Synthesis evidence

Synthesis and characterization of Fe3O4-supported metal–organic framework MIL-101(Fe) for a highly selective and sensitive hydrogen peroxide electrochemical sensor

Salman F., Zengin A., Celik Kazici H. · Ionics · 2020 · 5221-5232

3 structured synthesis routes

Completeness describes how fully the route could be reconstructed from the main article and supporting information.

Vague recipeSource: Main

Route 1: Solvothermal

5222 · Preparation of Fe3O4@MIL-101(Fe) nanoparticles

Metal precursorsnot fully reported in this paper
Solventsnot fully reported in this paper
Additivesmercaptoacetic acid / MAA modification reported
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
AdditiveMercaptoacetic acid (MAA)Not specified5222 · Preparation of Fe3O4@MIL-101(Fe) nanoparticles
Partial recipeSource: Main

Route 2: Other

5222 · Preparation of Fe3O4@MIL-101(Fe) nanoparticles

Metal precursorsFeCl3.6H2O, 10 mM
Linker precursorsH3btc, 10 mM
Solventsethanol washing; water or unspecified dispersion medium
AdditivesMAA@Fe3O4 nanoparticles
Atmospherevacuum during final drying
Temperature70 C for H3btc step; 200 C vacuum drying
Time0.25 h FeCl3 step; 0.5 h H3btc step; cycle repeated 21 times
Work-upmagnetic separation and washing with plenty of ethanol after FeCl3 step and after H3btc step
Activationdried under vacuum at 200 C
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherMAA@Fe3O4 nanoparticles100 mg5222 · Preparation of Fe3O4@MIL-101(Fe) nanoparticles
Metal SourceFeCl3.6H2O10 mM5222 · Preparation of Fe3O4@MIL-101(Fe) nanoparticles
LinkerH3btc10 mM5222 · Preparation of Fe3O4@MIL-101(Fe) nanoparticles
Solventethanolplenty for washing5222 · Preparation of Fe3O4@MIL-101(Fe) nanoparticles
Partial recipeSource: Main

Route 3: Drop Cast

5222 · Preparation of the MIL-101(Fe)@Fe3O4/NGCE sensor

Solventsethyl alcohol, water; ethyl alcohol/water 1:1 for cleaning; methyl alcohol and water rinse
AdditivesNafion 5% dispersion
AtmosphereN2 stream for electrode drying before modification
Temperature70 C drying after drop moulding
Timesonication 1 h; final drying approximately 1 h
Substrate orientationglassy carbon working electrode
Work-upGCE polished with 1.0, 0.3 and 0.05 um Al2O3; sonicated at least 10 min; rinsed/shaken with methanol and water
Activationdried at 70 C for approximately 1 h
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherMIL-101(Fe)@Fe3O41.0 mg/mL5222 · Preparation of the MIL-101(Fe)@Fe3O4/NGCE sensor
Additivenafion (5%) dispersion in ethyl alcohol0.5 mg/mL5222 · Preparation of the MIL-101(Fe)@Fe3O4/NGCE sensor
SolventwaterNot specified5222 · Preparation of the MIL-101(Fe)@Fe3O4/NGCE sensor
Solventethyl alcoholNot specified5222 · Preparation of the MIL-101(Fe)@Fe3O4/NGCE sensor