Synthesis · Enhanced VOC adsorption capacity on MOF thin layer with reduced particle size by cryogrinding and microwave method

9 structured synthesis routes

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

Vague recipeSource: Main

Route 1: Other

4 · 2.2.5

Atmosphereroom temperature; no liquid N2

Temperatureroom temperature

Work-upConventional grinding at room temperature without liquid N2.

ActivationNo separate post-grinding activation specified for powders beyond measurement-specific activation.

Partial recipeSource: Main

Route 2: Other

4 · 2.2.5 · Fig. 1

Additivesliquid N2

Atmosphereliquid nitrogen-cooled mortar vessel at 77 K

Temperature-196

Timeless than 0.0167 h grinding after 5 min pre-cooling

Work-upMortar vessel conditioned to frozen temperature for 5 min; frozen MOF particles physically ground with a pestle for less than 1 min.

ActivationNo separate post-grinding activation specified for powders beyond measurement-specific activation.

Scalability contextManual mortar/pestle grinding under liquid nitrogen.

Show 1 structured reagent record

Role	Reagent	Amount / concentration	Source
Additive	liquid N2	surrounded mortar vessel	4 · 2.2.5 · Fig. 1

Vague recipeSource: Main

Route 3: Other

3 · 2.1 Materials

Work-upCommercial Basolite C300 purchased from Sigma Aldrich.

ActivationActivated at 150 degC for 12 h before adsorption-isotherm measurements.

Scalability contextCommercial source.

Show 1 structured reagent record

Role	Reagent	Amount / concentration	Source
Other	Basolite C300 (HKUST-1)	not reported	3 · 2.1 Materials

Partial recipeSource: Main

Route 4: Solvothermal

4 · 2.2.4

Metal precursorschromium nitrate nonahydrate (1.2 g, 3 mmol)

Linker precursorsterephthalic acid (500 mg, 3 mmol)

SolventsH2O (15 mL), DMF wash, hot ethanol wash

AdditivesHF (5 M, 0.6 mL, 3 mmol); aqueous NH4F (30 mmol/L, 150 mL)

AtmosphereTeflon-lined stainless steel autoclave; atmosphere not otherwise specified

Temperature220

Time8

Work-upMother liquor removed by centrifugation at 5000 rpm; washed with DMF and hot ethanol; dispersed in 150 mL NH4F at 333 K for 10 h; washed with hot water at 333 K.

ActivationDried at 373 K for 6 h, followed by vacuum oven at 423 K for 12 h.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	chromium nitrate nonahydrate	1.2 g, 3 mmol	4 · 2.2.4
Linker	terephthalic acid	500 mg, 3 mmol	4 · 2.2.4
Acid	HF	0.6 mL, 3 mmol · 5 M	4 · 2.2.4
Solvent	H2O	15 mL	4 · 2.2.4
Additive	NH4F aqueous solution	150 mL · 30 mmol/L	4 · 2.2.4

Partial recipeSource: Main

Route 5: Drop Cast

4 · 2.2.6 · Fig. S1 and Table S1 cited

Solventsethanol (4 mL)

Atmospherenitrogen flow for substrate drying; otherwise not specified

Temperature150

Time5 h sonication; 12 h heating

Substrate orientationgold-coated quartz crystal of 5 MHz in a PTFE holder

Oxidant / reductantpiranha solution (98% H2SO4:30% H2O2, 3:1 v/v) used for cleaning

Work-upGold-coated quartz crystal cleaned with piranha solution and ultrapure water, dried under nitrogen; 20 mg MOF suspended in 4 mL ethanol and sonicated 5 h; suspension dropped onto QCM substrate.

ActivationQCM substrate coated with MOF heated at 150 degC in a furnace for 12 h before QCM measurements.

Scalability contextThin layer made by solution casting/drop casting.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	MOF particles	20 mg	4 · 2.2.6 · Fig. S1 and Table S1 cited
Solvent	ethanol	4 mL	4 · 2.2.6 · Fig. S1 and Table S1 cited
Oxidant	piranha solution (98% H2SO4:30% H2O2, 3:1 v/v)	not reported	4 · 2.2.6 · Fig. S1 and Table S1 cited

Partial recipeSource: Main

Route 6: Solvothermal

4 · 2.2.3

Metal precursorsZirconium chloride (0.169 g)

Linker precursorsterephthalic acid (0.121 g)

SolventsDMF (50 mL); anhydrous ethanol wash

AtmosphereTeflon-lined stainless steel autoclave; atmosphere not otherwise specified

Temperature120

Time24

Work-upFiltered and washed with DMF several times to remove unreacted terephthalic acid; washed with anhydrous ethanol twice.

ActivationDried at 80 degC for 24 h.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Zirconium chloride	0.169 g	4 · 2.2.3
Linker	terephthalic acid	0.121 g	4 · 2.2.3
Solvent	DMF	50 mL	4 · 2.2.3

Partial recipeSource: Main

Route 7: Other

4 · 2.2.2

Metal precursorsCo(OAc)2.4H2O (5 mmol)

Linker precursorsC6H8O7.H2O (5 mmol)

Solvents30 mL H2O:C2H5OH = 1:1

AdditivesKOH (15 mmol)

AtmosphereTeflon-capped glass vial; atmosphere not otherwise specified

Temperature90

Time4

Work-upSame washing and drying procedure as solvothermal UTSA-16.

ActivationDried at 90 degC under vacuum for 6 h by reference to solvothermal workup.

Scalability context300 W microwave oven (Discover SP, CEM, USA).

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(OAc)2.4H2O	5 mmol	4 · 2.2.2
Linker	C6H8O7.H2O	5 mmol	4 · 2.2.2
Base	KOH	15 mmol	4 · 2.2.2
Solvent	H2O:C2H5OH	30 mL · 1:1	4 · 2.2.2

Partial recipeSource: Main

Route 8: Solvothermal

3 · 2.2.1

Metal precursorsCo(OAc)2.4H2O (1 mmol)

Linker precursorsC6H8O7.H2O (1 mmol)

SolventsH2O (2.5 mL) and C2H5OH (2.5 mL)

AdditivesKOH (3 mmol)

Atmospheresealed Teflon-lined stainless steel reactor; atmosphere not otherwise specified

Temperature120

Time48

Work-upWashed with ethyl ether twice and methanol three times with centrifugation at 5000 rpm for 5 min; immersed in methanol replaced three times per day for three days.

ActivationDried at 90 degC under vacuum for 6 h.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(OAc)2.4H2O	1 mmol	3 · 2.2.1
Linker	C6H8O7.H2O	1 mmol	3 · 2.2.1
Base	KOH	3 mmol	3 · 2.2.1
Solvent	H2O	2.5 mL	3 · 2.2.1
Solvent	C2H5OH	2.5 mL	3 · 2.2.1

Vague recipeSource: Main

Route 9: Other

3 · 2.1 Materials

Work-upCommercial Basolite Z1200 purchased from Sigma Aldrich.

ActivationActivated at 140 degC for 12 h before adsorption-isotherm measurements.

Scalability contextCommercial source.

Show 1 structured reagent record

Role	Reagent	Amount / concentration	Source
Other	Basolite Z1200 (ZIF-8)	not reported	3 · 2.1 Materials