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Fra32m

Manufactured by Metrohm
Sourced in Netherlands

The FRA32M is a Frequency Response Analyzer designed for electrochemical impedance spectroscopy measurements. It is capable of performing high-precision impedance measurements over a wide frequency range.

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6 protocols using fra32m

1

Electrochemical Characterization of Energy Storage Devices

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Electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV) were performed with a Metrohm Autolab equipped with M101 potentiostat/galvanostat and FRA32 M modules. Galvanostatic measurements were performed with Arbin BT2000. Temperature tests were accomplished in a Memmert Oven UN30 with side opening for electrical cables. Electrolyte stability was studied by CV performed at 5 mV s−1 while increasing the window stepwise after every 10 cycles. These tests were run in three‐electrode configuration. From these measurements we obtained the electrode mass ratio in order to exploit the full electrolyte stability window. Then, we moved to device characterization. We performed at first CVs at several scan rates and EIS with Vp=5 mV and frequencies ranging from 1 MHz down to 10 mHz acquiring five points per decade. Galvanostatic measurements were run following an initial protocol aimed to evaluate the device rate capability, and then the cells were left cycling for 50000 cycles. Floating tests were also performed in order to evaluate device endurance under constant high‐voltage conditions.
Capacitances were derived from the energy, which was computed according to Equation 1: E=VtItdt
and using Equations (2) and 3: E=12Q2C
Q=Itdt
The power was calculated by applying Equation 4: P=EΔt
where Δtrepresents the discharge time, since all quantities were computed in discharge.
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2

Electrochemical Detection of L-Cysteine and SARS-CoV-2 Spike Protein

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All electrochemical measurements were performed in an AutoLab PGSTAT204 potentiostat/galvanostat with an impedance module FRA32M managed by NOVA 2.1.4 software (Metrohm, Utrecht, Netherlands). Cyclic voltammetry (CV) measurements were performed from 0.0 to +1.2 V, at a scan rate of 50 mV s−1, and chronoamperometry measurements at an applied potential of +0.55 V were used for the determination of L-cysteine. On the other hand, electrochemical impedance spectroscopy (EIS) was recorded from 100 kHz to 0.10 Hz, with an amplitude of 10 mV, and square wave voltammetry (SWV) measurements were performed with an amplitude of 80 mV, a frequency of 80 Hz, and a step potential of 10 mV. EIS and SWV were applied for the detection of the SARS-CoV-2 spike protein. For these analyses, 0.10 mol L−1 KCl (pH 7.0) was used as a supporting electrolyte, and an equimolar mixture of 5.0 mmol L−1 [Fe(CN)6]3−/4− was applied as a redox probe. The EIS measurements were calibrated by normalized impedance change (NIC%) [43 (link),44 (link)] concerning the control. The NIC% value was calculated using Equation (1), where, in this case, Zcontrol is the magnitude of charge transfer resistance (Rct) for a control sample without the antigen, and Zsample is the magnitude of Rct for each added point of concentration of the antigen.
NIC%=ZsampleZcontrolZcontrol×100      
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3

Electrochemical Characterization of Carbon-Paste Electrodes

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Voltammetric measurements were performed using a potentiostat/galvanostat PGSTAT® model 204 with module FRA32M (Metrohm Autolab) integrated with NOVA 2.1® software. The measurements were performed in a 25 mL one-compartment electrochemical cell, with a three-electrode system consisting of carbon-paste electrodes (CPEs) described in Table 1, and Pt wire and Ag/AgCl/KClsat (both purchased from Lab solutions, São Paulo, Brazil) representing the working, counter, and reference electrode, respectively. The carbon paste was mechanically renewed with every new analysis performed.
The experimental conditions for differential pulse voltammetry (DPV) were as follows: pulse amplitude = 25 mV, pulse width = 0.5 s, and scan rate = 10 mV s−1. The experimental conditions for cyclic voltammetry (CV) were as follows: scan rate = 50 mV s−1 and scan range from −0.4 to 1.4 V. The DPV were background-subtracted and baseline-corrected, and then all data were analyzed and treated with the software Origin 8®. All experiments were performed at room temperature (25 ± 2 °C) in triplicate (n = 3) and the main electrolyte used was the 0.1 mol L−1 KCl, 0.1 mol L−1 phosphate buffer solution (PBS) at pH 7.0.
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4

Characterization of Device Performance

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The device performance, including the transfer curves (drain–source current IDSversus gate-source voltage VGS), was characterized using a semiconductor device parameter analyzer (B1500A, Keysight). The transfer curves were recorded at a fixed drain-source voltage (VDS = 0.1 V) and by varying the gate-source voltage (VGS = 0–1 V) at a sweeping rate of 0.01 V s−1. Solutions of free chlorine were freshly prepared by diluting sodium hypochlorite pentahydrate, NaClO·5H2O (Tokyo Chemical Industry Co. Ltd, Japan), in DI water and their NaClO concentrations were standardized using a photometric free chlorine meter (AQUAB AQ-202P, SIBATA Scientific Technology Ltd, Japan). Phosphate buffer solution (PBS) was prepared with sodium dihydrogen phosphate dihydrate and disodium hydrogen phosphate (FUJIFILM Wako Pure Chemical Corp., Japan). The electrochemical properties were evaluated by cyclic voltammetry and electrochemical impedance spectroscopy measurements using an Autolab PGSTAT204 potentiostat/galvanostat system equipped with an impedance analyzer FRA32M (Metrohm, Utrecht, The Netherlands).
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5

Dielectric Relaxation Spectroscopy of Membranes

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DRS was performed
with a Metrohm FRA32M frequency response analyzer coupled to an ECI10M
impedance interface and a custom-built (in-house) two-electrode cell
(Figure S17). The cell was placed inside
the aforementioned Espec BTU-433 controlled-temperature/humidity chamber
to maintain constant conditions (between 30 and 150 °C and 30%
RH) during each measurement. Sample membranes of ∼12 mm diameter
and 1 mm thickness were sandwiched between 304L stainless steel electrodes
separated by a 1 mm thick PTFE spacer. Electrodes were polished to
a mirror finish with 8000-, 14 000-, and 60 000-mesh
diamond paste (Sandvik Hyperion; Worthington, OH) prior to use. For
each sample, dielectric/impedance spectra were collected at various
temperatures using a frequency range of 1–107 Hz
and alternating current amplitude of ±0.01 V. The stray admittance
and residual impedance of the test cell were evaluated by open cell
(no sample) and shorted cell measurements, respectively, using the
same experimental conditions outlined above; shorted measurements
were performed using a 12 mm dia by 1 mm thick disk of 99.99% pure
Cu as the sample. Compensations for stray admittance and residual
impedance were applied to all data via Excel, as outlined elsewhere.49 Additionally, all measured values of real dielectric
(ε′) were corrected for contribution from the spacer
according to the method described by Johari.50 (link)
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6

Intensity-Modulated Photocurrent Spectroscopy and Transient Absorption Spectroscopy

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Intensity-modulated photocurrent spectroscopy (IMPS) was implemented with a potentiostat (PGSTAT302N, Metrohm), an impedance analyzer (FRA32M, Metrohm), and a light-emitting diode (LED) driver kit (Metrohm) that drove illumination of 420-nm power UV LED in 1 M KOH at various voltages. Transient absorption spectroscopy (TAS) measurements were carried out on Helios (Ultrafast systems) spectrometers using a regeneratively amplified femtosecond Ti: sapphire laser system (Spitfire Pro-F1KXP, Spectra-Physics; frequency, 1 kHz; max pulse energy, ~8 mJ; pulse width, 120 fs), and the experimental results were examined using ultrafast systems commercial software (Surface Xplorer). An individual three-exponential decay model was used to calculate the fits of the decay. The measured decay dynamics was calculated the amplitude weighted average life (τav) using the equation of τav=SUM[Ai×τi]SUM[Ai]  , where Ai is the amplitude of the component with lifetime (τi), and τi is the amplitude weighted lifetime.
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