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PROJECT: SIMHAPURI ENERGY (P) LTD Sheet 2 x 150 MW CFBC BOILER 1 of 20 Plant area: BOILER PROCEDURE OF CHEMICAL CLEANING OF BOILER USING EDTA Sl.No. 1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0 11.0 PLANT DETAILS OBJECTIVES PROPOSALS SERVICES REQUIRED SAFETY PERECAUTIONS EMERGENCY PROCEDURES STATE OF THE PLANT METHOD COMPLETION CRITERIA WASTE TREATMENT & DISPOSAL APPENDICES LOG SHEET FORMATS ANALYTICAL PROCEDURES DRAWING LIST OF CONTENT

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PROJECT: SIMHAPURI ENERGY (P) LTD 2 x 150 MW CFBC BOILER Plant area: BOILER PROCEDURE OF CHEMICAL CLEANING OF BOILER USING EDTA 1.0 PLANT DETAILS Our CFBC boiler with steam-cooled cyclone consists of water wall panels, Water cooled screens and screen super heater coils in the furnace Zone and cyclone in second pass and all the high temperature super heater coils, low temperature super heater coils and economizer and enclosure panels in third pass of the boiler. 2.0 OBJECTIVE The objective of this procedure is to chemically clean and passivated the internal surfaces of the steam generating portion (water touched surfaces) and preheating surfaces (Economiser) using specified chemicals employing a single step process. This will render the above mentioned surfaces free of mill scale and other deposits and form uniform & smooth protective layer of magnetite to resist corrosion. 3.0 PROPOSAL The objectives are achieved by carrying out the following proposals. By carrying out one alkali flushing, one hot water flushing followed by cold DM water rinsing. Generally loose rust, debris, deposits and other materials left in the boiler are removed. Then, it is subjected to ammoniated EDTA cleaning for the removal of patchy mill scale and adherent rust. The acid pickled surface is passivated for the formation of uniform and adherent magnetite layer. Both chemical cleaning and passivation process are completed in a single step in the EDTA cleaning process. 4.0 4.1 SERVICES REQUIRED Prior to the commencement of chemical cleaning all the DM water storage tanks should be kept full and the DM water generating units kept in regenerated conditioned. Approximately 600m3 of DM water will be consumed during the entire process. At any time of acid cleaning a minimum of two boiler volumes (approximately 220m3) of DM water should be available in ready stock to facilitate rapid flushing of the system in the event of chemistry upset.

Sheet 2 of 20 STATUS

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PROJECT: SIMHAPURI ENERGY (P) LTD 2 x 150 MW CFBC BOILER

Sheet 3 of 20

Plant area: BOILER PROCEDURE OF CHEMICAL CLEANING OF BOILER USING EDTA 4.2 All the required quantities of chemical as given below should be made available prior to the commencement of the process: Name of Chemicals 1.Tri Sodium Phosphate (Na3PO4.12H2O as per IS573: 1992) 2.Disodium Hydrogen Phosphate (Na2PO4.12H2O as per IS566-1991) 3.Ammoniated EDTA 40% wt/wt as active EDTA Ammoniated solution (pH=9.5 to 9.8) (EDTA: Ethylene diamine tetra acetic acid) Sp gravity: 1.17 1.18 % Of active EDTA (W / V) - 47% to 48% 4.Ammonia solution (20% Min as NH3) Sp gr: 0.91) as per IS 799 / 1990 5.Hydrazine Hydrate (80% Min. conc.) IS 12086 / 1991 6.InhibitorChemicalsCoronilMax & CoronilSol ( Manufacturer by M/s. Arudra Eng (P) Ltd) 4.3 4.4 4.5 4.6 4.7 4.8 Quantity 300 Kgs 150 Kgs

18 tons

3000 liters 1000 liters Each 360 Ltrs

Temporary drum water level gauge glass and (Tell-tale lamp indication) at control room and low point drain area. HT / LT power supply to be available. Instrument / service Air to be available. Chemical Testing laboratory should be available for testing during the process. Flood lights, Telephones / walkie-talkie are available. For effluent treatment compressed air facility and suitable perforated Carbon Steel / polythene tubing arrangement shall be made available.

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PROJECT: SIMHAPURI ENERGY (P) LTD 2 x 150 MW CFBC BOILER

Sheet 4 of 20

Plant area: BOILER PROCEDURE OF CHEMICAL CLEANING OF BOILER USING EDTA 4.9 SAFETY EQUIPMENTS 1. Gum boots (Various sizes) 2. Rubber gloves 3. Rubber or Polythene aprons 4. Helmets 5. Safety goggles plain glass 6. Face mask (Transparent, plastic) 6 Pairs 6 Pairs 6 Nos 12 Nos 6 Nos 4 Nos

7. First aid box (containing dilute ammonium hydroxide, 50% sodium bicarbonate solution, eye lotion, bandages, tincture iodine, cotton, Burnol etc) 5.0 5.1 5.2 SAFETY PRECAUTIONS Flushing and washing water supplies should be available. Ample supplies of tepid flushing and washing water supplies should be provided at all possible points of discharge, spillage or escape of chemicals. Adequate provisions should be made for emergency treatment of the eyes, comprising eye wash bottles, located conveniently to places where discharge, spillage or escape of chemicals can occur. Safety shower should be provided. A suitable first aid treatment room with outside telephone facilities should be provided within a reasonable distance of the place where chemical are being used.

5.3

5.4 5.5

The protective clothing and apparatus required for emergency use should be made available near the acid cleaning area. Signatures 5.6

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PROJECT: SIMHAPURI ENERGY (P) LTD 2 x 150 MW CFBC BOILER Plant area: BOILER PROCEDURE OF CHEMICAL CLEANING OF BOILER USING EDTA 5.7 5.7.1
FIRST AID TREATMENT

Sheet 5 of 20 STATUS

Splashes of the eye

5.7.1.1 Immediately flood the eye with water. To be effective the eyelids must be opened. The eyelids should be pushed apart using the thumb and index finger of the left hand. The casualty will probably not be able to open the eye himself because of painful spasms. 5.7.1.2 If an eye wash bottle is used the jet should not be directed at the front of the eye. It should be directed in from the side so that flow is over the surface of the eye. 5.7.1.3 Irrigation should be continued for 5 - 10 minutes after which the casualty should be taken to the first aid room. 5.7.1.4 Irrigation should be continued in the first aid room. Remember vision is saved by thorough irrigation. No other treatment can prevent damage if this is omitted. 5.7.1.5 After thorough irrigation the eye should be covered with a pad. The patient should be referred for medical opinion. 5.7.2 IRRITATION OF THE SKIN

5.7.2.1 If signs of skin irritation occur the person should be removed from location and referred for medical opinion. In the event of splashing of chemicals on the skin the affected area should be thoroughly washed. 5.8 5.8.1 5.8.2 GENERAL Test area will be cordoned off and unauthorized entry should not be allowed. Suitable signboard should be displayed. Whenever any inspection is done during the cleaning process the location should be adequately ventilated.

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PROJECT: SIMHAPURI ENERGY (P) LTD 2 x 150 MW CFBC BOILER Plant area: BOILER PROCEDURE OF CHEMICAL CLEANING OF BOILER USING EDTA 5.9 5.9.1 SAFETY OF PLANT The Boiler should be suitably preserved after chemical cleaning if the light up for the subsequent activity could not be done within 4 weeks of completion of chemical cleaning. Temperature limitations specified for various steps should not be exceeded.
EMERGENCY PROCEDURES

Sheet 6 of 20

5.9.2 6.0 6.1 6.2 6.3 6.4

The testing team should be aware of the operating procedures of fire extinguishers to be used for quenching minor or major fires. The testing team should be aware of the procedure to be followed in case of accidents involving personnel injury. In case of failure of running pump the stand by pump should be started immediately without delay. An operator posted at the pump area, should be instructed to stop the pumps and properly isolate the system in the event of emergency. All operators should be well conversant with the emergency operating instructions. STATE OF THE PLANT Readiness of the following is to be ensured: During the acid cleaning process all the permanent Boiler instruments are isolated except providing a temporary pressure gauge of 0 to 10 kg/ cm2 in the drum for monitoring pressure in the drum during acid cleaning. Provisions should be made at the following locations for the measurement of temperature: A) Two locations in the drum (left & right) for the measurement of Boiler water temperature. Long thermocouples of around 600 mm length shall be installed directly In the spare / unused stubs In the drum. Alternatively; metal temperature measuring thermo couple with suitable adopter can be used.

7.0 7.1 7.2

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PROJECT: SIMHAPURI ENERGY (P) LTD 2 x 150 MW CFBC BOILER Plant area: BOILER PROCEDURE OF CHEMICAL CLEANING OF BOILER USING EDTA B) Water wall metal temperature measurements as given below: 2 number thermocouples shall be installed at Coal Nozzle elevation on corner water wall tubes (outside the furnace) and 2 numbers thermocouples shall be installed at Screen Superheater entrance elevation in the front and rear water wall (outside the furnace) at accessible locations. C) Two more thermocouples with pads one each at left and right side of ECO coil shall be welded at suitable locations inside the boiler (or penthouse) to measure the metal temperature in the gas side. (Total 4 nos. thermocouples will be used for measurement of water wall tube metal temperature and 2 nos. for economizer tube temperature) Peening type temporary thermocouples are to be provided in the measurement points on the water walls and economizer. Provision should be made for monitoring of temperatures in the control room. Light up of boiler for steam blowing to be done within 4 weeks after EDTA cleaning. To achieve this, erection of MS & other piping has to be planned accordingly. Further delay in light up leads to corrosion in boiler tubes. 7.3 7.1 SAMPLING DURING PROCESS To get representative samples of the process solution, sampling points with sample coolers are to be provided at the following locations: 25mm dia pipe shall be used for sampling line. One number of sampling point is to be provided from bottom ring header as shown in the drawing through temporary cooler. The sampling line from cooler outlet shall be extended to zero meter with an isolation valve. For alkali flushing, rinsing, chemical cleaning and passivation processes, essential control and instruments VIZ. protections, interlock, alarms, measurement, annunciation etc. required for safe light-up of boiler are made available as per O& M instruction at site.

Sheet 7 of 20

7.2

7.3

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PROJECT: SIMHAPURI ENERGY (P) LTD 2 x 150 MW CFBC BOILER Plant area: BOILER PROCEDURE OF CHEMICAL CLEANING OF BOILER USING EDTA 7.4 One set of boiler auxiliaries are made ready and available for boiler light up. A checklist, containing minimum requirements to be made ready prior to commencement of Chemical cleaning is enclosed at 7.15. All Drum internals including Primary separators, screen driers and secondary separators are to be installed in the upper drum. The economizer recirculation valve shall be kept open throughout the chemical cleaning process. Economiser inlet valve shall be kept closed. 0 & M instruction for the Boiler and other auxiliaries are to be available well in advance of the commencement of the cleaning process. All the safety measures discussed and implemented in advance with suitable instruction / caution tags provided at strategic places / equipment. Boiler water wall test tube coupons are placed at two ends inside the drum and bottom ring header to see the effectiveness of the cleaning. It is to be ensured that the test coupons placed in the boiler upper drum are properly kept immersed in the solution. Test coupons shall be kept suspended vertically and tied with stainless steel/thick steel wire to withstand the temperature during the EDTA process. Proper effluent treatment arrangement is to be made available at site. A cemented neutralizing pit of volume 500m3 approx. with compressed air scouring arrangement is to be made. Chemical cleaning system / equipment should be complete as per the approved scheme. Inhibitor efficiency test certificate shall be produced by EDTA supplier.

Sheet 8 of 20

7.5 7.6 7.7 7.8

7.9

7.10

7.11 7.12

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PROJECT: SIMHAPURI ENERGY (P) LTD 2 x 150 MW CFBC BOILER Plant area: BOILER PROCEDURE OF CHEMICAL CLEANING OF BOILER USING EDTA 7.13 MINIMUM OPERATIONAL REQUIREMENTS 1.Ensure the commissioning of the following including their protections, interlocks, measurements, alarms and annunciations: One ID Fan One PA Fan Boiler filling system Measurements, alarms, ammumciations pertaining to secondary air flue gas, feed water, steam & Boiler metal temp. 2. Ensure free expansion of the furnace and duct and provision of expansion markers. 3.Bolw down system of Boiler. 4. Proper drainage system of boiler area 5. Air in leak test of one pass of ESP 6. Mechanical readiness of two passes of ESP 7.Adequate quantity of light oil & readiness of light oil handling system 8.Temporary sampling system along with the cooling arrangement for collecting samples from the header drains during chemical cleaning is ready. 9.Water and steam systems are ready for operation. 10. Air and flue gas system ready for operation. 11. Effluent treatment pit to hold approximately 250m3 is ready 12. Drainage line to effluent treatment is ready. 13. Readiness of BFP and Feed system (optional) 14. Drum water sampling system along with sample cooling arrangement. 15.Availability of emergency supply for a. Emergency lighting Signatures

Sheet 9 of 20

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PROJECT: SIMHAPURI ENERGY (P) LTD 2 x 150 MW CFBC BOILER Plant area: BOILER PROCEDURE OF CHEMICAL CLEANING OF BOILER USING EDTA 16.UPS 17.Fire fighting system of concerned equipments 18.Equipment cooling water system shall be made ready 19.Availability of adequate quantity of DM water. 20.Adequate capacity of instrument air and service air system 21.Availability of HP dozing system 22.Availability of test coupons & their fixing arrangements. 23.Emergency operating instructions VIZ. AC power failure, DC. Power failure, APH fire etc. 24.Adequate lighting in operating areas. 25.Public address system at all operating locations, including telephone & Status 26.walkie-talkies at all working areas 27.Readiness of staircases, hand railings and platforms 28.Personal safety equipment. 29.Easy access and approaches to all the operating equipments. SH metal temperature measurement shall be made ready for continuous monitoring in the control room. 30.Data logging printer at control room shall be made available to record the boiler parameters periodically. 8.0 8.1 8.1.1 METHOD ALKALI FLUSHING Requisite quantities of Tri-sodium Phosphate (TSP) & Di Sodium Hydrogen Phosphate are added to the mixing tank along with DM Water and the solution is thoroughly mixed by recirculation so that final solution in the Boiler contains 0.1 % TSP and 0.05 % DSP. The solution will be injected into the Boiler through the bottom ring header drain and economizer drain operating the chemical filling pump. Further DM water will be taken in the Boiler up to normal level.

Sheet 10 of 20

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PROJECT: SIMHAPURI ENERGY (P) LTD 2 x 150 MW CFBC BOILER

Sheet 11 of 20

Plant area: BOILER PROCEDURE OF CHEMICAL CLEANING OF BOILER USING EDTA 8.1.2 Light up the boiler as per O&M instructions and gradually raise the boiler water temp. to 130-140 deg C. Trip the boiler and keep the fans cooling. 8.1.3 When the boiler water temperature comes down to 95 deg C and drain the boiler in the hot condition to the plant's water disposal system, by keeping open the drain valves fully. (Without throttling). The effluent is diluted with plenty of service water. HOT WATER RINSE Once the draining is complete Boiler is refilled with DM water. Boiler is lit up and the Boiler water temperature is gradually raised to 130-140 Dc. Then the Boiler is tripped and Fans are kept running for cooling Boiler is drained in hot condition to the plant drain system by keeping the drain valves wide open (without any throttling). The effluent is diluted with service water so as to bring pH and P04 in the effluent below 7.5 and 10 ppm respectively. COLD WATER RINSE Cold water rinsing is done using fill and dump method. Draining is done in the plant drain system. pH of the rinsed effluent is monitored during draining. The rinsing operation is continued until pH of the effluent is almost equal to pH of inlet water used for rinsing. All sampling and blow down lines are flushed. All temperature / pressure measurements relevant to the process are monitored in Control Room for their reliability. ACID CLEANING & PASSIVATION Required quantity of ammoniated EDTA (40% wt / wt) solution is kept ready in the EDT A storage tank. The inhibitors, Hydrazine hydrate and ammonia for addition in the Chemical dissolving tank are also made available near the mixing tank. All the Boiler Blow down valves are kept shut and drum vent valves & start up vent are kept open during Boiler filling.

8.2 8.2.1

8.2.2

8.3 8.3.1

8.3.2

8.4 8.4.1 8.4.2 8.4.3

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PROJECT: SIMHAPURI ENERGY (P) LTD Sheet 2 x 150 MW CFBC BOILER 12 of 20 Plant area: BOILER PROCEDURE OF CHEMICAL CLEANING OF BOILER USING EDTA 8.4.4 15 Cu.m of DM water is drawn in the mixing tank. The temporary chemical fill pump IS started and system put into recirculation. Required quantity of Ammoniated EDTA (40% wt / wt) solution is transferred from the EDTA storage tank to the mixing tank. The EDTA concentration in the mixing tank is checked. Transferring of the EDTA solution is stopped when the EDTA concentration reaches 3 1 % by weight. Required quantity of Hydrazine hydrate and inhibitors are also added. Recirculation is done till all the chemicals are uniformly mixed up. With this one batch of EDT A Chemical solution is ready for filling into the Boiler. 8.4.5 The approximate quantities of various chemicals that are to be mixed per batch of 15m3 is: 1.EDTA ammoniated (40 %) concentrate: 3 to 4 2.CORONIL SOL : 20Kgs 3.CORONIL MAX : 20Kgs 4.N2H4.H20 (80%) : 20 liters 8.4.6 8.4.7 Ammonia is added if required to adjust the pH between 9.0 and 9.8. DM water is used to make up to 15m3 This solution is filled into the Boiler through Low Point drain header with the temporary chemical fill pump. Fill the boiler up to +100 mm from the normal working level in the drum. Check the boiler water sample after 30 Mess. The cleaning solution is quite harmless in respect of corrosion and hence there is no time limitation for filling the Boiler and retaining the solution inside the Boiler. Preparation of Chemical solution and batch filling is repeated as explained in point no 8.4.4 till the solution level in the Drum reaches the center line of the gauge glass. The composition of the filling solution is: EDTA content :31%W/v Hydrazine :1000 ppm (min) PH : 9.0 to 9.8

8.4.8

8.4.9

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PROJECT: SIMHAPURI ENERGY (P) LTD Sheet 2 x 150 MW CFBC BOILER 13 of 20 Plant area: BOILER PROCEDURE OF CHEMICAL CLEANING OF BOILER USING EDTA 8.4.10 The Boiler is lighted up as per normal operating procedure with minimum firing rate. 8.4.11 The Drum and super heater vents are closed when steaming starts, say at 1 kg / sq. cm. pressure in the Drum. SH start up vents are kept crack open. 8.4.12 The drain valve in SH Header # 1 is kept in crack-opened condition. 8.4.13 The time at which the temperature of Boiler water reaches 110C is noted. 8.4.14 Raising of Boiler water temperature is continued till temp reaches140 C 8.4.15 Once the temperature of Boiler water reaches 140C, the firing rate is controlled in such a way that the Boiler water temperature is maintained at 140 - 145C, for a minimum period of 4 hours. Then the Boiler is tripped. 8.4.16 The ID Fan & PA Fans are allowed to run to bring down the Boiler water temperature. In case it appears that the results of iron concentration may not level out when temperature is expected to be 110 DC, ID / PA fans are stopped suitably during the cooling down phase & Boiler is boxed up and kept in this condition to achieve the EDTA contact period of 8 hours with temperature exceeding 110 C 8.4.17 Samples are taken at every 30 minutes interval from the sampling points at locations given in article 7.3 from the time when the temperature in the system had reached 110 C and analysed for pH, EDTA concentration and Iron content. 8.4.18 After attaining the completion criteria of pickling process, as per article 9.0, the system is allowed to cool with the ID & PA Fans in operation (ID & PA Fans are to be restarted, in case they have been stopped to meet the completion criteria, to bring down the Boiler water temperature). Open the Drum air vents when the pressure reaches 1 kg/sq.cm.

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PROJECT: SIMHAPURI ENERGY (P) LTD 2 x 150 MW CFBC BOILER Plant area: BOILER PROCEDURE OF CHEMICAL CLEANING OF BOILER USING EDTA 8.4.19 Boiler water temperature & Water Wall metal temperature at the locations indicated as per 7.2 are to be measured and logged. 8.4.20 When the temperature comes down to 950C the running CC pump is stopped and the system is drained completely in hot condition to the effluent pit by opening all the drain valves. 8.5 8.5.1 TREATED DM WATER RINSE Prepare a blended solution of ammonia & Hydrazine with calculated quantities in the dissolving tank in order to achieve a solution pH 9.0 to 9.5 and hydrazine content 50 ppm in the DM water being filled in the boiler. Fill the boiler with the above treated DM water through low point drains and economizer as practiced earlier, up to just above the centre gauge glass. Raise boiler water temperature up to 110 deg .C and then shut down the boiler. Allow the boiler to cool down naturally. When the boiler water temperature comes down to 95 deg C. drain the boiler in hot condition to plant drain and allow the system for natural aeration Boiler Drum manhole is opened for removal of Coupons. Manually clean the drums if required. Lower drums manholes are opened for inspection and cleaned manually, if required. Restore the boiler and prepare it for regular operation for steam blowing, safety valve floating etc.

Sheet 14 of 20

8.5.2

8.5.3

8.5.4 8.5.5 8.5.6

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PROJECT: SIMHAPURI ENERGY (P) LTD 2 x 150 MW CFBC BOILER Plant area: BOILER PROCEDURE OF CHEMICAL CLEANING OF BOILER USING EDTA 8.6 8.6.1 INSPECTION The test coupons placed at identified locations are taken out. All coupons should be free of deposits and should have uniform coating of the protective layer. The Drum internal surface is visually inspected for uniform smooth coating of protective layer. The ring headers will be inspected and loose debris if any, will be removed. COMPLETION CRITERIA COLD RINSE AFTER ALKALI FLUSHING The rinsing operation is continued until pH of the effluent is almost equal to pH of inlet water used for rinsing. EDT A CLEANING Cleaning process is to be continued till iron concentrations in three consecutive samples show equilibrium status. When the iron concentration in the cleaning solution is constant it indicates that all the oxides have been dissolved. However, a minimum EDT A contact period of 6 hours from the time of attaining the required temperature (110C) shall be allowed. If the iron concentration values do not level out and attain equilibrium status, regardless of analytical results, the EDTA contact period with temperature exceeding 1100C shall not be allowed for more than 8 hours (approx).

Sheet 15 of 20

8.6.2

9.0 9.1 9.1.1 9.2 9.2.1 9.2.2

9.2.3

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PROJECT: SIMHAPURI ENERGY (P) LTD 2 x 150 MW CFBC BOILER Plant area: BOILER PROCEDURE OF CHEMICAL CLEANING OF BOILER USING EDTA 10.0 10.1 WASTE TREATMENT & DISPOSAL Treatment and disposal of the waste and effluents of the chemical cleaning process should comply with the requirements / stipulations of State Pollution Control Board norms. Effluent of Hot DM water flushing should be drained into plant normal drain The spent EDTA chemical solution after the cleaning process is drained into the designated pit. The pH of the effluent will be in the range of 8.5 to 9.0 and hence no treatment for pH adjustment is required as it would meet the pH requirement for disposal. Compressed air is used to destroy the residual Hydrazine & organics and the effluent may be disposed after aeration for 10 days, as per state pollution control board norms. Effluent may be disposed to ash dyke in installments through existing ash slurry system (The organic chemical is completely bio- degradable). APPENDIX NOTE Drains should be provided at lowest points of temporary piping. All temporary connections to Boiler should be of good quality. They will be hydraulically tested at 14 kg/cm2 with the temporary boiler filling pump Service water supply should be available near the pump operating areas. Additional Checklists / Modifications in the layout, if found necessary, may be made at site in consultation with site Commissioning In-charge. All the sampling points along with sample coolers and the temperature measurement points with necessary thermocouples shall be provided as indicated in 7.3 & 7.2 respectively.

Sheet 16 of 20

10.2 10.3

10.4

11.0 11.1 11.2 11.3

11.4 11.5 11.6

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PROJECT: SIMHAPURI ENERGY (P) LTD 2 x 150 MW CFBC BOILER Plant area: BOILER PROCEDURE OF CHEMICAL CLEANING OF BOILER USING EDTA LOG SHEET PROJECT UNIT NO. ACTIVITY: I. Sl. No. EDTA ACID CLEANING AND PASSIVATION ADDITION OF CHEMICALS DATE TIME NAME OF CHEMICAL ADDED QUANTITY DATE: / /

Sheet 17 of 20

II.

ANALYTICAL DATA DATE TIME hrs. SAMPLE POINT TOTALEDTA % IRON ppm pH

SL.No
l. 2. 3. 4.

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PROJECT: SIMHAPURI ENERGY (P) LTD 2 x 150 MW CFBC BOILER

Sheet 18 of 20

Plant area: BOILER PROCEDURE OF CHEMICAL CLEANING OF BOILER USING EDTA PROCEDURE FOR DETERMINATION OF TOTAL EDTA CONCENTRATION IN PROCESS SOLUTION DURING CHEMICAL CLEANING 1. PRINCIPLE EDT A reacts with Zirconium ions under strong acid conditions to form a chelate. The end point of the titration is indicated by a Xylenol orange indicator. 2. REAGENTS AND APPARATUS REQUIRED APPARATUS 1. Erlenmeyer flask 300 ml capacity 2. Pipettes 3. Hot plate 4. Magnetic stirrer REAGENTS 1. Hydrochloric acid (conc.) 2. Standard Zirconium oxy chloride (ZrOCI2. 8H20) 0.1 M solution in 1 N HCI (Take a 1000 ml volumetric flask and add 32.25 gram of ZrOCI2.8 H20 and add DM water to about 500 ml. To this add 85 ml of conc. HCL. Make up to 1000 ml mark with DM water and mix well) 3. Ascorbic acid 4. Xylenol orange indicator 3. TEST PROCEDURE 1. Pipette out 10 cc of the water sample into a 300 ml Erlenmeyer Flask. 2. Add 10 ml of cone. HCI (the pH value is about 1.0) 3. Add a spatula of ascorbic acid.

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PROJECT: SIMHAPURI ENERGY (P) LTD 2 x 150 MW CFBC BOILER Plant area: BOILER PROCEDURE OF CHEMICAL CLEANING OF BOILER USING EDTA 4.

Sheet 19 of 20

Boil of the solvent on the heating plate for about 5 minutes. (The yellow colour of the ferric ion should disappear due to reduction to ferrous iron.

5. Immediately after the addition of 0.05 ml of 0.05 % Xylenol orange indicator the sample titrated with 0.1M ZrOCl2 until the colour changes from yellow to red violet, The colour changes from yellow to red violet. The colour change shall remain constant for at least 3 min. 4. CALCULATION The total EDTA concentration % = Volume ofO.1M ZrOCl2 consumed x 0.292 PROCEDURE FOR THE DETERMINATION OF IRON CONCENTRATION IN WATER SAMPLES DURING CHEMICAL CLEANING. 1. APPARATUS REQUIRED 1. Spectrophotometer. 2. Hot plate 3. Volumetric flasks 4. Pipettes 2. REAGENTS REQUIRED 1. Thioglycolic acid (pure Grade) 2. Ammonia solution (25%) AR Grade 3.TEST METHOD 1. Pipette out 25 ml of the water sample into a 50 ml capacity volumetric flask. 2. Add 2 ml of Thioglycolic acid using pro-pipette. Mix well 3. Heat it to 70 - 80 deg C for about 10 minutes. 4. Cool it to room temperature and make it up with DM water to the 50 ml mark and mix well. 5. Measure the extinction of the sample against a blank using DM water treated as the sample at 532.5 nm using Spectrophotometer. Signatures

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PROJECT: SIMHAPURI ENERGY (P) LTD 2 x 150 MW CFBC BOILER Plant area: BOILER PROCEDURE OF CHEMICAL CLEANING OF BOILER USING EDTA

Sheet 20 of 20

6. Plot a curve taking standard iron solution and measuring the extinction in the same way as that of the water sample. 7. Read the iron concentration of the sample from the calibration graph plotted. Alternatively, Pre-calibrated spectrophotometer (HACH USA / Lovibond ) with appropriate reagent for iron can be used ESTIMATION OF HYDRAZINE 1. REAGENTS Standard Potassium bromate 0.1 N Dissolve 2.7836 gram of Potassium bromate (Kbr03) and 10 gram of Potassium bromide (KBr) in DM / Distilled water and make up to 1000 ml 0.1% Methyl orange indicator solution. Hydrochloric acid (conc.) AR.

2. PROCEDURE Place 10 ml of sample in a titration flask. Add 10 ml of conc. HCI. Add about 5 drops of Methyl orang indicator. Titrate with standard Kbr03 titrant to the first appearance of yellow colour.

3. CALCULATION Hydrazine as N2H4 in ppm = liter value x 80

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