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8 protocols using vo acac 2

1

Synthesis of Transition Metal Complexes

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Bi(NO3)3·5H2O, VO(acac)2, MoO2(acac)2, oleic acid, oleyl amine, and octadecyl amine were obtained from Sigma Aldrich in Switzerland. Dried ethanol and tetrahydrofuran are the solvents used for this purpose and are procured from Sigma Aldrich and Merck. All chemicals obtained are 99.9% pure and can be used without further purification. The glycerol and potassium phosphate (K2HPO4) used to make the phosphate buffer for electrochemical measurement is 99% pure and can be procured from Sigma Aldrich and Fischer in Switzerland. The water used to make the electrolyte has been double distilled.
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2

Synthesis of Molybdenum-Doped BiVO4 Photoanodes

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All chemicals used in this study were of analytical grade and used without further purification. BiVO4 film was prepared by a modified metal-organic decomposition method with a slight modification from our previous procedure8 (link). Thus, 0.2 M Bi(NO3)·5H2O (99.8%; Kanto Chemicals) dissolved in acetic acid (99.7%; Kanto Chemicals), 0.03 M VO(acac)2 (98.0%; Sigma Aldrich) and 0.03 M MoO2(acac)2 (98.0%; Sigma Aldrich) in acetyl acetone (>99.0%; Kanto Chemicals) were prepared as a precursor solution. Then stoichiometric amount of each precursor was mixed to complete a precursor solution. For Mo doping, Bi:(V+Mo)=1:1 atomic ratio was applied for 1% Mo:BiVO4 films. For fabrication of a BiVO4 film, 60 μl of solution was dropped on a fluorine doped tin oxide (FTO) glass (2 cm × 2.5 cm) and dried for 15 min in Ar atmosphere. Depending on synthesis condition, 10–80 μl of precursor was used. The FTO glass (TEC 8; Pilkington) was cleaned by using KOH (0.1 M)+ethanol with ratio of 1:5, and washed with copious amount of deionized water and finally stored in acetone before usage. The greenish transparent precursor film was calcined at 550 °C for 25 min to form a yellow BiVO4 film. After annealing process, 2 cm × 2.5 cm BiVO4/FTO was split to obtain photoanodes with a net irradiation area of 0.24 cm2 connected by silver paste and copper wire and sealed with epoxy resin.
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3

Synthesis of Vanadium-Doped BiOI Photocatalysts

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A solution
(25 μL) of dimethyl sulfoxide (DMSO, ≥99.5%,
Sigma-Aldrich) containing 0.4 M vanadyl acetylacetonate (VO(acac)2, 98%, Sigma-Aldrich) with or without 0.004 M sodium molybdate
(Na2MoO4, ≥99%, Sigma-Aldrich) was added
on top of the BiOI-coated substrate and dried in a preheated drying
oven at 100 °C for 60 min. Samples were calcined immediately
at 450 °C for 2 h (at a heating rate of 2 °C/min). Afterward,
the excess of vanadium(III) oxide (V2O3) was
removed by placing 500 μL of an aqueous (Milli-Q) 1 M KOH (99.99%,
Sigma-Aldrich) solution on top of the sample for 30 min, rinsing with
Milli-Q water, and drying with compressed air, and repeating this
whole procedure. Subsequently, the samples were annealed in a tube
furnace at 300 °C for 0.5 h at a heating rate of 10 °C/min
in a 5% H2/95% Ar atmosphere at a flow of 500 sccm. The
microwire-structured samples were prepared in two batches, and all
samples in each batch were processed simultaneously. The data reported
in the results paragraph are based on samples from the same batch.
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4

Crystalline VO(acac)2 Inhibitor Purification

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Crystalline VO(acac)2, pNPP, TCEP, IPTG, EDTA, Tris, MES, spectrophotometric grade DMSO, and CM Sephadex G-50 were purchased from Sigma-Aldrich (St. Louis, MO 63103) and used without further purification. The phosphotyrosine containing undecapeptide DADEpYLIPQQG simulating residues 988-998 of the EGFR [15 (link)] was obtained from C. S. Bio, Co. (Menlo Park, CA 94025). VO(Et-malto)2 [18 (link)] and VO(mpp)2 [19 (link), 20 ] were synthesized according to published methods. Analytical data for elemental composition of each chelate showed good agreement with theoretical expectation. Sodium chloride, sodium orthovanadate, and sodium acetate were of analytical grade and were obtained from Fisher Scientific (Pittsburgh, PA 15275). All other reagents were of the highest quality available; deionized, distilled water was used throughout.
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5

Vanadium Compounds for Sodium-Ion Batteries

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V2O3 (Sigma-Aldrich, 98%), VCl3 (Sigma-Aldrich, 97%), V(acac)3 (Sigma-Aldrich, 97%), VO2 (Sigma-Aldrich, 99.9%), VOSO4·xH2O (Sigma-Aldrich, 97%), VO(acac)2 (Sigma-Aldrich, 97%), V2O5 (Sinopharm, 99.5%), NH4VO3 (Aladdin, 99.0%), NaVO3 (Aladdin, 99.0%), and Na3VO4·12H2O (Aladdin, 99.0%) were used as vanadium sources in this work. H3PO4 (85%) and NaH2PO4·2H2O (≥99%), Hydroxylamine (HONH2·HCl, 99.5%) and (NaF, ≥98%) were purchased from Beijing Chemical Reagent Co. with analytical grade. Other reagents used for the preparation of coin cells were Na (Sinopharm, 99.8%), NaClO4 (Alfa Aesar, 99%), fluoroethylene carbonate (FEC; Alfa Aesar, 99%), glass fiber separator (Whatman), KB (Lion, Carbon ECP600JD), and Acetylene black (AB; Alfa Aesar, ≥99.9%). The HC was purchased from KURARAY Co., Ltd, Japan. All reagents were used as received.
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6

Synthesis and Biological Evaluation of Novel Compounds

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The reagents used for the syntheses were of analytical grade and were used without further purification. They were as follows: VO(acac)2 (≥98%, Sigma-Aldrich, Saint Louis, MO, USA), N,N-bis(carboxymethyl)-dl-alanine trisodium salt (Na3bcma) (≥90%, Sigma-Aldrich), N-(Phosphonomethyl)iminodiacetic acid (H4pmida) (95%, Sigma-Aldrich), N-(2-carboxyethyl)iminodiacetic acid (H3ceida) (≥98.0%, VWR) and 4-amino-2-methylquinoline (4-NH2-2-Me(Q), ≥98%, Sigma-Aldrich). In a biological study, it was used anti-rabbit secondary antibodies as well as polyclonal anti-p53 and RAGE antibodies from Santa Cruz Biotechnology (Dallas, TX, USA). Polyclonal anti-cdk1, cyclinB1, p21, β-actin and LC3β antibodies were purchased from Abcam (Cambridge, UK). Anti-rabbit antibodies conjugated with Alexa Fluor546 were obtained from Thermo Fischer Scientific (Waltham, MA, USA). 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT), neutral red (NR), RNAse A, 2′,7′-dichlorofluorescin diacetate (DCF-DA), phalloidin, hoechst, bovine serum albumin (BSA), paraformaldehyde, gemcitabine, and propidium iodide were purchased from Sigma-Aldrich (Saint Louis, MO, USA). BrdU incorporation ELISA assay from Roche (Grenzach-Wyhlen, Germany) and LDH-Cytotoxicity Assay from Promega (Madison, WI, USA).
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7

Inert Atmosphere Synthesis of Carboxylates

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Prior to the addition of water
to the reaction mixtures, all manipulations were carried out in an
MBraun inert atmosphere glovebox under a nitrogen atmosphere unless
otherwise stated. Autoclave reactors and Teflon liners were pumped
down in an evacuated antechamber overnight prior to use in the glovebox.
Molecular sieves (3 Å, Fisher Scientific) were activated by heating
at 200 °C under vacuum overnight. Toluene was dried over activated
sieves (20% by weight) for at least 24 h, then purged with nitrogen
for at least 1 h before being transferred via a cannula to a Schlenk
flask. Toluene was then pumped into the glove box overnight in an
evacuated antechamber and stored over activated 3 Å molecular
sieves. VO(acac)2, stearic acid, decanoic acid, heptanoic
acid, hexanoic acid, and butyric acid purchased from Sigma-Aldrich
and lauric acid purchased from Millipore were pumped into the glovebox
overnight in an evacuated antechamber before use. Benzoic acid and
4-nitrobenzoic acid purchased from Oakwood, acetic acid purchased
from Fisher Scientific, and trifluoroacetic acid purchased from Sigma-Aldrich
were used without further purification.
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8

Synthesis of Functionalized Alcohols

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All starting materials were used without further purification. Pluronic F-127, vanadyl acetylacetonate (98%, VO(acac) 2 ), and ethanol ( p.a.), were purchased from Sigma Aldrich. Benzyl alcohol (BzOH, 99%), furfuryl alcohol (99%), 1-dodecanol (98%) and triethylamine were obtained from Acros Organics.
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