FePcBN-17

Date

16.03.2023

Synthesis

  1. Preheat Fisherbrand FB15049 ultrasonic bath filled with ethyleneglycol to 80°C
  2. Add 102 mg of h-BN, 29.9 mg of FePcCl and 200 ml of DMF to 250 ml 2-neck round-bottom flask
  3. Close wide neck with stopper and purge flask with Ar for 10 min through small neck.
  4. Close small neck with stopper
  5. Place flask to US-bath and treat for 4 hr
  6. Leave flask overnight in a room with air conditioner set to 22°C
  7. Separate solid particles from DMF using Hetich Universal 320 centrifuge at 6000 rpm for 60 min
  8. Wash with distilled water twice using ultrasonic treatment with US Bandelin Sonopuls UW 2200 at 50% power for 1 min and centrifugation at 6000 rpm for 60 min
  9. Make 80 ml of suspension and add it to 250 ml polypropylene flask
  10. Freeze suspension with liquid nitrogen
  11. Dry in Cryst alpha 1-2 LO plus freeze-dryer at 0.05 mbar for 4 days

ms = 31.3 mg

Sample after washing Sample after drying

ICP AES

  1. Place 10.8 mg of sample into 15 ml centrifuge tube
  2. Add 1.25 ml of concentrated HNO3 and 3.75 ml of concentrated HCl
  3. Place tube to US bath (NB: do under the hood) for 2 h
  4. Leave under the hood for another 2 h
  5. Centrifuge at 6000 rpm for 10 min
  6. Take 1 ml for analysis
  7. Make measurement of iron concentration by inductively coupled plasma atomic emission spectroscopy on an ICAP-6300 Radial spectrometer.

cFe = 32.1 mg/L

Phthalocyanine adsorption = 17.82 mg/100 mg BN