Successful and safe de- and recommissioning of a cold ammonia storage tank

Abstract The paper that Continental Engineers BV and OCP present discusses the decommissioning procedure to carefully and safely empty and inertize a cold ammonia storage tank and the problems that could and have occurred. The decommissioning took place in April/May/June 2004 and all together it covered a period of 6 weeks (emptying 4 weeks, inertizing 2 weeks). It also discusses the recommissioning of the same tank, which took place several months later. For the recommissioning first the oxygen had to be removed until a level of <1.5 volume % had been reached and after that a controlled filling with gaseous ammonia should take place in order to avoid too cold spots in the steel bottom or wall which could cause stress cracks. Recommissioning took a period of 2,5 weeks and went very successfully thanks to the excellent preparation and help of OCP management and employees. The tank was cleared and finally accepted by OCP on 19 October 2004 as being successfully recommissioned. Authors:

L.A.J. Tol and G.J. Tol
of Continental Engineers BV - The Netherlands in cooperation with: A. Bourras of OCP Jorf Lasfar at El Jadida, Morocco




• 2 coastal sites of chemical transformation (Safi and Jorf Lasfar) • 4 shipment ports (Casablanca. See fig. Jorf Lasfar. OCP’s production sites. safely refilled with ammonia until the fluid phase of –33oC was reached. Production sites • 4 phosphate mines in the country (Khouribga. O sioning of the cold ammonia storage tank IR5502. of which some data are given below: TankData: Liquid ammonia: Temperature of liquid: Diameter: Height of wall: Material of wall: Height of dome: Material of dome: Design code R NH3anh. In March 2004 Continental Engineers BV (C E) provided OCP with the required procedures for the de. inspection and re-insulation should take place and the tank would have to be recommissioned. 3. a place 100 km from Casablanca and located near the Atlantic coast and stored in two big tanks with a volume of 23. The pump suction line was however located somewhat above the bottom of the tank (300 mm) which means that a certain amount of liquid ammonia remains in the tank.Phosphoric acid: 1. 2% in the south part) 85 % of the world phosphate’s production is intended for fertilizer production. A great deal of this ammonia is transported to OCP’s site of Jorf Lasfar at El Jadida. The Netherlands.000 t/a. After that. amounting to. -33 oC 35 m 24 m ASTM A537 6m ASTM A516-70 API 620 app. Benguérir. 1.Phosphates: 12.20 m The tank is placed on a concrete ring foundation which is protected against freezing by a system of heating coils.2 Mt Volume: 23.1. Safi and Laâyoune) 2.e. It is important to state that there were no manholes available and there was not a provision for draining below tank bottom level.000 m3. it has to be emptied and all liquid and gaseous ammonia would have to be removed from the tank. • Exportations: . 2.0 Mt . i. OCP imports ammonia (NH3) by ship in the total amount of 400. The center of the ring is filled up with a layer of sand and a layer of 200 mm foam glass. approx. as reputed ammonia-engineers whether they could prepare a solid procedure for the safe decommis- 2.Fertilizers: 2. Production levels: • Phosphate production: 23 Mt (52% are transformed in phosphoric acid and fertilizers).000 m3 Insulationlayer: 120 mm (polyurethane). 300 t.0 Introduction ffice Cherifien des Phosphates Group (OCP) was founded in 1920 and its achievements are: 75 % of world phosphate reserves (98% in the middle of the country. production levels and position are as follows: 1. The route to use aqueous ammonia or to flare was not feasible at OCP’s location which meant that all re- AMMONIA TECHNICAL MANUAL 126 2005 .and recommissioning of the mentioned ammoniastoragetank nr. IR5502. OCP wanted to overhaul one of these tanks in 2004 (for the first time since the tank was put into operation in 1987) and they therefore inquired early 2004 at Continental Engineers BV (C E) at Zaandam. Position in the world market: • Leader in phosphate’s exportation under all its forms • Leader in phosphoric acid exportation To produce their fertilizer. Annular space between tank wall and concrete out side wall: 1. by estimation.1 Preparing the Procedure: Preparatory observations and actions: Before the tank can be inspected. Youssoufia and Boucraâ/Laâyoune).6 Mt P2O5 .

Possible options to remove the remaining ammonia as considered by C E are: 1. A quantity of 100 t ammonia should then remain in the tank and after that we could pump out another part of the ammonia by means of a flexible hose which could result in an extra reduction of at least 50 t. 4. of liquid ammonia at reduced flow and the required time for that should be approx. / 150 kg/h) 3. most of all.04%. 5.: ing: NB: 150 kg/h Estimated time/period for only emptyapprox. (spare) heater(s) for superheating ammoniavapour. 16-32 days (boiling off rate 0. 2. 12 days (pumping 60 t. which was fully acceptable. 2. 2005 127 AMMONIA TECHNICAL MANUAL . certain provisions have to be made such as: • a storage facility for liquid ammonia. According to our calculations indicating a pressure increase of 0. etc. The left over then would have to be evaporated For each of the aforementioned options. however not practible nor feasible Conclusions on methods for emptying: • Execution by method 1 was considered not to be safe. 3. Adding water to the tank and pumping aqueous ammonia out of the tank. 27 days (100 t. taking into account that the pressure relief valves at the tank were set at 1. because of our (previous) bad experience with bringing in flexible hoses • Methods 2 and 3 were considered as feasible methods on OCP’s site • Method 4: not applicable because of lack of enough water and OCP was not in a position to use aqueous ammonia • Method 5: not feasible because of safety but also for practicable reasons Based on the required time. calculated quantity of vaporized ammonia 1. Practicle calculations Increasing the pressure by increasing the set point of the compressor. “Natural” evaporation. Using only “hot” ammonia vapour.2 Be well prepared before you start!: Necessary equipment & tools Before entering into the right procedure and executing the necessary activities.03 bar. • availability of ‘hot’ gaseous ammonia (45 o C).02%-0. 2 with schematic diagram. practical considerations C E advised OCP to use method 3 “natural evaporation” for emptying the tank. the pump could remove an extra 200 t.16 bara. • flexible hoses and suitable pumps. the required investments and. 50 hours. • a fan for ventilation purposes etc. A combination of pumping liquid ammonia out of the tank through a flexible hose via the suctionline and evaporating the remaining liquid with “hot” ammonia vapour. • availability of nitrogen for purging purposes. not applicable nor feasible at OCP’s (see also point 2.maining ammonia would have to be removed by evaporation and drawn off as vapour. dependant of insulation quality of tank and ambient conditions) 4.) 2. calculations were made and the required “decommissioning” time was estimated resulting in: Option no. 10 days.1) 5. to minimise eventually the required heat for evaporation one could first reduce the liquid level in the tank by increasing the operating pressure of the tank (see below). Evaporating the remaining liquid by heating the annular space between the concrete wall and the storage tank (in that case the insulation had to be removed). Purging of the tank with nitrogen prior to entrance of oxygen (air) was necessary to avoid the (explosion) risk of ammonia in an oxygen-rich environment and which could occur in case of a 15-28 vol-% ammonia concentration. See fig. However. out in 1 day and 11 days for evaporation of 40 t.

loading and emptying 3. 2. emptying by natural evaporation. i. Theory The assumption was that 100 t. OCP ordered C E to start with the proposed activities mid April 2004. The measured levels varied from 28 cm to 45 cm liquid and the question was: Is the content 100 t.4 Air ventilation before inspection of the tank: Before inspection by maintenance people could take place. This procedure was presented to OCP’s management in both English and French language. this because of their different densities. 2. the facts and the figures. so the first uncertainty arose. but this meant that approx. of ammonia should remain in the tank after pumping out a part by means of pressure increase in the tank. Assuming a low line velocity of 3 m/s through a DN250 line the expected purging time should amount to 60-70 hrs (< 4 days).000 Nm3/h blowing through a manhole. A 25% aqueous ammonia could however not be handled by OCP and so both ideas had to be abandonned. Parallelly it was locally investigated whether one could use the “watermethod” described under option 4. However our commissioning manager could not check nor verify the level of ammonia in the tank.5 Permission to start: Continental Engineers BV produced based on its experience. or in other words: Reality Check of Practice vs. 7500 m3 of (demi)water should be needed. Based on this extensive procedure. despite the advice of C E to use option 3. Decommissioning and encountered problems. OCP could also not give a reliable measurement of the amount in the tank. it was decided to go back to the original method. The required time for air ventilation based on comparable situations was estimated at 7 days. Because of the “forced” methods to at first remove a big amount of ammonia would not fulfil the requirements to empty safely and adequately the tank. On the other hand emptying the liquid out of the tank by using the pumps was not successful since we did not get out the expected amount possibly due to gassing.= 38 cm height)? A lot of time was spent to install a reliable measuring device by means of a floater. one of the flexible hoses brought in from the top was too short. See fig. in order to come to a 2 % solution of ammonia and water for disposal off to the sewer of the harbour.e.000 m3 of nitrogen was required. nitrogen purging and air ventilation would cover probably 30 days. one through the underpressure relief valve and the other through the overpressure relief valve. [~145 m3] or is it (much) more than the measurements indicated (250 t. but mainly because of the assumed higher content of ammonia. However.2. a detailed procedure for the overall decommissioning of the ammonia storage tank.3 Purging requirements: After all the liquid NH3 is evaporated. purging with N2 of the tank can be started. The nitrogen content has to be measured and when the O2-concentration is in the range of 20 to 21% ventilation can be stopped and maintenance and inspection personnel can then safely enter the tank. AMMONIA TECHNICAL MANUAL 128 2005 . This could be performed by means of a high perfomance fan of 50. While pushing out the ammonia the concentration of it should be measured at the outlet of the tank towards the refrigeration compressor. estimated time period for emptying. This was all done while not in operation. a thick shelf and finally steel buses. Furthermore. it was decided to blow in “hot” ammonia in order to speed up the evaporation rate. ventilation by air has to be applied. 5 for overall schematic diagram of the ammonia storage system for cooling. In total the required. Flexible hoses were brought in into the tank. For this purging the availability of an amount of 30. The nitrogen should have to be carefully inserted since the layers of ammonia and nitrogen clouds can mix up with eachother when this is done "too wild".

more time was required. 3. When the level of nitrogen is about 1 meter above tank bottom. The air purge period took approx. When this level was reached. there is a sharp separation between the two cloud layers. auxiliary tools & equipment and ensure the local availability. • One could not adequately measure the liquid level i. at least for future to build tanks.000 m3 of nitrogen and it took eventually 2 days to feed this amount (in stead of 4). the schedule (30 days) could not be maintained (i. maintenance and for measuring purposes. 30. This can be achieved by adding nitrogen very slowly (1. 3. make a drain beneath the tank bottom level to secure emptying the liquid from the tank by means of pumps.e. We then could calculate how many hours it should take to reach the top of the tank (24 m). 4.2 Nitrogen purge & Air Purge Purging with nitrogen (N2) is based on the principle of creating a difference of density in the layers of NH3 (molecular weight 17) and nitrogen (molecular weight 28). 1. When the oxygen level is approx. To improve the evaporation rate of ammonia OCP removed the insulation at several places (which had to be removed anyway for renewal) by taking out 2x2 m spots allowing entering of heat through the wall. The first conclusions of the reality check were: • The pumps did for some unsolved reasons not fulfil the expected duty (possibly gassing) • We could not check. in this case ~45 days). It is advisable to make a very practicable procedure (with step-by-step actions and explanatory drawings) in stead of a desk report with theoretical assumptions and schemes. 2005 129 AMMONIA TECHNICAL MANUAL . See fig. For environmental reasons the tank is connected to the other tank because of ‘pushing out’ the NH3. Before preparing a (desk) procedure the engineer should execute a site visit to make notice of local circumstances and discuss the planned approach. 3 for a schematical diagram of air ventilation On the top of the tank we installed oxygen detectors to measure O2-content of the gas/air mixture. 2. the remaining quantity of ammonia • The alternative methods could not be applied or did not work • After all this. We needed an amount of approx. in order to ensure a safe environment for maintenance and inspection personnel. 3. the two tanks could be separated and the mixture of ammonia and the last nitrogen could be blown through a water tank in order to avoid environmental hazard.5 t ammonia/day. Perhaps the tank was too well insulated. 7. Contingency (x %) for the required time period should be timely communicated and built in to the proposal towards client/owner.The expected rate of the liquid level reduction was approx. Looking back the method with inserting “hot” gases had to be preferred. the amount can be increased to maximum capacity (~800 m3/h). 3 days. the amount of nitrogen can be increased (v=3 m/s). but in practice it did not work that way. Owner should install accessible manholes in the tank for inspection.1 Lessons learnt for both parties at the phase of emptying the tank as part of the overall decommissioning: 6. When this is done very carefully. The engineer should verify and list all the necessary measuring devices.5 m/s. Owner should. by removing parts of the insulation shield. One should monitor the pressure in the tank (which in the OCP case has to stay below 100 mbar). and when the level is about 2 meters above the tank bottom. 5. 1 cm/day equal to 6. from the outside of the wall what the level was (one could not observe a distinct colour difference) • There was not 100 t of ammonia in the tank but (much) more (some 250 t) • Flexible hoses should be available and if yes they should be of enough length. DN 250) in order to avoid turbulence via the manchet in the suction line to the bottom of the tank and take off the ammonia vapor with the compressors. 20 % (to be measured with Dräger tubes or similar) and the NH3-concentration is < 20 ppm (MAC value) the environment is safe for entering the tank.e. After two days already we could install the air fans [ ] for the purge with air via the manholes on the top and via the suction line at the bottom. it is however sometime quite difficult to insert these properly into the tank and liquid.

which was o.15 bara in order to observe and check whether all the connections are tight (by using bells of soap) and which took an extra day. So. temp. can be brought into the tank. The client undersigned mid June 2004 the taking over protocol stating that the decommissioning.k. • All manholes shall be closed. it could be filled with ammonia gas which should slowly be turned into cold liquid ammonia at –33 oC. but at least everything went in a controlled and a safe way. AMMONIA TECHNICAL MANUAL 130 2005 . the rabbit indeed survived this exercise. however with some delay. and later liquid ammonia. It was agreed between parties that when the rabbit survived at least 15 min. was finalised..14% O2 and this is considered to be a sufficiently safe value to start with blowing in gaseous ammonia. 5. First of all. The ammonia gas was taken from the other storage tank [nr. one should take into account a few safety measures up front: • All inspections and repairs should have taken place according to rules and legislation. • Availability of (enough) nitrogen for purging . Another risk is the build up of electrical charge due to static electricity while spraying liquid ammonia into an oxygen containing tank. However. but why? It is to state that the presence of oxygen in connection with (liquid) ammonia can lead to a considerable increased risk of stresss corrosion cracking (SCC) of tank material. Inspection and re-insulation OCP executed after the decommissioning the inspection of the tank which gave no major problems for the maintenance department.3 and 20. The procedure of feeding the ammonia vapour into the tank (at a rate of 500 Nm3/h.e. 5. Apart from the measurement by means of official detection the rabbit proof was also applied by the client. The re-insulation was executed by a Morroccan company and the whole wall and dome . bottom and manholes indicated an oxygen level between 20.. The explosion risk will be there when the air contains between 15 and 28 % of ammonia gases. During this process the tank temperature will be decreasing.2 tank Bringing in ammonia vapour into the 5. which should be removed first. While the detectionmeters at top. approx. C E estimated that this should take a few days and actually after 4 days the O2-level in the tank was <1. When nitrogen is inserted the oxygen content of the outcoming air will be continuously measured and one can see when the atmosphere in the tank becomes ‘inert’. ~40 oC)) should take several days and each time the laboratory (of the client) has to measure the ammonia content in the tank. Recommissioning and its features In September 2004 OCP was ready with the reinsulation and was ready to recommission the tank i. all the air in the tank should be evacuated by feeding nitrogen into the tank.Before entering the tank first of all enough lighting should be brought in and men should first inspect whether there was oil or other dirt on the bottom.5 %: we actually measured 1.7 %. were covered with a new layer of 120 mm polyurethane.1 Nitrogen purging and safety measures to avoid the risks 4. In stead of the estimated 4 weeks the total decommissioning period took 2 weeks extra. This has to be done safely and slowly in order to let the tank “follow” the required temperature change of less than or equal to 1 oC/h. • Availability of (enough) liquid ammonia for filling and cooling the tank gradually. • All relief valves to be checked and installed. 1. 4000 m2 . to execute this nitrogen purge. first the air will be “replaced” by nitrogen and just after that gaseous ammonia. This is an almost fail safe test to check whether a man can safely enter such a tank The method is simple: catch a rabbit and let it in into the tank and look if it survives after a while so: See fig. At the same time the tank had to be slightly pressurized to approx. the environment was to be considered safe for mankind. 4: Schematic drawing of a successful rabbit proof.

but for safety reasons we have chosen 3 x as much.1] on the premises of OCP and the liquid ammonia was later taken from the sphere.4 Closing of the recommissioning Due to excellent teamwork of all people involved. the total difference will be at least 52 oC. It took 4 to 5 days of filling with liquid ammonia (approx. If the temperature decreases too fast one should immediately slow down or stop the filling procedure to avoid any risk of stress corrosion cracking of the bottom or the side walls. L.5 %) At the end after three days the value measured was: 87 gr/m3 (~12. for giving us the opportunity and his cooperation to prepare and present this paper for the interested audience here at Toronto. It is of major importance to prepare a procedure. 6. which means that with an ambient temperature of +20 oC. Also up front the client should take the necessary measurements on site in order to secure a smooth execution of the activities and OCP did so. See fig.) of C E. manager projects dpt. 6.e. the recommissioning went very well and in total it covered approx. one can succeed in achieving the set goals. expert consultation and enough patience.5 days). but only by good communication.0 Summary and conclusions Thanks to the excellent cooperation between the commissioning manager of C E. especially Mr. Also our de/recommissioning manager. no persons were allowed by OCP in the neighbourhood. Continental Engineers likes to thank OCP that they were trustworthy to give the order for this decommissioning as well as the recommissioning to them. We can conclude that this recommissioning was indeed safely and successfully executed. 6: Photo of mr. the management and the operating personnel of OCP on site the decommissioning. during this procedure the temperature at the bottom and alongside the wall have to be carefully monitored by the responsible people. a time period of 18 days. -o-o-o-o-o-o-o-o-o-o-o- 2005 131 AMMONIA TECHNICAL MANUAL . Bourras of OCP (r. Gerrit Tol has to be mentioned since he was the ‘solid and cool’ factor for C E on OCP’s site during periods that the inside and outside temperatures were quite high…. i. The ammonia will be sprayed in from the top and will liquefy after a certain time period on the bottom of the tank. only one relief valve from a HE-vessel opened and blew off above the annular space. went well and after that the recommissioning even went perfectly. Because of the well taken safety precautions.) to cool down the tank to the level of -32 oC (actually measured). this is a measure to start with bringing in liquid ammonia for filling and further cooling down of the tank. At a flow rate of 70 to 120 kg/h the liquid ammonia has to brought into the tank. The actual NH3-values in the tank were measured each day: After one day the value was: 14 gr/m3 (~2 %) After two days it was: 38 gr/m3 (~5. subsequentely cooling down this bottom. 5. which is supported by experienced commissioning personnel and which is to be accepted by the clients’ representatives on forehand. There will be however always (unforeseen) problems on site.) and mr. No major problems occurred during this phase except for the blow off of a relief valve of a heat exchanger vessel. Note: No major incidents or problems occurred during this phase of recommissioning. there was only waiting time to let the ammonia vapourize. i. although quite some (unforeseen) problems occurred.e. 20 t.5 %) One should take samples from the tank until the N2content was below 5%..3 Cooling down the tank by spraying liquid ammonia. The total ammonia vapour time amounted to front of the ammoniatank. Mr.5 days. It is to be advised that the temperature drop has to be uniformly and be lower than 1 oC/h. It should therefore require a cooling down time of at least 52 hours. Finally C E like to thank OCP. Abdeljalil Bourras. Tol (l. 156 hours (~6. At the end of this activity the temperature at the bottom will be -32 oC. 5..

2: Schematic image of increasing the pressure in tank 2 AMMONIA TECHNICAL MANUAL 132 2005 .Attachments to paper 523 – AIChE Toronto Page 1 R obe du bac n o r m a l m in im u m liq u id le v e l D N 250 lig n e d e s o u tir a g e 250 m m c e n te r lin e 460 m m 300 m m 75 m m 100 m m Fond du bac Fig. 1: Location of suction pipeline near bottom of tank compressor open closed Tank 1 p=5 mb pump filter tank 2 p=150 mb Fig.

exhaust via nozzles (all valves were removed). 2005 133 AMMONIA TECHNICAL MANUAL .Attachments to paper 523 – AIChE Toronto Page 2 3 fans at middle manhole one fan at outer manhole one fan via the suction line Fig 3.: Extensive air ventilation by means of (5) air fans. air. After 15 minutes… Fig. 4: The rabbit proof for checking safe environment in tank after purging with nitrogen resp.

comp COMPRESSEUR 55IX01 55IP03/04 55IR03 CIRCUIT OF COOLING. LOADING & EMPTYING OF THE AMMONIA STORAGE at OCP 2005 . 5 HV603 HV604 DN 200 AG AMMONIA TECHNICAL MANUAL HV657 HV656 55IR01 55IR02 HV658/659/661 DN 400 AL HV651 55IS01 HV655 HV652 DOUBLE VANNE 55ID01 HV624 134 NH3 gaz Ref.Fig.

A.J.Attachments to paper 523 – AIChE Toronto Page 4 (Photograph) Fig. 6: Photograph in front of the big ammonia storage tank of Mr. 2005 135 AMMONIA TECHNICAL MANUAL . The Netherlands at the location of El Jadida. Morocco. Tol (l.A. and the author of the paper.). director of projects. L. Bourras of OCP (r.) of Continental Engineers BV. mr.

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