ML20080P446
| ML20080P446 | |
| Person / Time | |
|---|---|
| Site: | Catawba  |
| Issue date: | 05/12/1983 |
| From: | Dickey C, Evans L, Tuckman M DUKE POWER CO. |
| To: | |
| Shared Package | |
| ML20080P419 | List:
|
| References | |
| CP-O-B-8150-03, CP-O-B-8150-3, NUDOCS 8402220547 | |
| Download: ML20080P446 (17) | |
Text
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Form 34731 (10-81)
(Formerly SPD 10021?
DURE POWLt COMPANY (1) ID No: CP/0/B/8150/03 PROCEDURE PREPARATION Change (s) O to PROCESS RECORD o Incorporated (2) STATION: Catawba (3) PROCEDURE TITLE: Chemistrv Procedure for the Detemi. nation of Sodium.
Auto Analyzer (4) PREPARED BY: /$zn'flun _ hi _Af t& DATE: 5- 6 -fG (5) REVIEWED BY: /h X- kN DATE: F (- 73 Cross-Disciplinary Review By: 61 (6) TEMPORARY APPROVAL (IF NECESSARY):
By: (SRO) Date:
By: - i Date:
(7) APPROVED BY: -
Date: 6h 83 (8) MISCELLANEOUS:
Reviewed / Approved By: Date:
Reviewed / Approved By: Date:
l MASTER FILE l
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, Form 34634 (4-81) SPD 10012 DUKE POWER COMPANY NUCLEAR SAFETY EVALUATION CHECK LIST (1) STATION: Catawba UNIT: 1X 2 X 3 OTHER:
(2) CHECK LIST APPLICABLE TO: CP/0/B/8130/03 (3) SAFETY EVALUATION - PART A The item to which this evalum: ion is applicable represents:
Yes No / A change to the station or procedures as described in the FSI or a test or experiment not described in the FSAR7 If the answer to the above is "Yes", attach a detailed description of the iter being evaluated and an identification of the affected section(s) of the FSAR.
(4) SAFETY EVALUATION - PART B 1
Yes No / Will this item require a change to the station Technical Specifications?
If the answer to the above is "Yes," identify the specification (s) affected and/or attach the applicable pages(s) with the change (s) indicated.
(5) SAFETY EVALUATION - PART C As a result of the item to which this evahation is applicable:
Yes No / Will the probability of en accident previously evaluated in the FSAR be increased?
Yes No / Will the consequences of an accident previously evaluated
.in the FSAR be fneressed?
Yes No / May the possibility of av accident which is different
. than any already evaluated in the FSAR be created?
l Yes No / ,Will the probability of a malfunction of equipment l
important to safety previously evaluated in the FSAR be increased?
l Yes No / Will the consequences of a malfunction of equipment l important to safety previously evaluated in the FSAR l
be increased?
Yes No May the possibility of malfunction of equipment important-to safety different than any already evaluated l in'the FSAR be created?
Yes No / Will the margin of safety as defined in the bases to any l
Technical Specificatio'n be reduced?
l If the answer to any of the preceding is "Yes", an unraviewed safety l questio. is involved. Justify the conclusion that an unreviewed safety question is or is not involved. Attach additional pages as necessary.
(6) PREPARED BY: O#4ha.Omkw DATE: 5- G - 53 (7) REVIEWED BY: b DATE: T' ( - U (8) Page 1 of /
i i
_ _ - - . - ~ . , . . _ _ _ .
Form 18855 (3-80)
DUKE POWER COMPAhi ALARA EVALUATION CHECKLIST (1) Station Catawba- Unit: 1 x 2 x 3
~
Other:
(2) Checklist Applicable to: CP/0/B/8150/03 (3) ALARA Evaluation Check those items below which were considered applicable during the preparatien and review of this document.
Flushing and draining were used to minimize source - strength and con-tamination levels prior to performing an operation.
Permanent and/or movable shielding was specified for reduction of levels.
Use of permanent or temporary local exhaust ventilation systems was used for control of airborne contamination.
Operation was designed to be completed with the least practicable time spent in the radiation field.
Appropriate tool., and equipment were specified for the operation to be performed.
The operation was designed considering the minimum number of people necessary for safe job completion.
Remote handling equipment and other special tools were specified to reduce external dose.
Contamination - control techniques were specified.
The operation was designed to be conducted in areas'of as low an exposure as practicable.
Additional ALARA considerations were:
/ ALARA Principles were not considered since the procedure did not involve work in a radiation area.
(5) Prepared by: /! , e# m f inh,, Date 5- t- - ? 3 (6) Reviewed by: )h Date J-(-73
m CP/0/B/8150/03 DUKE POWER COMPANY CATAWBA NUCLEAR STATION CHEMISTRY PROCEDURE FOR THE DETERMINATION OF SODIUM, AUTO ANALYZER 1.0 DISCUSSION 1.1 Scope - This procedure covers the continuous in-line measurement of trace levels of sodium ion in water.
1.2- Principle - Sample stream enters the sodium monitor and passes through a filter, a pressure regulator, a flow meter and a calibration bypass valve. The sample then passes through reagent diffusion tubing in a monoethylamine solution bottle (where pH adjustment takes place) and flows to the electrode flow block. The electrode flow block contains a sodium ion-sensitive electrode, a reference electrode, and a thermistor for automatic temperature compensation. The sample passes from the electrode flow bicek to an atmospheric drain. See Enclosure 6.3.
The sodium electrode (glass electrode) is more responsive to H+ ions than to Na+ ions. For low level sodium ion measurement (ppb range),
sample pH is very important. Therefore, to avoid H+ ion interference, the sample pH is adjusted to about pH 11.3. The pH adjustment is accomplished by passive diffusion of moncethylamine.
, The sample passes through tubing in a reagent bottle containing monoethylamine solution. Monoethylamine diffuses through the tubing wall into the sample raising the sample pH.
The potential of the sodium electrode varies with the sodium ion concentration. At 25'C it exhibits a 59 mV change in potential for each ten-fold increase in Na+ ion concentration,
- l. During calibration, the sample is diverted through an ion exchange
-cartridge to provide a " low sodium" background. Using a variable speed syringe pump to inject a sodium standard into this polished sample, the sodium monitor can be calibrated "on-line".
NOTE: If monoethylamine is not available, concentrated ammonium hydroxide may be used. In this case pH adjustment is to approximately 10.3 instead of 11.3. For very low levels of Na+ (i.e., less than 2 ppb), monoethylamine is preferred.
I 1.3 Limits and Precision
-1.3.1 Na+ may be determined in the range of 0.1 ppb to 1000 ppb between temperatures of O'C to 50*C.
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C?/0/B/3150/03
. s Pass 2 of 10 1.3.2 Calibration precision is i 10%.
1.4 Interferences e
1.4.1 The sodium electrode exhibits an additive interference due to H+ ions, therefore sample pH is adjusted to 11.3 (10.3 with ammonium hydroxide) to mininiize this interference.
The pH adjustment is accomplished.by passive diffusion of either monoethylamine or ammonium hydroxide. To assure pH adjustment, the inlet sample should not be below pH 7.
1.5 Precautions 1.5.1 For low Na+ concentration (1-10 ppb) measurement, it will require a few minutes to flush all the Na+ standard from the electrode flow block after standardization.
1.5.2 Air bubbles trapped near the electrodes can cause a
" bouncing needle" movement. The bubbles can be released by lifting the electrodes up slightly in their holders and then resetting them.
1.5.3 If cooling water is required to reduce sample temperatures, precaution should be taken to prevent the cooling water from being secured'while there is sample flow to the sodium monitor. Live steam will permanently damage the sodium monitor.
1.5.4 The sodium monitor is automatically temperature compensated, dowever, rapid temperature changes in the sample should be avoided since these may create temporary
- = " swings" in the indicated Na+ values.
1.5.5 Be careful not to touch the contact portion of any BNC connector. The conducting film left by-finger prints should be removed be cleaning with a lint-free cloth and isopropyl alcohol or an aerosol contact cleaner.
1.5.6 If sample flow stops, monovalent ions (K+, Ag+, etc.) from
, the reference electrode electrolyte may diffuse through the quiescent solution in the electrode flow block causing the i
meter reading to increase gradually. However, reliable indication should begin after sample flow resumes.
1.5.7 Monoethylamine solution is strongly basic and all work should be performed in a fume hood. Gloves, lab coat, and
- safety glasses shall be worn, as well as having fume hood l closed as auch as possible.
L 1.5.8 Inlet sample pressure must be between 15 psig and 100 psig.
Inlet sample temperature must not exceed 30*C (122*F).
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" ' CP/0/B/8150/03 Pag 2 3 of 10 2.0 APPARATUS 2.1 Orion a/ SLED Sodium Monitor (Model 15-11-02) 2.2 Sodium Electrode (Orion.10-00-18) 2.3 Double Junction Reference Electrode (Orion 10-00-31) 2.4 Deioniza?:J'u Cartridge (Orion 15-00-10 or equivalent) 2.5 Dynamic calibrator (Orion 15-00-95 or equivalent)
- 2. 6 - Syringe. Kit (Orion 15-00-96 or equivalent) 2.7 1.00 ml glass volumetric pipet 2.8 10.00 ml glass volumetric pipet l 2.9 1000.00 ml glass volumetric flask 2.10 50 mi graduated cylinder 2.11 100 ml disposable plastic beaker e
3.0 REAGENTS ~-
3.1 Stock Sodium Standard - Use purchased stock Na+ standard solutions (100 ppe Na+ - Orion 94-11-07, 1000 ppm Na+ - Fisher So-S-139 or equivalent) or prepare a 1000 ppe Na+ stock standard as follows:
Dissolve 2.542 t .002 gm Nacl dryed at 140*C and dilute to 1 liter with Super-Q.
3.2- Sodium standard (1 ppm Na+) - Use 10.00 ml of 100 ppm Stock Sodium Standard and dilute to 1 liter with Super-Q water in a volumetric flask.
or Use 1.00 ml of 1000 ppe Stock Sodium Standard and dilute to 1 liter with Super-Q water in a volumetric flask.
3.3 Filling solution - use the filling solution supplied (Orion 15-00-71) with the double junction reference electrode (Orion 10-00-31).
3.4 Electrode rinse solution - Use the rinse solution supplied (Orion 15-11-13).
3.5 Purchased monoethylamine solution from Orion Cat No. 151111 or equivalent.
3.6 Ammonium Hydroxide, Fisher Cat. No. A-669 cr equivalent.
4.0 PROCEDURE 4.1. ' Calibration of Syringe Pump - before each monitor calibration.
. ~
CP/0/B/8150/03 Page 4 of 10 U
4.1.1 Fill 60 cc syringe with Super-Q water. Expel any air bubbles in the syringe. Connect calibration tubing to syringe.
4.1.2 Remove drive carriage from syringe pump. Clamp the syringe into the center cradle clamp of the syringe pump. Be sure the syringe flange is flush to the syringe clamp.
4.1.3 Replace drive carriage by re-engaging it with the gears on the syringe pump. Push the drive carriage forward until it is flush with the syringe plunger. Be sure drive carriage is aligned straight on syringe pump.
4.1.4 Turn the range switch of the syringe pump to 0FF. Plug syringe pump into an AC power source. Turn flow rate dial to read 500.
4.1.5 Thrn range switch to XI and allow calibration tubing to expel air. Turn range switch to 0FF.
4.1.6 Insert calibration tubing into a 50 ml graduated cylinder, turn range switch to X1 for 1 min. t i sec., or turn range switch to X 1/10 for 10 min. i 10 sec. When time is up, quickly turn switch to 0FF.
4.1.7 Remove tubing from graduated cylinder. Record volume in the graduated cylinder.
4.1.8 If volume in the graduated cylinder is 40 t 0.5 m1, record flow rate and proceed to Step 4.1.9. If not 40 0.5 m1, '
proceed as follows:
4.1.8.1 Adjust flow rate dial using volume recorded in step 4.1.7 as follows:
F * ( )
A v
P where: Fg= adjusted flow rate setting '
Vp = present vol. in ml from Step 4.1.7.
- 4.1.8.2 Repeat Steps 4.1.1 to 4.1.8 using adjusted flow rate setting (F )*
A 4.1.9 Turn flow rate to read 555.
4.1.10 Turn range switch to X1, allow calibration tubing to expel air, then turn range switch to 0FF.
4.1.11-Insert calibration tubing into a 50 ml graduated cylinder, turn range switch to X1 for 1 min. = 1 sec., or turn range switch to X 1/10 for 10 min. t 10 sec. When time is up, quickly turn switch to 0FF.
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- , CP/0/B/8150/03 Pega 5 of 10 4.1.12 If the volume in the graduated cylinder is between 44 al and 44.5 m1, record the flow rate setting and proceed to 4.2. If not in range, adjust the flow rate using the following:
4.1.12.1 FA" ( )
V p
where: FA = adjusted flow rate setting Vp = present vol. in ml from Step 4.1.11 4.1.12.2 Repeat Steps 4.1.10 to 4.1.12 using the new calculated flow rate (FA)*
4.2 Calibration of Sodium Monitor - once every three weeks 4.2.1 Turn sodium monitor ON/0FF switch to ON. Adjust sample pressure regulator to about 15 psig. Adjust sample flow to
, tabout 40 ml/ min. Allow sample to flow through ion exchange j cartridge for approximately 30 min, or until a minimum Na+
background is obtained, by diverting flow with the calibration bypass valve.
4.2.2 Fill 60 cc syringe with 1 ppm Na+ standard (Section 3.2).
Expel any air bubbles in the syringe. Connect calibration tubing to syringe.
4.2.3 Remove drive carriage from syringe pump. Clamp the syringe into the center cradle clamp of the syringe pump. Be sure the syringe flange is flush to the syringe clamp.
4.2.4 Replace drive carriage by re-engaging it with the gears on the syringe pump. Push the drive carriage forward until it i
is flush with the syringe plunger. By sure drive carriage is aligned straight on syringe pump.
4.2.5 Mount the syringe pump on the sodium monitor. Locate the four mounting studs on the upper portion of the sodium l monitor. Slip the upper stud screws of the sodium monitor l through the keyhole-shaped holes on back of the syringe pump.
( 4.2.6 Ensure range switch of the syringe pump is OFF. Plug
- syringe pump into an AC power source. Ensure flow rate
! dial is set on proper setting. Turn range switch to X1; L
allow calibration tubing to expel air; turn range switch 0FF.
4.2.7 Connect calibration tubing to the standard injection port
.at the base of the sample flow block. Turn injection port thumbwheel to align the scribed line along the length of the port. Ensure sample flow is about 40 ml/ min @ 15 psig.
l
CP/0/B/8150/03 Pega 6 of 10 4.?. 8 Adjust flow rate to the setting recorded in 4.1.8. Turn range switch to X 1/100. Wait until a stable reading is obtained (approximately 20 min.) and turn slope control to 100*. Turn calibration control so that meter reads 0.1 PPb .
4.2.9 Turn the pump to 0FF before changing the range setting. If the range is changed with the pump running, the carriage will rapidly move ahead before moving at the desired rate.
4.2.10 Adjust the flow rate to the setting recorded in 4.1.12.
Turn the range switch to X 1/10. Wait until a stable reading is obtained, (approximately 10 min.) then turn the slope control so that the meter reads 1 ppb.
4.2.11 Turn calibration control so that the meter reads 100 ppb.
4.2.12 Turn range switch to 0FF. Turn injection port thumbwheel to align scribed line across the length of the port.
Remove calibration tubing from the injection port.
4.2.13 If the tolerance of the second Na+ standard is not met (1 2 0.2 ppb) in Step 4.2.10, repeat Steps 4.2.2 to 4.2.12. If e the tolerance of the second Na+ standard is still not met, proceed to Section~-4.4.
4.2.14 Readjust calibration bypass valve so that the sample flows directly to the sample block and proceed with Section 4.3.
4.3 Na+ Measurement 4.3.1 Ensure sodium monitor is ON. If sodium monitor was turned 0FF, wait about 5 min. after turning to ON before reading Na+ concentration.
4.3.2. Ensure calibration bypass valve is allowing sample to flow directly to the sample block.
4.3.3 Adjust sample flow and pressure to about 40 ml/ min @ 15 psig. If sample flow has becn secured, wait until a stable reading is obtained (approximately 30 min. after initiating sample flow) before reading Na+ concentration.
4.3.4 Before taking a reading, check electrodes for crystal formation, coated tip, air bubbles at tip, cracks, or any
, deleterious condition. If such a condition is detected, refer to section 4.4 and 4.5.
4.3.5 The indicated Na+ concentration can be read uirectly from the upper scale of the meter in ppb.
4.4 Na+ Electrode Replacement / Rejuvenation - Na+ electrode will undergo a reduction in performance with age. A cracked or coated Na+
electrode will fail to'obtain a correct value for the second Na+
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_s _' CP/0/B/8150/03 Pagt 7 of 10 standard (1.0 0.2 ppb) after the meter has been standardized with the_first Na+ standard (0.1 ppb). If this is the case, the electrode must be replaced or rejuvenated.
4.4.1 Check the glass bulb at the tip of the electrode for cracks. A cracked glass bulb uill not respond to changes in Na+ concentration and should be discarded.
4.4.2 A coated electrode is sluggish in response to changes in Na+ concentration and should be rejuvenated as follows:
4.4.2.1 Swirl lower third of the electrode in the electrode rinse solution for about 30 seconds.
Then rinse thoroughly with Super-Q water.
4.4.2.2 Immerse lower third of the electrode in Super-Q for 3 hours3.472222e-5 days <br />8.333333e-4 hours <br />4.960317e-6 weeks <br />1.1415e-6 months <br />.
l 4.4.2.3 Standardize the electrode as per Section 4.2 before returning it to servica. If the electrode still will not star.dardize, it should be replaced.
4.5 Reference Electrode Maintenance - The reference electrode establishes an electrical cohtact with the solution being measured by means of a " liquid junction". A ceramic frit, porous fiber or mechanical sleeve at the tip of the electrode allows continuous capillary flow of the reference filling solution (electrolyte) into the sample to form this liquid junction.
If this electrical contact is interrupted, a drifting reading will result. This interruption can be caused and corrected by:
4.5.1 Level of electrolyte not covering internal reference i
i element.
[ 4.5.1.1 Refill with proper reference electrode filling solution (s) to just below filling hole (s).
NOTE: Always keep filling solution level higher than level of solution being measured.
7 4.5.2 ECL crystals inside the electrode clogging ceramic frit or
! porous fiber type liquid junction preventing leakage of electrolyte.
[ 4.5.2.1 Drain the electrolyte from the electrode.
l 4.5.2.2 Refill with Super-Q water and allow crystals to
! dissolve.
4.5.2.3 Drain the Super-Q water from the electrode.
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. ~ , CP/0/B/8150/03 Pags 8 cf 10 4.5.2.4 Repeat Steps 4.5.2.2 to 4.5.2.3 as necessary until all the crystals are removed.
4.5.2.5 Refill with proper reference electrode filling solution to just below filling hole.
4.5.3 Foreign material outside the electrode clogging ceramic frit or porous fiber type liquid junction preventing leakage of electrolyte.
4.5.3.1 Boil the tip of the electrode in Super-Q water.
Allow to cool.
4.5.3.2 Carefully apply air pressure to filling hole so that electrode becomes pressurized. A bead of electrolyte should form at the liquid junction.
4.5.3.3 Refill with proper reference electrode filling solution to just below filling hole.
4.5.4 A mechanical sleeve type liquid junction electrode can be disassembled, cleaned with Super-Q water, and reassembled.
Refill with proper reference electrode filling solution to just below filling hole.
4.5.5 Standardize the electrode as per Section 4.2 before returning it to service. If electrode still doesn't standardi:e, it should be replaced.
4.6 Diffusion Tubing / Reagent Bottle Maintenance - Every Month 4.6.1 Secure sample flow and release reagent bottle from electrode flow block. Release locking clamp and unscrew thumbscrew.
4.6.2 Working in a fume hood, remove the cap of the sodium reagent bottle.
4.6.3 Check diffusion tubing for cracks, kinks or signs of aging.
Old tubing will be bleached white and brittle. Replace tubing if necessary.
l l
4.6.4 Clear any obstructions in all fittings.
4.6.5 Check age of moncethylamine; replace with fresh reagent if older than 2 months. Obtain a new bottle of monoethylamine for use and date when put to use. (Anmonium hydroxide should be replaced every 6 months.)
l 4.6.6 Replace any 0-rings that are missing or that have signs of swelling or damage.
4.6.7 Replace caps on the sodium reagent bottle tightly.
l
'. _ CP/0/B/8150/03 Pcga 9 of 10 4.6.8 Reconnect reagent bottle to electrode flow block. Tighten thumbscrew and fasten locking clamp.
4.6.9 Re-establish sample flow at about 40 ml/ min at 15 psig.
4.7 Routine Maintenance 4.7.1 Daily Maintenance 4.7.1.1 Check level of reagent in diffusion bottle.
Normally the level of diffusion reagent wt.1 lower gradually. If the level ever goes up, the diffusion tubing has broken. If this happens, change tubins and reagent per Section 4.6.
4.7.1.2 Adjust the pressure regulator to read 15 psig, then adjust flow to 40 ml/ min if necessary.
4.7.2 Weekly Maintenance 4.7.2.1 Calibration check perform Steps 4.2.1 - 4.2.7.
Adjust flow rate to the setting recorded in 4.1.8. Turn range switch to X 1/100. Wait until a stable reading is obtained (approxikately 20 min). Turn calibration control so that the meter reads 10 ppb.
4.7.3 Tri-Weekly Maintenance 4.7.3.1 Drain, clean, and refill reference electrode per Section 4.5.
4.7.3.2 Calibrate sodium monitor according to Section 4.2.
4.7.4 Six-Week Maintenance 4.7.4.1 Check diffusion tubing and reagent per Section 4.6.
t 4.7.4.2 Condition sodium electrode per Section 4.4.
4.7.5 Three-Month Maintenance 4.7.5.1 After calibration, check deionization cartridge by diverting flow through cartridge for 30 min.
If the reading is above 1 ppb, the cartridge must be replaced. (Normally, a cartridge should last approximately 1 year.)
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'. .s ,, CP/0/B/8150/03 Pcga 10 of 10 4.7.6 Six-Month Maintenance 4.7.6.1 Replace inlet filter assembly. After restoring flow to analyzer, c?eck for leaks and retighten if necessary.
4.7.6.2 Replace both sodium and reference electrodes if six months or older to promote proper operation.
4.7.7 Yearly Maintenance 4.7.7.1 Replace deionination cartridge. One year is the expected lifetime of the cartridge.
5.0 REFERENCES
5.1 Orion Research Inc., Instruction Manual a/ Sled Low-Level Sodium Monitor 5.2 Oconee Nuclear Station, CP/0/B/3004/14 5.3 Marshall Steam Station, Chemistry Procedure for the Determination of Sodium Using Orion Sodium Monitor 6.0 ENCLOSURES '
6.1 Diagram of Sodium Monitor 6.2 Diagram of Calibration Bypass Valve 6.3 Diagram of Sample Flows and Electrode Flow Block 6.4 Diagram of Variable Speed Syringe Pump
I Duka Power Company Catawba Nuclear Station CP/0/B/8150/03 I Enclosure 6.1 Diagram of Sodium Monito
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- 5. pilot light ! l --
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- s. thornoster
- 9. reference electrode jedt - "
- 10. reference electrode ia t 11. recorder /elerm connector .
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- 12. power connector
- 13. ..- .1., studs QM v 14 siectrode holder
- 15. estibratean trypots valve -l1
- 18. fluid connec+ r block .,, jj
- 17. thumbeerow I Q
- 18. standard inject'on port
- a l F'
( 19. flow meter volve b,
- [gmy
- 20. locking clemp
- 21. reegent diffusion bottle l , k=
- 22. pressure requietor volve 7 Cb
- 23. deioniastion certridge 24 filter essembly
- 25. semple tyypass velve
- 26. semple inlet
- 27. drain (Note: CNS drain has been modified)
. I
- Duka Povar Company l Catawba Nuclear Station CP/0/B/8150/03 l
. Enclosure 6.2 Diagram of Calibration Bypass Valve om position of celibration trypass volve
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'- - : CP/0/B/8150/03
, Enclosure 6.3 Diagram of Sample Flows and Electrode Flow Block ,
semple flow during normal operation .
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CP/0/3/8150/03 Enclosure 6.4 Diagram of Variable Speed Syringe Pump l .
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- 1. syringe holder base 9
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- 2. round black knuried knob
- 3. square black knob
- 4. syrings clip - double section
- 5. drive carriage
- 6. end point adjustment knob
- 7. range switch
- 8. flow rate dial
- 9. syringe kit I
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