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TECHNICALDOCUMENT ON

CHEMICALANALYSISDURINGCHEMICALCLEANINGOF BOILERUSINGEDTA

DocumentNo.:PWR/TSX/BLR/02/269/00/12

BHARATHEAVYELECTRICALSLIMITED
POWERSECTORTECHNICALSERVICES KribhcoBhawan,A810,Sector1, Noida201301.

TECHNICALDOCUMENTONCHEMICALANALYSISDURING CHEMICALCLEANINGOFBOILERUSINGEDTA

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PROCEDUREFORCHEMICALANALYSISDURING CHEMICALCLEANINGOFBOILERUSINGEDTA

Introduction
BHEL has adopted procedure of Ammoniated EDTA with initial concentration of 4 1% for Chemical Cleaning of Boiler. The chemical cleaning process and chemical formulations used for each step is, as outlined below: S. No. 1 1.1 Step Preliminary Cleaning Step Alkali Flushing Tri Sodium Phospahte (1000 ppm) Di Sodium Phospahte (500 ppm) 1.2 1.3 Hot Water Flushing Nil Achieving drum water temperature of 140C Achieving drum water temperature of 140C Phosphate < 10 ppm and pH 7.0 2 2.1 Acid Pickling Step EDTA Pickling Ammoniated EDTA (4 1%) Hydrazine (1000 ppm) BHELmax (0.15% w/w) BHELsol (0.15% w/v) Ammonia (to maintain pH: 9.2 9.8) 2.2 Treated DM Water Rinsing Hydrazine (200 ppm) Ammonia (to maintain pH: 9.2 9.8) Iron Conc. stabilizes in three concurrent values or EDTA contact time of 8 hrs. at temperature above 110C None Chemical Formulation Completion Criteria

Cold Water Flushing Nil

The quality and quantity of chemicals required for Chemical Cleaning of Boiler using EDTA is as per Appendix I.

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Chemical Analysis
Chemical analysis is carried out to monitor and control the chemical parameters of the chemical cleaning process for ensuring safe and efficient chemical cleaning of boiler. Following chemical parameters are monitored during the process: Phosphate Concentration pH Total EDTA Concentration Hydrazine Concentration Iron Concentration

The chemical analysis to be carried out during various steps of Chemical Cleaning of Boiler using EDTA is listed as below: Chemical Cleaning Step 1. Cold Water Rinsing Chemical Analysis to be carried out a) Phosphate Concentration b) pH a) Total EDTA Concentration b) Hydrazine Concentration c) pH a) Total EDTA Concentration b) Iron Concentration c) pH a) Hydrazine Concentration b) pH

2. EDTA solution batches for Boiler filling

3. EDTA Pickling step

4. Boiler filling for Treated DM Water Rinsing

The quality and quantity of chemicals required for chemical analysis during Chemical Cleaning of Boiler using EDTA is as per Appendix II. The list of lab wares and other materials required for chemical analysis during Chemical Cleaning of Boiler using EDTA is as per Appendix III.

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PROCEDUREFORCHEMICALANALYSISDURING CHEMICALCLEANINGOFBOILERUSINGEDTA

Chemical Analysis Procedures 1. Determination of Phosphate Concentration


(Using Spectrophotometer) 1.1. Significance: It can be measured to estimate phosphate concentration in the system during Alkali Flushing, Hot Water Rinsing and Cold Water Rinsing. Its measurement is significant during Cold Water Rinsing for declaring its completion i.e. PO43- < 10 ppm. 1.2. Principle: Spectrophotometer works on the principle of absorption of light by elements/ ions present in a solution when it passes through the solution. Each element/ ion absorbs a specific wavelength of light which is characteristic to it. Thus when a light beam passes through a solution, element/ ion present in the solution absorbs its particular wavelength of light and thus intensity of that particular wavelength of light decreases after passing through the solution. The change in intensity indicates the amount of the particular element present in the solution. 1.3. Apparatus and Reagents Required: 1.3.1. Apparatus: a. Spectrophotometer Instrument with its kit; preferably HACH DR890 b. Pipette c. Volumetric Flask 1.4. Procedure: 1.4.1. 1.4.2. 1.4.3. Take the sample and dilute it 10 times. The dilution factor has to be chosen to get the value in the range of 0.5 2.9 ppm. Take Spectrophotometers sample bottle and fill it with DM Water up to the 20 ml mark. Place it in Spectrophotometer and put its cap.

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Switch on the Spectrophotometer and choose Function for determination of Phosphate concentration (in case of other spectrophotometer than HACH DR 890; kindly refer the procedure provided by the instrument manufacturer). Press 0 (or test button) for tare setting. Take out the sample bottle and dont switch off the Spectrophotometer. Now take the diluted sample in the sample bottle up to the 20 ml mark. Place it in the Spectrophotometer and put its cap. Now press the test button and allow it for 3 minutes of testing time.

1.4.4.

1.4.5. 1.4.6. 1.4.7. 1.4.8. 1.4.9.

1.4.10. After that, Phosphate concentration of the diluted sample will be displayed in the Spectrophotometer display. 1.4.11. If the value is in the range of 0.5 2.9 ppm, then it should be multiplied with the dilution factor and we will get the Phosphate concentration for the sample. 1.4.12. If the value is either less than 0.5 ppm or more than 2.9 ppm then the dilution factor of the sample has to be changed and testing to be repeated. 1.5. Calculation: Phosphate Concentration, ppm = Spectrophotometer Reading X Dilution Factor

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2. Determination of Total EDTA Concentration


2.1. Significance: It signifies the total active EDTA available in the solution. It includes free EDTA as well as EDTA that has reacted with iron present in the system. It is checked during batch making to ensure initial EDTA concentration and during the pickling step to ensure sufficient active EDTA is available in the solution. 2.2. Principle: EDTA reacts with Zirconium ions under strong acidic conditions to form a chelate. Thus, total EDTA concentration is determined by complexometric titration of EDTA solution with Zirconium Oxy-chloride solution and Xylenol Orange solution as an indicator for indicating the end point of this titration. 2.3. Titrant & Indicator: a. Titrant : b. Indicator: 0.1 M Standard Zirconium Oxy-chloride solution in 1 N HCl 0.05% Xylenol Orange solution

2.4. Apparatus and Reagents Required: 2.4.1. Apparatus: a. Erlenmeyer flask (250 ml capacity) b. Pipette c. Hot plate d. Test tube e. Spatula f. Burette g. Filter paper 2.4.2. Reagents: a. Hydrochloric acid (conc.) b. Ascorbic acid c. 0.1 M Standard Zirconium Oxy-chloride solution in 1 N HCl d. 0.05% Xylenol Orange solution

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2.5. Titration Procedure: 2.5.1. 2.5.2. 2.5.3. 2.5.4. 2.5.5. 2.5.6. 2.5.7. Take about 100 ml of DM water into a 250 ml Erlenmeyer flask. Pipette 5 ml of the sample to the flask. Add 5 ml (or half test tube) of conc. HCl (1:1) to the flask. Add a spatula of ascorbic acid to the flask. Boil off the solvent on the heating plate for about 5 minutes (yellow colour of the ferric ion should disappear due to reduction to ferrous iron). Allow the solution to cool. Add 5 to 6 drops of 0.05% Xylenol Orange indicator to the flask and immediately titrate it with 0.1M ZrOCl2 until the colour changes from yellow to red violet (colour change shall persist for at least 3 min).

2.6. Calculation : EDTA (w/v), % = Titre Value X 0.584

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3. Determination of Iron concentration


(Using Spectrophotometer) 3.1. Significance: It signifies the iron picked up by the EDTA solution. It is important to monitor iron concentration as it tells the completion of the process as well as indicates the healthiness of the process. If iron concentration increases very rapidly and is continuing to increase rapidly, then it indicates failure of inhibitors and EDTA solution should be drained immediately to save the boiler. 3.2. Principle: Spectrophotometer works on the principle of absorption of light by elements/ ions present in a solution when it passes through the solution. Each element absorbs a specific wavelength of light which is characteristic to it. Thus when a light beam passes through a solution, element present in the solution absorbs its particular wavelength of light and thus intensity of that particular wavelength of light decreases after passing through the solution. The change in intensity indicates the amount of the particular element present in the solution. 3.3. Apparatus and Reagents Required: 3.3.1. Apparatus: a. Spectrophotometer Instrument with its kit; preferably HACH DR890 b. Pipette c. Volumetric Flask 3.3.2. Reagents: a. Ferrover reagent 3.4. Procedure: 3.4.1. 3.4.2. 3.4.3.

Take the sample and dilute it 1000 times. The dilution factor has to be chosen to get the value in the range of 0.5 2.9. Take Spectrophotometers sample bottle and fill it with DM Water up to the 20 ml mark. Place it in Spectrophotometer and put its cap.

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Switch on the Spectrophotometer and choose Function for determination of Iron concentration (in case of other spectrophotometer other than HACH DR 890; kindly refer the procedure provided by the instrument manufacturer). Press 0 (test button) for tare setting. Take out the sample bottle and dont switch off the Spectrophotometer. Now take the diluted sample in the sample bottle up to the 20 ml mark. To it add a pouch of Ferrover reagent and shake well to mix it. A brown color in the sample should be observed. Place it in the Spectrophotometer and put its cap.

3.4.4.

3.4.5. 3.4.6. 3.4.7. 3.4.8. 3.4.9.

3.4.10. Now press the test button and allow it for 3 minutes of testing time. 3.4.11. After that, Iron concentration of the diluted sample will be displayed in the Spectrophotometer display. 3.4.12. If the value is in the range of 0.5 2.9, then it should be multiplied with the dilution factor and we will get the Iron concentration for the sample. 3.4.13. If the value is either less than 0.5 or more than 2.9 then the dilution factor of the sample has to be changed and testing to be repeated. 3.5. Calculation: Iron Concentration, ppm = Spectrophotometer Reading X Dilution Factor

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4. Determination of Hydrazine concentration


4.1. Significance: Hydrazine concentration is measured during EDTA batch making and Treated DM Water Rinse filling to maintain the required level of hydrazine in the system. 4.2. Titrant & Indicator: a. Titrant : b. Indicator: 0.1 N Standard Potassium Bromate solution 0.1% Methyl Orange solution

4.3. Apparatus and Reagents Required: 4.3.1. Apparatus: a. Erlenmeyer flask (250 ml capacity) b. Pipette c. Test tube d. Burette e. Filter paper 4.3.2. Reagents: a. Hydrochloric acid (conc.) b. 0.1 N Standard Potassium Bromate solution c. 0.1 % Methyl Orange solution 4.4. Procedure: 4.4.1. 4.4.2. 4.4.3. Pipette 10 ml of the sample into a 250 ml Erlenmeyer flask. Add 5 ml (or half test tube) of conc. HCl (1:1) to the flask. Add 5 to 6 drops of 0.1% Methyl Orange indicator to the flask and immediately titrate it with 0.1N KBrO3 until the colour changes from pink to yellow.

4.5. Calculation: Hydrazine as N2H4, ppm = Titre value X 80

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5. Determination of pH
5.1. Significance It indicates the pH or acidity/ basicity of the system as chemical cleaning is to be carried out in basic medium with pH around 9.2 9.8. It is measured to verify and maintain the required basicity in the system. pH is one of the completion criteria for Cold Water Rinsing step. 5.2. Apparatus and Reagents Required: 5.2.1. Apparatus: a. pH meter b. Beaker (50 ml) 5.2.2. Reagents: a. Buffer solutions 5.3. Procedure: 5.3.1. 5.3.2. 5.3.3. 5.3.4. 5.3.5. Take sample in beaker up to around half level of the beaker. Take out the pH meter probe from the buffer solution and wash it with DM water. Dip the pH meter probe into the sample solution. Note the reading for pH. Take out the pH meter probe from the sample solution and wash it with DM water and then put it back into the buffer solution.

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Appendix I List of Chemicals required for Chemical Cleaning of Boiler using EDTA

S.No. Chemicals& ChemicalFormulae


1. Na3(PO4).12H2O 2. Disodium Phosphate (DSP) Na2H(PO4).7H2O 3. Ammoniated EDTA C6H12N2O8(NH4)4 4. Ammonia NH3 5. Hydrazine N2H4.H2O 6. 7. BHELmax BHELsol

Standard

500MW 250MW 210MW 125MW


400 kg. 250 kg. 250 kg. 125 kg.

Trisodium Phosphate (TSP) IS 566 1991

IS 573 1992

200 kg.

125 kg.

125 kg.

65 kg.

----

42 M.T.

22 M.T.

21 M.T.

18 M.T.

IS 799 1990 1500 ltrs. 1000 ltrs. 1000 ltrs. 600 ltrs.

IS 12086 1992 1500 ltrs. 1000 ltrs. 1000 ltrs. 600 ltrs.

-------

700 kg.

350 kg.

350 kg. 350 ltrs.

250 kg. 250 ltrs.

700 ltrs. 350 ltrs.

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Appendix II List of Chemicals/ Reagents required for chemical analysis purpose S. No. 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. Chemicals/ Reagents Ascorbic Acid Conc. HCl Buffer Solutions for pH meter Ferrover Reagent Zirconium Oxy-chloride Xylenol Orange Hydroxylamine Hydrochloride Potassium Bromate Potassium Bromide Methyl Orange Grade AR AR --AR AR AR AR AR AR Quantity 100 g 500 ml 100 ml 60 pouches 100 g 25 g 50 g 50 g 50 g 100 g

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Appendix III List of Lab wares required for chemical analysis purpose S. No. 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19.

Apparatus Spectrophotometer; preferably HACH DR 890 pH meter Electronic Mass Balance Erlenmeyer flask Pipettes, graduated Pipettes, graduated Pipettes, graduated Burette Beaker Volumetric flask Volumetric flask Volumetric flask Measuring Cylinder Measuring Cylinder Measuring Cylinder Wash bottles DM water carboys Plastic buckets Plastic bottles (for DM Water)

Capacity ---250 ml 10 ml 5 ml 1 ml 50 ml 100 ml 1000 ml 500 ml 100 ml 50 ml 25 ml 10 ml 500 ml 5L 20 L 500 ml/ 1000 ml

Quantity 1 1 1 6 2 2 2 3 3 2 2 4 2 1 1 3 3 2 6

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S. No. 20. 21. 22. 23. 24. 25. 26.

Apparatus Sample Bottles Funnel Burette stand Hot plate Spatula Filter paper (qualitative) Electrical extension box

Capacity 500 ml -----5 A sockets

Quantity 6 2 2 1 2 1 box 3 points

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DISTRIBUTION LIST
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