Proceedings of the 2022 14th International Pipeline Conference IPC2022 September 26-30, 2022, Calgary, Alberta, Canada TMCP PIPE FOR SOUR SERVICE: A NEW QUALIFICATION APPROACH Brian Newbury1, Volker Schwinn2, Jens Schroeder3, Graham Alderton4, Andrew Prescott1, and Andrew Wasson1 1ExxonMobil Technology and Engineering Company Aktien-Gesellschaft der Dillinger Hüttenwerke (DILLINGER) 3EUROPIPE GmbH 4Liberty Steel 2 ABSTRACT Historically, C-Mn steels have been extensively used in line pipe applications for sour service oil and gas environments, i.e. in the presence of hydrogen sulfide (H2S). In the past few decades, the emergence of the Thermo-Mechanically Control Process (TMCP) manufacturing method has further optimized the benefits of increased fabricability, weldability, and large cost benefits over alternate materials for large diameter pipe manufacturing techniques. However, implementation of C-Mn steels in sour service does require increased focus on steel cleanliness and hardness control to avoid susceptibility to hydrogen damage mechanisms such as hydrogen induced cracking (HIC) and sulfide stress cracking (SSC). These additional requirements have been addressed in industry standards such as NACE MR-0175/ISO 15156. Despite these industry practices, recent pipeline projects have experienced failures related to SSC and have found increased surface hardness due to Local Hard Zones (LHZs) in delivered and installed pipe. The LHZ phenomena appears to be a relatively new concern to the industry, and has led to concern over use of TMCP steels after the Kashagan pipeline failure in 2013. ExxonMobil has developed a qualification program based on the requirements of NACE MR-0175/ISO 15156 and new insights regarding the root cause of LHZs. This work reports details on this qualification approach implemented for X65 grade line pipe from recent qualification activities with TMCP plate and line pipe suppliers. LCZ LHZ NDT POD QA/QC SSC TM Local Cold Zones Local Hard Zones None Destructive Testing Probability of Detection Quality assurance/control Sulfide Stress Cracking Thermo-Mechanical rolling process 1. INTRODUCTION Oil and gas resources that contain hydrogen sulfide (H2S), often called sour service, are an important part of the world’s energy portfolio. However, the presence of H2S can lead to hydrogen ingress into C-Mn steels as a result of corrosion reactions generating monoatomic hydrogen on the steel surface. In these environments it is important to ensure that the pipeline materials are resistant to hydrogen cracking and related damage mechanisms. Industry practice has been documented in the NACE MR-0175/ISO15156 standard, with common practice to limit the hardness of C-Mn steels to below 248 HV10 for Region 3 of Figure 1. While considered the most severe region of the diagram, it can be seen that Region 3 covers a large range of pH and H2S concentrations. Despite this environmental variance industry practice generally does not discriminate within the regions of Figure 1; and once a material is qualified for a higher region (e.g., Region 3) it is often accepted as qualified for lower regions. In September of 2013, the Kashagan project located in the Caspian Sea experienced the failure of two 28-inch x 95 km long pipelines [2-5]. While the pipelines in the Kashagan project were replaced with corrosion resistant alloy (CRA) clad material, ExxonMobil studied the failure with a longer term focus of reenabling use of C-Mn line pipe material in future company severe sour service applications. To service this goal, ExxonMobil published a detailed discussion of a hypothesized root cause for the Kashagan failures in Fairchild et al [6], and a discussion of a C-Mn line pipe qualification procedure in Newbury et al [7]. Subsequent to these papers, ExxonMobil has implemented this qualification program with a number of plate Keywords: C-Mn steel, sour service, sulfide stress cracking, local hard zones, TMCP, materials qualification NOMENCLATURE 4PB Four Point Bend ACC Accelerated Cooling AYS Actual Yield Stress FRT Full Ring Ovalisation Test HACC Heavy Accelerated Cooling HIC Hydrogen Induced Cracking 1 Copyright © 2022 by ASME and Exxon Mobil Downloaded from http://asmedigitalcollection.asme.org/IPC/proceedings-pdf/IPC2022/86588/V003T05A014/6965894/v003t05a014-ipc2022-87146.pdf by China University of Petroleum user on 13 May 2024 IPC2022-87146 FIGURE 1: NACE DIAGRAM INDICATING SOUR REGIONS FROM LOWEST (0) TO HIGHEST (3) SEVERITY. One key learning highlighted in the Kashagan root cause study reported by Fairchild et al [6] was the identification of local hard zones [LHZs] and their role in SSC crack initiation in material nominally qualified for sour service to industry practice. LHZs were found to be very thin (<500µm deep), very infrequent, and randomly distributed on the pipe surface. The authors’ experience in Fairchild et al has shown that LHZs may only affect a few percent of steel plate contained in a transmission pipeline steel order, and of that affected plate LHZs may make up a very small fraction (1-5%) of the final pipe’s surface area. It was hypothesized that even a very extensive random sampling program would have a small chance of success in locating LHZs in qualification or production, but that a transmission pipeline could have an unacceptable level of risk of containing LHZs in the constructed line. This realization led to the development of the qualification summarized in Newbury et al [7]. 2. QUALIFICATION PROGRAM Detailed discussion of the qualification program can be found in Newbury et al [7]. A few key considerations formed the basis of the program, which aims to identify process upsets in the plate manufacturing process which can create conditions that allow LHZs to form. This work details execution of the qualification program for X65 grade line pipe intended to be used on two different severe sour service pipeline projects. The first is that the root cause of LHZs lies in the steel- or plate making process as discussed in Fairchild et al [6], however the customer interface is often only with the pipe manufacturer. Due to the multitude of techniques to manufacture an API or DNV grade line pipe, the qualification program had to involve all aspects of materials manufacturing from steelmaking to final coating effects on the line pipe. It also meant that qualification 2 Copyright © 2022 by ASME and Exxon Mobil Downloaded from http://asmedigitalcollection.asme.org/IPC/proceedings-pdf/IPC2022/86588/V003T05A014/6965894/v003t05a014-ipc2022-87146.pdf by China University of Petroleum user on 13 May 2024 activities were initially considered specific to the production route and alloy chemistry. A second consideration was to manufacture multiple commercial-sized heats of steel plate while attempting to manufacture realistic bounds in plate chemistry and other manufacturing parameters. In addition, some plates were manufactured explicitly outside of commercial practice in an attempt to generate LHZs and ultimately SSC test failures. The combined body of data generated from this production would help define future production process boundaries, based on the boundary of passing and failing SSC tests. The commercial scale materials trials were thought to eliminate questions about lab-toproduction scale changes in manufacturing process, while also providing the best chance to generate actual LHZs based on the statistics challenge mentioned in the introduction. A third consideration was to ensure compliance with NACE MR-0175/ISO 15156 requirements when qualifying materials to project-specific test environments. The infrequency of LHZs raised concern amongst the authors in Newbury et al [7] that samples taken from pre-specified test coupon locations would not meet the requirements for NACE qualifications based on laboratory testing. Within NACE MR0175/ISO 15156 requirements in section 8.3.2 state it is up to the end user to verify that the test samples are metallurgically representative of the final product as well as represent the metallurgical condition of greatest susceptibility to sour cracking for the final product. The LHZ phenomena creates a scenario where it is easy to unknowingly test materials that are not representative of the greatest SSC susceptibility (i.e., containing potential LHZs) in a qualification program. To address this third consideration required a fundamental shift in QA/QC practice in the plate manufacturing process. In addition to standard temperature monitoring processes for process control, additional thermal monitoring that would characterize the temperature of 100% of the plate surface eventually exposed to the sour service environment was required. This requirement is also in effect for future production to ensure all plate surface is in compliance with the qualification. Monitoring was required just prior and after the accelerated cooling steps of TMCP plate manufacturing. This ensured that no phase transformations occurred prior to entering accelerated cooling due to temperature drop below process target, as well as identifying the coldest locations after accelerated cooling. Both of these temperatures are critical to controlling LHZ formation mechanisms as discussed in Fairchild et al [6]. The coldest regions of plate in both material heats post accelerated cooling, as identified by thermal monitoring, were deemed “regions of interest” (ROIs) to be labelled and traced through remaining plate processing, transportation, and pipe forming processes. These regions were then exposed to either full ring ovalization SSC testing (FRT) according to BS 8701, or small scale four point bending (4PB) testing according to NACE TM0316 [8, 9]. Because of the thin nature of LHZs, the tensile surface of the samples was left as-received for 4PB and very light sand blasting was applied on full ring tests. Prior to testing the mills, pipe mills, and fully integrated line pipe mills. This work will highlight some of these qualification efforts and discuss key learnings generated during qualification and materials production. FIGURE 2: INTEGRATED OVERALL PRODUCTION CONCEPT AT DILLINGER. The occurrence of damage by HIC or SSC depends on the fraction and morphology of material imperfections, material fracture toughness and the geometrical features of potential cracking sites. The fundamental requirements for appropriate steels can be defined in terms of cleanness, i.e. inclusion content and shape, plus internal homogeneity and toughness of the material, i.e. the microstructure design. Interfaces or imperfections where hydrogen can recombine should be prevented or reduced to a minimum amount. Remaining inclusions should be homogeneously distributed and clusters must be avoided. The general strategy of the integrated overall production concept takes into account all these aspects. Table 1 documents the key conditions of this concept. 3. PLATE PRODUCTION - CONCEPT For the qualification efforts plates were produced following the approach of the integrated overall production concept as explained in more detail below. Those plates represent the actual best practice condition and are designated below as “Design Condition”. In addition plates were produced with “Off-Design Condition” to identify the limits of the “Design Condition” and to elaborate the key parameters and the boundary conditions that could produce material with increased HIC or SSC susceptibility. Particular focus was placed on the ACC process, e.g. the influence of local cold zones (LCZ) created during ACC that may impair SSC [6, 7]. TABLE 1: KEY CONDTIONS OF THE PRODUCTION CONCEPT. 3.1 Integrated overall production concept In order to provide consistent properties, the production of sour service steels relies on the utilization of an integrated overall production concept (Figure 2). This involves the steel- and platemaking as well as the application of a specific quality assurance system and NDT testing to ensure delivery of plates free from LHZ. 3.2 Steelmaking For the steelmaking a specific production route is applied. A key point is the utilization of a vertical type caster with soft reduction (Figure 3). The cleanliness is improved by this caster, since inclusions are able to rise up to the casting powder and the remaining inclusions are distributed homogeneously across the slab thickness. Manganese is known to segregate and as a consequence could deteriorate HIC properties, a proper 3 Copyright © 2022 by ASME and Exxon Mobil Downloaded from http://asmedigitalcollection.asme.org/IPC/proceedings-pdf/IPC2022/86588/V003T05A014/6965894/v003t05a014-ipc2022-87146.pdf by China University of Petroleum user on 13 May 2024 sand blasting procedure was qualified to show any LHZs, if present, would not be removed. The ROIs were tested under NACE TM-0177 “solution A” as well as two project-specific environments within NACE Region 3 of Figure 1. This allowed direct comparison to both historical qualification efforts (to the NACE solution A environment) as well as addressing concerns regarding potential materials performance variability across Region 3. Upwards of 30 ROIs were selected to cover the SSC testing campaign over the three testing environments per pipe mill. Each ROI was selected to have a consistent temperature over an area of approximately 100 x 150 mm. If a ROI was designated for 4PB testing, three coupons were cut for testing in triplicate. If the ROI was selected for FRT SSC testing, it was left as-is in the required ring coupon. After execution of the extensive SSC testing campaign, the data was analyzed to identify manufacturing conditions which generate a concern for SSC. A qualification window was then designated for the manufacturing route customized to each line pipe manufacturer (plate chemistry, manufacturing parameters, and pipe forming process). application of a soft reduction during casting is essential to reduce the amount of macro-segregations (Figure 4). As a result, the limitation of the manganese content does not need to be overly restrictive. b.) FIGURE 5: TYPICAL MICROSTRUCTURE OF THE PLATES PRODUCED WITH THE “DESIGN CONDITION.” 3.4 QA/QC system - updated During design and qualification stage, all the relevant production and process parameters are defined with target values and tolerances to meet the complete properties profile. During production certain deviations or incidents can occur that have a potential influence on HIC or SSC properties. For that reason a special adapted QA/QC system was installed that is able to detect a deviation of the actual values and to decide if such slabs or plates must be prohibited from release and delivery (because of a major deviation) or additionally tested to prove conformity with the specification (because of minor deviation). The plates produced for the qualification with “Design Condition” had no deviations. As mentioned above the plates produced with “Off-Design Condition” by intention deviate from the target values of the “Design condition”. The previous mill practice relied on the temperature measurement by optical pyrometer in the center region of the plate as it passes under the pyrometer. As mentioned above, special attention was paid on the ACC process and the parameters that may create LHZs or may impair SSC resistance. As a consequence the new approach of the qualification program requires 100% plate surface temperature monitoring by a thermal camera at the entrance and exit of the ACC process (Figure 6). This temperature measurement of the thermal scanner is performed on the rolled plate (so called mother plate) and includes colder areas at the edges and ends. These areas are trimmed off at a later stage. Sample plate surface temperature scans prior to edge and end trimming can be found in Newbury et al. [7] A mother plate is divided typically in two or even three final plates (so called daughter plates). Therefore a specific program was developed and implemented in an upgraded QA/QC system that can clearly assign the temperature measurement of the thermal cameras to the final plate and provides additional features for the evaluation and traceability of the temperatures in local areas. This system was used to select the ROIs discussed in section 2, and is essential to correlate the ROI test results of the qualification program which define lower bound qualified values with the local temperatures measured during plate production. FIGURE 3: COMPARISON OF VERTICAL AND CURVED TYPE CASTERS. FIGURE 4: INFLUENCE OF SOFT REDUCTION DURING CASTING. 3.3 Plate making The metallurgical concept relies on a TM+HACC rolling and cooling process to achieve a homogeneous and fine granular bainite microstructure without banding (Figure 5). This implies finish rolling and start accelerated cooling above Ar3. However, for an optimized balance of HIC and SSC resistance the cooling rate is restricted and the finish cooling temperature is maintained high enough to limit macro- and micro-hardness. Another important point of the concept is the use of slabs with a sufficiently high thickness. For the qualification program slabs with a nominal thickness of 400 mm were used. Thus enhanced total deformation ratios during roughing and finish rolling are feasible and the metallurgical concept becomes more robust. 4 Copyright © 2022 by ASME and Exxon Mobil Downloaded from http://asmedigitalcollection.asme.org/IPC/proceedings-pdf/IPC2022/86588/V003T05A014/6965894/v003t05a014-ipc2022-87146.pdf by China University of Petroleum user on 13 May 2024 a.) FIGURE 6: SCHEMATIC POSITIONS OF THE THERMAL CAMERAS AT THE ENTRANCE AND EXIT OF ACC. 3.5 NDT for LHZ During steel and plate making different possible causes for LHZ exist. Due to the infrequent occurrence and small size, LHZ are difficult to detect using the standard hardness testing included in most specifications. Standard surface hardness testing could only work reliably if it was applied on a very fine grid scale involving thousands of hardness measurements. Therefore, large scale hardness testing for the detection of LHZ is inappropriate for an industrial plate production process. To overcome this problem, an Eddy Current testing technique was developed which allows 100 % plate surface inspection as an integral part of the industrial plate production process which reliably detects all areas with increased hardness and size resolution of 20mm [10]. In a first step and applied for this qualification program a manual NDT system for QA/QC was implemented and utilized with testing on both sides covering 100 % of the surface area. Since it was the most conclusive method, it was also previously used for the root cause analysis for LHZ and thus the parameters causing LHZ could be identified and optimized subsequently. However, it is worth to mention that although the amount of LHZs were clearly reduced, it is not possible to eliminate them completely. Within this qualification program two LHZs were detected by the NDT system and verified by hardness testing and metallographic investigations. These plates were not further processed to pipes. In order to increase the capacity of plate material inspected for LHZ during production, an inline automatic NDT device has been installed. The inline system allows inspection of all plates on both sides simultaneously without any impact on production rates. The commissioning and qualification including the POD (probability of detection) of this device was finalized after this qualification program. FIGURE 7: ROI SHOWING TOOLING WEAR MARKING (INSIDE DASHED YELLOW BOXES) ON THE OUTSIDE OF THE PIPE FROM PIPE FORMING. NOTE SOME WEAR MARKS APPEAR DARK OR BRIGHT DUE TO SHOP LIGHTING. THIS ROI WAS RE-LABELED FOR EASE OF VISUAL IDENTIFICATION DURING REMAINING PROCESSING. Mechanical properties were required in as-manufactured and aged condition and sour service testing was conducted in the aged condition. To accommodate all test conditions test rings were removed prior to ageing, the full pipe was then sent for 4. PIPE PRODUCTION AND TESTING In this work, TMCP plates were supplied to two UOE SAWL pipe mills. Each pipe mill received approximately twenty 5 Copyright © 2022 by ASME and Exxon Mobil Downloaded from http://asmedigitalcollection.asme.org/IPC/proceedings-pdf/IPC2022/86588/V003T05A014/6965894/v003t05a014-ipc2022-87146.pdf by China University of Petroleum user on 13 May 2024 plates for forming into pipe and testing. Prior to receiving the plates, it had already been identified that the ROI marking on the plate surface could not be solely relied upon as method for later identification at the pipe mill therefore the X-Y Co-ordinates of each ROI were recorded at the plate mill. Plate shipment can involve, rail, sea, and truck and therefore plates can be handled several times. Although these transport routes are well established and have shown not to be an issue with the standard plate marking, testing these specific ROI was a fundamental aspect of this qualification and warranted the backup traceability method. Pipe manufacture involves press forming of the plates and plate movement by roller tables so there was concern this could remove the ROI marking. As a precaution the ROI marking was transposed to the eventual outside pipe face of the plate by the plate mill. Loss of marking concern was mainly during the O pressing where the dies contact the top plate surface. The surface sees considerable frictional forces, and to reduce these a lubricant is applied, combined this gives the ideal condition for marking removal. After pressing and immediately before further processing plates were re-inspected, cleaned, and the marking reapplied. As a precaution this inspection and reapplication was conducted as necessary at every stage of the process. A ROI label to be re-marked is shown in Figure 7. To do this the production line must be stopped, and thus only reserved for major qualifications and not performed for commercial production. 4.1 Sour and Mechanical Testing The sour test program involved testing the ROIs plus the seam weld. These ROIs were spread across plate material manufactured in the design condition as well as the off-design condition. Across the two pipe mills, the evaluation consisted of four different steel production heats and involved 144 HIC specimens, 108 4PB SSC specimens and 48 full ring ovalisation SSC tests. HIC testing was conducted in accordance with NACE TM0284-2011 solution A and involved sets of three full wall thickness specimens at the standard NACE locations of seam weld, 90 degrees, and 180 degrees around the pipe circumference. SSC samples were extracted from the aged pipes and 4PB testing to NACE TM0316 for 720 hours was performed with an applied load of 90 % actual yield stress (AYS). The AYS was determined from tensile tests conducted in the aged condition. Longitudinal base metal SSC samples taken from within the ROI and had the inside surface left intact meaning without surface machining. This allowed potential LHZ cracking tendency to be quantified. Samples were loaded per the NACE standard as shown in Figure 10. There was a consideration to use a non-machined transverse weld specimen, but this was shown to overly load the weld toe as a direct result of the thicker and stronger weld metal as seen in Figure 11. Strain gauges were applied at the weld toe and within the base material and the sample loaded, whilst the weld toe reached loads exceeding AYS, the base material was still less than 50 % AYS. FIGURE 8: SAMPLE CUT SCHEMATIC SHOWING BULT RINGS TO BE REMOVED FROM THE FULL LENGTH LINE PIPE (TOP) AND THEN PER-RING TEST BLANK CUT PLANS TO ACCOUNT FOR SOME OF THE PROGRAM’S MECHANICAL TESTING. Pipe specifications often specify mechanical testing in the aged condition, but this is normally done on samples extracted from aged coupons or the samples themselves aged prior to testing and this can be managed within the test house. For this qualification it was a requirement for the full length to be aged. Thermocouples were attached to the pipe outer surface at positions away from any of the ROI. Multiple pipes were loaded into the furnace and heated to 250 °C, reaching temperature took more than 5 hours illustrated in Figure 9. Once the temperature was attained, it was held for a minimum of 60 minutes before allowing to cool in air. The ROI marking was then be reinspected and reapplied, as necessary. FIGURE 10: 4PB SSC TEST LOADING INDICATING NONMACHINED AS-RECEIVED PIPE INNER SURFACE. FIGURE 9: FURNACE SCHEMATIC FOR ARTIFICAL AGING FOUR LINE PIPES (RIGHT) AND THE RESULTANT THERMOCOUPLE DOCUMENTATION OF THE AGING HEAT TREATMENT (LEFT). UOE pipe forming is at ambient temperature and introduces cold deformation. One aspect of the qualification was to quantify the increase in hardness resulting from pipe forming. Direct testing on the pipe surface with a portable hardness tester was attempted but the curved surface of the pipe makes the result overly sensitive to the alignment of the probe and the surface preparation, and the outcome is often an excessive scatter in the measured values. Hardness testing on macro samples at 1 mm below the surface and micro hardness at 0.25 mm below the surface were conducted. FIGURE 11: NON-MACHINED SEAM WELD SSC COUPON ILLUSTRATING WELD REINFORCEMENT AND STRAIN GAUGE LOCATIONS. To accurately characterize the SSC performance of the seam weldment, fully machined coupons were required to address the applied stress discrepancies measured by the strain gauges. It 6 Copyright © 2022 by ASME and Exxon Mobil Downloaded from http://asmedigitalcollection.asme.org/IPC/proceedings-pdf/IPC2022/86588/V003T05A014/6965894/v003t05a014-ipc2022-87146.pdf by China University of Petroleum user on 13 May 2024 ageing, and then further test rings cut after the ageing. This involved a significant amount of planning and required a bespoke cutting instruction per pipe as shown in Figure 8. Across the two pipe mills over 180 rings were cut to account for the SSC and mechanical testing requirements. should be noted that LHZs, if present, would be erased by the heat input from seam welding and thus the fully machined samples are the most accurate way to characterize weldment microstructure SSC resistance. FIGURE 13: SCHEMATIC OF INTERNAL LOADING AND STRAIN GAUGE EQUIPMENT FOR FRT SSC TESTING. [12] C2 In this program, it was found that available internal loading equipment was not able to apply and hold constant the required applied stress. An applied load target of 80% AYS was chosen on recommendation of testing SMEs from the contracted test house executing the SSC program. This was chosen to account for residual stress remaining in the FRT pup pieces to approximate the 90% AYS applied in the small scale 4PB specimens. Residual stresses would be relieved in the small scale 4PB specimens. The reference yield stress was measured from aged tensile specimens to conservatively mimic the asinstalled pipe after coating. External loading as shown in Figure 14 below is an alternative method given in BS8701 and allows for higher loads to be applied. C3 C1 FIGURE 12: NACE DIAGRAM WITH TEST CONDITIONS. 4.2 Full Ring Ovalisation SSC Testing Both pipe mills conducted eight full ring ovalisation tests (FRT) in each of the same three conditions as used for the 4PB SSC scope. The rings were taken with the ROI in the centre of the ring and aligned as the target area for maximum applied tensile stress. Testing was conducted in accordance with BS 8701 [8]. Conducting full rings tests is not an easy task and requires specialist experience and therefore limited to laboratories with proven expertise in this area. The type of rig design has a direct impact on how the rings are loaded and the consistency of applied stress. Internal loading can be used by means of a turnbuckle with the maximum stress perpendicular to the applied load as indicated in Figure 13. The advantage of this design is that it allows UT examination during the exposure period, however, this method was designed for loading at 72 % SMYS and the threads on the turnbuckle may limit the maximum amount of load that can be applied. FIGURE 14: SCHEMATIC OF THE ALTERNATE EXTERNAL LOADING CLAMP FRT SETUP UTILIZED IN THIS TESTING PROGRAM. [12] 7 Copyright © 2022 by ASME and Exxon Mobil Downloaded from http://asmedigitalcollection.asme.org/IPC/proceedings-pdf/IPC2022/86588/V003T05A014/6965894/v003t05a014-ipc2022-87146.pdf by China University of Petroleum user on 13 May 2024 SSC testing was conducted in three different environmental conditions. They are listed in Figure 12 as C1, C2, and C3: Condition one: 1 bar pH2S, Solution A NACE TM017 pH3 (2500 ‐ 2800 ppm H2S) Condition two: A project-specific NACE region 3 condition with a mixture of H2S and CO2 totaling 14.5 psi Condition three: A project-specific NACE region 3 condition with a mixture of H2S and CO2 at positive pressure Strain gauges were placed in the region of interest and the bolts tightened until the target stress was achieved (Figure 15). Within a small distance from the location of maximum tensile stress there were noticeable changes in the strain gauge values. Additional gauges were added for the first tests and the procedure refined on site to maximize applied stress consistency. It was a challenge to achieve the 80% AYS loads at the ROI whilst also not overstressing areas outside of the ROI. Small clamp misalignments or minor geometric changes in the sample pipe, well within acceptable manufacturing geometrical tolerances specified in all line pipe standards, could lead to overstressed regions of the sample. If these are not well understood, it can lead to misinterpretation of test results. Strain gauges were removed after the applied load was proven to be stable. Pipe Transverse Yield Strength (Round Bar) 600 580 520 500 480 460 450 440 Codition As welded mill Aged As welded A Aged B Pipe Transverse Tensile Strength (Round Bar) 630 Rm [MPa] 610 590 570 550 535 530 Codition mill As welded Aged A As welded Aged B FIGURE 16: SAMPLE LINE PIPE YIELD AND TENSILE STRENGTH VALUES FOR BOTH PIPE MILLS IN THE ASFORMED AND AGED CONDITIONS. In terms of hardness, there was a 10 to 15 HV10 increase attributed to pipe forming and then a further smaller increase after ageing as shown in Figure 17 below. The average in pipe for X65 remained low, even in the aged condition. Over a larger production run the hardness range would widen therefore consideration is needed when setting any specification limit. For pipe a maximum hardness of 230HV10 is an appropriate maximum value for the base material, this gives allowance for potential hardness increase in the weldment so the installation contractor can remain below the NACE limit during girth welding. FIGURE 15: VALIDATION OF APPLIED STRESS AT ROI VIA STRAIN GAUGE MONITORING. [12] 5. RESULTS For both pipe mills the mechanical properties of DNVGL STF101 L450 SFD were confirmed with Charpy toughness at -30 °C and BDWTT and CTOD confirmed at -10 °C. The ageing coating simulation of the pipes made the yield strength increase by 20–40 MPa and the tensile strength by 10–15 MPa as shown in Figure 16. SSC testing was based on the AYS therefore this increase was seen as conservative to applied loads based on SMYS. FIGURE 17: HARDNESS CHANGE FROM PLATE TO ASFORMED PIPE TO AGED PIPE. Micro hardness was conducted 0.25 mm below the pipe surface and the values were measured to be approximately twenty points higher than 10 kg load values collected 1-2 mm below the surface. This level increase was expected because of the smaller microhardness sampling volume and ability to characterize surface-cooled microstructures. The near-surface microhardness 8 Copyright © 2022 by ASME and Exxon Mobil Downloaded from http://asmedigitalcollection.asme.org/IPC/proceedings-pdf/IPC2022/86588/V003T05A014/6965894/v003t05a014-ipc2022-87146.pdf by China University of Petroleum user on 13 May 2024 Rt0.5 [MPa] 560 540 FIGURE 18: PITTING CORROSION ON THE ID SURFACE OF AN FRT SAMPLE TESTED IN CONDITION TWO. The 4PB samples tested in conditions 2 and 3 would often show stress grooving as result of the severe environmental conditions. Stress grooves manifested as blunt features due to local corrosion at the surface aligned with prevalent stress fields in the 4PB samples. Figure 19 illustrates multiple stress grooves. These features are not sharp and not to be mistakenly reported as SSC. Post-test micro hardness measurements confirmed the hardness around and at the tip of these groves to be below the limits at which SSC would occur. Additional work within ExxonMobil showed that these features were exacerbated by the high applied loads (90 %AYS of aged tensile specimens). Decreasing the applied loads minimized and ultimately eliminated the stress grooves. FIGURE 20: SSC CRACK IN AN OFF-DESIGN SAMPLE INDICATING PLATE PRODUCTION OUTSIDE OF PARAMETERS SUITABLE FOR SSC-RESISTANT LINE PIPE. This qualification work has shown that SSC susceptibility is increased with increasing fraction of lath bainite, attributed to high cooling rates during plate quenching or low stop cooling temperatures. The critical amount of lath bainite to cause SSC susceptibility is dependent on the plate manufacturing process, and thus different for all plate suppliers. Critical parameters such FIGURE 19: STRESS GROOVING SEEN IN TESTING UNDER CONDITIONS TWO AND THREE. For the off-design condition, some of the samples representing the most aggressive localized cooling during plate 9 Copyright © 2022 by ASME and Exxon Mobil Downloaded from http://asmedigitalcollection.asme.org/IPC/proceedings-pdf/IPC2022/86588/V003T05A014/6965894/v003t05a014-ipc2022-87146.pdf by China University of Petroleum user on 13 May 2024 manufacture and tested in all three environmental conditions produced failures. This was as per program design as it identified plate manufacturing conditions unsuitable for SSC resistance. An example SSC crack in one of these off-design test samples is seen in Figure 20. Through careful evaluation of each of the small and large scale SSC samples, including microhardness on the post-test sections and correlation to the specific plate manufacturing parameters, a safe boundary for the relevant plate manufacturing processes could be defined for production QA/QC oversight. For all SSC test evaluations, the test acceptance criteria reported in Anderson et al [11] was used. This acceptance criteria were developed to aide in assessing SSC test coupons that show evidence of significant localized corrosion attack as seen in conditions two and three, which resulted from high amounts of CO2 present in the test environment. Both the large scale FRT and small scale 4PB SSC coupons were found to reliably characterize SSC performance of the tested line pipe. However, specialist knowledge regarding loading effects, test environment selection, and final test result interpretation was required for both types of tests. FRT testing showed significant sensitivity to loading clamp alignment and geometrical variation within the pipe samples (well within acceptable limits by common line pipe codes). This sensitivity could lead to over or underloading test samples if not fully understood. 4PB SSC samples showed tendency to develop stress grooves in certain test environments as a result of the test setup. Both scenarios required specialist knowledge to address and interpret test results appropriately. locations were required to accurately quantify presence of LHZs.For the design rolling condition, both pipe mills passed the HIC, the 4PB SSC, and the FRT SSC tests in all of three environmental conditions. Pitting corrosion was observed in the FRT samples tested in condition two as seen in Figure 18. An example of this is shown below. This occurrence of pitting was attributed to the increased level of CO2. 6. CONCLUSION A new qualification approach for C-Mn line pipe steels in severe sour service has been developed and implemented with a number of steel plate and line pipe manufacturers. A review of the experience implementing this qualification program with one steel plate manufacturer and two line pipe manufacturers has been provided. The program did not require a fundamental change in the metallurgical design of sour service plate, but did require a shift in the monitoring practice of critical plate manufacturing processes. This change involved measuring the surface temperature of 100% of the steel plates, and selecting regions of interest, representing the metallurgical condition most susceptible to SSC cracking, for testing after final manufacture into line pipe. This process was then implemented on the manufacturing line of both the plate mill and line pipe mills, ensuring representative product to a production order. Material was manufactured in “design condition” and “off-design” parameters to ensure a verified production window, with demonstrated SSC resistance, was identified. This process was executed successfully at the two line pipe mills. All sour tests were found to pass for the design condition line pipes at both mills. SSC test failures in the off-design condition material confirmed limits to plate manufacturing parameters that govern future the production of any commercial order. Full ring ovalisation tests for SSC require significant understanding of the load distribution to ensure valid tests and to prevent misinterpretation of results. The results of the qualification process have led to an updated QA/QC system in which the derived limits have been implemented. An additional component of this updated QA/QC system is the added in-line NDT inspection based on eddy current. The use of thermal cameras and in-line eddy current inspection has been found to be effective at identifying LHZs from both overcooling and carbon enrichment. The shift in QA/QC process and new in-line NDT inspection for LHZ detection did not inhibit production rates in the plate mill as demonstrated in a recent large sour service production order. ACKNOWLEDGEMENTS The authors would like to acknowledge Dr. Douglas Fairchild’s significant contributions and assistance during execution of the qualification program. REFERENCES [1] ANSI/NACE MR0175/ISO 15156-2015: Petroleum, petrochemical, and natural gas industries - Materials for use in H2Scontaining environments in oil and gas production 10 Copyright © 2022 by ASME and Exxon Mobil Downloaded from http://asmedigitalcollection.asme.org/IPC/proceedings-pdf/IPC2022/86588/V003T05A014/6965894/v003t05a014-ipc2022-87146.pdf by China University of Petroleum user on 13 May 2024 [2] https://www.ncoc.kz/Documents/Sustainability_report_2015_ en.pdf [3] D. Baxter, E. Ostby, S. Chong, A. Venas, “Use of C-Mn Linepipe for High H2S Service”, 37th Int’l Conf. OMAE, June 17-22, 2018, Madrid, Spain. [4] https://www.reuters.com/article/oil-kashaganidUSL6N0S52P420141010 [5] https://www.offshoreenergytoday.com/kashagan-notgetting-back-on-line-in-2014/ [6] Fairchild D.P. Newbury B.D., Anderson T.D., Thirumalai N.S., “Local Hard Zones in Sour Service Steels”, 38th Int. Ocean, Offshore and Arctic Eng. Conference, OMAE, Glasgow, Scotland, 2019 [7] Newbury B.D., Fairchild D.P., Prescott C.A., Anderson T.D., Wasson A.J., “Qualification of TMCP Pipe for Severe Sour Service: Mitigation of Local Hard Zones”, 38th Int. Ocean, Offshore and Arctic Eng. Conference, OMAE, Glasgow, Scotland, 2019 [8] BS8701-2016: Full ring ovalization test for determining the susceptibility to cracking of linepipe steels in sour service [9] NACE TM0316-2016: Standard Test Method Four-Point Bend Testing of Materials for Oil and Gas Applications. [10] Schneibel G., König C., Gopalan A., Dussaulx J.M., “Development of an Eddy Current based Inspection Technique for the Detection of Hard Spots on Heavy Plates”, 19th World Conference on Non-Destructive Testing, Munich, Germany, 2016 [11] T.D. Anderson, D.P. Fairchild, W. Huang, N. Thirumulai, G. Wadsworth, A. Ozekcin, H. Jin, “Micrographic Acceptance Criteria for SSC Testing”. Corrosion Conference & Expo, (Houston, TX: NACE 2020). [12] P. Dent, Element Materials Technology, NACE International Webinar “Mitigation of SSC Failure from TMCP Local Hard Zones” as plate chemistry, rolling schedule, descaling practice, finish rolling/ACC start/end quench temperatures all play a roll in the final microstructure and its SSC susceptibility.