Synthesis · Conductive Metal-Organic Frameworks as Ion-to-Electron Transducers in Potentiometric Sensors

9 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Hydrothermal

3 · Synthesis and Characterization of Conductive MOFs

Metal precursorsCoCl2.6H2O, 74 mg

Linker precursorsHHTP, 50 mg

Solventsdeionized water, 20 mL

Atmosphereair

Temperature70

Time24

Work-upCool 1 h at room temperature; filter through ceramic funnel/filter paper; wash with ultrapure water (1000 mL) and acetone (300 mL).

ActivationDried overnight under vacuum (20 mTorr) at 85 C.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	HHTP	50 mg	3 · Synthesis and Characterization of Conductive MOFs
Metal Source	CoCl2.6H2O	74 mg	3 · Synthesis and Characterization of Conductive MOFs
Solvent	deionized water	20 mL	3 · Synthesis and Characterization of Conductive MOFs

Complete recipeSource: Main

Route 2: Hydrothermal

3 · Synthesis and Characterization of Conductive MOFs

Metal precursorscopper(II) trifluoroacetylacetonate, 154 mg

Linker precursorsHHTP, 100 mg

Solventsdeionized water, 20 mL

Atmosphereair

Temperature70

Time24

Work-upCool 1 h at room temperature; filter through ceramic funnel/filter paper; wash with ultrapure water (1000 mL) and acetone (300 mL).

ActivationDried overnight under vacuum (20 mTorr) at 85 C.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	HHTP	100 mg	3 · Synthesis and Characterization of Conductive MOFs
Metal Source	copper(II) trifluoroacetylacetonate	154 mg	3 · Synthesis and Characterization of Conductive MOFs
Solvent	deionized water	20 mL	3 · Synthesis and Characterization of Conductive MOFs

Complete recipeSource: Main

Route 3: Drop Cast

3 · Preparation of Coated Wire Electrodes

SolventsISM suspension

AdditivesK+-ISM-II membrane components

Atmosphereroom-temperature drying

Time48

Substrate orientationISM directly on GCE

Work-upDrop-cast 10 uL ISM directly onto GCE; dry 24 h; immerse in 5 mL 1.0 x 10-3 M KCl for 24 h.

Activation24 h KCl conditioning

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	ISM suspension	10 uL	3 · Preparation of Coated Wire Electrodes
Electrolyte	KCl solution	5 mL · 1.0 x 10-3 M	3 · Preparation of Coated Wire Electrodes

Complete recipeSource: Main

Route 4: Drop Cast

3 · Preparation of MOF-Coated Electrodes

Metal precursorsM3HHTP2 MOF dispersion

Solventsacetonitrile dispersion

Atmospherenitrogen drying

Time3

Substrate orientationdrop-cast directly onto glassy carbon electrode

Work-upDrop-cast 5.0 uL aliquots of conductive MOF directly onto a solid contact; dry under nitrogen for 3 h.

Show 1 structured reagent record

Role	Reagent	Amount / concentration	Source
Other	conductive MOF dispersion	5.0 uL · 1 mg/mL dispersion described separately	3 · Preparation of MOF-Coated Electrodes

Complete recipeSource: Main

Route 5: Drop Cast

3 · Preparation of ISEs

Metal precursorsselected MOF dispersion

SolventsMOF dispersion and ISM suspension

Additivesion-selective membrane components

Atmosphereair storage for long-term stability; room-temperature drying

Time24

Substrate orientationMOF on glassy carbon, membrane on MOF

Work-upDrop-cast MOF on GCE and dry 3 h; drop-cast 10 uL ISM onto MOF; dry overnight; condition 24 h in 1.0 x 10-3 M KCl.

ActivationConditioning in 1.0 x 10-3 M KCl for 24 h before potentiometric and impedance experiments.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	selected MOF dispersion	not specified in this section	3 · Preparation of ISEs
Other	ISM suspension	10 uL	3 · Preparation of ISEs
Electrolyte	potassium chloride conditioning solution	1.0 x 10-3 M	3 · Preparation of ISEs

Complete recipeSource: Main

Route 6: Other

3 · Preparation of K+ and NO3- Sensing Membranes

Solventstetrahydrofuran, 1.5 mL

AdditivesPVC, DOS, NaTFPB, valinomycin or potassium ionophore II, TDMACl

Time0.5

Work-upDissolve ionophore/membrane components in THF and vortex 30 min.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Additive	valinomycin (K+-ISM-I) or potassium ionophore II (K+-ISM-II)	10 mmol kg-1	3 · Preparation of K+ and NO3- Sensing Membranes
Additive	NaTFPB	5 mmol kg-1	3 · Preparation of K+ and NO3- Sensing Membranes
Additive	PVC	33.3 wt % for K+ membranes; 33.2 wt % for NO3- membrane	3 · Preparation of K+ and NO3- Sensing Membranes
Additive	DOS	66.6 wt % for K+ membranes; 66.4 wt % for NO3- membrane	3 · Preparation of K+ and NO3- Sensing Membranes
Additive	TDMACl	5.0 mmol kg-1 in NO3--ISM	3 · Preparation of K+ and NO3- Sensing Membranes
Solvent	tetrahydrofuran	1.5 mL	3 · Preparation of K+ and NO3- Sensing Membranes

Complete recipeSource: Main

Route 7: Other

3 · Preparation of MOF Dispersion

Metal precursorsselected M3HHTP2 MOF powder

Solventsacetonitrile, 1.0 mL

Temperature25

Time4

Work-upSonicate selected MOF in acetonitrile to give a homogeneous dispersion.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	selected MOF	1.0 mg	3 · Preparation of MOF Dispersion
Solvent	acetonitrile	1.0 mL	3 · Preparation of MOF Dispersion

Complete recipeSource: Main

Route 8: Hydrothermal

2 · Synthesis and Characterization of Conductive MOFs

Metal precursorsNi(OAc)2.4H2O, 767 mg

Linker precursorsHHTP, 500 mg

Solventsdeionized water, 70 mL

Atmosphereair

Temperature85

Time24

Work-upCool 1 h at room temperature; filter through ceramic funnel/filter paper; wash with ultrapure water (1000 mL) and acetone (300 mL).

ActivationDried overnight under vacuum (20 mTorr) at 85 C.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	HHTP	500 mg	2 · Synthesis and Characterization of Conductive MOFs
Metal Source	Ni(OAc)2.4H2O	767 mg	2 · Synthesis and Characterization of Conductive MOFs
Solvent	deionized water	70 mL	2 · Synthesis and Characterization of Conductive MOFs

Complete recipeSource: SI

Route 9: Drop Cast

10 · Interferometry · Figure S7

Metal precursorsNi3HHTP2 MOF dispersion

Solventsacetonitrile dispersion

Substrate orientationdrop-cast onto glassy carbon electrode

Work-upDrop-cast 2, 5, or 10 uL of 1 mg/mL Ni3HHTP2-MOF suspension on GCE to tune thickness.

Show 1 structured reagent record

Role	Reagent	Amount / concentration	Source
Other	Ni3HHTP2-MOF suspension	2, 5, or 10 uL · 1 mg/mL	10 · Interferometry · Figure S7