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SSTPS, SINGRAULI.
Post operational chemical cleaning of boiler U#3 started on 16th of April, 2008.
This was actually scheduled to be started on 7th of April. The delay was due to
failure of acid inhibitor Rhodine A 213;Henkel ;Mumbai under laboratory
conditions. Which lead to fresh purchase of Coronil 213 special from Arudra
Engineering (Pvt.) Ltd., Chennai. New acid inhibitor was received on the site on
15th of April.
Before the decision of acid cleaning for boiler U#3 was taken, deposit analysis
was carried out in detail at NTPC R & D Center. Findings of R&D and method
of acid cleaning for boiler U#3 was given as follows:-
Introduction:
Internal deposit quantity of water wall tubes of boiler #3 was carried out in R &
D lab. It shows that the presence of 51-64 gm/cm2 on the hot surfaces and 37-47
mg/cm2 on the cold side of surfaces. Platen water wall tubes contain the internal
deposit quantity 161 mg/cm2 at lower side and 48 gm/cm2 at upper side of the
tube Internal deposit analysis consist of Copper 4.5-5.3%, Calcium 2.1-7.7%
and Silica 0.7-0.9% along with Iron oxide. On the basis of internal quantity and
analysis, single stage post operational chemical cleaning is recommended. The
experiments were conducted in laboratory to finalize the chemical cleaning
process. The procedure for chemical cleaning includes the following steps.
1. Alkali Boilout
2. Acid Pickling
3. Neutralization
4. Passivation
1. Alkali Boilout:
Back flush the super heater with DM water and backfill with treated water
containing 200 ppm hydrazine and ammonia to raise the pH > 10. Plug the super
heater connecting tubes inside the drum. Raise the pressure to 4-5 Kg/cm2 and
isolate super heater.
Suspend the water wall tube sample coupons inside the drum at both the end to
ascertain efficiency of cleaning and passivation before cutting of actual tube
from boiler.
Fill the system with DM water and establish circulation by pumps. Circulate for
about ½ an hour and drain.
Fill the system with DM water and establish circulation by pumps. Raise the
temperature of water to 55-600 C by passing the steam in circulating tank and
drain after circulation of half an hour.
5. Acid Pickling:
6. DM Water Rinse:
Fill the boiler system with DM water and establish circulation with circulation
pumps. Raise the temperature of circulating water up to 50-60 0 C by injecting
steam and circulate for 30 minutes. Drain the system under N2 capping.
Fill the boiler system with DM water and establish circulation. Raise the
temperature of circulating water up to 50-55 0 C and add 0.2% (w/v) citric acid.
Add liquor ammonia to raise the pH of circulating water to 3.5- 4.0. Circulate for
2 hours. Measure the pH and iron content in the solution at an interval of ½ an
hour. Drain the system under N2 capping.
Fill the boiler system with DM water and establish circulation. Raise the
temperature of circulating water up to 50-550 C and circulate ½ an hour. Measure
the iron content in the inlet and return line. Drain the system under N2 capping.
Restore the boiler after chemical cleaning by putting drum internal and all the
permanent connection. Prepare the boiler for regular operation as per the
guidelines of O&M. Fill the boiler with DM water containing 200 ppm of
hydrazine and ammonia to raise pH 10.0. Light up the boiler and raise the
pressure to 40 Kg/cm2 and maintain the pressure for 24 hours. During the
process, inject hydrazine in the feed water to maintain hydrazine concentration
25 ppm. After completion of II stage passivation, the boiler can be taken for
regular operation.
The effluent generated after each stage of acid pickling will be treated with
caustic soda flakes or caustic lye to a pH level from 5.5- 8.0 before discharging
from plant. The effluent after first stage passivation will be treated with
bleaching powder.
14. Effluent neutralization pit:
A neutralization pit should be made available near the site with the holding
capacity of around 400 M3. The pit should have non-corrosive lining, circulating
and discharging pumps capacity.
Drum manhole should be opened and visually inspected the drum internal
surface and water wall coupons placed in the drum for smooth uniform formation
of magnetite coating and effectiveness of cleaning. Arrangement should be made
to cut the water wall tube samples from high heat affected area after chemical
cleaning to calculate quantity of deposit on the internal surface, if any.
Check list:-
A check list was prepared with certain check points so as to ensure and assign
various responsibilities to concerned departments.
REAGENTS -
A.Sodium hydroxide solution , Standard 1.0 N
B.Mixed Indicator
PROCEDURE-
a. 10 ml of sample
CALCULATION –
% HCl = V x 0.36
Where V = Milliliters of 1.0 N NaOH used to obtain end point.
ESTIMATION OF HYDRAZINE:- (Method no. 1)
REAGENTS-
A. Standard 0.1 N Potassium Bromate
(Dissolve 2.7836 g of KBrO3 and 10 g of KBr in DM water and
make up to 1 Litre)
B. 0.1% Methyl Red indicator solution.
C. Conc. HCl Sp. Gr. 1.18
PROCEDURE-
a. 10 ml of sample.
b. Add 10 ml conc. HCl
c. 5-6 drops of methyl red indicator solution.
d. Titrate with standard 0.1N KBrO3 solution.
e. End point yellow colour.
CALCULATION-
REAGENTS-
CALCULATION-
Hydrazine as N2H4 (ppm) = (X-Y) x 80
REAGENTS-
a. Sodium bicarbonate
b. 0.1 N Iodine Solution
c. Starch Indicator
PROCEDURE-
a. 10 ml sample+ 25 ml DM water
b. Add a pinch of NaHCO3 + starch Indicator
c. Titrate against 0.1 N Iodine Solution.
d. End point gives blue colouration.
REAGENTS-
PROCEDURE-
a. 50 ml sample
b. 4-5 drops of mixed indicator
c. Titrate with 0.1 NaOH
d. End point colour changes from red through gray to blue green
(Record the volume A)
e. Take another sample
f. Add 4 drops of phenolphthalein indicator.
g. Titrate again with 0.1 N NaOH
h. End point colour changes to pink colour(Record the volume B)
CALCULATION-
ESTIMATION OF ALKALINITY:-
REAGENTS-
1. 0.1 M HCl acid (Standard): Dissolve 3.647 g (or 9 ml)of HCl in 1 litre
and standardize with standard Na2CO3 Solution.
2. Mixed Indicator :
a. Prepare 0.1% Bromocresol green in alchohol
b. Prepare 0.2% Methyl Red in alchohol
Mix 75 c.c. of former with 25 c.c. of later.
PROCEDURE-
A. 10.0 ml sample
B. 2-3 drops mixed indicator
C. Titrate against 0.1N HCl
D. End point colour is slight red.
CALCULATION-
REAGENTS-
A. Sodium Acetate
B. Chloroacetic Acid
C. Sulphosalicylic Acid
D. Potassium per sulphate (K2S2O8)
E. 0.01M Standard EDTA solution
PROCEDURE-
a. 10.0 ml sample
b. 1 g Sodium acetate + 1 g Chloroacetic acid + Sulphosalicylic Acid
c. Titrate against 0.01 M EDTA
d. End point pink to pale yellow. (Record volume as A)
e. To the same solution add 1 g potassium per sulphate
f. Titrate against 0.01 M EDTA already in the burette.
g. End point is pink to yellow. (Record the volume as B)
CALCULATION-
REAGENTS-
REAGENTS-
PROCEDURE-
CALCULATION-
REAGENTS-
PROCEDURE-
CALCULATION-
Day 1: 14/04/2008
Day 2: 15-04-08
Day 3: 16-04-08
o Third acid tanker could not reach before 16.30 hrs leading to late
start.
o Drain (equal to three volumes of mixing tank) started at 15:15 hrs
o Chemical addition
started at 17.00 hrs
30 liter HCl + 420 liters Coronil 213 special added at 17:00 hrs
500 Kg Ammonium bifluoride added at 17:30 hrs
2000 Kg Thiourea added at 17:45 hrs
completed at 18:20 hrs
Unloading of acid tanker
First:
• Started on 18:30 hrs
• Completed on 19:30 hrs
• Qty: 14.5 MT
Second:
• Started at 19:45 hrs
• Completed on 21:00 hrs
• Qty: 14.7 MT
Third:
• Started at 21:35 hrs
• Completed at 22:00 hrs
• Qty: 3.0MT
• Day 4:17-04-08
DM Water Rinse :-
Time Temp pH
I/L O/L I/L O/L
01:20 Draining completed and system filling started with DM water
04:40 System filling completed and kept under recirculation
05:00 55.7 46.6 1.9 1.7
06:00 59.7 49.1 1.94 1.91
06:50 DM Water draining started followed by N2 capping
08:45 Draining completed
Passivation Stage-I :-
Time Chemical Temp. pH Hydrazine Conc.
Addition (ppm)
(In Liters)
Ammo Hyd I/L O/L I/L O/L I/L O/L
17:00 350 200 - - - - - -
18:00 - - 74 50 9.5 9.5 584 880
18:30 105 - - - - - - -
19:00 - - 84 62 9.3 9.4 376 456
19:35 155 - - - - - - -
20:00 - - 85 67 10.06 10.0 360 384
21:00 - - 90 72 10.2 10.2 392 400
22:00 - - 85 75 10.2 10.18 360 368
23:00 - - 90 78 10.18 10.16 352 352
00:00 - - 91 79 10.18 10.17 352 352
(19/05/08)
01:00 90 80 10.16 10.15 336 328
02:00 - - 92 82 10.17 10.17 336 336
03:00 - - 93 83 10.17 10.17 328 328
04:00 - - 93 83 10.18 10.18 320 320
05:00 - - 94 83 10.18 10.18 320 320
06:00 70 10 94 81 10.28 10.28 320 320
07:00 - - 93 83 10.30 10.29 352 360
08:00 - - 94 83 10.20 10.10 336 352
09:00 50 - 85 81 10.20 10.10 320 336
10:00 - - 89 82 10.22 10.16 304 320
11:00 70 20 - - - - - -
11:05 - - 89 81 10.25 10.18 560 336
12:00 - - 90 81 10.24 10.27 468 440
13:10 - - 84 77 10.10 10.12 304 344
13:30 - - 91 80 - - - -
14:00 - - 89 80 10.06 10.14 320 336
14:45 70 10 - - - - - -
15:10 - - 91 79 10.03 10.02 344 336
16:00 - - 89 79 10.03 10.06 320 320
16:05 105 - - - - - - -
17:00 - - 87 78 10.0 9.98 328 344
17:40 - - 88 78 9.9 9.8 336 340
17:40 Recirculation stopped (Stage-I passivation completed)
17:45 Drain started
18:45 Drain of water circuit completed
19:30 SH drain started
Total chemical consumption in citric acid rinse :-
• Ammonia = 975 Liters
• Hydrazine = 240 Liters
Day 7: 29-04-08
Passivation Stage-II:
1 SH Filling 105 93 - - - - - -
Acid
2 Cleaning - - 32 420 2000 500 -
4 Neutralization - - - - - - - 2000