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14 protocols using nitromethane

1

TLC Analysis of Glucose Polymers

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TLC was performed as described in a previous study [17 (link)]. Briefly, TLC was performed using silica gel 60F254 (Merck, Darmstadt, Germany). Samples were spotted onto a TLC plate and developed twice in a presaturated chromatographic chamber using a developing solvent (nitromethane (Sigma-Aldrich, St. Louis, MO, USA):n-propyl alcohol (Samchun, Gyeonggi, Korea):distilled water, 2:5:1.5, v/v/v). The developed TLC plate was then dipped in 0.3 g/L (w/v) N-(1-naphthyl) ethylenediamine dihydrochloride (Sigma-Aldrich) and 5 g/L (v/v) sulfuric acid (Duksan, Seoul, Korea) in methanol (CARLO ERBA Reagents S.A.A., Val de Reuil, France) and then baked at 121 °C for 5 min. Glucose polymer (G1–G8; glucose, maltose, maltotriose, maltotetraose, maltopentaose, maltohexaose, maltoheptaose, and maltooctaose, Carbosynth Co., Berkshire, UK) was used as a standard sugar.
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2

TLC Analysis of Glucose Polymers

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Samples were spotted onto silica gel 60 F254 (Merck, Darmtadt, Germany), and the gel plates were developed twice using 2:5:1.5 nitromethane (Sigma-Aldrich, St. Louis, MO, USA):n-propyl alcohol (Samchun, Gyeonggi, Korea):water. The developed TLC plate was dipped in 0.3% (w/v) N-(1-naphtyl) ethylenediamine dihydrochloride (Sigma-Aldrich) and 5% (v/v) sulfuric acid (Duksan, Seoul, Korea) in methanol (CARLO ERBA Reagents S.A.A., Val de Reuil, France), and then baked at 121 °C for 5 min. Glucose polymers (G1–G7, of which the DPs are 1–7, respectively) purchased from Carbosynth Co. (Berkshire, UK) were used as standard sugars.
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3

Perovskite Solar Cell Fabrication

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PbI2 (99.999 %, Sigma–Aldrich), methylammonium iodide (Greatcell solar), phenylethylammonium iodide (Sigma–Aldrich), N,N‐dimethylformamide (extra dry, 99.8 %, Acros Organics), dimethyl sulfoxide (>99.5 %, Sigma–Aldrich), ethyl acetate (anhydrous, 99.8 %, Sigma Aldrich), chlorobenzene (extra dry, 99.8 %, Acros Organics), Spiro‐MeOTAD (Luminescence Technology Corp), LiTFSI (99.95 %, Sigma–Aldrich), 4‐tert‐butylpyridine (>96 %, TCI), acetonitrile (anhydrous, 99.8 %, Sigma–Aldrich), TiO2 paste (18 NR‐T, Greatcell Solar), titanium(IV) isopropoxide (>97 %, Sigma–Aldrich), PEDOT:PSS (M124 HTL Solar, Ossila), benzo[1,2‐b:4,5‐b′]dithiophene (BDT, TCI, 98 %), n‐butyllithium solution (n‐BuLi, 1.6 M in hexane, Sigma–Aldrich), 1,4‐dibromobutane (Fluorochem, 99 %), 1,6‐dibromohexane (Fluorochem, 95 %), ammonium acetate (ABCR, 97 %), nitromethane (Sigma‐Aldrich, 95 %), lithium aluminum hydride (LiAlH4, Sigma–Aldrich, 95 %), potassium phthalimide (Sigma–Aldrich, 98 %), and hydrazine hydrate (Alfa Aesar, 98 %) were used as received. Conductive patterned FTO was purchased from Lyoyang Guluo Glass Co. with a resistance of 7 Ω/sq.
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4

Synthesis of Thiophene-Based Compounds

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Dimethylformamide (DMF), pyridine,
chloroform, and nitromethane were purchased from Sigma-Aldrich and
dried over 4 Å molecular sieves. Toluene, tetrahydrofuran (THF),
and dichloromethane (DCM) were acquired from an Innovative Technology
Pure Solv solvent purification system. Solvents were degassed by sparging
with nitrogen for 30–90 min before use. Reactions were performed
under an inert N2 atmosphere and glassware was flame-dried
prior to use. Tetrakis(triphenylphosphine)palladium was obtained from
Strem Chemicals. FeCl3 was purchased from Acros. N-Methylpyrrolidone (NMP), Wang resin substituted with the
first amino acid, and Fmoc-protected amino acids were obtained from
Advanced ChemTech. N,N,N′,N′-Tetramethyl-O-(1H-benzotriazol-1-yl)uranium hexafluorophosphate
(HBTU), 2,3-dibromothiophene, and (benzotriazol-1-yloxy)tripyrrolidinophosphonium
hexafluorophosphate (PyBOP) were purchased from Oakwood Products Inc.
All other reagents and starting materials were obtained from Sigma-Aldrich
and were used as received. 3-(Tributylstannyl)thiophene (S4) was prepared using literature procedures.55 (link)
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5

Praziquantel Synthesis and Characterization

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Praziquantel (PZQ, (11bRS)-2-(Cyclohexylcarbonyl)-1,2,3,6,7,11b-hexahydro-4-H-pyrazino[2,1-a]isoquinolin-4-one)) was of Ph. Eur. grade and kindly donated by Fatro S.p.a. (Bologna, Italy). Nitromethane, acetonitrile, 1,4-dioxane, ethyl acetate, ethanol, methanol, 2-pyrrolidone and acetic acid of reagent grade were from SIGMA-Aldrich (Milano, Italy). The HiPersolv Chromanorm methanol used for the HPLC analysis was purchased from VWR Chemicals (BHD PROLABO, Milano, Italy).
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6

Synthesis of AuCl3 Dopant on MoS2 Devices

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The synthesis of AuCl3 dopant is according to the previous reports40 (link)–42 (link). Briefly, 30 mg gold chloride (AuCl3) powders (≥99.99 %, Sigma Aldrich) were dissolved in the 5 ml nitromethane (≥95 %, Sigma Aldrich), then the solutions (20 mM) were sonicated for 3 h at 60 degrees followed by filtration to filter the large Au aggregates. The 20 mM AuCl3 solutions were then diluted with different concentration (10 mM and 5 mM). Note that all operations were performed in glove box to protect the reagents from the air environment. About 3–5 drops of 5 mM AuCl3 solutions were dropped on the SiO2/Si substrate with MoS2 devices on top and spin-coated at 3000 rpm for 1 min, then baked on the hotplate at 100 °C for 5 min.
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7

Fabrication of Stretchable Electrode Device

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Key steps in the fabrication of the device are overviewed in Figure 2b. The key fabrication steps were as follows: i) the stretchable electrode was mounted under tension on a thin optical glass substrate (24 mm x 60 mm, #0‐thickness cover glass, Gold Seal) with 250 µm‐thick double‐sided acrylic tape (3M), and a drop (≈0.5–2 µL) of liquid acrylic photoresist (IP‐Dip, Nanoscribe, GmbH) was deposited over and beneath the recording array; ii) the glass and sample were inverted and the microclip cap (Figure 2c) printed through the optical glass substrate using a two‐photon‐polymerization‐based, dip‐in resonant direct laser writing (rDWL) process;[79] iii) the glass substrate and sample were righted, and the base of the microclip was printed with the rDWL process; iv) the photoresist was developed and tape adhesive dissolved by submerging the glass substrate, electrode, and nanoclip in nitromethane (Sigma Aldrich) for 20 min, and the whole device rinsed in methoxy‐nonafluorobutane (Novec 7100; 3M) to remove trace solvent residue; v) the assembly was removed from the glass slide and compression bonded to a connectorized PCB as described above. All mechanical design was performed with Solidworks (Dassault Systèmes). All tested and imaged devices were fabricated using a custom rDLW system.[79]
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8

Single-crystal Perovskite Synthesis and Growth

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The single-crystal samples were synthesized on the basis of our previously published method (35 (link)). For MAPbBr3, the precursor solution (0.45 M) was prepared by dissolving equal molar ratio of MABr (Dyesol, 98%) and PbBr2 (Sigma-Aldrich, ≥98%) in dimethylformamide (DMF; Sigma-Aldrich, anhydrous 99.8%). After filtration, the crystal was allowed to grow using a mixture of dichloromethane (Sigma-Aldrich, ≥99.5%) and nitromethane (Sigma-Aldrich, ≥96%) as the antisolvent (41 (link)). Similar method was used for CsPbBr3 crystal growth (42 ). The precursor solution (0.38 M) was formed by dissolving equal molar ratio of CsBr (Sigma-Aldrich, 99.999%) and PbBr2 in dimethyl sulfoxide (DMSO; EMD Millipore Co., anhydrous ≥99.8%). The solution was titrated by methanol until yellow precipitates show up and did not redissolve after stirring at 50°C for a few hours. The yellow supernatant was filtered and used for the antisolvent growth. Methanol was used for the slow vapor diffusion. All solid reactants were dehydrated in a vacuum oven at 150°C overnight, and all solvents were used without further purification.
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9

Rare Earth Mineral Characterization

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Two
major rare earth minerals,
bastnaesite and xenotime (as the main sources for light and heavy
rare earth elements), were used in this study. Bastnaesite (REE)CO2F and xenotime YPO4 were obtained from Zagi Mountain
in Pakistan and Bahia in Brazil, respectively. Both mineral samples
were highly crystalline. The surface of mineral specimens was sequentially
polished by 800, 1200, and 2400 grit silicon carbide grinding papers.
When passing from one polishing paper to the next finer grade, the
polished samples were immersed in and rinsed with acetone, ethanol,
and deionized water to remove any traces of contaminants and polishing
powder. This procedure was followed by drying the samples in the oven
at 50 °C. Five probe liquids with known surface energy components
were used for contact angle measurement and surface energy analysis:
distilled water, formamide (>99.5%), ethylene glycol (99.8%), nitromethane
(99.9%), and undecane (>99%), were purchased from Sigma-Aldrich
(St.
Louis, MO). The surface tension components of the used probe liquids
are presented in Table 1.
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10

Synthesis of Functionalized Polymer Microspheres

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4-Vinylbenzyl chloride
(VBC), divinylbenzene (DVB, 80%), and chlorosulfonic acid were purchased
from Sigma-Aldrich. Also, styrene, Span-80 (sorbitan monooleate, HLB
= 4.3), potassium persulfate (K2S2O8), calcium chloride dihydrate (CaCl2·2H2O), methanol, dimethylformamide (DMF), ethylenediamine (EDA), benzaldehyde
dimethyl acetal, nitromethane, malononitrile, ethanol, and toluene
were purchased from Merck and were used as received without further
purification. Distilled water was used for all experiments.
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