Optimization of Ni(II), Pb(II), and Zn(II) Ion Adsorption Conditions on Pliocene Clays from Post-Mining Waste
Abstract
:1. Introduction
2. Materials and Methods
2.1. Materials
2.2. Instruments
2.3. Methods
2.3.1. Physical and Chemical Analyses
2.3.2. Point of Zero Charge
2.3.3. Sorption Tests
2.3.4. Optimization of Adsorption Conditions
2.3.5. Adsorption Kinetics
2.3.6. Thermodynamic Studies
2.3.7. Leaching Studies
3. Results and Discussion
3.1. Material Characterization
3.1.1. Granulometric Analysis
3.1.2. Mineralogical Composition
3.1.3. Chemical Composition
3.1.4. Structural Properties
3.1.5. Point of Zero Charge pH
3.2. Optimization of Adsorption Conditions
3.3. Adsorption Kinetics
3.4. Thermodynamic Studies
3.5. Leaching Studies
4. Conclusions
- The chemical composition of the studied rocks allows for their use in the adsorption process without the risk of secondary contamination of the treated waters or sewage.
- Structural parameters, such as the specific surface area and the dominant pore size, indicate the potentially good sorption properties of the studied rocks.
- The pHpzc = 7.1 allows for the adsorption to be carried out in a nearly neutral pH.
- The optimization of the selection of adsorption conditions indicates that the optimal dose of the adsorbent is about 20 g/dm3, and the pH value should be about 6, which is consistent with the conclusions regarding the point of zero charge pH. The pH value may be lowered to avoid precipitation if necessary; however, this may weaken the adsorption.
- The results of the research on kinetics show that the adsorption process is very fast; after just a few minutes, the adsorbent is practically saturated with metal ions.
- The negative Gibbs free energy indicates that the adsorption is spontaneous and thermodynamically favored.
- The low leachability of the Pb, Zn, and Ni from the tested clays, weakly alkaline pH, and high ability to bind metal cations make the post-mine Pliocene clay waste a low-cost effective sorbent for Pb(II), Ni(II), and Zn(II) ions.
Funding
Data Availability Statement
Conflicts of Interest
References
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Component | SiO2 | Al2O3 | Fe2O3 | CaO | MgO | Cr2O3 | MnO |
Content, wt% | 56.8 | 21.1 | 5.3 | 3.5 | 1.4 | 0.025 | 0.35 |
Component | K2O | P2O5 | SO3 | Na2O | TiO2 | ZrO2 | Loss on ignition |
Content, wt% | 0.43 | 0.16 | <0.01 | 0.45 | 0.27 | <0.01 | 9.82 |
Content, mg/kg DM | |||||||||
---|---|---|---|---|---|---|---|---|---|
Ba | Cd | Co | Cr | Cu | Ni | Pb | Sr | Zn | |
Determined | 96.17 | <0.01 | 11.56 | 101.8 | 20.02 | 32.6 | <0.01 | 64.45 | 123.8 |
Permissible | 200 | 4 | 20 | 150 | 150 | 100 | 100 | - | 300 |
pH | Concentration, mg/dm3 | ||||||||
---|---|---|---|---|---|---|---|---|---|
Ag | Ba | Cd | Cr | Cu | Fe | Mn | Ni | ||
Determined | 7.5 | 0.079 | <0.01 | <0.01 | 0.047 | 0.026 | 0.12 | <0.01 | <0.01 |
Permissible | 6.5–9 | 0.1 | 2 | 0.4 | 0.5 | 0.5 | 10 | - | 0.5 |
Concentration, mg/dm3 | |||||||||
Pb | Sr | Zn | Mg2+ | Ca2+ | Na+ | K+ | Cl− | SO42− | |
Determined | <0.01 | 0.24 | 0.036 | 5.061 | 26.9 | 3.9 | 6.39 | <10 | <15 |
Permissible | 0.5 | - | 2 | - | - | 800 | 80 | 1000 | 500 |
[mg/dm3] | [g] | [mg/dm3] | Removal [%] | |||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|
Zn, Ni | Pb | Zn | Ni | Pb | Zn | Ni | Pb | |||||
−1 | 3.8 | −1 | 26 | 141 | −1 | 1.8 | 3.4 | 4.8 | 17.4 | 87.1 | 81.7 | 87.6 |
1 | 6.2 | −1 | 26 | 141 | −1 | 1.8 | 1.9 | 3.6 | 0.4 | 92.7 | 86.1 | 99.7 |
−1 | 3.8 | 1 | 74 | 259 | −1 | 1.8 | 21.7 | 22.2 | 67.5 | 70.6 | 69.9 | 74.0 |
1 | 6.2 | 1 | 74 | 259 | −1 | 1.8 | 18.3 | 24.1 | 1.9 | 75.1 | 67.4 | 99.3 |
−1 | 3.8 | −1 | 26 | 141 | 1 | 4.2 | 1.7 | 2.5 | 13.0 | 93.4 | 90.6 | 90.7 |
1 | 6.2 | −1 | 26 | 141 | 1 | 4.2 | 0.5 | 1.5 | 0.3 | 98.2 | 94.4 | 99.8 |
−1 | 3.8 | 1 | 74 | 259 | 1 | 4.2 | 8.9 | 13.2 | 42.9 | 88.0 | 82.1 | 83.5 |
1 | 6.2 | 1 | 74 | 259 | 1 | 4.2 | 6.3 | 11.0 | 0.5 | 91.4 | 85.1 | 99.8 |
0 | 5 | 0 | 50 | 200 | 0 | 3 | 6.1 | 7.3 | 10.1 | 87.9 | 85.3 | 95.0 |
0 | 5 | 0 | 50 | 200 | 0 | 3 | 5.8 | 8.2 | 12.2 | 88.5 | 83.6 | 93.9 |
0 | 5 | 0 | 50 | 200 | 0 | 3 | 5.9 | 7.3 | 10.8 | 88.1 | 85.4 | 94.6 |
−1.68 | 3 | 0 | 50 | 200 | 0 | 3 | 14.3 | 12.6 | 67.3 | 71.4 | 74.7 | 66.3 |
1.68 | 7 | 0 | 50 | 200 | 0 | 3 | 0.3 | 7.3 | 0.3 | 99.5 | 85.4 | 99.9 |
0 | 5 | −1.68 | 10 | 100 | 0 | 3 | 0.2 | 0.7 | 2.5 | 97.9 | 93.1 | 97.5 |
0 | 5 | 1.68 | 90 | 300 | 0 | 3 | 18.1 | 23.0 | 25.0 | 79.9 | 74.5 | 91.7 |
0 | 5 | 0 | 50 | 200 | −1.68 | 1 | 17.2 | 19.3 | 34.2 | 65.5 | 61.4 | 82.9 |
0 | 5 | 0 | 50 | 200 | 1.68 | 5 | 2.7 | 5.9 | 5.7 | 94.6 | 88.2 | 97.2 |
0 | 5 | 0 | 50 | 200 | 0 | 3 | 6.6 | 7.4 | 13.6 | 86.7 | 85.3 | 93.2 |
0 | 5 | 0 | 50 | 200 | 0 | 3 | 6.1 | 7.6 | 11.0 | 87.8 | 84.7 | 94.5 |
0 | 5 | 0 | 50 | 200 | 0 | 3 | 6.1 | 8.1 | 15.3 | 87.7 | 83.9 | 92.3 |
Parameter | Zn(II) | Ni(II) | Pb(II) | |||
---|---|---|---|---|---|---|
Variance, % | Variance, % | Variance, % | ||||
0 | 88.1 | - | 84.9 | - | 93.8 | - |
1 | 4.81 | 18 | 1.94 | 4 | 8.72 | 68 |
2 | −5.60 | 25 | −5.84 | 34 | −2.29 | 5 |
3 | 6.90 | 38 | 6.75 | 46 | 2.73 | 7 |
4 | - | - | −0.97 | <1 | 2.55 | 3 |
5 | - | - | - | - | −1.50 | 1 |
6 | 2.74 | 3.5 | 1.60 | 1 | - | - |
7 | - | - | −1.04 | <1 | −3.22 | 10 |
8 | - | - | - | - | 0.84 | <1 |
9 | −2.26 | 4.5 | −2.89 | 9 | −0.77 | <1 |
Unexplained | - | 11 | - | 5 | - | 5 |
Adjusted | 0.85 | - | 0.92 | - | 0.91 | - |
Metal | Maximum | |||
---|---|---|---|---|
pH0 | [g] | |||
Zn(II) | (1.68, 1.52) | 7.0 | 4.8 | |
Ni(II) | (0.93, 1.16) | 6.1 | 4.4 | |
Pb(II) | (1.22, 0.58) | 6.4 | 3.7 |
Parameter or Indicator | Unit | Ni(II) | Pb(II) | Zn(II) | |||
---|---|---|---|---|---|---|---|
PFO, Equations (1)–(4) | |||||||
mg/g | 6.45 ± 0.07 | 9.98 ± 0.07 | 9.74 ± 0.06 | 18.54 ± 0.10 | 6.59 ± 0.04 | 9.92 ± 0.15 | |
min−1 | 0.58 ± 0.11 | 0.45 ± 0.04 | 0.64 ± 0.09 | 0.68 ± 0.09 | 0.65 ± 0.09 | 0.45 ± 0.08 | |
min | 1.19 ± 0.22 | 1.53 ± 0.12 | 1.09 ± 0.15 | 1.02 ± 0.14 | 1.07 ± 0.16 | 1.55 ± 0.27 | |
mg/g | 0.20 | 0.20 | 0.18 | 0.30 | 0.13 | 0.42 | |
mg/g | 0.031 | 0.019 | 0.017 | 0.025 | 0.012 | 0.091 | |
PSO, Equations (5)–(8) | |||||||
mg/g | 6.51 ± 0.07 | 10.1 ± 0.05 | 9.77 ± 0.08 | 18.65 ± 0.08 | 6.60 ± 0.06 | 10.07 ± 0.13 | |
g/(mg min) | 0.43 ± 0.20 | 0.15 ± 0.02 | 0.55 ± 0.35 | 0.22 ± 0.06 | 0.92 ± 0.67 | 0.13 ± 0.04 | |
min | 0.35 ± 0.15 | 0.64 ± 0.07 | 0.19 ± 0.11 | 0.24 ± 0.06 | 0.16 ± 0.12 | 0.73 ± 0.21 | |
mg/g | 0.18 | 0.12 | 0.21 | 0.21 | 0.14 | 0.33 | |
mg/g | 0.024 | 0.0071 | 0.022 | 0.012 | 0.016 | 0.056 | |
IPD, Equation (10) | |||||||
mg/g min−0.5 | 0.025 ± 0.010 | 0.045 ± 0.021 | 0.0036 ± 0.014 | 0.045 ± 0.014 | 0 ± 0.010 | 0.078 ± 0.015 | |
mg/g | 6.17 ± 0.11 | 9.41 ± 0.23 | 9.66 ± 0.16 | 18.03 ± 0.16 | 6.56 ± 0.11 | 9.2 ± 0.17 | |
mg/g | 0.18 | 0.35 | 0.25 | 0.25 | 0.17 | 0.26 | |
mg/g | 0.024 | 0.065 | 0.032 | 0.017 | 0.021 | 0.036 | |
IPD1, Equations (12)–(15) | |||||||
mg/g | 6.47 ± 0.07 | 9.98 ± 0.07 | 9.74 ± 0.06 | 18.55 ± 0.10 | 6.59 ± 0.04 | 9.93 ± 0.15 | |
min−1 | 0.48 ± 0.11 | 0.35 ± 0.03 | 0.54 ± 0.09 | 0.58 ± 0.09 | 0.55 ± 0.09 | 0.34 ± 0.08 | |
min | 0.61 ± 0.14 | 0.85 ± 0.08 | 0.55 ± 0.09 | 0.51 ± 0.08 | 0.54 ± 0.09 | 0.86 ± 0.19 | |
mg/g | 0.20 | 0.19 | 0.18 | 0.30 | 0.13 | 0.42 | |
mg/g | 0.031 | 0.018 | 0.017 | 0.024 | 0.012 | 0.089 | |
μm2/min | 0.60 | 0.43 | 0.67 | 0.72 | 0.68 | 0.43 |
Temperature, [°C] | Equilibrium Concentration [mg/dm3] | The Gibbs Free Energy (ΔG) [kJ/mol] | ||||
---|---|---|---|---|---|---|
Pb(II) | Ni(II) | Zn(II) | Pb(II) | Ni(II) | Zn(II) | |
20 | 5.06 | 36.4 | 33.2 | −19.7 | −15.4 | −15.6 |
30 | 4.34 | 32.9 | 32.1 | −21.1 | −16.2 | −16.1 |
40 | 3.52 | 28.2 | 34.0 | −22.4 | −16.9 | −16.7 |
50 | 2.40 | 28.1 | 32.1 | −23.7 | −17.7 | −17.2 |
ΔH [kJ/mol] | 19.4 ± 3.3 | 7.4 ± 1.6 | 0.3 ± 1.2 | |||
ΔS [J/(mol K)] | 134 ± 11 | 77.0 ± 5.1 | 54.4 ± 3.9 | |||
R2 | 0.943 | 0.918 | 0.038 |
Metal | Mean Concentration in the Effluent, mg/dm3 | Standard Deviation, mg/dm3 | Relative Standard Deviation, % | Effluent pH | Leachabilty, mg/kg DM | Percentage Leachability, % | Permissible Leachability, mg/kg DM * | ||
---|---|---|---|---|---|---|---|---|---|
A | B | C | |||||||
Pb | 0.077 | 0.003 | 3.92 | 7.09 | 0.77 | 0.02 | 0.5 | 10 | 50 |
Ni | 0.454 | 0.002 | 0.44 | 7.15 | 4.54 | 0.14 | 0.4 | 10 | 40 |
Zn | 0.232 | 0.021 | 9.19 | 6.89 | 2.32 | 0.05 | 4 | 50 | 200 |
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Jabłońska, B. Optimization of Ni(II), Pb(II), and Zn(II) Ion Adsorption Conditions on Pliocene Clays from Post-Mining Waste. Minerals 2021, 11, 568. https://doi.org/10.3390/min11060568
Jabłońska B. Optimization of Ni(II), Pb(II), and Zn(II) Ion Adsorption Conditions on Pliocene Clays from Post-Mining Waste. Minerals. 2021; 11(6):568. https://doi.org/10.3390/min11060568
Chicago/Turabian StyleJabłońska, Beata. 2021. "Optimization of Ni(II), Pb(II), and Zn(II) Ion Adsorption Conditions on Pliocene Clays from Post-Mining Waste" Minerals 11, no. 6: 568. https://doi.org/10.3390/min11060568