title: Evaluation of grinding methods for pellets preparation aiming at the analysis of plant materials by laser induced breakdown spectrometry.
abstract: It has been demonstrated that laser induced breakdown spectrometry (LIBS) can be used as an alternative method for the determination of macro (P, K, Ca, Mg) and micronutrients (B, Fe, Cu, Mn, Zn) in pellets of plant materials. However, information is required regarding the sample preparation for plant analysis by LIBS. In this work, methods involving cryogenic grinding and planetary ball milling were evaluated for leaves comminution before pellets preparation. The particle sizes were associated to chemical sample properties such as fiber and cellulose contents, as well as to pellets porosity and density. The pellets were ablated at 30 different sites by applying 25 laser pulses per site (Nd:YAG@1064 nm, 5 ns, 10 Hz, 25J cm(-2)). The plasma emission collected by lenses was directed through an optical fiber towards a high resolution echelle spectrometer equipped with an ICCD. Delay time and integration time gate were fixed at 2.0 and 4.5 μs, respectively. Experiments carried out with pellets of sugarcane, orange tree and soy leaves showed a significant effect of the plant species for choosing the most appropriate grinding conditions. By using ball milling with agate materials, 20 min grinding for orange tree and soy, and 60 min for sugarcane leaves led to particle size distributions generally lower than 75 μm. Cryogenic grinding yielded similar particle size distributions after 10 min for orange tree, 20 min for soy and 30 min for sugarcane leaves. There was up to 50% emission signal enhancement on LIBS measurements for most elements by improving particle size distribution and consequently the pellet porosity.
authors.affiliation: Universidade Federal de São Carlos, Departamento de Química, Rodovia Washington Luiz km 235, São Carlos/SP, Brazil.
authors.forename: Marcos da Silva
authors.initials: Mda S
authors.lastname: Gomes
authors.forename: Dário
authors.initials: D
authors.lastname: Santos
authors.forename: Lidiane Cristina
authors.initials: LC
authors.lastname: Nunes
authors.forename: Gabriel Gustinelli Arantes
authors.initials: GG
authors.lastname: de Carvalho
authors.forename: Flávio de Oliveira
authors.initials: Fde O
authors.lastname: Leme
authors.forename: Francisco José
authors.initials: FJ
authors.lastname: Krug
mesh_terms: D053000:Analytic Sample Preparation Methods / Q000379:methods*; D007287:Inorganic Chemicals / Q000032:analysis; D007834:Lasers; D019684:Magnoliopsida / Q000737:chemistry*; D010316:Particle Size; D018515:Plant Leaves / Q000737:chemistry; D016062:Porosity; D013057:Spectrum Analysis / Q000379:methods*
chemical_list: D007287:Inorganic Chemicals