Carbonaceous Materials Porosity Investigation in a Wet State by Low-Field NMR Relaxometry
Abstract
:1. Introduction
2. Materials and Methods
2.1. Preparation of the Mesoporous Carbon Material
2.2. Thermoporometry Analysis
2.3. Adsorption of Nitrogen
2.4. H-NMR Relaxometry Analysis
2.5. NMR Data Evaluation Procedure
3. Results and Discussion
3.1. Characterization of MC Sample by TPM and N2 Physisorption
3.2. 1H-NMR Relaxation Measurements
3.2.1. Determination of Number of Components
3.2.2. Analysis of Found Components
3.2.3. Estimation of Surface Relaxivity
4. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Acknowledgments
Conflicts of Interest
References
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Sample | Mass of Dry Sample (g) | Mass of H2O (g) | Mass Ratio H2O/C |
---|---|---|---|
MC-0-A | 0.1368 | 0 | 0 |
MC-0-B | 0.1407 | 0 | 0 |
MC-30-A | 0.1108 | 0.0024 | 0.02 |
MC-30-B | 0.1142 | 0.0024 | 0.02 |
MC-100-A | 0.1536 | 0.0391 | 0.25 |
MC-100-B | 0.1520 | 0.0387 | 0.25 |
MC-1:2 | 0.1451 | 0.2939 | 2.03 |
MC-1:4-A | 0.1099 | 0.4341 | 3.95 |
MC-1:4-B | 0.1173 | 0.4643 | 3.96 |
MC-1:4-C | 0.1080 | 0.4342 | 4.02 |
MC-1:6 | 0.0899 | 0.5393 | 6.00 |
Method | Vultramicro (cm3/g) | Sultramicro (m2/g) | Vsupermicro (cm3/g) | Ssupermicro (m2/g) | Vmeso (cm3/g) | Smeso (m2/g) | Mesopore Diameter (*) (nm) |
---|---|---|---|---|---|---|---|
TPM | n/a | n/a | n/a | n/a | 0.92 | n/a | 14 |
N2 adsorption | 0.06 | 225 | 0.04 | 65 | 0.98 | 405 | 9 |
Number of Comp. | Relaxation Curve | Residues | Calculated Parameters | |
---|---|---|---|---|
A (%) | T2 (ms) | |||
1 | R2 = 0.888 | 100 | 2495.5 | |
2 | R2 = 0.996 | 67.8 32.2 | 49.0 3320.5 | |
3 | R2 = 0.999 | 43.4 27.9 28.6 | 17.5 113.9 3534.6 | |
4 | R2 = 0.999 | 32.2 69.5 5.2 27.5 | 11.9 35.1 429.5 3711.6 | |
5 | R2 = 0.999 | 22.8 30.8 16.7 3.4 26.3 | 8.4 39.9 128.2 1028.2 3861.2 |
Sample (Measurement) | τ (ms) | Number of Components | T2 (ms) |
---|---|---|---|
MC-100 (1) | 0.05 | 2 | 5.5 |
MC-100 (2) | 0.05 | 2 | 6.2 |
MC-100 (3) | 0.05 | 2 | 5.5 |
MC-1:2 (1) | 0.2 | 3 | 20.2 |
MC-1:2 (2) | 0.05 | 4 | 22.4 |
MC-1:4-A (1) | 0.2 | 5 | 1353 |
MC-1:4-A (2) | 0.2 | 5 | 1228 |
MC-1:4-A (3) | 0.05 | 5 | 1386 |
MC-1:4-A (4) | 0.05 | 5 | 1413 |
MC-1:4-B (1) | 0.2 | 5 | 1845 |
MC-1:4-B (2) | 0.05 | 5 | 1620 |
MC-1:4-C (1) | 0.2 | 5 | 1299 |
MC-1:4-C (2) | 0.05 | 5 | 1209 |
MC-1:6 (1) | 0.2 | 5 | 1086 |
MC-1:6 (2) | 0.05 | 5 | 1129 |
Interval T2 (ms) | <2 | 2–7 | 7–20 | 20–80 | 80–350 | 350–1500 | Above 1500 | |||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Sample | A (%) | T2 (ms) | A (%) | T2 (ms) | A (%) | T2 (ms) | A (%) | T2 (ms) | A (%) | T2 (ms) | A (%) | T2 (ms) | A (%) | T2 (ms) |
MC-100 (1) | 14.1 | 0.9 | 85.9 | 6.2 | ||||||||||
MC-100 (2) | 7.2 | 0.7 | 92.8 | 6.6 | ||||||||||
MC-100 (3) | 15.2 | 1.0 | 84.8 | 6.3 | ||||||||||
MC-1:2 (1) | 18.2 | 0.8 | 55.9 | 13.9 | 24.4 | 50.3 | 1.5 | 1781 | ||||||
MC-1:2 (2) | 14.9 | 5.6 | 58.0 | 15.4 | 25.3 | 49.8 | 1.8 | 1758 | ||||||
MC-1:4-A (1) | 18.8 | 11.8 | 25.3 | 50.8 | 15.7 | 195.6 | 7.6 | 823 | 32.6 | 3818 | ||||
MC-1:4-A (2) | 19.8 | 11.7 | 25.3 | 51.1 | 13.2 | 188.1 | 8.0 | 874 | 33.7 | 3318 | ||||
MC-1:4-A (3) | 18.4 | 10.9 | 23.9 | 47.4 | 15.0 | 165.1 | 8.5 | 592 | 34.1 | 3806 | ||||
MC-1:4-A (4) | 19.4 | 11.3 | 25.2 | 48.0 | 14.1 | 162.1 | 7.5 | 697 | 33.8 | 3916 | ||||
MC-1:4-B (1) | 19.5 | 13.0 | 27.4 | 56.9 | 7.7 | 182.6 | 5.3 | 1051 | 40.1 | 4382 | ||||
MC-1:4-B (2) | 17.8 | 10.6 | 22.1 | 43.8 | 14.3 | 105.4 | 4.1 | 410 | 41.6 | 3789 | ||||
MC-1:4-C (1) | 19.1 | 12.1 | 23.4 | 48.9 | 17.6 | 139.8 | 4.3 | 852 | 35.5 | 3449 | ||||
MC-1:4-C (2) | 19.9 | 12.1 | 23.4 | 49.0 | 17.7 | 132.4 | 5.3 | 551 | 33.7 | 3390 | ||||
MC-1:6 (1) | 22.8 | 8.4 | 30.8 | 39.9 | 16.7 | 128.2 | 3.4 | 1028 | 26.3 | 3861 | ||||
MC-1:6 (2) | 21.7 | 8.7 | 30.6 | 39.9 | 17.5 | 117.3 | 3.1 | 633 | 27.1 | 3965 | ||||
Average | 0.9 | 6.2 | 11.7 | 48.0 | 151.7 | 751 | 3436 |
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Kinnertová, E.; Slovák, V.; Zelenka, T.; Vaulot, C.; Delmotte, L. Carbonaceous Materials Porosity Investigation in a Wet State by Low-Field NMR Relaxometry. Materials 2022, 15, 9021. https://doi.org/10.3390/ma15249021
Kinnertová E, Slovák V, Zelenka T, Vaulot C, Delmotte L. Carbonaceous Materials Porosity Investigation in a Wet State by Low-Field NMR Relaxometry. Materials. 2022; 15(24):9021. https://doi.org/10.3390/ma15249021
Chicago/Turabian StyleKinnertová, Eva, Václav Slovák, Tomáš Zelenka, Cyril Vaulot, and Luc Delmotte. 2022. "Carbonaceous Materials Porosity Investigation in a Wet State by Low-Field NMR Relaxometry" Materials 15, no. 24: 9021. https://doi.org/10.3390/ma15249021