STANDARD OPERATING PROCEDURE FOR

SULFIDE STRESS CRACKING (SSC) TEST OF

STEEL PLATE

00 December 5th , 2014 Issued for review MD HJ SW

Rev. Date Revision Description Prepared by Reviewed by Approved by

METALLURGY AND MATERIAL ENGINEERING LABORATORY

Document No.
FACULTY OF MECHANICAL AND AEROSPACE ENGINEERING
052/SOP/Test/MT/12/2014 INSTITUT TEKNOLOGI BANDUNG
This document is property of Metallurgy and Material Engineering Laboratory – FTMD – ITB and must not be handed to a third
party or reproduce completely or in part without the explicit written consent of Metallurgy and Material Engineering Laboratory –
FTMD – ITB
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A. Scope :
This procedure covers the testing of metal and welding subjected to bending stress for
resistance to failure of steel plate in low pH aqueous environment containing Hydrogen
Sulfide (H2S).

B. Reference Standard
1. NACE TM 0177-05, Laboratory Testing of Metals for Resistance to Sulfide Stress
Cracking and Stress Corrosion Cracking in H2S Environments
2. ASTM G 39 – 99, Standard Practice for Preparation and Use of Bent-Beam Stress-
Corrosion Test Specimens.
3. API Specification 5L 45th Ed. 2013 Annex H.4, Acceptance Criteria for PSL 2 pipe
ordered for sour service.

C. Procedure
1. Reagent
 The test solution shall consist of nitrogen gas for purging, H2S gas, and solution B
(5.0 wt% sodium chloride, 2.5 wt% glacial acetic acid, and 0.41 wt% sodium acetate
dissolved in distilled or deionized water).
 Preparation of solution B, see Appendix A.

2. Test Specimens
 Testing frequency is 1 per heat number.
 The test specimen location for steel plate shall be at one end, mid-width of the plate,
with the longitudinal axis of the test specimen parallel to the principal rolling direction
of the plate. See Figure 1.
 Three test specimens shall be taken from each steel plate.
 Test specimen procedure include dimension refer to ASTM G 39-99
 Test specimens shall be subjected to four-point bending load. Figure 2 shows the
schematic diagram of loading system
 Test specimens shall be a flat strip of 25 mm wide and 127 mm long and 3 mm
thickness and shall contain a section of the longitudinal weld at its centre (if any).
 Specimens may be flattened prior to machining test specimens.
 The test specimens should be milled to an approximate size and then surface
ground to final dimensions. Surfaces and edges of the test specimen shall be
ground by hand on 240 grit emery paper.
 For specimen identification, the test specimens may be stamped or vibratory
stenciled.
 If the plate is cladded, The roller of the fixture and the plate shall be coated with
epoxy coating on the entire surface except the cladding metal surface before the
testing.
 The cladded surface shall be positioned on the tension surface (facing down) of the
fixture
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150

T=3

25
Figure 1 Location of Test Specimens

40 mm
20 mm 20 mm

Specimen : 127 mm x 25 mm x 3 mm

Ø : 10
mm
Steel
80 mm
Figure 2 Schematic Specimen and Holder Configurations
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3. The schematic diagram of apparatus used for testing can be seen in Figure 3.

Figure 3 Schematic Diagram for SSC Testing

4. Preparation of specimen’s surface :

- Blank for test specimen may be removed by sawing, grinding or machining. If a blank
is torch out, the HAZ of the torch cut surface shall be completely removed by
grinding, sawing or machining
- The four cut edge surfaces of each test specimen shall be ground either wet or dry
and finished with 320 grit papers.
- Identification or marking specimen used hard stamp.

5. Cleaning and Storing of Specimen

 The test specimens and jigs shall be degreased with solvent (1,1,1-trichloroethane )
and rinsed with acetone.
 The stressed section shall not be handled or contaminated after cleaning.
 After degreased, specimen may be stored in a desiccator or inhibited oil until ready
for testing.

6. Test Specimen Loading

 Measure the specimen accurately to determine their thickness.
 The test specimens shall be stressed to 0.72 x SMYS.
 Use the following formula to calculate the deflection.

Where:
 = maximum tensile stress,
E = modulus of elasticity,
t = thickness of specimen,
y = maximum deflection (between outer supports),
H = distance between outer supports,
A = distance between inner and outer supports.
 Place the test specimen on the four-point bending jig, put the load up to the desired
deflection. The inner weld shall be positioned on the tension side.
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7. Test Specimen Exposure

 Sulfide Stress Cracking test shall be performed in accordance with NACE TM 0177-
05, using standard test solution B (5.0 wt% NaCl, 2.5 wt% CH 3COOH, and 0.41 wt%
CH3COONa dissolved in distilled or deionized water). Preparation of solution B, see
Appendix A.
 The ratio of the volume of test solution to the total surface area of the test
specimens shall be a minimum of 30±10 mL per cm2.
 The test solution shall be deaerated within the test vessel by Nitrogen gas purging
at a rate of at least 100 mL/min for at least one hour/liter solution.
 Measure the pH solution in the chamber. Initial test solution pH is expected to range
between 3.4 and 3.6.
 Place the loaded specimens in the test vessel, then the vessel shall be sealed and
leak tested.
 The solution shall be purged again with Nitrogen gas of at least 100 mL/min for at
least 20 min after sealing the test vessel.
 The test solution shall then be saturated (2200 ppm minimum) with H2S at a rate of
at least 100 mL/min for at least 20 min/L of test solution.
 The H2S in the test vessel shall be replenished periodically by bubbling H 2S for a
duration of 30 min at a rate of at least 100 mL/min per liter of test solution three
times per week for the duration of the test. The days for the replenishment should be
the first, third, and fifth day of each week
 During the test pH measurement shall be carried out after initial H2S purging and in
daily basis.
 During the test, pH shall not exceed 4.0. This value will be used as an indication that
the solution is still saturated with H2S. If the pH exceeds 4.0, the test is invalid
 The temperature of test solution shall be 24 ± 3 oC
 The pressure of the test solution shall be ambient pressure or equal to atmospheric
pressure.
 For First Day Production (FDP) and Last Day Production (LDP), the test shall be
terminated after 720 hours.
 For PQT and production sample test duration shall be 96 hours.

8. Safety Consideration in Handling H2S Toxicity

 Tests shall be performed in a hood with adequate ventilation to exhaust all of the
H2S.
 The H2S flow rates during the test should be kept low to minimize the quantity
exhausted. A 10% caustic absorbent solution for effluent gas can be used to further
minimize the quantity of H2S gas exhausted. This caustic solution needs periodic
replenishing.
 Suitable safety equipment shall be used when working with H 2S.
 H2S detector shall be provided and used to detect maximum H2S content 10 ppm
 When the smell of H2S is detected, the testing equipment shall be checked of any
leakage and repaired immediately.
 Gas masks shall be provided and employed during testing preparation and daily pH
measurement.
 Particular attention should be given to the output pressure on the pressure
regulators.
 Gas cylinder, tubes, valves and testing chamber shall be securely fastened to
prevent tipping and breaking. Regular checking of any gas leakage shall be carried
out, especially before testing started.
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9. Check list procedure for SSC testing, see Appendix B

10. Check list of apparatus and consumable for SSC Testing, see Appendix C

11. Photographs of SSC test apparatus, see Appendix D

D. Evaluation
1. After completion of test, remove the specimens out of jigs, clean the specimens, and
examine the test specimen surface by means of 10 x visual examination for evidence of
cracking.
2. Acceptance Criteria: Acceptable if no cracks are visible at a magnification of 10 X.

E. Report
The Following shall be reported:
 Method of testing including the type of solution used.
 Pipe Number and Heat Number of As Received specimens.
 Number, code and location of specimens.
 Photo macrograph of each test specimen.
 Before testing
 During Testing
 After testing
 Any crack evidence for each test specimens.
 SSC test Log Sheet containing daily pH and temperature measurement. (see
Appendix E for the log sheet format)
 Comparison result of SSC actual data with the acceptance criteria.
 Photo micrograph of any imperfect and cracked specimens.
_____________________________
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Appendix A: Preparation of solution B - SSC (NACE TM0177-2005)

Test Solution B is an acidified and buffered, H2S saturated aqueous brine solution. Test Solution
B shall consist of 5.0 wt% sodium chloride, 2.5 wt% glacial acetic acid, and 0.41 wt% sodium
acetate dissolved in distilled or deionized water (e.g., 50.0 g of NaCl, 25 g of CH 3COOH, and
4.1 g of CH3COONa dissolved in 921 g of distilled or deionized water).
Test solution pH before or after H2S saturation but before contact with a test specimen is
expected to range between 3.4 and 3.6. During the test, pH may increase but shall not exceed
4.0. If the pH exceeds 4.0, the test is invalid. If the test-solution-volume to test-specimen-
surface-area ratio is maintained and steps are taken to exclude oxygen from the test vessel as
specified in this standard, the pH will not exceed this value.

Solution Composition
The amount of each component needed to prepare 1L of Test Solution B:
Demineralized water : 1000 mL = 1000 * 0.998 = 998 g
NaCl : 998 / 921 * 50 = 54.180 g
CH3COONa : 998 / 921 * 4.1 = 4.443 g
CH3COOH : 998 / 921 * 25 / 1.05 = 25.8 mL

Solution 1L 6L 18 L 20 L
Volume
NaCl 54.180 g 325.08 g 975.24 g 1083.6 g
CH3COOH 25.8 mL 154.8 mL 464.4 mL 516 mL
CH3COONa 4.443 g 26.658 g 79.974 g 88.860 g
Demineralized
balanced balanced balanced balanced
water

Procedures
Preparation of 1L Solution:
 Weigh out 49.9 g of NaCl on a watch glass, and then transfer it directly into a beaker of
1000 mL.
 Weigh out 4.092 g of CH3COONa on a watch glass, and then transfer it directly into the
beaker.
 Add about 800 mL of demineralized water to the beaker and stir the solution until all the
solids are dissolved.
 Add 23.8 mL of CH3COOH to the beaker and stir the solution gently.
 Transfer the solution to a volumetric flask of 1000 mL using a funnel. Rinse the beaker,
stirring rod and funnel thoroughly, and add the washings into the volumetric flask.
 Finally, additional demineralized water is added to the volumetric flask until the liquid
level reaches the calibration mark. The flask is capped and inverted as before until the
contents are thoroughly mixed.
Preparation of 2 L or more Solution:
 Weigh out such amount of NaCl and CH3COONa (as shown on the Table) on a watch
glass, and transfer it directly into a beaker of 2000 mL.
 Add about 1500 mL demineralized water to the beaker and stir the solution until all the
solids are dissolved.
 Add certain volume of CH3COOH (as shown on the Table) to the beaker and stir the
solution gently.
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 Transfer the solution to a volumetric flask of 2000 mL using a funnel. Rinse the beaker,
stirring rod and funnel thoroughly, and add the washings into the volumetric flask.
 Add demineralized water to the volumetric flask until the liquid level reaches the
calibration mark. The flask is capped and inverted as before until the contents are
thoroughly mixed.
 Transfer the solution into a vessel, and add the rest of needed volume of demineralized
water (needed volume – 2 L).

Solution pH at H2S Saturation

pH calculation:
[𝑎𝑐𝑖𝑑]
𝑝𝐻 = 𝑝𝐾𝑎 − log [𝑠𝑎𝑙𝑡] , where Ka = acid buffer constant.
[acid]: concentration of all acidic compounds in the solution, CH3COOH + H2S.
[salt]: concentration of conjugate base salt in the solution, CH 3COONa.

A buffer solution contains certain concentrations of acid and its conjugate base salt will have a
certain pH value. In case of Test Solution B, the presence of 2.5 w-% CH3COOH and saturated
H2S will give pH 3.4 before corrosion process. When corrosion proceeds, H + will be consumed.
Without addition of H2S, solution pH will raise and become greater than 4.0. Sufficient H 2S
addition will keep its saturation and solution pH value  4.0.
As long as the pH value does not exceed 4.0, the solution is considered as saturated with H 2S.
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Appendix B: Check list procedure for SSC testing

A PREPARATION
1 Provide the test apparatus and consumables
Receive the SSC specimens, check and confirm the coded specimen with PO
2
letter, check the specimen dimension
3 Record all as-received specimens (macrophotograph and other documentations)
4 Flatten the specimens (if necessary)
Cut and mill the specimens into final standardized dimension:
5
(127-254 mm) x (25-51 mm) x thickness
6 Grind the as-machined specimens with emery paper up to 240 grit
7 Measure the as-ground specimen dimension
8 Macro etch to determine specimens weld area (if necessary)
9 Mark and macrophotograph the as-ground specimens
10 Calculate and provide Solution B: 30 ± 10 mL/cm 2 of specimens total surface area
11 Calculate the deflection for each specimen
12 Provide detail SOP, pH Log-Sheet, and deflection table
13 Install the SSC testing assembly
B SPECIMEN LOADING AND TESTING
1 Check the testing apparatus and consumables
2 Turn on the exhaust system and the warning light
3 Prepare and use all safety equipment
4 Prepare the testing assembly; re-check every connection; calibrate pH meter
5 Degrease and rinse the specimens and fixtures
6 Place the specimens into desiccator
7 Provide the required volume of solution B and measure the pH
8 Provide 10% NaOH solution (ex. 1kg NaOH solid in 10L aqua dm)
9 Load the solution B into the vessel
10 Purging the test solution with N2 gas
11 Measure and record the initial pH solution, time, and room condition
12 Bend each specimen according to the calculated deflection; do not over bend!
13 Loading the specimens and fixtures
14 Purging the test solution with N2 gas
15 Bolt the test vessel tight enough; do not over tight
16 Seal the test vessel
17 Leak test; correction if any leak occurs
18 Stop N2 purging; make sure all the valves are closed
19 Measure and record the time, pH solution, and room condition
20 Start purge the solution with H2S gas; open the valves carefully
21 Stop H2S purging; make sure all the valves are closed
22 Measure and record after H2S purging condition (=Start SSC Test)
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Appendix B: Check list procedure for SSC testing (cont’d)

B SPECIMEN LOADING AND TESTING

Check the N2 and H2S regulator valve, hose line panel, and every connections for
23
any leakage
24 Record inappropriate parameters (if any)
25 Clean the testing room
26 Remove the safety equipments
27 Turn off the lamps except the warning light
C MONITORING
1 Provide the test apparatus and consumables
2 Prepare and use all safety equipment
3 Calibrate the pH meter
4 Measure and record testing condition, twice a day
Re-purge the H2S periodically at first, third and fifth day of each week
5
(or daily if it is necessary)
6 Stop H2S purging; make sure all the valves are closed
7 Measure and record after H2S purging condition
8 Leak test, correction if any leak occurs
Check the N2 and H2S regulator valve, hose line panel, and every connections for
9
any leakage
10 Record inappropriate parameters (if any)
11 Clean the testing room
12 Remove the safety equipments
13 Turn off the lamps except the warning light
D SPECIMEN UNLOADING
1 Provide the test apparatus and consumables
2 Prepare and use all safety equipment
Measure and record the final testing condition
3
(=Stop SSC Test)
4 Make sure all valves are closed
5 Disassembly the vessel from the hoseline
6 Take out and place the test vessel and solution entrapment to the open-air
7 Unseal and open the test vessel
8 Take out the specimens and fixtures
9 Dispose mixed ex-solutions into the waste sewer
10 Clean and rinse the specimens
11 Place the specimens in desiccator
12 Clean the apparatus and the testing room
13 Remove the safety equipments
14 Turn off all the lamp
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Appendix B: Check list procedure for SSC testing (cont’d)

E EVALUATION OF TEST SPECIMENS

1 Provide and check the test apparatus and consumables
2 Record all as-tested specimens (macrophotograph and other documentations)
3 Re-check the specimen codes
4 Prepare the grinding and polishing apparatus
5 Grind and polish the specimens
6 Provide the apparatus and the log-sheet for specimen evaluations
Observe the polished specimens (microphotography, any observed crack, and
7
other documentations)
8 Prepare the etchant solution and etch all the specimen
Observe the etched specimens (microphotography, any observed crack, and other
9
documentations)
10 Measure the crack length (if any)
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Appendix C: Check list of apparatus and consumable for SSC Testing

A PREPARATION
1 As Received Specimen Preparation
permanent markers
camera and statif
caliper
flattening (universal) machine
cutting machine
milling machine
grinding machine
emery paper; up to 240 grit
etchant
desiccator
silica gel
tissue paper
grafir
2 Solution B Preparation
NaCl, CH3COOH, CH3COONa, distilled or
deiozined water
weighing scale
bucket
water dipper
spatula
pH meter + buffer
3 Testing Assembly
N2 gas
H2S gas
hose line and panel
flowmeter
1 set of test vessel
scissor
cutter

4 Detail SOP, pH log sheet forms, and

deflection table
B SPECIMEN LOADING AND TESTING
1 Safety Equipments
lab coat
gas mask
solvent resistance gloves
normal/latex gloves
H2S gas detector
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Appendix C: Check list of apparatus and consumable for SSC Testing (cont’d)

B SPECIMEN LOADING AND TESTING

2 Specimens Cleaning and Storing
trichloroethylene
acetone
desiccator
silica gel
tissue paper
3 10% NaOH Solution Preparation
NaOH powder
aqua DM
spatula
4 Deflecting Equipment
four-point bend jig
jig holder
dial indicator
5 Measuring Equipments
pH meter + buffer
thermometer
measuring cylinder
6 Miscellanous
Solution B
bucket
water dipper
spanner
beaker glass
leak test foam
silicon rubber sealant
C MONITORING
1 Safety Equipments
lab coat
gas mask
solvent resistance gloves
normal/latex gloves
H2S gas detector
2 Measuring Equipments
pH meter + buffer
thermometer
3 Miscellaneous
beaker glass
leak test foam
silicon rubber sealant
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Appendix C: Check list of apparatus and consumable for SSC Testing (cont’d)

D SPECIMEN UNLOADING
1 Safety Equipments
lab coat
gas mask
solvent resistance gloves
normal/latex gloves
H2S gas detector
2 Measuring Equipments
pH meter + buffer
thermometer
3 Specimens Cleaning and Storing
detergent
sponge
wash brush
acetone
desiccator
silica gel
tissue paper
4 Miscellaneous
beaker glass
cutter
scissor
spanner
E EVALUATION OF TEST SPECIMENS
1 As Tested Specimen Preparation
permanent marker
grinding machine
polishing machine
emery paper
polishing cloth
diamond paste
etchant
specimens container
silica gel
tissue paper
2 Examination Equipment
camera and statif
evaluation log-sheet
magnification lens
optical microscopes
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Appendix D: Photographs of SSC test apparatus

1. MACHINING APPARATUS

Cutting Machine Flattening Machine and Jigs

Vibratory Stenciled Machine Grinding Machine

Polishing Machine Milling Machine

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Appendix D: Photographs of SSC test apparatus (cont’d)

2. SSC TESTING ASSEMBLY

SSC Test Assembly

3. MEASUREMENT / EXAMINATION DEVICE

Caliper Camera and Statif

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Appendix D: Photographs of SSC test apparatus (cont’d)

3. MEASUREMENT / EXAMINATION DEVICE

Four-Point Bend Jig, Jig Holder

Magnification Lens Stereo Optical Microscope
and Dial Indicator

Inverted Optical Microscope + Image

pH Meter + Buffer
Analyzer Software

Thermometer Weighing Scale

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Appendix D: Photographs of SSC test apparatus (cont’d)

4. SAFETY EQUIPMENT

Gas Mask H2S Detector

Lab Coat Normal Gloves

Solvent Resistance Gloves Warning Light

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Appendix E: SSC Log Sheet X hours (X = 96 or 720)