WO2017009528A1 - Procédé pour état d'observation de trajet optique en spectroscopie d'émission optique d'un échantillon et produit-programme informatique pour un dispositif de traitement - Google Patents

Procédé pour état d'observation de trajet optique en spectroscopie d'émission optique d'un échantillon et produit-programme informatique pour un dispositif de traitement Download PDF

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Publication number
WO2017009528A1
WO2017009528A1 PCT/FI2016/050504 FI2016050504W WO2017009528A1 WO 2017009528 A1 WO2017009528 A1 WO 2017009528A1 FI 2016050504 W FI2016050504 W FI 2016050504W WO 2017009528 A1 WO2017009528 A1 WO 2017009528A1
Authority
WO
WIPO (PCT)
Prior art keywords
sample
ratio
time
emission line
plasma
Prior art date
Application number
PCT/FI2016/050504
Other languages
English (en)
Inventor
Lauri KÖRESAAR
Björn SALMI
Arto OLLIKAINEN
Original Assignee
Outotec (Finland) Oy
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Outotec (Finland) Oy filed Critical Outotec (Finland) Oy
Priority to AU2016293213A priority Critical patent/AU2016293213B2/en
Priority to CA2991462A priority patent/CA2991462A1/fr
Priority to BR112018000233A priority patent/BR112018000233A2/pt
Publication of WO2017009528A1 publication Critical patent/WO2017009528A1/fr
Priority to ZA2018/00363A priority patent/ZA201800363B/en

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
    • G01N21/718—Laser microanalysis, i.e. with formation of sample plasma
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01—Arrangements or apparatus for facilitating the optical investigation
    • G01N21/15—Preventing contamination of the components of the optical system or obstruction of the light path
    • G01N2021/155—Monitoring cleanness of window, lens, or other parts
    • G01N2021/157—Monitoring by optical means
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/85—Investigating moving fluids or granular solids
    • G01N2021/8592—Grain or other flowing solid samples
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/66—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
    • G01N21/68—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence using high frequency electric fields
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/85—Investigating moving fluids or granular solids

Definitions

  • the invention relates to a method for observation state of optical path in optical emission spectroscopy of a sample as defined in the preamble of independent claim 1.
  • Figure 8 shows steps of a computer program product according to an embodiment
  • Figure 9 shows intensity ratio as a function of time for clean window and contaminated window as well as warning and alarm limit lines.
  • the invention relates to a method for observation state of optical path in optical emission spectroscopy of a sample, to computer program product for a processing device, and to the use of the method and of the computer program product in a method or in an apparatus for on-stream measurement of elemental concentrations in slurries for observing cleanliness of a window between a fluid sample flow of a slurry and a spectrometer of a spectroscopy system of the apparatus for on-stream measurement of elemental concentrations in slurries.
  • optical path is in this context meant the path of the light emitted by the plasma in the sample from the plasma to the spectrometer of the spectroscopy system.
  • the method can be for example used for observation state of optical path in optical emission spectroscopy of a sample in Inductively Coupled Plasma optical emission spectrophotometer (ICP-OES) apparatuses, as shown in figure 1, and arc spark optical emission spectrophotometer (Arc Spark OES) apparatuses, as shown in figure 2.
  • ICP-OES Inductively Coupled Plasma optical emission spectrophotometer
  • Arc Spark OES arc spark optical emission spectrophotometer
  • the method comprises providing a sample 1.
  • the method comprises applying electromagnetic energy 5 from a source 2 of electromagnetic energy 5 onto a surface 3 of the sample 1 to induce a plasma 4 in the sample 1.
  • the method comprises a first receiving step for receiving light 6 emitted by the induced plasma 4 for spectrum analysis with a spectrometer 7 of a spectroscopy system 8 at a time 1, wherein the spectrometer 7 is separated from the sample 1 by means of a window 9.
  • the method comprises a first analyzing step for analyzing the spectrum of light 6 emitted by the induced plasma 4 at time 1 to generate a first emission line (not marked with a reference numeral) for an element contained in the sample 1 at a first wavelength region and a second emission line (not marked with a reference numeral) for the element contained in the sample 1 at a second wavelength region that is more than 20 nm, preferably more than 100 nm, from the first wavelength region.
  • the method comprises a second receiving step for receiving light 6 emitted by the induced plasma 4 for spectrum analysis with the spectrometer 7 of the spectroscopy system 8 at a time 2 that is later than time 1.
  • the method comprises a second analyzing step for analyzing the spectrum of light 6 emitted by the induced plasma 4 at time 2 to generate a subsequent first emission line (not marked with a reference numeral) for the element contained in the sample 1 at the first wavelength region and a subsequent second emission line (not marked with a reference numeral) for the element contained in the sample 1 at the second wavelength region.
  • the method comprises a calculating step for (i) calculating a first ratio between the first emission line generated in the first analyzing step and the second emission line generated in the first analyzing step and for (ii) calculating a second ratio between the subsequent first emission line generated in the second analyzing step and the subsequent second emission line generated in the second analyzing step and for (iii) calculating a difference between the first ratio and the second ratio, to obtain a calculated intensity difference, the calculated intensity difference being indicative of cleanliness of the window 9.
  • the difference between the first ratio and the second ratio can be the absolute difference between the first ratio and the second ratio.
  • the difference between the first ratio and the second ratio can be the relative difference between the first ratio and the second ratio
  • the first ratio is preferably, but not necessarily, calculated for light 6 emitted by the induced plasma 4 and received by the spectrometer 7 of the spectroscopy system 8 through the window 9 in a state where the window 9 is considered to be clean.
  • the method may include repeating the second receiving step, the second analyzing step, and the calculating step, and following the calculated intensity difference between the first ratio and the second ratio as a function of time.
  • the first ratio is preferably, but not necessarily, calculated only once for light 6 emitted by the induced plasma 4 and received by the spectrometer 7 of the spectroscopy system 8 through the window 9 in a state where the window 9 is considered to be clean
  • a second ratio is preferably, but not necessarily, calculated several times during the process so that following of a trend of the calculated intensity difference between the first ratio and the second ratio as a function of time is possible.
  • Figure 5 shows calculated intensity difference in the form of calculated intensity ratio between a first ratio and a second ratio as a function of time. If the calculated intensity ratio between the first ratio and the second ratio is calculated at a time, when the window 9 is considered to be clean, by calculating a subsequent second ratio and a subsequent intensity ratio between the first ratio and the subsequent second ratio, cleanliness of the window 9 can be followed by following the line. If the line in the chart is about horizontal, the window is clean, but if the line in the chart starts to go up (or down), dirt has started to build up on the window 9. In figure 9, this has been illustrated in another way.
  • the electromagnetic energy 5 used for inducing plasma 4 at time 1 is preferably, but not necessarily, the same as the electromagnetic energy 5 used for inducing plasma 4 as at time 2.
  • the method may include using any one of the following as the source 2 of electromagnetic energy: a laser such as a Nd:YAG laser, an arc spark generator, and a high frequency coil.
  • a laser such as a Nd:YAG laser
  • an arc spark generator and a high frequency coil.
  • the method comprises preferably providing transfer optics between the window 9 and the spectrometer which is preferably, but not necessarily, an Echelle spectrograph as shown in figure 2.
  • the method may include cleaning the window 9 if the calculated intensity difference exceeds a threshold value, which can be a warning limit or an alarm limit as shown in figure 9.
  • a threshold value which can be a warning limit or an alarm limit as shown in figure 9.
  • light 6 may be lead from the plasma 4 to the spectrometer 7 of the spectroscopy system 8 in gas (not marked with a reference numeral).
  • light 6 may be lead from the plasma 4 to the spectrometer 7 of the spectroscopy system 8 in vacuum (not marked with a reference numeral).
  • light 6 may be lead from the plasma 4 to the spectrometer 7 of the spectroscopy system 8 without using optical fibers (not shown).
  • the first wavelength region, where the first emission line is generated at is preferably, but not necessarily, between 190 and 250 nm.
  • the second wavelength region, where the second emission line is generated at is preferably, but not necessarily, between 350 and 700 nm, more preferably between 350 and 500 nm.
  • the source 2 of electromagnetic energy which is used in the method, is preferably, but not necessarily, separated from the sample 1 by means of the window 9, as shown in figure 1.
  • the element contained in the sample 1 is preferably, but not necessarily, one of the following: Silicon, Calcium, Carbon, Aluminum, and a transition metal such as Scandium, Titanium, Vanadium, Chromium, Manganese, Iron, Cobalt, Nickel, Copper, Zinc, Yttrium, Zirconium, Niobium, Molybdenum, Ruthenium, Rhodium, Palladium, Silver, Cadmium, Hafnium, Tantalum, Tungsten, Rhenium, Osmium, Iridium, Platinum, Gold, and Mercury.
  • a transition metal such as Scandium, Titanium, Vanadium, Chromium, Manganese, Iron, Cobalt, Nickel, Copper, Zinc, Yttrium, Zirconium, Niobium, Molybdenum, Ruthenium, Rhodium, Palladium, Silver, Cadmium, Hafnium, Tantalum, Tungsten, Rhenium, Osmium, Iridium, Platinum, Gold, and Mercury.
  • the sample 1 that is provided in the method is preferably, but not necessarily, in the form of a fluid sample flow, and the fluid sample flow through a flow cell 10, and electromagnetic energy 5 is applied to the surface 3 of the fluid sample flow in the flow cell 10 as the fluid sample flow flows through the flow cell 10.
  • the spectrometer 7 of the spectroscopy system 8, which is used in the method is in such case preferably, but not necessarily, separated from the flow cell 10 by means of the window 9.
  • the source 2 of electromagnetic energy, which is used in the method is in such case preferably, but not necessarily, separated from the flow cell 10 by means of the window 9.
  • the fluid sample flow has preferably, but not necessarily, a solid concentration between 10 and 60 % in percentages of weight, the balance being preferably, but not necessarily, liquid. If the sample 1 at time 1 is in the form of a fluid sample flow and if the sample 1 at time 2 is in the form of a fluid sample flow, it follows that the sample 1 at time is different than the sample 1 at time 2.
  • the element which is contained in the sample 1 in the form of a fluid sample flow at time 1, and which is analyzed in the first analyzing step by generating a first emission line and a second emission line for the element, is the same element as the element, which is contained in the sample 1 in the form of a fluid sample flow at time 2, and which is analyzed in the second analyzing step by generating a subsequent first emission line and a subsequent second emission line for the element.
  • the computer program comprising code for:
  • the calculated intensity difference being indicative of cleanliness of a window 9 between the sample 1 and the spectrometer 7 of the spectroscopy system 8.

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  • Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Biochemistry (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Plasma & Fusion (AREA)
  • Optics & Photonics (AREA)
  • Engineering & Computer Science (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)

Abstract

L'invention concerne un procédé pour l'état d'observation d'un trajet optique en spectroscopie d'émission optique d'un échantillon (1). Le procédé comprend une étape de calcul consistant à (i) calculer un premier rapport entre une première ligne d'émission générée dans une première étape d'analyse et une seconde ligne d'émission générée dans une première étape d'analyse et consistant à (ii) calculer un second rapport entre une première ligne d'émission ultérieure générée dans une seconde étape d'analyse et une seconde ligne d'émission générée dans une seconde étape d'analyse et consistant à (iii) calculer une différence entre le premier rapport et le second rapport afin d'obtenir une différence d'intensité calculée, la différence d'intensité calculée étant indicative de la propreté du chemin optique. L'invention concerne également un produit-programme informatique pour un dispositif de traitement.
PCT/FI2016/050504 2015-07-10 2016-07-08 Procédé pour état d'observation de trajet optique en spectroscopie d'émission optique d'un échantillon et produit-programme informatique pour un dispositif de traitement WO2017009528A1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
AU2016293213A AU2016293213B2 (en) 2015-07-10 2016-07-08 Method for observation state of optical path in optical emission spectroscopy of a sample and computer program product for a processing device
CA2991462A CA2991462A1 (fr) 2015-07-10 2016-07-08 Procede pour etat d'observation de trajet optique en spectroscopie d'emission optique d'un echantillon et produit-programme informatique pour un dispositif de traitement
BR112018000233A BR112018000233A2 (pt) 2015-07-10 2016-07-08 método para o estado de observação de trajeto óptico em espectroscopia de emissão óptica de uma amostra e produto de programa de computador para um dispositivo de processamento
ZA2018/00363A ZA201800363B (en) 2015-07-10 2018-01-18 Method for observation state of optical path in optical emission spectroscopy of a sample and computer program product for a processing device

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FI20155546 2015-07-10
FI20155546A FI20155546A (fi) 2015-07-10 2015-07-10 Menetelmä optisen tien tilan valvomiseksi näytteen optisessa säteilyspektroskooppiassa ja tietokoneohjelma prosessointilaitetta varten

Publications (1)

Publication Number Publication Date
WO2017009528A1 true WO2017009528A1 (fr) 2017-01-19

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PCT/FI2016/050504 WO2017009528A1 (fr) 2015-07-10 2016-07-08 Procédé pour état d'observation de trajet optique en spectroscopie d'émission optique d'un échantillon et produit-programme informatique pour un dispositif de traitement

Country Status (6)

Country Link
AU (1) AU2016293213B2 (fr)
BR (1) BR112018000233A2 (fr)
CA (1) CA2991462A1 (fr)
FI (1) FI20155546A (fr)
WO (1) WO2017009528A1 (fr)
ZA (1) ZA201800363B (fr)

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002048683A2 (fr) * 2000-11-21 2002-06-20 Applied Materials, Inc. Procede et dispositif faisant appel a la spectroscopie d'emission optique pour la detection d'un defaut dans les conditions de traitement d'un semi-conducteur
DE102006028250A1 (de) * 2006-06-20 2007-12-27 Carl Zeiss Microimaging Gmbh Verfahren zur Überwachung von Laserbearbeitungsprozessen
US20080160618A1 (en) * 2005-02-28 2008-07-03 Commissariat A L'energie Atomique Method And System For Physicochemical Analysis Using A Laser Pulsed Ablation
US20090015824A1 (en) * 2007-07-09 2009-01-15 Gary Shubinsky Optical Multiwavelength Window Contamination Monitor for Optical Control Sensors and Systems
JP2013036779A (ja) * 2011-08-04 2013-02-21 Toshiba Corp レーザー誘起ブレークダウン分光分析装置
WO2015082752A1 (fr) * 2013-12-02 2015-06-11 Outotec (Finland) Oy Procédé et appareil d'analyse en ligne par spectroscopie induite par laser

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002048683A2 (fr) * 2000-11-21 2002-06-20 Applied Materials, Inc. Procede et dispositif faisant appel a la spectroscopie d'emission optique pour la detection d'un defaut dans les conditions de traitement d'un semi-conducteur
US20080160618A1 (en) * 2005-02-28 2008-07-03 Commissariat A L'energie Atomique Method And System For Physicochemical Analysis Using A Laser Pulsed Ablation
DE102006028250A1 (de) * 2006-06-20 2007-12-27 Carl Zeiss Microimaging Gmbh Verfahren zur Überwachung von Laserbearbeitungsprozessen
US20090015824A1 (en) * 2007-07-09 2009-01-15 Gary Shubinsky Optical Multiwavelength Window Contamination Monitor for Optical Control Sensors and Systems
JP2013036779A (ja) * 2011-08-04 2013-02-21 Toshiba Corp レーザー誘起ブレークダウン分光分析装置
WO2015082752A1 (fr) * 2013-12-02 2015-06-11 Outotec (Finland) Oy Procédé et appareil d'analyse en ligne par spectroscopie induite par laser

Also Published As

Publication number Publication date
CA2991462A1 (fr) 2017-01-19
BR112018000233A2 (pt) 2018-09-04
AU2016293213A1 (en) 2018-02-08
AU2016293213B2 (en) 2018-11-29
ZA201800363B (en) 2019-08-28
FI20155546A (fi) 2017-01-11

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