A New Approach to the Determination of Silicon in Zinc, Lead-Bearing Materials and in Waste Using the ICP-OES Method
Abstract
:1. Introduction
2. Results
2.1. Mineralization and ICP-OES Measurement Parameters
- 25 min to reach 190 °C
- 10 min to reach 220 °C
- 15 min for mineralization at 220 °C
- 40 min for cooling
2.2. Radial and Axial ICP-OES Systems
2.3. Spectral Interference
2.4. Validation Parameters
2.5. Silicon Content in Certified Reference Materials and Test Samples
3. Discussion
4. Materials and Methods
4.1. Reagents
4.2. Research Material
- CRM_1—Zinc concentrate (zinc sulfide) with a silicon content of 0.122%—produced by the Institute of Non-Ferrous Metals, Gliwice, Poland;
- CRM_2—Zinc concentrate (zinc sulfide) with a silicon content of 0.295%—produced by the Canadian Certified Reference Materials Project, Ottawa, Canada;
- CRM_3—Lead concentrate (lead sulfide) with a silicon content of 0.305%—produced by the Canadian Certified Reference Materials Project, Ottawa, Canada;
- CRM_4—Zinc oxide with a silicon content of 2.56%—produced by the Institute of Non-Ferrous Metals, Gliwice, Poland;
- CRM_5—Zinc concentrate (zinc sulfide) with a silicon content of 9.30%—manufactured by the China National Analysis Center for Iron and Steel, Beijing, China;
- CRM_6—Zinc ore with a silicon content 38.77%—manufactured by the China National Analysis Center for Iron and Steel, Beijing, China.
4.3. Apparatus
4.4. Selecting the Mineralization Parameters
4.5. Calculation Methods
- 15% of the lower result for a silicon content of 0.1–0.5%;
- 10% of the lower result for a silicon content of 0.51–2%;
- 5% of the result lower for a silicon content of 2.01–10%;
- 2.5% of the lower result for a silicon content above 10%.
4.5.1. Working Range
4.5.2. Linearity
4.5.3. Resistance
4.5.4. Limit of Detection (LOD) and Limit of Quantification (LOQ)
4.5.5. Selectivity
4.5.6. Precision
4.5.7. Correctness
4.5.8. Extended Uncertainty
5. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
Sample Availability
References
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Parameter | Value |
---|---|
Radio frequency power (RF) | 1150 W |
Gas flow in the nebulizer | 0.50 L/min |
Auxiliary gas flow | 0.5 L/min |
Plasma gas flow | 12 L/min |
Pump speed | 50 rpm |
Purge flow | standard |
Nebulizer pressure | 210 a |
Analytical Line, nm | RSD, % | LOQ, mg/L | Selectivity, 1/(mg/L) 1 | |||
---|---|---|---|---|---|---|
Axial | Radial | Axial | Radial | Axial | Radial | |
212.412 | 0.12 | 0.13 | 0.012 | 0.013 | 1285 | 196 |
251.611 | 0.92 | 0.12 | 0.091 | 0.012 | 4915 | 583 |
288.158 | 0.29 | 0.16 | 0.029 | 0.016 | 3188 | 374 |
Parameter | Criteria | Results |
---|---|---|
Working range | 0.10–50% | 0.10–50% |
Linearity | r ≥ 0.999 | r = 1 |
LOD | LOD ≤ 0.05% | LOD = 0.050% |
LOQ | LOQ ≤ 0.10% | LOQ = 0.10% |
Selectivity | Interference may not significantly affect the test results | Molybdenum, chromium and vanadium interference does not statistically significantly affect the test results |
Precision | 1. RSD < 15% in the range of silicon content of 0.10–0.50 % 2. RSD < 10% in the content of silicon > 0.51% | 1. Silicon content range of 0.10–0.50%: RSDmax = 10.2% 2. Silicon content > 0.51% RSDmax = 6.0% |
Correctness | 90% ≤ recovery ≤ 110% | 90.0–101.1% |
Extended uncertainty | 1. U(x) < 50% in the silicon content range of 0.10–0.50% 2. U(x) < 30% in the silicon content > 0.51% | 1. Silicon content range of 0.10–0.50%: U(x)max = 33.2% 2. Silicon content > 0.51%: U(x)max = 19.1% |
Certified Reference Material | Silicon Content Determined ± U(x), % | Silicon Content Given by the Manufacturer ± U(x), % |
---|---|---|
CRM_1 | 0.110 ± 0.035 | 0.122 ± 0.028 |
CRM_2 | 0.265 ± 0.063 | 0.295 ± 0.019 |
CRM_3 | 0.303 ± 0.069 | 0.305 ± 0.029 |
CRM_4 | 2.59 ± 0.29 | 2.56 ± 0.11 |
CRM_5 | 9.05 ± 0.65 | 9.30 ± 0.06 |
CRM_6 | 38.02 ± 1.69 | 38.77 ± 0.10 |
Test Samples | Silicon Content ± U(x), % |
---|---|
1 | 0.190 ± 0.051 |
2 | 0.310 ± 0.070 |
3 | 0.550 ± 0.103 |
4 | 1.65 ± 0.21 |
5 | 2.98 ± 0.31 |
6 | 5.35 ± 0.46 |
7 | 7.56 ± 0.58 |
8 | 12.11 ± 0.79 |
9 | 25.34 ± 1.29 |
Sample No. | Compound | Origin | Average Content of Zn and Pb, % | Appearance |
---|---|---|---|---|
1 | ZnO | obtained from zinc bearing waste (steel dust) | Zn ≈ 62; Pb ≈ 3 | |
2 | PbS | galena | Zn ≈ 3; Pb ≈ 63 | |
3 | ZnO | obtained from zinc bearing waste (sludge) | Zn ≈ 57; Pb ≈ 2 | |
4 | ZnS (blende) | imported from the Grot mine in Serbia | Zn ≈ 49; Pb ≈ 2.5 | |
5 | ZnS (blende) | imported from the Lece mine in Serbia | Zn ≈ 51; Pb ≈ 0.6 | |
6 | Zinc-bearing waste | sludge from flotation process (code 190205) | Zn ≈ 13; Pb ≈ 6 | |
7 | Zinc-bearing waste | Singen steel dust (code 100207) | Zn ≈ 35; Pb ≈ 0.1 | |
8 | Zinc-bearing waste | Tiroler Rohre sludge (code 100213) | Zn ≈ 31; Pb ≈ 0.6 | |
9 | Zinc-lead ore | imported from Swedish mines | Zn ≈ 8; Pb ≈ 4 |
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Przybyła, A.; Kuc, J.; Wzorek, Z. A New Approach to the Determination of Silicon in Zinc, Lead-Bearing Materials and in Waste Using the ICP-OES Method. Molecules 2022, 27, 3059. https://doi.org/10.3390/molecules27103059
Przybyła A, Kuc J, Wzorek Z. A New Approach to the Determination of Silicon in Zinc, Lead-Bearing Materials and in Waste Using the ICP-OES Method. Molecules. 2022; 27(10):3059. https://doi.org/10.3390/molecules27103059
Chicago/Turabian StylePrzybyła, Artur, Joanna Kuc, and Zbigniew Wzorek. 2022. "A New Approach to the Determination of Silicon in Zinc, Lead-Bearing Materials and in Waste Using the ICP-OES Method" Molecules 27, no. 10: 3059. https://doi.org/10.3390/molecules27103059