Synthesis · High efficient solid-phase microextraction based on a covalent organic framework for determination of trifluralin and chlorpyrifos in water and food samples by GC-CD-IMS

Complete recipeSource: Both

Route 1: Other

p002 · 2.4. SPME fibre preparation · Fig. S2

Linker precursorsPTA/TAPTT COF powder coating material

Solventsacetone, ethanol, water for cleaning; toluene in 10% w/w silicone glue solution

Additiveshigh-temperature silicone glue binder

Atmospherenitrogen flow during final thermal treatment

Temperature250

Time2

Substrate orientationstainless steel wire, 1.5 cm length and 0.25 o.d.

Work-upWire washed with acetone, ethanol, and water in an ultrasonic bath; dried; dipped in diluted glue; dipped in COF powder.

ActivationTreated at 250 deg C in the GC injection port with nitrogen flow for 2 h.

Scalability contextManual fibre coating method; no batch coating or scale-up reported.

Show 7 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	stainless steel wire	1.5 cm length and 0.25 o.d.	p002 · 2.4. SPME fibre preparation · Fig. S2
Solvent	acetone	washing solvent	p002 · 2.4. SPME fibre preparation · Fig. S2
Solvent	ethanol	washing solvent	p002 · 2.4. SPME fibre preparation · Fig. S2
Solvent	water	washing solvent	p002 · 2.4. SPME fibre preparation · Fig. S2
Additive	high-temperature silicon glue solution	10% w/w in toluene	p002 · 2.4. SPME fibre preparation · Fig. S2
Solvent	toluene	solvent for glue solution	p002 · 2.4. SPME fibre preparation · Fig. S2
Other	PTA/TAPTT COF powder	tube filled with COF powder	p002 · 2.4. SPME fibre preparation · Fig. S2

Complete recipeSource: Both

p002 · 2.3. Synthesis of PTA/TAPTT COF · Fig. S1

Linker precursorsCyanuric chloride; 4,4'-ethylenedianiline; 3,4,9,10-perylenetetracarboxylic dianhydride; TAPTT intermediate

Solvents1,4-dioxane for TAPTT synthesis; NMP (0.5 mL), mesitylene (0.5 mL), and THF workup for COF synthesis

AdditivesN,N-diisopropylethylamine scavenger in TAPTT synthesis; isoquinoline (0.05 mL) for COF synthesis

Atmospheresealed tube under nitrogen after three freeze-pump-thaw degassing cycles

Temperature160

Time120

Work-upAfter cooling, solvent decanted; solid washed with dry THF and immersed in fresh THF for 12 h.

ActivationDried in a vacuum oven at 70 deg C for 24 h.

Scalability contextSmall sealed ampoule recipe; reported yield 90%. No scale-up study reported.

Show 10 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	cyanuric chloride	184 mg, 1 mmol	p002 · 2.3. Synthesis of PTA/TAPTT COF · Fig. S1
Linker	4,4'-ethylenedianiline	excess amount	p002 · 2.3. Synthesis of PTA/TAPTT COF · Fig. S1
Solvent	1,4-dioxane	25 mL for solution 1; 30 mL for solution 2	p002 · 2.3. Synthesis of PTA/TAPTT COF · Fig. S1
Base	N,N-diisopropylethylamine	a few drops	p002 · 2.3. Synthesis of PTA/TAPTT COF · Fig. S1
Linker	3,4,9,10-perylenetetracarboxylic dianhydride	58.85 mg, 0.15 mmol	p002 · 2.3. Synthesis of PTA/TAPTT COF · Fig. S1
Linker	TAPTT	71.2 mg, 0.1 mmol	p002 · 2.3. Synthesis of PTA/TAPTT COF · Fig. S1
Solvent	NMP	0.5 mL	p002 · 2.3. Synthesis of PTA/TAPTT COF · Fig. S1
Solvent	mesitylene	0.5 mL	p002 · 2.3. Synthesis of PTA/TAPTT COF · Fig. S1
Additive	isoquinoline	0.05 mL	p002 · 2.3. Synthesis of PTA/TAPTT COF · Fig. S1
Solvent	THF	dry THF wash; fresh THF immersion for 12 h	p002 · 2.3. Synthesis of PTA/TAPTT COF · Fig. S1