prohibited.
7. Test Specimens
7.3 Storage:
7.1 Configuration:
7.3.1 Beforeplating,allspecimensshallbeprotectedduring
7.1.1 Seven specific dimensional drawings with tolerances
storage to prevent corrosion.Asuitable means of protection is
are given for the two types of specimens in the following
to coat the specimen with a corrosion preventive compound
annexes:
meeting the requirements of MIL-C-16173, Grade 2.
7.1.1.1 Type 1—Notched Specimens
7.4 Inspection:
7.1.1.2 Type 1a: Round Bar Tension—Constant Load
7.4.1 A lot shall consist of only those specimens cut from
7.1.1.3 Type1a.1—StandardSize—perFig.A1.1AnnexA1
the same heat of steel in the same orientation, heat treated
7.1.1.4 Type 1a.2—Oversized—per Fig. A1.2 Annex A1
together in the same furnace, quenched and tempered together,
7.1.1.5 Type 1b: Round Bar Tension—per Fig. A2.1, Fig.
and subjected to the same manufacturing processes.
A2.2, Fig. A2.3 Annex A2
7.4.2 All notched specimens shall be suitable for test
7.1.1.6 Type1c:RoundBarBend—perFig.A2.4,Fig.A2.5
purposes if the sampling and inspection results conform to the
Annex A2
requirements of Table 2.
7.1.1.7 Type 1d: C-ring Bend—per Fig. A2.6, Fig. A2.7
7.5 Sensitivity Test:
Annex A2
7.5.1 The sensitivity to hydrogen embrittlement must be
7.1.1.8 Type 1e: Square Bar Bend—per Fig. A3.1
demonstrated for each heat ofAISI 4340 steel by exposing six
Annex A3
trial specimens to two different embrittling environments after
7.1.1.9 Type 2—Smooth Specimens
manufacture and inspection in accordance with Section 7.
7.1.1.10 Type 2a: O-ring—per Fig. A4.1, Fig. A4.2 Annex
7.5.2 Three specimens shall be electroplated under the
A4
highly embrittling conditions produced in a cadmium cyanide
bath by Treatment A (Table 1) and the remaining three
NOTE 1—The notched round bar tension, bend, and square bar bend
specimens shall be electroplated under the less embrittling
shall be loaded in the longitudinal grain direction, but the C-ring and
O-ring can only be loaded normal to the longitudinal grain direction. conditions of Treatment B (Table 1). An equivalent plating or
imposedpotentialmaybeusedifitssensitivityisdemonstrated
7.2 Manufacture:
to be equivalent to that found in Table 1.
7.2.1 For all notched round specimens, a stress concentra-
tion factor (K)of3.1 6 0.2 shall be maintained.
t
TABLE 2 Lot Acceptance Criteria for Type 1 Notched Specimens
NOTE 2—For the relationship between geometry and K, see Peterson,
t
R. E., Stress Concentration Factors, John Wiley and Sons, 1974.
Sampling of
Type Item Requirement/Method
Each Lot
7.2.2 If the 60° notch angle does not permit plating to the
A
1 Hardness 5 % 51 to 53 HRC per ASTM
root of the notch, then an angle of 90° 6 1° shall be used. For
Test Method E 18.
theType 1.1 specimen, the K of 3.1 6 0.2 shall be maintained
Round the average of
t
three readings per
by reducing the root radius of the notch to 0.008 6 0.001 in.
specimen per Practice
for the 90° notch.
E 29.
7.2.3 Thetestspecimensshallbeproducedfromnormalized
1 Dimensions 100 % Meet tolerances of
corresponding
andtempered,hotorcolddrawnbarstock,AISI4340steelper
drawings. Notch
MIL-S-5000 and heat treated per MIL-H-6875 so as to meet
dimension verified with
the hardness requirement of 51 to 53 HRC per Test Method
shadow graphic
projection at 50 to
E18.RoundingperPracticeE29permitsanabsolutehardness
1003.
range of 50.6 to 53.4 HRC of the average of three measure-
1 Notched Fracture 10 ea NFS of each specimen
ments. Strength (NFS) must be within 10 ksi of
the average.
7.2.4 Tolerances unless otherwise specified are:
1c Self-loading 10 ea Alternate: The number of
X.X 60.1 in.
Notched round bar turns of the loading
X.XX 60.01 in.
bend fixture, bolt, which is required
X.XXX 60.001 in.
Fig. A2.5 to produce fracture in
each specimen, must be
7.2.5 The surface finish of all notches shall be 32 RMS or
within 5 % of the
average.
better. The other surfaces shall have a finish of 63 RMS or
1d Self-loading 10 ea Alternate: The change in
better.
Notched C-Ring diameter at fracture
7.2.6 The entire notch shall be ground to size after quench-
bend fixture, load specimens for each
Fig. A2.6 specimen must be
ingandtemperingtofinalhardnessbeforeplating.Single-point
within 0.005 in. of the
turning of the notch configuration is not permitted. Burnishing
average.
of the notch is not permitted. The notch shall not be shot
A
If the hardness requirements of any of the sampled specimens are not
peened or receive any blasting/mechanical cleaning operation
satisfied, only those specimens of the lot that are individually inspected for
after the notch is ground to size. conformance to these requirements shall be used for testing.
F 519
7.5.3 Each heat of steel shall be of suita
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