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9 protocols using valeronitrile

1

Synthesis and Characterization of Aβ40 Peptide

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The following chemicals were purchased from Sigma Aldrich (Taufkirchen, Germany): 2,2′-azobis(2-methylpropionitrile) (AIBN), ethanolamine, deuterated chloroform, isobutyronitrile, methyl trifluoromethanesulfonate, N-methylpropargylamine, THF (HPLC grade), valeronitrile and zinc acetate dihydrate. N,N-diethylamine and propargyl tosylate were purchased from Fluka (Taufkirchen, Germany). Calcium hydride was bought from Alfa Aesar (Karlsruhe, Germany). Sodium chloride and sodium sulfate were bought from Roth (Karlsruhe, Germany). Ce(SO4)·4H2O and (NH4)6Mo7O24·4H2O were obtained from VEB (Eschborn, Germany). Concentrated sulfuric acid was purchased from Th. Geyer (Renningen, Germany). deuterated chloroform was obtained from Chemotrade (Düsseldorf, Germany), and DMF (HPLC grade) was purchased from VWR-Prolabo (Darmstadt, Germany).
40 peptide was synthesized using the standard F-moc solid phase synthesis strategy at the core unit “Peptid-Technologien” of the Medical Faculty of the University of Leipzig [52 (link)].
The oxazoline monomers were stored over Calcium hydride and were freshly distilled before usage. All solvents were freshly distilled and degassed by bubbling with nitrogen for at least 20 min prior to usage. Acetonitrile (ACN) was dried with Calcium hydride by boiling for several hours followed by distillation. AIBN was recrystallized from ethanol twice before usage.
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2

Synthesis of 2-butyl-2-oxazoline and Polymer

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LDN-57444, 2-methyl-2-oxazoline, and other reagents for synthesizing 2-butyl-2-oxazoline (valeronitrile, cadmium acetate dehydrate and ethanolamine) and polymer (acetonitrile, n-boc-piperazine) were obtained from Sigma-Aldrich Inc (St. Louis, MO, USA).
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3

Dye-Sensitized Solar Cell Protocol

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N719 dye: [cis-bis(isothiocyanato)bis(2,2-bipyridyl-4,4-dicarboxylato)-ruthenium(II)bis-tetra butyl ammonium], acetonitrile, valeronitrile, guanidium thiocyanate, hexachloro platinic acid (H2PtCl6), 4-tert-butylpyridine (4-tBP) and 2-(N,N-dimethyl-4-aminophenyl) azobenzenecarboxylic acid were purchased from Sigma-Aldrich. Iodine (I2) and lithium iodide (LiI) were obtained from Merck. Titania pastes were prepared in research laboratory [3] . Dye solutions (0.3 mM) containing different amounts of CA were prepared and used to sensitize the TiO2 electrodes.
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4

Fabrication and Characterization of Dye D1

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The materials
used in the synthetic procedure and device fabrication were of analytical
grade and used without further purification. Zinc chloride (Merck),
ethyl cellulose (Himedia), 4-tert-butylpyridine (Himedia),
chloroplatinic acid hexahydrate (Sigma-Aldrich), ammonium hydroxide
(Merck), iodine (Merck), lithium iodide (Sigma-Aldrich), acetonitrile
(HPLC grade, Merck), dichloromethane (DCM, Merck), valeronitrile (Sigma-Aldrich),
terpineol (Himedia), hydrogen chloride (Merck), 1-butyl 3-methyl imidazolium
iodide (Sigma-Aldrich), and ethanol (TEDIA, USA) are used. Fluorine-doped tin oxide
(FTO, sheet resistance 12–14 Ω cm–2)-coated glass substrates were procured from Sigma-Aldrich. The water
used for the experiments is Milli-Q water (18.2 MΩ cm–2). All of the chemicals reagents used during the synthesis of dye D1 are mentioned in the synthetic protocol.
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5

Synthesis and Characterization of Dye-Sensitized Solar Cells

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Reagent grade 1,2-dihydroxybenzene (catechol, 99+%), iodine (I2) >99.8 purity, guanidinium thiocyanate (GuSCN >97%), 1-methylimidazole (>97%), polyethylene glycol (PEG-300), lithium iodide (LiI, 99.9%), 4-tert-butylpyridine (tBP, 96%), acetonitrile (ACN, 99.8%), valeronitrile (VLN, 99.5%), and hydrogen hexachloroplatinate (IV) hexahydrate (H2PtCl6∙H2 O,≥37.5%) were all purchased from Sigma-Aldrich. Fluorine-doped tin oxide (F-SnO2,14 Ω/sq.) glass, 1-iodopropane (>98%, TCI), cis-Bis(isothiocyanato) (2,2′-bipyridyl-4,4′-dicarboxylato) (4,4′-di-nonyl-2′-bipyridyl) ruthenium (II) (Z907, Organica), potassium iodide (KI, 99.5%, D.S.P), toluene (>99.5%, Daejung), and titanium (IV) oxide paste (20 nm, Head Solar, Korea) were purchased from different suppliers. All chemicals were used as purchased.
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6

Stainless Steel-Carbon Black Composite Fabrication

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Stainless steel (SS) was provided from POSCO. Carbon black (CB) powders purchased from Beilum Carbon Chemical Limited. Polyethylenimine (branched, average Mw ~25,000 by light scattering method, average Mn ~10,000 by GPC), trimethylolpropane triglycidyl ether, tert-butanol, iodine (I2), guanidinium thiocyanate (GuSCN), 4-tert-butylpyridine (tBP), acetonitrile (AN), and valeronitrile (VN) were purchased from Sigma-Aldrich. Fluorine-doped SnO2 (FTO) glass, Ti-nanoxide T/SP. Ti-nanoxide R/SP, cis-diisothiocyanato-bis(2,2′-bipyridyl-4,4′-dicarboxylato) ruthenium(II) bis(tetrabutyl-ammonium) (N719), 1-butyl-3-methylimidazolium iodide (BMII) were purchased from Solaronix SA. Spray gun (AIR BRUSH KIT, ABS-130) was purchased from Bluebird.
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7

Synthesis and Characterization of Dye-Sensitized Solar Cells

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Ammonium molybdate tetrahydrate ((NH4)6Mo7O24·4H2O, 99.98%), sodium sulfide nonahydrate (Na2S·9H2O, 99.99%), potassium chloride (KCl, 99%), acetonitrile (ACN, CH3CN, 99%), dimethyl sulfoxide (DMSO, (CH3)2SO, 99.5%), ethanol (EtOH, CH3CH2OH, 99.8%), guanidinium thiocyanate (NH2C(=NH)NH2·HSCN, 99%), iodine (I2, 99.8%), 1-methyl-3-propylimidazolium iodide (C7H13IN2, 98%), 4-tert-butylpyridine (C9H13N, 98%), valeronitrile (CH3(CH2)3CN, 99.5%), chloroplatinic acid hexahydrate (H2PtCl6·6H2O, ≥37.50% Pt), sulfuric acid (H2SO4, 95–98%), polyvinylpyrrolidone (PVP, (C6H9NO)n, average Mw 10,000), and sodium borohydride (NaBH4, 99%) were purchased from Sigma-Aldrich (Germany). Low-temperature thermoplastic sealant (Surlyn, 25 μm), 18NR-T transparent titania paste (particle size of 20 nm), 18NR-AO active opaque titania paste (particle sizes of 20 and 450 nm), fluorine-doped tin oxide (FTO, TEC8 glass plates, 8 Ω·cm−2, 2.2 mm thickness), and N719 industry standard dye (N719) were purchased from Dyesol (Australia). All commercial chemicals were of analytical grade and were used as supplied without further purification.
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8

Synthesis and Characterization of Dye-Sensitized Solar Cells

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All of the chemicals
were used for the experiments without further purification. SnCl2·2H2O power (Merck), terpineol (Himedia),
poly(ethylene glycol) (PEG)–poly(propylene glycol) (PPG)–PEG
triblock copolymer (Aldrich), SnCl4·5H2O (Aldrich), 2-methoxy ethanol (Himedia), absolute ethanol (TMEDA),
acetylacetone (Merck), 4-tert-butylpyridine (Himedia),
hexachloroplatinic acid (H2PtCl6, Aldrich),
Zn(NO3)2·6H2O (Aldrich), di-tetrabutylammonium cis-bis(isothiocyanato)bis(2,2′-bipyridyl-4,4′-dicarboxylato)ruthenium(II)
(Dyesol, Australia), ethanol (EtOH), CH3CN (Merck), PEG
200 (Merck), valeronitrile (Sigma-Aldrich), tert-butanol
(Merck) were used. Fluorine-doped tin oxide (resistivity ∼13–15
Ω/sq cm, Aldrich), and poly(tetrafluoroethylene) filter (0.2
μm, Axiva) were purchased. High-grade Milli-Q water (18.2 MΩ
cm) was used for all of the experiments.
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9

Purification of Nitrile Solvents

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General 1 and 2 were prepared as described elsewhere. 27, 28 Acetonitrile (MeCN), propionitrile (EtCN), butyronitrile (PrCN), valeronitrile (BuCN), caprylonitrile (HepCN), ethylene glycol (EG), methanol (MeOH) and ethanol (EtOH) solvents were purchased from Sigma Aldrich. MeCN was HPLC grade, MeOH and EtOH were spectroscopy grade and they were used without further purification. The other nitriles and the ethylene glycol were used after column chromatography purification using a mixed stationary phase (aluminium oxide 'Alumina B' and activated carbon) to remove the luminescent impurities.
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