The sample suspension medium was CHC. The received CHC (conductivity>>1,000 pS cm−1) was deionized by using molecular sieves (4 Å, Aldrich) and subsequent neutral aluminium oxide (Aldrich). After purification, CHC had a conductivity as low as around 5–10 pS cm−1. Rectangular capillaries (0.1 × 1 mm2, 0.1 × 2 mm2, 0.5 × 0.5 mm2, VitroCom, UK) were used as the sample cells. Electrodes consisting of a 3 nm layer of Cr and a 6–10 nm layer of Au were sputter-coated on two opposing outer surfaces of these capillaries and connected to a function generator and amplifier. The sample capillary was then fixed on a glass slide and sealed with UV-cured glue (Norland, No. 68).
Molecular sieves
Manufactured by Merck Group
Sourced in Germany, United States
Molecular sieves are porous, crystalline materials that are used to selectively adsorb molecules based on their size and shape. They function by allowing smaller molecules to pass through their pores while trapping larger molecules, effectively separating and purifying substances. Molecular sieves are commonly used in a variety of industrial applications, including gas separation, drying, and catalysis.
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Lab products found in correlation
Methanol, by Merck Group (4 mentions)
Acetone, by Merck Group (4 mentions)
Dimethyl sulfoxide (dmso), by Merck Group (3 mentions)
Whatman, by Cytiva (3 mentions)
Chloroform, by Merck Group (3 mentions)
Triethylamine, by Merck Group (3 mentions)
N n dimethylformamide (dmf), by Thermo Fisher Scientific (2 mentions)
Ferrocene, by Merck Group (2 mentions)
Ethanol, by Merck Group (2 mentions)
Tert butanol, by Merck Group (2 mentions)
Hydrochloric acid (hcl), by Merck Group (2 mentions)
Sodium hydroxide (naoh), by Merck Group (2 mentions)
Dimethyl carbonate, by Merck Group (2 mentions)
N n dimethylformamide (dmf), by Merck Group (2 mentions)
β cyclodextrin, by Merck Group (1 mentions)
Avance 3 spectrometer, by Bruker (1 mentions)
Dimethylaminopyridine, by Merck Group (1 mentions)
Methanol, by Thermo Fisher Scientific (1 mentions)
Phenol, by Thermo Fisher Scientific (1 mentions)
Dimethylformamide, by Thermo Fisher Scientific (1 mentions)
35 protocols using molecular sieves
1
Deionized Capillary Cell Suspension Characterization
2
Synthesis of Acetylated Salicylates
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Tris-(hydroxymethyl)aminomethane (THAM) (99%), β-cyclodextrin and molecular sieves (3 Å) were purchased from Aldrich Chemical Company, while N,N-dimethylformamide (DMF) (99.98%) was purchased from Fisher Scientific International Company.
O-acetyl salicylic acid (99%), 4-acetoxybenzoic acid (98%) and 5-acetylsalicylic acid (98%) from Lancaster Synthesis were used in this work.
O-acetyl salicylic acid (99%), 4-acetoxybenzoic acid (98%) and 5-acetylsalicylic acid (98%) from Lancaster Synthesis were used in this work.
3
General Organic Chemistry Procedures
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All reactions were performed on the benchtop under ambient atmosphere. Reagents and solvents were purchased from commercial suppliers (Sigma-Aldrich, Merck, Neon, Acros Organics, TCI, Reatec, Alphatec, CRQ, Neon, or Vetec) and used without further purification. Molecular sieves 3 Å 8–12 mesh (Aldrich Chemical Company) were used to remove water molecules formed during the reaction. TLC silica gel 60 Å plates (MACHEREY-NAGEL) were used to accompany the progress of the reactions (mobile phase: DCM 9 : 1 MeOH v/v), and UV light 254 nm was used to reveal them. NMR spectra were recorded on a Bruker Avance III spectrometer (500 MHz for 1H and 125 MHz for 13C). Chemical shifts were reported in parts per million (δ) relative to the residual solvent resonance (CDCl3 = 7.26 ppm for 1H and 77.0 ppm for 13C, CD3OD = 3.31 ppm for 1H and 49.0 ppm for 13C), and coupling constants (J) in hertz (Hz). The signal multiplicity was denoted by the abbreviations: s (simplet), d (doublet), dd (doublet of doublets), m (multiplet), and sept (septet). Melting points were recorded on a Microquímica MQAPF-302 melting point equipment. LC-HRMS analysis acquired on Dionex LC UltiMate 3000 coupled HRMS Q-Exactive Plus (Thermo Scientific, Frenton, CA, USA).
4
Preparation of Mg(TFSI)2 Electrolyte
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Example 2
Preparation of Electrolyte: Mg(TFSI)2 in THF and dimethylamine. Magnesium bis(trifluoromethane sulfonyl)imide (99.5%, Solvionic, France) was dried in a vacuum oven at 180° C. overnight before use. THF (Aldrich, anhydrous, 99.5%) solvent was pretreated with molecular sieves (Aldrich, 3 Å beads, 4-8 mesh) overnight and then added into the dried Mg(TFSI)2. Dimethylamine was added to the Mg(TFSI)2/THF electrolyte. The as-prepared electrolyte was then stirred overnight before use. Water levels of the as prepared electrolytes were determined from Karl-Fischer analysis, and the water content was observed to be less than 15 ppm. The solubility of Mg(TFSI)2 in THF-DMA is about 2.0 M.
5
Preparation of Mg(TFSI)2 Electrolyte
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Example 1
Preparation of Electrolyte: Mg(TFSI)2 in Diglyme. Magnesium bis(trifluoromethane sulfonyl)imide (99.5%, Solvionic, France) was dried in a vacuum oven at 180° C. overnight prior to use. Diglyme (Aldrich, anhydrous, 99.5%) solvent was pretreated with molecular sieves (Aldrich, 3 Å beads, 4-8 mesh) overnight and then added into the dried Mg(TFSI)2. The as-prepared electrolyte was then stirred overnight before use. Water levels of the as prepared electrolytes were determined from Karl-Fischer analysis, and the water content was observed to be less than 15 ppm.
6
Synthesis and Characterization of Functionalized Boltorn H40
7
3DISCO Tissue Clearing Protocol
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Tissue clearing was done using the 3DISCO protocol [10 (link)]. Briefly, samples were dehydrated in ascending concentrations (50, 70, 80 and 100%) of Tetrahydrofuran (THF, Roth) adding molecular sieves (Sigma) at the last step. The incubation of THF 100% was done for 3 × 12 h. Samples were then immersed in Dibenzylether (DBE, Merck) until clearing was completed, but at least for 3 days. Samples were then analyzed using a light sheet fluorescence microscope (UltraMicroscope II, LaVision BioTec).
8
Fabrication of Conductive AAO Membranes
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AAO membranes were purchased from Whatman (Anodisc 6809-6012, 25 mm diameter, 100 nm pore size) and rendered electrically conductive by depositing 100-nm Au on one side of the membrane via thermal evaporation. The electrolytes were prepared by dissolving the corresponding salts zinc bis(trifluoromethanesulfonyl)imide (Alfa Aesar), lithium bis(trifluoromethanesulfonyl)imide (Solvay), and/or tetrabutylammonium hexafluorophosphate (Sigma-Aldrich) in PC (anhydrous, 99.7%, Sigma-Aldrich), EG (anhydrous, 99.8%, Sigma-Aldrich), and/or dimethyl sulfoxide (Sigma-Aldrich). PC and EG were dried over molecular sieves (4 Å, Sigma-Aldrich) before use. Ferrocene and anthraquinone were purchased from Sigma-Aldrich.
9
Electrochemical Study of Ferrocene Derivatives
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Azulene (99.7%), FeTOS
hexahydrate (technical
grade), FeCl3 (97% reagent grade), ferrocene (98%), and
tetrabutylammonium tetrafluoroborate (TBABF4) (99%) were
purchased from Sigma-Aldrich. CuCl2 dihydrate (99–101%)
and CuBr2 were purchased from J. T. Baker, and CuCl2 dihydrate was dried in a vacuum oven. n-Butanol
(AR grade) and pyridine (AR grade) were obtained from Lab-scan analytical
sciences. Acetonitrile (MeCN) (anhydrous, 99.8%) was obtained from
VWR Chemicals. ferrocene, azulene, FeTOS, FeCl3, and n-butanol were used without further purification. TBABF4 was dried in a vacuum oven at 75 °C for 2 h before use.
MeCN was dried using molecular sieves (4 Å, Sigma-Aldrich) for
more than 24 h before electrochemical measurements.
hexahydrate (technical
grade), FeCl3 (97% reagent grade), ferrocene (98%), and
tetrabutylammonium tetrafluoroborate (TBABF4) (99%) were
purchased from Sigma-Aldrich. CuCl2 dihydrate (99–101%)
and CuBr2 were purchased from J. T. Baker, and CuCl2 dihydrate was dried in a vacuum oven. n-Butanol
(AR grade) and pyridine (AR grade) were obtained from Lab-scan analytical
sciences. Acetonitrile (MeCN) (anhydrous, 99.8%) was obtained from
VWR Chemicals. ferrocene, azulene, FeTOS, FeCl3, and n-butanol were used without further purification. TBABF4 was dried in a vacuum oven at 75 °C for 2 h before use.
MeCN was dried using molecular sieves (4 Å, Sigma-Aldrich) for
more than 24 h before electrochemical measurements.
10
Lithium-Sulfur Battery Electrolyte Preparation
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V2O5 (Pechiney), N-methyl-2-pyrrolidone
(NMP, anhydrous, Sigma-Aldrich),
poly(vinylidene fluoride) (PVdF, Solef 6020), carbon black (Super
C65, Imerys), glass fiber sheet (Whatman GF/F), LP30 (BASF, battery
grade), lithium metal (Honjo, battery grade), and dimethyl carbonate
(DMC, UBE, battery grade) were directly used as received. Molecular
sieves (3 Å, Alfa Aesar) were dried at 300 °C under vacuum
(10–3 mbar) for more than 1 week. LiTFSI (3M Co.,
Ltd.) was dried at 120 °C under vacuum (10–3 mbar) for 12 h before use. The residual water in tetraethylene glycol
dimethyl ether (tetraglyme, Sigma-Aldrich, 99%) was removed via the
dried molecular sieves before use.
(NMP, anhydrous, Sigma-Aldrich),
poly(vinylidene fluoride) (PVdF, Solef 6020), carbon black (Super
C65, Imerys), glass fiber sheet (Whatman GF/F), LP30 (BASF, battery
grade), lithium metal (Honjo, battery grade), and dimethyl carbonate
(DMC, UBE, battery grade) were directly used as received. Molecular
sieves (3 Å, Alfa Aesar) were dried at 300 °C under vacuum
(10–3 mbar) for more than 1 week. LiTFSI (3M Co.,
Ltd.) was dried at 120 °C under vacuum (10–3 mbar) for 12 h before use. The residual water in tetraethylene glycol
dimethyl ether (tetraglyme, Sigma-Aldrich, 99%) was removed via the
dried molecular sieves before use.
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