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3 protocols using ammonium tetrafluoroborate

1

Fabrication of Lithium-Ion Solid Electrolyte

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All chemicals and solvents were used as received without further purification. Titanium foil (99.5%, 100 μm in thickness), copper foil (99.9%, 30 μm in thickness), and copper mesh were purchased from Nilaco Corporation. Iron(ii) chloride tetrahydrate (FeCl2·4H2O, 98%), ammonium tetrafluoroborate (NH4BF4, 97%), 4,4′-bipyridine, 2,2′:6′,2′′-terpyridine (98%), 1-iodohexane, bis(trifluoromethane) sulfonimide lithium salt (LiTFSI, 99.95%), and lithium metal were purchased from Sigma-Aldrich. The Li+-ion solid electrolyte was purchased from Ohara Corporation. Ethylene carbonate (EC, water content < 30 ppm) and dimethyl carbonate (DMC, water content < 30 ppm) were obtained from Kishida Chemicals. The polyvinylidene fluoride (PVDF) binder was obtained from MTI Corporation. N-Methyl-2-pyrrolidone (NMP) was obtained from J&K Chemicals. Super P carbon was obtained from TIMCAL.
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2

Radiolabeling Precursor Preparation with Boron Trifluoride

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Methanol, acetonitrile (HPLC grade) and ethanol (HPLC grade) were purchased from Rathburn Chemicals UK Ltd. All the reagents, ammonium tetrafluoroborate, anhydrous acetonitrile, and anhydrous methanol were purchased from Sigma Aldrich (UK). Sep-Pak Accell Plus QMA Carbonate Plus Light Cartridge (46 mg of sorbent per cartridge, 40 μm particle size), Sep-Pak alumina N Plus Light Cartridge, Oasis WAX Plus short cartridge (225 mg sorbent per cartridge, 60 μm particle size), and Sep-Pak Florisil Plus Light Cartridge were purchased from Waters UK. 0.9 % saline was purchased from Greater Glasgow & Clyde NHS Pharmacy Distribution Centre. All Sep-Pak cartridges were used without prior conditioning.
Boron trifluoride acetonitrile complex solution, 15.2–16.8% BF3 basis; boron trifluoride-methanol solution, ~ 10% (~ 1.3 M), for GC derivatization; boron trifluoride dihydrate, 96% and aqueous ammonium hydroxide (25%) were purchased from Sigma-Aldrich. Precursors for [18F]TFB radiolabelling were diluted in an anhydrous solvent to the desired concentration as described in the "Results" and Discussion" sections. To obtain 1/500 dilution 3 µL of 10% boron trifluoride methanol solution was withdrawn from the original 10 mL shipment bottle by means of the 10 µL glass GC syringe and dissolved in 1500 µL of anhydrous acetonitrile in a sealed 2mL glass HPLC sample vial.
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3

Chrysotile Fiber Fluorination Yield

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Example 6

10 mg of chrysotile were immersed in equal volume of aqueous 0.12 M of Ammonium tetrafluoro borate (Sigma-Aldrich) and 0.2 M boric acid as fluorine scavenger. The reaction was monitored each hour for 8 FIRS using a pH meter to assess the pH. The precipitate was separated with a cellulose filter (low ashes) and was dried for one day in an oven at 55° C. Gravimetric analysis was implemented to assess the final yield. For the gravimetric analysis a temperature of 600° C. (for one minute) was reached to burn the filter. The yield after four measurements was of 95.3%. The optical measurements were assessed with a Nicolet 6700 Spectrophotometer.

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