ML041060388

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Emergency Plan Implementing Procedure Manual Volume B, Revision 2004-04
ML041060388
Person / Time
Site: Oconee  Duke Energy icon.png
Issue date: 04/12/2004
From: Rosalyn Jones
Duke Power Co
To:
Document Control Desk, Office of Nuclear Reactor Regulation
References
Download: ML041060388 (36)
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Text

ph Duke R. A. JONES c Power Vice President A Duke Energy Company Duke Power 29672 / Oconee Nuclear Site 7800 Rochester Highway Seneca, SC 29672 864 885 3158 864 885 3564 fax April 12, 2004 U. S. Nuclear Regulatory Commission Document Control Desk Washington, D. C. 20555

Subject:

Oconee Nuclear Station Docket Nos. 50-269, -270, -287 Emergency Plan Implementing Procedures Manual Volume B, Revision 2004-04 Please find attached for your use and review copies of the revision to the Oconee Nuclear Station Emergency Plan:

Volume B Revision 2004-04 April 2004 This revision is being submitted in accordance with 10 CFR 50-54(q) and does not decrease the effectiveness of the Emergency Plan or the Emergency Plan Implementing Procedures.

Any questions or concerns pertaining to this revision please call Rodney Brown, Emergency Planning Manager at 864-885-3301.

By copy of this letter, two copies of this revision are being provided to the NRC, Region II, Atlanta, Georgia.

yours, N

Nuclear Site xc: (w/2 copies of attachments)

Mr. Luis Reyes, Regional Administrator, Region II U. S. Nuclear Regulatory Commission 61 Forsyth St., SW, Suite 24T23 Atlanta, Georgia 30303 w/copy of attachments Mr. James R. Hall Rockville, Maryland (w/o Attachments, Oconee Nuclear Station)

NRC Resident Inspector J. R. Brown, Manager, Emergency Planning A6L15 www.duke-energy.com

April 12, 2004 OCONEE NUCLEAR SITE

SUBJECT:

Emergency Plan Implementing Procedures Volume B, Revision 2004-04 Please make the following changes to the Emergency Plan Implementing Procedures Volume B.

REMOVE INSERT Cover Sheet Rev. 2004-03 Cover Sheet Rev. 2004-04 Table of Contents, page 1,2,3 & 4 Table of Contents page 1,2,3, & 4 Laboratory Method Process Record Laboratory Method Process Record LM/O/P919 - 02/15/04 LM/O/P919 - 03/29/04

DUKE POWER EMERGENCY PLAN IMPLEMENTING PROCEDURES VOLUME B APPROVED:

L4 E. Nicholson, Manager Safety Assurance Date Approved 04/12/2004 Effective Date VOLUME B REVISION 2004-04 APRIL 2004

VOLUME B TABLE OF CONTENTS Chemistry Lab Determination Of Boron By Manual Colorimetric Titration 11/06/02 LM-O-P003C Chemistry Lab Boron Analysis by Mettler DL 58 Boron Titration 03/29/04 LM-O-P919 I CP/1lA/20021004C Operating Procedure For The Post Accident Liquid Sampling 01/10/03 System (PALSS)

CP/1&2/A/2002/005 Post Accident Caustic Injection Into The Low Pressure 01/07/04 Injection System CP/2/A12002/004C Operating Procedure For The Post Accident Liquid Sampling 01/10/03 System (PALSS)

CP/3/A/2002/004C Operation Procedure For The Post-Accident Liquid Sampling 01/10/03 System (PALSS)

CP/3IA/2002/005 Post Accident Caustic Injection Into The Low Pressure 01/07/04 Injection System HPIO/B/1009/009 Procedure For Determining The Inplant Airborne Radioiodine 12/03/97 Concentration During Accident Conditions JHP/O/B/1009l015 Procedure For Sampling And Quantifying High Level 07/23/01 Gaseous Radioiodine And Particulate Radioactivity HP/0I1B/1009/016 Procedure For Emergency Decontamination Of Personnel 12/29/97 And Vehicles On-Site And From Off-Site Remote Assembly Area HP/1/A/1009/017 Operating Procedure For Post-Accident Containment Air 09/13/00 Sampling System HP/2/A/1009/017 Operating Procedure For Post-Accident Containment Air 09/13/00 Sampling System HP/31A/1009/017 Operating Procedure For Post-Accident Containment Air 09/13/00 Sampling System RP/0/B/1000/011 Planned Emergency Exposure 02101/94 RP/O/B/10001025 Operational Support Center Manager Procedure 03/10/04 RPIOIB/1000/027 Re-Entry Recovery Procedure 05/30/00 1 Revision 2004-04 April 2004

VOLUME B TABLE OF CONTENTS SHIOIBI2005I003 Distribution of Potassium Iodide Tablets in the Event of a 11/06/03 Radioiodine Release Chemistry Manual Emergency Response Guidelines 02/17/04 5.1 Chemistry Manual Post Accident Procedure Use Guidelines 05/29/03 5.2 Maintenance Emergency Preparedness Plan Activation 08/06/02 Directive 9.1 WPG 1.5 Emergency Plan for Work Control Group 03/31/03 OMP 1-7 Operations Emergency Response Organization 08/31/00 Radiation Protection Radiation Protection Emergency Response 01/20/04 Manual 11.1 Radiation Protection Radiation Protection Site Assembly 01/20/04 Manual 11.4 Safety Services Safety Services Emergency Response Procedure 2.1 03/14/00 Procedure 2.1 2 Revision 2004-04 April 2004

Volume B Table Of Contents DELETED PROCEDURES CP1/O/A2003/02B Determination of Failed Fuel - (04/03186) DELETED CPIOIAI2004I02A Post Accident Determination of Boron Concentration Using the Orion Fluoroborate Electrode - (03/28/85) DELETED CP/0/A12004/02F Determination of Boron for High pH Samples Following Caustic

- (12/12/94) - DELETED CP/0/A12004/09D Post Accident Determination of PH - (03/28/85) DELETED CPIO/A/2004/037 Determination of Boron by Manual Colorometric Titration Using Phenolpthaline Indicator - (12/12/94) DELETED CP/0/AJ2005t2D Post Accident Determination of Gamma Isotopic Activity - (07109182)

DELETED CP/OIBI2001I05A Post Accident Analytical Procedure Guidelines- (06/14/85)

DELETED CP/O/B/2005/09 Determination of Failed Fuel - (10/05/90) DELETED CP/IOIBI4003IO1 Procedure for Environmental Surveillance Following a Large Unplanned Release of Gaseous Radioactivity - (07/25/85)

DELETED CP/0/B/4003102 The Determination of Plume Direction and Sector(s) to be Monitored Following a Large Unplanned Release of Gaseous Activity DELETED HP/0/1B/1009/10 Procedure for Quantifying Gaseous Releases Through Steam Relief Valves Under Post-Accident Conditions - (10/30/85) DELETED HP/IOIB/1009/111 Projection of Offsite Dose from the Uncontrolled Release of Radioactive Materials Through a Unit Vent - (05/24/85) DELETED HP/0/B/1009/012 Distribution of Potassium Iodide Tablets In The Event Of A Radioiodine Release - DELETED

]HPIOJBII1009114 Project Offsite Dose from Releases other than Through a Vent -

(02/12/85) DELETED IPIO/A/0050/001 Procedure to Provide Emergency Power to an HPI Pump Motor from the ASW Switchgear - (10/05/92) DELETED IP/01B100501004 Emergency Power - Telephone System - (03/30/87) DELETED DTA-1 Site Assembly (ESS - Maintenance Division) - (11/07/95)

DELETED 3 Revision 2004-03 March 2004

Volume B Table Of Contents DELETED PROCEDURES DTA-2 Station Support During a Site Assembly - (03126192) DELETED Integrated Sched. Integrated Scheduling Group Directive 6.0 - (10/26/89) DELETED STA. SVCS. 3.1.6 Industrial Safety, Health, and/Fire Protection Section - (09/18/89)

DELETED Commodities & Facilities Site Assembly CF 1 (111/01/94) - DELETED CF 1-10 Commodities & Facilities Station Support During a Site Assembly Functional Area Directive 102 Functional Area Directive 102 - (07/14/97) - DELETED from Volume B, moved to Volume C on 06/15/98 Rev. 98-04 LM-O-PO03A Determination of Boron Using The Mettler DL4OGP - 06/18/98 -

DELETED Maintenance Directive 9.2 Emergency Plan For Members Of The Work Control Group 04/07/03 DELETED 4 Revision 2004-03 March 2004

Duke Power Company Nu6itar Generation Department LABORATORY METHOD PROCESS RECORD Reference Use Station: Oconee LMI~OJP919 Rev. #: 9 Change:

(A, B, or C, etc.)

Title:

Boron Analysis by Mettler DL-58 Boron Titrator (check applicable boxes) 1 This Method is based on General Lab Method LMGI___ Rev, - without substantive changes.

[Er This Method is based on General Lab Method LM/G/6 9 / 9 Rev,- / with substantive changes.

0 This Method is not based on a General Lab Method.

0' This revision does not invalidate criteria for use of a laboratory method (reference SCM-6, Section 5.1.1)

(if any of these criteria are no longer valid, then a Technical Procedure must be used for this activity) o These changes affect the associated method development package.

0' Field testing performed. Date: - arr mv Initials: -LI5.

Description of Change: (Attach additional pages if necessary)

Basis for Change: (Attach additional pages if necessary) a 0P Field Testing Comments: (Attach additional pages if necessary)

Prepared by (ItL Date /a shah Technical Review by y 7-rAtdazj -Date 3/3k Additional Review by (optional) Date Approvedby ~ Al Date 3/Z K2-

LM/O/P919 Page 2 of 16 Boron Analysis by Mettler DL58 Boron Titration

1. Purpose NOTE: Seven Control Copies and one Information Only copy of this Lab Method shall be routed to the Emergency Preparedness Team within three (3) working days following any approved changes/modifications.  !

1.1 Scope CAUTION: This laboratory method describes the automatic titrimetric method for.

determining boron in aqueous solutions. This laboratory method is applicable for Primary Systems.

1.2 Principle Boric acid is a weak acid and cannot be titrated directly with a strong base to an accurate endpoint. Mannitol is added to stabilize the anion of boric acid and increase the strength of the acid.

The mannitol-borate complex can then be titrated with a strong base. The concentration of boron is proportional to the amount-of standard sodium hydroxide required to titrate the boron to a pH endpoint of 8.3.

The titration is performed by a Mettler DL58 automated titration system. Samples are loaded onto a Mettler ST20A Sample Transport Unit. A digital buret assembly dispenses titrant into the sample. The rate of titrant delivery is slowed near the equivalence point. This allows ample time for thorough mixing and reaction of titrant with the sample until the pH equivalence point is obtained.

1.3 Interferences 1.3.1 Carbon Dioxide is an interferent; however, the interference should be negligible if the following conditions are met:

  • Water used for preparing sodium hydroxide is boiled or deaerated.
  • Sodium hydroxide reservoir is air tight or equipped with a CO2 absorption tube filled with drying agent.
  • Sample is not over-stirred.
  • Sample exposure to air is minimized.

1.3.2 Lithium Hydroxide and Ammonium Hydroxide are potential interferences; however, these interferences have been determined to be negligible as the change in boron concentration that they cause is less than the required accuracy needed.

LMIO/P919 Page 3 of 16 1.3.3 Matrix interference has been found to occur due to possible inputs into the Reactor Building Normal Sump (RBNS) samples. Therefore, these samples should be pH'd prior to analysis (Step 4.5.2). All RBNS sample results are reported as Information Only and designated with an "N".

1.4 Limits This method is applicable for samples containing between 0.2 - 10,000 ppm boron as boric acid.

  • 1.5 Precautions 1.5.1 The pH electrode should be stored in a conditioning agent as recommended by the electrode manufacturer when not in use.

1.5.2 The sodium hydroxide reservoir should be emptied and refilled rather than "topped off" when the supply is low.

1.5.3 Typically, when the titrator-has been idle, the first standard/sample will show a high-bias result. Therefore, when the titrator has been idle, the first standard/sample of a titration series'should be run in duplicate, and the first result discarded.

1.5.4 If the titrator does not initiate analysis after pressing the [Run] key twice, then the [Run] key may need to be pressed again or the [Start] key may-be pressed.

1.5.5 If the titrator goes into the Hold mode when adding samples to a series, the [Hold] key may need to be press6d to resume analysis.

1.5.6 This laboratory method is related to plant Reactivity Management.

Reactor coolant boron directly impacts Reactivity Management. Reactor coolant and support system boron concentrations are determined by this method.

1.5.7 When determining the concentration of PALSS boron, results obtained must be multiplied by the PALSS dilution factor found in the appropriate PALSS procedure(s).

1.5.8 Wear the following minimum proper personal protective equipment (PPE) when performing this analysis.

9

  • Labcoat
  • Safety glasses
  • Gloves
  • Apron and faceshield or hood sash when handling 50% W/W Sodium Hydroxide or Hydrochloric Acid

LMO/P919 Page 4 of 16 1.5.9 When boric acid is heated at 1000 to 160'C, it gradually decomposes and loses water to form metaboric acid (HBO2) then pyroboric acid (H2 B4 07 ),

and finally boric anhydride (B203). Hence, in preparing a boron standard, boric acid is neither dried nor desiccated prior to weighing.

1.5.10 For error messages, malfunctions, and/or troubleshooting refer to Enclosure 6.3.

1.5.11 Sample concentration must not exceed a burette delivery volume of 40 mL. See Step 4.5.3 for selecting appropriate sample size.

1.5.12 Sodium Hydroxide lines and delivery tip must be kept free of air bubbles at all times. Air bubbles will result in unreliable sample results.

1.5.13 Samples should be bracketed with an appropriate QC. For samples < 100 ppm expected use a 10 ppm QC, for > 100 ppm expected a 1000 ppm QC.

1.5.14 Samples of unknown matrix with pH > 7 and buffering capacity may give skewed results if not pH adjusted prior to analysis (Step 4.5.2).

1.5.15 Large temperature swings in the lab will affect the analysis, requiring restandardization.

2. Apparatus 2.1 MettlerDL58 Compact Titrator System 2.1.1 DL58 Titrator 2.1.2 20 ml Buret or 10 mL Buret 2.1.3 ST20A Sample Transport 2.1.4 Printer 2.1.5 Electronic Balance with Data Output Module and Static Ionizers 2.1.6 Combination pH electrode, pH 0-14 2.2 Sample cups, 100 mL 2.3 Volumetric flasks 2.4 Volumetric pipets K>

uVOnPsls Page 5 of 16

3. Reagents CAUTION: Chemical hazards shall be known prior to use. For additional information and first aid requirements, refer to MSDS Sheets.

3.1 pH Buffers, 7, 9, 10 3.1.1 Fisher buffers or equivalent may be purchased or prepared and used per package instructions.

3.1.2 Use manufacturer stated shelf life OR record shelf life as 3 months.

3.2 Electrode Filling Solution 3.2.1 Use solution specified by the manufacturer of the electrode in use.

3.2.2 Use manufacturer stated shelf life.

NOTE: Reagents may be prepared in varying quantities as long as the ratios remain unchanged.

3.3 Sodium Hydroxide (NaOH), 0.10 N 3.3.1 Purchased NaOH (Fisher SS278-1 or equivalent) 3.3.1.1 Use manufacturer stated shelf life.

3.3.1.2 Store in an air tight container OR a container fitted with a carbon dioxide (CO2 ) absorption tube.

.3.3.1.3 Standardize solution once per week or prior to use, whichever is less frequent, per Section 4.3 (NaOH Standardization).

3.3.2 Prepared NaOH, 0.10N WARNING: Sodium Hydroxide is corrosive. Level III PPE (labcoat, safety glasses, gloves, and faceshield or hood sash) is required when handling 50% WJW Sodium Hydroxide.

3.3.2.1 Add 32.0 grams (31.5 - 32.5) of liquid 50% W/W NaOH to 3850 (3845 - 3855) mLs of boiled or dearated reagent grade water AND mix.

3.3.2.2 Store in an air tight container OR a container fitted with a carbon dioxide (CO2 ) absorption tube.

3.3.2.3 Record shelf life as 1 year.

3.3.2.4 Standardize solution once per week or prior to use, whichever is less frequent, per section 4.3 (NaOH Standardization).

LMIO/P919 Page 6 of 16 3.4 Electrode Storage Solution (0.5 mol/L KCL) 3.4.1 Weigh out 37.275g +/- 0.1g anhydrous KC1. Add to a 1 L volumetric flask and bring to volume with deionized water.

3.4.2 Record shelf life as 3 months.

3.5 Standard Boric Acid Solution (NaOH Standardization), 1000 mg/L 3.5.1 Dissolve 5.7194 grams (5.7189 - 5.7199) of Boric Acid (H3 B0 3 ) with reagent grade water in a 1000 mL volumetric flask AND dilute to volume.

3.5.2 Record shelf life as 1 year.

3.5.3 Verify solution concentration per section 4.4 (QC Check/Sample Analysis).

3.6 QC Boric Acid Solution, 1000 mg/L 3.6.1 Use purchased 1000 mg/L Boric Acid Standard 3.6.2 Use manufacturer stated shelf life.

3.6.3 Obtain certificate of analysis (COA) from Fisher for each lot number.

3.7 QC Boric Acid Solutibn, 10 mglL 3.7.1 Using a volumetric pipet and a volumetric flask, dilute 10 mL of the purchased Fisher standard to 1000 mL with deionized water.

3.7.2 Record shelf life as 1 month.

3.8 Mannitol WARNING: Hydrochloric acid is corrosive. Level III PPE (labcoat, apron, safety glasses, gloves, faceshield or hood sash) is required when handling concentrated Hydrochloric Acid.

3.9 Hydrochloric Acid (HCI), 0.0025N 3.9.1 Add 250 [iL of concentrated HCI to a 1000 mL volumetric flask partially filled with reagent grade water.

3.9.2 Dilute to volume with reagent grade water AND mix.

3.9.3 Record shelf life as I month.

LMIO/P919 Page 7 of 16 3.10 Hydrochloric Acid (HCI) 50% V/V 3.10.1 Adding the acid to reagent grade water, combine 50 mLs of reagent grade water and 50 mLs concentrated HCl.

3.10.2 Within a closed container, mix by inverting.

3.10.3 Record shelf life as 6 months. ,

NOTE: 1. It is NOT the intent of this procedure to perform the sections sequentially but to perform only those section(s) necessary to meet the need at the time.

2. During troubleshooting specific keystroke functions can deviate from this method in order to identify and correct instrument problems.

The programmed methods in the instrument are:

1. Probe Cal. (pH probe calibration)
2. Measure pH (pH 9 buffer check)
3. Blank (mannitol) >
4. Boron NaOH Standardization (titer factor)
5. Boron (density corrected) (QC/Sample analysis)
4. Procedure 4.1 Initial Setup 4.1.1 Ensure power to titrator, balance, sample changer, and printer is on.

4.1.2 Ensure sufficient volume of sodium hydroxide and reagent grade water in reservoirs.

4.1.3 If needed, refer to Enclosure 6.1. (Sample Changer-Manual Operation) to operate the sample changer in the manual mode at any time during the performance of this procedure 4.1.4 If needed, refer to Enclosure 6.2 (Sample Series Manipulations) to perform any of the following at any time during the performance of this procedure:

  • Delete a sample from a sample series
  • Add additional samples to end of sample series
  • Insert an urgent sample into a sample series
  • Add additional sample series to existing series.

K>~

LMIO/P9 l9 Page 8 of 16 4.2 NaOH Burret Rinse:

4.2.1 Perform this section:

  • When NaOH reservoir is refilled.

4.2.2 Stir NaOH reservoir to thoroughly mix AND perform the following:

4.2.2.1 Place empty sample cup in It 1 position of sample changer and refer to Enclosure 6.1 (Sample Changer Manual Operation) to position electrode assembly in sample cup by placing cup in middle position.

4.2.2.2 Perform the following to rinse buret:

A. Press [Burette]

B. Select "Dispense" C. Press [F5](OK)

D. Ensure the following are selected:

1: Burette drive 2

2. Burette volume per volume of dispenser being used.
3. Volume (mL) 100 for 20 mL dispenser or 50 (mL) for 10 rnL dispenser E. Press [F5] (Start)

NOTE: The buret will rinse 5 times the volume of the dispenser. I 4.2.2.3 Verify there are no air bubbles in the NaOH delivery line or tip.

4.2.2.4 IF air bubbles are present, repeat Steps 4.2.2.1 to 4.2.2.3.

4.3 Daily pH Electrode Standardization 4.3.1 Ensure electrode is clean.

4.3.2 Check filling solution level AND fill as necessary.

4.3.3 Ensure cap is not covering vent hole.

4.3.4 Using approximately 50 mL of each buffer,jplace cup of pH 7 buffer in sI" sample changer position, pH 10 buffer in 2" position, and pH 9 buffer in K> 3rd position.

LM/O/P919 Page 9 of 16 4.3.5 Press or select the following in the order listed:

4.3.5.1 [Sample]

4.3.5.2 [F5] (Add) 4.3.5.3 Select "New Sample Series" 4.3.5.4 [P5] (OK) 4.3.5.5 Select "Number of Samples" 4.3.5.6 [21 4.3.5.7 Scroll down and select "Method ID" 4.3.5.8 [1]

4.3.5.9 [F5] (OK) 4.3.5.10 [F5] (OK) 4.3.5.11 [135] (OK) 4.3.5.12 [F5] (Add) 4.3.5.13 Select "New Sample Series' 4.3.5.14 [F5] (OK) 4.3.5.15 Select "Number of Samples" 4.3.5.16 [1]

4.3.5.17 Scroll down and select "Method ID" 4.3.5.18 [2]

4.3.5.19 [F5] (OK) 4.3.5.20 [F5] (OK) 4.3.5.21 [Run]

4.3.5.22 [F5] (OK) 4.3.5.23 [F5] (START) 4.3.5.24 [F5] (OK)

LM/O/P919 Page 10 of 16

'- /

NOTE: Measurements will be made and calculations carried out automatically for the first two buffers.

4.3.6 After first sample series has completed and calibration results have printed, press [Run] to continue to 2nd sample series (pH 9 buffer).

4.3.7 IF pH 9 buffer result is outside 9 +/- 0L1 pH units, THEN repeat Steps 4.3.4

- 4.3.7.

4.3.8 On a daily basis, record slope value in appropriate database or logsheet for instrument performance trending.

4.4 NaOH Standardization 4.4.1 Perform this section:

  • Once per week-OR prior to use, whichever is less frequent.
  • VWIEN NaOH reservoir has been refilled and buret rinsed per Step 4.2.

4.4.2 Analyze a Blank as follows:

l NOTE: 5 grams of mannitol equates to 2 level teaspoons.

4.4.2.1 Place cup in 1It position of sample changer AND add -=5 grams (4 - 6) of Mannitol to empty sample cup.

4.4.2.2 Press or select the following in the order listed:

A. [Sample]

B. [F5] (Add)

C. Select "New Sample Series" D. [F5] (OK)

E. Select "Number of Samples" F. [1]

G. Scroll down and select "Method ID" H. [3]

I. [F5] (OK)

J. [F5](OK)

uMO/P919 Page 11 of 16 K. [Run]

L. [F5] (OK)

M. [P5] (START)

N. [F5] (OK)

NOTE: . The blank will run, results will be entered and printed out automatically.

A high blank value > 0.0300 mL will skew the results and should be verified by additional blank analysis by repeating Section 4.4.2.

4.4.3 Determination of titer factor with standard boric acid solution (1000 ppm) 4.4.3.1 Press or select the following in the order listed:

A. [Sample]

B. [F5] (Add)

C. Select "New Sample Series" D. [F51 (OK)

E. Select "Number of Samples" F. [2]

G. Scroll down and select "Method ID" H. [4]

I. [P5] (OK) 4.4.4 Place a sample cup on balance pan AND tare.

4.4.5 Transfer 20 g (18.0 - 22.0) of Standard Boric Acid Solution (NaOH Standardization) into sample cup.

4.4.6 When balance reading stabilizes, press [P4] (Balance).

4.4.7 Press [75] (OK) twice 4.4.8 Press [15] (OK) 4.4.9 Place sample cup containing Standard Boric Acid Solution in sample changer.

IMO/P919 Page 12 of 16 NOTE: 1. =5 grams of mannitol equates to 2 level teaspoons.

2. Mannitol may be added at anytime once the sample has been placed in the sample changer prior to starting the analysis (Step 4.4.14).

4.4.10 Add = 5 grams (4 - 6) Mannitol to eich sample cup.

1 4.4.11 Repeat Steps 4.4.4 to 4.4.10 once.

4.4.12 Press [Run]

4.4.13 Press [F5] (OK) 4.4.14 Press [F5] (START) 4.4.15 Press [F5] (OK)

NOTE: Boric Acid Standard Solution will run, results will be entered and printed out automatically.

4.4.16 Analyze a QC check per Step 4;5 (QC Check/Sample Analysis) to verify that the standardization is acceptable.

NOTE: Samples of unknown matrix or requiring pH adjustment shall be reported as Info. l Only unless results are documented as accurate, based on spiking data. l 4.5 QC Check/Sample Analysis 4.5.1 IF analyzing samples containing borax with pH >6.4 (following post accident conditions), THEN adjust sample pH to 6.2 (6.0 - 6.4) using 0.0025N HCL.

4.5.2 IF analyzing samples of unknown matrix or with a suspected pH1 7, THE N perform the following:

4.5.2.1 Detennine the pH.

4.5.2.2 IF the pH is < 7, continue to step 4.5.3.

LM/01P919 Page 13 of 16 4.5.2.3 IFthepHis>7, A. Add 2 even scoops of mannitol to approximately 25 mls of sample.

B. Recheck pH of the sample following addition of mannitol.

C. IF pH < 7, continue to Step 4.5.3.

D. IF pH > 7, THEN adjust sample pH to a range of 6.0 -

6.4 using 50% HCI in 10 pl increments.

4.5.2.4 Using the pH adjusted sample, continue to Step 4.5.3.

4.5.3 Select appropriate sample size:

Boron Concentration (ppm) +/- 50 ppm f Sample Size (grams) t+/-2 g 0-500 25 500 -2000 10 2000- 10,000 5 4.5.4 Press or select the following in the order listed:

4.5.4.1 [Sample]

4.5.4.2 [F5] (Add) 4.5.4.3 Select "New Sample Series" 4.5.4.4 [F75 (OK) 4.5.4.5 Select "Number of Samples" 4.5.4.6 [Enter number of samples in sample set, i.e. 6]

4.5.4.7 Scroll down and select "Method ID" 4.5.4.8 [5]

4.5.4.9 [F5] (OK) 4.5.5 IF entering sample ID is desired, press [A] to select "Sample ID" AND using the keyboard enter sample name, THEN press [v] to select "weight

[g]".

4.5.6 Place sample cup on balance pan AND tare.

4.5.7 Transfer appropriate amount of sample into the sample cup AND weigh.

LMIO/P919 Page 14 of 16 4.5.8 When balance reading stabilizes, press [P4] (Balance).

4.5.9 Press [F5] (OK) twice.

4.5.10 Place sample cup in sample changer.

NOTE: 1. 5 grams of mannitol equates to 2 level teaspoons.

2. Mannitol may be added at anytime once the sample has been placed in the sample changer prior to starting the analysis (Step 4.5.13).

4.5.11 Add - 5 grams (4 - 6) Mannitol to each sample cup.

4.5.12 IF analyzing more than one sample, THEN repeat Steps 4.5.5 - 4.5.11 for each additional sample.

4.5.13 Press [Run]

4.5.14 Press [F5] (OK) 4.5.15 Press [P5] (Start) 4.5.16 Press [F5] (OK) 4.6 Instrument Standby 4.6.1 Place sample cup of conditioning agent in last available position in sample changer.

4.6.2 Place red marker in hole next to sample cup of conditioning agent.

LMJO/P919 Page 15 of 16 lNOTE: The sample changer will recognize the marked sample cup as the last in the sample l I ~set and place the electrodes in it automatically.l 4.7 Calculations NOTE: These calculations are performed automatically by the instrument.

I I 4.7.1 Boron Result ppm Boron = Const x Wihtx V x Con 10.811 gBoron Where: Const = mol HB03 leq / mol Weight = Sample weight in grams 1

V =-ml Xtotal buret vol (ml)

V titrant consumption at the equivalence point in buret units.

1 IC Weight Const Reag V Cone = titrant concentration in milli-equivalents per buret volume 61.83 g JIBO / eq Const Reag = 1000 4.7.2 Density Correction

[B] w = [B] w * (0.99707 + (1.96082E-' * [B] , ))

Where: 1.96082E 6 = factor based on linear regression of boric acid solution densities.

0.99707 = density of water at 250 C.

5. References 5.1 Mettler Toledo DL58 Titrator Reference Handbook.

5.2 Nuclear Generation Department Analytical Quality Control Program.

LMIO/P919 Page 16 of 16

6. Enclosures 6.1 Sample Changer Manual Operation 6.2 Sample Series Manipulations 6.3 Error Messages, Malfunctions, and Troubleshooting 6.4 Operation of Primary Lab Temperature I Humidity Monitor 6.5 Routine Maintenance for the DI-58

Enclosure 6.1 LMIO/P919 Sample Changer Manual Operation Page 1 of 2

1. Change Lift Position 1.1 Press or select the following in the order listed:

1.1.1 [Changer] or [Fl] (Esc) to return to/bring up sample changer menu.

1.1.2 Select "Change lift position" 1.1.3 [F5] (OK) 1.1.4 [F4] (Modify) to select 'Top", "Bottom", or "Middle" 1.1.5 [F5] (Start) 1.1.6 [Fl] (Esc) to return to menu.

2. Rotate Turntable 2.1 Press or select the following in the order listed:

2.1.1 [Changer] or [Fl] (Esc) to return to/bring up sample changer menu.

2.1.2 Select "Rotate turntable" 2.1.3 [F51 (OK) 2.1.4 Select "Direction" 2.1.5 [F4] (Modify) to select "Forward" or "Backward" 2.1.6 Select "Number of Positions" 2.1.7 Enter the number of positions to move from the numeric keypad 2.1.8 [F5] (Start) 2.1.9 [Fl] (Esc) to return to menu.

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Enclosure 6.1 UM/O/P919 Sample Changer Manual Operation Page 2 of 2

3. Rinse Electrodes with Demineralized Water 3.1 Press or select the following in the order listed:

3.1.1 [Changer] or [Fl] (Esc) to return to/bring up sample changer menu.

3.1.2 Select "Dispense/rinse" 3.1.3 [F5] (OK) 3.1.4 [F4] (Modify) to select "Rinse" NOTE: The "Dose" and "Dispense" options are not used.

3.1.5 [F15] (Start)

INOTE: Water will rinse electrodes until [15] is pressed again. I.

3.1.6 [F5] (Stop) 3.1.7 [Fl] (Esc) to return to menu.

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Enclosure 6.2 LMIOIP919 Sample Series Manipulations Page 1 of 2

1. Delete a Sample from a Sample Series 1.1 Press or select the following in the order listed:

1.1.1 [Sample]

1.1.2 Select sample to be deleted 1.1.3 [1P2] (Delete) 1.1.4 [OKI.

.1;2 Remove deleted sample from sample changer AND move any remaining samples forward one position.

1.3 Press [Run] to return to measured values screen.

2. Add Additional Samples to Sample Series 2.1 Press or select the following in the order listed:

2.1.1 [Sample]

2.1.2 Select last sample in series 2.1.3 [P5] (Add) 2.1.4 Select "Sample to Series" 2.1.5 [F51 (OK).

2.2 Perform Steps 4.5.5 - 4.5.11 of the procedure.

2.3 Repeat Steps 2.1 - 2.2 of this enclosure for each additional sample.

2.4 Press [Run]

3. Insert an Urgent Sample into Sample Series NOTE: Active sample will continue to run while adding urgent sample.

3.1 Press or select the following in the order listed:

3.1.1 [Sample]

3.1.2 Select active sample 3.1.3 [F5] (Add) 3.1.4 Select "Urgent sample"

Enclosure 6.2 LMIO/P919 Sample Series Manipulations Page 2 of 2 3.1.5 [F5] (OK) 3.1.6 Select "Method ID" 3.1.7 [5]

3.1.8 [F5] (OK) 3.2 Repeat Steps 4.5.5 - 4.5.9 of the procedure. -

3.3 Place sample cup in appropriate position in sample-changer AND move remaining samples as needed.

3.4 Add = 5 grams (4 - 6) Mannitol to sample cup (equivalent to 2 level teaspoons).

3.5 When active sample completes and results print, press "Run" to start urgent sample.

3.6 When urgent sample completes and results print, press [F5] (OK) to continue with original sample series.

4. Add Additional Sample Series to Existing Series NOTE: The last sample in the current series must be selected prior to adding the new series' (F5(Add)).

4.1 At anytime up to 2 additional sample series/methods may be loaded into the titrator program along with the current method being run. This can be accomplished as follows:

4.1.1 Refer to the procedure section associated for the preferred method and perform as written:

  • Method 1 / Method 2 pH calibration /9 Buffer check Section 4.3
  • Method 3 Blank Analysis Section 4.4.2
  • Method 4 Titer Factor Section 4.4.3
  • Method 5 QC/sample analysis Section 4.5 4.1.2 After each sample series is complete, press [Run] to start the next programmed series.

4.1.3 Repeat at 4.1.1 as desired as long as no more than 3 sample series are programmed to run at one time.

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Enclosure 6.3 LMIO/P9I9 Error Messages, Malfunctions Page 1 of 3 and Troubleshooting

1. Malfunctions not reported by the DL-58 Titrator Malfunction Potential Cause Action No display on titrator Titrator not connected to power supply Connect to power supply, if fault

. persists contact METTLER TOLEDO Service Several points of the display Contact METTER TOLEDO missing Service Display does not match the Contact METTLER TOLEDO pressed key Service Stirrer does not rotate Stirrer not properly assembled or sensors Check stirrer and seating of the block it at the titration stand sensors Transfer error to attached Peripheral faulty or switched off Check attached device is peripheral functioning properly Device (printer, balance, Device not switched oh Switch on device terminal) at Centronics or RC interface do not react Wrong settings . . Settings and configuration must Configuration (switch settings) wrong match (see Section 2.7)

Burette does not move to zero Burette drive faulty - Contact METTLERTOLEDO position when switched en Service Wrong potential or pH values Electrode faulty -Check electrode (see electrode data sheet)

Calibration data wrong Check defined data Use new electrode Faulty cable Replace cable No dispensing, the titrant is Burette tip clogged Clean burette tip discharged from stopcook or piston Follower cam on burette mounted Insert follower cam correctly wrongly (see Section 10.2.3)

Enclosure 6.3 LMU/OP919 Error Messages, Malfunctions Page 2 of 3 and Troubleshooting

2. Error Messages generated by the DL-58 Titrator Message Potential Problem Action EPROM or RAM Test Failed Memory is faulty Contact Staff or ME'TLER

._ TOLEDO Support Internal Error Potential Hardware Failure has occurred Contact Staff or MEI`LER

__ .TOLEDO Support Memory Faulty Parts of User Memory is faulty Contact Staff or ME'ITLER TOLEDO Support Faulty Data Deleted Stored Methods have been partially or Reload Methods manually or from totally deleted memory card Storage Not Possible Memory capability of processor has Notify Staff been exceeded
3. Common Problems and Troubleshooting Message Potential Problem Action pli 9 Buffer Out of Control Bad pH probe (more likely problem) Replace probe Faulty cable Replace cable Observe jumpy pH readings Faulty cable (more likely problem') Replace cable with NaOH additions Faulty probe Replace probe Insufficient stirring of mannitol Broke propeller blades on stirrer Replace stirrer Insufficient water dispensed Worn pump tubing Replace small tubing inside pump

._ cover OOC QC and/or samples not any of above - see related action trending

- poor standardization - recalibrate and/or restandardize

- air bubbles-in NaOH dispensing line - clear line of air bubbles

- clogged dispensing line- - check line & change if needed

- worn buret and/or piston (visible - inspect, clean or replace as needed leakage)

- noticeable temperature shift in lab - write R005 for air handling problems and recalibrate &

standardize Sample Changer skips sample Sensor is dirty - Clean Sample Changer and Sensor Reset Electronics by switching Electronics confused DL58 and Sample Changer OFF then back ON

- Ensure Black sample spacers used on sampler changer Instrument lost contact with Lab x is not open or computer is locked Check associate computer & open computer up program or unlock computer Press OK - Titrator should restart, if not press reset & continue analysis by pressing run.

Enclosure 6.3 LMIO/P919 Error Messages, Malfunctions Page 3 of 3 and Troubleshooting 3.1 IF normal troubleshooting within the shift fails to correct the problem, the instrument should be declared out-of-service and documented per the QC Program.

3.2 IF both titrators are declared out-of-service at the same point of time, actions shall be taken (i.e. reagent preparation) to be ready to perform a-Manual Boron Analysis per LM/O/PO03C.

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Enclosure 6.4 LMIO/P919 Operation of Primary Lab Temperature / Page 1 of 3 Humidity Monitor NOTE: The following allows you to pull data from the Temperature/Humidity monitor, print the .

data, save the data, reset the device and restart the device.

1. Ensure PC-87 (Temperature/Humidity Monitor) is connected via cable to the lab computer.
2. From desktop, open MadgeTech 2.00 program icon
3. From Main Menu, Click "Device"
4. Select "Read Device Data". This will download data from the device.
5. WHE N download of data is complete, select "Summary Tab".
6. Record the following to comments on Enclosure 6.5:
  • Dates in service
  • Minimum Temperature e Maximum Temperature
  • Average Temperature
7. Print a hard copy of the "Summary" for staff review.

K-i 8. Compare the average to the previous week's data.

9. IF > 5 QC difference between the minimum and maximum for the current time frame or between the current and previous weeks mean, then contact staff.
10. To save the file perform the following:

10.1 Select "Data" tab 10.2 Select "File" 10.3 Select "Save As" 10.4 Select "Sections Drive" 10.5 Select "Chem" 10.6 Select "Primary" 10.7 Select "Instrument Backup Files"

Enclosure 6.4 LMIO/P919 Operation of Primary Lab Temperature / Page 2 of 3 Humidity Monitor 10.8 Select "Madge tech lab tempbhumidity" 10.9 Save using a format of datemonthyear for the file name Example: 20janO4.csv CAUTION: The following will clear all readings i1. MMHEN complete reset and restart the device:

11.1 Select "Device" from the main menu.

11.2 Select "Reset Device".

  • 11.3 WHEN prompted to continue, select "yes" 11.4 WHEN prompted that the device is reset, select "OK".

11.5 From main menu select the following:

11.5.1 "Device" 11.5.2 "Start Device" 11.6 . W EN prompted to continue, select "yes".

11.7 Verify on the "Start Device"-screen the following:

  • "Start Now" is checked
  • User ID is "RHTemp"
  • Reading Rate is 5 minutes 11.8 WHEN prompt screen appears, select "Start Device" button 11.9 Verify a message appears "Device Started" 11.10 WHEN pop up screen shows device started, select "OK".

Enclosure 6.4 LM/O/P919 Operation of PrimaryLab Temperature I Page 3 of 3 Humidity Monitor

12. IF you want to check device status perform the following:

12.1 Select "Device" from main menu.

12.2 Select " Identify Device and Read Status" 12.3 Verify from pop up screen Device Status Info.

12.4 Select "OK"

13. Close program when complete.

Enclosure 6.5 LM/O/P919 Routine Maintenance for the DL-58 Page 1 of 3 NOTE: Daily pH results shall be logged on the Chemdesk QC Chart for the appropriate instrument (Slope under "Raw Data", Zero Point / pH 9 results under "Comments.) Also recorded weekly on the appropriate QC Chart under "Comments" are the Blank data and Titer Factor. Major maintenance activities will be logged in the Maintenance Log.

WEEKLY Date / Initials Performed Wipe down instrument E Change pH probe filling SoI'n Empty NaOH dispensing line & refill with buret.

flush Standardize w/1000 ppm NIST Boron Standard _

Record Lab temp from Madge Tech Date Program (Enc. 6.4) Min . __ .

M ax _ _ _ _ _ _ _ _ _ _

Mean _ ..

Date /Initials Performed Wipe down instrument _. ____.

Change pH probe filling Soln . . . .

Empty NaOH dispensing line & refill with buret flush . ...

Standardize w1O000 ppm NIST Boron Standard .__ _ ._._.

Record Lab temp from Madge Tech Date .

Piogram (Enc. 6.4) Min . . __ _ ._ .

Max . __

Mean _ _.

Date /Initials Performed Wipe down instrument . . .. ._._.

Change pH probe filling Sol'n Empty NaOH dispensing line & refill with buret flush Standardize w/1000 ppm NIST Boron Standard .

Record Lab temp from Madge Tech Date . _ . _ -

Program (Enc. 6.4) MMn ..

Mean _.

Place in Maintenance Log when complete.

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Enclosure 6.5 LM/O/P919 Routine Maintenance for the DL-58 Page 2 of 3 MONTHLY

  • 7 t January February March April May June Clean Instrument &

Sample Changer Table Inspect and Clean Stirrer Propellers _ _

Inspect Burets for Leakage

& Change Piston as Required (Sect. 10.2 of Manual)

Clean Buret and Piston (Section 10.2.5 of Manual)

Change Out Drying Tubes _

July August September October November. December Clean Instrument & . . . .

Sample Changer Table Inspect and Clean Stirrer Propellers Inspect Burets for Leakage

& Change Piston as Required (Sect. 10.2 of Manual)

Clean Buret and Pistcm-(Section 10.2.5 of Manual)

Change Out Drying Tubes Place in Maintenance Log when complete.

Enclosure 6.5 LMIO/P919 Routine Maintenance for the DL-58 Page 3 of 3 BIANNUAL Date / Initials Performed Change Internal Tube of Water Pump ANNUALLY I Replace Static Ionizers PC-73 Control # Date Rec'd PC-74 Control'# Date Rec'd AS NEEDED Date / Initials Performed

!Clean under Balance Pan Replace pH Probe . ._._._ .

Replace Buret Replace pH Probe Cable __

Clean/Replace Buret Valve . l .

Place in Maintenance Log when complete.

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