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PROCEDURA OPERATIVA PO 04-175 RC
OPERA TING PROCEDURE REV. 0
Sulphide Stress Corrosion Cracking Test DATA 23/02/15
(Four point bending) PAG. 1 DI 6

SULPHIDE STRESS CORROSION CRACKING

TEST
(FOUR POINT BENDING)

CONTENTS

1. SCOPE AND APPLICATION .. 2

2. DEFINITIONS ........................... 2
3. RESPONSIBILITY......... .......... 2
4. REFERENCE DOCUMENTS .. 2
5. TESTING APPARATUS ........... 3
6. TEST METHOD ........................ 3
6. / Reagents .................................................................................................................................... 3
6.2 Test solutions ............ ... ............................................................................................................ 3
6.3 Test specimens ........................................................................................................................... 3
6.4 Stress applied ............................................................................................................................ 4
6.5 Testing sequence........................................................................................................................ 5
6.6 Failure detection ....................................................................................................................... 3
6.7 A cceptance criteria................................................................................................................... 6
REPORTING OF TEST RESULTS ............ 6
 SIDER TEST S.r.l
STATE FUNCTION PERSONNEL DATE SIGNATURE

Issue (’hem. Dept. Manager Stefano Antonielli 23/02/2015

Verified i .aboralory Manager Paolo Amani 23/02/2015

Approved Quality System Manager Barbara Ghibnudo 23/02/2015

Z:\QUALITA\OOCUMENTLLABORATORIO\POJUPO_IUPO 04-175 RC (an) R00 (SSC_4 point bending) PAOLO.doc
 S1DER TEST S.r.l
LA noRA TOR JO PRO) K E COUAUM/CONTROL! J NON DISTRUTT/I'I MECHANICAL AND
CHEMICAL TESTING/NONDESTRUCTIVE TESTING

PROCEDURA OPERATIVA PO 04-175 RC

REV. 0 DATA
OPERA TING PROCEDURE 23/02/15 PAG. 2
Sulphide Stress Corrosion Cracking Test DI 6
(Four point bending)
1. SCOPE AND APPLICATION
This document describes a general method for determining the susceptibility to stress corrosion cracking
of steel samples in H2S environment by Method B of NACE TM0177 and ASTM G39. It involves
deflecting each test specimen in a series by applying a bending stress, the stressed test specimens then
are exposed to the test environment and the failure (or no-failure) by cracking is determined.
2. DEFINITIONS
LM Laboratory Manager
QSM Quality System Manager
CDM Chemical Department Manager
OP Operating Procedure

3. RESPONSIBILITY
This OP is issued under the responsibility of CDM, verified by LM and approved by QSM.
Each qualified operator is responsible for the correct application of this OP and for ensuring that all
equipment employed is identified and calibrated.

4. REFERENCE DOCUMENTS
NACE TMO177 2005
Laboratory Testing of Metals for Resistance to Sulfide
Stress Cracking and Stress Corrosion Cracking in H2S
Environments.
NACE TM0284
Evaluation of Pipeline and Pressure Vessel Steels for
2011 Resistance to Hydrogen-Induced Cracking Solutions A
and B.
ISO 7539-2 1989

Corrosion of metals and alloys. Stress corrosion testing.

Part 2 - Preparation and use of bent beam specimen.
Standard Practice for the Preparation of Substitute Ocean
ASTM Dl 141 1998 (R2013)
Water.
 SIDER TEST S.r.l
LA no/n roRU) PRO\ T: E COLLA uni / CONTROL!.! NON DIS I HUTTIVI
MECHANICAL AND CHEMICAL
TESTING/NONDESTRUCTIVE TESTINU
PO 04-175 RC
REV. 0 DATA
PROCEDURA OPERAT/VA 23/02/15 PAG. 3
OPERA TING PROCEDURE DI 6
Sulphide Stress Corrosion Cracking Test
(Four point bending)

5. TESTING APPARATUS
All equipment and materials employed are clearly identified and calibrated.
The following apparatus and equipment are used:
• A vessel made of a material inert to the test environment, capable of being purged to remove
oxygen before beginning the test and of keeping air out during the test. The vessel is sized to
maintain a solution volume of 30 ± 10 ml/cm2 of test specimen surface area. The volume is less
than 10 L per test. The vessel is valved at both inlet and outlet to prevent contamination on the test
solution by oxygen.
• A deflection support with 4 fixing points for bending the samples (fig. 1). The support
immersed in the test solution resist general corrosion (UNS S31600 is commonly used). Fixture
elements contacting the test specimen are electrically isolated from it.
A fritted glass bubbler is used to introduce the inert gas and H2S below the array of the test
specimens. The bubbles do not impinge on the test specimens.
6. TEST METHOD

Reagents
6.1
• Nitrogen gas for purging
• H2S gas (99.5%)
Synthetic seawater
•

6.2 Test solutions

Solution B of NACE TM0284 shall be used.
The synthetic seawater shall be prepared in accordance with ASTM D1141 Stock Solutions No. 1 and No.
2 (without heavy metal ions).

NOTE; mS IS HIGHLY TOXIC AND MUST BE HANDLED WITH CAUTION.

6.3 Test specimens

6.3.1 Number, location, orientation and size

One sample shall be taken from the extrados of the bend body; three test pieces shall be taken from each
sample.
 SIDERTEST S.r.l
LAIIORA TORHt PROl E E COLIAUDI/CONTROLLI NON
DlSTRUTTfl7 MECHANICAL AND CHEMICAL TESTING/NONDESTRUCTIVE
TESTING
PO 04-175 RC
PROCEDURA OPERATIVA REV. 0 DATA
OPERA TING PROCEDURE 23/02/15 PAG.
Sulphide Stress Corrosion Cracking Test 4DI 6
(Four point bending)

Whatever the pipe thickness, the specimen is taken as close as possible to the pipe inside surface, with a
minimized depth of machining to obtain flat surfaces.
The specimen is cut longitudinally to pipe axis.
The dimensions of the bent-beam test specimen are 15 ± 0.13 mm wide, 5 ± 0.13 mm thick and from 115
to 140 ±1.3 mm long. After machining, test specimens are stored in a desiccator or in uninhibited oil
until ready for testing.
The test specimen is milled to an approximate size and then surface ground to final dimensions. The last
two passes on either side arc restricted to removal of 0.013 mm per pass (care must be taken to prevent
overheating).
Specimen is successively ground using a 280 grit emery paper involving the edges and making sure that
scratches are parallel to the test specimen axis.
6.3.2 Specimen identification
Specimens are stamped or stenciled m a region within 13 mm of either end on the compression side.

6.3.3 Specimen cleaning

The test specimen is degreased with solvent and rinsed with acetone.
The stressed section of the test specimen is not be handled or contaminated after cleaning.

6.4 Stress applied 6.4.1 Stress applied

If the material class is not specified SSC tests are conducted at the stress level of 80% of Specified
Minimum Yield Strength of pipe base material.
The deflection, which the specimen shall receive, is calculated on the base of the following equation:
<r -(3-// 2 —4 A2)
y-—* -------------------- -
12- E t
y = maximum deflection
o = 80% of actual yield strength
E = elasticity modulus of material
t = thickness of specimen
H = distance between outer supports
A = distance between inner and outer supports
 SIDER TEST S.r.l
LA BORA TORIO PROVE E COI.IA uni / CONTROL!J Nos DISTRUTTI I T
MECHANICAL AND CHEMICAL
TESTING/NONDESTRUCTIVE TESTING
PO 04-175 RC
REV. 0 DATA
PROCEDURA OPERATIVA 23/02/15 PAG.
OPERA TING PROCEDURE 5DI 6
Sulphide Stress Corrosion Cracking Test
(Four point bending)
Fig-1
Test specimens are stressed in fixtures by deflecting them to the nearest 0.0025 mm with dial gauge and

fixture:

6.5 Testing sequence

The deflection is carefully applied to avoid exceeding the desired value. If the desired deflection is
exceeded, the test shall be discarded.
The stressed test specimens shall be cleaned and placed into the test vessel.

Test duration:
720 hours. Test time shall begin immediately uoon
completion of the initial 60-minute FES
introduction period.
Test temperature: 24 ± 3°C

fiH HjS cone.

Nitrogen gas at a rate of at least 100 ml/min per / /
Pureinz of the emotv test liter of test vessel volume
vessel with specimens
already inside
Nitrogen gas at a rate of at least 100 ml/min per 1 8 2±0.1 /
Pureins of the test
solution in a separate hour / liter of solution.
vessel
8.2 ±0.1 /
Introduction of solution
into the test vessel
 iiJ S1DER TEST S.r.l
Li BORA TORIO PR(H L E CtH.lAUDl / CONTROL!.! N()N DI STRUTT!) 7
MECHANICAL AND CHEMICAL
TESTING/NONDESTRUCTIVE TESTING
PO 04-175 RC
PROCEDURA OPERATIVA
REV. 0 DATA
23/02/15 PAG. 6
DI 6
OPERA TING PROCEDURE
Sulphide Stress Corrosion Cracking Test (Four point bending)
Nitroeen gas at a rate of at least 100 ml/min per at 8.2 ±0.1 /
Pureine of the test
solution into the test least 20 minutes.
vessel
11 & saturation 4.8 ±5.4 /

H>S eas at a rate of at least 100 ml/min Der at

least 20 minutes / liter of test solution
HS neriodicaUv 4.8 ±5.4 /
replenished HxS eas at a rate of at least 100 ml/min Der liter of
solution for 20 to 30 minutes

End of test After 720 hours. 4.8 ±5.4 /

6.6 Failure detection

Crack presence is determined with the aid of a low-power binocular microscope. If the test specimen
contains only one or a few cracks, the shape of the test specimen may have changed considerably,
predominantly by kinking; this feature help to identify cracked test specimens. However, if many cracks
are present, a shape change may not be apparent. Because corrosion products may obscure cracks, a
careful examination is mandatory. Mechanical cleaning or metallographic sectioning of the test specimen
may be necessary in these instances to detect cracks. Failure is cracking of the test specimen.
Consequently, following exposure, the surface of the test specimens should be cleaned and visually
inspected at 10X for evidence of cracking following a 20- degree bending by hand. Further
metallographic examination can also be performed in case of visual examination does not provide any
conclusion.
Test specimens found to contain cracks shall be considered failed.
6.7 Acceptance criteria
No crack or rupture shall occur on any of the test specimen within the 30-day period of the test.
For evaluation, only SSC cracks and Stress Oriented HIC (SOHIC) are to be considered. Little grooves or
pits caused by corrosion loss will not be considered.

7. REPORTING OF TEST RESULTS

For every examination a test report (RC- R_SSCCStd) must be issued and filled in in all its parts.