Poster PO-27

INVESTIGATIONS INTO THE AGING EXTENT OF THE 9% NICKEL 500 M3 LNG STORAGE TANK OF THE NANTES CRYOGENIC TESTING STATION INVESTIGATIONS SUR LE DEGRE DE VIEILLISSEMENT DU RESERVOIR GNL DE 500 M3 EN ACIER 9% NICKEL DE LA STATION DESSAIS CRYOGENIQUE DE NANTES
Dominik Uznanski, Project Manager Emmanuel Chteau, Metallurgical Engineer Olivier Gorieu, Research Engineer Jean-Pierre Legrandais, Engineer Gaz de France Paris, France dominik.uznanski@gazdefrance.com Young-Myung Yang, Head of Center Seongho Hong, Principal Engineer Korea Gas Corporation Inchon, Korea Maki Yamashita, Engineer Osaka Gas Company, Ltd. Osaka, Japan Jean-Marc Cherasse, Principal Engineer Sudipta Jana, Metallurgical Engineer Dirk Goeminne, LNG Line Engineer Tractebel Gas Engineering S.A. Brussels, Belgium Jean-Yves Capelle, Project Manager Total S.A. Paris, France

ABSTRACT Gaz de France has been operating its Liquefied Natural Gas (LNG) Testing Station, located in Nantes near the Montoir methane terminal, for more than 40 years. This Testing Station, which was launched with the construction in 1959 and commissioning in 1960 of a 500 m3 9% nickel steel self-sustaining above ground LNG tank, allowed the qualification of various cryogenic installations and equipment, including the 9% nickel steel inner wall storage tank technique, an open-rack aluminum MARSTON type regasification unit and other equipment such as valves and flanges. Recently, the decision was made by Gaz de France to close down the Nantes Testing Station by the end of 2001 and the Testing Station was dismantled from September 2002 to March 2003. The dismantling of the Nantes Testing Station represents a unique and unprecedented opportunity to study the aging extent of various cryogenic materials commonly used in the LNG industry, some of which have been operated for more than 40 years at LNG temperatures. In particular, the 9% nickel steel inner walls of the 500 m3

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storage tank, as well as the tanks insulation material (perlite) have been targeted for detailed analysis. This work is being carried out within the framework of an international partnership, in view of sharing the results and promoting enhanced exchanges on the aging analysis of cryogenic materials. Initially, the Korea Gas Corporation, Osaka Gas Company, TotalFinaElf and Tractebel joined Gaz de France in this Joint Industrial Program. Today, this project is open for partnership to any company which can benefit from the assessment of the life span of cryogenic materials. This paper will focus on the non-destructive and destructive investigations carried out on the 9% nickel steel inner walls of the 500 m3 storage tank. By analyzing the aging extent of such cryogenic materials, an assessment of the longevity and durability of these materials can be realized, thus allowing possible improvements in the design of new methane terminals and of the maintenance procedures for various cryogenic equipments using such materials. Also, by possibly proving that the life span of a 9% nickel selfsustaining above ground tank can be increased from 30 years to more than 40 years, exemptions from inspections can be reaped, all this within a context of stricter regulations. Knowing that such inspections impose heavy costs on installations due to the stop of production, the cost saving benefits are evident. RESUME Gaz de France a exploit sa station dessais de Gaz Naturel Liqufi (GNL), situe Nantes proximit du terminal mthanier de Montoir, depuis plus de 40 ans. Cette station dessais, qui a t dmarre avec la construction en 1959 et la mise en service en 1960 dun rservoir GNL arien cuve autoporteuse de 500 m3 en acier 9% nickel, a permis la qualification de diverses installations cryogniques et quipement, incluant la technique de stockage cuve interne en acier 9% nickel, un regazifieur atmosphrique en aluminium de type MARSTON et dautre quipement comme des vannes et brides. Rcemment, Gaz de France a pris la dcision de fermer la station dessais de Nantes pour fin 2001 et la station dessais a t dmantele de septembre 2002 mars 2003. Le dmantlement de la station dessais de Nantes reprsente une opportunit unique et sans prcdent dtudier le degr de vieillissement de divers matriaux cryogniques couramment utiliss dans lindustrie du GNL, certains ayant t exploit pendant plus de 40 annes. En particulier, les parois internes en acier 9% nickel du rservoir de 500 m3, ainsi que lisolant du rservoir (perlite) ont t slectionns pour analyse pousse. Ce travail est ralis dans le cadre dun partenariat international, afin de partager les rsultats et de promouvoir des changes renforcs sur lanalyse du vieillissement de matriaux cryogniques. Initialement, Korea Gas Corporation, Osaka Gas Company, TotalFinaElf et Tractebel ont rejoint Gaz de France dans ce Joint Industrial Program. Aujourdhui, toute compagnie pouvant bnficier de lvaluation de la longvit des matriaux cryogniques peut se joindre au partenariat. Cette communication se focalisera sur les investigations non-destructives et destructives ralises sur les parois internes en acier 9% nickel du rservoir de 500 m3. En analysant le degr de vieillissement de ces matriaux, une valuation de leur longvit et durabilit peut tre ralise, permettant ainsi des amliorations possibles dans la conception de nouveaux terminaux mthaniers et des procdures de maintenance de

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divers quipement cryognique utilisant ces matriaux. Aussi, avec la preuve possible que la dure de vie dun rservoir arien en acier 9% nickel peut passer de 30 ans plus de 40 ans, des drogations pour des inspections peuvent tre obtenues, dans un contexte de rglementations plus strictes. Les bnfices en terme de rduction des cots qui en dcoulent sont vidents, connaissant les cots importants imposs par ces inspections sur les installations cause de larrt de la production. INTRODUCTION Gaz de France had been operating its Liquefied Natural Gas (LNG) testing station, located in Nantes near the Montoir methane terminal, for more than 40 years. This testing station, which was launched with the construction in 1959 and commissioning in 1960 of a 500 m3 9% nickel self-sustaining above ground LNG tank, allowed the qualification of various cryogenic installations and equipment, including the 9% nickel steel inner wall storage tank technique, an open-rack aluminum MARSTON type regasification unit (ORV) and other equipment such as valves and flanges. Figure 1 below gives a general view of the testing station (area which is delimited by the red contour). Some of the main elements of the testing station are indicated as well.

500 m3 tank

250 m3 tank

Test bench ORV

Figure 1. General view of Nantes LNG testing station The testing station consisted mainly of the following installations : an LNG storage tank with a capacity of 500 m3 (RL500), an LNG storage tank with a capacity of 250 m3 (RL250), an open rack MARSTON type LNG vaporization unit (ORV), a circuit for liquid transfer from RL250 to RL500, a second circuit for the recovery of boil-off gas from the 500 m3 tank, a circuit leading to the sites vent stack,

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an LNG tanker truck loading/unloading platform, two test bench areas, two data acquisition rooms, various safety devices (water curtains, foam generators, gas and infra-red radiation detectors, ).

Recently, the decision was made by Gaz de France to close down the Nantes Testing Station at the end of 2001. The testing station was first inerted during the first quarter of 2002 and was then dismantled from September 2002 to February 2003. The dismantling of the Nantes testing station represents a unique and unprecedented opportunity to study the aging extent of various cryogenic materials commonly used in the LNG industry, some of which have been operated for more than 40 years under cryogenic conditions [1]. In particular, the 9% nickel steel inner walls of the 500 m3 storage tank, which is one of the most widely used cryogenic steels in the LNG industry, in particular for above ground storage tanks, as well as the tanks insulation material (perlite) will be targeted for detailed analysis. It was therefore decided to implement the work on this topic within the framework of an international collaboration between major actors in the LNG business, allowing the sharing of the results and promoting enhanced exchanges on the aging analysis of cryogenic materials. Initially, the Korea Gas Corporation and Osaka Gas Company joined Gaz de France in 2002 in this Joint Industrial Program. More recently, Tractebel and Total joined this project in 2003 and it is hoped that additional companies which can benefit from the assessment of the life span of cryogenic materials will join this partnership. DESCRIPTION OF THE 500 M3 STORAGE TANK The 500 m3 LNG storage tank of the Nantes cryogenic testing facility was constructed by the company Socit des Forges et Ateliers du Creusot in 1959 and commissioned in 1960. It is a 9% nickel steel cylindrical self supporting tank with a vertical inner wall height of 8.5 m and a diameter of 8.5 m. The inner vertical wall was welded to the bottom base. The shape of the roof of the tank is conical. The inner vertical and bottom walls are both 4.5 mm thick and the inner roof is 5 mm thick. The outer vertical wall was made of carbon steel and had a diameter of 9.85 m. and a height of 11.20 m and was essentially homothetic to the inner wall of the tank. The insulation of the dome, shell and bottom walls of the tank originally consisted of multiple layers of expanded cork, combined with two layers of glass wool (0.24 m thickness) for the shell wall. The insulation of the roof and shell walls (initially made up of multiple layers of expanded cork) was revamped in 1980 due to the presence of abnormal heat leaks into the tank. The insulation of the shell wall was changed to layers of 0.1 m of glass wool and 0.57 m of loosely arranged perlite and that of the roof to perlite exclusively. The insulation space was then maintained under a nitrogen atmosphere with a small gage pressure, to avoid moisture buildup and insulation degradation. The bottom wall insulation was made of the original 0.5 m thick multilayered expanded cork. The maximum relative (gage) operating pressure was 150 mbarg. The tank was protected against possible excess pressure build-ups by two pilot controlled relief valves, each of which was able to exhaust up to 6500 m3(n)/h of gas flow.

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The tank rested on a circular concrete slab having a thickness of 0.1 m and which is 1.3 m above the ground. The shell wall was constructed with rectangular 1.157 m x 2.968 m 9% nickel plates which were welded together in pairs at the construction factory. The pairs were then welded together on site. There were 7 shell courses used for the shell wall and each shell course consisted of 9 rectangular plates. The welding was achieved by electric arc with Inco-weld type A Inconel electrodes. The bottom wall was constructed with plates of varying shapes and sizes. Both the shell and bottom wall plate thickness was 4.5 mm and the roof plates were 5 mm thick. The shell and bottom plates were connected by a curved plate of 7 mm thickness, in order to minimize mechanical strain on the shell/bottom wall weld joint. Before shipment of the plates on site, a Framalite paint layer was applied to the inner and outer sides of the plates for corrosion protection. The internal equipment of the tank had been composed of different filling, emptying and recycling devices, a level gauge, a pressure pick-up in the ullage space of the tank, two vertical measuring masts with a series of temperature and pressure probes, a vertically traveling Whessoe model 1146 Liquid Temperature Density (LTD) gage and an internal observation system consisting of an endoscope device. OPERATING HISTORY OF THE 500 M3 STORAGE TANK Numerous LNG behavior trials were carried out in the 500 m3 storage tank during its 40 year operating history. In particular, one can mention the experimental campaign conducted between 1987 and 1989 on the efficiency of LNG recycling devices and the behavior of LNG stratifications inclusive of the rollover event, but also the recently concluded campaign carried out in 2000 and 2001 on the characterization of six commonly used tank bottom and top injection LNG tank filling devices.

Figure 2. 500 m3 tank operating history from 1960 to 1980

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In these two testing campaigns, more than 80 trials were conducted in the 500 m3 tank, using a wide range of liquid levels, operating pressures and LNG qualities. Throughout its 40 year operating history, this tank has been subjected to numerous filling and emptying cycles, as well as to multiple openings to the atmosphere, which cause particular strain on the tanks walls, since their temperatures migrates from about 160C to ambient temperatures in a relatively short period of about 3 weeks. The operating history of the 500 m3 tank can be highlighted by the LNG level variation as a function of time, as shown in figure 2 above. As can be seen in figure 2, the LNG level varied quite extensively from a low heel value to the maximum filling level of about 7.5 m. Also, the tank was subjected to four openings to the atmosphere in this period of time (highlighted by circles in the figure). Figure 3 hereafter shows the more recent operating history of the tank from 1996 to 2001. Again, one can witness the frequency of thermal solicitation of the tank due to sharp LNG level variations, as well as the realization of five openings to the atmosphere in a span of 4 years.
Closing down of Nantes LNG Testing Station
8 7 LNG Height 6 5 4 3 2 1 0 01/06/1996

LNG Height RL500 (m)

01/06/1997

01/06/1998

01/06/1999

31/05/2000

31/05/2001

31/05/2002

Date

Figure 3. 500 m3 tank operating history from 1996 to 2001 NON-DESTRUCTIVE EXAMINATIONS OF THE 500 M3 TANK The non-destructive investigations, all of which were supervised by Gaz de France, consisted in realizing field examinations of the outer aspects of the 500 m3 tank and visual observations, paint dye penetrant tests and radiographic tests of selected areas of the inner walls of the tank. Visual Inspection of Outer Tank Wall A visualization of the outer tank shell and roof plates was carried out, as well as the shell plate holding down bolts and the junction between the shell and bottom plates.

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The outer tank shell and roof plates were found to be in good condition, as well as the junction between the shell and bottom plates. Most of the shell plate holding down bolts were corroded. The tank inlets and outlets through the outer roof wall did not show any corrosion nor defects. Visual and Paint Dye Penetration Tests of 9 % Nickel Walls Selected sections of the tanks inner shell and bottom 9% nickel walls were visualized (VT tests) in order to confirm their qualitative states, but also to make a first identification of eventually affected areas. Of particular interest was the weld joint between the shell and bottom walls, since this area experienced some of the largest strains, in particular for high levels of LNG in the tank. After conducting the visual examinations, paint dye penetrant (PT) tests using a red BABB CO DP55 penetrant were carried out on an entire 5 m wide vertical section of the tanks shell wall ranging from the tank bottom all the way to the roof plate junction, both on the tanks inner and outer sides. The objective of this examination was to allow the detection of eventual surface defects of the 9% nickel wall. Also, a 5 m wide horizontal section spanning an entire tank diameter on the inner side of the bottom wall of the tank was examined using both VT and PT tests. Bottom Wall VT and PT Examinations. The following figures show some of the observations made on the tanks inner side during the tests for the bottom wall welds.

Figure 4. Weld showing no visual defect

Figure 5. Weld with base metal irregularity

These observations show that the bottom wall welds which were examined by VT and PT tests did not reveal any defect linked to the aging of the metal, but only defects due to the original construction of the tank, such as undercuts, porosities and excess weld metal. Shell wall VT and PT results. The following figures show some of the observations which were made on the tanks inner side during the tests on the shell wall welds.

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Figure 6. Weld showing no visual defects

Figure 7. Weld with undercut

Figure 6 above shows a vertical weld with no defect revealed by either VT or PT tests. Figure 7 shows a vertical weld with an undercut. Again, the VT and PT tests which were carried out on the vertical shell wall welds and on the shell/bottom wall weld joint did not reveal any defects due to the aging of the tank. Radiographic Examinations of 9% Nickel Walls In order to confirm the degree of aging of the tanks walls, it is not sufficient to carry out VT and PT tests, since these will only allow detection of apparent surface defects, but not defects embedded inside the wall. For this, radiographic tests (RT) were used using an Iridium 192 (11 Curie source). These tests, coupled with the PT tests, allowed for a thorough screening of the eventual defects which exist. The RT tests were carried out on selected areas on the shell and bottom walls of the tank. The following figures show some of the defects detected with the radiographic examinations.

Figure 8. Weld with embedded cavity

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Figure 9. Weld with undercut (left arrow) and clustered porosities (right arrow) All of the defects appear to have occurred during the original construction of the tank and are not thought to be due to any aging process of the tank. In figure 8, an embedded cavity is possibly present in the weld shown, but this cavity did not have any effect on the integrity of the tank. This shows that even after 40 years of operation of the tank, this original cavity seemingly was not much affected by any aging process, thus showing the good durability of the weld. DESTRUCTIVE EXAMINATIONS OF THE 500 M3 TANK In order to complete the observations made with the non-destructive tests described above and confirm the aging extent of the 9% nickel inner wall of the 500 m3 tank by comparison with original tank data obtained in 1960, various destructive tests need to be carried out. Table 1 below summarizes the destructive tests which are being carried out on selected plates of the inner 9% nickel wall. Both Gaz de France and Kogas are carrying out in parallel the various destructive tests, in order to confirm repeatability of results emanating from two independent sources. In what follows, only the preliminary characterization results obtained by Kogas are shown. Table 1. Destructive tests carried out on 9% nickel steel
Test Items Base Metal and Welds of inner 9% nickel wall Chemical composition analysis Micro-hardness (Vickers 5) Macro- and micro-structure analysis Tensile tests at room, LNG and LN2 temperatures : yield strength, tensile strength, elongation Impact tests at room, LNG and LN2 temperatures Requirement ASTM A553 ASTM E384 ASTM E8M ASTM E23 Test temperature room room room room, -164C, -196C room, -164C, -196C

notch locations : base metal, weld metal, fusion line, fusion line + 1 mm, fusion line + 3 mm
CTOD tests at room, LNG and LN2 temperatures notch locations : base metal, weld metal, fusion line, fusion line + 1 mm, fusion line + 3 mm ASTM E1290 or BS 5762 room, -164C, -196C

The areas which are being examined concern the 1st shell course (lower part of shell wall adjoining the bottom wall), one of the middle shell courses (located in the uppermiddle part of the shell wall) and a section of the bottom wall adjoining the shell wall. In this way, various zones having endured different mechanical and thermal strains and stresses will be covered by the examinations. 9% Ni steel sample plates (each 1.4 m wide 2 m long) have been taken from the three areas mentioned above : bottom wall (K5), lower shell wall (K2) and middle shell wall (K4).
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Chemical Analysis Tests A chemical composition analysis was carried out of the base metal and weld metal for each of the three areas studied. The 9% nickel steel base metal needs to conform to the chemical requirements according to ASTM A553 type I (quenching and tempering steel) or ASTM A353 (double normalizing and tempering steel). The chemical analysis results of the base metal are shown in table 2 below. The lower (K2) and middle (K4) plates of the shell wall and bottom (K5) plate had almost the same chemical compositions. These results of the base metal composition conformed entirely to the requirements of ASTM A353 or ASTM A553 Type I. In particular, the phosphorous and sulfur contents were about 60 ppm and 120 ppm, respectively. It is known that the presence of these impurities lowers the toughness of 9% Ni steel under cryogenic temperatures. Table 2. Chemical analysis results of base metals
9% nickel steel ASTM A553 (Type I) or ASTM A353 Original tank data K2 (lower shell wall) K4 (middle shell wall) K5 (bottom wall) C 0.13 0.038 0.02 0.02 0.02 Mn 0.98 0.52 0.56 0.54 0.56 Chemical Composition (wt%) Si 0.13 ~ 0.45 0.27 0.25 0.24 0.25 P 0.035 0.007 0.005 0.006 0.006 S 0.035 0.013 0.012 0.012 0.012 Ni 8.40 ~ 9.60 9.36 9.24 9.21 9.24

Macro-Structure Analysis and Micro-Hardness Tests Macro-structure analysis and micro-hardness tests were carried out on two samples of each plate. Macro and microstructures of the base metal and welds was investigated using an optical microscope. The etching reagents used were 3% Nital for the base metal and HNO3 + HCl + Glycerol (1:2:3) for the weld metal. The micro hardness tests were performed with a micro Vickers hardness tester using an applied load of 0.5 kgf. The Vickers 5 micro-hardness test results are shown in figures 10, 11, 12 and 13 below. The heat affected zone had the highest value (around 330) and the hardness of deposit metal was slightly lower than that of base metal. It is presumed that the toughness of heat affected zone will be the lowest. This assumption will be checked by the Charpy impact tests and CTOD tests which will be carried out. Lower part of wall plate. Figure 10 below shows the macro-structure photographs of the lower shell wall K2 plate and figure 11 shows the micro-hardness distribution across the welded joint.

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Figure 10 (a) and (b). Macro-view of welded joint (K2 plate)

400

400

BM
350

HAZ

WM

HAZ

BM

350

BM

HAZ

WM

HAZ

BM

Vickers Hardness (Hv 0.5kg)

Vickers Hardness (Hv 0.5kg)

300

300

250

250

200

200

150

150

100 -15

-10

-5

10

15

100 -15

-10

-5

10

15

Distance from Center of WM (mm)

Distance from Center of WM (mm)

Figure 11. Micro-hardness distributions of welded joint (K2) Bottom plate. Figure 12 below shows the macro-structure photographs of the bottom wall K5 plate and figure 13 shows the micro-hardness distribution across the welded joint.

Figure 12. Macro-view of welded joint (K5)

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400
400

350

BM

HAZ

WM

HAZ

BM
BM
350

HAZ

WM

HAZ

BM

Vickers Hardness (Hv 0.5kg)

300

Vickers Hardness (Hv 0.5kg)

300

250

250

200

200

150

150

100 -15

-10

-5

10

15

100 -15

-10

-5

10

Distance from Center of WM (mm)

Distance from Center of WM (mm)

Figure 13. Micro hardness distributions of welded joint (K5) Micro-Structure Analysis of Base Metal and Welds The optical microstructures of the base metal (BM), weld metal (WM) and heat affected zone (HAZ) are compared in figure 14, photos (a) through (f). The microstructures of the weld metal show the typical solidification microstructures of austenitic steel (photo (a). The solidification type shows face centered cubic (FCC) single-phase solidification and there were no differences found in the sampling positions.

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(a) WM

(b) WM+FL

(c) HAZ+FL

(d) HAZ

(e) HAZ+BM

(f) BM

Figure 14. Optical microstructures of base metal and weld metal (K2-3) The basic structure of the base metal, shown in photo (f), was composed of tempered martensite with some portion of retained austenite. Due to the high hardenability of 9% nickel steel, it was very difficult to find out a difference in the microstructure. The visible black band from the photographs was due to segregation during the initial solidification period. From the microstructure observation of the heat affected zone, coarse grained regions existed near the fusion line and they decreased as the regions became more distant from the fusion line. The absence of micro cracks in the WM, HAZ and BM microstructures indicates that no phase transformation occurred in the tank material during its 40 year service life. Microstructures can be related to micro-hardness measurements as follows [2,3] :

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Weld Metal : Phases found in the welded structure depend on the filler material, an Inco-weld type A Inconel electrode in this case (around 76% Ni and 16% Cr). This material stabilizes austenitic phases, whose hardness range typically between 155 and 190 VPN. In figure 13(a), a higher value of micro-hardness is found for weld metal. This could result from a variation of heat input during welding, which indirectly affects the phase distribution and the grain size, and therefore enhance the hardness value. Base Metal : According to ASTM A553, base metal is tempered between 565 and 635C, then quenched (air cooling). Microstructure is expected to be tempered martensite, and the measured values of micro-hardness for BM are consistent with this microstructure. Heat Affected Zone : The structure is expected to be homogenous and coarse grained. However, as a result of the absence of post-weld treatment and the small thickness of the BM plates, which induces high cooling rates, hardness values remain high in the HAZ. CONCLUSION The non-destructive examinations (VT, PT and RT) which were carried out on the 9% nickel inner walls of the Nantes 500 m3 storage tank, which had been continuously operated for more than 40 years, did not reveal any significant defects and in particular no defects which were due to the aging of the tank. This finding contributes to proving that the operating lifetime of such a tank is at least 40 years. However, in order to confirm this proven lifetime, a comprehensive campaign of destructive tests needs to be carried out on selected samples from the 9% nickel walls. These destructive tests, which are being applied on the base metal and welds, include chemical analysis examinations, micro-hardness tests, macro and micro-structure analysis, tensile tests (yield strength, tensile strength and elongation), Charpy impact tests and Crack Tip Opening Displacement (CTOD) tests. The preliminary destructive characterizations results obtained so far using chemical analysis, macro and micro-structure analysis and micro-hardness tests on the base metal and welds confirm the properties expected of these metals. However, tensile, impact and CTOD tests will be needed to evaluate the aging extent of the 9% nickel steel (by comparison with the original 500 m3 tank data), as well as to determine the residual life expectancy of the tank, if it would have been operated beyond its 40 year service life. Thus, by analyzing the aging extent of the materials through both non-destructive and destructive tests, the longevity and durability of these materials can be confirmed, therefore allowing exemptions from inspections, all this within a context of stricter regulations. Knowing that such inspections impose heavy costs on installations due to the stop of production, the cost saving benefits are evident. By capitalizing on this improved knowledge of the aging of LNG installations, the LNG industry will be better positioned not only to possibly increase their proven life span, but also to improve their functioning and safety. In this way, further improvements in the capacity of the LNG industry in providing a cost-efficient, clean and safe energy source can be obtained.

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REFERENCES CITED 1. Uittenbroek D., Blaauw A., Wahab H., Hirose H., Hirai S. (1998) Demolition, inspection and tests of disused LNG tank in Brunei. LNG 12 Conference, May 47, 1998, paper 5.2. 2. Kawasaki Steel Technical Report, September 1982 3. Vishniakas, I. (2003) ISSN 1392-1320 Materials Science Vol. 9, no. 2

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