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8 protocols using cobalt 2 perchlorate hexahydrate

1

Synthesis and Characterization of Electrocatalysts

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Cobalt(II) perchlorate hexahydrate, iron (III) chloride (reagent grade, 97%), red phosphorus (reagent grade, 99.99%), 5 wt% of Nafion, and perchloric acid were purchased from Sigma-Aldrich. Benchmark 20 wt% Ir/C (commercial) and 20 wt% Pt/C (commercial) catalysts were purchased from Johnson Matthey and Premetek, Co. All the chemicals were of analytical grade and were used as received without further purification.
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2

Synthesis and Characterization of Organic Compounds

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4′-Bromo-2,2′:5′,2″-terpyridine (TCI, Tokyo, Japan), 3,6-bis(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-9-phenylcarbazole (ABCR, Karlsruhe, Germany), 1,1,1,3,3,3-hexafluoropropan-2-ol (Fluorochem, Hadfield, UK), dimethylformamide (DMF), acetone, acetonitrile, hexane, methanol, propan-2-ol, propylene carbonate, tetrabutylammonium hexafluorophosphate (NBu4PF6), and cobalt (II) perchlorate hexahydrate (all solvents of analytical grade, Sigma-Aldrich and Merck, Prague, Czech Republic) were used as-received. Tetrakis(triphenylphosphine)palladium(0) (Pd(PPh3)4 (Merck, Prague, Czech Republic) was washed three times with methanol (20 mL) and dried before use. Quartz substrates used for optical spectroscopy measurement were purchased from Präzisions Glas & Optik GmbH (Iserlohn, Germany). ITO-coated glass substrates with dimensions of 15 × 20 mm used for thin film preparation for the electrical and electrochemical measurements and the electrode setup required for the electrochemical measurement were purchased from Ossila BV (Leiden, The Netherland). Silicon oxide substrates were used for GIWAX and were purchased from Ossila BV (The Netherland).
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3

Spectrophotometric Cobalt(II) Binding Assay

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Quercetin (Que) (purity ≥ 95%, HPLC), cobalt(II) perchlorate hexahydrate (purity ≥ 98%), 4-morpholinepropanesulfonic acid (MOPS) (purity ≥ 99.5%, titration), dimethyl sulfoxide for spectroscopy (DMSO) (purity ≥ 99.8%), and poly(acrylic acid sodium salt) (PAA) (average Mw ~5100, GPC, purity ≥ 99%) were purchased from Sigma-Aldrich and used without purification. Stock solutions of Que were prepared in pure DMSO and then properly diluted in a buffered aqueous solution (pH 7.4, MOPS 10 mM) to have a final organic solvent content of only 5% v/v. Buffer solutions were prepared by weighing proper amounts of MOPS and titrating with a sodium hydroxide solution to the desired pH. All Que solutions were always freshly prepared and stored in the dark to avoid possible light-induced alterations. The cobalt(II) stock solution was prepared by dissolving the corresponding perchlorate salt in water and titrating the resulting solution with standard EDTA, using orange xylenol as an indicator [60 ]. Poly(acrylic acid) stock solutions were prepared at pH 7.4 in MOPS 10 mM; the concentration of the polymer was expressed per monomer unit of acrylic acid. High-purity water (Millipore, Milli-Q Element A 10 ultrapure water) and A-grade glassware were employed throughout.
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4

Titration of Cobalt(II) Complexes

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The synthesis of N-(2-hydroxybenzyl)phenylalanine (PhAlaSal) has been described in [14] (link). Solutions of cobalt(II) nitrate hexahydrate and cobalt(II) perchlorate hexahydrate (Sigma-Aldrich, Saint Louis, USA) were titrated with EDTA disodium salt in the presence of murexide. Solutions of carbonate-free 0.1 M and 1.0 M NaOH, methanol and water (HPLC-grade) were purchased from J.T. Baker. The acid solutions from Sigma–Aldrich were standardized alkalimetrically and determined by the Gran method [38] (link). Potassium nitrate(V) (J.T. Baker) and sodium perchlorate monohydrate (Sigma-Aldrich) solutions were used to adjust the ionic medium. Tris-HCl (Sigma-Aldrich), sodium chloride (Chempur, Piekary Śląskie, Poland) and argon of high purity (Linde, Dublin, Irlandia) were used.
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5

Synthesis and Characterization of AlaSal Compound

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N-(2-hydroxybenzyl)alanine (AlaSal) was synthesized as described previously [39 (link)]. Cobalt(II) nitrate hexahydrate and cobalt(II) perchlorate hexahydrate (Sigma-Aldrich), titrated with disodium salt of EDTA in the presence of murexide, were used as standard solutions. The alkali solutions (carbonate-free 0.1 M and 1.0 M NaOH), methanol and water (HPLC-grade) were purchased from J.T. Baker. The HNO3 and HClO4 solutions (Sigma-Aldrich) were standardized alkalimetrically and then determined by the Gran method [59 (link)]. Standard solutions of potassium nitrate(V) (J.T. Baker) and sodium perchlorate monohydrate (Sigma-Aldrich) were used to adjust the ionic medium. Tris-HCl (Sigma-Aldrich), sodium chloride (Chempur) and argon of high purity (Linde) were used.
The following materials were used in the biological studies: Mueller-Hinton liquid medium (Biocorp), Brucella medium (Biocorp), supplemented with 10% fetal bovine serum (FBS) (Sigma-Aldrich), RPMI-1640 with or without phenol red, amphotericin B, gentamicin, amoxicillin, penicillin, streptomycin, trypsin, MTT [(3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide)], 4′,6-diamidino-2-phenylindole (DAPI) (all from Sigma-Aldrich).
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6

Fabrication and Sensing of Metal Ions

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All reagents used for device fabrication and sensing were utilized without further pre-treatment. ARS, a commercially available river sample with trace elements in river water (Elevated Level, NMIJ CRM 7202-c, Supplementary Table S1), and iron(III) nitrate enneahydrate (Fe3+) were obtained from FUJIFILM Wako Pure Chemical Co., Ltd. The target metal ions including cobalt(II) perchlorate hexahydrate (Co2+), calcium perchlorate tetrahydrate (Ca2+), lead(II) perchlorate trihydrate (Pb2+), cadmium perchlorate hydrate (Cd2+), nickel(II) perchlorate hexahydrate (Ni2+), copper(II) perchlorate hexahydrate (Cu2+), magnesium perchlorate hexahydrate (Mg2+), aluminum perchlorate non-ahydrate (Al3+), mercury(II) perchlorate hydrate (Hg2+), and zinc perchlorate hexahydrate (Zn2+) were purchased from Sigma-Aldrich. The building blocks of the chemosensors purchased from Tokyo Chemical Industry Co., Ltd. were 3-NPBA, BPR, PR, and PV. A buffer material purchased from DOJINDO was 4-(2-hydroxyethyl)-1-piperazineethanesulfonic acid (HEPES). All aqueous solutions were prepared using Milli-Q water (18.2 Ω cm).
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7

Synthesis of Metal-Organic Frameworks

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1,3-Bis(3-carboxypropyl)tetramethyldisiloxane (H2Cx), [HOOC(CH2)3(CH3)2Si]2O, MW = 306.5 was prepared according to already published procedure [86 (link)], while 4,4′-azopyridine (APy), C10H8N4, MW = 184.20, Cobalt(II) perchlorate hexahydrate, Co(ClO4)2·6H2O, MW = 365.93 and Zinc perchlorate hexahydrate, Zn(ClO4)2·6H2O, MW = 372.38, 2,6-Dimethylpyridine, C7H9N, MW = 107.15, and ethanol were purchased from Sigma-Aldrich.
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8

Synthesis of Cobalt-Pyridine Complex

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All reagents and solvents were purchased from commercial sources and were used without further purification. Di(2-pyridyl)ketone, cobalt(II) perchlorate hexahydrate and fluorine-doped tin oxide coated glass (FTO) were purchased from the Sigma-Aldrich Company. Sodium carbonate was purchased from Merck Company.
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