CN103518121A - An emission spectrometer and method of operation - Google Patents
An emission spectrometer and method of operation Download PDFInfo
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- CN103518121A CN103518121A CN201280006560.7A CN201280006560A CN103518121A CN 103518121 A CN103518121 A CN 103518121A CN 201280006560 A CN201280006560 A CN 201280006560A CN 103518121 A CN103518121 A CN 103518121A
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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
- G01N21/17—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
- G01N21/27—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands using photo-electric detection ; circuits for computing concentration
- G01N21/274—Calibration, base line adjustment, drift correction
- G01N21/276—Calibration, base line adjustment, drift correction with alternation of sample and standard in optical path
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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
- 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
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Abstract
A method of calibrating an emission spectrometer (10) having a detector (11) capable of detecting spectral components of incident radiation, and a measurement optical path (28) which directs an energy beam (26) to a sample (20) and radiation emitted by the sample when irradiated by the energy beam to the radiation detector (11). The method comprises directing radiation of known spectral characteristic along an alternate path to the detector (11). The detector (11) to detects spectral characteristics of the radiation and makes a comparison with the known spectral characteristics. Drift data is determined on a basis of any variation between the detected and known spectral characteristics. The drift data is stored and subsequently used to adjust detected spectral characteristics of a sample in the measurement optical path (28) produce a drift calibrated output spectral analysis of the sample.
Description
Technical field
The present invention relates to emission spectrometer and operate the method for this spectrometer.
Background technology
Emission spectroscopy relates to and excites the atom of material and check by atom the wavelength to the photon of launching during compared with low-lying level transition in self-excitation state.Every kind of element in periodic table is launched the discrete wavelength of a feature group when its atom self-excitation state is back to compared with low-lying level.By detecting and analyze these wavelength, the element that can determine sample forms.Atom can be expressed the polytype energy source of characteristic of the type of emission spectrometer and supply with energy.For example, can irradiate excited atom by using such as the electromagnetic radiation line being caused by laser instrument, X-ray or electric discharge.
No matter energy source why, the accuracy of this emission spectrometer and reliability depend on for receiving from the detecting device of radioactive ray and the accuracy of optical device and the quality of sample transmitting.The output of spectrometer may be drifted about in time, for the reliable output from spectrometer is provided, should checks the response of detecting device and/or optical device and sometimes should calibrate spectrometer if desired.
Summary of the invention
In one aspect of the invention, a kind of method of using emission spectrometer to obtain the emission spectrum of sample is provided, the radioactive ray of being launched when described emission spectrometer has the detecting device of the spectral characteristic that can detect incident radioactive ray and energy beam guided to sample and sample is irradiated by energy beam guide to the optical path of detecting device, and described method comprises:
Operation is carried dress (onboard) calibration system to generate and the spectrometer relevant drift data that drifts about;
Sample is placed in optical path, the sample in this light path of radiation, and use detecting device to produce the original spectrum characteristic of the radioactive ray of being launched by sample; And
By produce the emission spectrum of sample for the original spectrum characteristic of spectrometer drift compensation sample with drift data.
In one embodiment, operation is carried a dress calibration system and is comprised the radioactive ray of known spectral characteristic are guided to detecting device.
In a second aspect of the present invention, a kind of method of operation issue spectrometer is provided, the radioactive ray of being launched when described emission spectrometer has the detecting device of the spectral characteristic that can detect incident radioactive ray and energy beam guided to sample and sample is irradiated by energy beam guide to the optical path of detecting device, and described method comprises:
With carrying dress drift calibration system, carry out calibration process (routine), described calibration process comprises: along replacing light path, the radioactive ray of known spectral characteristic are guided to detecting device; Operations detector is to detect the spectral characteristic of radioactive ray; The spectral characteristic and the known spectral characteristic that relatively detect; Drift data is determined in spectral characteristic based on detecting and any change between known spectral characteristic; And storage drift data; And,
Carry out measuring process, described measuring process comprises: sample is placed in light path, and the sample in this light path of radiation, detects the spectral characteristic of the radioactive ray of being launched by sample, and uses drift data for the spectral characteristic of spectrometer drift compensation sample.
In a third aspect of the present invention, a kind of method of using emission spectrometer to obtain the emission spectrum of sample is provided, the radioactive ray of being launched when described emission spectrometer has the detecting device of the spectral characteristic that can detect incident radioactive ray and energy beam guided to sample and sample is irradiated by energy beam guide to the optical path of radiation detector, and described method comprises:
The radioactive ray of known spectral characteristic are guided to detecting device;
Operations detector is to detect the spectral characteristic of radioactive ray;
The spectral characteristic and the known spectral characteristic that relatively detect;
Drift data is determined in spectral characteristic based on detecting and any change between known spectral characteristic;
Storage drift data; And
By produce the emission spectrum of sample for the original spectrum characteristic of the sample in spectrometer drift compensation optical path with drift data.
In one embodiment, the radioactive ray of known spectral characteristic being guided to detecting device comprises:
The master sample of known features is provided;
Make to be diverted to master sample from the energy beam of optical path; And
The radioactive ray of being launched by master sample are guided to detecting device.
Energy beam is turned to can be comprised: the first optical system is moved in optical path, the first optical system can operate energy beam is guided to master sample, and receive the radioactive ray of the master sample that the irradiation by energy beam causes, and the radioactive ray of the master sample subsequently irradiation by energy beam being caused guide to detecting device.
Described method changes the point of irradiation of energy beam on master sample to determine drift data in the time of can being included in the subsequent operation of spectrometer.
Changing point of irradiation can comprise: the position that changes master sample when maintaining the substantially constant track of energy beam.
The position that changes master sample can comprise: sample is arranged on X-Y mobile device, and under drift mode during each operation of spectrometer operating moving device with mobile in the plane master sample in one or two direction in X and Y-direction.
Alternately, changing point of irradiation can comprise: master sample is maintained in fixed position, and handle energy beam to irradiate the difference on master sample.
Additionally or alternately, the radioactive ray of known spectral characteristic are guided to detecting device can be comprised: the radiation source of known spectra is provided, and the radioactive ray of the radiation source from known spectra are guided to detecting device.
The radioactive ray of the radiation source from known spectra are guided to detecting device can be comprised: definition is moved to radioactive ray from radiation source in Zhong position, the visual field of detecting device for the second optical system of the light path of radiation source.
Described method can comprise: make to turn to from a part for the energy beam of optical path, and by this part turning to, monitor the energy level of energy beam.
Described method can comprise: when the energy level monitoring is during lower than predetermined minimum energy level, generate energy level alarm.
Described method can comprise: when the spectral characteristic detecting and the change between known spectral characteristic are greater than threshold value, and generating detector alarm.
Another aspect of the present invention comprises a kind of emission spectrometer that can operate to provide the spectral analysis of sample, and described spectrometer comprises:
Detecting device, can detect the spectral characteristic of incident radioactive ray;
Optical path, while being set to energy beam is guided to sample position and the sample at sample position place is irradiated by energy beam, the radioactive ray of transmitting guide to detecting device; And
Drift calibration system, the radioactive ray of known spectral characteristic can be guided to detecting device to produce the calibration spectrum characteristic detecting, and any change between the calibration spectrum characteristic based on known spectral characteristic and detection regulates the output spectrum analysis of sample.
Drift calibration system can comprise: master sample, when by energy beam radiation, launch the radioactive ray of known spectral characteristic; And the first optical system that can be mobile between drift calibrating position and measuring position, at drift calibrating position, the first optical system can operate energy beam is diverted to master sample, and receive the radioactive ray of the master sample that the irradiation by energy beam causes, and the radioactive ray of the master sample subsequently irradiation by energy beam being caused guide to detecting device, in measuring position, the first optical system is outside optical path.
Drift calibration system may be able to operate and when the subsequent operation of drift calibration system, change the incidence point of energy beam on master sample.
Drift calibration system can comprise the X-Y mobile device that master sample is installed on it, wherein, this mobile device can be when the subsequent operation of drift calibration system mobile in the plane master sample in one or two direction in X and Y-direction.
Additionally or alternately, drift calibration system can comprise: the radiation source of known spectra and can operating for the radioactive ray of the radiation source from known spectra being guided to the second optical system of detecting device.
In one embodiment, the second optical system definition is for the light path of radiation source, and can move to radioactive ray from radiation source in Zhong position, the visual field of detecting device.
Emission spectrometer can comprise can be based on following (a) and (b) one or two between the processor that relatively generates drift data: (a) spectral characteristic of the known spectral characteristic of master sample and the radioactive ray of launching from master sample that detected by detecting device when master sample is irradiated by energy beam; And (b) known spectra of radiation source and the spectrum of the radiation source that detected by detecting device.
Drift calibration system generates alarm in the time of may being greater than threshold value in the difference between the known spectral characteristic of master sample and the spectral characteristic of the radioactive ray of launching from master sample that detected by detecting device when master sample is irradiated by energy beam.
Drift calibration system generates alarm while also may the difference between the known spectra of radiation source and the spectrum of the radiation source being detected by detecting device being greater than threshold value.
Emission spectrometer can comprise energy level monitor, and described energy level monitor can monitor the energy level of energy beam, and the signal of the energy level that indication monitors is provided to drift calibration system.
Emission spectrometer also may generate in the energy level monitoring alarm during lower than threshold energy level.
Accompanying drawing explanation
Now will only with reference to accompanying drawing, by the mode of example, embodiments of the invention be described, in the accompanying drawings:
Fig. 1 be according to and in conjunction with the schematic diagram of the block diagram form of the laser-induced breakdown spectrometer (LIBS) of the embodiment of the present invention;
Fig. 2 shows LIBS in Fig. 1 work under normal measurement pattern, wherein operates spectrometer to detect the spectral characteristic of sample;
Fig. 3 is the expression of the LIBS shown in the Fig. 1 and 2 operating in aspect the Yi Ge of calibration mode;
Fig. 4 is the schematic diagram of the master sample that uses in the first aspect of calibration mode;
Fig. 5 is included in the expression of the sample mobile device in the LIBS shown in Fig. 1-3;
Fig. 6 is the schematic diagram of the LIBS shown in Fig. 1-4 that operate in the second aspect of calibration mode; And
Fig. 7 is the process flow diagram of embodiment of describing to obtain the method for emission spectrum.
Embodiment
About a kind of emission spectrometer, embodiments of the invention are described, it has the detecting device of the spectral characteristic that can detect incident radioactive ray, and energy is guided to sample and the radioactive ray of being launched by sample are guided to the optical path of detecting device when illuminated.In the context of laser-induced breakdown spectrometer (LIBS), describe following embodiment, but these embodiment can be applied to the emission spectrometer of the other types that include but not limited to XRF, XRD, NIR or NQR spectrometer, spark induced breakdown spectrometer or atomic emissions spectrometer.
In a broad sense, the embodiment of this method and system comprises year dress calibration system so that drift about and can compensate the original transmitted spectrum of sample for spectrometer.This can be by completing the radioactive ray guiding detecting device of known spectral characteristic.Can provide the different radiation source of known spectral characteristic to measure the different spectral responses of spectrometer, thereby make it possible to calibrate spectrometer to solve one or more drift situations (scenarios) of spectrometer.In this instructions, term " drift " expression, when different time points is in the same characteristic of measuring same (or identical different) sample under identical condition, the variation of measured value.Except other aspects, spectrometer drift may be that for example, variation due to the performance of the arbitrary optical element in the light path between energy beam (laser), energy beam and detecting device or detecting device causes.
Embodiments of the invention utilization is carried dress calibration system and drift about and measures and generate drift data, thereby drifts about so that can calibrate spectrometer and compensate original transmitted spectrum solution spectrometer.This permission is carried out the ultimate analysis of reliable scene/original position to the sample the ore sample such as from ore body.
The master sample of the principal component that an embodiment utilization of calibration system is irradiated by the energy source of spectrometer.Suppose that energy source, detecting device and optical device work with ideal style, actual (hereinafter referred to " original ") emission spectrum that detects/measure should be consistent with the known spectral characteristic of master sample.Original spectrum characteristic is compared with characteristic known or expection.Then change between known spectra and original spectrum can be used to generate calibration data, thereby makes it possible to calibrate spectrometer.
The radioactive ray of the known spectra being provided by the radiation source such as having the lamp of known spectra are provided for identical or alternative embodiment, and it is directed to detecting device.Operation spectrometer is to measure the spectral characteristic of radioactive ray.Then the known of radiation source or expectation spectrum are compared with the original spectrum of the radiation source being detected by detecting device, and use any change wherein with generation, to be used for the calibration data of spectrometer.Change between known spectral characteristic and original spectrum characteristic can be indicated the drift in the miscellaneous part of detecting device drift and/or spectrometer.
Fig. 1 is block diagram, and laser-induced breakdown spectrometer (LIBS) 10 comprises embodiments of the invention.LIBS10 is associated with transfer system 12, and transfer system 12 is for transmitting the sample of material by or pass through the analysis area of LIBS10.LIBS10 comprises laser instrument and optical device system (LOS) 14, analysis and power system (APS) 16, and the junction box 18 that interface is provided between LOS14 and APS16.APS16 comprises practical detector (that is, spectrometer) 11 and power supply 13 and the processor/computing machine 15 of LIBS10.
In accompanying drawing 2, illustrate in greater detail when LIBS10 is in the measurement pattern LOS14 in lower time.Under this pattern, LIBS10 detects or measures the spectral characteristic of sample of material, and sample of material can be for example iron ore sample 20.With reference to figure 1, sample 20 uploads at forwarder 12 analysis area that LIBS10 is crossed in the warp let-off.
The parts of LOS14 are arranged in shell or case 22.The parts of LOS14 comprise the laser instrument 24 of Emission Lasers bundle, and optical path 28: it guides to sample 20 by laser beam 26; And will guide to detecting device 11 from the radioactive ray 30 of sample 20 transmittings.Laser beam 26 provides and makes sample 20 produce the required energy of emission spectrum.
When the measurement pattern lower time of LIBS10 in operation, from the laser beam 26 of laser instrument 24 transmitting, be reflected at first 90 ° of mirror 36 reflections to catoptron 38, at catoptron 38 places, it is reflected again 90 °.Laser beam 26 is the aperture in scioptics 40 and perforated mirror 42 subsequently, by shield (shroud) 46 and arrive on sample 20.Laser beam shock sample 20 to higher energy level, is launched radioactive ray 30 by the atomic excitation in sample subsequently when atomic transition is back to lower energy state.The part transmission of the radioactive ray 30 of transmitting is by shield 46, and is reflected mirror 42 and reflexes to gatherer 48, and it reflexes to the radioactive ray of transmitting 30 the spectrometer optical fiber 50 end keeping in terminal block 51.These radioactive ray transmit subsequently by optical fiber 50, arrive at the spectrometer of settling in APS16.Catoptron 36 is set to allow a part of 26a of laser beam 26 to be turned into energy meter 52 further.From sample 20 to catoptron 42, gatherer 48 the radioactive ray 30 path of arriving at the transmitting of the optical fiber 50 end that terminal block 51 settles form plasma and detect path 34.
A plurality of optical elements in optical path 28 (that is, lens 40, catoptron 42, gatherer 48 and for the terminal block 51 of optical fiber 50) are installed in the moveable platform 56 that the self-focusing of LIBS10 feature is provided.Self-focusing feature is not essential part of the present invention or key component, at number of patent application US61/388, is described in detail in 722.
Therefore, under the measurement pattern of operation, optical path 28 guides to sample 20 by laser beam 26, and will guide to detecting device from the radioactive ray 30 of sample 20 transmittings subsequently.
Detecting device 11 operates to provide spectral analysis and the corresponding original transmitted spectrum of sample 20 subsequently.
Energy source laser instrument 24 in the present embodiment and can being repeated for the providing at various types of emission spectrometers of optical path 28 that energy is guided to sample 20 and subsequently the radioactive ray from sample 20 transmitting are guided to detecting device.Yet, by providing can operate along replacing light path, the radioactive ray of known spectral characteristic being guided to the prosthetics system of carrying of detecting device, the LIBS10 that makes it possible to realize in the present embodiment is calibrated to solve the ability of detecting device drift.Detecting device 11 can be operating as the spectral characteristic that detects known radioactive ray subsequently, and is compared between the spectral characteristic detecting and known spectral characteristic by processor 15.Then the change between the spectral characteristic of processor 15 based on detecting and known spectral characteristic generates drift data.Spectrometer 10 can be set to automatically carry out calibration process when each " startup ".But, additionally or alternately, can provide to control and move when needed calibration process.
In this embodiment, spectrometer comprises calibration system CS so that can calibrate spectrometer and compensate the original spectrum measurement that sample generates.When calibration system CS operates, spectrometer is known as in calibration mode.On the contrary, when calibration system CS does not operate, spectrometer 10 is in measurement pattern.
One or two in calibration system CS use Liang Ge mechanism or system is to guide to detecting device by the radioactive ray of known spectral characteristic.The first mechanism in these mechanisms is used and is located at test or the master sample 60 (referring to Fig. 3-5) in shell 22 and can operates to create the first optical system 62 that laser beam 26 is guided on master sample 60 and the radioactive ray from sample 60 transmittings are guided to the replacement light path of detecting device 11 by optical fiber 50.Optical system 62 comprises the prism 64 being arranged on moving slider 66.When operating LIBS10 under calibration mode, slide block 66 moves to right side to block the laser beam 26 between catoptron 42 and shield 46 and laser beam is reflected to 90 ° to master sample 60 by prism 64.The directed prism 40 that is back to of a part 68 of the radioactive ray of master sample transmitting, at prism 40 places, it is reflected onto catoptron 42 and by gatherer 48, is guided to optical fiber 50 subsequently.When by laser beam 26 radiation, the radioactive ray 68 of master sample transmitting have known (that is, " benchmark ") spectrum.This known spectra is stored in the storer of processor 15 or in the storer being associated with processor 15.Detecting device 11 receives the radioactive ray 68 of transmitting, and operation detects the spectral characteristic of radioactive ray.The spectrum of this measurement is also transferred into processor 15, between the spectral characteristic of measuring and the spectral characteristic of previously stored expection, compares.Spectral characteristic that can be based on measuring and the difference between known or expection spectral characteristic, produce for example calibration data of standard curve form by multiple mathematical technique.Some examples of mathematical tool comprise question blank, principle component regression, cluster regretional analysis, search-matching process, Gauss's technology, complete pattern method, the peak value modeling based on condition etc.Be appreciated that the suitable mathematical technique that one of ordinary skill in the art compensate the calibration data for by suitable will be familiar with.Subsequently, when 10 of LIS calibrates with calibration data during in measurement pattern or output (original) spectrum of standardization sample 20, thus the drift in compensation spectrometer or other are abnormal.
Once detecting device 11 has detected radioactive ray 68 and the calibration data of transmitting and has been generated, just by prism 64 being shifted out to plasma generation pass 32 first optical system 62 of retracting.LIBS10 can operate now under measurement pattern.
Drift calibration mode can be moved when needed, or automatically moves when each operation of LIBS10.There is following possibility: repeatedly the same point on radiation standard sample may cause producing different spectrum.Thereby when the subsequent operation of drift calibration mode, the point that change sample 60 is irradiated by laser beam 26 is to guarantee the consistance of the benchmark spectrum of sample.That is, when the subsequent operation of calibration mode, the difference that uses laser beam 26 to irradiate on sample 60.By the grid 70 shown in Fig. 4, the different points of irradiation on sample 60 are shown, each white box in grid represents the different points of irradiation on sample 60.
In this embodiment, by the X-Y mobile device 72 in being arranged on shell 74, sample 60 being installed, realize the change of point of irradiation.Mobile device 72 operation comes to increase sample 60 positions with respect to the first optical system 62, makes when each operation of calibration mode or operation, and the lip-deep difference of sample 60 is positioned as the path alignment with laser beam 26.
Fig. 6 illustrates the second mechanism of calibration system CS.This mechanism can be considered to provide wavelength calibration pattern, and it uses the lamp 78 (for example mercury argon lamp) of the radioactive ray that produce known wavelength and can optionally the radioactive ray from lamp 78 be guided to the second optical system 80 of detecting device 11 by optical fiber 50.Optical system 80 comprises optical fiber 82, and it is set at one end to receive from the light of lamp 78 and at the other end and remains in the coupling mechanism 84 being supported on platform 86 slidably.Coupling mechanism 84 keeps optical fiber 82 one end, thereby along with the Linear-moving of platform 86 moves together.The light scioptics 88 of optical fiber 82 transmission arrive at catoptron 90, and catoptron 90 reflects 90 ° to another lens 92 by radioactive ray.Lens 92 guide to optical fiber 50 by the radioactive ray from lamp 78, thereby to detecting device 11.The wave spectrum being produced by detecting device 11 is provided to processor 15.Processor 15 relatively the expectation of lamps 78 or known wave spectrum and measurement or original wavelength spectrum.The spectrum that processor 15 use are measured and any change between the spectrum of expectation generate wavelength calibration data, and wavelength calibration data are used to the original output of adjusting or standardization LIBS10 subsequently during the measurement pattern of LIBS10.When the inoperation of this aspect of calibration mode, platform 86 is moved to the left, and optical system 80 is shifted out from optical path 28, thereby LIBS10 can be operated under measurement pattern.
As previously mentioned, calibration mode can move when needed, or alternately in each continued operation of LIBS10 or operation while using.For example, can imagine, when each LIBS10 will be used to obtain the emission spectrum of sample, as powering on or the part of start-up course of LIBS10, automatically move calibration mode.Can generate calibration data subsequently, and regulate or the original output of standardization LIBS10 under its normal measurement pattern with it.This provides autonomous drift regime of calibration.Can further imagine, when generating calibration data, LIBS10, particularly processor 15, can be programmed to or otherwise be set to give the alarm when the change between master sample 60 or the known spectral characteristic of lamp 78 and the spectral characteristic of measurement surpasses predetermined threshold.This can be operated in conjunction with the measurement to the output power of laser instrument 24 of being undertaken by energy meter 52.Processor 15 can be programmed to determine that whether laser energy is in predetermined minimum energy level.When the energy level of laser beam is detected as lower than threshold value, LIBS10 can produce another alarm of this situation of indication.When the variation between known spectra between alignment epoch and measure spectrum is outside specified scope, this information is also useful.If such variation outside specified scope and laser energy magnitude in or higher than the minimum level requiring, can show that this variation is caused by detecting device or optical device, rather than the result of the minimizing of laser energy magnitude.
Fig. 7 describes roughly to use or operates LIBS10 with the process flow diagram of the method 100 of the emission spectrum of acquisition sample.
Once the calibration process at step 102 place completes, with regard to the next step 104 in manner of execution 100, at the operation LIBS10 of step 104 place, detect the spectral characteristic of sample 20.This produces original spectrum data or the original transmitted spectrum of sample 20.
Finally, at step 106 place of method 100, by using in step 102 offset data obtaining to compensate the original spectrum characteristic of sample 20, to produce the emission spectrum of the sample 20 that has compensated spectrometer drift.
Since describe embodiments of the invention in detail, for one of ordinary skill in the art, will be apparent that, in the situation that not deviating from invention basic conception, can make many modifications or modification.For example, the part that the ordinal shift that LIBS10 is used the calibration of master sample 60 to depend on the sample 60 that X-Y mobile device 72 causes is irradiated by laser beam 26 to change sample 60.Yet, in alternative embodiment, sample 60 maintain static in, by handling the executor optical device that laser beam 26 is guided to the difference on sample 60, can reach identical effect.In addition,, although the emission spectrometer of describing in this embodiment is laser-induced breakdown spectrometer, as previously mentioned, can utilize dissimilar emission spectrometer to operate and use embodiments of the invention.In addition, in described embodiment, removable being installed as that LOS14 has in optical path 28 makes it possible to realize self-focusing various optical element.Yet this is not an aspect of of the present present invention, embodiments of the invention adopt the emission spectrometer with fixed-focus system similarly to work.
One of ordinary skill in the art be it is evident that, all such modifications and modification and other changes are all considered within the scope of the invention, and character of the present invention is determined by above-mentioned instructions and appending claims.
Claims (27)
1. a method of using emission spectrometer to obtain the emission spectrum of sample, the radioactive ray of being launched when described emission spectrometer has the detecting device of the spectral characteristic that can detect incident radioactive ray and energy beam guided to sample and sample is irradiated by energy beam guide to the optical path of detecting device, and described method comprises:
Operation is carried dress calibration system to generate and the spectrometer relevant drift data that drifts about;
Sample is placed in optical path, the sample in this light path of radiation, and use detecting device to produce the original spectrum characteristic of the radioactive ray of being launched by sample; And
By produce the emission spectrum of sample for the original spectrum characteristic of spectrometer drift compensation sample with drift data.
2. according to the process of claim 1 wherein, operation is carried a dress calibration system and is comprised the radioactive ray of known spectral characteristic are guided to detecting device.
3. the method for an operation issue spectrometer, the radioactive ray of being launched when described emission spectrometer has the detecting device of the spectral characteristic that can detect incident radioactive ray and energy beam guided to sample and sample is irradiated by energy beam guide to the optical path of detecting device, and described method comprises:
With carrying dress drift calibration system, carry out calibration process, described calibration process comprises: along replacing light path, the radioactive ray of known spectral characteristic are guided to detecting device; Operations detector is to detect the spectral characteristic of radioactive ray; The spectral characteristic and the known spectral characteristic that relatively detect; Drift data is determined in spectral characteristic based on detecting and any change between known spectral characteristic; And storage drift data; And,
Carry out measuring process, described measuring process comprises: sample is placed in light path, and the sample in this light path of radiation, detects the spectral characteristic of the radioactive ray of being launched by sample, and uses drift data for the spectral characteristic of spectrometer drift compensation sample.
4. a method of using emission spectrometer to obtain the emission spectrum of sample, the radioactive ray of being launched when described emission spectrometer has the detecting device of the spectral characteristic that can detect incident radioactive ray and energy beam guided to sample and sample is irradiated by energy beam guide to the optical path of radiation detector, and described method comprises:
The radioactive ray of known spectral characteristic are guided to detecting device;
Operations detector is to detect the spectral characteristic of radioactive ray;
The spectral characteristic and the known spectral characteristic that relatively detect;
Drift data is determined in spectral characteristic based on detecting and any change between known spectral characteristic;
Storage drift data; And
By produce the emission spectrum of sample for the original spectrum characteristic of the sample in spectrometer drift compensation optical path with drift data.
5. according to the method for any one in claim 2-4, wherein, the radioactive ray of known spectral characteristic are guided to detecting device and comprise:
The master sample of known features is provided;
Make to be diverted to master sample from the energy beam of optical path; And
The radioactive ray of being launched by master sample are guided to detecting device.
6. according to the method for claim 5, wherein, energy beam is turned to be comprised: the first optical system is moved in optical path, the first optical system can operate energy beam is guided to master sample, and receive the radioactive ray of the master sample that the irradiation by energy beam causes, and the radioactive ray of the master sample subsequently irradiation by energy beam being caused guide to detecting device.
7. according to the method for claim 5 or 6, while being included in the subsequent operation of spectrometer, change the point of irradiation of energy beam on master sample to determine drift data.
8. according to the method for claim 7, wherein, change point of irradiation and comprise: the position that changes master sample when maintaining the substantially constant track of energy beam.
9. method according to Claim 8, wherein, the position that changes master sample comprises: sample is arranged on X-Y mobile device, and under drift mode during each operation of spectrometer operating moving device with mobile in the plane master sample in one or two direction in X and Y-direction.
10. according to the method for claim 7, wherein, change point of irradiation and comprise: master sample is maintained in fixed position, and handle energy beam to irradiate the difference on master sample.
11. according to the method for any one in claim 2-4, wherein, the radioactive ray of known spectral characteristic is guided to detecting device and comprise: the radiation source of known spectra is provided, and the radioactive ray of the radiation source from known spectra are guided to detecting device.
12. according to the method for any one in claim 2-10, also comprises: the radiation source of known spectra is provided, and the radioactive ray of the radiation source from known spectra are guided to detecting device.
13. according to the method for claim 11 or 12, wherein, the radioactive ray of the radiation source from known spectra being guided to detecting device comprises: definition is moved to radioactive ray from radiation source in Zhong position, the visual field of detecting device for the second optical system of the light path of radiation source.
14. according to the method for any one in claim 1-13, comprising: make to turn to from a part for the energy beam of optical path, and by this part turning to, monitor the energy level of energy beam.
15. according to the method for claim 14, comprising: when the energy level monitoring is during lower than predetermined minimum energy level, generate energy level alarm.
16. according to claim 4 or be subordinated to the method for arbitrary claim of claim 4, comprising: when the spectral characteristic detecting and the change between known spectral characteristic are greater than threshold value, and generating detector alarm.
17. 1 kinds of emission spectrometers that can operate to provide the spectral analysis of sample, described spectrometer comprises:
Detecting device, can detect the spectral characteristic of incident radioactive ray;
Optical path, while being set to energy beam is guided to sample position and the sample at sample position place is irradiated by energy beam, the radioactive ray of transmitting guide to detecting device; And
Drift calibration system, the radioactive ray of known spectral characteristic can be guided to detecting device to produce the calibration spectrum characteristic detecting, and any change between the calibration spectrum characteristic based on known spectral characteristic and detection compensates the original spectrum characteristic of sample.
18. according to the emission spectrometer of claim 17, and wherein, drift calibration system comprises:
Master sample is launched the radioactive ray of known spectral characteristic when by energy beam radiation; And
The first optical system that can be mobile between drift calibrating position and measuring position, at drift calibrating position, the first optical system can operate energy beam is diverted to master sample, and receive the radioactive ray of the master sample that the irradiation by energy beam causes, and the radioactive ray of the master sample subsequently irradiation by energy beam being caused guide to detecting device, in measuring position, the first optical system is outside optical path.
19. according to the emission spectrometer of claim 18, and wherein, drift calibration system can operate and when the subsequent operation of drift calibration system, change the incidence point of energy beam on master sample.
20. according to the emission spectrometer of claim 19, wherein, drift calibration system comprises the X-Y mobile device that master sample is installed on it, wherein, this mobile device can be when the subsequent operation of drift calibration system mobile in the plane master sample in one or two direction in X and Y-direction.
21. according to the emission spectrometer of claim 17, and wherein, drift calibration system comprises: the radiation source of known spectra and can operating for the radioactive ray of the radiation source from known spectra being guided to the second optical system of detecting device.
22. according to the emission spectrometer of claim 21, and wherein, the second optical system definition is for the light path of radiation source, and can move to radioactive ray from radiation source in Zhong position, the visual field of detecting device.
23. according to the emission spectrometer of claim 17, wherein, drift calibration system comprise can be based on following (a) and (b) one or two between the processor that relatively generates drift data:
(a) spectral characteristic of the known spectral characteristic of master sample and the radioactive ray from master sample transmitting that detected by detecting device when master sample is irradiated by energy beam; And
(b) spectrum of the known spectra of radiation source and the radiation source that detected by detecting device.
24. according to the emission spectrometer of claim 23, when wherein, drift calibration system can be greater than threshold value in the difference between the known spectral characteristic of master sample and the spectral characteristic of the radioactive ray of launching from master sample that detected by detecting device when master sample is irradiated by energy beam, generate alarm.
25. according to the emission spectrometer of claim 23 or 24, and wherein, drift calibration system generates alarm while can the difference between the known spectra of radiation source and the spectrum of the radiation source being detected by detecting device being greater than threshold value.
26. according to the emission spectrometer of any one in claim 17-25, comprises energy level monitor, and described energy level monitor can monitor the energy level of energy beam, and the signal of the energy level that indication monitors is provided to drift calibration system.
27. according to the emission spectrometer of claim 26, and wherein, described emission spectrometer can generate in the energy level monitoring alarm during lower than threshold energy level.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US201161436328P | 2011-01-26 | 2011-01-26 | |
| US61/436,328 | 2011-01-26 | ||
| PCT/AU2012/000016 WO2012100284A1 (en) | 2011-01-26 | 2012-01-11 | An emission spectrometer and method of operation |
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| Publication Number | Publication Date |
|---|---|
| CN103518121A true CN103518121A (en) | 2014-01-15 |
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| CN201280006560.7A Pending CN103518121A (en) | 2011-01-26 | 2012-01-11 | An emission spectrometer and method of operation |
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| Country | Link |
|---|---|
| CN (1) | CN103518121A (en) |
| AU (1) | AU2012211024A1 (en) |
| BR (1) | BR112013018523A2 (en) |
| CA (1) | CA2824940A1 (en) |
| CL (1) | CL2013002117A1 (en) |
| PE (1) | PE20141402A1 (en) |
| WO (1) | WO2012100284A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018184262A1 (en) * | 2017-04-05 | 2018-10-11 | 华中科技大学 | Dynamic calibration method for echelle spectrometer for laser induced breakdown spectrum collection |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2014202618A2 (en) * | 2013-06-17 | 2014-12-24 | University Of Neuchâtel | Method for determining the configuration of a structure |
| CN115839943B (en) * | 2023-02-13 | 2023-07-11 | 合肥金星智控科技股份有限公司 | Laser-induced spectrum system, spectrum calibration method and electronic equipment |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6621574B1 (en) * | 2000-05-25 | 2003-09-16 | Inphotonics, Inc. | Dual function safety and calibration accessory for raman and other spectroscopic sampling |
| US20060055932A1 (en) * | 2004-08-05 | 2006-03-16 | Mccandless James A | Self-referencing instrument and method thereof for measuring electromagnetic properties |
| US20060055919A1 (en) * | 2004-09-15 | 2006-03-16 | Yuan-Hsiang Lee | Apparatus and method for producing a calibrated raman spectrum |
| US20080315102A1 (en) * | 2006-11-30 | 2008-12-25 | Damien Weidmann | Infrared spectrometer |
| CN101354287A (en) * | 2007-07-24 | 2009-01-28 | 杭州远方光电信息有限公司 | Spectrometer and method for correcting the same |
| CN101689222A (en) * | 2007-05-07 | 2010-03-31 | 真实仪器公司 | Calibration of a radiometric optical monitoring system used for fault detection and process monitoring |
-
2012
- 2012-01-11 AU AU2012211024A patent/AU2012211024A1/en not_active Abandoned
- 2012-01-11 BR BR112013018523A patent/BR112013018523A2/en not_active IP Right Cessation
- 2012-01-11 WO PCT/AU2012/000016 patent/WO2012100284A1/en active Application Filing
- 2012-01-11 PE PE2013001595A patent/PE20141402A1/en not_active Application Discontinuation
- 2012-01-11 CA CA2824940A patent/CA2824940A1/en not_active Abandoned
- 2012-01-11 CN CN201280006560.7A patent/CN103518121A/en active Pending
-
2013
- 2013-07-24 CL CL2013002117A patent/CL2013002117A1/en unknown
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6621574B1 (en) * | 2000-05-25 | 2003-09-16 | Inphotonics, Inc. | Dual function safety and calibration accessory for raman and other spectroscopic sampling |
| US20060055932A1 (en) * | 2004-08-05 | 2006-03-16 | Mccandless James A | Self-referencing instrument and method thereof for measuring electromagnetic properties |
| US20060055919A1 (en) * | 2004-09-15 | 2006-03-16 | Yuan-Hsiang Lee | Apparatus and method for producing a calibrated raman spectrum |
| US20080315102A1 (en) * | 2006-11-30 | 2008-12-25 | Damien Weidmann | Infrared spectrometer |
| CN101689222A (en) * | 2007-05-07 | 2010-03-31 | 真实仪器公司 | Calibration of a radiometric optical monitoring system used for fault detection and process monitoring |
| CN101354287A (en) * | 2007-07-24 | 2009-01-28 | 杭州远方光电信息有限公司 | Spectrometer and method for correcting the same |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018184262A1 (en) * | 2017-04-05 | 2018-10-11 | 华中科技大学 | Dynamic calibration method for echelle spectrometer for laser induced breakdown spectrum collection |
| US10309831B2 (en) | 2017-04-05 | 2019-06-04 | Huazhong University Of Science And Technology | Dynamic calibration method for echelle spectrometer in laser-induced breakdown spectroscopy |
Also Published As
| Publication number | Publication date |
|---|---|
| AU2012211024A1 (en) | 2013-08-01 |
| CA2824940A1 (en) | 2012-08-02 |
| CL2013002117A1 (en) | 2013-12-13 |
| BR112013018523A2 (en) | 2017-08-01 |
| WO2012100284A1 (en) | 2012-08-02 |
| PE20141402A1 (en) | 2014-10-29 |
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