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Strategies for the direct analysis of sugar cane leaves by laser induced breakdown spectroscopy(LIBS)

Grant number: 12/16203-5
Support type:Scholarships in Brazil - Post-Doctorate
Effective date (Start): November 01, 2012
Effective date (End): October 31, 2015
Field of knowledge:Physical Sciences and Mathematics - Chemistry - Analytical Chemistry
Principal Investigator:Francisco José Krug
Grantee:Marcelo Braga Bueno Guerra
Home Institution: Centro de Energia Nuclear na Agricultura (CENA). Universidade de São Paulo (USP). Piracicaba , SP, Brazil

Abstract

The aim of this postdoctoral project is the evaluation of analytical strategies for the direct and simultaneous determination of macro-(P, K, Ca and Mg), micronutrients (Fe, Cu, Mn, Zn and B) and Si in sugarcane leaves by laser induced breakdown spectrometry (LIBS). The analyzes will be conducted in a high-resolution spectrometer equipped with Echelle grating and ICCD detector. The Nd: YAG laser is operated in the fundamental wavelength (1064 nm). The main objective of this project is to propose an experimental protocol for the determination of analytes on the surface of the leaves after washing and drying them. The following parameters that can affect the quality of analytical results will be optimized:- Laser wavelength,- The laser fluence (energy per pulse and spot size),- Number of laser pulses by subsample (obtained by sampling the middle third of each leaf),- Minimum number of segments by middle third of each leaf.Instrumental variables will be also evaluated as delay and integration times. Eventually, other laser wavelengths at different harmonics (532, 355 and 266 nm) will be tested depending on the laser stability. Factorial and Doehlert design will be used to assess the best instrumental conditions. Multivariate calibration strategies based on PLS (Partial Least Squares) using Pirouette 4.0 software will be used and compared with the univariate method. Preliminary results indicate a great potential and feasibility of the proposed method. The final steps of this project will test the possibility of analysis in situ and in real time with fresh samples. Among the advantages of this analytical method can be mentioned: it is a green method (will not be necessary to use toxic and corrosive reagents in the determination of analytes of interest); high analytical throughput, lower capital expenditures for leaf analyzes and possibilities of obtaining accurate and precise results in situ.

Scientific publications (8)
(References retrieved automatically from Web of Science and SciELO through information on FAPESP grants and their corresponding numbers as mentioned in the publications by the authors)
GUERRA, MARCELO B. B.; ADAME, ANDRESSA; DE ALMEIDA, EDUARDO; BRASIL, MARCOS A. S.; SCHAEFER, CARLOS E. G. R.; KRUG, FRANCISCO J. In situ Determination of K, Ca, S and Si in Fresh Sugar Cane Leaves by Handheld Energy Dispersive X-Ray Fluorescence Spectrometry. Journal of the Brazilian Chemical Society, v. 29, n. 5, p. 1086-1093, MAY 2018. Web of Science Citations: 3.
ARANTES DE CARVALHO, GABRIEL GUSTINELLI; SANTOS, JR., DARIO; GOMES, MARCOS DA SILVA; NUNES, LIDIANE CRISTINA; BUENO GUERRA, MARCELO BRAGA; KRUG, FRANCISCO JOSE. Influence of particle size distribution on the analysis of pellets of plant materials by laser-induced breakdown spectroscopy. SPECTROCHIMICA ACTA PART B-ATOMIC SPECTROSCOPY, v. 105, n. SI, p. 130-135, MAR 1 2015. Web of Science Citations: 18.
BUENO GUERRA, MARCELO BRAGA; ADAME, ANDRESSA; DE ALMEIDA, EDUARDO; ARANTES DE CARVALHO, GABRIEL GUSTINELLI; STOLF BRASIL, MARCOS AUGUSTO; SANTOS, JR., DARIO; KRUG, FRANCISCO JOSE. Direct analysis of plant leaves by EDXRF and LIBS: microsampling strategies and cross-validation. Journal of Analytical Atomic Spectrometry, v. 30, n. 7, p. 1646-1654, 2015. Web of Science Citations: 9.
PERUCHI, LIDIANE CRISTINA; NUNES, LIDIANE CRISTINA; ARANTES DE CARVALHO, GABRIEL GUSTINELLI; BUENO GUERRA, MARCELO BRAGA; DE ALMEIDA, EDUARDO; RUFINI, IOLANDA APARECIDA; SANTOS, JR., DARIO; KRUG, FRANCISCO JOSE. Determination of inorganic nutrients in wheat flour by laser-induced breakdown spectroscopy and energy dispersive X-ray fluorescence spectrometry. SPECTROCHIMICA ACTA PART B-ATOMIC SPECTROSCOPY, v. 100, p. 129-136, OCT 1 2014. Web of Science Citations: 28.
BUENO GUERRA, MARCELO BRAGA; DE ALMEIDA, EDUARDO; CARVALHO, GABRIEL G. A.; SOUZA, PAULINO F.; NUNES, LIDIANE CRISTINA; SANTOS JUNIOR, DARIO; KRUG, FRANCISCO JOSE. Comparison of analytical performance of benchtop and handheld energy dispersive X-ray fluorescence systems for the direct analysis of plant materials. Journal of Analytical Atomic Spectrometry, v. 29, n. 9, p. 1667-1674, SEP 2014. Web of Science Citations: 18.
CAMPOS, NAIARA V.; PEREIRA, TIAGO A. R.; MACHADO, MARIANA F.; GUERRA, MARCELO B. B.; TOLENTINO, GLAUCIA S.; ARAUJO, JOSIANE S.; REZENDE, MAIRA Q.; DA SILVA, MARIA CAROLINA N. A.; SCHAEFER, CARLOS E. G. R. Evaluation of micro-energy dispersive X-ray fluorescence and histochemical tests for aluminium detection in plants from High Altitude Rocky Complexes, Southeast Brazil. Anais da Academia Brasileira de Ciências, v. 86, n. 1, p. 285-296, Mar. 2014. Web of Science Citations: 6.
DE SOUZA, PAULINO FLORENCIO; SANTOS JUNIOR, DARIO; ARANTES DE CARVALHO, GABRIEL GUSTINELLI; NUNES, LIDIANE CRISTINA; GOMES, MARCOS DA SILVA; BUENO GUERRA, MARCELO BRAGA; KRUG, FRANCISCO JOSE. Determination of silicon in plant materials by laser-induced breakdown spectroscopy. SPECTROCHIMICA ACTA PART B-ATOMIC SPECTROSCOPY, v. 83-84, p. 61-65, MAY-JUN 2013. Web of Science Citations: 24.
BUENO GUERRA, MARCELO BRAGA; SCHAEFER, CARLOS E. G. R.; DE CARVALHO, GABRIEL G. A.; DE SOUZA, PAULINO F.; SANTOS JUNIOR, DARIO; NUNES, LIDIANE C.; KRUG, FRANCISCO J. Evaluation of micro-energy dispersive X-ray fluorescence spectrometry for the analysis of plant materials. Journal of Analytical Atomic Spectrometry, v. 28, n. 7, p. 1096-1101, 2013. Web of Science Citations: 16.

Please report errors in scientific publications list by writing to: cdi@fapesp.br.