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19 protocols using perchloric acid hclo4

1

Electrocatalyst Preparation and Characterization

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All of the chemicals are of analytical grade and used without further purification. Commercial references of Vulcan carbon-supported Pt electrocatalyst (50 wt%, TEC-10E50E) was purchased from TKK, Japan. Other reagents are as follows: isopropanol (IPA, >99.9%, analytical reagent grade, Kermel), Nafion D521 dispersion (5 wt%, EW = 1100, Ion Solution Inc), potassium tetrachloroplatinate (K2PtCl4, 98%, RHAWN), nickel dichloride (NiCl2, 99%, RHAWN), sulfuric acid (H2SO4, 95–98 wt%, analytical reagent grade, SCR, China), perchloric acid (HClO4, 70%, Sigma Aldrich). Argon and oxygen gases having high purity (>99.99%) were purchased from Yihong Gas Company, China. Deionized water (20 ± 1°C, pH 7, ρ = 18.3 MΩ/cm) was purified by passing through pure compact ultrapure water system (Arium mini, Sartorius).
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2

Quantification of Methacrylate Substitution in Hyaluronic Acid

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For 1H-NMR, a solution was prepared (6% (w/w)) of MeHA polymer in D2O and analyzed on a 300 mHz Gemini Spectrometer (Varian, Palo Alto, CA). All samples were measured with a relaxation delay of 0.6 seconds for 512 scans. The degree of methacrylate substitution was calculated by comparing the integrals of the peaks of the methacrylate groups at 1.9, 5.7 and 6.1 ppm relative to the integrals originating from the protons of HA.
For the HPLC measurements, 15 mg of MeHA was dissolved in 10 ml of 0.02 M NaOH solution, and incubated at 37°C for 30 minutes to ensure complete hydrolysis of the ester bonds. After that, 2 ml of 2 M acetic acid (Merck) was added to acidify the solution. Samples were filtered over 0.2 μm filters and injected onto a Sunfire RP-18 column (Lichrospher, Darmstadt, Germany). Samples were analyzed using a HPLC Waters 2695 system equipped with an UV detector model 2487 (λ = 210 nm, Waters Inc., Dublin, Ireland). The mobile phase consisted of a mixture of acetonitrile (Actu-All Chemicals, Oss, the Netherlands) and water (ratio: 15/85) adjusted to pH 2 with perchloric acid (HClO4, 70%, Sigma-Aldrich) and a flow rate of 1 ml/min was used. A calibration curve was obtained by injection of methacrylic acid solutions in eluent with a concentration range of 0 to 160 μg/ml. Empower Pro software (Waters) was used to calculate the concentration of methacrylic acid.
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3

Anodization of 316L Stainless Steel Foil

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An austenitic
316L stainless SS foil (0.5 mm) was cut into 1 × 1 cm-sized samples.
Prior to anodization, the samples were ultrasonically cleaned in acetone,
ethanol, and distilled water each for 10 min. For anodization, the
samples were connected to a DC power supply (Genesys 300V/5, TDK Lambda),
which had a two-electrode configuration. A platinum mesh was used
as the cathode and a 316L SS sample was used as the anode. 316L SS
samples were anodized in ethylene glycol monobutyl ether (EG, Sigma-Aldrich)
solution containing 7.5% (v/v) perchloric acid (HClO4,
Sigma-Aldrich) to obtain nanofeatured surfaces. Anodization experiments
were carried out at temperatures lower than 6 °C. To control
the feature size of the nanofeatures, the applied potentials were
altered between 25 and 80 V, and the anodization durations were set
between 1 and 20 min. After the anodization process, all the samples
were rinsed with distilled water and dried at room temperature.
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4

Fabrication of Fluorescent Sensing Probes

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Al foil (0.2 mm) was purchased from Zhonguo New Material (Beijing) Technology Co. Ltd. Perchloric acid (HClO4), phosphoric acid, chromium hemitrioxide (Cr2O3), oxalic acid, silver nitrate (AgNO3), rhodamine B (RhB), rhodamine 6G (R6G), 1H′,1H′,2H′,2H′-perfluorodecanethiol (97%) and ethyl alcohol (98%) were purchased from Sigma-Aldrich Co. Ltd.
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5

Electrochemical Analysis of Humic Acid

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Humic acid sodium salt (Sigma-Aldrich, Steinheim, Germany), graphite (flakes, mp 3652–3697 °C, density 1.9, Sigma-Aldrich, Saint Louis, MO, USA), perchloric acid (HClO4) (Sigma-Aldrich, Steinheim, Germany) and KBr (Scharlau, Barcelona, Spain) were utilized as received. The aqueous solutions were prepared with ultrapure deionized water (Millipore).
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6

Electrochemical Glucose Oxidation with f-CNT

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Carboxylic acid-functionalized multi-walled carbon nanotube (f-CNT), >80% carbon basis, >8% carboxylic acid-functionalized, avg. D × L 9.5 nm × 1.5 µm, N,N-Dimethylformamide (DMF), Nafion (5 wt.%), D-(+)-glucose (≥99.5%), sulfuric acid (H2SO4, 98%), and perchloric acid (HClO4, 70.0–72.0%) were purchased from Sigma Aldrich (USA) and used as received without further purification. Palladium (II) chloride (PdCl2, 59.8 wt.%) was obtained from Johnson Matthey (UK). All other chemicals used were of analytical reagent grade. The electrochemical electrooxidation of glucose was performed in 0.1 M PBS (pH 7.4), prepared using analytical grade reagents, Na2HPO4 and KH2PO4 dissolved in distilled water, purchased from Solvachim (Casablanca, Morocco). An amount of 200 mM glucose stock solution was prepared in 0.1 M phosphate buffer solution (PBS) and stored at 4 °C. Glucose stock solution was allowed to mutarotate under magnetic stirring for at least 24 h before use.
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7

Synthesis and Characterization of 2-Selenouracil

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2-Selenouracil (2-SeU) was synthesized according to the published procedures [51 (link)], with a slight modification elaborated by Kulik et al. [42 (link)]. General procedure consisted of condensation of selenourea with 3-oxopropanoate, yielding 2-SeU. The resulting 2-SeU was recrystallized from ethanol and analyzed using 1H-, 13C-NMR, and mass spectrometry techniques. Sodium azide (NaN3) (≥99.5% purity), sodium hydroxide (NaOH) (≥99.5% purity), 70% perchloric acid (HClO4) (99% purity), and nitrous oxide (N2O) > 98% were purchased from Sigma-Aldrich (St. Louis, MO, USA) and used without further purification.
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8

Lignin-Graphite Composite Synthesis

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Lignosulfonates (LS30, Mw = 13 400, MeadWestvaco), a lignin derivative. Graphite (flakes, mp 3652–3697 °C, density 1.9, Sigma-Aldrich), perchloric acid (HClO4) (Sigma-Aldrich), KBr (Scharlau) were used as received. The aqueous solutions were prepared with ultrapure deionized water (Millipore).
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9

Histamine Dihydrochloride Analysis Protocol

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Histamine dihydrochloride (99%), sodium 1-decanesulfonate, potassium monophosphate, potassium hydrogen phosphate trihydrate, acetonitrile, and perchloric acid (HClO4) were purchased from Sigma-Aldrich (Amsterdam, The Netherlands). All chemical reagents and solvents were of analytical grade. Ultrapure water was obtained from a MilliQ purification system (Merck, Darmstadt, Germany).
Phosphate buffer solution at pH 6.9 was prepared by weighing 1.7 g of potassium monophosphate, 2.85 g of potassium hydrogen phosphate trihydrate, and 0.49 g of sodium 1-decanesulfonate and dissolving these in 1 L of distilled water.
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10

Quantitative Analysis of Organic Acids

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The organic acids concentrations were determined in the colonic content (fermentation broth) of mice. In short, the colonic content was diluted four times with 1 mol/L perchloric acid (HClO4, Sigma-Aldrich, USA) to release the organic acids. Proteins and fat in the fermentation broth were precipitated by ultrasonication and removed by centrifugation for 10 min at 20,000×g. Organic acids, including the SCFAs, were determined by high performance anion exchange chromatography (HPAEC) with UV and refractive index (RI) detection. 25 µL of the supernatant was injected on a guard column in series with two Rezex ROA Organic acids H+ analytical columns (Phenomenex, USA). The organic acids were eluted isocratic with 5 mmol/L sulfuric acid (H2SO4), with a flow rate of 0.60 mL/min. The column oven was held at a temperature of 60 °C. Data analysis was done with Chromeleon software version 7.2 (Thermo Scientific). Quantitative analyses were performed by using standards of the organic acids (Sigma-Aldrich, USA).
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