Synthesis evidence

Triggering Anodic Luminol Electrochemiluminescence through Electrostatic Interactions: An Innovative Approach Utilizing Conductive Metal-Organic Framework Co-HHTP

Liu M., Wei J., Lin S.-J. et al. · ACS Applied Electronic Materials · 2024 · 2375-2382

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: Drop Cast

3 · 2.4. Electrochemical and ECL Measurements

Metal precursors1 mg catalyst (Co-HHTP, Ni-HHTP, HHTP, or guest-loaded analogue depending on electrode)
Linker precursorsframework already synthesised
Solvents200 uL water + 50 uL anhydrous ethanol
Additives10 uL Nafion
Atmospherenot specified
Temperatureroom temperature
Timesonicated for 40 min
Substrate orientationglassy carbon electrode, diameter 5 mm
Oxidant / reductantnone reported
Work-up5 uL suspension dropped onto glassy carbon electrode; drying details not stated
Activationnone reported
Scalability contextAnalytical electrode preparation; not a scalable film synthesis route.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Othercatalyst1 mg3 · 2.4. Electrochemical and ECL Measurements
Solventwater200 uL3 · 2.4. Electrochemical and ECL Measurements
Solventanhydrous ethanol50 uL3 · 2.4. Electrochemical and ECL Measurements
AdditiveNafion10 uL3 · 2.4. Electrochemical and ECL Measurements
Complete recipeSource: Main

Route 2: Drop Cast

3 · 2.4. Electrochemical and ECL Measurements

Metal precursors1 mg catalyst (HHTP)
Linker precursorsframework already synthesised
Solvents200 uL water + 50 uL anhydrous ethanol
Additives10 uL Nafion
Atmospherenot specified
Temperatureroom temperature
Timesonicated for 40 min
Substrate orientationglassy carbon electrode, diameter 5 mm
Oxidant / reductantnone reported
Work-up5 uL suspension dropped onto glassy carbon electrode; drying details not stated
Activationnone reported
Scalability contextAnalytical electrode preparation; not a scalable film synthesis route.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherHHTP catalyst1 mg3 · 2.4. Electrochemical and ECL Measurements
Solventwater200 uL3 · 2.4. Electrochemical and ECL Measurements
Solventanhydrous ethanol50 uL3 · 2.4. Electrochemical and ECL Measurements
AdditiveNafion10 uL3 · 2.4. Electrochemical and ECL Measurements
Complete recipeSource: Main

Route 3: Drop Cast

3 · 2.4. Electrochemical and ECL Measurements

Metal precursors1 mg catalyst (luminol@Co-HHTP)
Linker precursorsframework already synthesised
Solvents200 uL water + 50 uL anhydrous ethanol
Additives10 uL Nafion
Atmospherenot specified
Temperatureroom temperature
Timesonicated for 40 min
Substrate orientationglassy carbon electrode, diameter 5 mm
Oxidant / reductantnone reported
Work-up5 uL suspension dropped onto glassy carbon electrode; drying details not stated
Activationnone reported
Scalability contextAnalytical electrode preparation; not a scalable film synthesis route.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Otherluminol@Co-HHTP catalyst1 mg3 · 2.4. Electrochemical and ECL Measurements
Solventwater200 uL3 · 2.4. Electrochemical and ECL Measurements
Solventanhydrous ethanol50 uL3 · 2.4. Electrochemical and ECL Measurements
AdditiveNafion10 uL3 · 2.4. Electrochemical and ECL Measurements
Complete recipeSource: Main

Route 4: Other

3 · 2.2. Synthesis of Luminol@M-HHTP

Metal precursorsprepared Co-HHTP sample, 30 mg
Linker precursorsframework already present in Co-HHTP; luminol guest 0.010 g
Solvents9 mL deionized water + 9 mL methanol
Additivesnone reported
Atmosphereambient/not specified
Temperatureroom temperature
Time12
Oxidant / reductantnone reported
Work-upcollected by centrifugation, washed three times with methanol, dried at room temperature
Activationno separate activation reported
Scalability context30 mg MOF batch for guest loading; no yield or loading amount quantified.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Otherluminol0.010 g3 · 2.2. Synthesis of Luminol@M-HHTP
Otherprepared Co-HHTP sample30 mg3 · 2.2. Synthesis of Luminol@M-HHTP
Solventdeionized water9 mL3 · 2.2. Synthesis of Luminol@M-HHTP
Solventmethanol9 mL3 · 2.2. Synthesis of Luminol@M-HHTP
Complete recipeSource: Main

Route 5: Other

3 · 2.2. Synthesis of Luminol@M-HHTP

Metal precursorsprepared Ni-HHTP sample, 30 mg
Linker precursorsframework already present in Ni-HHTP; luminol guest 0.010 g
Solvents9 mL deionized water + 9 mL methanol
Additivesnone reported
Atmosphereambient/not specified
Temperatureroom temperature
Time12
Oxidant / reductantnone reported
Work-upcollected by centrifugation, washed three times with methanol, dried at room temperature
Activationno separate activation reported
Scalability context30 mg MOF batch for guest loading; no yield or loading amount quantified.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Otherluminol0.010 g3 · 2.2. Synthesis of Luminol@M-HHTP
Otherprepared Ni-HHTP sample30 mg3 · 2.2. Synthesis of Luminol@M-HHTP
Solventdeionized water9 mL3 · 2.2. Synthesis of Luminol@M-HHTP
Solventmethanol9 mL3 · 2.2. Synthesis of Luminol@M-HHTP
Complete recipeSource: Main

Route 6: Drop Cast

3 · 2.4. Electrochemical and ECL Measurements

Metal precursors1 mg catalyst (luminol@Ni-HHTP)
Linker precursorsframework already synthesised
Solvents200 uL water + 50 uL anhydrous ethanol
Additives10 uL Nafion
Atmospherenot specified
Temperatureroom temperature
Timesonicated for 40 min
Substrate orientationglassy carbon electrode, diameter 5 mm
Oxidant / reductantnone reported
Work-up5 uL suspension dropped onto glassy carbon electrode; drying details not stated
Activationnone reported
Scalability contextAnalytical electrode preparation; not a scalable film synthesis route.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Otherluminol@Ni-HHTP catalyst1 mg3 · 2.4. Electrochemical and ECL Measurements
Solventwater200 uL3 · 2.4. Electrochemical and ECL Measurements
Solventanhydrous ethanol50 uL3 · 2.4. Electrochemical and ECL Measurements
AdditiveNafion10 uL3 · 2.4. Electrochemical and ECL Measurements
Complete recipeSource: Main

Route 7: Hydrothermal

3 · 2.1. Synthesis of M-HHTP

Metal precursors0.1 g M(OAc)2; M = Co for Co-HHTP, Ni for Ni-HHTP
Linker precursors0.07 g 2,3,6,7,10,11-hexahydroxytriphenylene (HHTP)
Solvents40 mL deionized water
Additivesnone reported
Atmospherenot specified; sealed 50 mL reaction vessel
Temperature85
Time12
Oxidant / reductantnone reported
Work-upcooled to room temperature, centrifuged, washed several times with deionized water and acetone, dried at room temperature
Activationno separate activation reported
Scalability context50 mL reaction vessel; no yield or scale-up discussion reported.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceM(OAc)2 (M = Co or Ni)0.1 g3 · 2.1. Synthesis of M-HHTP
Linker2,3,6,7,10,11-hexahydroxytriphenylene (HHTP)0.07 g3 · 2.1. Synthesis of M-HHTP
Solventdeionized water40 mL3 · 2.1. Synthesis of M-HHTP
Complete recipeSource: Main

Route 8: Hydrothermal

3 · 2.1. Synthesis of M-HHTP

Metal precursors0.1 g Ni(OAc)2
Linker precursors0.07 g 2,3,6,7,10,11-hexahydroxytriphenylene (HHTP)
Solvents40 mL deionized water
Additivesnone reported
Atmospherenot specified; sealed 50 mL reaction vessel
Temperature85
Time12
Oxidant / reductantnone reported
Work-upcooled to room temperature, centrifuged, washed several times with deionized water and acetone, dried at room temperature
Activationno separate activation reported
Scalability contextNo yield or scale-up discussion reported.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(OAc)20.1 g3 · 2.1. Synthesis of M-HHTP
Linker2,3,6,7,10,11-hexahydroxytriphenylene (HHTP)0.07 g3 · 2.1. Synthesis of M-HHTP
Solventdeionized water40 mL3 · 2.1. Synthesis of M-HHTP
Complete recipeSource: Main

Route 9: Drop Cast

3 · 2.4. Electrochemical and ECL Measurements

Metal precursors1 mg catalyst (Ni-HHTP)
Linker precursorsframework already synthesised
Solvents200 uL water + 50 uL anhydrous ethanol
Additives10 uL Nafion
Atmospherenot specified
Temperatureroom temperature
Timesonicated for 40 min
Substrate orientationglassy carbon electrode, diameter 5 mm
Oxidant / reductantnone reported
Work-up5 uL suspension dropped onto glassy carbon electrode; drying details not stated
Activationnone reported
Scalability contextAnalytical electrode preparation; not a scalable film synthesis route.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherNi-HHTP catalyst1 mg3 · 2.4. Electrochemical and ECL Measurements
Solventwater200 uL3 · 2.4. Electrochemical and ECL Measurements
Solventanhydrous ethanol50 uL3 · 2.4. Electrochemical and ECL Measurements
AdditiveNafion10 uL3 · 2.4. Electrochemical and ECL Measurements