Physical and Chemical Matrix Effects in Soil Carbon Quantification Using Laser-Induced Breakdown Spectroscopy

DOI: 10.4236/ajac.2014.511080   PDF   HTML   XML   3,731 Downloads   4,743 Views   Citations


Advanced field methods of carbon (C) analysis should now be capable of providing repetitive, sequential measurements for the evaluation of spatial and temporal variation at a scale that was previously unfeasible. Some spectroscopy techniques, such as laser-induced breakdown spectroscopy (LIBS), have portable features that may potentially lead to clean and rapid alternative approaches for this purpose. The goal of this study was to quantify the C content of soils with different textures and with high iron and aluminum concentrations using LIBS. LIBS emission spectra from soil pellets were captured, and the C content was estimated (emission line of C (I) at 193.03 nm) after spectral offset and aluminum spectral interference correction. This technique is highly portable and could be ideal for providing the soil C content in a heterogeneous experiment. Dry combustion was used as a reference method, and for calibration a conventional linear model was evaluated based on soil textural classes. The correlation between reference and LIBS values showed r = 0.86 for medium-textured soils and r = 0.93 for fine-textured soils. The data showed that better correlation and lower error (14%) values were found for the fine-textured LIBS model. The limit of detection (LOD) was found to be 0.32% for medium-textured soils and 0.13% for fine-textured soils. The results indicated that LIBS quantification can be affected by the texture and chemical composition of soil. Signal treatment was shown to be very important for mitigation of these interferences and to improve quantification.

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Segnini, A. , Xavier, A. , Otaviani-Junior, P. , Ferreira, E. , Watanabe, A. , Sperança, M. , Nicolodelli, G. , Villas-Boas, P. , Oliveira, P. and Milori, D. (2014) Physical and Chemical Matrix Effects in Soil Carbon Quantification Using Laser-Induced Breakdown Spectroscopy. American Journal of Analytical Chemistry, 5, 722-729. doi: 10.4236/ajac.2014.511080.

Conflicts of Interest

The authors declare no conflicts of interest.


[1] Segnini, A., Santos, L.M., Silva, W.T.L., Martin-Neto, L., Borato, C.E., Melo, W.J. and Bolonhezi, D. (2008) Comparative Study of Carbon Quantification Methods in Soil with High Fe Contents (Oxisols). Química Nova, 3, 94-97. (in Portuguese, with Abstract in English)
[2] Nelson, D.W. and Sommers, L.E. (1982) Total Carbon, Organic Carbon, and Organic Matter. In: Page, A.L., Miller, R.H. and Keeney, D.R., Eds., Methods of Soil Analysis. Part 3: Chemical Methods, American Society of Agronomy, Madison, 961-1010.
[3] Miyazawa, M., Pavan, M.A., Oliveira, E.L., Ionashiro, M. and Silva, A.K. (2000) Gravimetric Determination of Soil Organic Matter. Brazilian Archives of Biology and Technology, 43, 475-478.
[4] Tabatabai, M.A. and Bremner, J.M. (1991) Automated Instruments for Determination of Total Carbon, Nitrogen, and Sulfur in Soils by Combustion Techniques. In: Smith, K.A., Ed., Soil Analysis: Modern Instrumental Techniques, Marcel Dekker, New York, 261-286.
[5] Jimenez, R.R. and Ladha, J.K. (1993) Automated Elemental Analysis—A Rapid and Reliable but Expensive Measurement of Total Carbon and Nitrogen in Plant and Soil Samples. Communications in Soil Science and Plant Analysis, 24, 1897-1924.
[6] Cremers, D.A., Ebinger, M.H., Breshears, D.D., Unkefer, P.J., Kammerdiener, S.A., Ferris, M.J., Catlett, K.M. and Brown, J.R. (2001) Measuring Total Soil Carbon with Laser-Induced Breakdown Spectroscopy (LIBS). Journal of Environmental Quality, 30, 2202-2206.
[7] Ebinger, M.H., Norfleet, M.L., Breshears, D.D., Cremers, D.A., Ferris, M.J., Unkefer, P.J., Lamb, M.S., Goddard, K.L. and Meyer, C.W. (2003) Extending the Applicability of Laser-Induced Breakdown Spectroscopy for Total Soil Carbon Measurement. Soil Science Society of America Journal, 67, 1616-1619.
[8] Da Silva, R.M., Milori, D.M.B.P., Ferreira, E.C., Ferreira, E.J., Krug, F.J. and Martin-Neto, L. (2008) Total Carbon Measurement in Whole Tropical Soil Sample. Spectrochimica Acta Part B—AtomicSpectroscopy, 63, 1221-1224.
[9] Belkov, M.V., Burakov, V.S., De Giacomo, A., Kiris, V.V., Raikov, S.N. and Tarasenko, N.V. (2009) Comparison of Two Laser-Induced Breakdown Spectroscopy Techniques for Total Carbon Measurement in Soils. Spectrochimica Acta Part B—Atomic Spectroscopy, 64, 899-904.
[10] Martin, M.Z., Labbe, N., Andre, N., Wullschleger, S.D., Harris, R.D. and Ebinger, M.H. (2010) Novel Multivariate Analysis for Soil Carbon Measurements Using Laser-Induced Breakdown Spectroscopy. Soil Science Society of America Journal, 74, 87-93.
[11] Burakov, V.S., Raikov, S.N., Tarasenko, N.V., Belkov, M.V. and Kiris, V.V. (2010) Development of a Laser-Induced Breakdown Spectroscopy Method for Soil and Ecological Analysis (Review). Journal of Applied Spectroscopy, 77, 595-608.
[12] Diaz, D., Hahn, D.W. and Molinat, A. (2012) Evaluation of Laser-Induced Breakdown Spectroscopy (LIBS) as a Measurement Technique for Evaluation of Total Elemental Concentration in Soils. Applied Spectroscopy, 66, 99-106.
[13] Ayyalasomayajula, K.K., Fang, Y.Y., Singh, J.P., McIntyre, D.L. and Jain, J. (2012) Application of Laser-Induced Breakdown Spectroscopy for Total Carbon Quantification in Soil Samples. Applied Optics, 51, B149-B154.
[14] Fortes, F.J., Moros, J., Lucena, P., Cabalin, L.M. and Laserna, J.J. (2013) Laser-Induced Breakdown Spectroscopy. Analytical Chemistry, 85, 640-669.
[15] Nicolodelli, G., Marangoni, B.S., Cabral, J.S., Villas-Boas, P.R., Senesi, G.S., Santos, C.H., Romano, R.A., Segnini, A., Lucas, Y., Montes, C.R. and Milori D.M.B.P. (2014) Quantification of Total Carbon in Soil Using Laser-Induced Breakdown Spectroscopy (LIBS): A Method to Correct Interference Lines. Applied Optics, 53, 2170-2176.
[16] Pareja, J., Lopez, S., Jaramillo, D., Hahn, D.W. and Molina, A. (2013) Laser Ablation-Laser Induced Breakdown Spectroscopy for the Measurement of Total Elemental Concentration in Soils. Applied Optics, 52, 2470-2477.
[17] Izaurralde, R.C., Rice, C.W., Wielopolski, L., Ebinger, M.H., Reeves, J.B., Thomson, A.M., Harris, R., Francis, B., Mitra, S., Rappaport, A.G., Etchevers, J.D., Sayre, K.D., Govaerts, B. and McCarty, G.W. (2013) Evaluation of Three Field-Based Methods for Quantifying Soil Carbon. PLoS ONE, 8, Article ID: e55560.
[18] Milori, D.M.P.B., Segnini, A., Da Silva, W.T.L., Posadas, A., Mares, V., Quiroz, R. and Martin-Neto, L. (2011) Emerging Techniques for Soil Carbon Measurements. CCAFS Working Paper No. 2. CGIAR Research Program on Climate Change, Agriculture and Food Security (CCAFS), Copenhagen, Denmark.
[19] Nomura, C.S., Da Silva, C.S. and Oliveira, P.V. (2008) Solid Sampling Grafite FurnaceAtomic Absortion Spectroscopy: A Review. Quimica Nova, 31, 104-113. (in Portuguese)
[20] Kurfüst, U. (1998) Solid Sample Analysis. Springer-Verlag, Berlin & Heidelberg.
[21] Trevizan, L.C., Santos Jr., D., Samad, R.E., Vieira Jr., N.D., Nunes, L.C., Rufini, I.A. and Krug, F.J. (2009) Evaluation of Laser Induced Breakdown Spectroscopy for the Determination of Micronutrients in Plant Materials. Spectrochimica Acta Part B: Atomic Spectroscopy, 64, 369-377.
[22] Pasquini, C., Cortez, J., Silva, L.M.C. and Gonzaga, F.B. (2007) Laser-Induced Breakdown Spectroscopy. Journal of the Brazilian Chemical Society, 18, 463-512.

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