Synthesis · Piperazine-linked metal covalent organic framework-coated fibers for efficient electro-enhanced solid-phase microextraction of chlorophenols

2 structured synthesis routes

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

Partial recipeSource: Both

Route 1: Other

p.2 · 2.3.2. Preparation of CuPc-MCOF-coated fibers · Fig. S1

SolventsHydrofluoric acid solution for etching; ultrapure water, ethanol and acetone washes

AdditivesPolyimide resin binder

AtmosphereAir drying/oven ageing; atmosphere not specified

Temperature60 drying; 280 ageing

Time0.5 etching; 3 ageing

Substrate orientationEtched end of about 3-4 cm, 0.3 mm stainless steel fibre

Work-upFibres washed three times with ultrapure water, ethanol and acetone, dried at 60 degC; CuPc-MCOF powder ground and passed through 280-mesh sieve.

ActivationAged at 280 degC for 3 h to remove excess impurities and pollutants on the fibre surface.

Scalability contextManual physical coating/rolling procedure on short stainless steel fibre sections.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	stainless steel fiber	about 3-4 cm; 0.3 mm	p.2 · 2.3.2. Preparation of CuPc-MCOF-coated fibers · Fig. S1
Acid	hydrofluoric acid solution	30 min etching	p.2 · 2.3.2. Preparation of CuPc-MCOF-coated fibers · Fig. S1
Additive	polyimide resin	coated on etched fibre end	p.2 · 2.3.2. Preparation of CuPc-MCOF-coated fibers · Fig. S1
Other	CuPc-MCOF powder	ground and sieved through 280 mesh	p.2 · 2.3.2. Preparation of CuPc-MCOF-coated fibers · Fig. S1

Partial recipeSource: Both

Route 2: Solvothermal

p.2 · 2.3.1. Synthesis of CuPc-MCOF

Metal precursorsCuPcF16, prepared from tetrafluorophthalonitrile and anhydrous copper chloride at 200 degC for 3 h according to literature methods

Linker precursors3,3'-diaminobenzidine

Solvents1 mL acetonitrile and 1 mL 1,3,5-trimethylbenzene; THF for Soxhlet rinse

Additives150 uL triethylamine

AtmosphereSealed Pyrex tube after 3 freeze-thaw pump cycles

Temperature120

Time168

Work-upCollected black precipitate by centrifugation; washed successively with water, methanol, acetone and dichloromethane, 10 mL x 3 each.

ActivationRinsed with tetrahydrofuran in a Soxhlet extractor for one week; vacuum oven at 80 degC for 12 h.

Scalability contextSmall sealed-tube reaction using 21.98 mg CuPcF16 and 10.72 mg diamine; no scale-up data reported.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	CuPcF16	21.98 mg, 0.025 mmol	p.2 · 2.3.1. Synthesis of CuPc-MCOF
Linker	3,3'-diaminobenzidine	10.72 mg, 0.050 mmol	p.2 · 2.3.1. Synthesis of CuPc-MCOF
Solvent	acetonitrile	1 mL	p.2 · 2.3.1. Synthesis of CuPc-MCOF
Solvent	1,3,5-trimethylbenzene	1 mL	p.2 · 2.3.1. Synthesis of CuPc-MCOF
Base	triethylamine	150 uL	p.2 · 2.3.1. Synthesis of CuPc-MCOF
Solvent	tetrahydrofuran	Soxhlet rinse for one week	p.2 · 2.3.1. Synthesis of CuPc-MCOF