Purpose - Nuclear Materials and Fuel Cycle Research · Web viewUsing a wrench, screw the valve...

Laboratory Specific Operating Procedure

(Center for Nuclear Materials and Fuel Cycle Research)

Written By Shaoqiang Guo (guo946osuedu)

Reviewed By Jinsuo Zhang

(zhang3558osuedu)

Location E396 amp E465

Revision 00

Date of revision 11102015

NMFC Laboratory Specific Operating Procedure of 77

Table of Contents

10 Purpose220 Scope 230 Responsibilites240 General Laboratory Procedures250 Chemical handling storage and transportation360 Laboratory Training4Appendix 1 General Glove box operation6Appendix 2 Kerr Auto Electro-Melt Furnace11Appendix 3 Gamry Interface 100013Appendix 4 High-Temperature Electrochemical Cell15Appendix 5 High-Temperature High-Pressure corrosion cracking system17Appendix 6 High-Temperature High-Pressure flow loop23

Appendix 6-1 Large flow pump operation instructions49Appendix 6-2 Small flow pump operation instructions51Appendix 6-3 U3000 ultrasonic flow meter operation instructions52

Appendix 7 Glass cell system54Appendix 8 Shaker table setup60Appendix 9 Use of Pipettes65Appendix 10 Solubility experiment procedure67Appendix 11 NMFC Laboratory Specific Operating Procedure Sign off Sheet71

NMFC Laboratory Specific Operating Procedure Page 2 of 77

10 PURPOSE

The purpose of this Lab Operating Procedures is to provide guidance to ensure the safety and integrity for the experimental work in Center for Nuclear Materials and Fuel Cycle Research (NMFC) The detailed procedures for all facilities currently in our lab are included Any procedure or instructions can be added to this Lab Operating Procedure if you found it is important but missing in this document The electronic copy can be found on the NMFCrsquos website and the hard copy in the lab needs to be updated annually

20 SCOPE

This NMFC Lab Operating Procedure is applicable to all students and employees working in NMFCrsquos laboratory

30 RESPONSIBILITES

1) Laboratory workers are required to complete the Environmental Health and Safety (EHS) online trainings and the related equipment training for their experiments

2) Laboratory workers are responsible for planning and conducting all operations in accordance with the Lab Standard Operating Procedures

3) Laboratory worker are capable of recognizing the risk associated with their experiments and addressing them with their supervisor

4) Laboratory workers are required to get approval from the supervisor before conducting experiments in laboratory

40 GENERAL LABORATORY PROCEDURES

1) No-smoking no food or drink in the laboratory2) Horseplay and practical jokes are expressly forbidden3) Confine long hair and loose clothing Wear shoes at all times in the

laboratory Open toed shoes such as Crocs or sandals are not allowed in the laboratory

4) Laboratory workers shall be aware of the location and proper operation of all laboratory safety equipment (ie eyes washes first aid kit fire extinguisher fire alarms)

5) Visitors to the laboratory are to be escorted by an employee and are the responsibility of that employee

6) Lab areas aisles and counter space are to be kept clean


7) Return any item to proper location or where you found them when you are finished

8) Label any and all unattended beakers bottles vials etc even if they just contain water

9) All acid work should be performed in fume hood10) Wear required personal protective equipment (ie safety glasses

safety helmet gloves mask) for specific tasks that may pose potential injury11) If a garbage can is full place it in the hallway to be emptied12) Remove waste from glove box when frac34 full If filled completely it will

not fit in the transfer port13) Minimize the items left in the fume hood to reduce contamination and

leave space available for wet chemistry work to be done14) Manuals for each piece of equipment in the lab are stored in manual

drawer15) Electric wire and socket are not allowed to put on the floor in case of

water flood in the laboratory16) If you notice any items running low write it up on the shopping list17) When you break something write it up on the shopping list18) The signed experimental approval form should be attached 19) Description of experiment risks associated with the experiment and

protection actions to be taken in case of an emergence should be filled in 20) Only well understood reaction are permitted to run unattended in the

laboratory21) The signed experimental approval form should be attached near the

unattended experiment Then other laboratory workers in the lab understand the experimental condition risks associated with the experiment contact person and priority steps to follow in case of an emergence

22) Avoid working alone in the lab If working alone in the lab notify another person in the group when you come to the lab and leave

23) Prior to beginning non-routine tasks involving hazardous chemicals orand experimental equipment that may pose physical hazards during operation procedure Laboratory worker should completely understand the Standard operating procedures (SOP) for these chemicals and experimental equipment An experimental buddy should stand in a safe distance and keep eyes on the laboratory worker when he or she is doing the non-routine tasks The experimental buddy should also know the SOPs of these chemicals and equipment emergency procedures and the personal protective equipment to be used

24) If you are the last to leave performing the following tasksa Check O2 and H2O reading on the glove boxes


b Check the necessary parameters for on-going experiments in the labc Turn off lightsd Lock the lab door

50 CHEMICAL HANDLING STORAGE AND TRANSPORTATION

1) Chemicals should not be smelled tasted or directly contacted with skin2) Wear gloves and lab coat when handling chemicals as they may be

contaminated3) Remove gloves before using the lab computer The chemicals you left on the

keyboard and mouse may hurt next userrsquos fingers4) Clean the counter instrument and other area you may left chemicals on it 5) Any apparatus that may discharge toxic chemicals must be vented outdoors

through the exhausting system located on the laboratory ceiling6) Check the chemical inventory before purchasing any chemical7) Check the proper handling storage disposal procedures of the chemical

before use Those information could be found from its Safety Data Sheet (SDS)

8) All Safety Date Sheets (SDS) received with shipments to the lab shall be maintained on file

9) Check the incompatibility of the chemical from its SDS before use and storage For example concentrated nitric acid reacts violently with acetone (explosive reaction may occur) So do not mix them do not immerse the metal specimen with remaining nitric acid on surface in acetone Those incompatible chemicals should be stored separately in different locations

10) Incompatible chemicals in containers of 20 L or 5 pounds capacity must be segregated At a minimum corrosives flammables and combustibles oxidizers poisons and water reactive chemicals should have their own designated storage areas in the laboratory

11) All chemical containers must have a legible firmly attached label The containers shall be dated when received and also when opened

12) Water reactive amp Pyrophoric chemicals must be stored in accordance with instructions on the label or SDS and separately from all other chemicals regardless of quantity

13) Carcinogens mutagens teratogens and reproductive toxins shall be stored in ventilated storage or a glove box in unbreakable chemically resistant secondary containment

14) Compressed gas cylinders must be stored in the upright position with caps on when not in use


15) Chemicals should not be distributed without approval from PI or supervisor

16) Ensure all chemicals are properly labeled before transporting17) Carts should be used when transporting multiple chemical containers18) The compressed gas cylinder can only be transported with caps in

place and secured to a cylinder cart19) Chemical spills in lab should be cleaned using correct procedures

recommended by the Chemical Spill Clean-up online training in EHS website Laboratory worker should know the location of chemical spill kit in the laboratory and the types of chemical spills that can only be handled by EHS

20) All hazardous chemicals including compressed gas cylinders shall be updated to the chemical inventory on EHS assist system The username to login EHS assist online system is jzhang and the password is NMFC The new hazardous chemicals purchased should be updated to the chemical inventory by EHS assist system You do not need to update the inventory every time you use a portion of the chemical A hardcopy of the chemical inventory shall be stored in the laboratory and renewed annually

60 LABORATORY TRAINING

1) Laboratory worker must complete required training prior to starting work in laboratory

2) Laboratory worker should read and sign the Hazard Communication Program in the laboratory and know who the departmental responsible person is

3) Laboratory worker should read and sign the Chemical Hygiene Plan in the laboratory

4) Laboratory worker should read and sign the NMFC Laboratory Specific Operating Procedures

5) Laboratory worker should complete the Laboratory Standard OSU Building Emergency Action Plan and Chemical Spill Clean-up training on the EHS online system

6) Laboratory worker should know the proper disposal of hazardous waste and how to send a waste pickup request to EHS

7) Laboratory worker should review the specific Standard Operation Procedure included in the Chemical Hygiene Plan

8) Laboratory should complete and sign the operating procedure of specific experimental equipment included in the NMFC Laboratory Operating Procedure

9) All the training records are documented in the laboratory


Appendix 1General Glove box operation1 Changing the compressed gas cylinder

11 Complete ldquoCompressed Gas Cylinderrdquo training from EHS website before manually exchanging gas cylinders

12 To remove current cylinder turn valve on top of tank clockwise to close it13 Using a wrench twist the bolt connecting cylinder to safety valve in an

upward motion to loosen it Continue twisting the bolt until the safety valve is removed Replace protective valve covering on gas cylinder

14 Important Tear off the contents tag on the cylinder to show the tank is ldquoEmptyrdquo

15 To attach new gas cylinder remove protective valve covering and insert the safety valve in the port on top of the cylinder

16 Using a wrench screw the valve bolt in a downward motion to tighten it completely

17 Turn the control valve in top of the cylinder counter-clockwise to open flow from cylinder

18 Tear off the contents tag on the cylinder to show the tank is ldquoIn Userdquo19 The cylinder is now fully attached and ready to use

2 Antechamber controlsThese steps assume the atmosphere in the glove box is purified and not open to the outside air Security Code for glove box controls 799021 Large antechamber

211Inserting an item into the glove box1) Important Verify the antechamber contains purified gas before

opening the inner door2) Ensure the inner door and refill valve are fully closed3) Open the outside door and insert the object into the Antechamber4) Close the outside door and open the vacuum valve and evacuate to -

29 in Hg5) Close the vacuum valve and open the refill valve until pressure

reaches -15 in Hg6) Repeat evacuation and refill at least 3 times finally reaching

atmospheric pressure7) Close the refill valve and open the inner door to remove the object

from the chamber212Removing an item from the glove box


1) Ensure that the outside door and refill valve are fully closed2) Open the inner door3) Insert the object into the Antechamber and close the inner door4) Open the outside door and remove the object5) Purge the antechamber before re-opening the inside door

22 Small antechamber221Inserting an item into the glove box

1) Ensure the inner door and 3-way valve for mini-chamber are fully closed

2) Open the outside door and insert the object into the Antechamber3) Close the outside door and turn 3-way valve to evacuate and

evacuate to -29 in Hg4) Turn the 3-way valve to refill until pressure reaches -15 in Hg5) Repeat evacuation and refill at least 3 times6) Close the 3-way valve and open the inner door to remove the object

from the chamber222Removing item from the glove box

1) Important Verify the antechamber contains purified gas before opening the inner door

2) Ensure that the outside door and 3-way valve are fully closed3) Open the inner door and insert the object4) Close the inner door5) Open the outer door and remove the object6) Purge the antechamber before re-opening the inside door

3 Removing front panel to expose glove box31 Verify that toxic materials will not be present inside of glove box at the

time32 If planning to purge glove box and reset inert Argon atmosphere verify

that at least six (6) full tanks of argon are available for the glove box 33 Close valve on argon tank by turning the valve clockwise34 Turn off power to glove box my pressing switch on front-facing panel

located beneath antechamber35 Raise light fixtures over the top of the glove box Light fixtures rotate along

hinge36 Remove gloves from the front panel by removing the two bands securing

the glove and then pulling off the glove itself


37 While carefully holding onto the front panel open each safety lock sealing the front panel and the glove box IMPORTANT Start at the top work down the sides and finally unlock the bottom

38 Warning Avoid letting the panel edge contact the sealing on front of glove box This may lead to a scratch that prevents the seal from forming when system restarts

39 Be extra careful when removing the front panel from the glove box Set the panel aside

4 Restarting glove box after exposing atmosphere41 Make sure at least 6 full argon tanks are on hand to purge and refill the

glove box42 Verify that all seals are secured on front panels each antechamber door is

tightly closed exhaust system is functioning and cooling system is functioning (if applicable)

43 Note If a front panel was removed from the glove box at any point clean the seal with rubbing alcohol and apply high vacuum grease

44 Turn on argon feed to the glove box by turning the top valve clockwise45 Turn on glove box power using the switch located on the front panel

beneath the antechambers46 Perform a pressure check on the glove box (see section 50)47 (step 5-8 is the purging method for the antechamber) Set the Working

Maximum pressure to +100 mbar and the Working Minimum Pressure to +50 mbar To do this press the System Config button and adjust the numeric values with the blue display The working gas will enter the box automatically

48 Turn on the vacuum pump by pressing the Start button on the main screen

49 Open the evacuate valve on the Large Antechamber and allow the chamber to evacuate to evacuate to -30

410 Close the evacuate valve and repeat for the mini antechamber411 Wait 10 minutes for the glovebox to stabilize412 Use the appropriate foot pedal to addremove gas tofrom the glovebox to

reach desired pressure413 Important See section 50 to perform a pressure test on the glove box and

verify that all seals are secured414 It is extremely important to purge the glove box to displace as much air in

the box as possible with inert gas Important Purging the glovebox requires 3 full cylinders of working gas (6 cylinders for large glove box) Follow the steps in section 40 to purge the system

5 Purging the glove box


51 Purging the glove box requires 3 full cylinders of working gas (6 cylinders for large glove box) Verify sufficient cylinders are in inventory (lab and 1st floor garage)

52 Set Working Maximum pressure to +100 mbar and the Working Minimum Pressure to +50 mbar (see section 30)

53 Open the manual purge valve located on the back panel of the glove box beneath the antechambers

54 Adjust the flow using the purge valve so that there is a steady flow of incoming gas and the box pressure is maintained at gt1 mbar

55 Create turbulence in the box to increase purge efficiency This can be done by pressing in the gloves or using an electric fan or vacuum inside the glove box

56 As the working gas cylinder empties close the purge valve and change the cylinder Open the valve on the cylinder and then re-open the purge valve

57 Purge the system with the required number of cylinders or until Oxygen content is 25 ppm or less Then close the manual purge valve

58 The oxygen content might increase once the blower has been turned on (Main Screen -gt Blower Control) If oxygen level rises above 100 ppm stop the blower and continue to purge

59 Important When Oxygen level is sufficiently low briefly turn on the blower to circulate atmosphere through the blower line Do not leave blower running this will drastically reduce the lifetime of the oxygen removal system and the blower

510 The blower system circulates the atmosphere through the purification system It can be set to low speed during weighing or set to high speed to recover from operator error

511 Set the blower to 50 during normal operation (100 = full blower speed)6 Performing a pressure test (check seal quality)

61 Perform a pressure test anytime the front panel of the glove box is removed and replaced A pressure test should also be performed periodically for safety and quality assurance

62 Close purge valve located on back of glove box panel beneath antechamber

63 Turn compressed cylinder on by rotating the valve on top of the cylinder counter-clockwise

64 Set Maximum Working pressure to 120 mbar and the Minimum Working pressure to 100 mbar

65 Allow 10 minutes for the glovebox to stabilize at 110 mbar Use the foot pedals to finely adjust the pressure


66 Watch the current pressure in the glove box carefully for 25 minutes If the pressure fluctuates more than 1 mbar the system is not secured Troubleshoot the sealsconnections or contact Innovative Technology Inc


LAB SPECIFIC OPERATION TRAINING RECORD

Title of lab operating procedure RevisionGeneral Glove box operation 00

TRAINEE INFORMATIONName Signature Date


Appendix 2 Kerr Auto Electro-Melt Furnace1 Starting the furnace

11 Before use make sure that all equipment materials etc are at least 18rdquo away from the furnace to protect them from heat

12 Make sure that furnace is clean and free of debris containing only desired experimental materials

13 Turn on the switch located on the front panel of the furnace The display will read

14 ldquoAtr 142rdquo while it performs a self-test 15 Once the display reads ldquoAtr 142rdquo the furnace will begin heating up to the

set temperature point2 Starting furnace to desired temperature

21 Note The temperature controller has a very high overshoot For best results set temperature to about 23 of the desired temperature and increase set point periodically

22 To set the temperature use the up and down arrow keys located next to the display on the front panel

3 Cleaning furnace31 Open the furnace and give the furnace sufficient time to cool depending on

the temperature at which it operated32 Let the graphite crucible sufficiently cool so that it can be handled directly33 Remove the crucible from the furnace and pour entire contents into

sealable waste container inside glove box34 Inspect the graphite crucible inside and outside for defects contamination

or debris35 Replace the graphite crucible inside the glove box

4 Warning41 Turn on chiller when operating furnace in glovebox42 Never allow the glovebox to exceed 110degF This will degrade the seals on

the glovebox requiring costly repair and delaying experimental work for several weeks If 110degF is reached in the glovebox shut off all furnaces immediately

43 If an operating furnace will be unattended for prolonged periods of time (eg overnight early morning or late evening operation) plug it into a thermostat Kerr furnace controllers can lose their integrity resulting in rapid heating of the furnace and therefore the glovebox Never leave a furnace unattended unless it is plug into a thermostat


44 Never remove the lid from a furnace when hot unless absolutely necessary This causes hot surface to be exposed and the temperature to spike in the glovebox

45 When cool remove your items from the furnace and clear the surrounding area for the next person to use the furnace



Title of lab operating procedure RevisionKerr Auto Electro-Melt Furnace 00



Appendix 3 Gamry Interface 10001 See Userrsquos manual (available online)2 Only some of the leads need to be used in most cases For normal operation

only the blue green white and red need to be connected to the electrodes as shown below21 For 3-electrode setup

22 For 2-electrode setup



Title of lab operating procedure RevisionGamry Interface 1000 00



Appendix 4 High-Temperature Electrochemical Cell1 Install the working electrode reference electrode and counter electrode2 Starting the furnace3 Setting furnace to desired temperature4 Connecting potentiostat with experiment

41 Before connecting make sure furnace is off and is at room temperature42 Make sure working electrode and reference electrode is clipped by alligator

clip and small binder clip and is not touching the bottom of the crucible43 Hook up the alligator clips from the potentiostat with the electrodes The

corresponding color are listed in table below

5 Perform electrochemical measurements51 Immerse the working electrode in the molten salt52 Turn on the potentiostat and turn on the Gamry software in the lab

computer53 Perform desired electrochemical measurements

6 Stop the test61 Turn off the furnace62 Allow system to cool to room temperature before handingdisconnecting

electrode leads7 Clean the furnace



Title of lab operating procedure RevisionHigh-Temperature Electrochemical Cell 00



Appendix 5 High-Temperature High-Pressure corrosion cracking system1 Introduction

The purpose of the High Temperature amp Pressure Corrosion Cracking System is to develop control and measure stress corrosion cracks under well-defined material and environmental conditions and ensure that the crack growth rate (CGR) response is reproducible and characteristic of the test conditions The system simulates light water reactor (LWR) environments up to 350 degC at 2500 psi Features expected in a good crack-growth system include active constant K load control active temperature control a sensitive crack length measurement apparatus a flowing high temperature water system control over all aspects of water chemistry and continuous monitoring of all pertinent tests parameters The Student Training Plan aims to train intended users to acquire all the technical knowledge and safety concerns to independently operate on the system

2 Points of contactThe system belongs to The Center for Nuclear Materials and Fuel Cycle Research of The Ohio State University It is located at Scott Lab W396 201 W 19th Ave Columbus OH

3 System componentsThe key components of the system include (1) A servo-electric load control system capable of holding constant load for very long periods of time (2) A high pressure piston pump to pressurize and flow water through the high temperature loop (3) An autoclave to sustain samples and solution for experiments (4) A custom-made water board for precise water chemistry control (5) A reversing DCPD system for crack length estimation (6) A continuous data acquisition system31 Servo-electric load control system

The Interactive Instruments Model 5K Servo Creep Controller is a fully programmable electromechanical load controller system which capable of controlling tensile loads to 5000 lbs continuous over the 325 inch stroke for long periods of time The control panel can be manually or remotely configured to control the load stroke or strain control point in real-time A built-in waveform generator can be programmed to cycle or ramp the control point for hours days or even months for unattended testing The system includes the software to remote control and record the loading dataThe procedures to load must refer to the manual thatrsquos placed on the shelf near the system

32 High pressure piston pump


The Pulsafeeder Model 7440 Hydraulic Diaphragm Metering Pump is to precise metering and long-term reliably stroking It consists of a three-phase powered motor and a liquid end separated by the hydraulically operated diaphragm A pulse dampener which requires sufficient volume a gas charge of 60 of the operating pressure and a short liquid path to the pulse dampener is used to eliminate almost all pressure pulsing associated with the pump The pressure gauge of nitrogen cylinder is to control the stabilizing pressure on target Pump oil must be changed after a period of time The first oil change should be done after 6 months of continuous operation and them every 12 months for normal service and every 6 months for severe service The procedures to change oil can be found on the manual the pump [1]

33 AutoclaveThe HiP Model 802858 4-Liter Autoclave is made of SS316 to sustain samples and high temperature amp pressure solution for experiments The autoclave contains eight sealing threads and one sealing gasket 206964 The gasket must be replaced once any defect was found or any leaking occurred during high pressure operation if the right procedures have been followed

34 Water boardFigure 5-1 is the water flow diagram displaying the components and flow direction After passing through the autoclave and heat exchanger system the water in the loop operates as usual in a closed loop where the autoclave effluent is continuously demineralized and re-equilibrated for dissolved gases in the glass column The impurities are added to the glass column from the 10 liters impurity reservoir with a metering pump at a fixed flow-rate or controlled by the conductivity meter and signal transmitter Buffered chemistries are created by a pre-conditioning mixed bed demineralizer (full-flow demineralization) to the target chemistry BLi chemistries tend to drift in composition because the Fe2+ is the most common impurity in hydrogenated water and the demineralizer releases H+ and Li+ as it absorbs Fe2+ The system can compensate for the rise in Li+

level versus time Two 140 microns filters are connected in the water loop to filter out the large molecular diameter particles More concentrated chemistries can also be used but then full flow (demineralized) cleanup of trace impurities is not possible thus the more concentrated chemistries will not be easily tried


P

7- flo

w me

ter

19- Transm itter

6-Sensor

Filter

11-P ump

15-P ump

10- Rese rvior

4-BP R

cooling water return

cooling water supply

Fromhigh pr essurepump

Tohigh pr essure pump

To autoclave 3

2-Rup ture disk

3 3

6-Sensor

8- Dem i

5

9-Fil ter

17

1818

13-Co lumn

14-E nd plateP 1

16

Figure 5-1 Water flow diagram of the system (include water board) 1- digital pressure gauge 2- safety head for rupture disk 3- removable filter 4- back

pressure regulator 4000 psi 5- 100 psi pressure gauge 6- digital conductivity sensor 7- flow meter 8- cartridge 9- fiber filter 10- 10-Liter reservoir 11- Q

pump 13- glass column 14- stainless steel plate 15- micropump 16- gas tubing 17- 1 psi check valves 18- 10 psi check valve 19- conductivity sensor

transmitter

35 Reversing DCPD systemHigh-resolution direct current potential drop (DCPD) is used to measure crack length in-situ and enable interactive control of loading conditions


Figure 5-2 Schematic of DCPD system

36 Data acquisition systemThe computer receives the data from water board conductivity sensors load control system and DCPD system Received data include temperature influent and effluent conductivity loading frequency location and force DCPD current timedata etc

4 Standard Operating ProcedureThe following procedures show the methods to make the system operate at 300 degC and 2000 psi for corrosion cracking experiments

1) Exam all the connections are well-connected and sealed (Note if any connection leaked during the operation stop the test immediately and drain all the solution out of the loop The system cannot be operated at high temperature or pressure until the leaking is solved)

2) Install the samples and connect the DCPD cables3) The way to seal the autoclave i) lift the autoclave with crane and place

on the bottom plate ii) match the holes of the autoclave body with the threads of bottom plate iii) install the 8 autoclave threads and tight with fingers iv) use the electronic torque wrench to tight the threads to 30 ft-lb 60 ft-lb 90 ft-lb till 110 ft-lb at the final

4) Open the valves for solution flow and close the valves for draining5) Record the readings of pressure gauges and the flow meter6) Inject ultra-pure water till the water level of glass column reaches the top7) Close the injection valve8) Turn on the powers of pump and micropump9) The loop flow rate can be adjusted by the stroke of pump10) Slowly increase the loop pressure by turning the back pressure

regulator (clockwise) and observe the reading of loop pressure regulator At the same time adjust the pressure regulator of compressed nitrogen cylinder to make the discharge solution and the gas balance in the pressure dampener

11) Once the reading of loop pressure regulator reaches 2000 psi stop the last step

12) Turn on the power of heater Set the target temperature at 300 degC and wait it to heat

13) Wrap the insulation cover on the heating mantle14) Once the temperature reaches 300 degC record the readings of pressure

regulators and the flow meter15) Turn on the data acquisition system to receive readings


16) Turn on the load control system for loading and save the loading data by the software

17) The chemistries can be injected into the loop by manually controlling or automatically releasing through the Q-pump and conductivity sensors The injection depends on the objective of the experiment

18) Exam the system daily to make sure itrsquos sealed and recorded19) At the end of tests turn off the powers of pump and micropump close

the valve of nitrogen cylinder and open the needle valve under the nitrogen pressure gauge to relieve the residual gas

20) Thoroughly open the back pressure regulator (anti-clockwise turn)21) Save the data and quit the data acquisitions Disconnect the cables

from data acquisitions and samples and make them well-keep 22) Open the needle valve of autoclave and pump to drain the solution 23) Release the 8 threads of autoclave and life the autoclave with crane 24) Uninstall the samples and well-keep the autoclave inner components25) If chemistries were added during the experiment rinse the loop with DI

water for couple of days till the reading of digital conductivity sensor reduces to the conductivity of ultra-pure water ie below 18 MΩ-cm

5 References[1] PULSA Series diaphragm metering pumps installation operation maintenance instruction



Title of lab operating procedure RevisionHigh-Temperature High-Pressure corrosion cracking system 00



Appendix 6 High-Temperature High-Pressure flow loop1 Equipment and supplies

11GeneralA flowing autoclave loop has been designed and used to conduct material corrosion and leaching tests The loop was designed in house and fabricated by Swagelok This document is aimed to provide detailed description of the loop and comprehensive guidance of the test procedure

12PampIDThe PampID of the flowing autoclave is shown in Figure 6-1 A picture of the flowing autoclave system is shown in Figure 6-2

Figure 6-1 PampID of the flowing autoclave system (in Mode 1)


Figure 6-2 Picture of the flowing autoclave system

13EquipmentTable 6-1 Flowing autoclave loop Equipment list from OSU

Name Description Manufacturer Model A1 Autoclave 8 Dia 5 Gal 2 Tri Clover Input 1 NPT

Male Output 316LApache NA (Custom)

CA1

Compressed Air Supply

Building Gas Supply NA NA

FD Flow Diverter 6 Dia 12 Tall 125 semi-eliptoide base 304L

OSU Machine Shop

NA (Custom)

HC1

Heating Coil 1 Tubing Coil Swagelok NA (Custom)

HE1

Heat Exchanger Stainless Steel 16-38 x 4-316 Head Diameter

McMaster-Carr

35185K999

HE2

Upstream Sample Cooler

Square Coiled Tube 2 dia 1 spacing 3 4 OL

NA NA (Custom)

LI Level Indicator PFA Tubing 14 x 0062 Wall Swagelok NA (Custom)PR1

TK1 Pressure Regulator

Building Built-in-Regulator OSU NA

PR2

A1 Pressure Regulator


T1 TK 1 Thermocouple Copper-Constantan SS Sheath 18 Dia 12 long

Omega Engineering

TJ36-CPSS-18U-12-SB-SMPW-M

T2 Loop Thermocouple K Type Thermocouple SMP Male Omega Engineering

SA1XL-K-72-SRTC

T3 A1 Thermocouple Copper-Constantan SS Sheath 18 Dia 6 long

Omega Engineering



T4 LabView A1 Thermocouple

Copper-Constantan SS Sheath 18 Dia 6 long

Omega Engineering


T5 UFM Thermocouple Self-adhesive T Type Thermocouple 80 molded SMP male

Omega Engineering

SA1XL-T-72

T6 Downstream Loop Cooler

Self-adhesive T Type Thermocouple 80 molded SMP male

Omega Engineering

SA1XL-T-72

T7 Upstream TV1 Self-adhesive T Type Thermocouple 80 molded SMP male

Omega Engineering

SA1XL-T-72

T8 Downstream TK1 Self-adhesive T Type Thermocouple 80 molded SMP male

Omega Engineering

SA1XL-T-72

TK1

Water Storage Tank 12 Dia 10 Gal 1 NPT Male Input 1 NPT Male Output 316L

Apache NA (Custom)

UFM

Ultrasonic Flow Meter Ultrasonic In-line Flow Meter 01-20 ms Micronics PF 330

VSP1

High Flow Variable Speed Pump

1 14 Input 1 14 Output 304 gpm Grundfos CRN 5-9 A-P-G-V-HQQV

VSP2

Low Flow Variable Speed Pump

38 Input 38 Output Fluid Metering Inc

QG400 Q2CSC

NA Pipe Insulation Fiberglass McMaster-Carr

NA

NA Heat Tape 05 x 16 1248W HTS Amptek AWH-052-160D

Table 2 Flowing autoclave loop Equipment list from SwagelokEquip

Name Description Model

CV2 VSP 2 Discharge Check Valve

CHECK VALVE 1PSIG 38 SS-CHS6-1

CV3 TK1 Check Valve CHECK VALVE 1PSIG 1 SS-CHS16-10CV5 FM3 Check Valve CHECK VALVE 1PSIG 38 SS-CHS6-1CV6 HE2 Check Valve CHECK VALVE 1PSIG 34 SS-CHS12-1HC1 Heating Coil Swagelok 1 Tubing Coil NA (Custom)HE3 Downstream Loop Cooler Swagelok Coiled Tube 2 dia 1

spacing 3 4 OLNA

P1 VSP 1 Suction Pressure Gauge

GAUGE 0-100 PSIG PGI-63C-PG100-CBGX-G



P3 VSP 1 Discharge Pressure Gauge




P5 TK 1 Pressure Gauge GAUGE 0-100 PSIG PGI-63C-PG100-CBGX-G

P6 A1 Pressure Gauge GAUGE 0-100 PSIG PGI-63C-PG100-CBGX-G

P7 UFM Upstream Pressure Gauge


P8 UFM Downstream Pressure Gauge


RV1 TK 1 Pressure Relief Valve RELIEF VALVE 14 75 PSIG SS-RL3S4RV2 A1 Pressure Relief Valve RELIEF VALVE 14 95 PSIG SS-RL3S4TV1 A1 Bypass Throttle Valve NEEDLE VALVE WITH REGULATING TIP

1SS-12NRS16

TV2 Upstream GSL NEEDLE VALVE 14 SS-1RS4-ATV3 Downstream GSL NEEDLE VALVE 14 SS-1RS4-A


3V1 TK1 SupplyBypass Valve 3-WAY BALL VALVE 1 SS-65XTS16-F163V2 VSP SupplyBypass Valve 3-WAY BALL VALVE 1 SS-65XTS16-F163V3 Flow Meter SupplyBypass

Valve3-WAY BALL VALVE 1 SS-65XTS16-F16

3V4 HE1 SupplyBypass Valve 3-WAY BALL VALVE 1 SS-65XTS16-F16V1 TK1 Air Supply Valve 2 WAY BALL VLV 14 SS-43GS4V2 HE1 Isolation Valve 2 WAY BALL VLV 14 SS-43GS4V4 A1 Air Supply Valve 2 WAY BALL VLV 14 SS-43GS4V5 A1 Supply Valve 2 WAY BALL VLV 14 SS-43GS4V6 System Drain Valve 3-piece 60 Series Ball Valve 1 SS-65TF16V7 A1 Discharge Isolation

Valve2 WAY BALL VLV 14 SS-43GS4

V8 VSP 1 Downstream valve 3-piece 60 Series Ball Valve 1 SS-65TF16V9 FM2 Downstream valve 3-piece 60 Series Ball Valve 1 SS-65TF16V V1 TK1 Vent Valve PURGE VALVE 14 SS-4P-4TV V2 A1 Vent Valve PURGE VALVE 14 SS-4P-4T

14Supplies1) Fisherbrand polypropylene rectangular carboys2) Labware3) Nitrile gloves4) High temperature protection gloves5) Protective eyewear6) Masks7) Safety hats8) Lab coats9) Ice bucket10) Safety hats

15Automation system


An automation system was designed and built for data acquisition and system control on the flowing autoclave loop The data acquisition system is aimed to monitor and store the system parameters including the temperature and flow rate The thermocouples and flow meters are used to measure the system temperature and flow rates The output signals from the thermocouples and flow meters were received by the thermocouple module and current input module respectively A customized LabView configuration was programmed to process these signals and the temperature and flow rate information can be monitored on the computer In addition to the data acquisition system the automation system was also designed to control the system temperature which serves to protect the heat tapes from overheated and maintaining the solution temperature during tests The heat tapes were used to heat up the solution in the flowing autoclave loop Each heat tape was deployed with a k-type thermocouple a stand-alone temperature controller and a contactor A high temperature limit was pre-set on the temperature controller that monitors the temperature on an individual heat tape Once the heat tape is overheated and the temperature exceeds the limit the temperature controller gives out signals to the corresponding contactor and switches off the electrical circuit for providing power to the heat tape The autoclave (A1) and water tank (TK1) was deployed with thermocouples (T1 and T3) which were used to measure the solution temperature in the two vessels Similarly a stand-alone temperature controller and a contactor was used to maintain the solution at the target temperature A full list of the automation system components are summarized in Table 6-3 The junction box and data acquisition system are shown in Figure 6-3

Table 6-3 Automation system component listComponents Vendor Model NumberThermocouples Modules

NI NI9213

Modules Chassis NI NI9174Current Input Modules NI NI9203Temperature Controllers

Auber Instruments

syl-2362

Contactor Honeywell db2040b-1002

T-type Thermocouple Wires

Omega EXPP-T-20-TWSH-SLE-100

K-type Thermocouple Wires

Omega EXPP-K-20-TWSH-SLE-500

K-type TC Connectors Omega UST-K-FT-type TC Connectors Omega USTW-T-FElectrical Wires McMaster Carr Different AWGs


Figure 6-3 Junction box and data acquisition system

2 Operation modesThe four primary Modes of Operation of the OSU test loop are as defined below1) Pre-heat mode

Heat the system and test solution to the desired test temperature2) Solution transferring mode

Transfer of fluid heated in Mode 1 to Autoclave Test configuration Mode 23) Test operation mode

Operate the system under the required test experimental design conditions4) Cool down and sample removal mode

Cool the system solution in preparation for sample removal21Pre-heat mode

It is necessary to raise the temperature and pressure of the water solution to the desired conditions before running the corrosion tests since the water solution with deviating conditions may introduce uncertainties to the results The PampID of the loop during the pre-heat mode is shown in Figure 6-4 Approximately 45 L of the water solution are circulated through the flow path using the high flow pump (VSP1) In the meantime the heat tape that is wrapped on the tube coils will be used to heat the solution in the flow path Compressed air will be introduced into the water tank and autoclave from the instrumentation port to pressurize the loop which is aimed to maintain the water solution subcooled in the loop


Figure 6-4 Flow path in the pre-heat mode (Mode 1)

22Solution transferring modeThis mode is aimed to transfer the solution at target temperature from the water tank to the autoclave for corrosion tests Therefore the corrosion samples can be exposed to the solution at target temperature After the solution transferring mode is complete the water level should be equal to the instrumentation port and the water tank should be bypassed from flow recirculation

23Test operation modeThis flow autoclave loop is used to perform corrosion tests with controlled velocities According to the design inputs tests with different velocities will be conducted For the tests with velocities greater than 005 fts the high flow pump (VSP1) and ultrasonic flow meter (UFM) are used For the tests with velocities lower than 001 fts the low flow pump (VSP2) is used The flow paths for both two velocity tests are shown in Figure 6-5 and Figure 6-6


Figure 6-5 Flow path in the test operation mode (greater than 005 fts)


Figure 6-6 Flow path in the test operation mode (lower than 001 fts)

During the tests ICP samples need to be taken at different time instants Upstream and downstream grab sample line (upstream and downstream GSL) will be separately opened and for collecting ICP samples by adjusting the needle valves

24Cool down and sample removal modeAfter a test is finished the metal sample needs to be pulled out in a relatively short time (typically several minutes) to prevent any further undesired corrosion The flowing autoclave loop needs to be depressurized and sufficiently cooled down to touchable temperature before opening the autoclave and retrieving the metal samples The flow path for the cool down and sample removal mode is shown in Figure 7 The high flow pump VSP1 will be used to recirculate the flow in the loop The loop cooler HE1 will be used to cool down by chilled water provided by the lab In the meantime the bleed valve on the autoclave VV2 is cracked to depressurize the loop The metal samples can be retrieved once the system pressure is atmospheric and the temperature of the solution is touchable


Figure 6-7 Flow path in the cool down and sample removal mode (Mode 4)

3 Pre-test preparationThe following activities should be completed prior to starting the test Verify all necessary supplies (DI water cold air and power supplies) are

available Verify inventory of all chemicals corrosion coupons etc to be used in the

test Verify pH meter is working properly Check the temperature of the hotplate with a calibrated thermometer31 pH calibration

1) Collect 1 L of DI watera Use 500 mL graduated cylinderb Press and hold large dark blue switch on top of the DI water supply to

dispense waterc Check the electrical resistivity of DI water and make sure it is higher

than 175 MΩcm


2) Calibrate analytical balance -- Internal adjustment (see the manual of your balance fordetailed instruction if necessary)a Allow scale to warm up for 1 hour if it was powered offb Remove anything on the balance and use brush to clean the scalec Press and hold weight symbol until you see ldquoADJ INTrdquo d When the scale reads ldquoADJ DONErdquo the internal calibration is completee Check if internal calibration is correct by placing 100 g weight on scale

i If scale does not read 1000000 with plusmn00001 g make sure scale is clean and try an internal calibration again

ii If scale does not read 1000000 within plusmn00001 g then externally calibrate according to Mettler Toledo procedure using 100 g weight

3) Calibrate pH meter before every test (see the manual of your pH meter for more detailed instruction if necessary)f Preparation

i Wash three 100 ml beakers using tap water and soapii Rinse beakers with DI wateriii Dry using Kimwipes

g Calibration of ATC pH probei Pour 50 ml pH = 401 700 and 1001 standards into three

beakers respectively and label the date and person (pH standard solutions should be replaced every month)

ii Turn on the pH meter and hook up the ATC probeiii Loose the black cap before pulling the pH probe out from the

bottleiv Rinse the pH probe with DI water and dry it with Kimwipes Blot

do not rub as this may create staticv Place the ATC pH probe in the pH = 7 standard solution vi Press ldquoCALrdquo and the meter will show ldquoCArdquo (This is the only time

to press CAL in the entire calibration process)vii Keep stirring the standard solution and wait until the pH meter

reads a constant number for at least 2 minutesviii Press ldquoENTERrdquo button to confirm calibration pointix Rinse the probe with DI water and dry it with Kimwipesx Place the probe in the pH = 1001 standard solution xi Keep stirring the standard solution and wait until the pH meter

reads a constant number for at least 2 minutes


xii Press ldquoENTERrdquo button to confirm calibration pointxiii Rinse the probe with DI water and dry it with Kimwipesxiv Place the probe in the pH = 401 standard solution xv Keep stirring the standard solution and wait until the pH meter

reads a constant number for at least 2 minutesxvi Press ldquoENTERrdquo button to confirm calibration point

h Verify the calibrationi Check all the standard solution points with the calibrated probe

rinse the probe with DI water and dry it with Kimwipes place the probe in the pH = 7 standard and stir repeat these two steps with pH = 1001 and 401 standards

ii In the test log record the actual pH readings of three standards from the pH meter include the operatorrsquos name date and time and actual pH readings

iii If any of the three readings is off by more than 003 the calibration needs to start over

iv If with recalibrating the solution pH still differs by more than 01 see troubleshooting guide in Appendix B

i Clean upi Rinse the probe with DI water and dry it with Kimwipesii Insert the probe into the black cap before screw the cap back

onto the bottle (make sure the tip of the probe immersed in the storage solution but does not touch the bottle)

iii Wash all the glassware with tap water and soapiv Rinse them with DI water and dry themv Seal the three standards with parafilm Reminder Standards

must be replaced monthly32Samples preparation

All the samples are cut by the machine shop The detailed dimension information can be found in the sample holder design document [1]

Before putting the samples into the sample holders

a Carve 1 cm mark on the corner of every sample when samples are loaded this corner should point towards test column center and upwards direction

b All the samples need to be labeled and weighed using the scale and the total weight needs to be recorded on the log book

c Pictures of the samples before and after tests need to be taken for all the samples for record and save them in the computer


321 Test with a test column as the test section

1) Loosen the six screws on the top cap of the low velocity sample holder with a 564rdquo allen wrench

2) Insert six coupon samples in the grooves

3) Put the top cap back on and tighten the screws

4) Loosen the six screws on the end cap of the sample holder

5) Insert the sample holder into the test column

6) Stack four sample holder bodies and connect them with dowel pins

7) Tighten the top cap using screws with a 564rdquo allen wrench

8) Align the thread holes on the end cap with the holes at the bottom of the test column

9) Insert the screws from the bottom of the test column and tighten them

The sample holder without and with samples loaded is shown in Figure 6-8


(a) (b) (c) (d)Figure 6-8 a) Four sample holders without samples b) Test column c) Four sample

holders with sample loaded d) Entire assembly

4 Test procedureThe four primary modes of operation of the OSU flowing autoclave loop are as defined below

Mode 1 Pre-heat mode (Figure 6-4)

o Purpose Heat the system and test solution to the desired test temperature


Mode 2 Solution transferring mode (Initial valve positions referred to Figure 6-4)

o Purpose Transfer of fluid heated in Mode 1 to autoclave for test configuration in Mode 3

Mode 3 Test mode (Figure 6-5 and Figure 6-6)

o Purpose Operate the system under the required test experimental design conditions

Mode 4 Cool down and sample removal mode (Figure 6-7)

o Purpose Cool the system solution in preparation for sample removal

Before running the tests the date time test operator test name test contents (samples solutions duration purpose etc) should be recorded on a log book

Table 6-6 Initial system alignment

Component

Initial set point Purpose

TK1 On-lineFluid storage during system heat-up Allow for fluid expansion Provides system overpressure to keep fluid sub-cooled and NPSHa as needed

CA1 with PR1 35 PSIG Provide system overpressure via TK1

CA1 with PR2 35 PSIG Provide system overpressure via A1V1 Open Air supply to TK1V4 Open Air supply to A1

V V1 Closed TK1 Bleed ValveRV1 60 PSIG TK1 Pressure Relief Valve3V2 Aligned to

VSP1 Supply to VSP1VSP2VSP1 Stop Recirculate Solution through heat-up loopV8 Open Allow flow through VSP1

VSP2 Isolated Pump flow for tests with 001 fts velocityV2 Closed HE1 Isolation ValveV3 Closed Sample Valve HE1 ventTV1 Open A1 Bypass ValveTV2 Closed Upstream GSL need valveTV3 Closed Downstream GSL need valveV5 Closed A1 Supply ValveA1 Isolated Autoclave

V V2 Closed A1 Vent ValveRV2 75 PSIG A1 Pressure Relief Valve3V3 Aligned to V9 Supply to UFMV6 Closed System Drain


V7 Closed A1 Discharge IsolationV9 Open valve3V4 Aligned to

System HE1 supply IsolationHE1 Isolated Loop Cooler3V1 Aligned to TK1 TK1 Pump Supply Valve

41Mode 1 Pre-heat and pressurization mode1) System preparation

a Adjust the valve positions shown in Figure 6-4 3V1- To water tank 3V2 ndash High flow pump 3V3 ndash High flow meter 3V4 ndash Flow thru V5 and V7 ndash Off TV1 ndash Fully open (counter-clockwise all the way)

b Pour all the 40 L solutions in the water tank with a 4 L clean plastic beaker

c Start VSP1 ldquoHIGH FLOW PUMPrdquo at 30 Hz to mix the flow for 10 minutes d Cover the water tank with the lid and make sure the lid and gasket are

well alignede Seal the water tank with the clamp and tighten the bolts (2 on one side

and 1 on the other side) with a 38rdquo allen wrench and an adjustable wrench There are two nuts for each bolt The smaller nut goes inside and the larger one goes outside Tighten all three sets of bolts and nuts back and forth to make sure all of them are tight


Figure 6-9 Smaller and larger nuts securing the water tank clamp

f Install the sample holderi) Tests using the test column connect the flange of the test column

with flow diverter and the flange underneath the lid with four 58rdquo bolts and nuts connect the plastic hose with the stainless steel tube for downstream grab sample line

ii) Tests using the autoclave slide the autoclave sample holder assembly to the bottom of the autoclave

g Cover the autoclave with the lid and make sure the lid and gasket are well aligned

h Seal the autoclave with the clamp and tighten the bolt with an adjustable wrench

2) System pressurizationa Pressurize the autoclave and water tank by turning on V1 and V4 until

the reading of P5 and P6 reaches 25 psi then turn V1 and V4 off (PR1 and PR2 not used)

Smaller nutsLarger nuts


b Wait for 10 minutes and check the readings on P5 and P6 to see if the pressure drops due to leakage

i) if no move forward to further flow mixingii) if P5 reading drops depressurize the water tank by fully opening the

VV1 loosen the bolt and nut on the lid to take the lid off realign the lid and then repeat step e and f in System Preparation repeat step a and b in System pressurization to check if the leakage still exists

iii) if P6 reading drops depressurize the autoclave by fully opening the VV2 loosen the bolts and nuts on the lid to take the lid off repeat step a and b in System Pressurization until no more leakage is found

3) Further flow mixing this step serves to further mix the solutions with the VSP1 ldquoHIGH FLOW PUMPrdquoa Switch on the DC power supply for the flow meters the digital display

on the flow meters should be on (Figure 6-10)

Figure 6-10 Power supply box and VFD for VSP1 ldquoHIGH FLOW PUMPrdquo

b Open the LabView file named ldquoAutoclave control1rdquo on the computer (ZHANG-W396-04) click ldquoRunrdquo and the front panel is shown as the screenshot below in Figure 6-11


Figure 6-11 Screenshot of the front panel of the DAQ system

c Switch on the electrical box for the pump and press ldquoRunrdquo on the variable frequency drive (VFD) Increase the pump frequency to 45 Hz by pressing the up arrow on the VFD

Personnel performing the procedures listed below need to wear the high temperature proof gloves

4) Pre-heating a Tune down the water tank pressure to 10 psib Plug in the Junction box and the digital display on the temperature

controllers should be on as shown in Figure (HT2-HT6 are the heat tapes on the tube coil which are preset to be 240 C AUTO SOL and HT1 are the autoclave solution temperature and heat tape wrapped around the autoclave which should be set to the target temperature of specific tests) Please find the temperature controller manual in ref [2]

c Switch on power supply for the heat tape in Figure 6-12


Figure 6-12 Power supply box for the heat tapes

d Monitor the solution temperature in the water tank (T3) on the front panel of the DAQ system shown in Figure 6-11

e When the T3 temperature is 3 0C higher than the target temperature tune down the HT2-HT6 temperature to 200 0C

f Move on to Mode 2


Figure 6-13 Junction box picture

42Mode 2 Solution transferring mode Mode 2 needs to be finished in a fast manner typically within 8 minutes so as to keep the temperature on target 3 persons are needed to operate one controls the VSP1 ldquoHIGH FLOW PUMPrdquo while the second one controls the valve positions and takes baseline ICP and the last one takes lab notes The initial valve positions for Mode 2 should be referred back to Figure 6-4

a Person 1 fully open V5 and V7

b Person 2 dial down the pump frequency to 25 Hz

c Person 1 Take baseline ICP Person 1 opens V2 clears 30 mL liquid and then takes 30 mL ICP sample using a 30 mL sample bottle


d Person 1 cracks the bleed valve on the water tank (VV2) Person 1 and 2 need to adjust the opening extent of VV2 and compressed air For 100 0C T3 = 40 psi for 115 0C T3 = 55 psi for 130 0C T3 = 70-75 psi

e At the moment that liquid water comes out from VV2 (the level indicator (Figure 6-14) that hooks with the outlet of VV2) close VV2 Open the needle valve on the upstream GSL until solution comes out for 15 seconds (purging air bubbles in the solution)

Figure 6-14 Level indicator

f Check the water level through the level indicator if the water level is below the instrumentation port repeat steps b and c

g Person 1 opens TV2 and collects liquid with a beaker until continuous liquid (for 100 0C tests) or flashing flow (for 115 or 130 0C) comes out from upstream GSL

h Person 1 bypasses TK1 by switching 3V1 to ldquoflow thrurdquo and depressurizes the TK1 pressure to be 25 psi by opening VV1

i Crack VV2 until no solution comes out


j Minimize the opening of VV2 direct the hose with VV2 to a beaker with water maintain the bubbling rate in the water to be approximately 1 bubblesecond keep the A1 pressure as stated in step c by adjusting the PR2

k Person 3 records all the activities and timing on the test log

43Mode 3 Test mode1) Loop preparation

a Pipe sample holder test for greater than 005 fts (Figure 6-5)b Turn on the large flow pump VSP1 ldquoHIGH FLOW PUMPrdquo adjust the

pump frequency with the VFD until the UFM reads at the target flow rate (214 gpm for 05 fts 042 gpm for 01 fts 021 gpm for 005 fts)

2) Actual test runninga Record the time that test startsb Keep V9 open c Grab solution sample from upstream and downstream GSL for ICP tests

at different time instants (30 mins 1 hr 2 hrs 4 hrs 8hrs and 24 hrs)i Take two 30 mL Nylgene bottles ii Wear high temperature proof glovesiii Open TV2 to release 20 mL solution before taking 30 mL upstream

sample with the first bottle then label the bottle with date time test name location and personnel name

iv Open TV3 to release 30 mL solution before taking 30 mL downstream sample with the second bottle then label the bottle with date time test name location and personnel name

v After the sample grabbing is done measure the water level on the level indicator and record it in the test log

44Mode 4 Cool down and sample removal mode(Valve positions can be referred to Figure 6-7)Switch off the power supply to the heat tapes1) Switch 3V4 from ldquoflow thrurdquo to ldquoloop coolerrdquo2) Adjust the pump frequency to 45 Hz3) Crack VV2 to maintain the autoclave pressure lower than 75 psi (set

pressure on relief valve)4) When the T3 is lower than 100 C open VV2 to fully depressurize the

autoclave5) Fully open the valves for chill water ldquosupplyrdquo and ldquoreturnrdquo lines


6) Monitor AUTO SOL temperature on the temperature controller7) When the temperature on the DAQ system drops to 50 C and the

autoclave pressure drops to 0 take the insulation cap away on the autoclave

8) Stop the pump VSP1 ldquoHIGH FLOW PUMPrdquo45Autoclave draining and sample retrieving

1) Close V5 and V7 to isolate the autoclave2) Turn on V1 and open V6 to purge the solution to the drain from the

autoclave3) Close V6 and repeat step b until no water comes out from V64) Open TV3 to purge the remaining solution in the flow diverter 5) Unscrew the clamps on and above the autoclave lid take off the tube

above the lid unscrew the downstream grab sample line6) for the autoclave sample holder pull the sample holder out directly 2) for

the test column sample holder unscrew the bolts and nuts on the flange7) Reverse the operation steps in Section 33 to take the samples out of the

sample holders8) Rinse all the samples with DI water and acetone and dry them off by

blowing compressed air9) Weigh all the samples and record the total weight on the log book10) Take pictures for all the samples and save pictures on the computera Store the samples in a large size zip lock bag and write down the test

name personnel names date and time on the bag5 Post-test cleanup procedure

1) Draining remaining solution

a Set the valve positions as shown in Figure 6-4 open V5

b Unhook the outlet hose and P2 hose hook the outlet hose with P2 as shown Figure 6-15 switch 3V2 to VSP2 ldquohigh flow pumprdquo (use VSP2 as the flow path)

c Repeat Section 41 1 degh to seal the water tank and autoclave

d Hook V6 with a 30-gal closed drum

e Open V1 and V4 to pressurize the water tank and autoclave to 50 psi

f Crack the drain valve V6 and slowly purge the water out from the loop once the system pressure is 50 psi

g Repeat step e and f until no water comes out from the drain valve


Figure 1 VSP2 hoses

h Switch 3V1 to ldquoflow thrurdquo and repeat g until no water comes out

i Switch 3V2 to ldquolarge pumprdquo and repeat g until no water comes out

j Open V7 and repeat g until no water comes out

k Close V5 and V7 keep the autoclave pressure at 20 psi and open the needle valve for downstream GSL until no solution comes out

l Close V1 V4 and V6

2) Base Washa Make 45L of NaOH solution (Initial valve positions are in Figure 6-4)b Prepare 018g of NaOH dissolve into 1L deionized waterc Transfer 44L of deionized water into the large secondary containerd Transfer 1L prepared NaOH into the large secondary containere Stir the NaOH solution in the large secondary container with a stirring bar and measure the

pH at multiple locations with a calibrated pH meter (Must be below 985 typically around 950) keep stirring until the variation of the pH readings are less than +- 01 (about 10 mins)

f Transfer 40 L NaOH solution to the water tank


g Repeat Section 41 1 degh to seal the water tank and autoclave

h System cleaning process (Turn on the heat tape to accelerate dissolution Identical to Acid WashDI Rinse)

I Stage 1 (Water Tank Level) i Turn on VSP1 ldquohigh flow pumprdquo at 45 Hz

ii Keep the loop running for 2 hoursII Stage 2 (Autoclave high flow)

iii TV1 Closediv V5 Openv V7 Open

i Drain Solution repeat Section 50 A 3) Acid Wash (Initial valve positions are in Figure 6-4)

a Make 45L of acid solution such as boric acid if the test solution is borated solution (hotplate needed)

b Prepare 657g of H 3BO3

c Keep adding H 3BO3 into 4L beaker on a hotplate with stirring rod until precipitates are observed

d Transfer prepared 4L of diluted H 3BO3 into the large secondary containere Repeat Step 3-4 at least 6 times Avoid putting any H 3BO3(s) into the final solution f Transfer deionized water into the large secondary container until there is 45L total (45-

46=21)g Test the pH of the solution with a calibrated pH meter (Must be above 415 typically around

43-46)h Transfer 40 L H3BO3 solution to the water tank

i Repeat Section 41 1 degh to seal the water tank and autoclave

j System cleaning process (Turn on the heat tape to accelerate dissolution Identical to Acid WashDI Rinse)

I Stage 1 (Water Tank Level) i Turn on VSP1 ldquoHIGH FLOW PUMPrdquo at 45 Hz



k Drain Solution repeat Section 50 A

4) DI Rinse (the same procedure as base wash)a Take water sample ( Measure amp Record turbidity and Conductivity in the test log)b Transfer 40 L DI water into the autoclave


d System cleaning process (Turn on the heat tape to accelerate dissolution Identical to Acid WashDI Rinse)

I Stage 1 (Water Tank Level)


i Turn on VSP1 ldquoHIGH FLOW PUMPrdquo at 45 Hzii Keep the loop running for 2 hours

II Stage 2 (Autoclave high flow) iii TV1 Closediv V5 Openv V7 Open

e Drain Solution repeat Section 50 A

5) Loop drying (optional)b TV1 openc 3V1 To water tankd 3V2 To high flow pumpe 3V3 To high flow meterf 3V4 To flow thrug V5 V6 and V7 openh Open V1 and V4 to introduce compressed air into the loop for overnight


Appendix 6-1 Large flow pump operation instructions1 Operation conditions

The large flow pump (VSP1) has restrict requirements on the conditions up which it is running All these requirements should be rigorously to prevent potential damage to the pump

Temperature pumps with Cool-Top ndash up to 356 F (180 C) when the operating temperature is higher than 266 F (130 C) the minimum flow rate should be higher than 25 gpm which is 10 of the flow capacity of the pump

Minimum inlet pressure (NPSHR)+2 ft

Maximum operation pressure 232 psi

Material compatibility see manuals for detailed information

Liquid level check The pump CANNOT run without being filled with liquid otherwise permanent damage will be caused on the impellers To top off the pump liquid should be dumped into the loop through the water tank Then unscrew top bolt shown in the figure below If liquid comes out from the hole the pump is then filled with liquid


2 Pump operation

- Switch on the power supply shown in Figure

- Press ldquoRUNrdquo and ldquoSTOPrdquo on the VFD to start and shut the pump

- Press up and down arrow to increase and decrease the pump frequency


Appendix 6-2 Small flow pump operation instructions

1 Operation conditions


Temperature 300 F (149 C)


2 Pump operation

To adjust the flow rate rotate the black knob on the left hand side in the picture shown below

The dial shows the percentage of the max flow rate


Appendix 6-3 U3000 ultrasonic flow meter operation instructions1 Operation conditions

The maximum allowable temperature 200 C

Flow rate range

2 Operation procedure

Rail and transducer installation

For detail see the manual online

httpwwwheattracingcoukuploadMicronics-Ultrasonic-Clamp-On-Flow-Meter---Portable-and-Permanent-Flow-Meters---Ultraflo-U3000-and-U4000---User-Manualpdf

REFERENCE

[1] Flowing Autoclave 116rdquo Sample Holder Prototype Design Rev 01 Document No CET-OSU-SAMPLE-HOLDER

[2] SYL-2362A2 PID Temperature Controller Instruction Manual Version 24 httpauberinscomimagesManualSYL-236220instruction2016pdf Auber Instruments

[3] OSU Flowing Autoclave System PampID Rev 04

[4] Design Inputs for Flowing Autoclave System MEMO-9050-MEM-2014-1 Rev 1



Title of lab operating procedure RevisionHigh-Temperature High-Pressure flow loop 00



Appendix 7 Glass cell system1 Experimental setup

Figure 7-1 shows the three-electrode electrochemical system in a glass cell The washer specimen mounted on a rotating cylinder electrode (RCE) or the disk specimen mounted on a rotating disk electrode (RDE) can be used as the working electrode The Pine speed controlled rotator (0 to 5000 revolutions per minute (RPM)) is used to control the rotation speed of the working electrode A 025rdquo diameter graphite rod 12rdquo in length seated inside a fritted glass tube is used as a counter electrode (CE) A silversilver chloride in 4 molar sodium chloride solution (AgAgCl4 M KCl) reference electrode (RE) is connected to the cell externally via a Luggin capillary tube The glass cell was filled with 1 liter of a test solution The pH is monitored with a pH probe immersed in the test solution Solution temperature is maintained within plusmn1 degC by using a thermocouple and hot plate with built-in temperature control unit The test solution is exposed to the atmosphere via a condenser which is also used to avoid the evaporation of water All electrochemical measurements are performed using a Gamry Interface 1000 potentiostat controlled by the Gamry Framework software

Figure 7-1 Glass cell setup2 Components and supplies

1) 1 liter OpenTop glass cell (Pine Instruments product number RRPG143)2) Pine modulated speed rotator (MSR) (accuracy plusmn10 rotation rate)3) Pine rotating cylinder electrodes (RCE) and rotating disk electrode (RDE)4) Potentiostat Gamry Interface 10005) Reference electrode Pine Instruments F0DR-0021 (4 M AgAgCl)6) Counter electrode


7) Luggin tube8) Thermocouple and Thermowell Pine Instruments 9) Thermo Scientific hot plate (accuracy plusmn 1 C)10) Hexagonal head screwdriver11) Condenser12) Air supply tube13) C clamps14) 500 mL graduated cylinder15) Oakton automatic temperature compensation (ATC) pH probe16) Oakton portable pH 5+ meter (accuracy plusmn001 pH plusmn 05 C)17) pH standards for calibration18) Mettler Toledo 204 analytical balance (readability 00001 g)19) Weigh boats20) Microspatula21) Kimwipes lab disposable wipes22) Magnetic stir bar

3 Pre-test planningThe following activities should be completed prior to starting the test1) Inspect bench test assembly and repair any issues noted during the previous

test2) Verify all necessary supplies (DI water cold air and power supplies) are

available3) Verify inventory of all chemicals corrosion specimens etc to be used in the

test4) Verify pH meter is working properly5) Check the temperature of the hotplate with a calibrated thermometer6) Check the accuracy of the motor rotation speed7) Check the potential of the reference electrode with the lab standard

reference electrode4 Specimen and solution preparation

41Solution preparation1) Collect 1 L of deionized water using the 500 mL graduated cylinder Check

the electrical resistivity of deionized water and make sure it is higher than 175 MΩ∙cm


2) Take desired amount of deionized water to fill a clean beaker Place on stirring plate with clean stir-bar in beaker

3) Calibrate analytical balance ndash Internal adjustment (see the manual of the balance)

4) Measure required mass of chemicals using the analytical balance and weigh boat

5) Dissolve the chemicals in the deionized water and set the rotation speed of the stir-bar

6) Allow solution to mix until components are dissolved7) Calibrate pH meter before every test (see the manual of the pH meter)8) Check solution with Eutech Oakton pH +5 meter pH values should read

with plusmn005 9) If pH value is achieved add the 1 L concentrated solution to the cleaned 1

L glass cell42Metal specimen preparation

1) Measure and record dimensions of specimens in test log A surface area of 3016 cm2 is targeted for the washer specimen A surface area of 0196 cm2 is targeted for the disk specimen

2) Rinse specimens with deionized water acetone or isopropanol subsequently Dry by blower (cold wind)

3) Weigh and record initial mass of each specimen in test log4) Take a picture of the specimen5) Load specimen into specimen holder6) Place specimen holder onto modulated speed rotator (MSR) RCE or RDE

bearing shaft5 Test operation

51Glass cell preparation1) Add 1L test solution to the glass cell2) Place the MSR RCE (high velocity tests)rotating disk electrode (RDE) (low

velocity tests) bearing shaft into solution assuring the bottom of the shaft rests in the appropriate slot in the glass cell (lift the electrode slightly to make sure its bottom is not in contact with the bottom of the glass cell)

3) Place the lid on the cell4) Raise the motor by using the black knob on the side of the motor5) Connect the MSR RCE bearing shaft to the motor

a Open the clamshell doors that protect the brushes


b Assure the MSR RCE bearing shaft is inserted into the adapter (it is a bronze color) that transfers the motorrsquos power to the shaft DOUBLE CHECK TO ASSURE THE SHAFT IS AS FAR INTO THE ADAPTER AS POSSIBLE

c Tighten the screws on both sides of the adapter by using the hexagonal head screwdriver

d Close the clamshell doors and tighten the screw to hold them closed6) Add the following accessories into the appropriate penetrations

a Place the reference electrode into the luggin tubeb Place the counter electrode into the tube with fiterc Place the thermocouple in the thermowell and make sure the

thermowell has oil or water in it to assure good thermal contact between the solution and the thermocouple

d Place the pH probe as needede Install the condenser

7) Connect air (or cold tap water) supply to the bottom of the condenser and then turn on air (water) supply

8) Connect the thermocouple to the hotplate and place it in the thermowell9) Connect potentiostat leads

a Connect the white lead to the reference electrodeb Connect the red and orange leads to the counter electrodec Connect the blue and green leads to the red banana cables that

connect to the brushes of the rotating cylinder electroded Connect the black lead to the electrical ground

10) Secure the lid using the special C clamps11) Set hotplate to heat to desired temperature

a ASSURE NO WIRES ARE CONTACTING THE HOTPLATE SURFACEb Press the ldquoSetrdquo button to the right of the knobc Rotate the knob the set desired temperatured Press the ldquoSetrdquo button again

12) Confirm target temperature in solution is reached Record temperature and pH

13) Immerse aluminum specimen in test solution by lowering the RCE or RDE bearing shaft The position of specimen should be at the same level of the tip of Luggin tube

14) Place plexiglass shield over the glass cell


15) Set motor to rotate at the desired speed52Perform electrochemical measurements using Gamry Interface 1000 and

Gmary software (manual available online)1) Turn on potentiostat2) Open ldquoGamry Frameworkrdquo Gamry software for potentiostatSelect desired

electrochemical test from the ldquoExperimentrdquo tab or set up a battery of tests using the ldquoSequence Wizardrdquo function



5) Set motor to rotate at the desired speed6) Run tests by clicking ldquoRun Sequencerdquo button7) After electrochemical measurements

a Calibrate the pH probe and then measure the solution pH while the solution is still at the target temperature and record in test log

b Collect solution sample for Inductively Coupled Plasma (ICP) analysis as needed

c Stop the test following the Cleanup proceduresd Rinse corrosion specimen with DI water and acetone air dry Take a

picture record weight and follow the Specimen storage procedures8) Always record test person date and time List analysis still to be run with

expected deadline6 Clean up

1) Set the motor to 0 rpm and then turn the motor off2) Remove the plexiglass shield3) Turn off the hotplate4) Replace the plexiglass shield and allow for the solution to cool5) Remove the pHATC probe6) Turn off the potentiostat and disconnect the potentiostat leads7) Remove the accessories rinse them in deionized water and dry them off

before putting them away8) Remove the rotating cylinder from the motor9) Remove the lid10) Remove the rotating cylinder from the solution


11) Carefully dismantle the specimen from rotating cylinder12) Check if solution leaks inside the gap between corrosion specimen and

rotating cylinder or specimen holder13) Rinse the specimen with deionized water and isopropanol (or acetone)

subsequently14) Dry the specimen by blower (selecting cold wind)15) Take a picture of the tested specimen (with corrosion product)16) Ensure specimen is stored in pure nitrogen gas (N2) filled bag or box

and labeled for post-test analysis17) Take 30 mL sample of solution into a 30 mL acidified (02 mL nitric acid

as needed) bottle The sample bottle should be labeled with sample takerrsquos initials date time and sample ID

18) Use the bottle information to complete a chain-of-custody for the samples to be taken for inductively coupled plasma (ICP) analysis

19) Store any sample not immediately taken for ICP analysis20) Pour remaining solution down the drain (Store the solution and ask EHS

to pick up as needed)21) Wash the glass cell with tap water and deionized water subsequently

and dry



Title of lab operating procedure RevisionGlass cell system 00



Appendix 8 Shaker table setup1 Experimental setup

The primary components of the shaker table test system are a shaker (VWRreg Advanced Orbital ShakermdashModel 10000) a high-stability immersion digital circulator and a Nalgene rectangular polypropylene tank The tank is placed on the platform of the shaker A bottle holder with 5x5 bottle ports is placed at the bottom of the tank One liter Nalgene polypropylene bottles filled with the test solution are placed inside the port of the bottle holder The water in the tanks is circulated by the high-stability immersion digital circulator (built in heater and temperature control unit) to control the temperature of test solutions in the bottles After the solution is heated to the desired temperature the samples such as metal coupons are submerged in the test solution in the bottle The platform of the shaker can be set to 75 RPM of rotation speed to simulate the flowing condition

Figure 1 Shaker table setup (a) Circulator (built in heater and temperature control unit) (b) Inside view of water tank (c) whole system


2 Components and supplies1) VWRreg Advanced Orbital ShakermdashModel 100002) High-Stability Immersion Digital Circulator 240 V Techne TE-10D 3) Acrylic sample housing box4) Power converter from 240V to 110V5) Thermo Scientific Nalgene Rectangular Polypropylene Tank with cover6) Mettler Toledo ML 204 Analytical Balance readabilitymdash00001 g7) Blue Hawk 116rdquo x 800 ft-Nylon Rope8) Eutech Oakton pH 5+ meter with ATC probe9) H-B Instrument Durac Plus Certified Total Immersion Thermometer10) Fisherbrand polypropylene rectangular carboys11) Dial-Calipers 12) 1 L Nalgene polypropylene bottles13) 30 mL Nalgene polypropylene bottles14) Magnetic stir bar

3 Pre-Test Planning1) Inspect orbital shaker and immersion circulator for an issues noted in the

previous test2) Indicate chemical supplies are adequate for testing3) Indicate all lab supplies involved are adequate for testing4) Verify deionized water filter is providing required resistance that corresponds

with 175 Megaohm or higher Grade 1 water5) Verify enough deionized water is available for the test solution and testing

facility6) Check water level in bath is to appropriate height7) Check water level in sample holder box is at least the height of the grating8) Set heater to three degrees higher than target temperature9) Determine pH meter is reading buffers properly after calibration has been

performed10) Check analytical balance is turned on and warmed up for at least one

hour4 Sample and solution preparation

41Sample preparation1) Pre-cut metal coupon to desired dimensions2) Drill frac14rdquo hole into each coupon to hold nylon string


3) Cut 18rdquo pieces of nylon string for each coupon you are testing4) Clean individual coupons with deionized water followed by acetone or

isopropanol 5) Allow coupons to air dry6) Assign coupons to sample number7) Weigh coupons using Mettler Toledo ML 204 Analytical Balance and record

initial weight along with time and date of measurements8) With dial calipers (English units) measure and record the width height and

thickness of the coupon in two locations each and take the average9) Take a piece of nylon string and evenly tie string around hole in coupons10) Store coupons in appropriately labeled bags and string in Ziploc bags

until time of test Labels will have sample identification number date type of sample preparerrsquos initials and status of sample (ie post-test or pre-test)

42Solution preparation421 Thoroughly rinse polypropylene carboys and spigots with deionized

water422 Fill carboy with deionized water needed 423 Take desired amount of deionized water to fill a clean beaker Place on

stirring plate with clean stir-bar in beaker424 Measure out the desired amount of chemicals for the test solution and

add to the beaker425 Allow solution to mix until components are dissolved426 Check solution with Eutech Oakton pH +5 meter pH values should

read with plusmn005 427 If pH value is achieved add the 1 L concentrated solution to the

cleaned 1 L bottle428 Shake entire bottle vigorously and place in acrylic box sitting on the

orbital shaker429 Label each bottle with sample number pH value and other information

as needed 5 Test Operation

During interaction with the water bath and orbital shaker thermal gloves lab coat and goggles must be worn for personal safety1) Place solution-filled bottles into assigned matrix positions2) Once all bottles are in sample holder box fill water level to 3rdquo from the

bottom of the sample holder box


3) Set the circulating water heater to 2 degrees higher temperature than the target temperature if 85˚C or 55˚C If target temperature is 25˚C set only 1 degree higher

4) Allow water bath sample holder box and bottles to heat for approximately 24 hours to reach desired temperature

5) After 24 hours check and record the pH and temperature (with certified thermometer) of a representative solution

6) Before loading samples into each bottle increase heater temperature by 1 degree to prevent heat loss if target temperature is 85˚C or 55˚C

7) Insert aluminum fiberglass or cal-sil into the 500 mL solutions by hanging the nylon string from the sides of the bottles so the sample is submerged at the midpoint of solution the middle of the height and the middle of the diameter

8) Place bottles back into the sample holder box and record the time This will be the start time of the test duration

9) Set VWRreg Advanced Orbital ShakermdashModel 10000 to desired rotation speed and lower circulating heater temperature to just 2 degrees above target temperature if 85˚C or 55˚C

10) Check water level of shaker table boxes daily to make sure water is covering the bottom of the bottles

11) After pre-determined time for each test is completed remove bottle from matrix as quickly as possible

12) Remove sample from solution measure and record pH value temperature and time sample was pulled

13) Rinse metal coupon with DI water followed by acetone or isopropanol allow it to air dry and cool to room temperature Note formation of precipitate in the bottle or on the surface of the coupon

14) Place coupon in labeled bag until post-cleaning and weighing will be performed

15) Store the coupon for further analysis16) Shake the solution in the bottle and pour off 30 mL of solution for ion

concentration testing17) Label 30 mL bottles with for Inductively coupled plasma (ICP) analysis



Title of lab operating procedure Revision00



Appendix 9 Use of Pipettes1 Please be careful with the use of the pipettes as they are very sensitive

instruments meant for precision delivery of liquids They can be very easily damaged and cause erroneous readings

2 If you drop a pipette check the mass of the ldquosamerdquo volume of DI water with the other pipette

3 Avoid getting liquid into the delivery mechanism of the instrument This will cause damage

4 During the suction phase place the tip about 15 cm inside the liquid interface (from the top) The plunger must be pressed to only the first setting Suck liquid very deliberately and slowly

5 During delivery press to plunger slowly all the way down to second stop



Title of lab operating procedure RevisionUse of Pipettes 00



Appendix 10 Solubility experiment procedureInitial Weighing

1 Weigh ~1 gram of lanthanide metal pieces and ~ 2 grams of alkali metal using aluminum weighing dishes _________________=__________ g = __________ g

2 Weigh open tubing __________ g3 Weigh cap to be on tubing __________ g 4 Place lanthanide sample within the tubing and weigh system5 Place alkali sample within the tubing and weigh system6 Weigh the cut tantalum mesh piece __________ g

Welding Welder operation in ldquoWelder SOPrdquo7 Place open tubing on insulator material (Teflon) that is located on the inner

glovebox floor8 Place mesh at the top open end of the pipe and place a cap sandwiching the

mesh between pipe and cap9 Attach ground clamp to the tubing10Ensure the torch has pure argon running

a If the torch hasnrsquot been run in over 6 hours then the initial weld should be made without any testing materials (alkalis or lanthanides) nearby This weld will cause the impurity sensors within the glovebox to jump several ppm but within several minutes the levels should return to the minimum

b If the torch has been run in the previous 6 hours then the coolant line will have only pure argon gas

11The gas lines between the welder controller and the torch should all be open12Place torch into position for the mesh Weld the cappipe interface vaporizing

off any excess mesh13Run welder for 5-10 second intervals with a break in between intervals to

allowing cooling14Continue welding until the interface has been seal

Operation Tips for weldinga If any point of the interface is no longer touching filler wire may be

needed to be added at that locationb The welder torch should be moved in a circlular motion with the center

stationary on the interface The torch should always be angled toward the interface as the circular motions are made Once the material has melted together using the same circular motion move the center of the circle along the interface

c Ensure that no alkali or lanthanides are at the area of welding as vaporization can occur


d Ensure that the torch electrode is a compatable material No thorium electrodes (radioactive) No ceriated electrodes for this project since this would introduce added rare earth of interest For this project use lanthanated electrodes

e Initially pressure needs to be applied to the cap to keep it in place Use tongs to apply the pressure with a welder glove on

f The welder gloves can cause micro-holes in the glove when wearing Extreme care must be taken and the operator can also hold the glove over the glovebox glove

Furnace Furance operation in ldquoFurnace SOPrdquo15Weigh completed tubing crucible16Place tubing in furnace with weld cap the upper portion17Close furnace and set temperature to desired temperature ________ K =

C18Once at desired temperature allow the determined equilibration time to pass

before moving on ____________ minutes19Once equilibration time is reached flip tubing

a Use the long tongs and welder gloves Initially grab the top of the crucible and flip it back into the crucible

b Shake tubing slightly as placing back into furnace to help break surface tension of the liquid alkali and let it flow into the collector

20Allow a small amount of time (~10 minutes) at temperature with the crucible inverted ___________ minutes

21Turn furnace set point to room temperature and allow to cool Once the set point is set for room temperature the furnace can actually be turned off as well

22Once cooled to room temperature weigh the entire crucible system __________ g

a For temperatures below (550 C) and 24 hours equilibration the chilling water heat exchanger donrsquot have to be turned on but itrsquos better to have the system cooled

b For threaded crucibles the threads must have been tightened as far as possible for hand tightening to prevent alkali vapor from being able to leave the system However at this tightening the threads cannot be taken off by hands or pliers and the crucible must be cut open

c During and after heating the crucible will appear to have a more brownish tint than originally This is due to the graphite crucible in the furnace carbonizing the crucible material for testing This carburization only affects the outside of the crucible as the inside and inner contents appear unchanged

d Mesh of less than 80 x 80 sieve must be used 80 x 80 sieve of tantalum allow sodium to flow through but not the stainless steel sieve 50 x 50 stainless steel sieve with a small hole cut at the center appeared to work for the sodium flow


Sample Preparation23With cap end down cut open the tubing just below the mesh24Weigh the entire system __________ g Weigh the alkali and lanthanides

pieces ________ g25Scrap clean the alkali from the collector cap and place within bottle26Remove the bottle with alkali metal and the collector from the glovebox27Immediately move the alkali metal into a solution of isopropanol to dissolve

the metal of cap with alcohol 28Transfer solution to a polyethylene bottle29Etch collector with HCl and transfer solution to the polyethylene bottle30Add 3 N NaOH (075 ml) and H2O (50 ml) to the polyethylene bottle and mix31Remove precipitate by decantation32Dissolve precipitate in 6 N HCl and wash with 001 N HCl into a volumetric

flask33Dilute solution to volume34Transfer solution to a polyethylene bottle for ICP analysis



Title of lab operating procedure RevisionSolubility experiment procedure 00



Appendix 11 NMFC Laboratory Specific Operating Procedure Sign off SheetHard copy of the NMFC Laboratory Specific Operating Procedure can be found in the Safety Document binder maintained in each lab (W396 amp W 465) You signature below acknowledges that you have read and understood the information within the laboratory specific operating procedure

Name (Print) Signature Date

10 Purpose

20 Scope

30 Responsibilites

40 General Laboratory Procedures

50 Chemical handling storage and transportation

60 Laboratory Training

Appendix 1 General Glove box operation

Appendix 2 Kerr Auto Electro-Melt Furnace

Appendix 3 Gamry Interface 1000

Appendix 4 High-Temperature Electrochemical Cell

Appendix 5 High-Temperature High-Pressure corrosion cracking system

Appendix 6 High-Temperature High-Pressure flow loop

Appendix 6-1 Large flow pump operation instructions


Appendix 6-3 U3000 ultrasonic flow meter operation instructions

Appendix 7 Glass cell system

Appendix 8 Shaker table setup

Appendix 9 Use of Pipettes

Appendix 10 Solubility experiment procedure

Appendix 11 NMFC Laboratory Specific Operating Procedure Sign off Sheet


Table of Contents

10 Purpose220 Scope 230 Responsibilites240 General Laboratory Procedures250 Chemical handling storage and transportation360 Laboratory Training4Appendix 1 General Glove box operation6Appendix 2 Kerr Auto Electro-Melt Furnace11Appendix 3 Gamry Interface 100013Appendix 4 High-Temperature Electrochemical Cell15Appendix 5 High-Temperature High-Pressure corrosion cracking system17Appendix 6 High-Temperature High-Pressure flow loop23

Appendix 6-1 Large flow pump operation instructions49Appendix 6-2 Small flow pump operation instructions51Appendix 6-3 U3000 ultrasonic flow meter operation instructions52

Appendix 7 Glass cell system54Appendix 8 Shaker table setup60Appendix 9 Use of Pipettes65Appendix 10 Solubility experiment procedure67Appendix 11 NMFC Laboratory Specific Operating Procedure Sign off Sheet71


10 PURPOSE


20 SCOPE


30 RESPONSIBILITES



























































































































































































P

7- flo

w me

ter

19- Transm itter

6-Sensor

Filter

11-P ump

15-P ump

10- Rese rvior

4-BP R





To autoclave 3

2-Rup ture disk

3 3

6-Sensor

8- Dem i

5

9-Fil ter

17

1818

13-Co lumn

14-E nd plateP 1

16




transmitter






































CA1




OSU Machine Shop

NA (Custom)

HC1


HE1


McMaster-Carr

35185K999

HE2



NA NA (Custom)




PR2




Omega Engineering



SA1XL-K-72-SRTC


Omega Engineering





Omega Engineering



Omega Engineering

SA1XL-T-72



Omega Engineering

SA1XL-T-72


Omega Engineering

SA1XL-T-72


Omega Engineering

SA1XL-T-72

TK1


Apache NA (Custom)

UFM


VSP1



VSP2



QG400 Q2CSC


NA







spacing 3 4 OLNA
















1SS-12NRS16









15Automation system




NI NI9213


Auber Instruments

syl-2362
































than 175 MΩcm



























































Component
















































f Move on to Mode 2

















































Figure 1 VSP2 hoses














































2 Pump operation










2 Pump operation






Flow rate range





REFERENCE














































































and dry












































































































10 Purpose

20 Scope

30 Responsibilites



















10 PURPOSE


20 SCOPE


30 RESPONSIBILITES



























































































































































































P

7- flo

w me

ter

19- Transm itter

6-Sensor

Filter

11-P ump

15-P ump

10- Rese rvior

4-BP R





To autoclave 3

2-Rup ture disk

3 3

6-Sensor

8- Dem i

5

9-Fil ter

17

1818

13-Co lumn

14-E nd plateP 1

16




transmitter






































CA1




OSU Machine Shop

NA (Custom)

HC1


HE1


McMaster-Carr

35185K999

HE2



NA NA (Custom)




PR2




Omega Engineering



SA1XL-K-72-SRTC


Omega Engineering





Omega Engineering



Omega Engineering

SA1XL-T-72



Omega Engineering

SA1XL-T-72


Omega Engineering

SA1XL-T-72


Omega Engineering

SA1XL-T-72

TK1


Apache NA (Custom)

UFM


VSP1



VSP2



QG400 Q2CSC


NA







spacing 3 4 OLNA
















1SS-12NRS16









15Automation system




NI NI9213


Auber Instruments

syl-2362
































than 175 MΩcm



























































Component
















































f Move on to Mode 2

















































Figure 1 VSP2 hoses














































2 Pump operation










2 Pump operation






Flow rate range





REFERENCE














































































and dry












































































































10 Purpose

20 Scope

30 Responsibilites


































































































































































































P

7- flo

w me

ter

19- Transm itter

6-Sensor

Filter

11-P ump

15-P ump

10- Rese rvior

4-BP R





To autoclave 3

2-Rup ture disk

3 3

6-Sensor

8- Dem i

5

9-Fil ter

17

1818

13-Co lumn

14-E nd plateP 1

16




transmitter






































CA1




OSU Machine Shop

NA (Custom)

HC1


HE1


McMaster-Carr

35185K999

HE2



NA NA (Custom)




PR2




Omega Engineering



SA1XL-K-72-SRTC


Omega Engineering





Omega Engineering



Omega Engineering

SA1XL-T-72



Omega Engineering

SA1XL-T-72


Omega Engineering

SA1XL-T-72


Omega Engineering

SA1XL-T-72

TK1


Apache NA (Custom)

UFM


VSP1



VSP2



QG400 Q2CSC


NA







spacing 3 4 OLNA
















1SS-12NRS16









15Automation system




NI NI9213


Auber Instruments

syl-2362
































than 175 MΩcm



























































Component
















































f Move on to Mode 2

















































Figure 1 VSP2 hoses














































2 Pump operation










2 Pump operation






Flow rate range





REFERENCE














































































and dry












































































































10 Purpose

20 Scope

30 Responsibilites






















































CA1




OSU Machine Shop

NA (Custom)

HC1


HE1


McMaster-Carr

35185K999

HE2



NA NA (Custom)




PR2




Omega Engineering



SA1XL-K-72-SRTC


Omega Engineering





Omega Engineering



Omega Engineering

SA1XL-T-72



Omega Engineering

SA1XL-T-72


Omega Engineering

SA1XL-T-72


Omega Engineering

SA1XL-T-72

TK1


Apache NA (Custom)

UFM


VSP1



VSP2



QG400 Q2CSC


NA







spacing 3 4 OLNA
















1SS-12NRS16









15Automation system




NI NI9213


Auber Instruments

syl-2362
































than 175 MΩcm



























































Component
















































f Move on to Mode 2

















































Figure 1 VSP2 hoses














































2 Pump operation










2 Pump operation






Flow rate range





REFERENCE














































































and dry












































































































10 Purpose

20 Scope

30 Responsibilites





















Omega Engineering



Omega Engineering

SA1XL-T-72



Omega Engineering

SA1XL-T-72


Omega Engineering

SA1XL-T-72


Omega Engineering

SA1XL-T-72

TK1


Apache NA (Custom)

UFM


VSP1



VSP2



QG400 Q2CSC


NA







spacing 3 4 OLNA
















1SS-12NRS16









15Automation system




NI NI9213


Auber Instruments

syl-2362
































than 175 MΩcm



























































Component
















































f Move on to Mode 2

















































Figure 1 VSP2 hoses














































2 Pump operation










2 Pump operation






Flow rate range





REFERENCE














































































and dry












































































































10 Purpose

20 Scope

30 Responsibilites

























15Automation system




NI NI9213


Auber Instruments

syl-2362
































than 175 MΩcm



























































Component
















































f Move on to Mode 2

















































Figure 1 VSP2 hoses














































2 Pump operation










2 Pump operation






Flow rate range





REFERENCE














































































and dry












































































































10 Purpose

20 Scope

30 Responsibilites





















NI NI9213


Auber Instruments

syl-2362
































than 175 MΩcm



























































Component
















































f Move on to Mode 2

















































Figure 1 VSP2 hoses














































2 Pump operation










2 Pump operation






Flow rate range





REFERENCE














































































and dry












































































































10 Purpose

20 Scope

30 Responsibilites











































than 175 MΩcm



























































Component
















































f Move on to Mode 2

















































Figure 1 VSP2 hoses














































2 Pump operation










2 Pump operation






Flow rate range





REFERENCE














































































and dry












































































































10 Purpose

20 Scope

30 Responsibilites












































































Component
















































f Move on to Mode 2

















































Figure 1 VSP2 hoses














































2 Pump operation










2 Pump operation






Flow rate range





REFERENCE














































































and dry












































































































10 Purpose

20 Scope

30 Responsibilites

























































f Move on to Mode 2

















































Figure 1 VSP2 hoses














































2 Pump operation










2 Pump operation






Flow rate range





REFERENCE














































































and dry












































































































10 Purpose

20 Scope

30 Responsibilites


































































Figure 1 VSP2 hoses














































2 Pump operation










2 Pump operation






Flow rate range





REFERENCE














































































and dry












































































































10 Purpose

20 Scope

30 Responsibilites























































2 Pump operation










2 Pump operation






Flow rate range





REFERENCE














































































and dry












































































































10 Purpose

20 Scope

30 Responsibilites
























2 Pump operation






Flow rate range





REFERENCE














































































and dry












































































































10 Purpose

20 Scope

30 Responsibilites





















Flow rate range





REFERENCE














































































and dry












































































































10 Purpose

20 Scope

30 Responsibilites



























































































and dry












































































































10 Purpose

20 Scope

30 Responsibilites





























































































































10 Purpose

20 Scope

30 Responsibilites


















Purpose - Nuclear Materials and Fuel Cycle Research · Web viewUsing a wrench, screw the valve...

Documents

Transcript of Purpose - Nuclear Materials and Fuel Cycle Research · Web viewUsing a wrench, screw the valve...