Synthesis evidence

NiPd mediated by conductive metal organic frameworks with facilitated electron transfer for assaying of H2O2 released from living cells

Chen Z., Qian Y., Zhang L. et al. · Journal of Electroanalytical Chemistry · 2022 · 115985

7 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Drop Cast

2 · 2.4. Preparation of different modified electrodes

Metal precursorsNi3HHTP2
Solventsnot specified for drop-cast dispersion
Atmospheredried under nitrogen before drop-casting
Temperatureroom temperature drying
Substrate orientationglassy carbon electrode, 3.0 mm diameter
Work-upPrepared by the same GC cleaning/drop-casting method as NiPd@Ni3HHTP2/GC.
Scalability contextElectrode-level drop-casting; mass loading 0.14 mg cm-2.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
OtherNi3HHTP2mass loading 0.14 mg cm-22 · 2.4. Preparation of different modified electrodes
Partial recipeSource: Main

Route 2: Hydrothermal

2 · 2.3. Synthesis of NiPd@Ni3HHTP2 hybrid

Metal precursors456 mg nickel acetate tetrahydrate
Linker precursors200 mg HHTP
Solvents28 mL deionized water
Atmospherenot reported
Temperaturenot reported for reaction; dried at 49 C
Time24 h reaction; 24 h drying
Work-upSonicated 10 min; stirred in oil bath 24 h; suction filtered after cooling; washed with deionized water and acetone several times.
ActivationVacuum oven drying for 24 h at 49 C and 50 kPa.
Scalability context100 mL round-bottom flask batch synthesis.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHTP200 mg2 · 2.3. Synthesis of NiPd@Ni3HHTP2 hybrid
Metal Sourcenickel acetate tetrahydrate456 mg2 · 2.3. Synthesis of NiPd@Ni3HHTP2 hybrid
Solventdeionized water28 mL2 · 2.3. Synthesis of NiPd@Ni3HHTP2 hybrid
Partial recipeSource: Main

Route 3: Drop Cast

2 · 2.4. Preparation of different modified electrodes

Metal precursorsNiPd nanoparticles
Solventsnot specified for drop-cast dispersion
Atmospheredried under nitrogen before drop-casting
Temperatureroom temperature drying
Substrate orientationglassy carbon electrode, 3.0 mm diameter
Work-upPrepared by the same GC cleaning/drop-casting method as NiPd@Ni3HHTP2/GC.
Scalability contextElectrode-level drop-casting; mass loading 25 ug cm-2.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
OtherNiPd nanoparticlesmass loading 25 ug cm-22 · 2.4. Preparation of different modified electrodes
Complete recipeSource: Main

Route 4: Drop Cast

2 · 2.4. Preparation of different modified electrodes

Metal precursorsNiPd@Ni3HHTP2 hybrid
Solventsdeionized water; ethanol/water 1:1 cleaning solution
Atmospheredried under nitrogen before drop-casting
Temperatureroom temperature drying
Substrate orientationglassy carbon electrode, 3.0 mm diameter
Work-upGC polished with 1.0 and 0.3 um alumina slurry; rinsed; sonicated in water and ethanol/water 1:1 for 5 min each; dried under nitrogen; 5 uL hybrid drop-cast and dried.
Scalability contextElectrode-level drop-casting; mass loading 0.165 mg cm-2.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherNiPd@Ni3HHTP2 hybrid5 uL2 · 2.4. Preparation of different modified electrodes
Otherglassy carbon electrode3.0 mm diameter2 · 2.4. Preparation of different modified electrodes
Complete recipeSource: Main

Route 5: Other

2 · 2.3. Synthesis of NiPd@Ni3HHTP2 hybrid

Metal precursorsNiPd NPs solution; Ni3HHTP2 water solution
Linker precursorsHHTP contained in preformed Ni3HHTP2
Solventswater
Atmospherenot reported
Temperature4
Time2
Work-upMixed Ni3HHTP2 water solution (2 mg mL-1) and NiPd NPs solution at 10:1 volume ratio; sonicated for 2 h at 4 C.
Scalability contextSimple solution mixing/sonication route.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherNi3HHTP2 water solution10 volume equivalents · 2 mg mL-12 · 2.3. Synthesis of NiPd@Ni3HHTP2 hybrid
OtherNiPd NPs solution1 volume equivalent2 · 2.3. Synthesis of NiPd@Ni3HHTP2 hybrid
Partial recipeSource: Main

Route 6: Other

2 · 2.3. Synthesis of NiPd@Ni3HHTP2 hybrid

Metal precursors13.0 mg NiCl2; 5 mL H2PdCl4 solution containing 7.5 mg H2PdCl4
Solvents100 mL deionized water plus final 5 mL water dispersion
Additives51.6 mg trisodium citrate
AtmosphereN2 purged for 30 min to remove dissolved oxygen
Temperaturenot reported
Time0.333 h after NaBH4 addition and H2PdCl4 injection, plus N2 purge
Oxidant / reductant10 mL freshly prepared NaBH4 solution (2 mg mL-1)
Work-upWashed with water several times and centrifuged at 8000 rpm for 10 min each time.
Scalability context250 mL three-necked flask batch synthesis.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Additivetrisodium citrate51.6 mg2 · 2.3. Synthesis of NiPd@Ni3HHTP2 hybrid
Metal SourceNiCl213.0 mg2 · 2.3. Synthesis of NiPd@Ni3HHTP2 hybrid
Solventdeionized water100 mL2 · 2.3. Synthesis of NiPd@Ni3HHTP2 hybrid
ReductantNaBH4 solution10 mL · 2 mg mL-12 · 2.3. Synthesis of NiPd@Ni3HHTP2 hybrid
Metal SourceH2PdCl45 mL solution; 7.5 mg H2PdCl42 · 2.3. Synthesis of NiPd@Ni3HHTP2 hybrid
Partial recipeSource: Main

Route 7: Drop Cast

2 · 2.4. Preparation of different modified electrodes

Metal precursorsNiPd nanoparticles; commercial ZIF-8
Solventsnot specified for drop-cast dispersion
Atmospheredried under nitrogen before drop-casting
Temperatureroom temperature drying
Substrate orientationglassy carbon electrode, 3.0 mm diameter
Work-upPrepared by the same GC cleaning/drop-casting method as NiPd@Ni3HHTP2/GC.
Scalability contextElectrode-level drop-casting; mass loading 0.165 mg cm-2.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
OtherNiPd@ZIF-8mass loading 0.165 mg cm-2 · NiPd:ZIF-8 mass ratio 5:282 · 2.4. Preparation of different modified electrodes