CA2490420A1 - Method and apparatus for molten material analysis by laser induced breakdown spectroscopy - Google Patents
Method and apparatus for molten material analysis by laser induced breakdown spectroscopy Download PDFInfo
- Publication number
- CA2490420A1 CA2490420A1 CA002490420A CA2490420A CA2490420A1 CA 2490420 A1 CA2490420 A1 CA 2490420A1 CA 002490420 A CA002490420 A CA 002490420A CA 2490420 A CA2490420 A CA 2490420A CA 2490420 A1 CA2490420 A1 CA 2490420A1
- Authority
- CA
- Canada
- Prior art keywords
- tube
- gas
- analyzing
- bubble
- processing
- Prior art date
- Legal status (The legal status 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 status listed.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract 34
- 239000012768 molten material Substances 0.000 title claims abstract 5
- 238000002536 laser-induced breakdown spectroscopy Methods 0.000 title abstract 3
- 238000004458 analytical method Methods 0.000 title 1
- 239000000463 material Substances 0.000 claims abstract 40
- 238000012545 processing Methods 0.000 claims abstract 13
- 239000000203 mixture Substances 0.000 claims abstract 11
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract 7
- 229910052802 copper Inorganic materials 0.000 claims abstract 7
- 239000010949 copper Substances 0.000 claims abstract 7
- 238000003723 Smelting Methods 0.000 claims abstract 4
- 239000007789 gas Substances 0.000 claims 18
- 239000000470 constituent Substances 0.000 claims 12
- 230000003595 spectral effect Effects 0.000 claims 9
- 210000002381 plasma Anatomy 0.000 claims 8
- 230000015572 biosynthetic process Effects 0.000 claims 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims 6
- 238000003780 insertion Methods 0.000 claims 6
- 230000037431 insertion Effects 0.000 claims 6
- 230000005855 radiation Effects 0.000 claims 5
- 238000001228 spectrum Methods 0.000 claims 5
- 238000011088 calibration curve Methods 0.000 claims 3
- 238000013213 extrapolation Methods 0.000 claims 3
- 229910052742 iron Inorganic materials 0.000 claims 3
- 238000011545 laboratory measurement Methods 0.000 claims 3
- 238000012544 monitoring process Methods 0.000 claims 3
- 230000003287 optical effect Effects 0.000 claims 3
- 230000008685 targeting Effects 0.000 claims 3
- 238000002679 ablation Methods 0.000 claims 2
- 238000009825 accumulation Methods 0.000 claims 2
- 239000000443 aerosol Substances 0.000 claims 2
- 239000000835 fiber Substances 0.000 claims 2
- 239000011344 liquid material Substances 0.000 claims 2
- 239000011261 inert gas Substances 0.000 claims 1
- 238000010223 real-time analysis Methods 0.000 abstract 2
- -1 e.g. Substances 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
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
- 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
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
- C23C2/50—Controlling or regulating the coating processes
- C23C2/52—Controlling or regulating the coating processes with means for measuring or sensing
- C23C2/521—Composition of the bath
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
- G01J3/28—Investigating the spectrum
- G01J3/443—Emission spectrometry
-
- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/314—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths
- G01N21/3151—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths using two sources of radiation of different wavelengths
-
- 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
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6402—Atomic fluorescence; Laser induced fluorescence
- G01N21/6404—Atomic fluorescence
-
- 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
- G01N21/8507—Probe photometers, i.e. with optical measuring part dipped into fluid sample
Abstract
An apparatus and a method are disclosed for use with Laser Induced Breakdown Spectroscopy (LIBS) systems that can be applied to the real time analysis of molten materials or liquid. Since it is difficult to prepare a surface representative of the bulk when dealing with high temperature molten materia l, the invention, in one aspect, uses a forced gas flow through a tube insertab le inside the molten material to generate a bubble. The inner surface of the bubble is a representative of the composition of the material. LIBS performe d on such a surface produces an accurate real time analysis of material, even when other processing of material, e.g., copper smelting, etc., is being conducted.
Claims (40)
1.~A method of analyzing a molten or liquid material by laser induced spectrography, comprising steps of:
preparing, by a flow of a gas, a portion of the material representative of its composition;
sending at least one laser pulse to the prepared portion to produce a plasma of the material;~
transmitting radiation generated by the plasma to a spectrum analyzer, and analyzing a spectrum of the transmitted radiation to determine a composition of the material.
preparing, by a flow of a gas, a portion of the material representative of its composition;
sending at least one laser pulse to the prepared portion to produce a plasma of the material;~
transmitting radiation generated by the plasma to a spectrum analyzer, and analyzing a spectrum of the transmitted radiation to determine a composition of the material.
2. ~The method according to claim 1, further comprising steps of:
injecting the gas under pressure through a tube to produce a bubble inside the material, the inner surface of the bubble being the prepared portion of the material;
sending the laser pulse through the tube to the prepared portion, and transmitting radiation through the tube to the spectrum analyzer.
injecting the gas under pressure through a tube to produce a bubble inside the material, the inner surface of the bubble being the prepared portion of the material;
sending the laser pulse through the tube to the prepared portion, and transmitting radiation through the tube to the spectrum analyzer.
3. ~The method according to claim 2, wherein the gas is selected from a group of gases which include air, an inert gas and any of reactive gases used for processing of the material.
4. ~The method according to claim 3, wherein the gas is a reactive gas selected from a group of gases which are used for processing of the material, and the method further comprising step of:
controlling processing of the material in response to the composition so determined.
controlling processing of the material in response to the composition so determined.
5. ~The method according to claim 4, further comprising a step of:
optically monitoring through the tube the prepared portion to assist targeting the laser pulse.
optically monitoring through the tube the prepared portion to assist targeting the laser pulse.
6. ~The method according to claim 5, wherein the step of analyzing comprises a step of:
plotting a ratio of two spectral lines, one of said spectral lines related to a specific constituent in the material and the other of said spectral lines related to a constant major constituent.
plotting a ratio of two spectral lines, one of said spectral lines related to a specific constituent in the material and the other of said spectral lines related to a constant major constituent.
7. ~The method according to claim 6, wherein the step of analyzing further comprises a step of:
finding by extrapolation a ratio representative of a bulk of the material.
finding by extrapolation a ratio representative of a bulk of the material.
8. ~The method according to claim 7, wherein the step of analyzing further comprises a step of:
calibrating the composition thus far determined by using a calibration curve established on samples which have been calibrated through independent laboratory measurements.
calibrating the composition thus far determined by using a calibration curve established on samples which have been calibrated through independent laboratory measurements.
9. ~The method according to claim 8, wherein the processing of the material is copper smelting and the specific constituent is iron and the constant major constituent is copper.
10. ~The method according to claim 9, further comprising a step of:
adjusting an angle of insertion of the tube into the material to control formation of the bubble.
adjusting an angle of insertion of the tube into the material to control formation of the bubble.
11. ~The method according to claim 8, wherein the processing of the material is a hot dip galvanization process.
12. ~The method according to claim 11, further comprising a step of:
adjusting an angle of insertion of the tube into the material to control formation of the bubble.
adjusting an angle of insertion of the tube into the material to control formation of the bubble.
13. ~The method according to claim 5, further comprising steps of:
sending a series of laser pulses to produce a plurality of plasmas, and repeating the step of analyzing for each of the plurality of plasmas to determine the composition of the material.
sending a series of laser pulses to produce a plurality of plasmas, and repeating the step of analyzing for each of the plurality of plasmas to determine the composition of the material.
14. ~The method according to claim 13, wherein the step of analyzing comprises a step of:
plotting a ratio of two spectral lines, one of said spectral lines related to a specific constituent in the material and the other of said spectral lines related to a constant major constituent.
plotting a ratio of two spectral lines, one of said spectral lines related to a specific constituent in the material and the other of said spectral lines related to a constant major constituent.
15. ~The method according to claim 14, wherein the step of processing comprises a step of:
finding by extrapolation a ratio representative of a bulk of the material.
finding by extrapolation a ratio representative of a bulk of the material.
16. ~The method according to claim 15, wherein the step of analyzing further comprises a step of:
calibrating the composition thus far determined by using a calibration curve established on samples which have been calibrated through independent laboratory measurements.
calibrating the composition thus far determined by using a calibration curve established on samples which have been calibrated through independent laboratory measurements.
17. ~The method according to claim 16, wherein the processing of the material is copper smelting and the specific constituent is iron and the constant major constituent is copper.
18. ~The method according to claim 17, further comprising a step of:
adjusting an angle of insertion of the tube into the material to control formation of the bubble.
adjusting an angle of insertion of the tube into the material to control formation of the bubble.
19. ~The method according to claim 16, wherein the processing of the material is a hot dip galvanization process.
20. ~The method according to claim 19, further comprising a step of:
adjusting an angle of insertion of the tube into the material to control formation of the bubble.
adjusting an angle of insertion of the tube into the material to control formation of the bubble.
21. ~The method according to claim 5, further comprising steps of:
sending a series of laser pulses of different wavelengths to produce a series of plasmas, and repeating the step of analyzing a spectrum of each plasma to determine the composition of the material.
sending a series of laser pulses of different wavelengths to produce a series of plasmas, and repeating the step of analyzing a spectrum of each plasma to determine the composition of the material.
22. ~The method according to claim 21, wherein the step of analyzing comprises a step of:
plotting a ratio of two spectral lines, one of said spectral lines related to a specific constituent in the material and the other of said spectral lines related to a constant major constituent.
plotting a ratio of two spectral lines, one of said spectral lines related to a specific constituent in the material and the other of said spectral lines related to a constant major constituent.
23. ~The method according to claim 22, wherein the step of processing comprises a step of:
finding by extrapolation a ratio representative of a bulk of the material.
finding by extrapolation a ratio representative of a bulk of the material.
24. ~The method according to claim 23, wherein the step of analyzing further comprises a step of:~
calibrating the composition thus far determined by using a calibration curve established on samples which have been calibrated through independent laboratory measurements.
calibrating the composition thus far determined by using a calibration curve established on samples which have been calibrated through independent laboratory measurements.
25. ~The method according to claim 24, wherein the processing of the material is copper smelting and the specific constituent is iron and the constant major constituent is copper.
26. ~The method according to claim 25, further comprising a step of:
adjusting an angle of insertion of the tube into the material to control formation of the bubble.
adjusting an angle of insertion of the tube into the material to control formation of the bubble.
27. ~The method according to claim 24, wherein the processing of the material is a hot dip galvanization process.
28. ~The method according to claim 26, further comprising a step of:
adjusting an angle of insertion of the tube into the material to control formation of the bubble.
adjusting an angle of insertion of the tube into the material to control formation of the bubble.
29. ~A laser induced spectrography apparatus for analyzing a molten or liquid material, comprising:
a tube having a transparent window at one end and for injecting a gas under pressure into the material to prepare a portion of the material representative of its composition;
a laser source for sending a pulsed laser beam through the tube and the window toward the prepared portion to produce a plasma of the material;
an optical arrangement for transmitting radiation from the plasma through the tube and window, and a spectrum analyzer for analyzing the radiation to determine a composition of the material.
a tube having a transparent window at one end and for injecting a gas under pressure into the material to prepare a portion of the material representative of its composition;
a laser source for sending a pulsed laser beam through the tube and the window toward the prepared portion to produce a plasma of the material;
an optical arrangement for transmitting radiation from the plasma through the tube and window, and a spectrum analyzer for analyzing the radiation to determine a composition of the material.
30. ~The apparatus according to claim 29, wherein at least a portion of the tube is made of a resistance material and is adapted to be immersed in the material.
31. ~The apparatus according to claim 30, wherein the optical arrangement comprises a combination of lenses, mirrors and fiber optics.
32. ~The apparatus according to claim 31, further comprising:
a vision system for monitoring the prepared portion to assist in targeting the pulsed laser beam.
a vision system for monitoring the prepared portion to assist in targeting the pulsed laser beam.
33. ~The apparatus according to claim 32, further comprising:
a gas injecting mechanism for injecting the gas to create the bubble inside the material when the tube is immersed therein.
a gas injecting mechanism for injecting the gas to create the bubble inside the material when the tube is immersed therein.
34. ~The apparatus according to claim 32, wherein the gas injected by the gas injecting mechanism prevents accumulation of aerosols and ablation debris along the laser beam path.
35. ~The apparatus according to claim 33, wherein a tip of the tube is designed to control formation of the bubble.
36. ~The apparatus according to claim 29, wherein the tube is designed such that it can be inserted into a tuyere provided on a processing equipment of the material, and such that it does not disturb the flow of the reactive gas through the tuyere.
37. ~The apparatus according to claim 36, wherein the optical arrangement comprises a combination of lenses, mirrors and fiber optics.
38. ~The apparatus according to claim 37, further comprising:
a vision system for monitoring the prepared portion to assist in targeting the pulsed laser beam.
a vision system for monitoring the prepared portion to assist in targeting the pulsed laser beam.
39. ~The apparatus according to claim 38, further comprising a gas injecting mechanism for injecting the gas to create the bubble inside the material when the tube is immersed therein.
40. ~The apparatus according to claim 38, wherein the gas injected by the gas injecting mechanism prevents accumulation of aerosols and ablation debris along the laser beam path.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US10/176,586 | 2002-06-24 | ||
| US10/176,586 US6909505B2 (en) | 2002-06-24 | 2002-06-24 | Method and apparatus for molten material analysis by laser induced breakdown spectroscopy |
| PCT/CA2003/000910 WO2004001394A2 (en) | 2002-06-24 | 2003-06-17 | Laser induced breakdown spectroscopy for the analysis of molten material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CA2490420A1 true CA2490420A1 (en) | 2003-12-31 |
| CA2490420C CA2490420C (en) | 2012-01-10 |
Family
ID=29734173
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA2490420A Expired - Lifetime CA2490420C (en) | 2002-06-24 | 2003-06-17 | Method and apparatus for molten material analysis by laser induced breakdown spectroscopy |
Country Status (7)
| Country | Link |
|---|---|
| US (1) | US6909505B2 (en) |
| EP (1) | EP1520164B1 (en) |
| JP (1) | JP2005530989A (en) |
| KR (1) | KR101009845B1 (en) |
| AU (1) | AU2003245143A1 (en) |
| CA (1) | CA2490420C (en) |
| WO (1) | WO2004001394A2 (en) |
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2002
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2003
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- 2003-06-17 AU AU2003245143A patent/AU2003245143A1/en not_active Abandoned
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| AU2003245143A1 (en) | 2004-01-06 |
| US6909505B2 (en) | 2005-06-21 |
| KR101009845B1 (en) | 2011-01-19 |
| EP1520164A2 (en) | 2005-04-06 |
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