Laser-induced breakdown spectroscopy (LIBS) for analysis of precious metals in minerals

The use of LIBS to quantify naturally-occurring gold and silver was investigated with the purpose of exploring its future application as an in situ and online monitoring technique for the precious metal mining industry. Two types of samples were prepared as pressed pellets and analyzed with conventi...

Full description

Autores:
Diaz Ordonez, Daniel Hernando
Tipo de recurso:
Doctoral thesis
Fecha de publicación:
2017
Institución:
Universidad Nacional de Colombia
Repositorio:
Universidad Nacional de Colombia
Idioma:
spa
OAI Identifier:
oai:repositorio.unal.edu.co:unal/60162
Acceso en línea:
https://repositorio.unal.edu.co/handle/unal/60162
http://bdigital.unal.edu.co/58180/
Palabra clave:
62 Ingeniería y operaciones afines / Engineering
Laser-induced breakdown spectroscopy
Gold ore
Gold
Silver
Conditional analysis
Principal component analysis
spectroscopia de plasma inducido por láser
Minerales de oro
Oro
Plata
Rights
openAccess
License
Atribución-NoComercial 4.0 Internacional
id UNACIONAL2_133169f5e495e69e2a0036843169f8b2
oai_identifier_str oai:repositorio.unal.edu.co:unal/60162
network_acronym_str UNACIONAL2
network_name_str Universidad Nacional de Colombia
repository_id_str
dc.title.spa.fl_str_mv Laser-induced breakdown spectroscopy (LIBS) for analysis of precious metals in minerals
title Laser-induced breakdown spectroscopy (LIBS) for analysis of precious metals in minerals
spellingShingle Laser-induced breakdown spectroscopy (LIBS) for analysis of precious metals in minerals
62 Ingeniería y operaciones afines / Engineering
Laser-induced breakdown spectroscopy
Gold ore
Gold
Silver
Conditional analysis
Principal component analysis
spectroscopia de plasma inducido por láser
Minerales de oro
Oro
Plata
title_short Laser-induced breakdown spectroscopy (LIBS) for analysis of precious metals in minerals
title_full Laser-induced breakdown spectroscopy (LIBS) for analysis of precious metals in minerals
title_fullStr Laser-induced breakdown spectroscopy (LIBS) for analysis of precious metals in minerals
title_full_unstemmed Laser-induced breakdown spectroscopy (LIBS) for analysis of precious metals in minerals
title_sort Laser-induced breakdown spectroscopy (LIBS) for analysis of precious metals in minerals
dc.creator.fl_str_mv Diaz Ordonez, Daniel Hernando
dc.contributor.advisor.spa.fl_str_mv Hahn, David (Thesis advisor)
dc.contributor.author.spa.fl_str_mv Diaz Ordonez, Daniel Hernando
dc.contributor.spa.fl_str_mv Molina Ochoa, Alejandro
dc.subject.ddc.spa.fl_str_mv 62 Ingeniería y operaciones afines / Engineering
topic 62 Ingeniería y operaciones afines / Engineering
Laser-induced breakdown spectroscopy
Gold ore
Gold
Silver
Conditional analysis
Principal component analysis
spectroscopia de plasma inducido por láser
Minerales de oro
Oro
Plata
dc.subject.proposal.spa.fl_str_mv Laser-induced breakdown spectroscopy
Gold ore
Gold
Silver
Conditional analysis
Principal component analysis
spectroscopia de plasma inducido por láser
Minerales de oro
Oro
Plata
description The use of LIBS to quantify naturally-occurring gold and silver was investigated with the purpose of exploring its future application as an in situ and online monitoring technique for the precious metal mining industry. Two types of samples were prepared as pressed pellets and analyzed with conventional LIBS setups: a) surrogate samples were prepared by doping gold-free matrices with Au and Ag standard solutions, and b) ore samples from a Colombian mine company containing naturally-occurring gold. The ore samples were extracted from underground locations and from a processing plant. The LIBS setups included Nd:YAG lasers (1064 and 355 nm), two Czerny-Turner spectrometers and ICCD detectors (1024×256 pixels). The net peak height, peak-to-base ratio and the background intensities were measured and compared to understand the influence of LIBS parameters on analytical results. From 100 to 5 000 sampling shots were fired over the pellets and an equal number of single-shot spectra were acquired. Single-shot as well as ensemble-averaged spectra were considered. LIBS performance was evaluated using calibration curves, limits of detection and quantification, relative standard deviation and coefficients of determination. Quantification of silver was achieved through conventional ensemble-average calculation and calibration curves. On the other hand, gold quantification was not possible with conventional LIBS spectra processing (ensemble-averaging). However, under specific conditions of sampling, spectra manipulation and the use of conditional analysis to improve gold detection and quantification, a semi-quantitative approach to quantify gold was developed. Finally, Principal Component Analysis was applied to the discrimination of single-shot spectra containing Au emission lines.
publishDate 2017
dc.date.issued.spa.fl_str_mv 2017-09-15
dc.date.accessioned.spa.fl_str_mv 2019-07-02T17:40:39Z
dc.date.available.spa.fl_str_mv 2019-07-02T17:40:39Z
dc.type.spa.fl_str_mv Trabajo de grado - Doctorado
dc.type.driver.spa.fl_str_mv info:eu-repo/semantics/doctoralThesis
dc.type.version.spa.fl_str_mv info:eu-repo/semantics/acceptedVersion
dc.type.coar.spa.fl_str_mv http://purl.org/coar/resource_type/c_db06
dc.type.content.spa.fl_str_mv Text
dc.type.redcol.spa.fl_str_mv http://purl.org/redcol/resource_type/TD
format http://purl.org/coar/resource_type/c_db06
status_str acceptedVersion
dc.identifier.uri.none.fl_str_mv https://repositorio.unal.edu.co/handle/unal/60162
dc.identifier.eprints.spa.fl_str_mv http://bdigital.unal.edu.co/58180/
url https://repositorio.unal.edu.co/handle/unal/60162
http://bdigital.unal.edu.co/58180/
dc.language.iso.spa.fl_str_mv spa
language spa
dc.relation.spa.fl_str_mv http://minas.medellin.unal.edu.co/gruposdeinvestigacion/biofrun/
dc.relation.ispartof.spa.fl_str_mv Universidad Nacional de Colombia Sede Medellín Facultad de Minas Escuela de Procesos y Energía
Escuela de Procesos y Energía
dc.relation.references.spa.fl_str_mv Diaz Ordonez, Daniel Hernando (2017) Laser-induced breakdown spectroscopy (LIBS) for analysis of precious metals in minerals. Doctorado thesis, Universidad Nacional de Colombia - Sede Medellín.
dc.rights.spa.fl_str_mv Derechos reservados - Universidad Nacional de Colombia
dc.rights.coar.fl_str_mv http://purl.org/coar/access_right/c_abf2
dc.rights.license.spa.fl_str_mv Atribución-NoComercial 4.0 Internacional
dc.rights.uri.spa.fl_str_mv http://creativecommons.org/licenses/by-nc/4.0/
dc.rights.accessrights.spa.fl_str_mv info:eu-repo/semantics/openAccess
rights_invalid_str_mv Atribución-NoComercial 4.0 Internacional
Derechos reservados - Universidad Nacional de Colombia
http://creativecommons.org/licenses/by-nc/4.0/
http://purl.org/coar/access_right/c_abf2
eu_rights_str_mv openAccess
dc.format.mimetype.spa.fl_str_mv application/pdf
institution Universidad Nacional de Colombia
bitstream.url.fl_str_mv https://repositorio.unal.edu.co/bitstream/unal/60162/1/13070440_2017.pdf
https://repositorio.unal.edu.co/bitstream/unal/60162/2/13070440_2017.pdf.jpg
bitstream.checksum.fl_str_mv 18779c8afaf7c9eae633a8ea3c5c84c4
dcf98410afe27c22db0d145acd93b35c
bitstream.checksumAlgorithm.fl_str_mv MD5
MD5
repository.name.fl_str_mv Repositorio Institucional Universidad Nacional de Colombia
repository.mail.fl_str_mv repositorio_nal@unal.edu.co
_version_ 1812169123117924352
spelling Atribución-NoComercial 4.0 InternacionalDerechos reservados - Universidad Nacional de Colombiahttp://creativecommons.org/licenses/by-nc/4.0/info:eu-repo/semantics/openAccesshttp://purl.org/coar/access_right/c_abf2Molina Ochoa, AlejandroHahn, David (Thesis advisor)f9822b64-bc1a-4424-8c14-039f0a928a20-1Diaz Ordonez, Daniel Hernandoe081be61-5ac4-4555-b8d8-2e39191cf4903002019-07-02T17:40:39Z2019-07-02T17:40:39Z2017-09-15https://repositorio.unal.edu.co/handle/unal/60162http://bdigital.unal.edu.co/58180/The use of LIBS to quantify naturally-occurring gold and silver was investigated with the purpose of exploring its future application as an in situ and online monitoring technique for the precious metal mining industry. Two types of samples were prepared as pressed pellets and analyzed with conventional LIBS setups: a) surrogate samples were prepared by doping gold-free matrices with Au and Ag standard solutions, and b) ore samples from a Colombian mine company containing naturally-occurring gold. The ore samples were extracted from underground locations and from a processing plant. The LIBS setups included Nd:YAG lasers (1064 and 355 nm), two Czerny-Turner spectrometers and ICCD detectors (1024×256 pixels). The net peak height, peak-to-base ratio and the background intensities were measured and compared to understand the influence of LIBS parameters on analytical results. From 100 to 5 000 sampling shots were fired over the pellets and an equal number of single-shot spectra were acquired. Single-shot as well as ensemble-averaged spectra were considered. LIBS performance was evaluated using calibration curves, limits of detection and quantification, relative standard deviation and coefficients of determination. Quantification of silver was achieved through conventional ensemble-average calculation and calibration curves. On the other hand, gold quantification was not possible with conventional LIBS spectra processing (ensemble-averaging). However, under specific conditions of sampling, spectra manipulation and the use of conditional analysis to improve gold detection and quantification, a semi-quantitative approach to quantify gold was developed. Finally, Principal Component Analysis was applied to the discrimination of single-shot spectra containing Au emission lines.Resumen: Con el propósito de explorar la aplicación de LIBS como una técnica de monitoreo in situ y en tiempo real de procesos de minería de metales preciosos se investigó su uso en la cuantificación de oro y plata en minerales naturales. Se analizaron dos tipos de muestras preparadas como comprimidos (pellets): a) sucedáneos que se obtuvieron dopando matrices libre de oro y plata con soluciones estándar de los dos elementos, y b) muestras de rocas provenientes de una mina colombiana. Los montajes experimentales de LIBS incluyeron láseres Nd:YAG (1064 y 355 nm), dos espectrómetros Czerny-Turner y detectores ICCD (1024×256 pixeles). Para determinar la influencia de los parámetros LIBS sobre los resultados analíticos se midió las intensidades de la altura de las líneas de emisión, el ruido y se el cociente de la altura de la emisión y el ruido. Las muestras se analizaron con entre 100 y 5 000 pulsos láser y se obtuvieron el mismo número de espectros LIBS individuales. Se estudiaron espectros individuales y promedio. El desempeño de LIBS se evaluó mediante curvas de calibración, límites de detección y cuantificación, valores de desviación estándar relativa y coeficientes de determinación. Se logró la cuantificación de plata mediante los procedimientos de cálculo de espectros promedio y curvas de calibración. Por otra parte, no fue posible cuantificar oro con los mismos métodos. Sin embargo, bajo ciertas condiciones de muestreo, tratamiento de espectros y el uso de análisis condicional para mejorar la detección y cuantificación, se desarrolló una metodología semi-cuantitativa para medir oro. Finalmente, la técnica de Análisis de Componentes Principales se aplicó para clasificar espectros individuales que contenían líneas de emisión de oro.Doctoradoapplication/pdfspahttp://minas.medellin.unal.edu.co/gruposdeinvestigacion/biofrun/Universidad Nacional de Colombia Sede Medellín Facultad de Minas Escuela de Procesos y EnergíaEscuela de Procesos y EnergíaDiaz Ordonez, Daniel Hernando (2017) Laser-induced breakdown spectroscopy (LIBS) for analysis of precious metals in minerals. Doctorado thesis, Universidad Nacional de Colombia - Sede Medellín.62 Ingeniería y operaciones afines / EngineeringLaser-induced breakdown spectroscopyGold oreGoldSilverConditional analysisPrincipal component analysisspectroscopia de plasma inducido por láserMinerales de oroOroPlataLaser-induced breakdown spectroscopy (LIBS) for analysis of precious metals in mineralsTrabajo de grado - Doctoradoinfo:eu-repo/semantics/doctoralThesisinfo:eu-repo/semantics/acceptedVersionhttp://purl.org/coar/resource_type/c_db06Texthttp://purl.org/redcol/resource_type/TDORIGINAL13070440_2017.pdfTesis de Doctorado en Ingeniería - Sistemas Energéticosapplication/pdf10834321https://repositorio.unal.edu.co/bitstream/unal/60162/1/13070440_2017.pdf18779c8afaf7c9eae633a8ea3c5c84c4MD51THUMBNAIL13070440_2017.pdf.jpg13070440_2017.pdf.jpgGenerated Thumbnailimage/jpeg5035https://repositorio.unal.edu.co/bitstream/unal/60162/2/13070440_2017.pdf.jpgdcf98410afe27c22db0d145acd93b35cMD52unal/60162oai:repositorio.unal.edu.co:unal/601622023-10-11 11:59:26.173Repositorio Institucional Universidad Nacional de Colombiarepositorio_nal@unal.edu.co