PIKE Technologies Jackfish User manual

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PIKE Technologies, Inc.
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Phone [phone]
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Web Site www.piketech.com
Mar 18, 2023

Contents
Introduction ......................................................................................................................1
Unpacking Your Accessory................................................................................................2
Cell Assembly....................................................................................................................2
JF Face-Angled Crystal Cell Base: Packing List...................................................................3
JF Face-Angled Crystal Cell Base: Assembly......................................................................4
JW ATR Wafer Cell Base: Packing List ...............................................................................8
JW ATR Wafer Cell Base: Assembly...................................................................................9
J1 Glass Cell: Packing List ................................................................................................14
J1 Options –Sold Separately...........................................................................................15
J1 Glass Cell: Assembling the Glassware.........................................................................16
J1 Reference Electrode Assembly...................................................................................17
J1 Reference Electrode Maintenance.............................................................................17
J2 Glass Cell: Packing List ................................................................................................18
J2 Options –Sold Separately...........................................................................................19
J2 Glass Cell: Assembling the Glassware.........................................................................19
Installing the Jackfish Cell Assembly onto the VeeMAX III .............................................20
Selecting the Angle of Incidence.....................................................................................21
Cleaning ..........................................................................................................................21
Support ...........................................................................................................................21

PN 350-1624710-02 P a g e | 1
Introduction
The Jackfish SEC Spectroelectrochemical Cell enables fundamental studies of the electrified metal-
solution interface and applications in molecular self-assembly, interfacial sensing, and next-generation
energy solutions. It is designed for surface-sensitive FTIR spectroelectrochemistry using the attenuated
total reflectance surface-enhanced infrared spectroscopy (ATR-SEIRAS) technique. High quality IR spectra
can be obtained from sub-monolayer amounts of adsorbed molecules. By controlling the electrical
potential applied to the Au thin film electrode on the ATR crystal surface, the user can perform vibrational
characterization of potential-dependent changes at the interface.
By design, the cell is fully compatible with the PIKE VeeMAX III variable angle ATR sampling accessory.
Two different crystals can be accommodated: the JF fits the PIKE face-angled crystal (FAC) and the JW is
designed for use with microgrooved ATR wafers. In a previous study investigating the adsorption of a
pyridine derivative, the spectral response was two times stronger when using Si 60 degrees FAC compared
to a Si hemisphere with an angle of incidence of 65 degrees. Additionally, the FAC exhibited higher energy
throughput and lower spectral noise. The short pathlength through the ATR wafers allows improved
signal-to-noise in the fingerprint region of the IR spectrum and a lower frequency cutoff compared to the
FAC.
Jackfish J1F Cell assembled on the VeeMAX III accessory.

PN 350-1624710-02 P a g e | 2
Unpacking Your Accessory
In order for you to quickly verify receipt of your accessory, we have included a packing list. Please
inspect the package carefully. Contact PIKE Technologies immediately if any discrepancies are found.
Cell Assembly
To assemble your cell, first follow the assembly instructions for your cell base type (JF or JW), and then
complete the assembly of the glassware (J1 or J2). The following table provides the relevant page
numbers for each cell model.
Cell Model
Cell Base
Glassware
J1F
JF: Face-Angled Crystal (p 3)
J1: (p 14)
J1W
JW: ATR Wafer (p 8)
J1: (p 14)
J2F
JF: Face-Angled Crystal (p 3)
J2: (p 18)
J2W
JW: ATR Wafer (p 8)
J2: (p 18)
Finally, proceed to Installing the Jackfish Cell Assembly onto the VeeMAX III (p 20), and read to the end
of the manual for information on cell cleaning.
First, assemble
the cell base.
Then move on to
the glassware.

PN 350-1624710-02 P a g e | 3
JF Face-Angled Crystal Cell Base: Packing List
JF Cell Base with Al Flange
PTFE or PEEK available
Quantity 1
JF PEEK FAC Holder
Color may vary
Quantity 1
Au-coated Pins
PN 162-4773
Quantity 6
#8-32 Stainless-Steel Screws
Perfluoro O-Ring (lower)
-012 round profile, black
Perfluoro O-Ring (upper)
-116 round profile, black
Quantity 12
Quantity 1
Quantity 1
#2-56 Stainless-Steel Contact Screws
Quantity 6
Viton™O-Ring (lower)
-012 square profile, black
Quantity 2
Viton™O-Ring (upper)
-116 square profile, black
Quantity 2
#2-56 Nylon Pin-Retaining Screws
Quantity 6
5/64” hex screwdriver
Quantity 1

PN 350-1624710-02 P a g e | 4
JF Face-Angled Crystal Cell Base: Assembly
1. Assemble Contact Pins
Use the 5/64” hex screwdriver to install the stainless-steel contact screws (#2-56) into the three
uppermost screw holes on the sides of the cell base (Fig. 1a). Tighten them until they bottom out at
the end of the blind hole. Place a gold contact pin in each hole on the bottom of the cell base. Verify
that the pin protrudes out from the bottom surface of the call base by approximately 2 mm (Fig. 1b).
If the screw does not protrude from the hole appreciably, it is likely the contact screw was
insufficiently tightened. Remove the pin, tighten down the contact screw, and check again. It is
recommended to measure the resistance between the pin and its corresponding screw to ensure
electrical contact. If the measurement reads open circuit but the pin protrudes correctly, try blowing
some compressed air through the holes to remove any plastic swarf or other foreign material that
may prevent good contact.
Fig. 1a) Cross section of J1,
flipped upside down so that
the gold pin doesn’t fall out.
Fig. 1b) Two of these pins protrude correctly,
however the third has sunk to the bottom of
the hole because the contact screw was
tightened inadequately.
One by one, depress each pin and screw in a nylon #2-56 screw into the remaining (lower) hole
corresponding to the compressed pin. This screw acts as a set screw to retain the gold pin. The gold
pin should remain compressed once this screw is fastened down (Fig. 1c).
Fig. 1c) The nylon set screw retains the gold pin in the compressed state.
Gold pin
Set Screw Hole
Contact Screw
Contact Screw
Nylon Pin-Retaining Screw
Gold pin

PN 350-1624710-02 P a g e | 5
2. Assemble the Cell Base
It is recommended to apply one or two wraps of Teflon tape to the threads on the cell base. This will
provide some torsional resistance, preventing the flange from unscrewing in the subsequent steps. Screw
the aluminum flange onto the threaded PEEK/PTFE cell base. Ensure the threads are properly aligned to
prevent cross-threading the cell base. The bottom of the cell base needs to be flush with the aluminum
flange and the O-ring (-012) should protrude beyond the aluminum flange to ensure a proper seal with
the crystal surface (Fig. 2a).
Fig. 2a) Side view. Ensure the Al flange is flush
with cell base and O-Ring protrudes slightly from
base.
Fig. 2b) Top-down view.
3. Fasten Glass Body to Cell Base
Insert the large black O-ring (-116) into the PEEK/PTFE cell base (Fig. 2b). Thread the glass cell body
into the base until it bottoms out and seals against the O-ring, being careful not to overtighten. You
should not need to tighten more than 45 degrees (1/8th of a turn) past the point where you start to
feel resistance.
Fig. 3a) Side view.
Fig. 3b) Top down view.
Short Bubbler Joint
Reference Arm Joint
Clearance
holes
Al Flange Screw Holes
-116 O-Ring
Contact Screw
Pin-Retaining Screw
-012 O-Ring

PN 350-1624710-02 P a g e | 6
4. Load the Crystal
Place the Au coated face angled crystal in the holder and place in the VeeMAX III top plate (Fig. 4a
and 4b).
Fig. 4a) Orientation of FAC in crystal holder.
IMPORTANT: Remove the top plate from the VeeMAX III and secure to ensure it does
not shift during assembly. The assembly and initial filling of the cell with electrolyte
needs to be done off the VeeMAX III. This is to avoid damage to the VeeMAX III if a leak
occurs.
IMPORTANT: When placing the crystal holder with the FAC in the top plate, be sure
the FAC is oriented correctly to allow for incident light through the FAC (Fig. 4b).
Fig. 4b) Orientation of FAC in crystal holder in top plate.
IR Beam Incident
IR Beam Incident

PN 350-1624710-02 P a g e | 7
5. Attach the Cell
Carefully fasten the cell assembly onto the VeeMAX III Jackfish top plate (specialized plate with round
pocket to accommodate the Jackfish Cell) using the six screws (#8-32) provided. These screws are best
fastened by hand (finger tight), although a 9/64” hex drive may be used if additional sealing force is
required. Be sure to stabilize the cell and evenly tighten the screws in a star pattern to distribute
pressure evenly while tightening (Fig. 5). Tighten each screw with a 1/4 turn on each rotation to ensure
an even distribution of pressure.
Fig. 5) Order for tightening screws to apply and even sealing force.
6. Making Contact with the Crystal
Loosen each of the three nylon pin-retaining screws (the lower screws only) counter-clockwise several
full turns. This allows the spring-loaded pin to extend and make contact with the electrode surface.
You may hear a click as the pin engages. Check for electrical contact by measuring the resistance
across the three contact screws (the upper screws).
Fig. 6) Cross section of the cell assembled atop the crystal.
The Aluminum flange and crystal holder are omitted for clarity.
Contact Screw
Pin-Retaining Screw (loose)
Gold pin
Glass Body
-116 Upper O-Ring
-012 Lower O-Ring
Face Angled Crystal
1
2
3
4
5
6

PN 350-1624710-02 P a g e | 8
JW ATR Wafer Cell Base: Packing List
JW Cell Base
PTFE or PEEK available
Quantity 1
JW PEEK Wafer Holder
Color may vary
Quantity 1
Au-coated Pins
PN 162-4732
Quantity 4
#8-32 Stainless Steel Screws
Perfluoro O-Ring (lower)
-010 round profile, black
Perfluoro O-Ring (upper)
-116 round profile, black
Quantity 12
Quantity 1
Quantity 1
#2-56 Stainless Steel Contact Screws
Quantity 6
Viton™O-Ring (lower)
-010 round profile, white
Quantity 2
Viton™O-Ring (upper)
-116 square profile, black
Quantity 2
#2-56 Nylon Pin-Retaining Screws
Quantity 6
5/64” hex screwdriver
Quantity 1

PN 350-1624710-02 P a g e | 9
JW ATR Wafer Cell Base: Assembly
1. Assemble Contact Pins
Use the 5/64” hex screwdriver to install the stainless-steel contact screws (#2-56) into the uppermost
screw holes on the sides of the cell base (Fig. 7a). Tighten them until they bottom out at the end of
the blind hole. Place a gold contact pin in each hole on the bottom of the cell base. Verify that the pin
protrudes out from the bottom surface of the call base by approximately 2 mm (Fig. 7b). If the screw
does not protrude from the hole appreciably, it is likely the contact screw was insufficiently tightened.
Remove the pin, tighten down the contact screw, and check again. It is recommended to measure the
resistance between the pin and its corresponding screw to ensure electrical contact.
Depress each pin and install a nylon #2-56 screw into the remaining (lower) hole for that pin. This
screw acts as a set screw to retain the gold pin and the gold pin should remain compressed once this
screw is fastened down (Fig. 7c).
Fig. 7c) The nylon set screw retains the gold pin in the compressed state.
Fig. 7a) Cross section of JW,
flipped upside down so that the
gold pin doesn’t fall out.
Fig. 7b) The right pin protrudes correctly,
however the left pin has sunk to the
bottom of the hole because the contact
screw was tightened inadequately.
Contact Screw
Pin-Retaining Screw
Gold pin
Gold pin
Set Screw Hole
Contact Screw

PN 350-1624710-02 P a g e | 10
2. Assemble the Cell Base
Insert the large black O-ring (-116) into the cell base. Thread the glass cell body into the base until it
bottoms out and seals against the O-ring, being careful not to overtighten. You should not need to
tighten more than 45 degrees (1/8th of a turn) past the point where the cell starts to feel tight. Insert
the small white O-ring (-010) into the pocket on the underside of the body, pressing firmly to ensure
it is level and seated properly. The O-ring should be nearly flush with the body.
Fig. 8a) Side view of JW.
Fig. 8b) Top view of JW.
Short Bubbler Joint
Reference Arm Joint
Clearance
holes

PN 350-1624710-02 P a g e | 11
Side Note: How to Identify the Face Angle of a Wafer
Microgrooved wafers are available in a choice of two different face angles: 35° and 55°. To identify
the face angle of the wafer, observe the ends of the grooves. The ends of the 55° grooves are square,
while the ends of the 35° grooves are capped by a triangle. The orientation of the grooves with respect
to the wafer length and width is not a reliable indicator of the face angle. Please use the ends of the
grooves to identify the wafer face angle.
The ends of the 35° groove profile are triangular.
The ends of the 55° groove profile are square.
3. Orienting and Sealing the Wafer in the Cell
The microgrooved wafers can be installed such that the grooves are either parallel or perpendicular
to the incident beam. The performance is comparable for both orientations for most applications.
If one orientation is preferred for a given set of experimental conditions, take note of the direction of
the grooves with respect to the side-lengths of the wafer. (Some batches of wafers have the grooves
aligned parallel to the long side-length of the wafers, while other batches have the grooves aligned
parallel to the short side-length.) Place the wafer holder in the VeeMAX III top plate and place the
wafer groove-side down in the holder. Rotate the wafer holder in the pocket of the VeeMAX top plate
such that the incident beam is oriented with respect to the grooves according to the desired result.
Use the table below as a guide to aid installation.
IR beam parallel to grooves
IR beam perpendicular to grooves
Wafer grooves
are parallel to
short side-
length.
Wafer grooves
are parallel to
long side-
length.
Alignment nub faces front of VeeMAX.
Alignment nub faces side of VeeMAX.
IR beam
incident
IR beam
incident
IR beam
incident
IR beam
incident
Alignment nub faces side of VeeMAX.
Alignment nub faces front of VeeMAX.

PN 350-1624710-02 P a g e | 12
IMPORTANT: The wafers are brittle and can easily snap if mishandled. To avoid wafer
breakage, ensure that the pins are flush with the body and the O-ring is level and as deep in
its pocket as possible. In the next steps, avoid twisting motions or applying uneven pressure
to one side of the cell.
Orient the body so that the groove is over top of the tongue on the wafer holder (Fig. 10). Carefully slide
the tongue into the groove, holding the cell at an angle to avoid scratching or moving the wafer. Then,
gently lower the body onto the wafer so that it is sandwiched between the body and the wafer holder.
Fig. 10) Sealing the wafer in the cell. This step should be done with the wafer holder
installed in the VeeMAX III top plate (not shown for clarity).
4. Fasten the Cell to the Top Plate
Carefully install the #8-32 screws through the clearance holes and into the VeeMAX III top plate, but
do not tighten them completely yet. Note: depending on the orientation of the wafer, you will need
either four or six screws to fasten the cell onto the top plate. When all the screws are in place, grip the
cell by the base and gently push down to compress the O-ring against the wafer. Working in a star
pattern (Fig. 5 in the JF Face-Angled Crystal Cell Assembly section), tighten each screw ¼ to ½ turn,
working your way around the cell until each screw is snug but not tight against the body. Do not over
tighten the screws –this risks breaking the wafer! The O-ring is very soft, so only moderate pressure
is needed to maintain a good seal. Test the seal by pipetting 1 or 2 mL of solution into the cell and
observing for several minutes.
5. Making Contact with the Wafer
Loosen each nylon pin-retaining screw several turns to back it off the pin. You may hear a small click
as the pin springs open and contacts the wafer surface. Check for proper contact by measuring the
resistance across the two stainless-steel contact screws.

PN 350-1624710-02 P a g e | 13
Fig. 11) Cross section of the JW cell assembled atop the crystal.
The wafer holder is omitted for clarity.
IMPORTANT: There is a small chance of breaking a wafer due to the impact of the pin. To
eliminate this chance, it is possible to omit the nylon pin-retaining screws during assembly.
It is challenging to assemble the cell by this alternative method since neither the pins nor the
wafer are held in place. The basal plane of the cell needs to be held nearly vertically (Fig. 12).
Take care that the wafer does not fall out and break.
It will not be possible to reliably use an electroless deposited film using this “omitted nylon
screw” method, since the pins can scrape the film and damage it during assembly,
preventing electrical contact.
Fig. 12) Alternative, more challenging assembly method to mitigate
the risk of breaking wafers without using the nylon pin-retaining screws.
Contact Screw
Set Screw (loose)
Gold pin
Glass Body
-116 Upper O-Ring
-010 Lower O-Ring
Microgrooved wafer

PN 350-1624710-02 P a g e | 14
J1 Glass Cell: Packing List
User Manual
Jackfish SEC Cell Body
Reference Arm with Stopcock
PN 350-1624710
PN 162-4749
PN 162-4734
Quantity 1
Quantity 1
Quantity 1
Exhaust Gas Trap
Cell Cap with Ports
Cell Cap, blank
PN 162-4740
Quantity 1
Quantity 1
Quantity 1
Long Bubbler
Short Bubbler
Stopper
PN 162-4736
PN 162-4738
Quantity 2
Quantity 3
Quantity 4

PN 350-1624710-02 P a g e | 15
Stopcock Clip
Reference Arm/Cell Body Spring
Quantity 1
Quantity 1
Use to secure stopcock
in reference arm
J1 Options –Sold Separately
Ag/AgCl Reference Electrode
Pt Counter Electrode
Au Counter Electrode
PN 162-4723
PN 162-4720
PN 162-4722
Quantity 1
Quantity 1
Quantity 1

PN 350-1624710-02 P a g e | 16
J1 Glass Cell: Assembling the Glassware
NOTE: The ground glass joints seal best when they have a thin layer of water between. This is especially
important on the stopcock to ensure it rotates properly. It is recommended to wet all the ground glass
surfaces before assembly.
1. Attach the reference arm with the stopcock to the cell body and secure it with the spring.
2. After filling the cell with electrolyte place the bubblers, gas trap, and counter electrode in the
cell. The port for the long bubbler is indicated with a glass nodule (Fig. 13). Best practice is to
have the reference arm stopcock closed when first filling the cell with electrolyte and during the
subsequent step.
3. Purge the cell with inert gas for at least 30 minutes to ensure there are no leaks and remove dissolved
oxygen before fastening the assembled cell on the VeeMAX III. After the solution is purged, open the
stopcock while plugging the hole on the gas trap to fill the reference arm.
Close the stopcock when sufficient solution is in the reference arm.
NOTE: The absolute orientation of the side ports with respect to the VeeMAX III is not critical. Do not
overtighten the cell body onto the cell base trying to obtain a particular alignment of the side ports.
Electrolyte Maximum Fill
Port for long bubbler
indicated with glass nodule
Fig. 13) Complete J1F cell assembly.