AU2016293213A1 - Method for observation state of optical path in optical emission spectroscopy of a sample and computer program product for a processing device - Google Patents
Method for observation state of optical path in optical emission spectroscopy of a sample and computer program product for a processing device Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 79
- 238000004590 computer program Methods 0.000 title claims abstract description 31
- 230000003287 optical effect Effects 0.000 title claims abstract description 18
- 238000001636 atomic emission spectroscopy Methods 0.000 title claims abstract description 14
- 238000012545 processing Methods 0.000 title claims abstract description 10
- 230000003749 cleanliness Effects 0.000 claims abstract description 11
- 238000004611 spectroscopical analysis Methods 0.000 claims description 31
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- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 2
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- 229910052763 palladium Inorganic materials 0.000 claims description 2
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- 229910052702 rhenium Inorganic materials 0.000 claims description 2
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- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
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- 229910052726 zirconium Inorganic materials 0.000 claims description 2
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Classifications
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- 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
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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)
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- General Health & Medical Sciences (AREA)
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- Plasma & Fusion (AREA)
- Optics & Photonics (AREA)
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention relates to a method for observation state of optical path in optical emission spectroscopy of a sample (1). The method comprises a calculating step for (i) calculating a first ratio between a first emission line generated in a first analyzing step and a second emission line generated in a first analyzing step and for (ii) calculating a second ratio between a subsequent first emission line generated in a second analyzing step and a subsequent second emission line generated in a 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 optical path. The invention relates also to a computer program product for a processing device.
Description
METHOD FOR OBSERVATION STATE OF OPTICAL PATH IN OPTICAL EMISSION SPECTROSCOPY OF A SAMPLE AND COMPUTER PROGRAM PRODUCT FOR A PROCESSING DEVICE
Field of the invention
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.
The invention also relates to computer program product for a processing device as defined in claim 22.
Atomic/optical emission spectroscopy is a method to measure the presence or quantity of an element in a sample. By means of a source for electromagnetic energy such as a laser, plasma is induced in the sample and electrons in an element are excited to a higher level, and as the electrons decay back to a lower energy level they emit photons at a characteristic wavelength. Light i.e. photons emitted by the plasma are received and analyzed in a spectroscopy system. The wavelength is proportional to the energy difference between the exited state and the state it decays to. The measured intensity is proportional to the concentration of the measured element in the plasma, the atomic parameters of the measured transition including the transition probability and the energy of the excited state, and parameter of the plasma including electron density and temperature.
Atomic/optical emission spectroscopy can for example be used for to measure the presence or quantity of an element / elements in sample in the form of a fluid sample flow.
In online applications, it is advantageous to use a window between the source for electronic energy and the sample and between the spectroscopy system and the sample to prevent contamination of the source for electronic energy and of sensitive optics of the spectroscopy system. The window needs to have high transmission in all wavelengths used in the measurement in order to ensure maximum light collection by the spectroscopy system. If the window is contaminated the measured intensity is scattered or absorbed by the window. The contamination might not be visually observed. The decrease in intensities is usually not linear across the all wavelengths used in the measurement, but intensities in shorter wavelength UV-regions decrease faster if the window is contaminated.
The non-linear decrease in intensities across wavelengths will affect the calibration of the apparatus. Contaminated window will produce false analysis results. The calibration process itself is time consuming and expensive, and recalibration should be avoided whenever possible. The current method for observing window cleanliness is by visual observation.
Objective of the invention
The object of the invention is to provide an easy and reliable method for validation of the measurement results and for observing the state of the optical path.
Short description of the invention
The method for observation state of optical path in optical emission spectroscopy of a sample of the invention is characterized by the definitions of independent claim 1.
Preferred embodiments of the method are defined in the dependent claims 2 to 21.
The computer program product for a processing device of the invention is correspondingly characterized by the definitions of independent claim 22.
Preferred embodiments of the computer program product are defined in the dependent claims 23 to 25.
The invention relates also to the use of the method according to any of the claims 1 to 21 or to the use of the computer program product according to any of the claims 22 to 25 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.
An advantage of the method and of the computer program product is that they enable observation state of optical path in optical emission spectroscopy of a sample on-line without the need of performing any prior reference measurements for example with an absolutely clean window or without a window between the sample and the spectrometer.
Another advantage of the method and of the computer program product is that the observation state of optical path can be started and performed at the same time as the normal analyzing of a sample is performed.
List of figures
In the following the invention will described in more detail by referring to the figures, of which
Figure 1 shows in schematic side-view illustration a first embodiment of an arrangement for carrying out the method,
Figure 2 shows in schematic side-view illustration a second embodiment of an arrangement for carrying out the method,
Figure 3 shows with a solid line spectroscopic data in a situation where the window is clean and with a dotted line spectroscopic data in a situation where the window is contaminated,
Figure 4 shows calculated intensity difference of contaminated/clean window in percentages % as a function of wavelength,
Figure 5 shows calculated intensity difference in the form of calculated intensity ratio as a function of time,
Figure 6 shows an embodiment of a processing device,
Figure 7 shows in schematic side-view illustration a third embodiment of an arrangement for carrying out the method,
Figure 8 shows steps of a computer program product according to an embodiment, and
Figure 9 shows intensity ratio as a function of time for clean window and contaminated window as well as warning and alarm limit lines.
Detailed description of the invention
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.
By the definition “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.
First the method for observation state of optical path in optical emission spectroscopy of a sample 1 will be described in greater detail.
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
In the method, 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. In the method, 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, and 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.
The method according may include repeating the second receiving step, the second analyzing step, and the calculating step at regular time intervals, and following the calculated intensity difference between the first ratio and the second ratio as a function of time.
The method may comprise creating charts as shown in figures 4, 5, and 9.
Figure 4 shows calculated intensity difference of contaminated/clean window in percentages as a function of wavelength. When some time has lapsed and dirt starts to build up on the window 9, the calculated intensity difference increases and figure 4 shows that the drop in intensity is not linear, but that the intensity drops more for short wavelength than for long wave lengths.
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 electromagnetic energy 5 used for inducing plasma 4 between time 1 and for inducing plasma 4 at time 2 is preferably the same as the electromagnetic energy 5 used for inducing plasma 4 at time 1 and for inducing plasma 4 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.
In case the method included using an arc spark generator as the source 2 of electromagnetic energy, 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 replacing 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.
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.
In the method, 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).
In the method, 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).
In the method, 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.
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.
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, 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.
Next the computer program product for a processing device will be described in greater detail.
The computer program comprising code for: receiving a first electric signal representing at a time 1 light 6 emitted by plasma 4 induced in a sample 1 and received by a spectrometer 7 of a spectroscopy system 8, analyzing the spectrum of light 6 emitted by the induced plasma 4 at time 1 to generate a first emission line for the an element contained in the sample 1 at a first wavelength region and a second emission line for the element contained in the sample 1 at a second wavelength region that is more than 20 nm from the first wavelength region, receiving a first electric signal representing at a time 2, which is later than time 1, light 6 emitted by plasma 4 induced in the sample 1 and received by the spectrometer 7 of the spectroscopy system 8, analyzing the spectrum of light 6 emitted by the induced plasma 4 at time 2 to generate a subsequent first emission line for the element contained in the sample 1 at the first wavelength region and a subsequent second emission line for the element contained in the sample 1 at the second wavelength region, calculating a first ratio between the first emission line and the second emission line, calculating a second ratio between the subsequent first emission line and the subsequent second emission line, and 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 a window 9 between the sample 1 and the spectrometer 7 of the spectroscopy system 8.
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 computer program product comprising preferably, but not necessarily, additionally code for 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 computer program product comprising preferably, but not necessarily, additionally code for repeating the second receiving step, the second analyzing step, and the calculating step at regular time intervals, and following the calculated intensity difference between the first ratio and the second ratio as a function of time.
The computer program product comprising preferably, but not necessarily, additionally code for generating the first emission line at a first wavelength region between 190 and 250 nm.
The computer program product comprising preferably, but not necessarily, additionally code for generating the second emission line at a second wavelength region between 350 and 700 nm, preferably between 350 and 500 nm.
The computer program product comprising preferably, but not necessarily, additionally code for generating a control signal for a process controller to generate a signal indicative of a state of an optical path.
The processing device 11 may include a communications module 12 for sending and receiving signals, a memory 13 for storing the computer program 16, and a processor 15 for executing the computer program 16.
The invention relates also to the use of the method or 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 9 between a fluid sample flow of a slurry and a spectrometer 7 of a spectroscopy system 8 of the apparatus for on-stream measurement of elemental concentrations in slurries.
It is apparent to a person skilled in the art that as technology advances, the basic idea of the invention can be implemented in various ways. The invention and its embodiments are therefore not restricted to the above examples, but they may vary within the scope of the claims.
Claims (26)
- Claims1. A method for observation state of optical path in optical emission spectroscopy of a sample (1), wherein the method comprising: providing a sample (1), applying electromagnetic energy (5) from a source (2) of electromagnetic energy onto a surface (3) of the sample (1) to induce plasma (4) in the sample (1), 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), and 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 for an element contained in the sample (1) at a first wavelength region and a second emission line for the element contained in the sample (1) at a second wavelength region that is more than 20 nm from the first wavelength region, characterized by 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, by 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 for the element contained in the sample (1) at the first wavelength region and a subsequent second emission line for the element contained in the sample (1) at the second wavelength region, by 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), and by one of replacing and cleaning the window (9) if the calculated intensity difference exceeds a threshold value.
- 2. The method according to claim 1, characterized by repeating the second receiving step, the second analyzing step, and the calculating step, and by following the calculated intensity difference between the first ratio and the second ratio as a function of time.
- 3. The method according to claim 1, characterized by repeating the second receiving step, the second analyzing step, and the calculating step at regular time intervals, and by following the calculated intensity difference between the first ratio and the second ratio as a function of time.
- 4. The method according to any of the claims 1 to 3, characterized by the electromagnetic energy (5) used for inducing plasma (4) at time 1 being the same as the electromagnetic energy (5) used for inducing plasma (4) at time 2.
- 5. The method according to any of the claims 1 to 4, characterized by the electromagnetic energy (5) used for inducing plasma (4) between time 1 and for inducing plasma (4) at time 2 being the same as the electromagnetic energy (5) used for inducing plasma (4) at time 1 and for inducing plasma (4) at time 2.
- 6. The method according to any of the claims 1 to 5, characterized by 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.
- 7. The method according to any of the claims 1 to 6, characterized by leading light (6) from the plasma (4) to the spectrometer (7) of the spectroscopy system (8) in gas.
- 8. The method according to any of the claims 1 to 6, characterized by leading light (6) from the plasma (4) to the spectrometer (7) of the spectroscopy system (8) in vacuum.
- 9. The method according to any of the claims 1 to 8, characterized by leading light (6) from the plasma (4) to the spectrometer (7) of the spectroscopy system (8) without using optical fibers.
- 10. The method according to any of the claims 1 to 9, characterized by the first wavelength region, where the first emission line is generated at, is between 190 and 250 nm.
- 11. The method according to any of the claims 1 to 10, characterized by the second wavelength region, where the second emission line is generated at, is between 350 and 700 nm, preferably between 350 and 500 nm.
- 12. The method according to any of the claims 1 to 11, characterized by the source (2) of electromagnetic energy, which is used in the method, is separated from the sample (1) by means of the window (9).
- 13. The method according to any of the claims 1 to 12, characterized by the element contained in the sample (1) being 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.
- 14. The method according to any of the claims 1 to 13, characterized by providing the sample (1) in the form of a fluid sample flow, and by passing the fluid sample flow through a flow cell (10).
- 15. The method according to claim 14, characterized by the spectrometer (7) of the spectroscopy system (8), which is used in the method, is separated from the flow cell (10) by means of the window (9).
- 16. The method according to claim 14 or 15, characterized by the source (2) of electromagnetic energy, which is used in the method, is separated from the flow cell (10) by means of the window (9).
- 17. The method according to any of the claims 14 to 16, characterized by the fluid sample flow having a solid concentration between 10 and 60 % in percentages of weight.
- 18. The method according to any of the claims 14 to 17, characterized by the sample (1) at time 1 being in the form of a fluid sample flow and by the sample (1) at time 2 being in the form of a fluid sample flow, whereby the sample (1) at time being different than the sample (1) at time 2.
- 19. The method according to any of the claims 14 to 18, characterized by the element that is contained in the sample (1) in the form of a fluid sample flow at time 1 and that is analyzed in the first analyzing step by generating a first emission line and a second emission line for the element being the same as the element that is contained in the sample (1) in the form of a fluid sample flow at time 2 and that is analyzed in the second analyzing step by generating a subsequent first emission line and a subsequent second emission line for the element.
- 20. The method according to any of the claims 1 to 19, characterized by the difference between the first ratio and the second ratio is the absolute difference between the first ratio and the second ratio.
- 21. The method according to any of the claims 1 to 19, characterized by the difference between the first ratio and the second ratio is the relative difference between the first ratio and the second ratio.
- 22. A computer program product for a processing device, the computer program comprising code for: receiving a first electric signal representing at a time 1 light (6) emitted by plasma (4) induced in a sample (1) and received by a spectrometer (7) of a spectroscopy system (8), analyzing the spectrum of light (6) emitted by the induced plasma (4) at time 1 to generate a first emission line for the an element contained in the sample (1) at a first wavelength region and a second emission line for the element contained in the sample (1) at a second wavelength region that is more than 20 nm from the first wavelength region, receiving a first electric signal representing at a time 2, which is later than time 1, light (6) emitted by plasma (4) induced in the sample (1) and received by the spectrometer (7) of the spectroscopy system (8), analyzing the spectrum of light (6) emitted by the induced plasma (4) at time 2 to generate a subsequent first emission line for the element contained in the sample (1) at the first wavelength region and a subsequent second emission line for the element contained in the sample (1) at the second wavelength region, calculating a first ratio between the first emission line and the second emission line, calculating a second ratio between the subsequent first emission line and the subsequent second emission line, and 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 a window (9) between the sample (1) and the spectrometer (7) of the spectroscopy system (8).
- 23. The computer program product according to claim 22, by the computer program product comprising additionally code for: 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.
- 24. The computer program product according to claim 22 or 23, by the computer program product comprising additionally code for: repeating the second receiving step, the second analyzing step, and the calculating step at regular time intervals, and following the calculated intensity difference between the first ratio and the second ratio as a function of time.
- 25. The computer program product according to any of the claims 20 to 24, by the computer program product comprising additionally code for: generating a control signal for a process controller to generate a signal indicative of a state of an optical path.
- 26. Use of the method according to any of the claims 1 to 19 or of the computer program product according to any of the claims 20 to 25 in a method or in an apparatus for on-stream measurement of elemental concentrations in slurries for observing cleanliness of a window (9) between a fluid sample flow of a slurry and a spectrometer (7) of a spectroscopy system (8) of the apparatus for on-stream measurement of elemental concentrations in slurries.
Applications Claiming Priority (3)
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|---|---|---|---|
| FI20155546A FI20155546A (en) | 2015-07-10 | 2015-07-10 | METHOD FOR MONITORING THE OPTICAL ROAD STATUS IN THE OPTICAL RADIATION SPECTROSCOPY OF THE SAMPLE AND A COMPUTER PROGRAM FOR THE PROCESSING DEVICE |
| FI20155546 | 2015-07-10 | ||
| PCT/FI2016/050504 WO2017009528A1 (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 |
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| AU2016293213A1 true AU2016293213A1 (en) | 2018-02-08 |
| AU2016293213B2 AU2016293213B2 (en) | 2018-11-29 |
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| US6603538B1 (en) * | 2000-11-21 | 2003-08-05 | Applied Materials, Inc. | Method and apparatus employing optical emission spectroscopy to detect a fault in process conditions of a semiconductor processing system |
| FR2882593B1 (en) * | 2005-02-28 | 2007-05-04 | Commissariat Energie Atomique | METHOD AND SYSTEM FOR PHYSICOCHEMICAL ANALYSIS USING PULSE LASER ABLATION |
| DE102006028250A1 (en) * | 2006-06-20 | 2007-12-27 | Carl Zeiss Microimaging Gmbh | Monitoring laser welding processes with or without spontaneous plasma zone formation, images optical radiation from processing region, analyzes spectrally and evaluates |
| US7948617B2 (en) * | 2007-07-09 | 2011-05-24 | Fluke Corporation | Optical multiwavelength window contamination monitor for optical control sensors and systems |
| JP2013036779A (en) * | 2011-08-04 | 2013-02-21 | Toshiba Corp | Laser-induced breakdown spectral analyzer |
| CA2931919C (en) * | 2013-12-02 | 2021-05-04 | Outotec (Finland) Oy | Method and apparatus for online analysis by laser-induced spectroscopy |
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| BR112018000233A2 (en) | 2018-09-04 |
| FI20155546A (en) | 2017-01-11 |
| CA2991462A1 (en) | 2017-01-19 |
| ZA201800363B (en) | 2019-08-28 |
| AU2016293213B2 (en) | 2018-11-29 |
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