cMOF Evidence Base

Synthesis evidence

Conductive metal organic framework for ion-selective membrane-free solid-contact potentiometric Cu2+ sensing

Xu L., Gan S., Zhong L. et al. · Journal of Electroanalytical Chemistry · 2022 · 115923

3 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Drop Cast

p002 · 2.3 Fabrication of Cu3(HHTP)2-based SC-ISEs

Metal precursorsCu3(HHTP)2/PVDF-coated GCE electrode
SolventsTHF for ISM cocktail
Additives65.7 wt% DOS, 32.9 wt% PVC, 1.0 wt% copper ionophore I, 0.86 wt% NaTFPB
AtmosphereAir drying at room temperature; aqueous CuCl2 conditioning.
Time24 h membrane drying; overnight CuCl2 conditioning
Substrate orientationCu3(HHTP)2/PVDF-coated GCE
Work-up30 uL ISM cocktail drop-cast and dried for 24 h in air at room temperature.
ActivationConditioned in 1 x 10^-4 M CuCl2 solution overnight.
Scalability contextElectrode-scale membrane drop-casting only.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Additivebis(2-ethylhexyl) sebacate (DOS)65.7 wt% of 100 mg membrane componentsp002 · 2.3 Fabrication of Cu3(HHTP)2-based SC-ISEs
AdditivePVC32.9 wt% of 100 mg membrane componentsp002 · 2.3 Fabrication of Cu3(HHTP)2-based SC-ISEs
Additivecopper ionophore I1.0 wt% of 100 mg membrane componentsp002 · 2.3 Fabrication of Cu3(HHTP)2-based SC-ISEs
AdditiveNaTFPB0.86 wt% of 100 mg membrane componentsp002 · 2.3 Fabrication of Cu3(HHTP)2-based SC-ISEs
SolventTHF1 mLp002 · 2.3 Fabrication of Cu3(HHTP)2-based SC-ISEs
ElectrolyteCuCl2 conditioning solution1 x 10^-4 Mp002 · 2.3 Fabrication of Cu3(HHTP)2-based SC-ISEs
Complete recipeSource: Main

Route 2: Drop Cast

p002 · 2.3 Fabrication of Cu3(HHTP)2-based SC-ISEs

Metal precursorsAs-synthesised Cu3(HHTP)2 powder
SolventsN-methyl pyrrolidone (NMP)
AdditivesPVDF binder, 1 mg per 4 mg Cu3(HHTP)2
AtmosphereAir drying after coating; conditioning in aqueous CuCl2.
Temperature60
Substrate orientation5 mm diameter polished GCE with Teflon body
Work-upCoated electrode dried at 60 deg C.
ActivationConditioned in 1 x 10^-4 M CuCl2 solution for 4 h or within 15 min.
Scalability contextElectrode-scale coating; no large-area or batch scalability study.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherCu3(HHTP)24 mg · 10 mg mL-1 dispersionp002 · 2.3 Fabrication of Cu3(HHTP)2-based SC-ISEs
AdditivePVDF1 mgp002 · 2.3 Fabrication of Cu3(HHTP)2-based SC-ISEs
SolventN-methyl pyrrolidone (NMP)400 uLp002 · 2.3 Fabrication of Cu3(HHTP)2-based SC-ISEs
ElectrolyteCuCl2 conditioning solution1 x 10^-4 Mp002 · 2.3 Fabrication of Cu3(HHTP)2-based SC-ISEs
Complete recipeSource: Main

Route 3: Hydrothermal

p002 · 2.2 Synthesis of Cu3(HHTP)2

Metal precursorsCu(COOCH3)2.H2O 20.8 mg (0.104 mmol)
Linker precursorsHHTP 25 mg (0.077 mmol)
Solvents5 mL degassed deionised water
AtmosphereDegassed water; vial loosely capped; no inert gas stated.
Temperature70
Time24
Work-upBlack solid precipitate centrifuged and filtered, then washed with deionised water (25 mL), ethanol (25 mL), and acetone (25 mL).
ActivationDried under vacuum at 70 deg C.
Scalability contextSmall-vial batch synthesis; no yield or scalability data reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(COOCH3)2.H2O20.8 mg (0.104 mmol)p002 · 2.2 Synthesis of Cu3(HHTP)2
Linker2,3,6,7,10,11-hexahydroxytriphenylene hydrate (HHTP)25 mg (0.077 mmol)p002 · 2.2 Synthesis of Cu3(HHTP)2
Solventdegassed deionised water5 mLp002 · 2.2 Synthesis of Cu3(HHTP)2
Solventdeionised water wash25 mLp002 · 2.2 Synthesis of Cu3(HHTP)2
Solventethanol wash25 mLp002 · 2.2 Synthesis of Cu3(HHTP)2
Solventacetone wash25 mLp002 · 2.2 Synthesis of Cu3(HHTP)2