A potentiostat/galvanostat model GAMRY Reference 3000 was used for carrying out the electrochemical experiments. A conventional three-electrode system consisting of the Au/NiFe2O4@GO-Ch modified glassy carbon electrode (GCE) (diameter of 3 mm) as the working electrode, a platinum wire as the counter electrode and Ag/AgCl as the reference electrode was used. Prior to modification, the bare GCE was hand-polished successively with 0.3 μm and 0.5 μm micropolish alumina (Buehler, USA) using polishing cloth to obtain a cleaned and polished surface.20 (link) It was then washed with ethanol and water in a sonication bath and dried at room temperature. A 10 μL Au/NiFe2O4@GO-Ch nanocomposite was dropped onto the GCE surface and dried at room temperature for 24 h. The as-prepared Au/NiFe2O4@GO-Ch modified GC electrode is denoted as the Au/NiFe2O4@GO-Ch/GCE. The various electrochemical analyses carried out in the present study include cyclic voltammetry (CV), differential pulse voltammetry (DPV) and electrochemical impedance spectroscopy (EIS).
Micropolish alumina
Manufactured by Buehler
Sourced in United States
Micropolish alumina is a fine polishing compound used for the preparation of metallographic and other samples. It is a high-purity aluminum oxide abrasive material available in various particle sizes. Micropolish alumina is used to achieve a mirror-like finish on the surface of the sample being prepared.
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5 protocols using micropolish alumina
1
Electrochemical Characterization of Au/NiFe2O4@GO-Ch
2
Pneophyllum cetinaensis: Karst River Algae Analysis
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Specimens of Pneophyllum cetinaensis were collected in the Cetina River (southern Croatia) at a depth of 0.5 m in December 2013 at Otok Ljubavi (43°26.180′ N–16°45.785′ E). The Cetina River is a typical permanent karst river discharging into the Adriatic Sea. Pneophyllum cetinaensis is present throughout almost the entire length of the Cetina River from 0 to 300 m above sea level, reaching about 75 km from the river mouth. The Cetina River physico–chemical characteristics at the site of collection were: pH = 8.21 ± 0.02 SD (NBS scale), salinity < 0.5, temperature: 10.20 ± 0.08 SD °C (annual average; 12.9 ± 3.3 SD °C), Mg = 7.52 ± 4.11 SD, mg/L, Ca = 68.86 ± 6.18 SD mg/L.
Prior to the mechanical properties and trace elements analysis carried out at the University of Portsmouth, nine specimens were embedded in epoxy resin (EpoFix Kit, batch no: 8134-01, Struers ApS, Ballerup, Denmark) and gently polished (Micropolish Alumina, Buehler, Esslingen, Germany). Analyses were carried out on the internal layers of the algae (Figure 5 d). The LA-ICPMS spots size and the Nano indentation grid allowed us to analyse the entire layers.
Prior to the mechanical properties and trace elements analysis carried out at the University of Portsmouth, nine specimens were embedded in epoxy resin (EpoFix Kit, batch no: 8134-01, Struers ApS, Ballerup, Denmark) and gently polished (Micropolish Alumina, Buehler, Esslingen, Germany). Analyses were carried out on the internal layers of the algae (
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Galactose Oxidase Biosensor Development
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All chemicals were of analytical grade and used as received. D-(+)-galactose, sodium dihydrogen, and poly(ethylene glycol)diglycidyl ether (PEGDGE, MW 500) were supplied by Sigma-Aldrich (St. Louis, MI, USA). Di-sodium hydrogen phosphate 12-hydrate was obtained from VWR Chemicals (Solon, OH, USA). Micropolish alumina with 1, 0.3, and 0.05 µm particle sizes were purchased from Buehler. The redox polymer [poly(1-vinylimidazole) Os(2,2′-bipyridine)2Cl]+, named as PVI-Os, was synthesized by modification of reported methods [39 (link),40 (link)]. P(VI-SS) was synthesized as reported by Lielpetere et al. [38 (link)]. MPC was synthesized as described by Jayakumar et al. [25 (link)]. Galactose oxidase (GaOx) from Dactlylium dendroides (500–1500 U mg−1) was supplied by Sigma-Aldrich. Human plasma was received from Skånes Universitetssjukhus (Lund, Sweden). All aqueous solutions were prepared with ultrapure deionized water (18.2 MΩ cm) from a Milli-Q water system.
4
Synthesis and Characterization of Metal Oxides from Pomegranate
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From pomegranate (Punica granatum L) fruit, peels were sourced and used by cleaning and drying them in the sun for few days (2–3 days). Metal precursors such as zinc acetate, copper acetate, 15 mL polyesterine graduated tubes and 0.22 μm hydrophilic filters (Whatman) were used in the synthesis and characterisation of the metal oxides while potassium bromide (KBr), potassium hydroxide (KOH) and silver/silver chloride (Ag/AgCl, 3 M) were used in FTIR and electrochemical measurements. Materials and reagents were purchased from Sigma-Aldrich. The cleanliness of the working electrode was maintained using alumina micropolish (1.0, 0.3, and 0.05 μm alumina slurries) and polishing pads supplied by Buehler, IL, USA.
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Characterization of Glass-Ceramic Microstructure
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Glass-ceramic specimens were polished to 1µm alumina micropolish (Lot no: 0335-0275, Buehler, Coventry, UK) and etched using 0.1% hydrofluoric acid for 60 s.
Specimens were gold coated using a sputter coater (Agar Scientific Ltd., UK) for 30 s at 40 mA and imaged using a field emission scanning electron microscope (FEI Inspect F, Hillsboro, Oregon, USA), using secondary electron imaging. Quantitative image analysis (Sigma Scan Pro 5.0, Systat Software, Inc., Chicago, IL, USA) was used on the SEM photomicrographs to ascertain (× 3500 magnification, area =2255 μm 2 ) the particle size and area fraction.
Specimens were gold coated using a sputter coater (Agar Scientific Ltd., UK) for 30 s at 40 mA and imaged using a field emission scanning electron microscope (FEI Inspect F, Hillsboro, Oregon, USA), using secondary electron imaging. Quantitative image analysis (Sigma Scan Pro 5.0, Systat Software, Inc., Chicago, IL, USA) was used on the SEM photomicrographs to ascertain (× 3500 magnification, area =2255 μm 2 ) the particle size and area fraction.
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