JINDAL SAW LIMITED

Presentation on

Sour Service & Hydrogen

Induced Cracking

Contents

Introduction

What is HIC, SOHIC, Blistering and SSCC?

List of Equipments in NACE Lab

Typical Hydrogen Induced Cracking Test Method

Sample preparation ?

Cleaning and storing.

Solution preparation.

Orientation of sample in test vessel

Purging and introduction of HS.

Evaluation of test specimen.

Measuring Crack

Reporting

Safety precaution

Introduction
Sour Service
Definition : As per ISO 15156
Exposure to oilfield environments that contain

H2S and can cause cracking of materials by

the mechanisms addressed by ISO 15156-1
Mechanisms in ISO 15156

SSC, HIC, SOHIC, SZC etc.

IntroductionContinue
The hydrogen driven cracking is observed in
several modes/mechanism. The modes or
mechanisms are sulfide-stress corrosion
cracking (SSC), hydrogen blistering,
hydrogen-induced (stepwise) cracking (HIC),
and stress oriented hydrogen-induced
(stepwise) cracking (SOHIC).
The wet H2S /Hydrogen cracking mechanisms
require the presence of an aqueous phase,
temperatures from ambient to 150C, and the
evolution of hydrogen by a corrosion reaction
at the environment/steel interface.

IntroductionContinue
The presence of hydrogen ions does not strongly
promote its absorption into the steel at the
interface. Presence of the bi-sulfide (HS -) promote
hydrogen absorption into the steel, poisoning the
recombination of hydrogen into a gas in the
corrosion reaction. HS- promote the transport of
hydrogen across the environment-metal interface
and promote blistering, HIC, and SOHIC.
The cracking mechanism for SSC requires
extremely low concentrations of hydrogen in the
metal (5 ppm). Low quantity of HS- can produce
this level of hydrogen in the steel.

IntroductionContinue
Typical Reactions
Following two reaction takes place in corrosion
Fe = Fe+2 + 2e --- Anodic Reaction
2H+ + 2e =2 Ho --- Cathodic Reaction
Hydrogen produced at cathode either enters
into the steel (in the presence of H2S/HS-) or
converts into H2 gas and (in the absence of
H2S/HS-) escapes.
HS- Ion produced by following reaction
H2O+H2S= H3O+ + HS-

What is HIC
This type of cracking occurs in an

aqueous environment with HS. when

there is no external stress. Crack are
generated parallel to the plate surface,
starting from nonmetallic inclusion
present in the steel and progress
linearly or step like from with the
passage of time(see figure 1)

HIC Cracking (Figure 1)

What is SOHIC
SOHIC is a hydrogen-damage mechanism

like HIC. The damage mechanism, however,

is driven not only by the high pressures that
are generated by the hydrogen at the
inclusion to steel interface, but also by the
external applied stress. These stresses
cause the crack path between inclusions to
move more directly through the plate. The
cracking morphology is more similar to a
ladder than a stair step. The inclusions link
not as stair steps, but more in a vertical
direction like the rungs on a ladder . Another
common term that is used to describe this

SOHIC (Figure 2)

What is Blistering
Blistering occurs from molecular

hydrogen that collects at internal planar

nonmetallic inclusions or laminations.
Under the internal hydrogen pressure the
inclusion (lamination) disbonds from the
steel matrix and forms a blister. This type
of defect is generated immediately under
the surface are called blistering and is
generally not considered as a critical. An
example of Blistering is shown in Figure 3

Blistering (Figure 3)

What is SSCC
This type of cracking occurs in the

presence of stress in an aqueous

environment with H2S.
Many crack are generated at sites with
defect on the surface or inside where
stress is concentrated, and extend in
the direction perpendicular to the stress
axis. These cracks tend to occur easily
in hard welded zones, heat affected
zones (HAZ) and other hard places. An
example of SSC is shown in below
figure.

SSCC (Figure-4)

List of Equipments
SR.
NO.

INSTRUMENT NAME

Nos

Test Vessel and accessories

1

(for

HIC & Four point bend test)

2
Auto Titration Unit
3
Automatic Polishing unit
4
Four point bend test fixture
5
Proof Rings (SSCC tensile test)
pH Meter (for measurement of pH of
6
test solution)
7
Weighing Balance (0-200 gm )
8 Weighing Balance (0-200 gm & 0-2 Kg)
9
H2S Detector (with 5 sensor)
10
H2S Detector (Hand held type)
Water Distillation unit (Capacity 5
11
Liter/Hr)
12
Microscope with image analyzer

5
1
1
30
5
2
1
1
1
1
1
1

Automatic Polishing Machine

Microscope

Digital pH meter

Automatic Titrator

Typical Hydrogen Induced

Cracking Test Method

Sample preparation
Sample cutting From Plate

Sample cutting From LSAW pipe.

Test specimen shall be taken from the

weld ,90 degree from weld and 180

degree from weld
Three sample per pipe shall be taken
1) parallel to the longitudinal axis of pipe
from 90 degree and 180 degree from
weld
2) Perpendicular to the weld for weld area

Dimension :- Length :

100 1 mm
Width :
20 1 mm
Thickness : Actual thk-1
mm Maximum from each side.
Test specimen shall be full thickness of
pipe upto max. 30 mm WT.
Test specimen blank shall not be
flattened

Cleaning and storing

Degrease with suitable solution and

rinse with an appropriate solvent, such

as acetone.
Test specimen may be stored in
desiccators after degreasing.

Solution Preparation
Calculate the surface area of test specimen
Ratio of test solution to the surface area of

test specimen shall be minimum 3 mL/cm

Solution type A is used for HIC test. Solution
shall consist of 5.0 wt% NaCl and 0.5 wt%
Acetic Acid(CHCOOH) in distilled water.
All reagent added to the test solution shall
be 1.0% of specified quantities.
Initial pH shall be 2.7 0.1 pH and should
be checked by digital pH meter.

Orientation of sample in test vessel

Typical Test Assembly

Test specimen shall be placed with wide face

vertical and separated from test vessel and other

test specimen by glass or other nonmetallic rods
with minimum diameter of 6 mm
Purging and introduction of HS
Test solution shall prepare in separate sealed
vessel that is purged with nitrogen for at least
one hour at a rate of 100 cm/min per liter of test
solution.
Then transfer the test solution to the Test vessel
and purged it with nitrogen for atleast one hour at
a rate of 100 cm/min/liter of test vessel volume.
Purging shall start immediately after the test
vessel filled up with test solution.

After purging, HS gas shall be bubbled

through the test solution. The rate of

bubbling shall be at least 200 cm/min/
liter of test solution for the first one Hour.
Then positive pressure of HS gas shall be
maintained at constant gas flow rate to
ensure that the test solution remains
saturated with HS.
After 1 hour of H2S bubbling, Check the pH
& concentration of HS. pH immediate after
HS saturation shall be within the range of
2.7 to 3.3 Concentration of HS in test
vessel shall be minimum 2300 ppm.
Concentration should be checked by
automatic titration machine or iodometric

Test Duration & Test

Temperature
The test duration shall be 96 Hours. Test

time begins immediately after

completion of HS saturation.
Temperature of test solution during the
test shall be 25 3 C.
pH shall not exceed 4.0 for the valid
test.

Evaluation of Test specimen

After testing, Exposed test specimen may be

cleaned with detergent, but shall not be

cleaned with acid or any other means that
might promote hydrogen absorption.
Each test specimen shall be sectioned for
Evaluation as per the below figure.
For longitudinal base sample & Plate sample

 For transverse to the weld Sample

 Crack shall be evaluated as defined in the

following section

Crack shall be check on 100X magnification.

All visible cracks shall be measured ,except

those which lie entirely within 1.0 mm of the
internal or external surface.
Following equations are used for the
calculation of CSR, CLR and CTR.
For crack Sensitivity Ratio(CSR)

CSR=[(a X b)/(W X T)] X 100%

For Crack Length Ratio(CLR)

CLR =[a / W ] X 100%

For Crack Thickness Ratio(CTR)

CLR =[b / T ] X 100%

Reporting
Report shall consist of the followings as per

NACE TM 0284:2003
1. Method of testing adequacy of test specimen
degreasing
2. Type of Test Solution
3. pH of test solution before HS introduction
4. pH of test solution after HS saturation(start
of test)
5. pH of test solution at the end of test
6. Temperature of test etc.

Safety precaution
Following the safety precautions implemented in
NACE Lab
Restricted entry.
Smoking is prohibited.
Use of Mobile phone is not allowed.
Mandatory use of Face shield, Surgical hand
gloves and other PPE in NACE lab area.
Five numbers of H2S gas detectors are installed
in NACE lab area, audio-visual alarm system is
integrated with gas detectors.
One hand held type H2S gas detector.
Three numbers of breathing apparatus available
for any emergency.

Safety precaution Continue

First aid box available, CO2 type fire

extinguisher are available in NACE lab area.

Exhaust system to drive out H2S gas from the
test and gas storage area.
Emergency Preparedness Plan implemented.
Emergency control room & ambulance phone
no displayed in NACE Lab.

H2S gas Detector

First Aid kit

Breathing Apparatus

Fire Extinguisher

JINDAL SAW LIMITED

THANK YOU for your time and patience