Growth of Chitosan nano brushes using FMED as electropolymerization method

Eric S McLamore, Maria J Torres, Lidadi Agbomi

Published: 2024-06-21 DOI: 10.17504/protocols.io.eq2lyjz6elx9/v1

Disclaimer

Abstract

This protocol describes the electropolymerization of chitosan nanobrushes in the working electrode of a Laser-induced graphene (LIG) sensor. The process requires approximately 36 minutes (including baseline analysis). The electropolymerization times are not included in this protocol. A 2-channel function / arbitrary waveform generator (SINGLENT SDG 1032X) was used throughout this protocol.

This protocol uses the Microwave Synthesis of the low molecular weight deacylated chitosan protocol as an electropolymerization solution in the working electrode of an LIG. See the protocol below.

Microwave synthesis of low molecular weigth deacylated chitosan

Before start

Be sure to wear appropriate safety PPE throughout (lab coat, gloves, eyewear).* Electronic or physical lab notebook may be used throughout

See experimental plan guide for tips on planning your work

Steps

SECTION 1) Preparation

Prepare a glass cell vial with lower molecular weight deacylated chitosan solution.

Previous microwave-assisted synthesis of lower molecular weight deacylated chitosan solution prepared is required required following the next protocol ( Link here) :

Microwave synthesis of low molecular weigth deacylated chitosan

Note

Storage the solution at 4°C for at least 24h 0m 0sThis will ensure the density of the solution is accurate for electropolymerization.

Set up the work conditions in the SINGLET SDG1032X.

Figure 1. A) SIGLENT wave generator panel of options, including ON/OFF button, conditions panel (left bottom), the panel of numbers (upper right), output signal button (bottom right), and activation of parameters (middle bottom). B) Selecting the parameter conditions measurement units.

Turn on the SIGLET wave generator by pressing the "ON/OFF" button once and wait until the equipment turns on completely.

Note

Set up the conditions for the electropolymerization as follows:Frequency 500 HzAmplitude 5.0 VppOffset 5.0 VdcPhase 0.0 gradesHarmonic OFFWaveform SINE

Press the waveform button (See Fig. 1A ) to select the Sine waveform for the conditions using the same procedure mentioned in this note.

Note

NOTE 1: To set up the conditions in each category, press the condition button once (Fig. 1A, bottom left) , introduce the number for the condition in the number panel (Fig. 1A, upper right) , select the measurement unit, press in the option that you wanted and change to the next to the right button (Fig. 1B, center bottom ) to make changes in the other conditions.NOTE 2: It is recommended to ensure the parameters button is activated (to know if it is activated, it must be green).

SECTION 2) Electropolymerization using FMED method

Conduct an electropolymerization

Add in a glass cell vial the 8000µLof the previous lower molecular weight deacylated chitosan solution.

Figure 2. A) Set up the clips for the wave signal generation. B) Connection to the Laser-Induced Graphene (LIG) sensor in the working electrode for the FMED of Chitosan nanobrushes.
Introduce the three-electrode LIG sensor in the digital oscilloscope clip in the lower molecular weight deacylated chitosan solution (Fig. 2A).

Figure 3. Laser-Induced Graphene (LIG) sensor, a three-electrode system (reference, working and counter electrode)
Connect the alligator clip to the working electrode of the Laser-Induced Graphene (LIG) sensor. Ensure it is connected correctly in the middle of the metal tape of the working electrode.
Introduce the LIG sensor in the lower molecular weight deacylated chitosan solution.

Note

Introduce the bottom part of the LIG sensor, ensuring that the working electrode (black circle, Fig. 3 ) is completely submerged in the solution (Fig. 2B ).

Figure 4. Output signal button. Green light indicates that itis active and functioning.

Set up the time with a timer for the FMED electropolymerization of lower molecular weight deacylated chitosan in the working electrode of the LIG sensor. Start the time and, at the same time , press the Output button ( Fig. 4 ). Be sure that the output button is ON (A green light indicates that it is already working).

Note

Critical step Stop the timer when the time is already complete. At the same time , press the "output" button to stop the wave generator and the FMED electropolymerization.

SECTION 4) Stabilization and storage

Wash, dry and storage the sensor

Clean the LIG working electrode with DI/nano-pure water and dry the water carefully without touching the sensor electrodes. Dry from the sides with a kimitech wipe.
Let it dry for 0h 5m 0s in a paper towel and then storage the sensor in the fridge at 4°C

SECTION 5) Clean up

Clean up space and dispose of waste

Turn off the SIGLENT Wave generator and unplug it from the power outlet.
Dispose of used chemicals according to the lab safety plan. Chitosan has a dedicated chemical disposal container.

Note

Chitosan has a dedicated chemical disposal container in the waste area.

Wash all glass containers used in the experiment and let it dry.

Growth of Chitosan nano brushes using FMED as electropolymerization method

Disclaimer

Abstract

Before start

Steps

SECTION 1) Preparation

SECTION 2) Electropolymerization using FMED method

SECTION 4) Stabilization and storage

SECTION 5) Clean up

推荐阅读