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Gamry FlexCell Operator's Manual

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Flexcell Cell Kit
Operator's Manual

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  • Page 1 Flexcell Cell Kit Operator’s Manual...

  • Page 2: Limited Warranty

    Limited Warranty Gamry Instruments, Inc. warrants to the original user of this product that it shall be free of defects resulting from faulty manufacture of the product or its components for a period of one year from the original shipment date of your purchase.
  • Page 3 Flexcell Kit Operator’s Manual Copyright  1997−2017 Gamry Instruments, Inc. Part No. 990-00121 Revision 4.11 November 30, 2017...

  • Page 4: If You Have Problems

    Copyrights and Trademarks Flexcell Operator’s Manual copyright  1997−2017 Gamry Instruments, Inc. The names Flexcell, TDC2, TDC4, Gamry Framework, PC4, PCi4, Series G, and Reference 600 are all trademarks of Gamry Instruments, Inc. Tygon is a registered trademark of Saint-Gobain Performance Plastics Corp.

  • Page 5: Table Of Contents

    If You Have Problems ........................4 Chapter 1: Introduction ......................... 1-1 Chapter 2: Metal Specimens ......................2-1 Chapter 3: Unpacking and Assembling Your Flexcell Kit ..............3-1 Checking for Shipping Damage ..................3-1 Checking Parts against the Packing List ................3-4 Assemble the cell.
  • Page 6 Controlling the De-ionized Water Flow Rate ..............4-6 Heating, Cooling, and Stirring ................... 4-7 Temperature-control via the Cooling Coil ............. 4-7 Temperature-control via an External Heating Jacket ..........4-7 Usage at High Temperatures ................4-8 Usage at Low Temperatures ................. 4-8 Temperature Gradients within the Cell ..............

  • Page 7: Chapter 1: Introduction

    The Flexcell components were selected to be as chemically inert as possible. In normal use, the only materials in contact with the test solution are glass, filter paper, and PTFE. The cell is therefore usable with a wide variety of test solutions, including non-aqueous media.
  • Page 8 --Checking for Shipping Damage 1 - 2...

  • Page 9: Chapter 2: Metal Specimens

    Chapter 2: Metal Specimens--Checking for Shipping Damage Chapter 2: Metal Specimens A commercial source for suitable flat metal specimens is Metal Samples Co., Inc. Their P/N CO0130 series works well. The dimensions of this part are 2" × 2" × ∕...
  • Page 10 Chapter 2: Metal Specimens--Checking for Shipping Damage 2 - 2...

  • Page 11: Chapter 3: Unpacking And Assembling Your Flexcell Kit

    Unfortunately, no matter how carefully glass pieces are packaged, damage will sometimes occur. When you first receive your Flexcell kit, please check it for any signs of shipping damage. Be especially careful if the shipping container shows signs of rough handling.
  • Page 12 Chapter 3: Unpacking and Assembling Your Flexcell Kit--Checking for Shipping Damage Figures 3-1 Flexcell Assembly G l a s s Do m e G a m r y P/ N: 9 3 0 - 0 0 0 1 6 Q u i c k...
  • Page 13 Chapter 3: Unpacking and Assembling Your Flexcell Kit--Checking for Shipping Damage Figure 3-2 Flexcell: Reference Well Assembly R eferenc e W ell B and S trap P /N : 935-00038 R eferenc e W ell P /N : 930-00017 B all J oint C lamp (S J 12)

  • Page 14: Checking Parts Against The Packing List

    Flexcell components are labeled with their Gamry Instruments, Inc. part number (P/N). Be careful, for some of the Flexcell components are small enough to be lost in the cell’s packing material. If you are in doubt about the identity of a component, refer to Figures 3-1 and 3-2. These figures are also useful if you must check the completeness of an older kit.

  • Page 15: Assemble The Sample Holder

    Chapter 3: Unpacking and Assembling Your Flexcell Kit--Assemble the cell. Assemble the Sample Holder. The sample holder mounts underneath the cell. It is held in place by the wingnuts mounted on the cell’s legs. 1. Place the bottom cap on a table top with the conical depression facing the table.
  • Page 16 The rest of the reference-well assembly procedure is explained later. 3. Install the Drain Cap. The Flexcell kit does not include drain plumbing. If you wish to add drain capability to the cell, you are responsible for providing any fittings, valves and tubing that may be required.

  • Page 17: Install The Cooling Coil

    You should always use the Flexcell with de-ionized water flowing through the flooded gasket seal. Paradoxically, in the absence of this flow, the Flexcell suffers from crevice effects far worse than those in conventional cells. If you need to test flat-metal specimens and you don’t need a true crevice-free cell, you should use a ParaCell.

  • Page 18: Complete The Reference Well Assembly

    Chapter 3: Unpacking and Assembling Your Flexcell Kit--Assemble the cell. 2. Install the large O-ring. The large O-ring is P/N 935-00016. Install it in the bottom cap by pressing it into the groove on the upper surface of the cap. It often stays in place even when the cell is inverted.

  • Page 19: Test The Partially Assembled Cell For Leaks

    Chapter 3: Unpacking and Assembling Your Flexcell Kit--Test the Partially Assembled Cell for Leaks. Procedure: 1. Rotate the glass dome on the cell until one of the four #7 ACE-Thred™ ports on the dome is lined up with the reference Luggin capillary (installed previously). An exact alignment is not required.

  • Page 20: Test For Leaks

    3. Check all the seals for leaks, both immediately after filling, and 15 minutes after filling. You should not see any water on any fitting. Contact Gamry Instruments’ technical support department if you have a leak, and you are uncertain how to remedy the problem.

  • Page 21: Chapter 4: Routine Use Of The Flexcell

    Gas Bubbler A bubbler/vent tube is provided with the Flexcell. This tube fits in a 24/40 ground-glass joint. If you use both a stirrer and this bubbler tube, the stirrer enters the cell though the central 24/40 port and the bubbler is placed in the other 24/40 port.

  • Page 22: Install The Metal Specimen

    Chapter 4: Routine Use of the Flexcell--Install the Metal Specimen. Gamry Instruments currently sells two suitable reference electrodes. They are an SCE (P/N 930-00003) and a Ag|AgCl electrode (P/N 930-00015). Each is equipped with a male-pin plug connector. You may also use other reference electrodes. Avoid commercial reference electrodes with a 15 mm outside diameter (the reference well inside diameter is 14 mm).
  • Page 23 Install the De-ionized Water System. You normally use the Flexcell with a slow flow of de-ionized water through the water inlet. This water is essential to the crevice-free, flooded seal described above. The optimal water flow rate depends on the details of your experiment.

  • Page 24: Emptying The Cell

    Chapter 4: Routine Use of the Flexcell--Emptying the Cell Avoid overfilling the cell. Remember that the de-ionized water will slowly fill the cell during the experiment. Assume that 300 mL will fill the cell from the fill point suggested above to overflowing. With a de-ionized water flow of 6 mL/hour, 300 mL is added to the cell in 50 hours.

  • Page 25: Stirrer Installation

    Additional heating instructions and safety information are given later in this chapter. Stirrer Installation Stirring in the Flexcell is normally done using a stirrer inserted through the central port on the top of the cell. Gamry Instruments offers several optional accessories useful in adding stirring capability to your cell.

  • Page 26: Electrode Connections

    The stirring rod is easily broken. Take care if you must remove the dome with the rod in place. Electrode Connections If you are using your Flexcell with a Gamry Instruments, Inc. potentiostat, make the following connections to the electrodes: 1. Plug the reference-electrode lead into the white pin jack on the cell cable.

  • Page 27: Heating, Cooling, And Stirring

    The cooling coil allows heating or cooling via heat exchange with a liquid flowing through the coil. If the cell is to be both heated and cooled via this coil, a recirculating temperature bath is a suitable source of controlled- temperature fluid. Gamry Instruments’ Critical Pitting Test software allows computer control of several Thermo Scientific baths.

  • Page 28: Usage At High Temperatures

    Allow the jacket to dry thoroughly if it does become wet. Usage at High Temperatures The Flexcell has been designed for high-temperature operation. Many electrolytes will not boil until the temperature is well above 100°C. When the cell is operated at high temperature, many exposed surfaces of the cell become dangerous.

  • Page 29: Electrolyte Deaeration

    On the other hand, if the system you are studying is oxygen-free, do your tests after deaeration of the test electrolyte. The Flexcell includes a means for deaerating the electrolyte by passing an electrochemically inert gas (such as nitrogen) through the solution. The oxygen in the solution is swept away in the stream of inert gas.
  • Page 30 Chapter 4: Routine Use of the Flexcell--Electrode Area 4 - 10...

  • Page 31: Chapter 5: Accessory Equipment

    Heaters Introduction In the interests of flexibility, a heater is not included with either the Flexcell or with any Gamry Instruments temperature controller. However, Gamry does offer Flexcell-compatible heating jackets as options at extra cost. Two different heating jackets are available: one rated for 120 VAC operation (P/N 990-00115) and the other rated for 240 VAC (P/N 990-00119).

  • Page 32: Modification Of The Heater Cord For Use With The Tdc2

    It remains fixed at the AC power-line voltage. The heating jackets can be used with any duty-cycle-modulating controller. The Gamry Instruments TDC4 and TDC2 are two such controllers. You may already have a suitable controller in your laboratory.

  • Page 33: Using The Heating Jackets

    Chapter 5: Accessory Equipment--Stirrer 11) Reassemble the connector, using the longer screw to hold the two sides of the connector together. Using the Heating Jackets Always use the heating jacket with a closed-loop temperature-control system. Never plug it directly into an AC wall output: It is too easy to become distracted and walk away from your cell, which can quickly overheat.
  • Page 34 Gamry Instruments sells a stirring motor kit (P/N 990-00118) as an option at extra cost. This kit includes a stirring motor and controller, a flexible coupling to connect to the stirring rod, and a heavy-duty ring stand. The motor and controller in this kit operate from 120 VAC only.

  • Page 35: Chapter 6: Troubleshooting

    Chapter 6: Troubleshooting--Very small current or no current when you run an experiment Chapter 6: Troubleshooting This section of the manual is a list of problems that you may encounter. Following each problem are possible causes for that problem. Neither the list of problems nor the lists of their causes is comprehensive. This troubleshooting guide only applies if you are running a potentiostatic experiment on the cell.
  • Page 36 Chapter 6: Troubleshooting--Poor experimental reproducibility 6 - 2...

  • Page 37: Appendix A: Specifications

    Appendix A: Specifications--Volume Appendix A: Specifications Volume Volume 1000 mL minimum 1300 mL maximum Metal Specimen Active Area 5.00 cm (0.775 in ) nominal Minimum Size 4.0 cm × 4.0 cm Maximum Size 7.5 cm × any length or 11.0 cm × 11.0 cm (rectangular) 11.0 cm diameter (circular) Temperature Range Operating...
  • Page 38 Appendix A: Specifications--Volume 7 - 2...

  • Page 39: Index

    Index-- Index electrode connections, 4-6 emptying the cell, 4-4 escape path, 4-9 ball joint, 4-1 Faraday shield, 4-6 band strap, 3-8 fiber washer, 1-1 barbed fitting, 3-7 filling the cell, 4-3 barbed hose fitting, 3-10 flexibility, 4-1 blanket, 4-9 flooded gasket seal, 1-1, 4-3 bottom cap, 3-4 flow rate, 4-6 bottom cap fittings, 3-5...
  • Page 40 Index-- stirring, 4-8 noble metal counter, 4-1 stirring motor, 4-5, 5-3 noise, 4-6 stirring motor kit, 5-4 stirring paddle, 4-5, 5-3 o-ring, 3-8 stirring rod, 4-5, 5-3 oxygen, 4-9 stirring rod kit, 4-5, 5-3 packing list, 3-4 TDC1, 5-1 Packing List, 3-4 TDC2, 4-5, 5-1 phenolic crossbar, 3-5 temperature...

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