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45 protocols using nafion 117

1

Synthesis of Ir/C and IrO2 Ink Catalysts

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To prepare the Ir/C ink, 11 mg of Ir/C (5 wt% of Ir, Premetek Co.) was dispersed in 1 ml of water and ethanol solution (1:4, v/v), followed by the addition of 45 μl of Nafion 117 solution (Sigma-Aldrich). The mixture was then magnetic stirred to form a homogenous ink. Meanwhile, the IrO2 ink was also prepared, namely 5.14 mg of IrO2 and 5 mg of Ketjen Black dispersed in 1 ml of water and ethanol solution (1:4, v/v), followed by the addition of 40 μl of Nafion 117 solution (Sigma-Aldrich). The mixture was then sonicated briefly to form a homogenous ink. The ink was drop-casted onto the Ni foam and Ni/Audisc electrodes and left dried in air.
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2

Electrochemical Sensing of Biomolecules

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Chloroauric acid (HAuCl4), d-glucose, copper(ii) chloride, sodium hydroxide (NaOH), uric acid (UA), l-glutamic acid, ascorbic acid (AA), dopamine (DA), sodium phosphate dibasic (Na2HPO4), sodium phosphate monobasic (NaH2PO4), and Nafion™ 117 (approximately 5% in a mixture of lower aliphatic alcohols and water) were purchased from Sigma-Aldrich Canada. Potassium chloride (KCl), sodium chloride (NaCl), nitric acid (HNO3) and hydrochloric acid (HCl) were purchased from ACP Chemicals Canada. All these chemicals were of analytical grade and were used as received. A 0.1 M NaOH solution was used as the supporting electrolyte. Deionized (DI) water (with resistivity ≥ 18 MΩ cm) was used for preparing various aqueous solutions. A 100 mM glucose stock solution was prepared in DI water and stored in a refrigerator in a dark plastic bottle. Different concentrations of glucose were prepared by diluting the stock solution with 0.1 M NaOH. Suitable amounts of KCl, NaCl, Na2HPO4, and NaH2PO4 were dissolved in DI water to prepare 100 mM phosphate buffered saline (PBS) solutions of various pH, containing 2.7 mM KCl and 137 mM NaCl.
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3

Electrochemical Sensor for miRNA Detection

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Ttc, thiodiacetic acid (tda), mercaptosuccinic acid (MSA), Nafion 117 (formulas are shown in Figure 1), titanium(IV) isopropoxide, graphite flakes, NaNO3, KMnO4, sodium acetate trihydrate, acetic acid, Hg(NO3)2, water and other chemicals were purchased from Sigma-Aldrich (St. Louis, MO, USA) in ACS purity (chemicals meet the specifications of the American Chemical Society). MiRNA was also purchased from Sigma-Aldrich and its sequence was 5′ UAA GGC ACG CGG UGA AUG CCA AAA AAA AAA 3′. Standard nucleobases were adenine and cytosine (MP Biomedicals, Santa Ana, CA, USA), guanine and uracil (Sigma-Aldrich, St. Louis, MO, USA).
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4

Perfluorosulfonic Acid Membrane Synthesis

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Commercial Nafion-117 (Sigma-Aldrich, Saint-Louis, MO, USA) and MF-4SC (Plastpolymer, Saint-Petersburg, Russia) perfluorosulfonic acid membranes, an isopropyl alcohol solution of the MF-4SC perfluorosulfonic acid polymer in the lithium form (10 wt%, equivalent weight is 1100; Plastpolymer, Saint-Petersburg, Russia), aniline hydrochloride (>99%, Merck, Darmstadt, Germany), 3,4-ethylenedioxythiophene (98%, Sigma-Aldrich, Saint-Louis, MO, USA), ammonium persulfate (>98%, Sigma-Aldrich, Saint-Louis, MO, USA), hydrochloric acid (special purity grade, Chimmed, Moscow, Russia), potassium chloride (reagent grade, Chimmed, Moscow, Russia), sodium hydroxide (standard titer, REAGENT, Moscow, Russia), sulfanilamide (4-aminobenzenesulfonamide, >99%, Sigma-Aldrich, Saint-Louis, MO, USA), sulfacetamide (N-[(4-aminophenyl)sulfonyl]acetamide, >99%, Sigma-Aldrich, Saint-Louis, MO, USA), “Sulfacyl sodium-SOLOpharm” eye drops (Grotex, Saint-Petersburg, Russia), deionized water (resistance 18.2 MΩ, pH 5.41 ± 0.05) were used.
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5

Electrochemical Sensing Reagents Protocol

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Urea (CO(NH2)2, 99.0‐100.5%), Tin(II) Chloride (SnCl2·2H2O, 98.0%), silver nitrate (AgNO3, 99.0%), potassium hydroxide (KOH, >85.0%), ethylenediaminetetraacetic acid disodium salt dihydrate (EDTA, 99.0–101.0%), sodium pyruvate (Na‐pyruvate, 99%), 4‐hydroxy‐2,2,6,6‐tetramethylpiperidin‐1‐oxyl (TEMPOL, 97%), TCH (95.0%), MB (1.5%), CIP (98.0%), nitrotetrazolium blue chloride (NBT, 90.0%), DMPO (for ESR spectroscopy), peroxide assay kit (MAK311‐1KT), and Nafion 117 containing solution (≈5% in a mixture of lower aliphatic alcohols and water) were purchased from Sigma–Aldrich. RhB (95.0%) was purchased from TCI. Ethanol and isopropanol (IPA) were purchased from J. T. Baker. All the reagents were used as accepted without further purification. DI water (18.2 MΩ) was used in all the experiments.
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6

Quantifying O2 Evolution via Electrochemistry

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To quantify the O2 evolved during controlled-potential electrolysis, electrochemical measurements were performed in a gastight H-type electrochemical cell with two chambers divided by a perfluorinated membrane (Nafion 117, Sigma-Aldrich). The PbFeO2F/FTO working electrode and an Ag/AgCl reference electrode were separated from a Pt-wire counter electrode in each chamber. The other conditions were identical to those mentioned in the description of the photoelectrochemical measurements. The evolved O2 was detected using a gas chromatograph (MGC3000A, Inficon) equipped with a thermal conductivity detector and an MS-5A column. Ar gas was used as the carrier gas.
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7

Fabrication of SWCNT-Based Electrochemical Sensors

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The SWCNT networks were first collected
on a filter by aerosol chemical
vapor deposition. The deposition process is described in more detail
in refs (44 (link)) and (45 (link)). The synthesized networks
were then press-transferred onto an A4-sized PET substrate, densified
with isopropanol, and baked at 100 °C for 10 min. To form reference
electrodes and contact pads, silver was screen-printed on top of the
collected SWCNT network.
The SWCNT counter and working electrodes
were then laser-patterned from the SWCNT sheet. Lastly, the patterned
strips were coated with 5% Nafion 117 (Sigma) with a slot-die coater
(FOM Technologies). The fabricated strips were then cut out from the
sheet by hand and wrapped in poly(tetrafluoroethylene) (PTFE, Saint-Gobain
Performance Plastics CHR 2255–2) tape with a 6 mm diameter
hole to define the measurement area. A step-by-step fabrication process
is provided in ref (17 (link)). Two sheets were fabricated with a total of 144 sensor strips.
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8

Analytical Grade Reagent Protocol

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All chemicals were of analytical grade and used without further purification. Solutions were prepared with doubly distilled water (18.2 MΩ cm). Reagents used were Nafion® 117 at 5% w/v solution; H2SO4; NaCO3 and NaHCO3 (Sigma–Aldrich, Merck KGaA, Darmstadt, Germany); CuSO4 (Carlo Erba Regents, Milan, Italy); Na2SO4 (Fluka, Buchs, Switzerland); NaNO3 (Alfa Aesar, Karlsruhe, Germany).
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9

Electrochemical Sensing with AuNPs and MWCNT

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The experiment conducted made use of analytical-grade chemicals. Chloroauric acid (HAuCl4,) ultrapure 99.99%, MWCNT extrapure 95%, and graphite synthetic powder (Type IV) pure were purchased from SRL Pvt. Ltd. Sodium biphosphate (Na2HPO4) extra pure 99% and Sodium monophosphate (NaH2PO4) extra pure AR 99% were obtained from SRL. Ltd. Picloram, extra pure 95% was also obtained from SRL Pvt. Ltd. Hexaammineruthenium (III) chloride 98% pure and Nafion® 117 were purchased from Sigma-Aldrich Chemical Co. All of the electrochemical analyses were carried out using an electrochemical workstation (Palm sense 4.0) with silver/silver chloride (Ag/AgCl) (saturated with KCl, as a reference electrode), platinum wire (Pt, as an auxiliary electrode) and GCE (as a working electrode).
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10

Electrochemical Oxygen Evolution Catalyst

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Cobalt (II) nitrate hexahydrate (Co(NO3)2·6H2O, ACS reagent, ≥ 98.0%), Nickel nitrate hexahydrate (Ni(NO3)2.6H2O, ACS reagent, ≥ 98.0%), ammonium metavanadate (NH4VO3, ACS reagent, ≥ 98.0%), sodium hypophosphite (NaH2PO2, MW:87.98 g mol−1), urea (powder, Bioreagent), ammonium fluoride (NH4F, ACS reagent, ≥ 98.0%), and potassium hydroxide (KOH, ACS reagent, ≥ 85%, pellets), Pt on activated carbon (20% Pt loading), ruthenium (IV) oxide, and nafion 117 containing solution were obtained from Sigma‐Aldrich while Ni foam (porosity ≈98%, Ni percentage ≈ 99.9%, length ≈250 mm, thickness ≈ 1.5 mm, pore size ≈0.2–0.5 mm and density ≈ 380 g m2 ± 20,) was obtained from China (Taiyuan Liyuan Lithium Technology Co. Ltd.). All chemicals were used as received without any further purification.
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