EL-CELL PAT-Cell-Gas User manual

© 2022 EL-Cell GmbH
User Manual
Release 1.34
PAT-Cell-Gas
Electrochemical test cell for in-situ gas analysis in a flow-through set-up

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User Manual PAT-Cell-Gas
Release 1.34
The information in this manual has been carefully checked and believed to be accurate;
however, no responsibility is assumed for inaccuracies.
EL-Cell GmbH maintains the right to make changes without further notice to products
described in this manual to improve reliability, function, or design. EL-Cell GmbH does not
assume any liability arising from the use or application of this product.
EL-Cell GmbH
Tempowerkring 8
21079 Hamburg - Germany
phone: [phone]
fax: [phone]
e-mail: [e-mail]
web: www.el-cell.com

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User Manual PAT-Cell-Gas
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Content
1 Product description.................................................................................................................................4
2 Technical data ..........................................................................................................................................6
3 Variants .....................................................................................................................................................7
4 Safety precautions...................................................................................................................................8
5 Assembly of the PAT-Cell-Gas ..............................................................................................................9
6 Working modes of the PAT-Cell-Gas.................................................................................................11
7 Disassembly and cleaning....................................................................................................................13
8 Sample valve with septum port (options S and SP) ........................................................................14
9 Unpacking ...............................................................................................................................................15
10 Spare parts and consumables ...........................................................................................................17
11 Troubleshooting ...................................................................................................................................22
12 Technical support................................................................................................................................22
13 Warranty ...............................................................................................................................................22

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User Manual PAT-Cell-Gas
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1Product description
The PAT-Cell-Gas is a test cell dedicated for in-situ gas analysis of battery materials in a flow-
through set-up. For that purpose, the test cell features a gas inlet and outlet and optionally a
built-in pressure sensor and a valve port for gas sample removal with a syrin ge. The test cell is
typically connected to peripherical equipment for gas supply and gas analysis. This manual
covers the test cell only.
Features
▪PAT series test cell with gas inlet and outlet
▪The inside PAT-Core (cell stack) is comprised of a lower gas permeable electrode, a
separator and the upper (counter) electrode.
▪The cell can be operated with or without reference electrode
▪The gas-permeable electrode is seated on a special lower plunger for current and gas
feed.
▪Two different lower plungers are available: with perforated plate (for minimum pressure
drop) or with flow field (for optimized plug flow)
▪The incoming gas is directed to the lower electrode of the cell stack and leaves the cell
through the central bore in the lower plunger.
▪Option P: Laser welded pressure sensor, 0 to 3 bar abs (0.5 to 4.5V). This option is only
operable in combination with the PAT-Tester-x or the PAT-Press box.
▪Option S: Gas sample port
▪Self-locking couplings compatible with 1/16 inch Swagelok Tube Fitting
Gas sample port
Pressure sensor
Valve block with gas
inlet and outlet and
self-locking couplings

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Schematic view: Gas inlet and outlet
Inlet
Outlet

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2 Technical data
▪Length: 95 mm
▪Width: 43.7 mm
▪Height: 116 mm
▪Weight: 0.7 kg
▪Gas connection:
1/16 inch Swagelok Tube Fitting
▪Electrode diameter: 18 mm
▪Temperature resistance -20 to +80 °C
2.1 Dead volume
PAT-Cell-Gas with metal seal:
▪PAT-Cell-Gas without PAT-Core: 8.275 ml
▪PAT-Cell-Gas with PAT-Core (Lower plunger AIR): 4.638 ml
▪PAT-Cell-Gas with PAT-Core (Lower plunger flow field): 3.915 ml
2.2 Spring force in relation to the thickness of the upper electrode:
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
0200 400 600 800 1000
Spring force applied on cell stack / N
Thickness of upper electrode / µm
Compression spring,
FED9028

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3Variants
PAT-Cell-Gas
PAT-Cell-Gas P
PAT-Cell-Gas S
Features
Gas inlet and outlet
Features
▪Gas inlet and outlet
▪Gas pressure sensor, 0 to 3 bar abs
Features
▪Gas inlet and outlet
▪Gas sample port

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PAT-Cell-Gas SP
4Safety precautions
Use proper safety precautions when using hazardous electrode materials and electrolytes.
Wear protective glasses and gloves to protect you against electrolyte that may accidentally
spill out during disassembly. Upon cell disassembly, dispose all materials properly. Metallic
lithium and some insertion compounds may decompose heavily in contact with water and
other solvents, and can cause fire.
Features
▪Gas inlet and outlet
▪Gas sample port
▪Gas pressure sensor, 0 to 3 bar abs

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5Assembly of the PAT-Cell-Gas
This section describes how to assemble the PAT-Cell-Gas test cell. A more detailed description of
the PAT-Core can be found in a separate manual.
Note: The assembly has to take place under the protective atmosphere in a glove box.
Screw cap
Sealing ring
Upper plunger
Upper electrode
Electrolyte
Insulation sleeve
Lower electrode (gas permeable)
Lower plunger with perforated
plate or flow field
Cell base

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1. Put the special lower plunger onto the worktop with the perforated plate / flow field
pointing upwards. Make sure that the O-ring seal at the bottom of the plunger is in place.
Make sure that the perforated plate is properly inserted on top of the plunger (only when
using the two-piece perforated version of lower plunger)
2. Put the insulation sleeve onto the worktop with the smaller side pointing upwards.
3. Insert the lower gas-permeable electrode into the sleeve with the active layer facing
downwards.
4. Push the lower plunger into the insulation sleeve.
5. Align the contact spring of the sleeve with the reference pin inside the cell base. Then
insert the assembly into the cell base.
6. Evenly dispense approx. 100 µL of electrolyte on top of the separator with a pipette.
Note: The optimum amount of electrolyte will depend on the thickness and porosity of the
separator and the electrodes used.
7. Insert the upper electrode into the insulation sleeve with the active layer facing
downwards.
8. Attach the upper plunger.
9. Attach the cell lid and tighten the wing nut in order to seal the cell. NOTE: Replace the lid
seal after each experiment. You can choose between different sealing materials: PE, PEEK,
PTFE and Al. PE has lower water permeability than PEEK, but significantly higher air
permeability. PE should not be used above 50°C. Al seals show the best overall
performance.
10. The cell can now be removed from the glovebox and connected to the peripheral
equipment such as gas supply and mass spectrometer.

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6Working modes of the PAT-Cell-Gas
There are two dedicated lower plunger available for the PAT-Cell-Gas for different testing
purposes.
6.1 Mode 1: Air mode
The lower plunger with perforated plate allows for electrochemical characterization of gas
diffusion electrodes used for instance in Li-air batteries. The lower electrode is contacted by
and “breathes” through the perforated stainless steel current collector supporting it. During
operation, the pressure gradient building up between cell headroom and the gas volume
below the perforated plate effectively prevents back-mixing. The relatively large volume below
the perforated is at the expense of time resolution, but makes this solution robust against
clogging of the gas path.
PAT-Core configuration example
Upper plunger (current collector), stainless steel
Counter electrode e.g. LFP
Insulation sleeve, PEEK with Separator and
reference electrode
Working electrode e.g. gas
diffusion electrode
Lower plunger (current collector) with
perforated plate, stainless steel
Gas flow inside the lower plunger

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6.2 Mode 2: OEMS mode
The PAT-Core setup using a lower plunger with flow field provides almost perfect plug-flow of
the purge gas being essential for quantitative time-resolved analysis. Gases evolved or
consumed at the working electrode may be analysed through the composition change of the
gas stream that is to be passed along the spiral-type flow field below the working electrode.
The composition of the outgoing gas can be analyzed by e.g. mass spectrometry. The pressure
gradient between cell headroom and spiral-type flow field effectively prevents back-mixing.
This and the tiny gas volume of the flow field ensure best possible time resolution.
PAT-Core configuration example
Upper plunger (current collector), stainless steel
Counter electrode e.g. LFP
Insulation sleeve, PEEK with
Separator and reference electrode
Working electrode e.g. gas
diffusion electrode
Lower plunger (current collector) with
flow field, stainless steel
Gas flow along the flow field

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7Disassembly and cleaning
When working with aprotic, moisture-sensitive electrolytes such as LiPF6, it is best to always
leave the cell base and cell lid in the glove box and only expose the PAT core components to
room air for cleaning or disposal.
Note that excess electrolyte may leak from the PAT-Core and cause contamination in the cell
base and on the contact pins. For standard electrodes and standard separators use 100 µl
electrolyte.
If the cell base or lid has been in contact with ambient air or if they are being used for the
first time, they must be dried in a vacuum at 80°C for at least 12 hours before use.
Stainless steel plungers can be cleaned with water, acetone, or ethanol. If necessary, persistent
stains can be removed from the plungers with aqueous nitric acid (20%, 2 hours at room
temperature). Insulating sleeves made of PP are intended for single use. Insulating sleeves
made of PEEK or PPS can be cleaned with water, acetone, or ethanol and are reusable after
careful drying (120°C, vacuum, >12 hours).
Never immerse the cell base in liquid. In particular, avoid contact of the electronic
components on the bottom of the cell base with liquid.
For the cell variants with pressure sensor (options P and SP),
the two adjacent holes at the top of the cell base (circeled in
the picture below) make connection to the laser welded
pressure sensor located inside the lower part of the cell base.
In order to avoid corrosion, no liquids must enter these holes
during cell assembly, cell operation and cleaning. Refer to the
troubleshooting section for help, if liquid did get into one of
the holes.
For the cell variants without pressure sensor, the two adjacent
holes are dead-ended. Still, avoid contamination with
electrolyte and other liquids.
Notes:
▪Protect yourself against chemical hazards. Electrolytes may spill out during cleaning.
Electrode materials and electrolytes may react with ambient atmosphere or solvents used
for cleaning. Wear appropriate protective equipment, goggles, and gloves.
▪Clean all cell parts right after disassembly. Leaving cell par ts in contact with the ambient
atmosphere while still being wetted with electrolytes may result in severe corrosion.
Holes towards the stainless steel
membrane of the laser welded pressure
sensor (options P and SP). For all other
options, these holes are dead-ended.
Avoid contact with electrolyte or
other liquids!

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8Sample valve with septum port (options S and SP)
The gas sample valve serves to draw gas samples for further characterization from the head
space of the test cell.
Gas sample port (PAT)
ECC1-00-0155-C
In the closed state, the valve spindle is seated on the PTFE ferrule and is thus preventing any
bleeding through the pierced septum.
8.1 How to draw gas samples
1. Pierce the septum with a sample syringe appropriate for the subsequent gas analysis with
e.g. a gas chromatograph. We recommend using a syringe with a pencil-point needle in
order to prevent clogging when the septum of the sample port is pierced. A 1 ml syringe
(LAB0024) and a pencil-point needle (LAB0039) are provided with the equipment.
2. Open the valve by turning the valve handle counter-clockwise by approx. 90 degrees
3. Fill the syringe by drawing back the syringe piston.
4. Close the valve by turning the valve handle clockwise till finger tight, and remove the
syringe.
Note: Do not connect the sample port directly or permanentely to an external device.
Valve Seating
PAT-Press
Ferrule 1.0
Valve Stem
Septum Thrust Screw II
Septum

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9Unpacking
Check the contents of the packages against the list given below to verify that you have
received all of the required components. Contact EL-CELL, if anything is missing or damaged.
NOTE: Damaged shipments must remain within the original packaging for freight company
inspection.
List of components
PAT-Cell-Gas:
▪PAT-Cell-Gas test cell without PAT-Core
Note: The components of the PAT-Core (insulation sleeves and plungers) must be purchased
separately.
▪Sealing ring PEEK (5x) ECC1-00-0232-D/V
▪Sealing ring PE (10x) ECC1-00-0232-A/X
PAT-Cell-Gas P:
▪PAT-Cell-Gas test cell without PAT-Core
Note: The components of the PAT-Core (insulation sleeves and plungers) must be purchased
separately.
▪Sealing ring PEEK (5x) ECC1-00-0232-D/V
▪Sealing ring PE (10x) ECC1-00-0232-A/X
PAT-Cell-Gas S:
▪PAT-Cell-Gas test cell without PAT-Core
Note: The components of the PAT-Core (insulation sleeves and plungers) must be purchased
separately.
▪Septum (10x) ECC1-00-0097-B/X
▪Syringe 1ml (w/o Luerlock) LAB0024
▪Spinal needle pencil-point (27g) LAB0039
▪Sealing ring PEEK (5x) ECC1-00-0232-D
▪Sealing ring PE (10x) ECC1-00-0232-A/X
▪Ferrule 1.0 (2x) ECC1-00-0029-B/2

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PAT-Cell-Gas SP:
▪PAT-Cell-Gas test cell without PAT-Core
Note: The components of the PAT-Core (insulation sleeves and plungers) must be purchased
separately.
▪Septum (10x) ECC1-00-0097-B/X
▪Syringe 1ml (w/o Luerlock) LAB0024
▪Spinal needle pencil-point (27g) LAB0039
▪Sealing ring PEEK (5x) ECC1-00-0232-D
▪Sealing ring PE (10x) ECC1-00-0232-A/X
▪Ferrule 1.0 (2x) ECC1-00-0029-B/2

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10 Spare parts and consumables
PAT-Cell-Gas SP, complete
Screw cap insulated (PAT), complete
ECC1-00-0236-D
Valve block I (PAT-Gas), assy
ECC1-00-0555-A
O-Ring 3mm x 1.5mm (AP370)
DIC9059
Cell bases divided (GAS), assy
ECC1-00-0530-E
Gas sample port (PAT), assy
ECC1-00-0155-C

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Screw cap insulated (PAT), complete
ECC1-00-0236-D

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Cell base divided (GAS), assy
ECC1-00-0530-E
Cell bases divided (GAS), assy
ECC1-00-0530-E
O-Ring 3mm x 1.5mm (AP370)
DIC9059

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Valve block I (PAT-Gas), assy
ECC1-00-0555-A
O-Ring 3mm x 1.5mm
DIC9059
Adapter flange 1/16“ (male), welded
ECC1-01-0071-C
O-Ring 1.5mm x 2mm
DIC9007
Valve body IV
ECC1-00-0391-D
Nut for 1/16 in. Swagelok Tube
Fitting
Quick connect set
ECC1-01-0080-A
Socket Screw
DIN 912 M 2,5x8