Electrochemistry Application — Piperazine-linked metal covalent organic framework-coated fibers for efficient electro-enhanced solid-phase microextraction of chlorophenols

5 measurement groups · 30 results

Reported values remain attached to the sample, method, conditions, extraction quality and source location that produced them.

Electro-enhanced solid-phase microextraction (EE-SPME) optimisation

CuPc-MCOF-coated stainless steel fibre · Electrode

Three-electrode system with coated fibre working electrode, platinum counter electrode and saturated calomel reference; 10.0 mL extraction solution in 15.0 mL cell.

Temperature: room temperature
Geometry: Coated fibre working electrode
Context: composite coated fibre containing CuPc-MCOF active coating
Measurement source: p.3-p.6 · 2.4. EE-SPME procedure; 3.2. Optimization · Fig. 3

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Optimised desorption temperatureMarked as a best value within this paper	290 degC	—	—	Text Exact Reported	p.6 · 3.2. Optimization · Fig. 3e
Optimised desorption timeMarked as a best value within this paper	4 min	—	—	Text Exact Reported	p.6 · 3.2. Optimization · Fig. 3f
Optimised extraction timeMarked as a best value within this paper	20 min	—	—	Text Exact Reported	p.4 · 3.2. Optimization · Fig. 3b
Optimised NaCl concentrationMarked as a best value within this paper	2.0 mg mL-1	—	—	Text Exact Reported	p.6 · 3.2. Optimization · Fig. 3d
Optimised solution pHMarked as a best value within this paper	pH = 6	—	—	Text Exact Reported	p.4-p.6 · 3.2. Optimization · Fig. 3c
Optimised extraction voltageMarked as a best value within this paper	0.5 V	—	—	Text Exact Reported	p.4 · 3.2. Optimization · Fig. 3a

Adsorption comparison and interferent selectivity test

CuPc-MCOF-coated stainless steel fibre · Electrode

CuPc-MCOF fibre compared with DVB/PDMS-65 um, PA-85 um and CAR/PDMS-75 um fibres using 500 ng L-1 chlorophenol mixed standards; PAEs, AAs and PCBs added as interferents.

Geometry: Coated fibre extraction phase
Context: composite coated fibre containing CuPc-MCOF active coating
Measurement source: p.6-p.7 · 3.4. Adsorption properties and selectivity · Fig. 5; Table S1

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Enrichment factor without interferents, high endMarked as a best value within this paper	339-988	—	range upper bound	Text Range	p.6 · 3.4. Adsorption properties and selectivity · Fig. 5b
Enrichment factor without interferents, low end	339-988	—	range lower bound	Text Range	p.6 · 3.4. Adsorption properties and selectivity · Fig. 5b
Enrichment factor with interferents, high end	280-794	—	range upper bound	Text Range	p.6 · 3.4. Adsorption properties and selectivity · Fig. 5b
Enrichment factor with interferents, low end	280-794	—	range lower bound	Text Range	p.6 · 3.4. Adsorption properties and selectivity · Fig. 5b

Fibre stability, continuous electrification, solvent/pH soaking and recycling tests

CuPc-MCOF-coated stainless steel fibre · Electrode

Continuous 0.5 V electrification; soaking in DCM, ACN, MeOH, pH 4 and pH 10 for 24 h; repeated extraction cycles on a single fibre.

Geometry: Coated fibre working electrode
Context: composite coated fibre containing CuPc-MCOF active coating
Measurement source: p.6-p.7 · 3.3. Stability of CuPc-MCOF coated fibers · Fig. 4b-d; Fig. S8-S9

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Peak-area response decrease after 150 cycles, high end	6.8-11.8%	—	range upper bound	Text Range	p.6 · 3.3. Stability · Fig. 4d
Peak-area response decrease after 150 cycles, low end	6.8-11.8%	—	range lower bound	Text Range	p.6 · 3.3. Stability · Fig. 4d
Continuous electrification stability	did not change until at least 120 min at 0.5 V	—	at least	Text Approximate	p.6 · 3.3. Stability · Fig. 4b

Control-variable optimisation conditions for commercial comparison fibres

CuPc-MCOF-coated stainless steel fibre · Electrode

Table S1 reports optimum adsorption/desorption conditions for DVB/PDMS-65 um, PA-85 um and CAR/PDMS-75 um comparison fibres.

Geometry: Commercial SPME fibres used as comparison controls
Context: application comparison context for CuPc-MCOF coated fibre
Measurement source: p.7-p.8 · Supplementary materials · Table S1

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Commercial fibre optimal desorption temperature for CAR/PDMS-75 um	285 degC	—	—	SI Table Exact Reported	p.7-p.8 · Supplementary materials · Table S1
Commercial fibre optimal desorption time for CAR/PDMS-75 um	6 min	—	—	SI Table Exact Reported	p.7-p.8 · Supplementary materials · Table S1
Commercial fibre optimal extraction time for CAR/PDMS-75 um	40 min	—	—	SI Table Exact Reported	p.7-p.8 · Supplementary materials · Table S1
Commercial fibre optimal NaCl concentration for CAR/PDMS-75 um	0.002 g mL-1	—	—	SI Table Exact Reported	p.7-p.8 · Supplementary materials · Table S1
Commercial fibre optimal pH for CAR/PDMS-75 um	pH 6	—	—	SI Table Exact Reported	p.7-p.8 · Supplementary materials · Table S1
Commercial fibre optimal desorption temperature for DVB/PDMS-65 um	290 degC	—	—	SI Table Exact Reported	p.7-p.8 · Supplementary materials · Table S1
Commercial fibre optimal desorption time for DVB/PDMS-65 um	5 min	—	—	SI Table Exact Reported	p.7-p.8 · Supplementary materials · Table S1
Commercial fibre optimal extraction time for DVB/PDMS-65 um	35 min	—	—	SI Table Exact Reported	p.7-p.8 · Supplementary materials · Table S1
Commercial fibre optimal NaCl concentration for DVB/PDMS-65 um	0.002 g mL-1	—	—	SI Table Exact Reported	p.7-p.8 · Supplementary materials · Table S1
Commercial fibre optimal pH for DVB/PDMS-65 um	pH 6	—	—	SI Table Exact Reported	p.7-p.8 · Supplementary materials · Table S1
Commercial fibre optimal desorption temperature for PA-85 um	285 degC	—	—	SI Table Exact Reported	p.7-p.8 · Supplementary materials · Table S1
Commercial fibre optimal desorption time for PA-85 um	5 min	—	—	SI Table Exact Reported	p.7-p.8 · Supplementary materials · Table S1
Commercial fibre optimal extraction time for PA-85 um	30 min	—	—	SI Table Exact Reported	p.7-p.8 · Supplementary materials · Table S1
Commercial fibre optimal NaCl concentration for PA-85 um	0.002 g mL-1	—	—	SI Table Exact Reported	p.7-p.8 · Supplementary materials · Table S1
Commercial fibre optimal pH for PA-85 um	pH 6	—	—	SI Table Exact Reported	p.7-p.8 · Supplementary materials · Table S1

Zeta potential before and after chlorophenol adsorption

Dynamic light scattering and zeta potential

CuPc-MCOF after chlorophenol adsorption · Powder

Zetasizer Nano range analyser; detailed sample preparation associated with Fig. S11 is not available in the caption-only SI text.

Geometry: Powder/dispersion before and after CP adsorption
Context: guest-loaded adsorption state compared with pristine framework
Measurement source: p.8 · 3.7. Extraction mechanism · Fig. S11

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Zeta potential after CP adsorption	-10.9 mV	—	—	Text Exact Reported	p.8 · 3.7. Extraction mechanism · Fig. S11
Zeta potential before CP adsorption	-20.5 mV	—	—	Text Exact Reported	p.8 · 3.7. Extraction mechanism · Fig. S11