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Major Ammonia leak incident in Urea plant Oman India Fertiliser Company was commissioned in April-2005. The performance in the first five commercial years of operation has been very good and all the envisaged project targets have been accomplished. Meticulous Root Cause Analysis of the problems surfaced at various stages have been analysed by the OMIFCO engineers in close association with the vendors and the consultants and implementation of the identified corrective measures in the shortest possible time has been the key to the achieved success of the company. The paper highlights about a critical Ammonia leak incident that occurred in the Urea 21 plant and how the situation was analysed to prevent re-occurrence of similar incidents. In chemical Industry, Careful Root Cause Analysis of the problems is very important and complacency cannot be ensured unless the remedies identified are convincing and consistent with the findings of the Root Cause Analysis made. S G Gedigeri Oman India Fertiliser Company Introduction MAN INDIA FERTILIZER COMPANY S.A.O.C. (OMIFCO) was set up as a joint venture project under the initiative of Government of Sultanate of Oman and Government of India. OMIFCO is owned 50% by Oman Oil Company, 25% by Indian Farmers Fertilizer Co-Operative Ltd (IFFCO) and 25% by Krishak Bharati Co- Operative Ltd (KRIBHCO). OMIFCO was registered in the Sultanate of Oman as a closed joint stock company in the year 2000. The Ammonia Urea complex comprises two trains, each with a design capacity of 1750 MTPD Ammonia and 2530 MTPD granulated Urea, along with all supporting Utilities. It is designed to produce total 1.65 million tonnes of granulated Urea and 0.25 million tonnes of surplus liquid ammonia annually for export, using natural gas. Storage facilities for Urea (2X 75000 MT) and Ammonia (2X30000 MT) as well as jetty with ship loaders are part of the project. Photo-01: OMIFCO Complex-Sur, Oman O 1 2011 AMMONIA TECHNICAL MANUAL

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  • 2011 [1] AMMONIA TECHNICAL MANUAL

    Major Ammonia leak incident in Urea plant

    Oman India Fertiliser Company was commissioned in April-2005. The performance in the first five

    commercial years of operation has been very good and all the envisaged project targets have been

    accomplished. Meticulous Root Cause Analysis of the problems surfaced at various stages have been

    analysed by the OMIFCO engineers in close association with the vendors and the consultants and

    implementation of the identified corrective measures in the shortest possible time has been the key to

    the achieved success of the company.

    The paper highlights about a critical Ammonia leak incident that occurred in the Urea 21 plant and

    how the situation was analysed to prevent re-occurrence of similar incidents. In chemical Industry,

    Careful Root Cause Analysis of the problems is very important and complacency cannot be ensured

    unless the remedies identified are convincing and consistent with the findings of the Root Cause

    Analysis made.

    S G Gedigeri

    Oman India Fertiliser Company

    Introduction

    MAN INDIA FERTILIZER

    COMPANY S.A.O.C. (OMIFCO) was

    set up as a joint venture project under

    the initiative of Government of Sultanate of

    Oman and Government of India. OMIFCO is

    owned 50% by Oman Oil Company, 25% by

    Indian Farmers Fertilizer Co-Operative Ltd

    (IFFCO) and 25% by Krishak Bharati Co-

    Operative Ltd (KRIBHCO). OMIFCO was

    registered in the Sultanate of Oman as a closed

    joint stock company in the year 2000.

    The Ammonia Urea complex comprises two

    trains, each with a design capacity of 1750

    MTPD Ammonia and 2530 MTPD granulated

    Urea, along with all supporting Utilities. It is

    designed to produce total 1.65 million tonnes of

    granulated Urea and 0.25 million tonnes of

    surplus liquid ammonia annually for export,

    using natural gas. Storage facilities for Urea (2X

    75000 MT) and Ammonia (2X30000 MT) as

    well as jetty with ship loaders are part of the

    project.

    Photo-01: OMIFCO Complex-Sur, Oman

    O

    12011 AMMONIA TECHNICAL MANUAL

  • 2011 [2] AMMONIA TECHNICAL MANUAL

    The complex has two service Boilers of capacity

    2 X 70 MT/hr and two HRSG boilers of

    capacity 2 X 110 MT/hr. Also the complex has

    its own captive power plant with two 30 MW

    Frame 6B Gas Turbine Generators and Import

    power connectivity with the national grid for

    backup power.

    Description of the System:

    OMIFCO owns and operates two Urea Plants

    designed by M/S SAIPEM, Italy (Previously

    Snamprogetti). The Urea manufacturing

    technology used at OMIFCO is based on the

    Ammonia Stripping Process.

    As per the process steps involved for producing

    Urea, feed Ammonia is fed to the reactor at

    elevated pressure. In the Urea plant the liquid

    Ammonia at about 15°.C (59°.F) and 23.5 Bar G

    (340.84 psig) pressure is initially received in an

    Ammonia receiver (V-105). Later by using an

    Ammonia booster pump (P-105-A/B), liquid

    Ammonia is pumped to the suction of the high

    pressure Ammonia feed pumps (P-101-A/B).

    The high pressure feed Ammonia pump

    transfers liquid ammonia to the Urea reactor

    through an ejector where the liquid Ammonia

    acts as a propellant for the high pressure

    Ammonium carbamate solution. (Figure-01)

    Liquid Ammonia from

    Ammonia Plant

    Ammonia

    Receiver-V-105Ammonia Booster

    Pump P-105

    High Pressure

    Ammonia Pump P-101Recycle Ammonium

    Carbamate solution

    SCHEMATIC DIAGRAM FOR

    THE INCIDENT LOCATION

    CO2

    To HP StripperFailure Location

    Figure: 01

    21-HV-1021

    Location of the failed pipe:

    The location of the failed weld joint was on the

    pipe rack in the Urea-21 unit of the OMIFCO

    complex. The pipeline going from the Ammonia

    booster pumps common discharge to the

    common suction of the high pressure Ammonia

    feed pumps has several weld joints. One of the

    weld joints nearer to the location where booster

    pumps common discharge pipe line joins the

    pipe rack had developed leakage during the

    normal running of the plant and later failed

    subsequently.

    Incident Scenario of Ammonia Leakage:

    In Urea-21 unit on 17th January 2008 at 04.40

    hours the weld joint on the common suction line

    of HP Ammonia feed pumps P-101 A/B had

    failed and caused heavy Ammonia leak.

    Immediately the plant emergency shutdown was

    initiated and the affected system was isolated

    and depressurized. Control valve 21-HV-1021,

    located at the outlet of Ammonia receiver V-

    105, on the common pipeline going to the

    suction of P-105-A/B pumps was closed from

    2 2011AMMONIA TECHNICAL MANUAL

  • 2011 [3] AMMONIA TECHNICAL MANUAL

    the central control room to isolate large

    Ammonia hold up equipment like Ammonia

    receiver V-105, MP Absorber C-101, and

    Ammonia condenser E-109 from the snapped

    off pipeline. This had helped in significantly

    reducing the Ammonia quantity leaked into the

    Atmosphere. A Level-1 emergency was

    declared and all the affected area was cordoned

    off and cleared of any workforce present in that

    vicinity. As all the working staff moved to a

    safe location nobody had received any

    Ammonia exposure.

    OMIFCO’S HSE (Health, Safety &

    Environment) team and the Production staff

    controlled and confined the leakage to within

    the plant battery limits by using their own fire

    tender and the personnel protection appliances.

    On scrutiny it was found that the elbow to pipe

    spool piece of the line 8”-21-P57-53A-V on the

    North-South pipe rack of Urea-21 plant had

    snapped off. The plant was back on stream on

    19th January 2008 at 10.50 hours after the repair

    and rehabilitation of the failed pipe line [Photo-

    05].

    Pre failure history of the affected pipe:

    One of the weld joints, on the elbow to pipe

    spool piece of the line 8”-21-P57-53A-V on the

    North-South pipe rack leaked at the 4 o’clock

    position. In the first week of Sept. 2007 the

    leaky joint was sealed on line by means of

    clamp [Photo-02]. It again started leaking

    through the clamp on 4th Jan 2008 and an on

    line sealing compound was re-injected to stop

    the leakage. However, on 17th Jan 2008 morning

    hours this joint fully snapped off from the weld

    joint leading to leakage of substantial amount of

    ammonia [ Photos-03 &-04].

    Photo-02: Weld joint with Sealing Clamp.

    Photo-03: Counterparts of Off-centred pipe.

    Photo-04: Side view of the snapped pipe.

    32011 AMMONIA TECHNICAL MANUAL

  • 2011 [4] AMMONIA TECHNICAL MANUAL

    Photo-05: Pipeline view after rehabilitation.

    Detailed specification of the pipe:

    Line Number: 8”-21-P57-53A-V

    Service Class: 53A (Mean Pressure

    Ammonia - Ammonia

    (First & Second ST) –

    Liquid Ammonia (With

    Stress Relieving)

    Pipe Material: A333 Gr.6 SMLS

    (0.3 C% & 1% Mn.)

    Normalized & tempered

    Steel

    Design: Line Size 8” (203.2 mm)

    Sch. 20 (6.35 mm Thick)

    Temp. & Pressure: (-) 45 O C (- 49 °F) and

    43 bar, (623.66 psi)

    Max Hydro Test 64.6 Bar. Abs (936.94 psi)

    Pressure.

    Corrosion Allowance: 1.27 mm (internal)

    (0.05 Inch)

    WPS: SPC.WL.ES.360

    Welding Class: 3T

    PWHT: Yes, (All Thickness

    Require PWHT for this

    Piping Class.)

    As per ASME Sect-II Part ‘A and ASME Sec

    IX for above grade material:

    Investigation and observations:

    This particular butt weld joint which had failed

    circumferentially was in operation for a period

    of 39 months, before its failure.

    After the failure and after removing the on line

    sealing clamp in the Visual examination the

    following were observed:

    •••• Complete snapping of the pipe at the failure

    location from the weld joint.

    •••• The weld joint failed circumferentially

    through the butt weld only and not cracked

    from the parent metal of elbow / pipe.

    •••• Rust marks were seen in the area adjacent to

    the weld of painted pipeline. (Refer Photos

    03 & 04)

    •••• ID surface of the pipe looked blackish

    brown indicating a general form of

    corrosion. (Photo: 03)

    •••• Fractured surface was flat and in transverse

    direction. At one location weld material had

    peeled off.

    •••• The counterparts of the failed joint displaced

    off center.

    •••• Circumferential corrosion damage is seen

    near to the failure location where the paint

    peeled off precisely at the region of clamp.

    •••• Fracture occurred perpendicular to

    longitudinal direction and in a single plane

    from the weld / HAZ region.

    •••• Fracture surface comprised of both fatigue

    and brittle nature. (Photos: 06 & 07).

    •••• Low magnification view confirms cracking

    both from OD and ID and in the weld zone

    near weld HAZ (Photo: 06)

    •••• SEM (Scanning Electron Microscopy)

    analysis confirmed that the cracking is a

    typical fatigue damage starting both from ID

    and OD and assisted by mild corrosive

    atmosphere. (Photo: 06)

    Failed Weld Joint

    4 2011AMMONIA TECHNICAL MANUAL

  • 2011 [5] AMMONIA TECHNICAL MANUAL

    Photo-06: SEM Result showing Crack initiation &

    propagation under the combined influence of

    corrosion and fatigue.

    • Crack movement was under the combined

    influence of high cycle fatigue and corrosion

    mode prevailed due to the marine

    environment.

    • Secondary cracks of corrosion fatigue were

    also noticed on the fracture surfaces along

    with corrosion products. (Photo:09)

    • EDS (Energy Dispersive Spectrum) Analysis

    confirmed that the corrosion damage on

    fracture surface was due to salt containing

    moisture from marine atmosphere. (Figure:

    02)

    • Overall microstructure of weld metal, HAZ

    and parent metal was normal and acceptable

    for the service. Pitting like corrosion damage

    at OD surface was also seen. (Photos: 11 &

    12)

    Repair and rehabilitation carried out:

    The pipe spool piece was cut from the other end

    also which was welded to the downstream side

    elbow. Both the elbows ends bevel edges were

    prepared by means of in-situ grinding. A new

    pipe spool piece was cut from the pipe of same

    size and same LTCS material grade available in

    warehouse.

    The bevel edge preparation at both the ends of

    the pipe spool piece was done as per the

    approved WPS for proper fit up. After proper fit

    up of both the elbow to pipe spool piece butt

    weld joints for the root and fill for both the

    joints was carried out by the TIG welding

    process (GTAW) using 2.4 mm (0.094 Inch)

    dia. filler wire ER 70S-6 as per the Welding

    Procedure Specification (WPS) approved for the

    given Pipe Service Class and Welding Class.

    During the welding process an inter pass

    temperature of 140 oC (284 °F) was maintained

    by means of digital thermometer.

    Dye Penetrant tests of both the root weld and

    final weld joints were carried out. No defect was

    observed.

    Hardness of newly made 02 nos. elbows to pipe

    weld joints was also checked on the weld, heat

    affected zone (HAZ) and the parent metal in the

    near vicinity and found to be within the

    acceptable limit of 225 BHN.

    Insitu Radiography of both the butt weld joint

    was carried out using IR 192 source of four Ci

    strength. No significant defect was observed.

    Stress Relieving (PWHT) of both the weld

    joints was carried out subsequently as per the

    SR Cycle prescribed in the approved WPS as

    mentioned below.

    PWHT:

    Heating: @ 150 °C (302 °F)/ Hr after

    200 °C (392 °F)

    Holding Time: 2.4 Minutes/mm of

    thickness @ 600 to 630 °C

    (1112 to 1166 °F)

    (01 Hr Min. in this case)

    Cooling: @ 150 °C (302 °F)/ Hr in air to a

    temperature of 300 °C (572 °F).

    Subsequently natural cooling in wrapped condition.

    52011 AMMONIA TECHNICAL MANUAL

  • 2011 [6] AMMONIA TECHNICAL MANUAL

    Hardness: Hardness measurement at the weld,

    pipe and HAZ area after the PWHT was again

    carried out and found to be within the

    recommended limit of 225 BHN.

    Non Destructive Tests carried out:

    •••• Tensile test was carried out on the sample

    and the results met the requirements of

    ASTM A 333 Gr.6 material for tensile

    properties.

    •••• V notch charpy Impact test was carried out

    on the sample drawn at -56.0°.C. (-68.8°F)

    Impact test results met the requirement of

    ASTM A 333 Gr.6 material.

    •••• General hardness was measured at different

    locations and results were found to be

    matching with the requirements of ASTM A

    333 Gr.6 material.

    Causes of Failure:

    •••• The pipe is exposed to sea water atmosphere

    and the paint had peeled off at some places

    near welding and corrosion has taken place.

    •••• The failure had taken place on account of

    fatigue cracking assisted by mild corrosion

    initiated at weld and HAZ both from OD and

    ID. Fatigue was due to cyclic load caused by

    unexpected shutdowns, start-ups, pump

    change overs and vibrations on the pipe.

    • The prevailing marine atmosphere, the

    vibration stresses from the pipe line while in

    operation and the surface corrosion that acted

    as stress concentration site, had resulted in

    corrosion fatigue.

    • Low Magnification Examination confirmed

    multiple origins of the cracks all over the

    circumference starting from both OD as well

    as ID. (Photo: 07)

    Photo-07: Low Magnification View at the fractured

    Surface. Multiple origins observed from OD & ID

    surfaces.

    Photo-08: Low magnification (33X) shows multiple

    origins in the form of ratchet marks.

    Photo-09: Presence of corrosion products observed

    at the cracked surface.

    6 2011AMMONIA TECHNICAL MANUAL

  • 2011 [7] AMMONIA TECHNICAL MANUAL

    •••• Optical metallography indicated pitting like

    damage on the OD surface of the pipe.

    (Photo: 10)

    Photo-10: Corrosion entering metal due to

    pitting like surface damage at weld location

    •••• Both SEM (Scanning Electron Microscopy)

    Analysis and Optical Metallography

    confirmed the failure to be on account of

    high cycle fatigue arising out of system’s

    cyclic operations and piping vibrations,

    assisted by corrosion.

    •••• The cracking has taken place in the weld and

    HAZ zone as seen in WFMPI (Wet

    Fluorescent Magnetic Particle Inspection)

    and Optical Metallography. (Photos 11, 12,

    and 13)

    •••• All the cracks are filled with corrosion

    products. Even the secondary cracks seen on

    the fracture surface were having corrosion

    fatigue nature. ( Photo-09)

    •••• EDS (Energy Dispersive Spectrum) analysis

    confirmed that the corrosion damage on

    fracture surface was due to salt containing

    moisture from marine environment. (Figure-

    02)

    Photo-11: Indicates that fracture has taken

    place at the fusion zone and perhaps moved

    into the weld.

    Photo-12: Corrosion fatigue crack moving

    precisely along the fusion zone of the weld.

    Photo-13: WFMPI revealed Secondary

    transverse hairline cracks at HAZ on the weld

    ID surface.

    72011 AMMONIA TECHNICAL MANUAL

  • 2011 [8] AMMONIA TECHNICAL MANUAL

    Figure-02: Results of Energy Dispersive Spectrum.

    Elements Percentage

    Present Elements

    Percentage

    Present

    Oxygen 37.22 Chlorine 1.07

    Sodium 1.31 Calcium 0.87

    Magnesium 0.87 Iron 57.74

    Silicon 0.93

    •••• Presence of Oxygen, Sodium, Magnesium,

    Chlorine and Calcium confirms that the

    corrosion is induced by the Salty marine

    atmosphere.

    •••• HAZ microstructure shows slight inclination

    towards having some internal stresses which

    is reflected from micro-hardness values.

    •••• The surface corrosion in form of tiny pits has

    provided favorable sites for stress

    concentration to take place both from OD and

    ID

    •••• Micro Structure examination has also

    confirmed corrosion fatigue cracking having

    trans granular nature of propagation.

    (Photo:14)

    •••• Matrix has banded ferrite and pearlite with

    mild branching nature. (Photo:14)

    Photo-14: Corrosion Fatigue Cracking-showing

    trans granular nature of propagation. Matrix is

    banded ferrite and pearlite.

    • Crack observed adjacent to fracture surface

    on pipe indicating another origin of fatigue

    crack.

    • The humid salty marine atmosphere

    provided the climate for corrosion to take

    place.

    8 2011AMMONIA TECHNICAL MANUAL

  • 2011 [9] AMMONIA TECHNICAL MANUAL

    •••• Pipe has been supported especially at elbow

    joint where the change in the direction of the

    Liquid Ammonia takes place.

    •••• The prevailing vibrations on the pipe line

    induced the fluctuating stresses.

    Thus, naturally the most vulnerable site for

    corrosion fatigue damage to take place is weld

    and HAZ.

    Micro Hardness Profile did not indicate any

    severe abnormality. Values at HAZ and Weld

    were slightly on higher side (Refer Figure-03).

    Figure-03: Micro Hardness Profile Diagram.

    Most Probable Cause of failure:

    •••• This failure might be due to corrosion,

    material defect and internal stresses owing to

    welding joint.

    •••• The stresses might have developed on

    welding due to injection of sealing compound

    and clamping

    Corrective Measures taken:

    •••• Flexibility and stress analysis of the pipe

    line from Ammonia receiver (V-105) to the

    Ammonia Booster pumps (P-105-A/B) and

    from the discharge of the Ammonia booster

    pumps to the suction of the HP Ammonia

    Pumps (P-101A/B) was carried out

    separately by a reputed local consultant and

    a foreign consultant of International repute.

    •••• The reports indicated no over stressing at

    any point in the pipe line and no alarming

    forces and moments are noticed at the

    restrained points.

    •••• Reports also indicated that stresses are

    within the allowable limits and the failure

    of pipe weld joint is not due to

    overstressing.

    •••• WFMPI (Wet Fluorescent Magnetic

    Particle Inspection), testing and Insitu

    metallography of all other weld joints on

    the affected pipe line were examined and

    those weld joints which did not pass all the

    tests were repaired. Radiography was

    carried out for checking the ID cracking.

    •••• One new On-Off type control valve HV-

    1013 has been installed on C-101 MP

    Absorber outlet Ammonia vapours line in

    both the Urea plants. This will facilitate

    quick isolation of C-101 in the event of any

    leakage (Figure-04).

    92011 AMMONIA TECHNICAL MANUAL

  • C-101

    MP Absorber

    E-109

    Ammonia Condenser

    CW

    P-101

    H.P Ammonia feed Pump

    To Urea

    Reactor R-101Ammonia

    Booster Pump

    P-105

    Condenate

    LP Steam

    P-102

    Carbamate Recycle Pump

    Ammonia

    Receiver

    E-111

    Ammonia from B/L

    V-105

    C-105

    HP Stripper Over head Vapors

    From MP

    Condneser

    21-HIC-1013

    Location of new ON/OFF

    control valve

    Carbamate

    Condenser

    V-101

    Carbamate Separator

    To MP Decomposer

    or Flare

    Cold

    Condneate

    To flare

    Figure-04: NEW CONTROL VALVE AT THE VAPORS OUTLET OF C-101

    •••• New on line Breathing Air sets with

    extendable hose of 50 meters length have

    been provided inside the plant field area to

    facilitate quick isolation in the event of

    Ammonia leaks.

    •••• Care is being taken for the quality of the

    painting on the pipe surface particularly

    near weld joints to avert peeling of paint

    and subsequent underneath corrosion

    damage.

    Conclusion:

    •••• Corrosion-fatigue is the result of the

    combined action of an alternating or cycling

    stresses and a corrosive environment.

    •••• On line sealing of leakages either from pipes

    or weld joints should be avoided which

    otherwise might cause inadvertent additional

    stresses, to the component which has been

    already under the influence of some parental

    residual stresses.

    •••• Contrary to a pure mechanical fatigue, there

    is no fatigue limit load in corrosion-assisted

    fatigue.

    •••• Much lower failure stresses and much

    shorter failure times can occur in a corrosive

    environment compared to the situation

    where the alternating stress is in a non-

    corrosive environment.

    •••• OMIFCO has decided not to do online

    sealing for any developed leakages of

    Ammonia pipe lines.

    10 2011AMMONIA TECHNICAL MANUAL