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38 protocols using tbapf6

1

Drying and Purification of Electrochemical Reagents

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All experiments were performed
in dried glassware under an Ar atmosphere unless stated otherwise.
1,2-Dimethoxyethane (DME) (CHROMASOLV, for HPLC grade, Sigma-Aldrich)
was dried over activated basic Al2O3, filtered,
and distilled over liquid Na/K alloy. Caution: All steps involving
Na/K alloy should be carried out with extreme caution under strict
exclusion of air or moisture, under inert gas and appropriate personal
protection (hood, blast shields, face shield, protective, and fire-resistant
clothing) should be used and worn at all times. Tetrabutylammonium
hexafluorophosphate (TBAPF6) (for electrochemical analysis,
Sigma-Aldrich) was dried in vacuum (∼10–2 mbar) at 100 °C for 24 h. TBAPF6 (0.15 M) in DME
was prepared in a glovebox and used without further purification.
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2

Electrochemical Characterization of Carbon Cloth

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Electrochemical measurements were conducted in methanol (Sigma‐Aldrich, assay GLC≥99.9 %) with tetrabutylammonium hexafluorophosphate (TBAPF6 0.1 M) as supporting electrolyte. TBAPF6 (Sigma‐Aldrich, 98 %) was recrystallized twice from hot ethanol and dried before use. A single compartment cell was used for CV measurements. The pristine carbon cloth, CC, (GPP050 M, Cetech Co. ltd) was cut in pieces of 3.4 cm2 and ultrasonically cleaned in 50 % wt 2‐propanol solution in Milliq water for 15’ and in pure Milliq water for additional 20’, then dried in an oven at 60 °C for one hour, in a similar manner as previously reported.[23b] A double compartment cell was used for CPE measurements. CC was employed as working electrode, alongside a Pt counter electrode and an Ag/AgCl (KCl 3 M) as reference electrode. Under our experimental conditions, the reference ferrocene/ferrocenium (Fc/Fc+) redox is at E1/2=0.40 V (ΔEp=65 mV) vs. Ag/AgCl.
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3

Cyclic Voltammetry and Differential Pulse Analysis

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Cyclic voltammetry was carried out in argon-purged (>10 min) acetonitrile with 0.10 M TBAPF 6 (Sigma-Aldrich) in a conventional three electrode setup, with a platinum disk working electrode, a rod-shaped glassy carbon auxiliary electrode and a salt-bridged (acetonitrile/0.1 M TBAPF 6 ) SCE reference electrode. A scan speed of 0.1 V s -1 was used. Irreversible reductions were evaluated by differential pulse voltammetry. Subsequent to measurement, ferrocene was added as an internal standard, and the Fc 0/+ couple appeared at +417.5 mV with a peak-to-peak separation of 114 mV. The differential pulse voltammetry for the reductions were collected using pulse width 60 ms, pulse period 200 ms, pulse amplitude 50 mV and sampling width 20 ms.
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4

Electrochemical CO2 Reduction: Protocols

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Acetonitrile used for the experiments was freshly distilled over calcium hydride and purged with Ar before use. 0.5–1 mM solutions of the complexes were prepared with tetrabutylammonium hexafluorophosphate (TBAPF6, Sigma-Aldrich, 98%) as supporting electrolyte (0.1 M). A single-compartment cell was employed for CV measurements, equipped with working a glassy carbon electrode (GCE, Ø = 1 mm), alongside a Pt counter electrode and a Ag/AgCl (KCl 3 M) reference electrode. The Ar- and CO2-saturated conditions were achieved by purging gases for 5 min before each potential sweep. A double-compartment H-type cell was used for CPE measurements, thus allowing to separate through a glass frit the anodic compartment from the cathodic one (a Pt wire is placed as counter electrode). A glassy carbon rod is employed as working electrode jointly with the Ag/AgCl reference electrode. A controlled and constant flow of CO2 (50 mL min−1) was maintained during the CPE measurements by means of a Smart Trak 100 (Sierra) flow controller. Under these experimental conditions, the redox couple (Fc+/Fc) is located at E1/2 = 0.35 V.
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5

Synthesis of P3HT and NaPSS Polymer Blends

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P3HT
was purchased from Merck (Mn = 24 kg mol–1, PDI = 1.8, regioregularity
= 95.9%). Sodium polystyrenesulfonate (NaPSS) was purchased
from Sigma-Aldrich. Mo(tfd-COCF3)3 was synthesized
as previously described.26 (link) Anhydrous acetonitrile
(AcN; purity >99.9%), chloroform (CHCl3; purity >99.5%), o-dichlorobenzene (oDCB; purity >99%), and TBAPF6 were purchased from Sigma-Aldrich and used as received.
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6

Electropolymerization of Electrochromic PEDOT:PSS

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Electropolymerization of electrochromic polymer PEDOT:PSS was performed using a three-electrode configuration. A custom-made platinum coil (Alfa Aesar, 13039) and Ag/AgCl (Warner Instruments, 64-1282) were used as the counter electrode and reference electrodes, respectively. Conducting substrate was used as the working electrode. An aqueous solvent of 10 mM EDOT monomer and 0.1 M NaPSS was deposited using a galvanostatic approach. A constant current of 0.48 mA/cm2 was applied for 1.67 s for each 5-nm PEDOT:PSS film (fig. S4). Electropolymerization process was confirmed by CV measurements in 0.1 M TBAPF6 (Sigma-Aldrich, 281026) in propylene carbonate solution (Sigma-Aldrich, 310328). Selective deposition of PEDOT:PSS on the Au surface was achieved using the same aqueous solvent solution under potentiostatic conditions (740 mV versus Ag/AgCl) for 6.5 s.
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7

Synthesis and Electrochemical Evaluation of Nickel Complexes

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Tetra(n-butyl)ammonium hexafluorophosphate,
(TBA)PF6; ethanol, EtOH; and anhydrous acetonitrile used
were of electrochemical grade and purchased from Sigma-Aldrich. Sodium
hydroxide (NaOH) used was of analytical grade and purchased from POCH.
The carbon paper FuelCellsETc was purchased from College Station,
TX. The NiSaltMe and meso-NiSaldMe monomers were
synthesized according to the procedure described elsewhere.30 (link),35 (link),40 (link)
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8

Electrochemical Polymerization of Pyrrole

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Sodium dodecylbenzenesulfonate (NaDBS, 99%), ethylene glycol (EG, 99.8%), tetrabutylammonium hexafluorophosphate (TBAPF6, >99%), phosphotungstic acid hydrate (PTA, PW12O403−, reagent grade), and propylene carbonate (PC, 99%) were supplied from Sigma-Aldrich (Taufkirchen, Germany). Commercial Durapore (Millipore, 0.22 μm, Sigma-Aldrich) was used as supplied. Pyrrole (Py, 98%) from Sigma-Aldrich was distilled prior to use and stored at a low temperature (−20 °C) in the dark under a nitrogen atmosphere. Milli-Q+ (Tallinn, Estonia) deionized water was used as supplied.
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9

Resistin ELISA Assay Protocol

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Tetrabutylammonium
tetrafluoroborate (TBAPF4), sodium perchlorate/lithium
perchlorate (NaClO4/LiClO4), and tetrabutylammonium
hexafluorophosphate (TBAPF6) were from Sigma-Aldrich. Anti-resistin
antibody (0.75 mg/mL), resistin from mouse (25 ug), neuron-specific
enolase human (NSE, 10 μg), vascular endothelial growth factor
(VEGF), calreticulin human (CALR, 10 μg), p53 protein human
(50 μg), GM2-activator protein (GM2A, 3.70 mg/mL), human serum,
and bovine serum albumin (BSA) were from Sigma-Aldrich. Elabscience
Biotechnology Inc. (USA) provided the ELISA Resistin kit.
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10

Photoelectrochemical Water Splitting System

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All reagents,
including pyrrole, pentylbenzene, methyl 4-formylbenzoate, acetic
acid 99%, Hemin ≥96%, acetonitrile and N,N-dimethylformamide anhydrous 99.8% (ACN and DMF), triethanolamine
99% (TEOA), tetrabutylammonium hexafluorophosphate ≥99.0% (TBAPF6), 2,6-lutidine, and iron(II) bromide (FeBr2) were
purchased from Sigma-Aldrich and were used as received without further
purification. TBAPF6 was dried under vacuum before use.
FTO conducting glass substrates (TEC 15 Ω/cm2 resistance)
were purchased from Xop Glass, Castellón, Spain. Nanocrystalline
titania paste was purchased from Dyesol (30NR-D titania paste, 20
nm particle size). Aluminum oxide, 20% in H2O, colloidal
dispersion was purchased from Alfa Aesar.
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