cMOF Evidence Base

Synthesis evidence

Employing Triphenylene-Based, Layered, Conductive Metal-Organic Framework Materials as Electrochemical Sensors for Nitric Oxide in Aqueous Media

Ambrogi E.K., Li Y., Chandra P. et al. · ACS Sensors · 2025 · 553-562

8 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Hydrothermal

S3 · Synthesis Of Triphenylene-Based Metal-Organic Frameworks · Figure S1

Metal precursorscobalt(II) acetate tetrahydrate, 327 mg (1.85 mmol)
Linker precursorshexahydroxytriphenylene (HHTP), 300 mg (0.925 mmol)
Solvents15 mL DI water
Atmosphereopen to air
Temperature85
Timeovernight
Work-upCollected by vacuum filtration and washed with water and ethanol.
ActivationSoaked in water for 3 days, ethanol for 3 days, then acetone for 3 days; dried in vacuum oven at 50 deg C, 20 torr overnight.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Linkerhexahydroxytriphenylene (HHTP)300 mg (0.925 mmol)S3 · Synthesis Of Triphenylene-Based Metal-Organic Frameworks · Figure S1
Metal Sourcecobalt(II) acetate tetrahydrate327 mg (1.85 mmol)S3 · Synthesis Of Triphenylene-Based Metal-Organic Frameworks · Figure S1
SolventDI water15 mLS3 · Synthesis Of Triphenylene-Based Metal-Organic Frameworks · Figure S1
Complete recipeSource: Both

Route 2: Hydrothermal

S4 · Synthesis Of Triphenylene-Based Metal-Organic Frameworks · Figure S1

Metal precursorscopper(II) trifluoroacetylacetonate, 515 mg (1.39 mmol)
Linker precursorshexahydroxytriphenylene (HHTP), 225 mg (0.667 mmol)
Solvents15 mL 9:1 water:ethanol mixture
Atmosphereopen to air
Temperature85
Timeovernight
Work-upCollected by vacuum filtration and washed with water and ethanol.
ActivationSoaked in water for 3 days, ethanol for 3 days, then acetone for 3 days; dried in vacuum oven at 50 deg C, 20 torr overnight.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Linkerhexahydroxytriphenylene (HHTP)225 mg (0.667 mmol)S4 · Synthesis Of Triphenylene-Based Metal-Organic Frameworks · Figure S1
Metal Sourcecopper(II) trifluoroacetylacetonate515 mg (1.39 mmol)S4 · Synthesis Of Triphenylene-Based Metal-Organic Frameworks · Figure S1
Solventwater:ethanol15 mL · 9:1S4 · Synthesis Of Triphenylene-Based Metal-Organic Frameworks · Figure S1
Complete recipeSource: Both

Route 3: Drop Cast

555 · General Preparation of HHTP MOF Electrodes

Metal precursorsNi3(HHTP)2 powder
Solventswater
Atmosphereambient air drying
Timesonication at least 5 h; air dry 0.5-1 h after each drop
Substrate orientation3 mm diameter polished glassy carbon electrode
Work-upPolished with 0.05 um alumina slurry and rinsed with water and ethanol before drop-casting.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherNi3(HHTP)2 powder5 mg · 5 mg/mL suspension555 · General Preparation of HHTP MOF Electrodes
Solventwater1 mL555 · General Preparation of HHTP MOF Electrodes
OtherMOF suspension droptwo 2.5 uL drops555 · General Preparation of HHTP MOF Electrodes
Complete recipeSource: SI

Route 4: Drop Cast

S7 · Polymer Coatings · Figure S26

Metal precursorsNi3(HHTP)2 powder
Solventswater
AdditivesNafion solution, 0.25-1 wt% prepared from 5% Nafion
Atmosphereambient air drying
Time30 min-1 h air drying
Substrate orientationNi3(HHTP)2 film on glassy carbon
Work-up5 uL Nafion solution dropcast onto bare GCE or GCE previously dropcast with MOF.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
AdditiveNafion50-200 uL 5% Nafion diluted to 1 mL total · 0.25-1 wt%S7 · Polymer Coatings · Figure S26
Solventwater800-950 uLS7 · Polymer Coatings · Figure S26
OtherNafion solution drop5 uLS7 · Polymer Coatings · Figure S26
Complete recipeSource: SI

Route 5: Drop Cast

S7-S8 · Polymer Adhesives · Figures S29-S30

Metal precursorsNi3(HHTP)2 powder
SolventsDI water
AdditivesPEDOT:PSS dispersion, 0.3-0.4%
Atmosphereambient air drying
Timeair dry after PEDOT:PSS layer; MOF drops air dried 0.5-1 h
Substrate orientationPEDOT:PSS adhesive layer on polished glassy carbon
Work-upDropcast PEDOT:PSS adhesive layer, air dry, then dropcast MOF as for pristine electrode.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
AdditivePEDOT:PSS dispersion2.5 uL · 0.3-0.4%S7-S8 · Polymer Adhesives · Figures S29-S30
SolventDI water900 uL used with 100 uL 3-4% PEDOT:PSS dispersionS7-S8 · Polymer Adhesives · Figures S29-S30
OtherNi3(HHTP)2 suspensiontwo 2.5 uL drops · 5 mg/mLS7-S8 · Polymer Adhesives · Figures S29-S30
Complete recipeSource: Both

Route 6: Hydrothermal

S3-S4 · Synthesis Of Triphenylene-Based Metal-Organic Frameworks · Figure S1

Metal precursorsnickel(II) acetate tetrahydrate, 177 mg (1.00 mmol)
Linker precursorshexahydroxytriphenylene (HHTP), 162 mg (0.500 mmol)
Solvents15 mL DI water
Atmosphereopen to air
Temperature85
Timeovernight
Work-upCollected by vacuum filtration and washed with water and ethanol.
ActivationSoaked in water for 3 days, ethanol for 3 days, then acetone for 3 days; dried in vacuum oven at 50 deg C, 20 torr overnight.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Linkerhexahydroxytriphenylene (HHTP)162 mg (0.500 mmol)S3-S4 · Synthesis Of Triphenylene-Based Metal-Organic Frameworks · Figure S1
Metal Sourcenickel (II) acetate tetrahydrate177 mg (1.00 mmol)S3-S4 · Synthesis Of Triphenylene-Based Metal-Organic Frameworks · Figure S1
SolventDI water15 mLS3-S4 · Synthesis Of Triphenylene-Based Metal-Organic Frameworks · Figure S1
Complete recipeSource: SI

Route 7: Drop Cast

S8 · Preparation of Ni3(HHTP)2-functionalized screen-printed electrodes · Figure S35

Metal precursorsNi3(HHTP)2 suspension prepared as for GCE films
Solventswater
Atmosphereambient air drying
Time15-20 min air drying between drops
Substrate orientationWE1 of carbon-paste screen-printed electrode on PET
Work-upDropcast two 0.5 uL drops on WE1; used same day.
Scalability contextMiniaturised circular electrode area approximately 3.5 mm diameter; 2-4 mL electrolyte volume.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
OtherNi3(HHTP)2 suspensiontwo 0.5 uL drops · prepared as described aboveS8 · Preparation of Ni3(HHTP)2-functionalized screen-printed electrodes · Figure S35
Complete recipeSource: Both

Route 8: Hydrothermal

555 · Experimental Methods

Metal precursorszinc chloride, 0.045 mmol (6.1 mg)
Linker precursorshexahydroxytriphenylene, 0.03 mmol (9.7 mg)
Solventswater
Additivessodium acetate, 150 mg (1.8 mmol)
Temperature70
Time24
Work-upCollected by vacuum filtration and washed with water and ethanol.
ActivationActivated by soaking in ethanol followed by acetone.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Linkerhexahydroxytriphenylene0.03 mmol (9.7 mg)555 · Experimental Methods
Metal Sourcezinc chloride0.045 mmol (6.1 mg)555 · Experimental Methods
Additivesodium acetate150 mg (1.8 mmol)555 · Experimental Methods
SolventwaterNot specified555 · Experimental Methods