CN101592608A - The method for quick of multichannel Laser-induced Breakdown Spectroscopy - Google Patents

The method for quick of multichannel Laser-induced Breakdown Spectroscopy Download PDF

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Publication number
CN101592608A
CN101592608A CNA2009100408132A CN200910040813A CN101592608A CN 101592608 A CN101592608 A CN 101592608A CN A2009100408132 A CNA2009100408132 A CN A2009100408132A CN 200910040813 A CN200910040813 A CN 200910040813A CN 101592608 A CN101592608 A CN 101592608A
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China
Prior art keywords
sample
laser
light
quick
induced breakdown
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CNA2009100408132A
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Inventor
周伦彬
蔡永洪
王自鑫
陆林轩
周建英
李润华
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Guangzhou City Institute Of Measurement Detection Technology
South China University of Technology SCUT
National Sun Yat Sen University
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Guangzhou City Institute Of Measurement Detection Technology
South China University of Technology SCUT
National Sun Yat Sen University
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Priority to CNA2009100408132A priority Critical patent/CN101592608A/en
Publication of CN101592608A publication Critical patent/CN101592608A/en
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Abstract

The invention discloses a kind of method for quick of multichannel Laser-induced Breakdown Spectroscopy, this method comprises the steps: A. laser instrument output laser at least and shines on the sample, outwards launches light when the sample interior element decomposes; B. the emission light that spreads out of from sample is imported in the monochromator, through being spread out of by each outgoing seam respectively behind the grating polarization; C. each photo-electric conversion element is converted to electric signal respectively with the light at outgoing seam place, respectively photosignal is transferred to signal processing apparatus again, simultaneously each signal is handled by signal processing apparatus.The present invention can detect at least two kinds of elements, and detection speed is fast, and the cost of pick-up unit is low.

Description

The method for quick of multichannel Laser-induced Breakdown Spectroscopy
Technical field
The present invention relates to a kind of method for quick of multichannel Laser-induced Breakdown Spectroscopy.
Background technology
Heavy metal element in industrial and agricultural products or the environment is (as lead, mercury, cadmium, chromium, copper, manganese ...) having had a strong impact on the healthy of the mankind, a spot of lead, mercury, cadmium or chromium can cause acute poisoning.Medical evidence, the lead of oral 2-3 gram can cause poisoning, and 50 grams can cause death.And if trace heavy metals long-term accumulation in vivo also can cause slow poisoning, cause organ dysfunction decline and immune system disorder.So European Union's concentration of lead, chromium, cadmium and the mercury four heavy metal species elements in all electronic products has for a long time made regulation, i.e. ROHS standard, wherein plumbous, mercury of regulation and positive hexavalent chromium concentration must not surpass 1000ppm, and cadmium concentration must not surpass 100ppm.
The technological means that is used for the detection by quantitative micro heavy at present mainly contains X-ray fluorescence method, atomic absorption spectroscopy and inductively coupled plasma atomic emission spectrum technology.Wherein X-ray fluorescence method can be realized fast detecting, but its sensitivity is lower; The accuracy of detection height of atomic absorption spectroscopy and inductively coupled plasma atomic emission spectrum technology, good stability, but because apparatus expensive, sample pre-treatments is time-consuming, generally needs a couple of days, is difficult to widely apply.
The Laser-induced Breakdown Spectroscopy technology is a kind of novel spectral detection means, it is widely used in for example soil, water body, alloy, fruit and vegetable, pigment, antique historical relic etc. being carried out ultimate analysis in the fields such as environmental pollution monitoring, industrial products detection, food quality detection and archaeology analysis.It has simple fast, need not sample pretreatment, to sample damage little and wide accommodation, be convenient to advantage such as remote control, particularly its characteristics that need not sample pre-treatments have very big advantage.
The principle of Laser-induced Breakdown Spectroscopy technology: Laser-induced Breakdown Spectroscopy is as a kind of detection technique, its principle is to sample surfaces with pulse laser focusing, atom in the sample is owing to absorb photon energy and the effect of electronic atom collision, produced " puncture " effect and formed high-temperature plasma, part of atoms or ion transition are to the high-energy attitude in this process; After laser pulse finished, plasma cooled off rapidly, was in the atom of high-energy attitude or ion this moment and got back to ground state and give off characteristic spectrum owing to transition.Can carry out qualitative or quantitative test to element contained in the sample by studying this spectrum.
The atomic radiation of Laser-induced Breakdown Spectroscopy is only very faint, can't use common lens to gather through the spectrum that launches after grating or the prismatic decomposition, because its insufficient sensitivity.Gather Laser-induced Breakdown Spectroscopy at present both at home and abroad and mainly use two kinds of means: first, use hyperchannel multiplication imager to gather spectrum, so just can disposable whole spectrum be collected, realize the disposable detection of multielement, but shortcoming is a hyperchannel multiplication imager to cost an arm and a leg, and need to be equipped with relevant liquid nitrogen refrigerating system, be difficult to bear for common laboratory or production mechanism; Second, use the collection of photomultiplier single channel, this method must add a slit (promptly becoming monochromator) at the exit end of grating beam splitting spectrum, can only gather the light intensity of a wavelength at every turn, and will be detecting a plurality of elements, then need rotating shutter to change output wavelength, gather simultaneously so can't realize multielement.
Summary of the invention
The object of the present invention is to provide a kind of method for quick of multichannel Laser-induced Breakdown Spectroscopy.The present invention can detect at least two kinds of elements, and detection speed is fast, and the cost of pick-up unit is low.
Pick-up unit structure of the present invention is:
A kind of device for fast detecting of multichannel Laser-induced Breakdown Spectroscopy, comprise laser instrument, sample placement position, optical communication means, monochromator and signal processing apparatus, laser instrument is placed the position towards sample, on monochromator, be provided with incident seam and outgoing seam, the place is provided with photo-electric conversion element at the outgoing seam, and photo-electric conversion element and signal processing apparatus are electrically connected; The described outgoing seam of being located at described monochromator end is at least two, is equipped with described photo-electric conversion element at these at least two outgoing seam places, and each photo-electric conversion element all is electrically connected with described signal processing apparatus.
Described photo-electric conversion element is a photomultiplier.
Be provided with convex lens between described laser instrument and described sample placement position, described optical communication means is an optical fiber.
It is two-dimentional mobile platform that described sample is placed the position, and promptly the sample mounting table can produce slight mobilely, avoids crossing and forming hole for a long time owing to laser radiation, and then influences the ejaculation of plasma.
Described color analyzer also comprises first concavees lens, second concavees lens, inverse mirror and grating, and the light of injecting from incident seam behind catoptron, first concavees lens, grating and second concavees lens, spreads out of through described outgoing seam successively again.
Described signal processing apparatus comprises modulus acquisition module and computing machine, and modulus acquisition module and computing machine are electrically connected, and described two photo-electric conversion elements and modulus acquisition module are electrically connected.
Described outgoing seam and photomultiplier are four.
Place the position side at described product to be tested and also be provided with photoelectric switch, this photoelectric switch and described signal processing apparatus are electrically connected.When laser instrument arrived product to be tested with laser radiation, photoelectric switch sent a synchronizing signal for the modulus acquisition module, so that modulus acquisition module and laser instrument are synchronous.
The method for quick of multichannel Laser-induced Breakdown Spectroscopy of the present invention comprises the steps: at least
A, laser instrument output laser planoconvex lens shine on the sample after focusing on, and outwards launch light when the sample interior element decomposes;
B, the emission light that spreads out of from sample stitch through the incident that optical fiber imports monochromator into, to launch the light criterion through mirror reflects, first concavees lens successively again is directional light, directional light is focused on by second concavees lens through grating polarization again, and the light of focusing is injected respectively in four outgoing seams;
The light that the photo-electric conversion element at C, four outgoing seam places will be located respectively is converted to electric signal, simultaneously each signal is handled by signal processing apparatus again.
In sum, advantage of the present invention is: the present invention is provided with four outgoing seams on monochromator, the wavelength of respectively corresponding lead, chromium, cadmium and mercury four heavy metal species elements, when detecting, can disposablely carry out check and analysis to four heavy metal species elements in the sample, analysis speed greatly improves, and the cost of pick-up unit is low simultaneously.
Description of drawings
Fig. 1 is the structural representation of detection method detection device thereof of the present invention;
Fig. 2 is among Fig. 1, the partial enlarged drawing of monochromator;
Fig. 3 is the process flow diagram of detection method of the present invention;
Description of reference numerals:
1, laser instrument, 2, sample places the position, 3, monochromator, 4, the modulus acquisition module, 5, computing machine, 6, sample, 7, convex lens, 8, first concavees lens, 9, second concavees lens, 10, catoptron, 11, grating, 12, photoelectric switch, 13, incident seam, 14, first outgoing seam, 15, second outgoing seam, the 16, the 3rd outgoing seam, 17, the 4th outgoing seam, 18, first photomultiplier, 19, second photomultiplier, 20, the 3rd photomultiplier, the 21, the 4th photomultiplier, 22, optical fiber.
Embodiment
As Fig. 1 to the structure that Figure 2 shows that detection method detection device thereof of the present invention, a kind of device for fast detecting of multichannel Laser-induced Breakdown Spectroscopy, comprise laser instrument 1, sample placement position 2, optical communication means, monochromator 3 and signal processing apparatus, laser instrument 1 is placed position 2 towards sample, on monochromator 3, be provided with incident seam 13 and outgoing seam, the place is provided with photo-electric conversion element at the outgoing seam, and photo-electric conversion element and signal processing apparatus are electrically connected; The described outgoing seam of being located at described monochromator 3 ends is at least two, is equipped with described photo-electric conversion element at these at least two outgoing seam places, and each photo-electric conversion element all is electrically connected with described signal processing apparatus.
Wherein, described outgoing seam is four (first outgoing seam, 14, second outgoing seam the 15, the 3rd outgoing seam the 16, the 4th outgoing seams 17), and it is photomultiplier (first photomultiplier 18, second photomultiplier 19, the 3rd photomultiplier 20, the 4th photomultiplier 21) that four outgoing seam places are provided with four photo-electric conversion elements respectively.
It is two-dimentional mobile platform that described sample is placed position 2, is provided with convex lens 7 between described laser instrument 1 and described sample placement position 2, and described optical communication means is an optical fiber 22; Described color analyzer also comprises first concavees lens 8, second concavees lens 9, inverse mirror and grating 11, and the light of injecting from incident seam behind catoptron 10, first concavees lens 8, grating 11 and second concavees lens 9, spreads out of through four outgoing seams respectively successively again.Described signal processing apparatus comprises modulus acquisition module 4 and computing machine 5, and modulus acquisition module 4 is electrically connected with computing machine 5, and described two photo-electric conversion elements and modulus acquisition module 4 are electrically connected.Sample is placed position 2 sides and also is provided with photoelectric switch 12, and this photoelectric switch 12 is electrically connected with modulus acquisition module 4.
Be illustrated in figure 3 as the process flow diagram of the method for quick of multichannel Laser-induced Breakdown Spectroscopy of the present invention, it comprises the steps:
A, laser instrument 1 output laser planoconvex lens 7 shine on the sample 6 after focusing on, and outwards launch light when sample 6 interior elements decompose;
B, the emission light that spreads out of from sample 6 stitch through the incident that optical fiber 22 imports monochromator 3 into, to launch the light criterion through catoptron 10 reflections, first concavees lens 8 successively again is directional light, directional light is through grating 11 polarizations, focused on by second concavees lens 9, the light of focusing is injected respectively in four outgoing seams again;
The light that the photo-electric conversion element at C, four outgoing seam places will be located respectively is converted to electric signal, simultaneously each signal is handled by signal processing apparatus again.
In sum, the advantage of present embodiment is: be provided with four outgoing seams on monochromator 3, the wavelength of respectively corresponding lead, chromium, cadmium and mercury four heavy metal species elements, when detecting, can disposablely carry out check and analysis to four heavy metal species elements in the sample 6, analysis speed greatly improves, and the cost of pick-up unit is low simultaneously.
Be preferred embodiment of the present invention only below, do not limit protection scope of the present invention with this; Any replacement and the improvement done on the basis of not violating the present invention's design all belong to protection scope of the present invention.

Claims (3)

1, the method for quick of multichannel Laser-induced Breakdown Spectroscopy is characterized in that, this method comprises the steps: at least
A, laser instrument output laser also shine on the sample, outwards launch light when the sample interior element decomposes;
In B, the emission light input monochromator that spreads out of from sample, through spreading out of by each outgoing seam respectively behind the grating polarization;
C, each photo-electric conversion element are converted to electric signal respectively with the light at outgoing seam place, respectively photosignal are transferred to signal processing apparatus again, simultaneously each signal are handled by signal processing apparatus.
2, the method for quick of multichannel Laser-induced Breakdown Spectroscopy according to claim 1 is characterized in that, in the step A, shines on the described sample after described laser instrument output laser planoconvex lens focuses on again.
3, the method for quick of multichannel Laser-induced Breakdown Spectroscopy according to claim 1, it is characterized in that, in the step B, the emission light that spreads out of from described sample stitches through the incident that optical fiber imports monochromator into, the light of injecting through incident seam behind catoptron, first concavees lens, grating and second concavees lens, spreads out of through described outgoing seam respectively successively again.
CNA2009100408132A 2009-07-03 2009-07-03 The method for quick of multichannel Laser-induced Breakdown Spectroscopy Pending CN101592608A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102313731A (en) * 2010-07-09 2012-01-11 中国科学院沈阳自动化研究所 Method for detecting content of component in unknown object on line
CN103616351A (en) * 2013-11-26 2014-03-05 中国科学院广州地球化学研究所 Laser-induced breakdown spectroscopy analyzer and laser-induced breakdown spectroscopy analysis method
CN104034703A (en) * 2014-06-12 2014-09-10 中国科学院上海技术物理研究所 Improved system and method for detecting composition of material by LIBS (Laser Induced Breakdown Spectroscopy) with high signal and noise ratio and low detection limit
CN104297218A (en) * 2013-07-15 2015-01-21 中国科学院沈阳自动化研究所 In situ on-line detection device and method for remote metallurgy liquid metal component
CN106725309A (en) * 2016-11-29 2017-05-31 中国科学院长春光学精密机械与物理研究所 High speed frequency-sweeping laser source sweep characteristic verifies device
CN108051410A (en) * 2017-10-31 2018-05-18 浙江农林大学 A kind of tobacco root cadmium content rapid detection method based on laser induced breakdown spectroscopy
CN109001184A (en) * 2018-08-07 2018-12-14 中国海洋大学 A kind of rotary scanning type element detection device based on LIBS technology

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102313731A (en) * 2010-07-09 2012-01-11 中国科学院沈阳自动化研究所 Method for detecting content of component in unknown object on line
CN102313731B (en) * 2010-07-09 2012-12-26 中国科学院沈阳自动化研究所 Method for detecting content of component of unknown object on line
CN104297218A (en) * 2013-07-15 2015-01-21 中国科学院沈阳自动化研究所 In situ on-line detection device and method for remote metallurgy liquid metal component
CN104297218B (en) * 2013-07-15 2016-09-14 中国科学院沈阳自动化研究所 The remote original position of components of metallurgical liquid metal, on-line measuring device and method
CN103616351A (en) * 2013-11-26 2014-03-05 中国科学院广州地球化学研究所 Laser-induced breakdown spectroscopy analyzer and laser-induced breakdown spectroscopy analysis method
CN104034703A (en) * 2014-06-12 2014-09-10 中国科学院上海技术物理研究所 Improved system and method for detecting composition of material by LIBS (Laser Induced Breakdown Spectroscopy) with high signal and noise ratio and low detection limit
CN106725309A (en) * 2016-11-29 2017-05-31 中国科学院长春光学精密机械与物理研究所 High speed frequency-sweeping laser source sweep characteristic verifies device
CN108051410A (en) * 2017-10-31 2018-05-18 浙江农林大学 A kind of tobacco root cadmium content rapid detection method based on laser induced breakdown spectroscopy
CN109001184A (en) * 2018-08-07 2018-12-14 中国海洋大学 A kind of rotary scanning type element detection device based on LIBS technology

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Open date: 20091202