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LINDE AG

Process Engineering and Contracting Division Engineering

Work Instruction

Chemical Cleaning

QPB 09.02
(English) Sheet 1 of 9 Sheets

Table of Contents
Sheet 1 2 3 4 4.1 4.2 4.3 4.4 4.5 4.6 4.7 4.8 4.9 5 6 7 8 Scope of Validity..........................................................2 Purpose .......................................................................2 Definitions....................................................................2 Responsibilities, Procedure .........................................2 Extent of cleaning ........................................................3 Alkaline cleaning (boiling)............................................4 Pickling ........................................................................6 Passivation ..................................................................7 Checking the system once cleaned.............................7 Preservation ................................................................7 Protective coating process ..........................................7 Suction pipes from piston compressor and expansion turbines ......................................................8 Disposing of rinsing media and solutions ....................8 Other Applicable Documents and Notes .....................8 Documentation, QSE-Records ....................................8 Amendments ...............................................................8 Distribution...................................................................9

Attachment: QPB 09.02.01

Alkaline Boiling Process

Supplementation Issue 02: Definition of the responsibility of the Commissioning Manager QSE-Supplementation Inclusion of the draft QPB 04.14 for Compressor Suction Lines in para 4.1 e

02 01
Issue:

20.04.98 12.94
Date:

CBA/Bairlein CBA/Bairlein
Prepared:

DQ-H/Dr.Heucke D / Wege CB / Mndel D / Dr.Belloni


Reviewed: Approved:

QSU-Supplementation
Remarks:

Intellectual property rights reserved.


QM-template: QMRICHTE.DOT/Rev. Jun 95

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Sheet 2

QPB 09.02

Issue 02

LINDE AG Process Engineering and Contracting Division

Scope of Validity This work instruction applies to all sections responsible for commissioning of plants except the manufacturing sections.

Purpose This work instruction describes the chemical cleaning process for plant components. It also describes the extent of cleaning, i.e. which parts of a plant have to be cleaned and the possible ways of doing this. This work instruction is a guideline for those responsible for commissioning the plants. The operating instructions issued by the plant component manufacturer have priority. A contractor usually performs chemical cleaning. Therefore his process description and cleaning program must be checked, including the special risks refering to safety, health and environment when handling chemicals - see also para 4.9.

Definitions Alkaline Cleaning Process (Boiling) Boiling describes the process of cleaning the system using alkaline agents, preferably with changing pressure. In conjunction with the systems breathing (pressure changes), the chemicals used remove loose iron oxide coatings, bring dust particles into suspension and emulsify oil and grease. Rinse Cleaning Rinse cleaning refers to rinsing the system out using boiler feed water. Pickling The system is cleaned using a pickling solution. Passivation A passivation solution is used to passivate the bare internal pipe surfaces. Protective Coating (of steam systems) During the protective coating process, a thin magnetite layer builds up on the inside of the pipe. This magnetite coating protects against surface corrosion.

Responsibilities, Procedure In case Linde has the contractual responsibilities for precommissioning, Linde's commissioning manager is obliged to perform and check/proof the chemical cleaning activities according to the following instruction. If commissioning is within Client's scope under Linde's supervision, this instruction should be brought to client's attention. To ensure that the systems work properly, the high pressure steam and feed water systems and the suction lines from the piston compressor and expansion turbine must be cleaned thoroughly before commissioning. Begin by rinsing the systems thoroughly to remove loose dirt, rust, scale and foreign particles. Rinsing is followed by alkaline de-greasing or pickling.

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QM-template: QMRICHTE.DOT/Rev. Jun 95

LINDE AG Process Engineering and Contracting Division

Issue 02

QPB 09.02

Sheet 3

If you do not rinse the systems or rinse them insufficiently, damage and blockages are likely to occur despite thorough boiling and pickling. The formation of the magnetite protective layer is slowed down, and the steam will fail to meet purity standards for an extended period of time.

4.1

Extent of cleaning Existing condensate lines can be used to circulate the cleaning solutions. Otherwise, temporary lines must be used. Basically, the following plant parts have to be cleaned chemically: a) Boiler feed water high pressure system (HP-BFW) The boiler feed water system includes deaerator, up to the cracking furnace steam drums and steam boilers, the boiler feed water control stations and the feed lines to the high pressure steam desuperheaters, but does not include the boiler feed water pumps (suction and discharge lines only). Boiler feed water lines to the steam let-down stations.

b)

High pressure steam systems of cracking furnaces Pipes from the boiler feed water control station to the entrance of the feed water preheater. Transfer line exchanger and steam drums including risers and downcomers. Feed water preheater and high pressure steam superheater. High pressure steam pipes up to the high pressure steam shut-off valves.

c)

Steam boiler high pressure systems Steam boiler comprising of feed water preheater, steam generator (diaphragm walls), superheater and steam drum including downcomers and risers. Pipes from the boiler feed water control station to the boiler feed water preheater entrance(s). Pipes from the end superheater to the high pressure steam shut-off valves.

d)

High pressure steam system High pressure steam shut-off valves at the cracking furnace steam drums and steam boilers, with connections to the high pressure steam line including start-up line outlets. High pressure steam lines up to turbines. High pressure steam line up to the let-down station for high to medium pressure steam.

e)

Suction lines from piston compressors and expansion turbines

The Machine Department specifies the scope of delivery of reciprocating compressor units and expansion turbines as follows: Pulsation dampeners and prefabricated gas-lines are to be pickled, neutralized and suitably protected before shipment to site. The machine manufacturer specified the applicable pickling process and protection. Machine pipes leading process gas in Lindes scope of supply and pipes which cannot be prefabricated completely in the machine manufacturers shop are to be pickled or cleaned mechanically after being welded on site. The Machine Department identifies these pipes in the PIdiagrams with regard to the scope of pickling and gives these to the Department Flow Diagrams and Operation for inclusion in the Linde construction and operation manual of the plant.

QM-template: QMRICHTE.DOT/Rev. Jun 95

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Sheet 4

QPB 09.02

Issue 02

LINDE AG Process Engineering and Contracting Division

Construction and Commissioning Supervision on site inspects the pickled pipes before assembly and connection to vessels (pulsation dampeners, heat exchangers, etc.) Additional measures are to be taken if the systems are not clean. The scope of pickling in the case of very long pipes (> 100m) and large vessels (> 5m) upstream of reciprocating compressors, it is advisable to install a vessel type filter on the suction side. The installation of such a filter is to be determined by the Machine Department in agreement with the Department Flow Diagrams and Operation. This will be shown in the PI-diagram. The exact cleaning programme is drawn up by the contracted cleaning company, taking the suppliers guidelines into account. You will only achieve a good cleaning effect if the following points are adhered to: Plan and prepare for pickling far enough in advance. Define the extent of pickling. Define the pickling process and the pickling agent. Define the materials which should not be allowed to come into contact with the pickling solution. Remove these parts or take preventative measures. Provide cleaning nozzles correctly and in sufficient quantity. The cleaning program should include the following points: Circulatory systems employed. Information on the chemicals and utilities (see relevant accident prevention regulation and hazardous material data sheets). PI-diagram of circulation station and provisional lines. List of piping parts to be removed. Information on treatment/disposal of cleaning chemicals, etc.

4.2

Alkaline cleaning (boiling) An alkaline solution is used for boiling. It consists of: 1 kg solid sodium hydroxide or 1.3 l hydrated caustic soda (50%) per m water. 1 kg trisodium phosphate in flake form with approximately 20% P205 per m water. In the case of rusty surfaces, a good method of treatment is adding an oxygen binding agent such as 0.2 l hydrazine 15 or 100 g sodium sulphite per m water. Boiling can be performed in two ways: A) System breathing The system pressure is increased to approximately 50% of the nominal pressure and the temperature to approximately 250 C. This pressure is maintained for 2 - 4 hours, and then decreased to about 25% of nominal pressure. Following de-pressurisation, the system is cooled to approximately 120 C. This procedure is repeated 2 or 3 times. B) System circulation: The boiling solution is circulated in the system using temporarily installed pipes and pumps. The system pressure is increased to around 50 - 60% of nominal pressure, and kept at that pressure and increased temperature (see QPB 09.02.01) for approximately 50 hours. A magnetite coating forms during this type of boiling. Procedure Before boiling or pickling can begin, the systems must be checked for leaks, pressure tested, rinsed and de-greased with alkaline. Pre-rinse the systems using boiler feed water with a flow of 1 - 1.5 m/s using temporary centrifugal pumps. Debris is discharged at intermediate discharge points. The turbidity (extinction) of the rinsing water is photometrically measured at each of these intermediate discharge points. Once the turbidity value is satisfactory you can move on to the next rinsing section. Pre-rinsing is complete when the turbidity at the end of the system is almost exactly the same as the turbidity of the water entering the system.

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QM-template: QMRICHTE.DOT/Rev. Jun 95

LINDE AG Process Engineering and Contracting Division

Issue 02

QPB 09.02

Sheet 5

The subsequent de-greasing process is performed using an alkaline de-greasing agent. Attempt to achieve a water flow of 0.2 - 0.5 m/s when circulating the alkaline solution. The treatment temperature should be around 90 C. See the operating instructions of the manufacturer or the chemical cleaning contractor for exact details on how to prepare the alkaline feed water. During de-greasing, the phosphate content, pH value and conductivity are measured at defined intervals. Circulation is stopped when phosphate is no longer being used up and the circulation solution is optically clean. The alkaline solution is then removed from the system. In the case of steam drums and evaporators this is done by draining it off, and in the case of pipes and heating surfaces it is done by flooding with boiler feed water. For system components that are not going to be boiled or pickled subsequently, the alkaline de-greasing treatment should be repeated one or two more times (e.g. high pressure steam and condensate lines). The remaining alkaline solution that accumulates should be collected and neutralised using hydrochloric or sulphuric acid. Boiling out boilers and furnace steam drums Before beginning the procedure on a plant component you must make sure that the part concerned (boiler, furnace) is prepared for burner ignition, i.e. the ready-for-operation protocol has been issued. Isolate the system to be boiled from the rest of the plant. The boiling procedure should correspond to the manufacturers instructions, which should specify the maximum operating pressure and temperature, the duration of boiling and the concentration of the boiling chemicals. Fill the boiler or furnace steam drum to a visible water level with boiler feed water from the deairator, then add the chemicals at a suitable place using a pump. Continue by filling the steam drum to the normal level, and then close off the boiler feed water filling line. The pressure in the system is produced by igniting the burners (existing heat source), and increased as described in the manufacturers instructions. Important: When commissioning, the furnace and/or boiler lining are normally dried out as part of the boiling procedure. If this is being done, ensure that the heating curve with the lowest temperature increase rate is applied (drying curve for lining or heating curve for alkaline boiling process). Annex QPB 09.02.01 contains a diagram showing the alkaline boiling process for the transfer line exchanger / steam drum unit. A boiling time of at least 48 hours is necessary, and the first blowdown should take place after about 6 hours of boiling at 4 bar. Heating causes the drum water level to rise. The blowdown process is performed using pre-defined pressure stages and outlets. The boiling procedure is monitored by conducting analyses; the phosphate content of the boiler water, the p- value, the conductivity and the turbidity of the water are all measured at defined intervals. If the phosphate level drops to below half, phosphate can be added using the installed pump. The pressure should not be increased during the blowdown process. The boiling procedure, pressure increase rates, dwell times, blowdown times and maximum permissible pressure for blowdown should be specified by the manufacturer. The boiling process can be stopped once the phosphate level has been constant for several hours and the boiling solution is optically clean. After boiling, the entire contents of the transfer line exchanger must be drained off and the system rinsed at least 4-5 times with boiler feed water. The rinsing process can be stopped as soon as the water drained off reaches 0.1 mval/l caustic, or as soon as the pH value and conductivity of the water drained off are approximately the same as those of the fresh rinsing water. The water drained off should also be optically clean. Continue by opening the steam boiler drum and removing any dirt found inside. Check the fittings inside the drum. If the system has become very dirty after a long period of disuse or transport, you will have to repeat the boiling procedure described above several times. The hot caustic solution drained off during and after boiling, which has a pH value of 12-14, must be cooled down and neutralised with acid before being disposed of in a biological treatment plant. The system operator should take the steps necessary for this before beginning the boiling procedure.

QM-template: QMRICHTE.DOT/Rev. Jun 95

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Sheet 6

QPB 09.02

Issue 02

LINDE AG Process Engineering and Contracting Division

If the system is not going to be used immediately after boiling, it must be preserved as specified by the manufacturer. Upon inspection of the steam drum you will see that a magnetite layer has formed (black to blue-black). This layer will become thicker during subsequent operation. If the boiling procedure has been deemed successful, the boiler or furnace can be put into operation, provided the furnace/boiler lining has dried out completely.

4.3

Pickling Pickling is another method of preparing the high pressure steam and boiler feed water systems for operation. Pickling is performed using weak acids (e.g. citric acid) at a temperature of approximately 90 C. Like boiling, pickling must always be preceded by rinsing. Following pickling, the system must be passivated and, if necessary, preserved. Pickling offers the following advantages: The firing and heating gas systems do not have to be ready for operation. As the system is cleaned out more thoroughly, commissioning will normally be quicker. As pickling creates bare metallic surfaces, a homogeneous magnetite coating can subsequently build up on these surfaces. Disadvantage of pickling: It is usually difficult to dispose of pickling solution. Pickling of boiler and cracking furnace If pickling is to be used instead of boiling, it must be remembered that pickling involves a number of technical and chemical problems. Accordingly, pickling should only ever be carried out by a specialist firm. This firm must have several years of experience with the pickling processes, pickling agents and additives used. Because of this, these instructions contain no more than a description of the various stages involved in pickling. Before beginning pickling, the pickling company must make sure that all flange connections, glands, etc. do not leak, and that the pickling solution is not going to damage anything. The surface being pickled should be checked thoroughly, and the nature of the scale coating and its solubility should be assessed. The high pressure valves should be kept open so that foreign particles cannot damage the seat surfaces and so that the gland packing is protected against the pickling fluid. If some of the valves are to be closed during pickling, the seats should be removed and cleaned and the packing replaced. The pickling process can be divided up into 11 stages: 1. Rinse with water to remove loose dirt. 2. Alkaline de-greasing at approximately 80 - 90 C; duration 8 hours. 3. Emptying and neutralisation. 4. Rinsing of system. 5. System pickled at approximately 85 - 90 C; duration 15 - 18 hours. The pickling solution should remove iron oxide among other things, so that the surface ends up clean and shiny in appearance. Adding suitable inhibitors limits the acids corrosive effect on the metal itself (maximum material loss: < 20 g iron/m = < 0.0025 mm). The pickling process is complete when the iron content in the pickling solution is seen to change by no more than + 0.2 g Fe/l over a period of 2 hours. 6. Emptying and neutralisation. (e.g. with ammonia solution) 7. Rinsing with boiler feed water. 8. Secondary pickling at approximately 60 C; duration approximately 8 hours. One of the purposes of this step is to remove rust that has formed in steps 6 and 7. To avoid further corrosion, steps 8 to 11 should be carried out without interruption. Secondary pickling is complete when the iron content in the pickling solution is almost constant and does not exceed 0.5 g Fe/l. After pickling, all of the surfaces that have been pickled should be clean and free of rust and loose magnetite. The material loss as a result of pickling should not exceed 20 g/m. This can be checked by installing a representative piece of iron in the system before pickling. 9. Adjust the pickling solutions pH value to approximately 10 by adding a solution such as 25% ammonia. Temperature approximately 50 C.

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QM-template: QMRICHTE.DOT/Rev. Jun 95

LINDE AG Process Engineering and Contracting Division

Issue 02

QPB 09.02

Sheet 7

10.

11.

Passivate the surfaces by circulating an alkaline solution. Duration: approximately 12 hours of circulation at about 80 C. The pH value should remain between 9.5 and 10. Empty the system and neutralise the passivation solution. Finish by rinsing the system thoroughly with boiler feed water. Following complete emptying, the system should be brought into operation immediately or preserved as described by the manufacturer (e.g. dry preservation using nitrogen).

4.4

Passivation Fill the system with boiler feed water of the specified quality, adding Levoxin (activated hydrazine hydrate) to a concentration of 0.1% and ammonia to a concentration of 0.2%. The temperature of the passivation solution should be around 95 C. The passivation solution, whose pH value should be 9.5 to 10, is then pumped in the system for 12 hours at normal system pressure as produced by the auxiliary pumps. Empty the passivation solution out of the drums and piping systems using pressurised nitrogen, and cool the solution to 50 C before emptying it into the wastewater system. Dry the system out by purging with nitrogen.

4.5

Checking the system once cleaned Before beginning the checking procedure, use air (100% free of oil and water; instrument air) to remove the nitrogen put into the system during passivation. Perform random sampling checks. Checking the low-points in the piping: experience has shown that deposits collect at these points and in the valves. These deposits must be removed completely. In the region of the waste heat block you will need to cut out test sections to check the surface condition. The inspection nozzles on the distributors and headers are suitable for this purpose. Re-welding and 100% x-ray are the responsibility of the installation company and must be included in their contract accordingly.

4.6

Preservation We differentiate between wet and dry preservation. In the case of dry preservation(< 30% relative air humidity), the system is filled with nitrogen. To do this, the system must be completely dry and pure nitrogen must be used. In the case of wet preservation, the system is filled with degassed boiler feed water. An oxygen binding agent (e.g. hydrazine (100-300 mg/l)) is also added to the feed water.

4.7

Protective coating process After the circulatory system has been cleaned, a thin protective magnetite coating is applied to the internal surfaces of the pipes by heating the system to above 500C. The oxygen needed for forming Fe3O4 comes from the water, leaving hydrogen whose concentration in steam normally drops to around 5 to 10 g/l of condensate after 2 days. The iron and iron oxide brought into the system in the feed water (along with some iron from the pipe wall) continues to be converted into magnetite during operation; the extent of this depends a lot on the way the plant is run. The hydrogen level of approximately 5 g/l corresponds to iron conversion of 100 g/l in Fe3O4. Note: If passivation is done using NaNO2 or KNO2 (more expensive), a magnetite coating will begin to form during passivation. An additional protective coating process is not required.

QM-template: QMRICHTE.DOT/Rev. Jun 95

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Sheet 8

QPB 09.02

Issue 02

LINDE AG Process Engineering and Contracting Division

4.8

Suction pipes from piston compressor and expansion turbines If the internal diameters are small, the best approach is to remove the suction pipes, clean them mechanically and de-grease them, and place them in a pickling bath. The working procedure for this is described in section 4.3. If internal diameters are large, isolate the pipes you want to clean from the rest of the system using blind flanges before starting work. The pipes are then mechanically cleaned, de-greased, and pickled as described in section 4.3.

4.9

Disposing of rinsing media and solutions As already mentioned, all rinsing media and solutions must be collected and neutralised before being fed into the operators wastewater treatment system. It is important that the operator, Linde and the cleaning company work together to make the necessary arrangements well in advance. The alkaline and acid resistant condensate treatment tank is suitable for collecting solutions; sometimes rainwater catch tanks and ballast water tanks are suitable for this purpose as well. The local rules and regulations concerning safety, health and environmental protection (disposal) are to be followed.

Other Applicable Documents and Notes P&I Diagrams Operating manual Data sheets Transfer report for mechanical completion Manufacturers operating instructions Contracted cleaning companys cleaning programme Technical specifications for chemical cleaning of high pressure steam and feed water systems Relevant protection and safety measures when handling the chemicals used (accident prevention regulations, information sheets on hazardous materials) Ready-for-operation report for furnaces and boilers including a list of commissioning preparation work already done (only required for boiling)

Documentation, QSE-Records This Work Instruction is administered and archived by the Department Flow Sheets and Commissioning of Chemical and Gas Plants. The chemical cleaning performed must be recorded in a protocol by the contractor who carries out the cleaning. The protocol must contain all important information and data such as dwell times, pressures, analysis values, etc. One copy of the protocol goes to the customer, one to the project manager, and one to the commissioning department for administration and their archives. Archiving period is stipulted in QPA 05.03

Amendments Amendment proposals to this Work Instruction can be submitted informally to the Department Flow Sheets and Commissioning Chemical and Gas Plants.

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QM-template: QMRICHTE.DOT/Rev. Jun 95

LINDE AG Process Engineering and Contracting Division

Issue 02

QPB 09.02

Sheet 9

Distribution This Work Instruction is distributed by the QSE-Management.

QM-template: QMRICHTE.DOT/Rev. Jun 95

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