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22 protocols using diethyl carbonate

1

Synthesis of LiFePO4 Coin Cell Electrolyte

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Trimethylolpropane triglycidyl ether (TMPTE, technical grade) and LiFSI (ultradry, 99.9%) were obtained from Sigma-Aldrich (Seoul, South Korea). Solvents of ethylene carbonate (EC, ≥99%, acid <10 ppm, H2O <10 ppm), diethyl carbonate (DEC, ≥99%, acid <10 ppm, H2O <10 ppm), and N-methyl-2-pyrrolidone (NMP) were procured from Sigma-Aldrich (Seoul, South Korea). Coin cell cases, aluminum foil, copper foil, and related components were purchased from the MTI Corporation (Richmond, CA, USA). Lithium iron (II) phosphate (LiFePO4), carbon black (super P, Timcal), and poly(vinylidene fluoride) (PVDF, power) were purchased from Alfa Aesar (Seoul, South Korea).
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2

Lithiation of Thin-Film and Bulk MoS2 for TDTR Analysis

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The thin-film and bulk MoS2 samples were assembled into battery configuration inside an argon-filled glovebox for lithium ion intercalation. Lithiation of thin-film MoS2 was performed in a glass vial. The thin-film MoS2 and a piece of lithium foil were used as the cathode and anode, respectively, and 1.0 M LiPF6 in 30:70 (vol%) ethylene carbonate/dimethyl carbonate (Sol-Rite) as the electrolyte. The thin-film sample was wrapped around by a piece of stainless steel foil, which was used as the electrical contact. The discharge current was 14 μA. The lithium ion intercalation of the bulk MoS2 was carried out using 2025 coin cells, with MoS2 as the cathode, lithium foil as the anode, 1.0 M LiPF6 in 30:70 (vol%) ethylene carbonate/dimethyl carbonate as electrolyte, and a Celgard 2400 separator. The discharge current used for the bulk MoS2 was 10 μA. After the discharge process, all samples were relaxed for days before they were cleaned by diethyl carbonate (anhydrous, Sigma Aldrich) inside the glovebox to remove the electrolyte left on the sample surfaces. Samples were sealed in air-tight aluminium pouches before they were transferred out of the glovebox and mailed from Ann Arbor, MI to Urbana, IL for sputtering deposition of Al or NbV for TDTR measurements.
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3

Synthesis and Characterization of Polycaprolactone

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ε-Caprolactone (εCL) (98%, Sigma-Aldrich,
Sweden) was dried over calcium hydride for at least 24 h and subsequently
distilled at reduced pressure under an inert gas atmosphere prior
to use. All of the other chemicals were used as received. These chemicals
included initiators (i.e., benzyl alcohol (≥99%, Sigma-Aldrich,
Sweden) and 2-naphthalene ethanol (98%, Sigma-Aldrich, Sweden)), catalysts
(i.e., 1,5,7-triazabicyclo[4.4.0]-dec-5-ene (TBD) (98%, Sigma-Aldrich,
Sweden)), and a phosphazene base P2-tBu
solution (P2-tBu, ∼2 M in THF,
Sigma-Aldrich, Sweden). In addition, sodium hydride (NaH) (60% dispersion
in mineral oil, Sigma-Aldrich, Sweden), diethyl carbonate (99%, Sigma-Aldrich,
Sweden), trimethylolpropane allyl ether (98%, Sigma-Aldrich, Sweden),
acetic acid (technical, Fisher Scientific, Germany), acetic acid anhydride
(ReagentPlus, ≥ 99%, Sigma-Aldrich, Sweden),
triethylamine (TEA) (≥99%, Sigma-Aldrich, Sweden), dichloromethane
(anhydrous, ≥ 99.8%, Sigma-Aldrich, Sweden) chloroform (HPLC
grade, Fisher Scientific, Germany), chloroform-d (99.8%,
with silver foil, Cambridge Isotope Laboratories), and methanol (general
purpose grade, Fischer Scientific, Germany) were used.
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4

Synthesis and Characterization of Nickel Complexes

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Procedures previously described in the literature were used to synthesize [NiAmben] [15 (link)], and [NiSalen] [52 (link)]. Their structures were confirmed by 1H and 13C NMR. Dimethyl sulfoxide (Acros Organics, Fair Lawn, NJ, USA, 99.7%), ethylene carbonate (Acros Organics, 99+%), diethyl carbonate (Sigma-Aldrich, 99%), and 1,2-dichloroethane (Sigma-Aldrich, MO, USA 99.8%) were used as received. Tetraethylammonium tetrafluoroborate Et4NBF4 (Sigma-Aldrich, 99%) was recrystallized from isopropyl alcohol and dried at 65 °C for 72 h before use. All solutions were prepared in an argon-filled glove box.
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5

Synthesis of Polymeric Precursors

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Hexanediol (Sigma-Aldrich, Sweden) and 1,8-diazabicyclo[5.4.0]undec-7-ene
(DBU) (Sigma-Aldrich, Sweden) were stored under an inert gas atmosphere
prior to use. Chloroform (HPLC grade, Fisher Scientific, Germany),
methanol (general purpose grade, Fisher Scientific, Germany), dichloromethane
(anhydrous, ≥ 99.8%, Sigma-Aldrich), toluene (anhydrous, ≥
99.8%, Sigma-Aldrich), acetonitrile (anhydrous, ≥ 99.8%, Sigma-Aldrich),
dichloromethane (DCM) (Fisher Scientific, Germany), sodium hydride
(NaH) (60% dispersion in mineral oil, Sigma-Aldrich, Sweden), diethyl
carbonate (99%, Sigma-Aldrich, Sweden), trimethylolpropane allyl ether
(98%, Sigma-Aldrich, Sweden), acetic acid (technical grade, Fisher
Scientific, Germany), and acetic acid anhydride (ReagentPlus, ≥
99%, Sigma-Aldrich, Sweden) were used as received.
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6

Synthesis and Characterization of Cobalt Complex

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Procedures previously described in the literature were used to synthesize the starting ligand H2Amben and [Co(Amben)] complex [21 (link)]. Their structures were confirmed by CHN elemental analysis for both compounds and 1H and 13C NMR for the ligand. Ethylene carbonate (Acros Organics, NJ, USA, 99+%) and diethyl carbonate (Sigma-Aldrich, MO, USA 99%) were used as-received. Tetraethylammonium tetrafluoroborate Et4NBF4 (Sigma-Aldrich, MO, USA 99%) was recrystallized from isopropyl alcohol and dried at 65 °C for 72 h before use. All electrochemical experiments were performed in an argon-filled glove box.
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7

Biochemical Mechanisms of Traditional Herbal Remedy

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XMJ crude drugs were purchased from Beijing Tong Ren Tang Co., Ltd. (Beijing, China). Phospho-eNOS-3 antibodies were purchased from Beijing Boaosen Biotechnology Co., Ltd. (BS-3447R; Beijing, China), horseradish peroxidase-labeled goat anti-rabbit IgG (heavy and light chains) antibody was purchased from Beijing Zhongshan Golden Bridge Biotechnology Co., Ltd. (PV-9003; Beijing, China) and Cy3-labeled goat anti-rabbit IgG (heavy and light chain) antibodies were purchased from Biyuntian Institute of Biotechnology (P0183; China). Lovastatin, H2O2, diethyl carbonate, XTT, phenazine methosulfate (PMS), diethylpyrocarbonate and avian myeloblastosis virus were purchased from Sigma-Aldrich (St. Louis, MO, USA). Zhibituo was purchased from Chengdu Diao Jiuhong Pharmaceutical Factory (Chengdu, China). Hematoxylin and eosin (HE) and Coomassie Brilliant Blue stains were purchased from Changsha Lixin Biotechnology Co., Ltd. (Changsha, China). Kits for the detection of malondialdehyde (MDA), superoxide dismutase (SOD), NO, interleukin (IL)-1, IL-6, intracellular adhesion molecule (ICAM)-1, vascular adhesion molecule (VCAM)-1, matrix metalloproteinase (MMP)-2, tissue inhibitor of metalloproteinase (TIMP)-2 and nuclear factor (NF)-κB were purchased from R&D Systems (Minneapolis, MN, USA). Other reagents were analytically pure and made in China.
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8

Coin Cell Assembly for TiO2 Anode Evaluation

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TiO2 and
TiO2–TUD-1 samples were mixed with poly(vinylidene
fluoride) (PVDF, Aldrich, >99%) and conductive Super P carbon (Alfa
Aesar, >99%) at a mass ratio of 14:3:3 and stirred overnight in
2
mL of 1-methyl 2-pyrrolidinone (NMP, Alfa Aesar, >99%). The slurry
was spread onto a clean copper surface to obtain a 20 μm thick
film that was then dried in an oven at 110 °C. The copper sheets
were cut to obtain disks to be used as the working electrodes in a
Li–metal half cell. The coin cells (the components of which
were purchased from MTI) were then assembled in a glovebox under an
argon atmosphere. The electrolyte consisted of 1 M lithium hexafluorophosphate
solution (LiPF6, Sigma-Aldrich) in a 50/50 v/v mixture
of ethylene carbonate (EC, Sigma-Aldrich) and diethyl carbonate (Sigma-Aldrich).
Layers were assembled in the order of the bottom case, anode, polypropylene
separator (Celgard), electrolyte, lithium metal (MTI), spacer (stainless
steel), wave spring, and top case. Coin cells were cycled on a Neware
battery testing system using a voltage window of 0.01 to 2.5 V. Nanosized
TiO2 (COM-TiO2, <25 nm particle size, Aldrich,
99.7% anatase) was used as received for comparison purposes.
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9

Synthesis and Characterization of Dyes

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Methyl chloroformate 98%, 3-amino phenol, ethyl acetoacetate, ethyl benzoate, diethylcarbonate 97% and 4-bromoacetophenone 98% were purchased from Sigma Aldrich (Germany) and used directly without any further purification. All solvents used (dioxan, dimethylsulfoxide, dimethylformamide, acetonitrile, acetic acid and acetone) were of spectroscopic grade. 100% polyester fabric (91 g/m2, yarn count: dtex 44) was supplied by El-Mahalla El-Kobra Company, Egypt. The fabrics were scoured before application in an aqueous bath containing 2 g.L−1 of nonionic detergent at 80 °C for 30 min to remove any processing oils and impurities. Thin-layer chromatography (TLC) was performed by a Kieselgel 60 F254 (Merck, Darmstadt, Germany), for observation of reaction progress and the purity of the prepared intermediates and synthesized dyes.
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10

Preparation of Dry Lithium-Ion Electrolyte

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3A molecular sieves (eight mesh) were cleaned and dried, transferred into an argon glove box (<0.2-ppm O2 and <0.01-ppm H2O), regenerated in an oven at 250°C for 12 hours, and allowed to slowly cool back to room temperature. A 1:1 (v/v) mixture of ethylene carbonate (99+%; Acros) and diethyl carbonate (>99% anhydrous; Sigma-Aldrich) was prepared in the glove box and then dried over 4A molecular sieves for at least 1 week to achieve minimal H2O impurities. In the glove box, LiPF6 salt (≥99.99% trace metals basis; Sigma-Aldrich) was dried at 65°C for 48 hours to minimize any H2O impurities in the salt. The dried electrolyte was then prepared by mixing the salt with the 1:1 (v/v) mixture of ethylene carbonate and diethyl carbonate to achieve a 1 M concentration. All coin-cell materials were then dried in the glove box oven at 50°C for 2 hours before cell assembly.
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