Author Pereira, E. R.

Different sample preparation methods for the analysis of suspension fertilizers combining LIBS and liquid-to-solid matrix conversion: determination of essential and toxic elements

Author: Andrade, D. F. ; et. al.

Journal: Analytical Methods (2017)

Applications Chemometrics

DOI: 10.1039/c7ay01049d

Authors
Pereira, E. R. ; Speranca, M. A.

Keywords

INDUCED BREAKDOWN SPECTROSCOPY; OPTICAL-EMISSION-SPECTROMETRY; TRACE-ELEMENTS; MICRONUTRIENTS; MEMBRANE; CADMIUM; WATER

Abstract

A novel calibration method was developed for the determination of macronutrients in suspension fertilizer samples by laser-induced breakdown spectroscopy(LIBS). The fertilizer samples were mixed with 10% m/v polyvinyl alcohol (PVA) and dried for approximately 2 h at 50 degrees C, resulting in a solid polymer film with the immobilized liquid sample. This study describes the use of LIBS and 12 normalization strategies to determine Cu, K, Mg, Mn and Zn as well as As, B, Ca, Cd, Cr, Fe, Na, P and Pb in suspension fertilizers by inductively coupled plasma optical emission spectrometry (ICP OES) and inductively coupled plasma mass spectrometry (ICP-MS) analyses. LIBS equipment parameters were chosen following optimization with a Doehlert design. The results clearly demonstrate a good agreement between the LIBS predicted concentrations and the reference concentrations determined by ICP OES after microwave-assisted acid digestion (AOAC 2006.03 Official Method). Correlations of R-2 = 0.9958, 0.9489, 0.9992, 0.9968 and 0.9809 for Cu, K, Mn, Mg and Zn, respectively, were obtained. Significant levels of potentially toxic elements such as 10 mg L-1 As, 4.0 mg L-1 Cd, 8.0 mg L-1 Cr and 20 mg L-1 Pb were detected after ICP-MS analysis. The results with low standard errors of prediction for LIBS (from 0.02 to 0.06%) indicate that this proposed suspension sample preparation procedure exhibits significant potential for the development and implementation of methods for determining essential nutrients in suspension fertilizers and other samples for which mineralization is difficult.

Area:

Agriculture ; Nutrition

Material:

Fertilizer

Elements:

Mg

Lines [nm]:

Mg II 279.55 nm Mg II 279.08 nm Mg II 279.80 nm Mg II 280.27 nm Mg I 285.21 nm Mg I 383.23 nm Mg I 383.83 nm Mg I 516.73 nm Mg I 517.27 nm Mg I 518.36 nm

K

Lines [nm]:

K I 766.49 nm K I 404.41 nm K I 404.72 nm K I 578.24 nm K I 580.17 nm K I 581.21 nm K I 583.19 nm K I 693.88 nm K I 691.11 nm K I 769.90 nm

Mn

Lines [nm]:

Mn II 257.61 nm Mn II 259.37 nm Mn II 260.57 nm Mn II 293.93 nm Mn II 294.92 nm Mn I 354.78 nm Mn I 356.95 nm Mn I 403.08 nm Mn I 403.31 nm Mn I 403.45 nm

Cu

Lines [nm]:

Cu I 324.75 nm Cu II 213.60 nm Cu II 219.57 nm Cu I 222.57 nm Cu I 224.43 nm Cu II 224.70 nm Cu II 236.99 nm Cu I 327.40 nm Cu I 521.82 nm Cu I 515.32 nm

Zn

Lines [nm]:

Zn I 213.86 nm Zn II 250.20 nm Zn II 255.80 nm Zn I 328.23 nm Zn I 330.26 nm Zn I 334.50 nm Zn I 468.01 nm Zn I 472.22 nm Zn I 481.05 nm Zn I 636.23 nm

Emmision lines:
Cu II 213.60 nm
Zn I 213.86 nm
Cu II 219.57 nm
Cu I 222.57 nm
Cu I 224.43 nm
Cu II 224.70 nm
Cu II 236.99 nm
Zn II 250.20 nm
Zn II 255.80 nm
Mn II 257.61 nm
Mn II 259.37 nm
Mn II 260.57 nm
Mg II 279.08 nm
Mg II 279.55 nm
Mg II 279.80 nm
Mg II 280.27 nm
Mg I 285.21 nm
Mn II 293.93 nm
Mn II 294.92 nm
Cu I 324.75 nm
Cu I 327.40 nm
Zn I 328.23 nm
Zn I 330.26 nm
Zn I 334.50 nm
Mn I 354.78 nm
Mn I 356.95 nm
Mg I 383.23 nm
Mg I 383.83 nm
Mn I 403.08 nm
Mn I 403.31 nm
Mn I 403.45 nm
K I 404.41 nm
K I 404.72 nm
Zn I 468.01 nm
Zn I 472.22 nm
Zn I 481.05 nm
Cu I 515.32 nm
Mg I 516.73 nm
Mg I 517.27 nm
Mg I 518.36 nm
Cu I 521.82 nm
K I 578.24 nm
K I 580.17 nm
K I 581.21 nm
K I 583.19 nm
Zn I 636.23 nm
K I 691.11 nm
K I 693.88 nm
K I 766.49 nm
K I 769.90 nm

Fast and direct detection of metal accumulation in marine sediments using laser-inducedbreakdown spectroscopy (LIBS): a case study from the Bay of Cienfuegos, Cuba

Author: Pena-Icart, M. ; et. al.

Journal: Analytical Methods (2017)

Applications Chemometrics

DOI: 10.1039/c7ay00578d

Authors
Alonso-Hernandez, C. ; Bolanos-Alvarez, Y. ; de Aquino, F. W. B. ; Pereira, E. R. ; Pomares-Alfonso, M. S.

Keywords

MULTIVARIATE-ANALYSIS; TRACE-METALS; CLASSIFICATION; POLLUTION; CHEMOMETRICS; COMBINATION; DIGESTION; SAMPLES

Abstract

Laser-induced breakdown spectroscopy (LIBS) is an emerging, multi-elemental and green technique, particularly suitable for the direct analysis of solid samples. In this study, thirty-two superficial sediments collected from Cienfuegos Bay in 2011-2013 were analyzed by LIBS without requiring sample digestion. Al, Ca, Fe, K, Mg, Mn, Na and Ti emission lines were detected in all samples. The full LIBS spectra of the samples were subjected to principal component analysis (PCA) and hierarchical cluster analysis (HCA). Most samples showed a similar emission signal pattern, whereas two samples collected in 2012 and another two in 2013 showed anomalously higher emission signals for Na, Mg and Ca, Mg, respectively. In three of the sediments, the impact of external factors on the ecosystem is the presumable cause of the observed anomalies. The combination of LIBS with multivariate data analysis demonstrated a high capacity for the fast detection of anomalous metal compositions in marine sediments.

Area:

Geology

Material:

Marine sediment

Elements:

Ca

Lines [nm]:

Ca I 616.22 nm Ca I 616.91 nm Ca II 393.37 nm Ca II 396.85 nm

Na

Lines [nm]:

Na I 589.00 nm Na I 589.59 nm

Mg

Lines [nm]:

Mg II 279.55 nm Mg I 280.98 nm

Al

Lines [nm]:

Al I 394.40 nm Al I 396.15 nm

Emmision lines:
Mg II 279.55 nm
Mg I 280.98 nm
Ca II 393.37 nm
Al I 394.40 nm
Al I 396.15 nm
Ca II 396.85 nm
Na I 589.00 nm
Na I 589.59 nm
Ca I 616.22 nm
Ca I 616.91 nm

Comparison of ICP OES and LIBS Analysis of Medicinal Herbs Rich in Flavonoids from Eastern Europe

Author: Andrade, D. F. ; et. al.

Journal: Journal of the Brazilian Chemical Society (2017)

Applications Chemometrics

DOI: 10.21577/0103-5053.20160236

Authors
Konieczynski, P. ; Pereira, E. R.

Keywords

medicinal herbs; essential and toxic metals; LIBS; ICP OES; chemometrics;INDUCED BREAKDOWN SPECTROSCOPY; PRINCIPAL COMPONENT ANALYSIS; TRACE-ELEMENTS; NEUTRON-ACTIVATION; INFUSIONS; INFORMATION; FINGERPRINT; CALCIUM; PLANTS; HONEY

Abstract

Essential and toxic metals were determined in eighteen samples of medicinal herbs from Poland, Lithuania and Serbia by means of laser-induced breakdownspectroscopy (LIBS) and inductively coupled plasma optical emission spectrometry (ICP OES). Calcium, K and Mg concentrations were obtained in % (m/m) and other metals (Na, Co, Cu, Fe, Mn, Ni, Zn, Cd, Cr and Pb) in mg kg-1. The fact that the herb samples analyzed belonged to specific plant species and represented different morphological plant parts explained the characteristic distribution in two-dimensional scores plots obtained by principal component analysis (PCA). A strong correlation of LIBS results was achieved in comparison to those obtained by ICP OES for Ca, K and Mg. Differences in the types of infusions were observed, in that leaves are related to Zn and Ni concentrations, leaves and flowers to Co, Ca and Mn concentrations and flowers to K, Na, Mg and Fe content.

Area:

Agriculture ; Health

Material:

Herb

Elements:

Ca

Lines [nm]:

Ca II 393.37 nm Ca II 396.85 nm Ca I 422.67 nm Ca I 527.03 nm Ca I 612.22 nm Ca I 616.22 nm Ca I 643.91 nm

Mg

Lines [nm]:

Mg II 279.55 nm Mg II 280.27 nm Mg I 285.21 nm Mg I 517.27 nm

K

Lines [nm]:

K II 396.67 nm K I 693.88 nm K I 766.49 nm K I 769.90 nm

N

Lines [nm]:

N I 821.63 nm N I 871.17 nm N I 868.34 nm

O

Lines [nm]:

O I 777.19 nm O I 844.64 nm

...

Emmision lines:
C I 247.86 nm
Mg II 279.55 nm
Mg II 280.27 nm
Mg I 285.21 nm
Ca II 393.37 nm
K II 396.67 nm
Ca II 396.85 nm
Ca I 422.67 nm
Mg I 517.27 nm
Ca I 527.03 nm
Ca I 612.22 nm
Ca I 616.22 nm
Ca I 643.91 nm
K I 693.88 nm
K I 766.49 nm
K I 769.90 nm
O I 777.19 nm
N I 821.63 nm
O I 844.64 nm
N I 868.34 nm
N I 871.17 nm

Identification and classification of polymer e-waste using laser-induced breakdownspectroscopy (LISS) and chemometric tools

Author: Costa, V. C. ; et. al.

Journal: Polymer Testing (2017)

Applications Chemometrics

DOI: 10.1016/j.polymertesting.2017.02.017

Authors
Aquino, F. W. B. ; Paranhos, C. M. ; Pereira, E. R.

Keywords

Laser-induced breakdown spectrometry; Polymers recycling; E-waste; Chemometrics;ELECTRONIC EQUIPMENT WEEE; MASS-SPECTROMETRY; PLASTICS; LIBS; INFORMATION; FRACTIONS; EFFICIENT

Abstract

In the recycling of polymer e-waste, there is a pressing need for rapid measurement technologies for the simple identification and classification of these materials. The goal of this work was to instantly identify e-waste polymers by laser-induced breakdown spectrometry (LIBS). The studied polymers were acrylonitrile-butadiene-styrene (ABS), polystyrene (PS), polyethylene (PE), polycarbonate (PC), polypropylene (PP), and polyamide (PA). Emission lines were selected for C (247), H (656), N (742 + 744 + 747), and 0 (777), as well as the molecular band of C2 (516), and the ratios of the emission lines and molecular band were utilized. Classification models, k-nearest neighbors (KNN) and soft independent modeling of class analogy (SIMCA), were used to rank the polymers. Both constructed models gave satisfactory results for the validation samples, with average accuracies of 98% for KNN and 92% for SIMCA. These results prove the predictive analytical capabilities of the LIBS technique for plastic identification and classification. (C) 2017 Elsevier Ltd. All rights reserved.

Area:

Industry

Material:

Polymer waste

Elements:

N

Lines [nm]:

N I 742.36 nm N I 744.23 nm N I 746.83 nm

O

Lines [nm]:

O I 777.19 nm O I 777.42 nm O I 777.54 nm

H

Lines [nm]:

H I 656.28 nm

C

Lines [nm]:

C I 247.86 nm

Emmision lines:
C I 247.86 nm
H I 656.28 nm
N I 742.36 nm
N I 744.23 nm
N I 746.83 nm
O I 777.19 nm
O I 777.42 nm
O I 777.54 nm

Quantitative analysis of Lead Zirconate Titanate (PZT) ceramics by laser-induced breakdownspectroscopy (LIBS) in combination with multivariate calibration

Author: Hernandez-Garcia, R. ; et. al.

Journal: Microchemical Journal (2017)

Applications Chemometrics

DOI: 10.1016/j.microc.2016.07.024

Authors
Aquino, F. W. B. ; Calderon-Pinar, F. ; Durruthy-Rodriguez, M. D. ; Pereira, E. R. ; Pomares-Alfonso, M. S. ; Villanueva-Tagle, M. E.

Keywords

Laser induced breakdown spectrometry; Partial Least Squares; PZT ceramics; Calibration strategies;ATOMIC EMISSION-SPECTROMETRY; ABSORPTION-SPECTROMETRY; CLASSIFICATION; CHEMOMETRICS

Abstract

In PZT (Lead Zirconate Titanate) ceramics, stoichiometric composition is closely related with physical properties and applications. Laser-induced BreakdownSpectroscopy (LIBS) have shown to be a suitable technique for analyzing many types of solid samples, usually in combination with multivariate techniques. In this study, a method for quick determination of Pb, Zr, Ti and Sr in PZT ceramics using LIBS was proposed. Spectral data is analyzed with PLS (Partial Least Squares), providing results better than Multiple Linear Regression (MLR) and external calibration, when compared with previous determination of the same group of ceramics by PIXE (Particle Induced X-ray Emission). Most of predicted individual concentrations were between 98 and 102% of the reference value for Pb, and between 90 and 110% for the rest of the elements. (C) 2016 Elsevier B.V. All rights reserved.

Area:

Industry

Material:

Ceramics

Elements:

Zr

Lines [nm]:

Zr I 468.78 nm Zr I 471.01 nm Zr I 477.23 nm Zr I 481.56 nm Zr II 274.26 nm

Pb

Lines [nm]:

Pb I 261.42 nm Pb I 280.20 nm Pb I 283.31 nm Pb I 405.78 nm Pb II 220.35 nm

Ti

Lines [nm]:

Ti I 498.17 nm Ti I 499.11 nm Ti I 499.95 nm Ti I 500.72 nm

Sr

Lines [nm]:

Sr I 460.73 nm Sr II 407.77 nm Sr II 421.55 nm

Emmision lines:
Pb II 220.35 nm
Pb I 261.42 nm
Zr II 274.26 nm
Pb I 280.20 nm
Pb I 283.31 nm
Pb I 405.78 nm
Sr II 407.77 nm
Sr II 421.55 nm
Sr I 460.73 nm
Zr I 468.78 nm
Zr I 471.01 nm
Zr I 477.23 nm
Zr I 481.56 nm
Ti I 498.17 nm
Ti I 499.11 nm
Ti I 499.95 nm
Ti I 500.72 nm

Author: Pereira, E. R.

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Co-author: Pereira, E. R.

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