CN104111249A - Highly-sensitive rapid detection device for elements in liquid - Google Patents

Highly-sensitive rapid detection device for elements in liquid Download PDF

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Publication number
CN104111249A
CN104111249A CN201410343007.3A CN201410343007A CN104111249A CN 104111249 A CN104111249 A CN 104111249A CN 201410343007 A CN201410343007 A CN 201410343007A CN 104111249 A CN104111249 A CN 104111249A
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liquid
rapid detection
detection device
cylindrical container
pulse
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CN201410343007.3A
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周卫东
苏雪娇
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Zhejiang Normal University CJNU
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Zhejiang Normal University CJNU
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Abstract

The invention discloses a highly-sensitive rapid detection device for elements in liquid. The highly-sensitive rapid detection device comprises a YAG (yttrium-aluminum-garnet) laser, a focusing lens, optical fibers, a spectrograph, a trigger and a computer. The highly-sensitive rapid detection device for the elements in the liquid is characterized by being internally provided with a system composed of a vacuum cavity body and a pulse sampling device, and the vacuum cavity body and the pulse sampling device are connected through a guide tube. The device has obvious characteristics that liquid column samples with different diameters are rapidly detected in a vacuum environment, on one hand, the limit of ambient gas to plasma expansion and interference of an air background spectrum to a plasma spectrum are reduced in the vacuum environment, on the other hand, the liquid is excited by lasers in a form of a thin liquid column, so as to overcome negative effects of liquid level fluctuation and atomic radiation quenching and facilitate the laser induction to generate strong and stable plasma radiation, and additionally, the controllable pulse liquid column samples are adopted, so that the detection stability can be improved and the sample consumption can be reduced.

Description

Element high-sensitivity rapid detection device in a kind of liquid
Technical field
The invention belongs to Laser-induced Breakdown Spectroscopy technology material element analysis field, be specifically related to element high-sensitivity rapid detection device in a kind of liquid.
Background technology
Along with the development of modern industry, China is in the exploitation of heavy metal, smelting, process, because failing to do suitable processing, cause many heavy metals to enter in atmosphere, water, soil, cause serious harm to ecologic environment, wherein the heavy metal pollution of water environment is especially outstanding, is therefore necessary heavy metal element in water to detect.At present, water environment heavy metal detects technology used electrochemical analysis, atomic absorption spectroscopy (AAS), inductively coupled plasma atomic emission (ICP-AES) and inductively coupled plasma mass spectrometry mass spectroscopy (ICP-MS) etc.These methods all need additive reagent sample to be separated or enrichment processing substantially, make testing process become complicated and consuming time, and meanwhile, additive reagent is often harmful to environment, must cause producing in testing process secondary pollution.And above-mentioned method is except ICP-AES, other method can only detect single sample at every turn, although and ICP-AES method can one-time detection several samples, the method needs complicated pretreatment operation.Therefore develop a kind of Heavy Metal Pollution in Water Environment detection technique quick, real-time, that can simultaneously detect multiple element and just seem particularly necessary.
Laser-induced Breakdown Spectroscopy technology (LIBS) is as a kind of new material element detection technique, due to have the amount that do not need the sample to carry out pre-service, required sample seldom, research object pollute again probability little, can carry out the advantages such as on-line analysis to multiple element simultaneously, be widely used in the fields such as water, soil and air pollution, just developing into a kind of material composition detection technique that has application prospect.The detection of LIBS in gas and solid at present has higher stability and sensitivity, even realized commercialization.But, when detection in fluid sample, thereby because the negative effects such as liquid fluctuating and atomic radiation cancellation cause the detection sensitivity of LIBS in liquid very low.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, element high-sensitivity rapid detection device in a kind of liquid has been proposed, the outstanding feature of this device is to utilize the fluid column sample to different-diameter under vacuum environment to carry out fast detecting, and vacuum environment has reduced the restriction of ambient gas article on plasma measure expansion and the interference of air background spectral line plasma spectrum on the one hand; Liquid, with the form of thin fluid column by laser excitation, has overcome the negative effect such as liquid fluctuating and atomic radiation cancellation on the other hand, is conducive to induced with laser and produces stronger and stable plasma resonance; Moreover, adopt controlled pulse fluid column sample, be conducive to improve the stability detecting and reduce sample consumption.This device has improved the sensitivity of element tracer liquid effectively from above three aspects.
Concrete technical scheme of the present invention is:
In a kind of liquid, element high-sensitivity rapid detection device comprises YAG laser instrument, condenser lens, optical fiber, spectrometer, trigger and computing machine, it is characterized in that in described a kind of liquid, element high-sensitivity rapid detection device is provided with a system being made up of vacuum cavity and pulse sample injection device, vacuum cavity is connected by conduit with pulse sample injection device.
Described vacuum cavity is by cylindrical container, receive sampling device, patterning device and vacuum pump form, cylindrical container lower right is connected by conduit with vacuum pump, receive sampling device and be positioned at cylindrical container bottom, also be connected by conduit with outside patterning device, it is symmetrical between two all around that right cylinder side is provided with four transparent windows, pulse laser is by condenser lens window transmission through the right after the window on the cylindrical container left side focuses on fluid column center, window is equipped with a condenser lens below, optical fiber is gathered spectrum and is delivered to computing machine by these lens, window can be observed spectra collection situation above.
Described pulse sample injection device is made up of sampling receptacle, electric control pulse valve and removable tiny pin hole, electric control pulse valve is positioned on the conduit that is connected sampling receptacle and cylindrical container successively with removable tiny pin hole, formation and duration that electric control pulse valve can be controlled fluid column make it to synchronize with pulse laser, and the selection range of pinhole diameter is 50um-1mm.
The conduit that described vacuum pump is connected with cylindrical container with patterning device is all equipped with controlled valve, and while ensureing to detect, cylindrical container inside is vacuum environment.
The process of using pick-up unit of the present invention to detect is as follows:
Open vacuum pump valve, utilize vacuum pump to realize chamber vacuum environment.Vacuum cavity internal gas pressure is low, and sampling device sampling receptacle is connected with outside atmosphere, atmospheric pressure acts on liquid level, due to the poor effect of external and internal pressure, make in the time that in sampling device, impulse valve is opened, liquid penetrates from pin hole, form jet fluid column, the switching time of regulating impulse valve and duration, can make the fluid column spraying near laser interaction pin hole and after lens focus, the plasma spectrometry producing is equipped with the collection window collection of condenser lens and is entered in spectrometer through optical fiber transmission, spectrometer further transfers data to computing machine and processes and analyze.
Brief description of the drawings
Fig. 1 is element high-sensitivity rapid detection device in a kind of liquid of the present invention.
Wherein cylindrical container 1, sampling receptacle 2, receipts sampling device 3, patterning device 4, vacuum pump 5, spectrometer 6, computing machine 7, DG535 trigger 8, YAG laser instrument 9, optical fiber 10, condenser lens 11, pin hole 12, collection window 13, optical transmission window 14, watch window 15, light portal 16, electric control pulse valve 17.
Embodiment
Below in conjunction with accompanying drawing, the present invention is further illustrated:
Element high-sensitivity rapid detection device in a kind of liquid, comprise YAG laser instrument 9, condenser lens 11, optical fiber 10, spectrometer 6, DG535 trigger 8 and computing machine 7, it is characterized in that in described a kind of liquid, element high-sensitivity rapid detection device is provided with a system being made up of vacuum cavity and pulse sample injection device, vacuum cavity is connected by conduit with pulse sample injection device.
Described vacuum cavity is by cylindrical container 1, receive sampling device 3, patterning device 4 and vacuum pump 5 form, on cylindrical container, 1 lower right is connected by conduit with vacuum pump 5, receive sampling device 3 and be positioned at cylindrical container 1 bottom, also be connected by conduit with outside patterning device 4, it is symmetrical between two all around that cylindrical container 1 side is provided with four transparent windows, pulse laser is by condenser lens optical transmission window 14 transmissions through the right after the light portal 16 on cylindrical container 1 left side focuses on fluid column center, collection window 13 is equipped with a condenser lens below, optical fiber 10 is gathered spectrum and is delivered to computing machine 7 by these lens, watch window 15 can be observed spectra collection situation above.Described pulse sample injection device is made up of sampling receptacle 2, electric control pulse valve 17 and removable tiny pin hole 12, electric control pulse valve 17 is positioned on the conduit that is connected sampling receptacle 2 and cylindrical container 1 successively with removable tiny pin hole 12, formation and duration that electric control pulse valve 17 can be controlled fluid column make it to synchronize with pulse laser, and the selection range of pin hole 12 diameters is 50um-1mm.
In sampling receptacle 2, inject the fluid sample that will detect, close the switch gate of electric control pulse valve 17 and patterning device 4, open vacuum pump 5 cylindrical container 1 is evacuated.DG535 trigger 8 sends trigger pulse gating pulse valve 17 and opens, and the outgoing from pin hole 12 under the poor effect of external and internal pressure of the liquid in sampling receptacle 2 forms jet fluid column.Open pulsed laser 9, under the control of DG535 trigger 8, laser beam line focus lens 11 enter cylindrical container 1 by the light portal 16 on the left side, regulate DG535 trigger 8, pulse laser is all interacted near pin hole with the fluid column spraying at every turn, and focus on fluid column center.The collection window 13 that the plasma spectrometry that induced with laser fluid column produces is equipped with condenser lens is collected and imports in spectrometer 6 and send into computing machine 7 and carry out processing and the analysis of material element through optical fiber 10.Observe collection situation at watch window 15, in the time that the liquid in receipts sampling device 3 reaches a certain amount of, open the controlled valve of patterning device 4 and discharge sample.In experiment, change the diameter of fluid column by changing the diameter of pin hole 12, to obtain the most stable spectrum.

Claims (4)

1. in a liquid, element high-sensitivity rapid detection device comprises YAG laser instrument, condenser lens, optical fiber, spectrometer, trigger and computing machine, it is characterized in that in described a kind of liquid, element high-sensitivity rapid detection device is provided with a system being made up of vacuum cavity and pulse sample injection device, vacuum cavity is connected by conduit with pulse sample injection device.
2. element high-sensitivity rapid detection device in a kind of liquid according to claim 1, it is characterized in that, vacuum cavity is by cylindrical container, receive sampling device, patterning device and vacuum pump form, cylindrical container lower right is connected by conduit with vacuum pump, receive sampling device and be positioned at cylindrical container bottom, also be connected by conduit with outside patterning device, it is symmetrical between two all around that right cylinder side is provided with four transparent windows, pulse laser is by condenser lens window transmission through the right after the window on the cylindrical container left side focuses on fluid column center, window is equipped with a condenser lens below, optical fiber is gathered spectrum and is delivered to computing machine by these lens, window can be observed spectra collection situation above.
3. element high-sensitivity rapid detection device in a kind of liquid according to claim 1, it is characterized in that, described pulse sample injection device is made up of sampling receptacle, electric control pulse valve and removable tiny pin hole, electric control pulse valve is positioned on the conduit that is connected sampling receptacle and cylindrical container successively with removable tiny pin hole, formation and duration that electric control pulse valve can be controlled fluid column make it to synchronize with pulse laser, and the selection range of pinhole diameter is 50um-1mm.
4. element high-sensitivity rapid detection device in a kind of liquid according to claim 2, it is characterized in that, the conduit that described vacuum pump is connected with cylindrical container with patterning device is all equipped with controlled valve, and while ensureing to detect, cylindrical container inside is vacuum environment.
CN201410343007.3A 2014-07-12 2014-07-12 Highly-sensitive rapid detection device for elements in liquid Pending CN104111249A (en)

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Cited By (5)

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Publication number Priority date Publication date Assignee Title
CN104502330B (en) * 2014-12-12 2017-06-27 大连理工大学 A kind of LIBS detection means for detecting fluid sample
CN107917901A (en) * 2017-11-01 2018-04-17 青岛大学 A kind of method and apparatus of fluid sample elemental composition on-line checking
CN108444982A (en) * 2018-04-26 2018-08-24 安徽师范大学 A kind of fluidic device for laser induced breakdown spectroscopy
CN112378897A (en) * 2020-11-05 2021-02-19 石家庄职业技术学院(石家庄广播电视大学) Food production heavy metal detection device
CN115201179A (en) * 2022-06-27 2022-10-18 北京市农林科学院信息技术研究中心 Device and method for detecting nutrient elements in plant nutrient solution

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104502330B (en) * 2014-12-12 2017-06-27 大连理工大学 A kind of LIBS detection means for detecting fluid sample
CN107917901A (en) * 2017-11-01 2018-04-17 青岛大学 A kind of method and apparatus of fluid sample elemental composition on-line checking
CN108444982A (en) * 2018-04-26 2018-08-24 安徽师范大学 A kind of fluidic device for laser induced breakdown spectroscopy
CN112378897A (en) * 2020-11-05 2021-02-19 石家庄职业技术学院(石家庄广播电视大学) Food production heavy metal detection device
CN112378897B (en) * 2020-11-05 2023-03-10 石家庄职业技术学院(石家庄广播电视大学) Food production heavy metal detection device
CN115201179A (en) * 2022-06-27 2022-10-18 北京市农林科学院信息技术研究中心 Device and method for detecting nutrient elements in plant nutrient solution

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Application publication date: 20141022