Ionic Liquid—Solidified Floating Organic Drop Microextraction for the Preconcentration of Lead in Environmental Water Samples Prior to Its Determination with Electrothermal Atomic Absorption Spectrometry
Abstract
:1. Introduction
2. Results
2.1. Optimization of IL-SFODME Method
2.1.1. Selection of Extraction Solvent
2.1.2. Optimization of pH
2.1.3. Optimization of Buffer Amount
2.1.4. Optimization of Ionic Liquid Amount
2.1.5. Optimization of Extraction Time
2.1.6. Optimization of Extraction Temperature
2.1.7. Optimization of Extraction Speed
2.1.8. Optimization of Added Dodecanol Amount
2.1.9. Optimization of Final Volume
2.2. Interference Studies
2.3. Analytical Performance of Proposed Method
2.4. Accuracy of the Method
2.5. Analysis of Real Samples
3. Materials and Methods
3.1. Reagents and Materials
3.2. Instrumentation
3.3. Procedure
4. Discussion
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Conflicts of Interest
References
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Organic Solvent | Melting Point (°C) | Extraction Efficiency of Pb (%) |
---|---|---|
1-dodecanol | 21–24 | 98.1 |
2-dodecanol | 17–18 | 97.2 |
1-undecanol | 16 | 96.5 |
1-bromohexadecane | 17–18 | 97.1 |
n-hexadecane | 18 | 95.8 |
1,10-diclorodecane | 14–16 | 96.2 |
Ion | [Pb(II)]/[Ion] | Added As | Ion | [Pb(II)]/[Ion] | Added As |
---|---|---|---|---|---|
K+ | >1/5000 | KCl | Al3+ | >1/500 | Al(NO3)3 |
Na+ | >1/5000 | NaCl | Fe3+ | 1/300 | Fe(NO3)3 |
Zn2+ | 1/500 | Zn(NO3)2 | Cr3+ | >1/75 | Cr(NO3)3 |
Ca2+ | >1/400 | CaCO3 | Co2+ | 1/1000 | Co(NO3)2 |
Cd2+ | 1/500 | Cd(NO3)2 | Se3+ | 1/2000 | Na2SeO4 |
Hg2+ | >1/50 | HgCl2 | SCN− | 1/2000 | NH4SCN |
Mn2+ | >1/2000 | Mn(NO3)2 | Cl− | >1/5000 | NaCl |
Ni2+ | 1/500 | Ni(NO3)2 | CO32− | 1/500 | Na2(CO3) |
Mg2+ | 1/300 | MgSO4 | SO42− | 1/5000 | MgSO4 |
Cu2+ | >1/200 | Cu(NO3)2 | CH3COO− | 1/2000 | CH3COONa |
Regression Equation | A = xC + y | 0.2135C + 0.0003 |
---|---|---|
Correlation Coefficient | 0.9983 | |
Enhancement Factor | 71.2 | |
Linear Range | µg/L | 0.2–2.5 |
Linear Range without enrichment | µg/L | 15–125 |
LOD | 3s (µg/L) | 0.054 |
LOQ | 10s (µg/L) | 0.18 |
Precision | RSD (%) [0.5 µg/L] n = 7 | 2.30 |
Sample | Certified (μg/L) | Found (μg/L) | Recovery % |
---|---|---|---|
NRC-AQUA-1 Drinking Water | 1.37 ± 0.09 | 1.39 ± 0.12 | 101.1 |
Tap Water (Beytepe—Ankara) | Seawater (Marmara Sea—Istanbul) | Wastewater (Big Scale WWTP—Ankara) | ||||||
---|---|---|---|---|---|---|---|---|
Added (μg/L) | Found (μg/L) | Efficiency (%) | Added (μg/L) | Found (μg/L) | Efficiency (%) | Added (μg/L) | Found (μg/L) | Efficiency (%) |
* BDL | - | * BDL | - | * BDL | - | |||
1.00 | 1.01 | 101.0 | 1.00 | 0.98 | 98.0 | 1.00 | 1.03 | 103.0 |
2.00 | 2.03 | 101.5 | 2.00 | 1.99 | 99.5 | 2.00 | 2.05 | 102.5 |
Stage | Temperature (°C) | Ramp Time (s) | Hold Time (s) | Gas Flow (mL/min) |
---|---|---|---|---|
Drying 1 | 110 | 1 | 20 | 250 |
Drying 2 | 130 | 15 | 20 | 250 |
Pyrolysis | 1000 | 10 | 10 | 250 |
Atomization a | 1500 | 0 | 3 | 0 |
Clean-Out | 1800/2450 b | 1 | 3 | 250 |
Preconcentration Method | Instrument | Enhancement Factor | Limit of Detection (µg/L) | Reference |
---|---|---|---|---|
SPE | FAAS | 20 | 3.7 | [29] |
SPE | FAAS | 200 | 0.4 | [30] |
DLLME | FAAS | 70 | 2.6 | [31] |
UAµE-DES | FAAS | 71.6 | 0.66 | [32] |
UA-SS-LPME | FAAS | 101.6 | 0.63 | [33] |
CPE | ETAAS | 50 | 0.08 | [34] |
DLLME | ETAAS | 78 | 0.039 | [35] |
LPME | ETAAS | 52 | 0.2 | [36] |
DLLME | ETAAS | - | 0.08 | [37] |
LLE | ICP-MS | 23.3 | 0.011 | [38] |
IL-SFODME | ETAAS | 69.2 | 0.075 | This work |
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Durukan, İ.; Yildiz, B. Ionic Liquid—Solidified Floating Organic Drop Microextraction for the Preconcentration of Lead in Environmental Water Samples Prior to Its Determination with Electrothermal Atomic Absorption Spectrometry. Molecules 2024, 29, 4189. https://doi.org/10.3390/molecules29174189
Durukan İ, Yildiz B. Ionic Liquid—Solidified Floating Organic Drop Microextraction for the Preconcentration of Lead in Environmental Water Samples Prior to Its Determination with Electrothermal Atomic Absorption Spectrometry. Molecules. 2024; 29(17):4189. https://doi.org/10.3390/molecules29174189
Chicago/Turabian StyleDurukan, İlknur, and Barış Yildiz. 2024. "Ionic Liquid—Solidified Floating Organic Drop Microextraction for the Preconcentration of Lead in Environmental Water Samples Prior to Its Determination with Electrothermal Atomic Absorption Spectrometry" Molecules 29, no. 17: 4189. https://doi.org/10.3390/molecules29174189