PIKE Technologies Jackfish User manual

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Address Comments to:

PIKE Technologies, Inc.

6125 Cottonwood Drive

Madison, WI 53719

Phone (608) 274-2721

Fax (608) 274-0103

E-mail [email protected]

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

#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

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

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