CN107894511A - A kind of Elemental Speciation Analysis instrument - Google Patents
A kind of Elemental Speciation Analysis instrument Download PDFInfo
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- CN107894511A CN107894511A CN201711026654.1A CN201711026654A CN107894511A CN 107894511 A CN107894511 A CN 107894511A CN 201711026654 A CN201711026654 A CN 201711026654A CN 107894511 A CN107894511 A CN 107894511A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/00584—Control arrangements for automatic analysers
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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Abstract
The invention discloses a kind of Elemental Speciation Analysis instrument of technical field of analytical instruments, including the positive and negative valence state electrophoretic separation device of sampling device, valence state separation chromatogram arrangement, direct current, Relative-State intervention device, Electrochemical hydriding device, gaseous hydride stability to derive transition device, AFS and liquid waste treating apparatus.The present invention separates mode derived from hydrogenated thing using high performance liquid chromatography electrophoresis valence state and carries out sample pre-treatments, detected subsequently into atomic fluorescence spectrophotometry, solve the problems, such as existing elemental analyser poor reproducibility, sensitivity is low, morphological data is inaccurate, while avoid cumbersome sample pretreatment process.
Description
Technical field
The present invention relates to a kind of analytical instrument, specially a kind of Elemental Speciation Analysis instrument.
Background technology
Heavy metal pollution refers to the environmental pollution as caused by heavy metal or its compound, and heavy metal can be enriched with human body,
Once the tolerance limit more than human body will be poisoned, body is caused greatly to endanger.And its extent of injury depends on heavy metal
Concentration and chemical form, the heavy metal of the same concentration toxicity under different forms differs greatly, thus needs to not similar shape
The heavy metal element of state is analyzed.
In morphological analysis spectral detection application at present, often by cumbersome sample pretreatment process, and can not be to thing
The relevant ions of Relative-State, substituent, functional group eliminate or shielded in matter or pre-treatment reagent, so as to disturb the inspection of examined element
Survey, often poor reproducibility, sensitivity is low, morphological data is inaccurate.
The content of the invention
It is an object of the invention to provide a kind of Elemental Speciation Analysis instrument, is asked with solve to propose in above-mentioned background technology
Topic.
To achieve the above object, the present invention provides following technical scheme：
A kind of Elemental Speciation Analysis instrument, it is characterised in that：It is positive and negative including sampling device, valence state separation chromatogram arrangement, direct current
Valence state electrophoretic separation device, Relative-State intervention device, Electrochemical hydriding device, gaseous hydride stability derive transition device,
AFS and liquid waste treating apparatus；Wherein：The sampling device, valence state separation chromatogram arrangement, the positive and negative valence state of direct current
Device, Relative-State intervention device, Electrochemical hydriding device, gaseous hydride stability is separated by electrophoresis and derives transition device, atom
It is sequentially connected in series between XRF by the tetrafluoroethene pipeline that insulate；Device, electrification is separated by electrophoresis in the positive and negative valence state of direct current
Hydrogenation apparatus is learned with liquid waste treating apparatus by the tetrafluoroethene pipeline that insulate to be connected.
Further technical scheme is：The sampling device includes liquid chromatogram separation eluent conveying device and and liquid phase
The sample intervention device of chromatographic isolation eluent conveying device connection；The sample intervention device is that liquid chromatogram six leads to sample introduction
Valve.
Further technical scheme is：The valence state separation chromatogram arrangement includes liquid-phase chromatographic column temperature control device and located at liquid
Liquid-phase chromatographic column inside phase chromatographic column temperature control device；The output of the input port connection sample intervention device of the liquid-phase chromatographic column
Mouthful, the positive and negative valence state electrophoretic separation device of liquid-phase chromatographic column delivery outlet connection direct current；The liquid-phase chromatographic column shaft is melten glass
Pipe.
Further technical scheme is：The positive and negative valence state electrophoretic separation device of direct current includes main body one, the main body one
On set seal nipple, sample and carrier input port, guiding gutter, adjustable high voltage electric field electrode, permeable membrane, adjustable low-pressure permeability electricity
Pole, non-detection valence state diffluence pass, detection valence state diffluence pass, low-pressure permeability superpressure seepage port, fixed sleeve part；The sample and carrier
Input port connects with liquid-phase chromatographic column delivery outlet；It is high pressure pre-separation area between the both positive and negative polarity of the adjustable high voltage electric field electrode；
The upper end electrode opening position of the adjustable low-pressure permeability electrode sets non-detection valence state diffluence pass, and lower end electrode opening position sets detection valency
State diffluence pass, it is low-pressure permeability Disengagement zone between the two poles of the earth；Low-pressure permeability Disengagement zone centre position is provided with permeable membrane；It is described to ooze
Permeable membrane is connected with low-pressure permeability superpressure seepage port；The low-pressure permeability superpressure seepage port and non-detection valence state diffluence pass are and waste liquid
Processing unit is connected.
Further technical scheme is：The Relative-State intervention device includes the solid fast conveying device of detection valence state, negative electrode electricity
The blender that solution liquid conveying device and fast conveying device solid with detection valence state, catholyte conveying device delivery outlet are connected；
The solid fast conveying device input port of detection valence state is connected with detection valence state diffluence pass, the catholyte conveying device input
Mouth connection catholyte.
Further technical scheme is：The Electrochemical hydriding device includes main body two, main body three, main body four, the master
Hydrogenation room is fixedly connected to form by fastening screw between body two, main body three, main body four；Hydrogenation gas delivery outlet is set in main body two, is surpassed
Press seepage port, sealing gasket；Main body three is provided with cathode chamber input port, cathode chamber seepage port；Set in main body four anode chamber input port,
Anode chamber's refluxing opening；Anode electrode, amberplex, cathode electrode, gas-liquid separation membrane and gas infiltration are set in the hydrogenation room
Film, for the anode electrode between anode chamber input port, anode chamber's refluxing opening, the cathode electrode is located at cathode chamber input
Between mouth, cathode chamber seepage port, the amberplex is between anode electrode and cathode electrode, the gas-liquid separation membrane position
Above cathode electrode, the gas-permeable membrane is located above gas-liquid separation membrane；The main body four is intermembranous for sun with ion exchange
Pole room, intermembranous amberplex and gas-liquid separation are cathode chamber, are plenum chamber between gas-liquid separation membrane and gas-permeable membrane, gas
It is low pressure gas area between permeable membrane and main body two；The delivery outlet of the cathode chamber input port connection threeway；The threeway input port one
Connected with blender delivery outlet, threeway input port two connects with hydrogenation gas；The anode chamber input port and Electrochemical hydriding anode
Electrolyte conveying device delivery outlet connects；Anode chamber's refluxing opening is directly back to anolyte reservoir；The cathode chamber
Seepage port, superpressure seepage port connect with liquid waste treating apparatus；The hydrogenation gas delivery outlet derives with gaseous hydride stability
Transition device connects.
Further technical scheme is：The gaseous hydride stability, which derives transition device, includes the mirror of low UV absorption
Face aluminium derives box；The specular aluminium of the low UV absorption derive box be provided with the fixed suit of input, the derivative helix tube of quartz,
253.7nm ultraviolet lamp tubes, the fixed suit of output, lamp socket, temperature detection sensor, ultraviolet radiation sensor, leakage warning device；
The 253.7nm ultraviolet lamp tubes are assemblied in the derivative helix tube spiral of quartz；The fixed suit of input is disguised with electrochemical hydrogen
The delivery outlet connection of hydrogenation gas is put, the fixed suit of output connects with AFS.
Further technical scheme is：The liquid waste treating apparatus includes main body housing, and the is provided with the main body housing
First, second, third back pressure regulating valve, first, second, third check valve, first, second, third electronic flowmeter, first,
2nd, the 3rd waste liquid mixing tee, first, second, third liquid waste processing additive conveying peristaltic pump, first, second, third waste liquid
Handle pipeline, liquid waste tank and waste liquid delivery outlet；The first back pressure regulating valve input port connects with non-detection valence state diffluence pass,
Second back pressure regulating valve input port connects with low-pressure permeability superpressure seepage port, the 3rd back pressure regulating valve input port and superpressure seepage port
Connection, first, second, third back pressure regulating valve delivery outlet connects with first, second, third check valve input port respectively, described
First, second, third check valve delivery outlet connects with first, second, third electronic flowmeter input port respectively, described first,
Second, third electronic flowmeter delivery outlet connects with an input port of first, second, third waste liquid mixing tee respectively, institute
First, second, third another input port of waste liquid mixing tee is stated to convey with first, second, third liquid waste processing additive respectively
Peristaltic pump delivery outlet connects, first, second, third liquid waste processing additive conveying peristaltic pump input port respectively with it is corresponding
Liquid waste processing additive connects；First, second, third waste liquid mixing tee delivery outlet and first, second, third liquid waste processing pipe
Road input port connects, and the first, second, third liquid waste processing pipeline delivery outlet flows directly into liquid waste tank, the waste liquid storage
Stirring rotator is provided with inside groove, bottom is provided with magnetic agitation, and the neck of liquid waste tank is provided with waste liquid delivery outlet, the waste liquid output
Mouth flows directly into waste liquid storage device.
Further technical scheme is：It are furnished with 1mm turbulent flow baffle plates in the derivative helix tube of quartz.
Further technical scheme is：The solid speed conveying dress of the liquid chromatogram separation eluent conveying device, detection valence state
Put, catholyte conveying device, blender, Electrochemical hydriding anolyte conveying device are accurate constant flow pump, described
The pumping cylinder of accurate constant flow pump is melten glass pipe, and plunger rod is quartzy plunger rod.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) entered by the way of high performance liquid chromatography-electrophoretic separation-hydrogenation generation-Hydride generation-atomic fluorescence spectrophotometry
Row detection, avoids cumbersome sample pretreatment process, avoids interference element from intervening, multistage is exaggerated detection sensitivity；
(2) continued using variable field strength, pulse direct current electric field realizes the separation of positive and negative valence state by the ion of element to be measured
Freed in the molecular structure complicated from raw sample, realization efficiently separates；
(3) hydrogenate element to be measured using Electrochemical hydriding mode, reduce while hydrogenation effect is ensured carrier fluid and
The use of reducing agent；
(4) gaseous hydride stability is derived transition device and spread out using the derivative helix tube of quartz and low UV absorption specular aluminium
Raw box, maximize ultraviolet radioactive and derive, be furnished with 1mm turbulent flow baffle plates in quartzy helix tube, in the case of separating degree is not lost, realize
Turbulent flow, so as to improve ultraviolet derivative efficiency；
(5) gaseous hydride stability derives the leakage that transition device monitors derivative confined space using warning device in real time
Situation, while provided with derivative radiation intensity monitoring device, derivative device for detecting temperature to the temperature and radiation intensity in derivative box
It is monitored, ensures safety；
(6) gaseous hydride stability derivative transition device monitors uviol lamp in real time using derivative radiation intensity monitoring device
Intensity, the bombardment ionic strength of uviol lamp power supply is adjusted according to Strength Changes, it is stable to reach UV intensity, ensure derivative stable
Property；
(7) liquid waste treating apparatus ensures that waste liquid is effectively handled, reduced to environment using each unit waste liquid mode is handled respectively
Harm；
(8) liquid waste treating apparatus uses flow monitoring and conveying linkage function, to save the use of liquid waste processing additive
Amount, it is ensured that maximization reduces cost, environmental protection.
Brief description of the drawings
Fig. 1 is the structural representation of the present invention；
Fig. 2 is the structural representation that device is separated by electrophoresis in the positive and negative valence state of direct current；
Fig. 3 is the structural representation of Electrochemical hydriding device；
Fig. 4 is the structural representation that gaseous hydride stability derives transition device；
Fig. 5 is the structural representation of liquid waste treating apparatus；
In figure：1- liquid chromatogram separation eluents conveying device, 2- samples intervention device, 3- valence states separation chromatogram arrangement,
The positive and negative valence state electrophoretic separation device of 4- direct currents, the solid fast conveying device of 5- detection valence states, 6- catholytes conveying device, 7- mixing
The Electrochemical hydriding anolyte conveying device of device, 8-, the Electrochemical hydriding devices of 9-, 10- gaseous hydrides stability derive jump
Device, 11- AFSs and liquid waste treating apparatus, 12- seal nipples, 13- samples and carrier input port, 14- is moved to lead
Chute, 15- are adjustable high voltage electric field electrode, 16- high pressure pre-separations area, 17- permeable membranes, 18- is adjustable low-pressure permeability electrode, 19- are non-
Detect valence state diffluence pass, 20- detection valence states diffluence pass, 21- low-pressure permeabilities Disengagement zone, 22- low-pressure permeability superpressures seepage port, 23-
Fixed sleeve part, 24- main bodys one, 25- threeways, 26- cathode chambers input port, 27- cathode electrodes, 28- cathode chambers seepage port, 29- are cloudy
Pole room, 30- anode chambers input port, 31- anode electrodes, 32- anode chambers, 33- anode chambers refluxing opening, 34- amberplexes, 35-
Gas-liquid separation membrane, 36- plenum chambers, 37- gas-permeable membranes, 38- hydrogenation gas delivery outlet, 39- low pressure gas area, 40- superpressure seepage flow
Mouth, 41- hydrogenation room, 42- main bodys two, 43- main bodys three, 44- main bodys four, 45- fastening screws, the fixed suit of 46- inputs, 47- stones
English derives helix tube, 48-253.7nm ultraviolet lamp tubes, the fixed suit of 49- outputs, 50- lamp sockets, 51- temperature detection sensors, 52-
Ultraviolet radiation sensor, 53- leakages warning device, the specular aluminium of the low UV absorptions of 54- derive box, 55- first, second, third
Back pressure regulating valve, the check valves of 56- first, second, third, the electronic flowmeters of 57- first, second, third, 58- first, second,
3rd waste liquid mixing tee, the liquid waste processing additives of 59- first, second, third conveying peristaltic pump, 60- first, second, third
Liquid waste processing pipeline, 61- liquid waste tanks, 62- stirring rotators, 63- magnetic agitations, 64- waste liquids delivery outlet, 65- main body housings.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other under the premise of creative work is not made
Embodiment, belong to the scope of protection of the invention.
As Figure 1-5, the invention provides a kind of Elemental Speciation Analysis instrument, including including sampling device, valence state separation
The positive and negative valence state electrophoretic separation device 4 of chromatogram arrangement 3, direct current, Relative-State intervention device, Electrochemical hydriding device 9, gaseous hydride
Stability derives transition device 10, AFS and liquid waste treating apparatus 11.
Wherein：
The sampling device includes liquid chromatogram separation eluent conveying device 1 and conveyed with liquid chromatogram separation eluent
The sample intervention device 2 that device 1 connects, the sample intervention device 2 is liquid chromatogram six-way injection valve.
The valence state separation chromatogram arrangement 3 includes liquid-phase chromatographic column temperature control device and in liquid-phase chromatographic column temperature control device
Liquid-phase chromatographic column；The liquid-phase chromatographic column shaft is melten glass pipe；The input port connection sample of the liquid-phase chromatographic column is situated between
Enter the delivery outlet of device 2, the positive and negative valence state electrophoretic separation device 4 of chromatographic column delivery outlet connection direct current.
The positive and negative valence state electrophoretic separation device 4 of direct current includes main body one, and seal nipple 12, sample are set in the main body 1
Product and carrier input port 13, guiding gutter 14, adjustable high voltage electric field electrode 15, permeable membrane 17, adjustable low-pressure permeability electrode 18, non-inspection
Survey valence state diffluence pass 19, detection valence state diffluence pass 20, low-pressure permeability superpressure seepage port 22, fixed sleeve part 23；The sample and load
Body input port 13 connects with liquid-phase chromatographic column delivery outlet；Divide in advance for high pressure between the both positive and negative polarity of the adjustable high voltage electric field electrode 15
From area 16；The upper end electrode opening position of the adjustable low-pressure permeability electrode 18 sets non-detection valence state diffluence pass 19, lower end electrode position
The place of putting sets detection valence state diffluence pass 20, is low-pressure permeability Disengagement zone 21 between the two poles of the earth；The interposition of low-pressure permeability Disengagement zone 21
Permeable membrane 17 is installed；The permeable membrane 17 is connected with low-pressure permeability superpressure seepage port 22.
The Relative-State intervention device include the solid fast conveying device 5 of detection valence state, catholyte conveying device 6 and with inspection
Survey the connected blender 7 of the solid fast conveying device 5 of valence state, the delivery outlet of catholyte conveying device 6；The solid speed of detection valence state
The input port of conveying device 5 is connected with detection valence state diffluence pass 20, the input port of the catholyte conveying device 6 connection negative electrode electricity
Solve liquid.
The Electrochemical hydriding device 9 includes main body 2 42, main body 3 43, main body 4 44, the main body 2 42, main body three
43rd, hydrogenation room 41 is fixedly connected to form by fastening screw 45 between main body 4 44；Hydrogenation gas delivery outlet 38 is set in main body 2 42, is surpassed
Press seepage port 40, sealing gasket；Main body 3 43 is provided with cathode chamber input port 26, cathode chamber seepage port 28；Sun is set in main body 4 44
Pole room input port 30, anode chamber's refluxing opening 33；Anode electrode 31, amberplex 34, cathode electrode are set in the hydrogenation room 41
27th, gas-liquid separation membrane 35 and gas-permeable membrane 37, the anode electrode 31 are located at anode chamber input port 30, anode chamber's refluxing opening 33
Between, between cathode chamber input port 26, cathode chamber seepage port 28, the amberplex 34 is located at the cathode electrode 27
Between anode electrode 31 and cathode electrode 27, the gas-liquid separation membrane 35 is located at the top of cathode electrode 27, the gas-permeable membrane
37 positioned at the top of gas-liquid separation membrane 35；Be anode chamber 32 between the main body 4 44 and amberplex 34, amberplex 34 with
It is cathode chamber 29 between gas-liquid separation membrane 35, is plenum chamber 36 between gas-liquid separation membrane 35 and gas-permeable membrane 37, gas-permeable membrane
It is low pressure gas area 39 between 37 and main body 2 42；The cathode chamber input port 26 connects the delivery outlet of threeway 25；The threeway 25 is defeated
Entrance one connects with the delivery outlet of blender 7, and the input port two of threeway 25 connects with hydrogenation gas；The anode chamber input port 30 and electrification
Learn the delivery outlet connection of hydrogenation anolyte conveying device 8；Anode chamber's refluxing opening 33 is directly back to anolyte appearance
Device；The cathode chamber seepage port 28, superpressure seepage port 40 connect with liquid waste treating apparatus 11；The hydrogenation gas delivery outlet 38 with
Gaseous hydride stability derives transition device 10 and connected.
The gaseous hydride stability, which derives transition device 10, includes the specular aluminium derivative box 54 of low UV absorption；It is described
The specular aluminium of low UV absorption derives box 54 and is provided with the fixed suit 46 of input, the derivative helix tube 47 of quartz, 253.7nm ultraviolet lamp tubes
48th, the fixed suit 49 of output, lamp socket 50, temperature detection sensor 51, ultraviolet radiation sensor 52, leakage warning device 53；Institute
253.7nm ultraviolet lamp tubes 48 are stated to be assemblied in the derivative spiral of helix tube 47 of quartz；The fixed suit 46 of input and hydrogenation gas are defeated
The connection of outlet 38, the fixed suit 49 of output connect with AFS.
The liquid waste treating apparatus 11 includes main body housing 65, and first, second, third back of the body is provided with the main body housing 65
Press regulating valve 55, first, second, third check valve 56, first, second, third electronic flowmeter 57, first, second, third useless
Liquid mixing tee 58, first, second, third liquid waste processing additive conveying peristaltic pump 59, first, second, third liquid waste processing
Pipeline 60, liquid waste tank 61 and waste liquid delivery outlet 64；The first back pressure regulating valve input port and non-detection valence state diffluence pass 19
Connection, the second back pressure regulating valve input port connect with low-pressure permeability superpressure seepage port 22, and the 3rd back pressure regulating valve input port is with surpassing
Pressure seepage port 40 connect, first, second, third back pressure regulating valve delivery outlet respectively with first, second, third check valve input port
Connection, the first, second, third check valve delivery outlet connect with first, second, third electronic flowmeter input port respectively,
The first, second, third electronic flowmeter delivery outlet is defeated with one of first, second, third waste liquid mixing tee 58 respectively
Entrance connect, first, second, third waste liquid mixing tee, 58 another input port respectively with first, second, third waste liquid
Additive conveying peristaltic pump 59 delivery outlet connection is managed, the first, second, third liquid waste processing additive conveying peristaltic pump 59 is defeated
Entrance connects with corresponding liquid waste processing additive respectively；The delivery outlet of first, second, third waste liquid mixing tee 58 and first,
Second, third input port of liquid waste processing pipeline 60 connects, and the first, second, third liquid waste processing pipeline, 60 delivery outlets are direct
Liquid waste tank 61 is flowed to, the inside of liquid waste tank 61 is provided with stirring rotator 62, and bottom is provided with magnetic agitation 63, liquid waste tank 61
Neck be provided with waste liquid delivery outlet 64, the waste liquid delivery outlet 64 flows directly into waste liquid storage device.
It are furnished with 1mm turbulent flow baffle plates in the derivative helix tube 47 of quartz.
The liquid chromatogram separation eluent conveying device 1, the solid fast conveying device 5 of detection valence state, catholyte conveying
Device 6, blender 7, Electrochemical hydriding anolyte conveying device 8 are accurate constant flow pump, the pump of the accurate constant flow pump
Cylinder is melten glass pipe, and plunger rod is quartzy plunger rod.
The analysis principle and process of elementary analysis are carried out using the present invention：
Liquid chromatogram separation eluent is inputted in instrument through liquid chromatogram separation eluent conveying device 1, testing sample warp
Sample intervention device 2 is intervened, and after liquid chromatogram post separation, the high pressure into the positive and negative valence state electrophoretic separation device 4 of direct current is divided in advance
From area 16, under DC electric field effect, cation (charged group) moves to negative pole (low potential), anion (charged group) phase
Instead, zwitterion is separated from each other, then realizes that positive and negative valence state separates (electric field by the ion exchange of low-pressure permeability Disengagement zone 21
Intensity can be adjusted by electrical potential difference), flowed out in the presence of hydraulic pressure by corresponding diffluence pass.
Detection valence state separating liquid after separation carries electric charge, it is necessary to use insulation pipeline and encapsulated with melten glass, ensures
Electric charge only has micro transfer, while will be divided using accurate constant flow pump (accurate constant flow pump avoids electric charge transfer using quartzy plunger rod)
Detection valence state separating liquid from after is transported to blender 7；Using the same manner by the catholyte (Relative-State containing element to be measured
Counterion) it is transported to blender 7 and is mixed.
After the mixed liquor that blender 7 exports mixes with hydrogenation gas, into the cathode chamber 29 of Electrochemical hydriding device 9, electrification
Learning hydrogenation anolyte conveying device 8 makes anolyte be circulated in anode chamber 32.Realized under the adjustable electrical potential difference of anode and cathode
Electrolysis, generate the gaseous hydride of element to be measured after element is free with hydrogenation solid/liquid/gas reactions under electrolysis, made by osmotic pressure
Exported with through gas-liquid separation membrane infiltration 35 to plenum chamber via hydrogenation gas delivery outlet 38, to ensure that gaseous hydride normally oozes
Go out, back pressure mode is used in cathode chamber seepage port 28.
The gaseous hydride of output enters the derivative helix tube 47 of quartz, and being excited by ultraviolet radiation makes surveyed element transition
Hydrogenated derivatives are produced to excitation state, hydrogenated derivatives enter back into AFS and detected.
Security describes, and because ultraviolet is harmful, therefore deriving device often uses air-tight manner, the derivative spiral of quartz
Hydrogenation gas (micro liquid) in pipe is flammable and combustible liquids gas, once leaking, the liquid or gas after leakage can not
Smooth discharge, because ultraviolet source long-play discharges heat, temperature accumulation to a certain extent, can turn into incendiary source；Therefore
Easily explode, laboratory accident occurs.The present invention monitors the leakage situation of derivative confined space with warning device in real time,
Ensure safety, while the temperature in deriving device and radiation intensity are monitored provided with derivative device for detecting temperature.It is once warm
Degree exceedes safety value, and ultraviolet source will automatically power off；Provisioned liquid waste treating apparatus can handle the waste liquid of each unit respectively,
Ensure the person and Environmental security.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of changes, modification can be carried out to these embodiments, replace without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (11)
1. a kind of Elemental Speciation Analysis instrument, it is characterised in that positive and negative including sampling device, valence state separation chromatogram arrangement (3), direct current
Valence state electrophoretic separation device (4), Relative-State intervention device, Electrochemical hydriding device (9), gaseous hydride stability derive transition
Device (10), AFS and liquid waste treating apparatus (11)；Wherein：The sampling device, valence state separation chromatogram arrangement
(3), the positive and negative valence state electrophoretic separation device (4) of direct current, Relative-State intervention device, Electrochemical hydriding device (9), gaseous hydride are steady
It is sequentially connected in series between qualitative derivative transition device (10), AFS by the tetrafluoroethene pipeline that insulate；The direct current
Positive and negative valence state electrophoretic separation device (4), Electrochemical hydriding device (9) pass through the tetrafluoroethene that insulate with liquid waste treating apparatus (11)
Pipeline is connected.
A kind of 2. Elemental Speciation Analysis instrument according to claim 1, it is characterised in that：The sampling device includes liquid phase color
Compose separation eluent conveying device (1) and the sample intervention device connected with liquid chromatogram separation eluent conveying device (1)
(2)。
A kind of 3. Elemental Speciation Analysis instrument according to claim 2, it is characterised in that：The valence state separates chromatogram arrangement
(3) liquid-phase chromatographic column temperature control device and the liquid-phase chromatographic column inside liquid-phase chromatographic column temperature control device are included；The liquid phase color
Compose the delivery outlet of the input port connection sample intervention device (2) of post, the positive and negative valence state electrophoretic separation of chromatographic column delivery outlet connection direct current
Device (4).
A kind of 4. Elemental Speciation Analysis instrument according to Claims 2 or 3, it is characterised in that：The positive and negative valence state electricity of direct current
Swimming separator (4) includes main body one, set on the main body one (24) seal nipple (12), sample and carrier input port (13),
Guiding gutter (14), adjustable high voltage electric field electrode (15), permeable membrane (17), adjustable low-pressure permeability electrode (18), non-detection Valence States
Head piece (19), detection valence state diffluence pass (20), low-pressure permeability superpressure seepage port (22), fixed sleeve part (23)；The sample and load
Body input port (13) connects with liquid-phase chromatographic column delivery outlet；It is high pressure between the both positive and negative polarity of the adjustable high voltage electric field electrode (15)
Pre-separation area (16)；The upper end electrode opening position of the adjustable low-pressure permeability electrode (18) sets non-detection valence state diffluence pass (19),
Lower end electrode opening position sets detection valence state diffluence pass (20), is low-pressure permeability Disengagement zone (21) between the two poles of the earth；The low-pressure permeability
Disengagement zone (21) centre position is provided with permeable membrane (17)；The permeable membrane (17) is connected with low-pressure permeability superpressure seepage port (22)；
The low-pressure permeability superpressure seepage port (22) and non-detection valence state diffluence pass (19) are connected with liquid waste treating apparatus (11).
A kind of 5. Elemental Speciation Analysis instrument according to claim 4, it is characterised in that：The Relative-State intervention device includes
Detect the solid fast conveying device (5) of valence state, catholyte conveying device (6) and fast conveying device (5) solid with detection valence state, negative electrode
The connected blender (7) of electrolyte conveying device (6) delivery outlet；Solid fast conveying device (5) input port of detection valence state with
Detect valence state diffluence pass (20) to be connected, catholyte conveying device (6) input port connects catholyte.
A kind of 6. Elemental Speciation Analysis instrument according to claim 5, it is characterised in that：The Electrochemical hydriding device (9)
Including main body two (42), main body three (43), main body four (44), between the main body two (42), main body three (43), main body four (44)
Hydrogenation room (41) is fixedly connected to form by fastening screw (45)；Hydrogenation gas delivery outlet (38), superpressure seepage flow are set in main body two (42)
Mouth (40), sealing gasket；Main body three (43) is provided with cathode chamber input port (26), cathode chamber seepage port (28)；In main body four (44)
Anode chamber input port if (30), anode chamber's refluxing opening (33)；Anode electrode (31), amberplex are set in the hydrogenation room (41)
(34), cathode electrode (27), gas-liquid separation membrane (35) and gas-permeable membrane (37), it is defeated that the anode electrode (31) is located at anode chamber
Between entrance (30), anode chamber's refluxing opening (33), the cathode electrode (27) is located at cathode chamber input port (26), cathode chamber seepage flow
Between mouth (28), the amberplex (34) is located between anode electrode (31) and cathode electrode (27), the gas-liquid separation
Film (35) is located above cathode electrode (27), and the gas-permeable membrane (37) is located above gas-liquid separation membrane (35)；The main body
It is anode chamber (32) between four (44) and amberplex (34), is cathode chamber between amberplex (34) and gas-liquid separation membrane (35)
(29), between gas-liquid separation membrane (35) and gas-permeable membrane (37) it is plenum chamber (36), gas-permeable membrane (37) and main body two
(42) it is between low pressure gas area (39)；The delivery outlet of cathode chamber input port (26) the connection threeway (25)；The threeway (25) is defeated
Entrance one connects with blender (7) delivery outlet, and threeway (25) input port two connects with hydrogenation gas；The anode chamber input port (30)
Connected with Electrochemical hydriding anolyte conveying device (8) delivery outlet；Anode chamber's refluxing opening (33) is directly flowed back Zhiyang
Pole electrolyte container；The cathode chamber seepage port (28), superpressure seepage port (40) connect with liquid waste treating apparatus (11)；It is described
Hydrogenation gas delivery outlet (38) derives transition device (10) with gaseous hydride stability and connected.
A kind of 7. Elemental Speciation Analysis instrument according to claim 6, it is characterised in that：The gaseous hydride stability is spread out
The specular aluminium that raw transition device (10) includes low UV absorption derives box (54)；The specular aluminium of the low UV absorption derives box
(54) the fixed suit (46) of input, the derivative helix tube (47) of quartz, 253.7nm ultraviolet lamp tubes (48), the fixed suit of output are provided with
(49), lamp socket (50), temperature detection sensor (51), ultraviolet radiation sensor (52), leakage warning device (53)；It is described
253.7nm ultraviolet lamp tubes (48) are assemblied in derivative helix tube (47) spiral of quartz；The fixed suit (46) of input and electrification
Hydrogenation apparatus (9) hydrogenation gas delivery outlet (38) connection is learned, the fixed suit (49) of output connects with AFS.
A kind of 8. Elemental Speciation Analysis instrument according to claim 7, it is characterised in that：Liquid waste treating apparatus (11) bag
Include main body housing (65), be provided with the main body housing (65) first, second, third back pressure regulating valve (55), first, second,
3rd check valve (56), first, second, third electronic flowmeter (57), first, second, third waste liquid mixing tee (58),
First, second, third liquid waste processing additive conveying peristaltic pump (59), first, second, third liquid waste processing pipeline (60), waste liquid
Storage tank (61) and waste liquid delivery outlet (64)；The first back pressure regulating valve input port connects with non-detection valence state diffluence pass (19),
Second back pressure regulating valve input port is connected with low-pressure permeability superpressure seepage port (22), and the 3rd back pressure regulating valve input port is oozed with superpressure
Head piece (40) connects, and first, second, third back pressure regulating valve delivery outlet connects with first, second, third check valve input port respectively
Logical, the first, second, third check valve delivery outlet connects with first, second, third electronic flowmeter input port respectively, institute
It is defeated with one of first, second, third waste liquid mixing tee (58) respectively to state first, second, third electronic flowmeter delivery outlet
Entrance connect, another input port of the first, second, third waste liquid mixing tee (58) respectively with first, second, third waste liquid
Treatment additive conveying peristaltic pump (59) delivery outlet connection, the first, second, third liquid waste processing additive convey peristaltic pump
(59) input port connects with corresponding liquid waste processing additive respectively；First, second, third waste liquid mixing tee (58) delivery outlet
Connected with first, second, third liquid waste processing pipeline (60) input port, the first, second, third liquid waste processing pipeline (60)
Delivery outlet flows directly into liquid waste tank (61), is provided with stirring rotator (62) inside the liquid waste tank (61), bottom is provided with magnetic force
Stir (63), the neck of liquid waste tank (61) is provided with waste liquid delivery outlet (64), and the waste liquid delivery outlet (64) flows directly into waste liquid
Storage device.
A kind of 9. Elemental Speciation Analysis instrument according to claim 6 or 8, it is characterised in that：The derivative helix tube of quartz
(47) it are furnished with 1mm turbulent flow baffle plates in.
A kind of 10. Elemental Speciation Analysis instrument according to claim 9, it is characterised in that：The liquid chromatogram separation elution
Liquid conveying device (1), the solid fast conveying device (5) of detection valence state, catholyte conveying device (6), blender (7), electrochemistry
It is accurate constant flow pump to hydrogenate anolyte conveying device (8), and the pumping cylinder of the accurate constant flow pump is melten glass pipe, plunger
Bar is quartzy plunger rod.
A kind of 11. Elemental Speciation Analysis instrument according to claim 1 or 9, it is characterised in that：The liquid-phase chromatographic column shaft
For melten glass pipe.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108333034A (en) * | 2018-05-14 | 2018-07-27 | 中山大学 | A kind of air film for Surface enhanced Raman spectroscopy detection detaches sample pretreatment device |
| CN109163081A (en) * | 2018-10-24 | 2019-01-08 | 中广核检测技术有限公司 | A kind of lubrication oil filtration system of wind turbine gearbox |
| CN112304926A (en) * | 2020-10-27 | 2021-02-02 | 湖南有色金属职业技术学院 | Solid waste decomposes and uses elemental analysis device |
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Cited By (4)
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|---|---|---|---|---|
| CN108333034A (en) * | 2018-05-14 | 2018-07-27 | 中山大学 | A kind of air film for Surface enhanced Raman spectroscopy detection detaches sample pretreatment device |
| CN109163081A (en) * | 2018-10-24 | 2019-01-08 | 中广核检测技术有限公司 | A kind of lubrication oil filtration system of wind turbine gearbox |
| CN112304926A (en) * | 2020-10-27 | 2021-02-02 | 湖南有色金属职业技术学院 | Solid waste decomposes and uses elemental analysis device |
| CN112304926B (en) * | 2020-10-27 | 2023-07-18 | 湖南有色金属职业技术学院 | Element analysis device for decomposing solid waste |
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