Synthesis evidence

3D Co-doped Ni-based conductive MOFs modified electrochemical sensor for highly sensitive detection of L-tryptophan

Huang W., Chen Y., Wu L. et al. · Talanta · 2022 · 123596

5 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

3 · 2.3.2

Metal precursorsCo-Ni-MOFs-1% powder
SolventsAnhydrous ethanol
Additives0.5% chitosan binder; 0.05 um alumina slurry used for electrode polishing
Atmosphereambient drying, not otherwise specified
Substrate orientationglassy carbon electrode surface
Work-up2 mg Co-Ni-MOFs-1% dispersed in 1 mL ethanol by ultrasonication for 30 min; polish GCE; wash in ethanol and water for 1 min each; dry naturally; pipette 5 uL suspension; dry at room temperature; cover with 2 uL 0.5% chitosan; store at 4 C.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherCo-Ni-MOFs-1% material2 mg · 2 mg mL^-1 suspension3 · 2.3.2
Solventanhydrous ethanol1 mL3 · 2.3.2
Additivechitosan2 uL · 0.5%3 · 2.3.2
Otheralumina slurry0.05 um3 · 2.3.2
Complete recipeSource: Main

Route 2: Solvothermal

3 · 2.3.1

Metal precursorsNi(NO3)2.6H2O, 2.3263 g; Co(NO3)2.6H2O added at Co/Ni molar ratios 0.1%, 1%, 2% and 5%
Linker precursorsTerephthalic acid (H2BDC), 0.6645 g
SolventsDMF, 30 mL for mixed metal solution plus 30 mL for linker solution
Additives500 uL hydrochloric acid
Atmospherenot specified
Temperature180
Time24
Work-upCool to room temperature; transfer to beaker; centrifuge at 8000 r min^-1; wash with DMF and anhydrous ethanol 5 times.
ActivationDried in vacuum drying oven for 12 h at 60 C; separate BET activation under vacuum at 150 C for 4 h before sorption measurement.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(NO3)2.6H2O solid2.3263 g3 · 2.3.1
Metal SourceCo(NO3)2.6H2O soliddifferent amount · Co/Ni molar ratio 0.1%, 1%, 2%, 5%3 · 2.3.1
LinkerTerephthalic acid (H2BDC)0.6645 g3 · 2.3.1
SolventN,N-dimethylformamide (DMF)30 mL + 30 mL3 · 2.3.1
Acidhydrochloric acid500 uL3 · 2.3.1
Partial recipeSource: Both

Route 3: Drop Cast

2 · Supplementary figure captions · Fig. S3

Metal precursorsCo-Ni-MOFs-0.1%, Co-Ni-MOFs-1%, Co-Ni-MOFs-2% and Co-Ni-MOFs-5% powders
SolventsAnhydrous ethanol, inferred same as Co-Ni-MOFs-1%/GCE route
Additives0.5% chitosan binder, inferred same as Co-Ni-MOFs-1%/GCE route
Atmosphereambient drying, not otherwise specified
Substrate orientationglassy carbon electrode surface
Work-upElectrode labels in Fig. S3 indicate each Co/Ni-ratio powder was prepared as a GCE-modified electrode; exact fabrication not repeated beyond the Co-Ni-MOFs-1%/GCE procedure.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherCo-Ni-MOFs ratio-series material0.1%, 1%, 2%, 5% Co/Ni2 · Supplementary figure captions · Fig. S3
Solventanhydrous ethanolinferred 2 mg mL^-1 suspension from 1% route2 · Supplementary figure captions · Fig. S3
Additivechitosan0.5%, inferred from 1% route2 · Supplementary figure captions · Fig. S3
Complete recipeSource: Main

Route 4: Drop Cast

3 · 2.3.2

Metal precursorsNi-MOFs powder
SolventsAnhydrous ethanol
Additives0.5% chitosan binder
Atmosphereambient drying, not otherwise specified
Substrate orientationglassy carbon electrode surface
Work-upFabricated in the same way as Co-Ni-MOFs-1%/GCE.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherNi-MOFs material2 mg mL^-1 inferred same-way suspension3 · 2.3.2
Additivechitosan2 uL inferred same-way addition · 0.5%3 · 2.3.2
Complete recipeSource: Main

Route 5: Solvothermal

3 · 2.3.1

Metal precursorsNi(NO3)2.6H2O, 2.3263 g
Linker precursorsTerephthalic acid (H2BDC), 0.6645 g
SolventsDMF, 30 mL for Ni solution plus 30 mL for linker solution
Additives500 uL hydrochloric acid
Atmospherenot specified
Temperature180
Time24
Work-upCool to room temperature; transfer to beaker; centrifuge at 8000 r min^-1; wash with DMF and anhydrous ethanol 5 times.
ActivationDried in vacuum drying oven for 12 h at 60 C; separate BET activation under vacuum at 150 C for 4 h before sorption measurement.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(NO3)2.6H2O solid2.3263 g3 · 2.3.1
LinkerTerephthalic acid (H2BDC)0.6645 g3 · 2.3.1
SolventN,N-dimethylformamide (DMF)30 mL + 30 mL3 · 2.3.1
Acidhydrochloric acid500 uL3 · 2.3.1