CN104237178B - The method and apparatus of trace metal element in direct-current discharge vaporization auxiliary laser induced breakdown spectroscopy detection water body - Google Patents
The method and apparatus of trace metal element in direct-current discharge vaporization auxiliary laser induced breakdown spectroscopy detection water body Download PDFInfo
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- CN104237178B CN104237178B CN201410526476.9A CN201410526476A CN104237178B CN 104237178 B CN104237178 B CN 104237178B CN 201410526476 A CN201410526476 A CN 201410526476A CN 104237178 B CN104237178 B CN 104237178B
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Abstract
The invention discloses the apparatus and method of trace metal element in a kind of direct-current discharge vaporization auxiliary laser induced breakdown spectroscopy detection water body.Fluid sample is vaporized by HVDC electric discharge, the sample of vaporization is separated by separator, by in gas injection to graphite carrying tablet, graphite carrying tablet containing element to be measured produces plasma by pulse laser ablation induction and launches spectral signal, tested and analyzed eventually through spectrometer, so as to realize the measurement to the trace metal in water body.Using this method and its device, the efficiency of pulse laser ablation sample is greatly improved, and the spectral signal of detection obtains larger enhancing, improves detection sensitivity, the detection limit of metallic element is reduced, feasible method is provided for the metallic element in online efficient, quick detection water body.
Description
Technical field：
It is especially a kind of to be used for Heavy Metals in Waters metal the present invention relates to laser diagnostics and spectral measurement analysis field
Quick detection apparatus and method, the technology can be online to metallic element in industrial wastewater, sanitary sewage, food, medicine
Fast and efficiently detected.
Background technology：
Current water pollution has become global problem, and has a strong impact on children and be grown up healthy or even raw
Life safety, if human body absorbs excessive molybdenum element and can cause gout sample syndrome, arthralgia and deformity, compromised kidneys, and has life
Long hypoevolutism, artery sclerosis, connective tissue denaturation etc. illness.Heavy metal Hg is savings property poisonous substance, except chronic and acute poisoning
Outside, also carcinogenic and mutagenesis, Japanese minamata disease is to be due to caused by methyl mercury is accumulated in people and animals' brain.Cadmium enters human body
Afterwards, cadmium albumen is formed in vivo, whole body is reached by blood circulation, and selectively put aside in target organ-kidney, liver.Chromium
Harm be mainly reflected in intoxicating effect, stimulation, cumulative function, allergy, carcinogenesis and mutagenesis, it is right
The harm of nerve cell is maximum.In order to effectively prevent and reduce heavy metal to human body and biological harm, preserve the ecological environment,
We must strengthen the detection and monitoring of heavy metal element.At present, the method that heavy metal is detected mainly has light splitting light
Degree method, volt-ampere leaching, atomic absorption spectrography (AAS), fluorescent spectrometry and mass spectrography.The need for meeting on-line continuous detection,
It is badly in need of finding the detection method that a kind of sensitivity height, fast and easy, multielement are detected simultaneously.
LIBS (Laser-Induced Breakdown Spectroscopy, LIBS) is a kind of
Brand-new material element analysis method.LIBS technologies have without complicated sample pretreatment, contactless Non-Destructive Testing, quickly
Analysis, multielement real-time online detection, it is not necessary to the features such as vacuum, available for conductive metal material and nonconducting nonmetallic
Material (such as plastics, ceramics) constituent analysis, has extensive in fields such as environmental pollution, archaeology, metallurgy, survey of deep space and medical science
Application prospect.But it is still higher to the detection limit of Water body metallic element using LIBS at present, it is impossible to
Meet the requirement of some field detections.It is conventional at present when being detected using LIBS to fluid sample
Method be to be detected using liquid jet, it was found that, liquid excite produce plasma excitation threshold generally compare
It is larger, and detect the less stable of signal in an experiment, its maximum shortcoming be heavy metal element detection limit compared with
Height, these all constrain the practical application that LIBS is detected to fluid sample.
The content of the invention：
It is an object of the invention to which liquid cathode glow discharge technique is combined with LIBS, drop
The breakdown threshold of low LIBS, improves detection sensitivity, reduces detection limit, meets actual to metallic element
The requirement of detection.Fluid sample is converted into gas by the present invention by HVDC charging method, then through gas-liquid separation device point
From metallic element concentration to be measured is improved, detected finally by LIBS.Due to golden in gaseous sample
Belong to element density small, when being punctured in atmosphere, be easily excited, breakdown threshold can be reduced, ablation efficiency can also obtain pole
Big to improve, because ablation breakdown process is carried out in atmosphere, suffered environmental pressure will be far smaller than in liquid environment
Middle pressure, so the life-span of plasma is also extended, is conducive to causing atomic emission spectrum from continuous radiation and a piece of wood serving as a brake to halt a carriage
Separated in the noise spectrums such as radiation, and then improve detection sensitivity, strengthen signal intensity.
The detection means of the present invention, mainly including peristaltic pump, direct-current discharge device, high-voltage DC power supply, carrier gas supply dress
Put, gas-liquid separator, micro pump, gas buffer room, assemble quartz lens, Nd:YAG pulse lasers, fiber coupling equipment,
Optical fiber, spectrometer, enhanced charge coupled cell (ICCD), computer.Peristaltic pump stably injects fluid sample, direct-current discharge
Device carries out electric discharge to fluid sample and produces high-temperature steam, and it is cold that carrier gas delivery sample vapors enter gas-liquid separator back warp cold water
But, part vapor is separated, and gas enters in surge chamber stabilizing gas flow velocity, gas injection to graphite flake, graphite flake
Generation plasma is excited through pulse laser ablation and launches spectral signal, by the spectrometer with ICCD to the optical signal that is collected into
Light splitting and detection are carried out, eventually through software analysis output spectrum information.
It is a further object to provide a kind of method of metallic element detection.
Realizing the technical scheme that the object of the invention is used is：
The method of trace metal in direct-current discharge vaporization auxiliary laser induced breakdown spectroscopy detection water body.This method is：It is first
First stably sample solution is transported in direct-current discharge device, fluid sample discharged by high-voltage DC power supply, its
Voltage is 900V~1400V, and discharge current is 50mA~110mA, and electrode spacing is 1mm~6mm, and it is height to make fluid sample gasification
Warm steam, high-temperature gas is transported in gas-liquid separator by carrier gas, the cooling and separation of the condensed water of high-temperature gas, and part water steams
Gas is separated, and metallic element concentration to be measured is improved, and the gas containing metallic element to be measured is stable into gas buffer room
Gas flow rate, gaseous sample is ejected on graphite flake by internal diameter for 0.2~2mm nozzle, airflow direction and graphite flake surface
Angle be 30~60 °.The pulse laser of concentrated lens focus excites generation etc. to gas injection position irradiation on meta anthracite
Gas ions simultaneously launch spectral signal, and the optical signal of collection device plasma is collected, by spectrometer light splitting and by ICCD
Detection, finally exports the spectral signal detected by analysis software, realizes the detection to trace metal element in water body.
Brief description of the drawings：
The present invention is further described below in conjunction with the accompanying drawings.
Fig. 1 is the dress that direct-current discharge of the present invention vaporizes trace metal in auxiliary laser induced breakdown spectroscopy detection water body
Structural representation is put, wherein 1,2 be peristaltic pump, 3 be direct-current discharge device, and 4 be high-voltage DC power supply, 5 carrier gas feeding mechanisms, 6
It is micro pump for gas-liquid separator, 7,8 be gas buffer room, and 9 be Nd:YAG pulse lasers, 10 is assemble quartz lens,
11 be graphite flake, 12 fiber coupling devices, and 13 be optical fiber, and 14 be spectrometer, and 15 be enhanced charge coupling device (ICCD),
16 be computer.
Fig. 2 is direct-current discharge apparatus structure schematic diagram, wherein 16 be electric discharge pond, 17 be metal anode, and 18 be electrode spacing
Adjusting knob, 19 be negative electrode, and 20 be inlet nozzle, and 21 be waste liquid outlet, and 22 be carrier gas inlet, and 23 be gaseous sample outlet, 24
It is high-voltage DC power supply for porcelain tube resistance, 25.
Fig. 3 is gas-liquid separation device structural representation, wherein 26 be air inlet, 27 be discharge outlet, 28 water inlets, and 29 be
The mouth of a river, 30 be gas outlet.
Fig. 4 is gas buffer cell structure schematic diagram, wherein 31 be sealed glass jars, 32 be injection port, and 33 be outlet.
Fig. 5 is excitation device schematic diagram, wherein 34 be laser beam, 35 be convergent lens, and 36 be nozzle, and 37 are
Fiber coupler, 38 be graphite flake.
Fig. 6 is HgCl2Solution concentration is respectively 1000 μ g/L, 500 μ g/L, 100 μ g/L, 50 μ g/L spectrogram, A:Hg
Atom 253.65nm characteristic spectral lines.
Embodiment：
Referring now to brief description of the drawings one embodiment of the present of invention.
Inventor completes following experiments, using described invention device to HgCl2Hg elements in solution are examined
Survey.
First, the sample solution in sample bottle is transported in direct-current discharge device 3 by peristaltic pump 1, the flow velocity of peristaltic pump 1
For 8.7mL/min, the negative electrode 19 of electric discharge device 3 is connected after current-limiting resistance 24 (2.7k Ω) with the negative pole of high-voltage DC power supply 25,
The positive pole of high-voltage DC power supply 25 and solid tungsten bar (a diameter of 2mm, end into 15 ° of cone angles) anode 17 is connected, specific on-link mode (OLM)
As shown in Figure 2.In experiment, apply 1200V voltages between liquid cathode 19 and tungsten bar anode 17, the air of two interpolars can be breakdown,
Produce atmospheric pressure plasma, at the same time fluid sample is gasified as high-temperature steam, by electrode spacing adjusting knob 18 come
Electrode spacing is adjusted, it is 80mA to make discharge current, the waste liquid produced after electric discharge is excluded through peristaltic pump 2.Carrier gas feeding mechanism 5 is provided
High-temperature steam is sent in gas-liquid separator 6 by carrier gas (air), and Fig. 3 gives the concrete structure of gas-liquid separator 6, gas from
Air inlet 26 enters gas-liquid separation device, simultaneously micro pump by cold water from water inlet 28 is input to device, finally from
Delivery port 29 is exported, and the flow velocity of micro pump 7 is 0.75L/min, gaseous sample by during the inner tube of gas-liquid separator by cold water
Part vapor in cooling, gas is separated to be flowed out from discharge outlet 27, and the gas after separation is exported by gas outlet 30.
In order that the gas flow rate after processing is stable, the gas after separation is passed into gas buffer room 8, gas buffer
The concrete structure of room is exported from outlet 33 as shown in figure 4, gas is inputted by injection port 32.
The gas exported from gas buffer room 8 is sprayed by internal diameter for 2mm nozzle 36, sprays air-flow and the table of graphite flake 38
Face is in 45 °.The Nd of 1064nm wavelength:To gas on meta anthracite after the concentrated focusing of lens 35 of the output laser 34 of YAG pulse lasers 9
Body eject position carries out ablation, and laser single-pulse energy is 16mJ, excites generation plasma and launches spectral signal, Ran Houyou
Collection device 10 and 12 is collected and is delivered to spectrometer 14 by optical fiber 13, after the light splitting of spectrometer 14, then through ICCD detectors
15 detection outputs (gain is 500, is delayed as 0.7 μ s, and gate-width is 10 μ s), are finally handled by analysis software, pass through and calculate
The output spectrum information of machine 16.Fig. 6 is the various concentrations HgCl detected using the invention device2Hg solution atom 253.65nm
Characteristic spectral line intensity.
Claims (10)
1. the method for metallic element in direct-current discharge vaporization auxiliary laser induced breakdown spectroscopy detection water body, it is characterised in that：It is first
FirstPass through the adjustable peristaltic pump of speedFluid sample is stably injected,Using metal as anode, using liquid as negative electrode,Using straight
Banishing electric installation makes fluid sample produce high-temperature steam fluid sample progress electric discharge,The waste liquid produced after electric discharge is defeated through peristaltic pump Go out,Carrier gas carrying high temperature steam enters gas-liquid separator, the gas containing element to be measured through gas-liquid separator separates,Micro pump to Gas-liquid separator injection cold water carrys out cooling down high-temperature steam, and part vapor is separated,Gas after separationInto buffering After the stable flow velocity in roomIt is ejected on graphite flake, wherein, gas injection direction and graphite flake surface are into 30°~60 °, lured by laser
Lead puncture device and excite the steam being sprayed on around graphite flake, plasma emission spectroscopy signal is produced, finally by spectral detection
Device is analyzed spectral signal, so as to realize the detection to trace metal element in water body.
2. trace metal member in direct-current discharge vaporization auxiliary laser induced breakdown spectroscopy detection water body according to claim 1
The method of element, it is characterised in that make it be changed into gaseous state from liquid sample electric discharge using liquid cathode glow discharge device, then by
LIBS is detected, realizes the detection to metallic element in water body.
3. trace metal member in direct-current discharge vaporization auxiliary laser induced breakdown spectroscopy detection water body according to claim 1
The method of element, it is characterised in that metallic element concentration to be measured in gas is improved by gas-liquid separator.
4. the detection means that detection method according to claim 1 is designed, the device is characterised by：The device passes through
The adjustable peristaltic pump of speed stably injects fluid sample, and high-voltage DC power supply provides voltage for electric discharge device, using metal as
Anode, using liquid as negative electrode, carries out electric discharge to fluid sample and produces high-temperature steam, the waste liquid produced after electric discharge is defeated through peristaltic pump
Go out, micro pump carrys out cooling down high-temperature steam to gas-liquid separator injection cold water, and part vapor is separated, and gas enters slow
Rush in the stable flow velocity in room, gas injection to graphite flake, the pulse laser of concentrated lens focus is to gas injection position on meta anthracite
Irradiation is put to excite generation plasma and launch spectral signal, the spectrometer with ICCD optical signal being collected into is carried out light splitting with
Detection.
5. direct-current discharge vaporization auxiliary laser induced breakdown spectroscopy detects trace metal element in water body according to claim 4
Device, it is characterised in that the internal diameter of the inner tube of the gas-liquid separation device be 2~3mm, 2~4mm of thickness, outer tube diameter is 10
~20mm, external diameter is 20mm, and whole device length is 200~400mm.
6. direct-current discharge gasification auxiliary laser induced breakdown spectroscopy detects trace metal element in water body according to claim 4
Device, it is characterised in that described gas buffer room and gas-liquid separator are connected with airway tube, and gas buffer room has two to lead
Tracheae, wherein air inlet pipe are passed into close to bottom of bottle position, and the escape pipe mouth of pipe is close to bottleneck, and air guide bore is 5~10mm, buffering
Device makes gaseous sample flow speed stability.
7. direct-current discharge vaporization auxiliary laser induced breakdown spectroscopy detects trace metal element in water body according to claim 4
Device, it is characterised in that the pulse laser be Nd：YAG pulse lasers, laser output wavelength is 1064nm, 532nm
Or 266nm, pulsed laser energy is 10mJ~100mJ.
8. direct-current discharge vaporization auxiliary laser induced breakdown spectroscopy detects trace metal element in water body according to claim 4
Device, it is characterised in that gas nozzle internal diameter size is in 0.2~2mm scopes, the angle of gas injection direction and graphite surface
For 30~60 °.
9. direct-current discharge vaporization auxiliary laser induced breakdown spectroscopy detects trace metal element in water body according to claim 4
Device, it is characterised in that laser pulse active position is in gas injection to graphite place-centric.
10. trace metal is first in direct-current discharge vaporization auxiliary laser induced breakdown spectroscopy detection water body according to claim 4
The device of element, it is characterised in that the spectrometer includes ICCD, and ICCD delays are in the selection of 200ns~2000ns scopes, ICCD
It is wide to be selected between the μ s of 1 μ s~50.
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