CN105445484B - Method for exhausting during Flow Injection Analysis device and Flow Injection Analysis with degassing function - Google Patents
Method for exhausting during Flow Injection Analysis device and Flow Injection Analysis with degassing function Download PDFInfo
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- CN105445484B CN105445484B CN201510976695.1A CN201510976695A CN105445484B CN 105445484 B CN105445484 B CN 105445484B CN 201510976695 A CN201510976695 A CN 201510976695A CN 105445484 B CN105445484 B CN 105445484B
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- 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
- G01N35/08—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor using a stream of discrete samples flowing along a tube system, e.g. flow injection analysis
- G01N35/085—Flow Injection Analysis
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Abstract
The Flow Injection Analysis device with degassing function that the present invention is provided, including low-lift pump, six-way injection valve, the first blender, reactor, optical flow cell, fluorescence detector, computer processing system, waste fluid container, magnetic valve and the matching used time relay of magnetic valve.Present invention also offers method for exhausting during Flow Injection Analysis, the method uses the above-mentioned Flow Injection Analysis device with degassing function, and manual exhaust or automatic on-line exhaust can be realized during Flow Injection Analysis, and bleeding is simple, good exhaust effect, is conducive to improving analysis efficiency.
Description
Technical field
The invention belongs to Flow Injection Analysis field, Flow Injection Analysis device and stream more particularly to degassing function
Method for exhausting during dynamic Injection Analysis.
Background technology
During Flow Injection Analysis (FIA), enter in the reagent current-carrying that sample or standard specimen are injected into pipeline in the form of the sample plug
Row analysis test.During Flow Injection Analysis, because the joint air-tightness of flow path system is bad, valve degree of closure is poor,
Using reasons such as peristaltic pump feed liquors, bubble is easily sucked from outside stream system, or due to being needed during Flow Injection Analysis
Heat, cause solubility of the gas in sample or standard specimen solution and current-carrying to decline and discharge bubble or stream system
Liquid evaporation in system forms bubble, and unstable decomposition of reagent produces bubble, reaction to produce bubble or reagent volatilization to produce gas
The reasons such as bubble produce bubble in flow path system.The detection for introducing often Interference Flow Injection Analysis signal of bubble, influence
The accuracy of measurement result, even makes measure to carry out when serious, therefore should be kept away as far as possible during Flow Injection Analysis
Exempt to produce bubble and try to eliminate the bubble for having produced.
In order in Flow Injection Analysis it is as few as possible to flow path system in introduce bubble, will be promoted generally before sample introduction
Liquid, nitrite ion and sample solution etc. vacuumize degassing or ultrasonic oscillation treatment is to reduce the gas for wherein dissolving but this
Operation can only be reduced to introducing bubble in flow path system, but cannot eliminate the bubble produced in stream, when in flow path system
When the minute bubbles of generation are trapped in the normal detection of interference in optical flow cell, can only Flow Injection Analysis device out of service, will
Optical flow cell is taken out, and the outer wall of optical flow cell is repeatedly flicked with finger, is flicked while transform optics flow cell
Angle, makes to be trapped in minute bubbles therein and gradually up moves, and again fills optical flow cell after minute bubbles are all discharged
Continuation is analyzed in entering to flow injection analyzer, and the operation of the mode of this exhaust bubble is very cumbersome, is unfavorable for analysis efficiency
Improve, be also an impediment to save human cost during Flow Injection Analysis.Li Jinxin etc. enters to existing Flow Injection Analysis device
Improvement is gone, installing a back-pressure circle additional after optical flow cell increases the pressure of stream system, the pressure increase of stream system
Volatilization, the increase solubility of the gas in water of solution can be reduced, so reduce bubble to analyze interference (rock and mineral testing,
1996,15(2):104-106), the improved Flow Injection Analysis device can only be reduced and discharge bubble or because molten because of heating
Liquid volatilization produces bubble, but cannot eliminate the bubble that other reasonses are produced in flow path system, restricted application, and back-pressure
The pressure that circle is likely to result in flow path system is too high, causes flow cell to damage.
The content of the invention
It is an object of the invention to overcome the deficiencies in the prior art, there is provided the Flow Injection Analysis device with degassing function
And method for exhausting during Flow Injection Analysis, to simplify bleeding during Flow Injection Analysis, improve analysis efficiency.
The Flow Injection Analysis device for having a degassing function of the present invention, there is three kinds of structures, and they belong to a total hair
Bright design.
The Flow Injection Analysis device with degassing function of the first structure of the present invention, structure is as follows：
The device include low-lift pump, six-way injection valve, the first blender, reactor, optical flow cell, fluorescence detector,
Computer processing system and waste fluid container, the optical flow cell include optical detecting channel and communicate with optical detecting channel
Feed pathway, liquid outlet channel, the fluorescence detector include light path system box and light signal collection processing system, optical flow cell
Optical detecting channel be arranged in the light path system box of fluorescence detector, the detection light path of fluorescence detector passes through the optics
Sense channel is simultaneously parallel with the optical detecting channel, also including the first magnetic valve, the time relay and support, first electricity
Magnet valve is three-way magnetic valve；
The light path system box of fluorescence detector by the support slant setting of support, enter by the feed pathway of optical flow cell
Outlet port of the mouth position less than liquid outlet channel；The part liquid outlet of low-lift pump is mixed through six-way injection valve by pipe fitting with first
The entrance connection of device, the part liquid outlet of low-lift pump is connected by entrance of the pipe fitting directly with the first blender, the first blender
Outlet connected with the entrance of reactor by pipe fitting, the import company that the outlet of reactor passes through pipe fitting and the first magnetic valve
Logical, another import of the first magnetic valve is communicated with air, and the outlet of the first magnetic valve passes through entering for pipe fitting and optical flow cell
Liquid channel connection, the liquid outlet channel of optical flow cell is connected by pipe fitting with waste fluid container, the light signal collection of fluorescence detector
Processing system is connected with computer processing system, and the time relay is connected with the first magnetic valve, and the first magnetic valve of control is to optics
Input air or reaction solution in flow cell, first magnetic valve are arranged on the top of optical flow cell.
The Flow Injection Analysis device with degassing function of second structure of the present invention, is in above-mentioned the first knot
The second blender and the second magnetic valve are increased on the basis of the device of structure, second magnetic valve is two three-way electromagnetic valves, reaction
The outlet of device is connected by pipe fitting with the entrance of the second blender, the outlet of the second blender by pipe fitting respectively with the first electromagnetism
One import of valve, the inlet communication of the second magnetic valve, the outlet of the second magnetic valve are connected by pipe fitting with waste fluid container, described
The time relay is connected with the first magnetic valve and the second magnetic valve respectively, and the second magnetic valve of control holds reaction solution input waste liquid
Device, the first magnetic valve of control are input into input air in optical flow cell, or the first magnetic valve of control in optical flow cell
Reaction solution, the second closed electromagnetic valve import of control, block reaction solution into the path of the second magnetic valve.
The Flow Injection Analysis device with degassing function of the third structure of the present invention, is in above-mentioned the first knot
The 3rd magnetic valve is increased on the basis of the device of structure, the 3rd magnetic valve is three-way magnetic valve, and the outlet of reactor passes through
The inlet communication of pipe fitting and the 3rd magnetic valve, the one outlet of the 3rd magnetic valve passes through an import of pipe fitting and the first magnetic valve
Connection, another outlet of the 3rd magnetic valve is connected by pipe fitting with waste fluid container, and the time relay is electric with first respectively
Magnet valve and the 3rd magnetic valve are connected, and reaction solution is input into waste fluid container, the first magnetic valve of control to optics by the 3rd magnetic valve of control
Input air in flow cell, or the 3rd magnetic valve of control and the first magnetic valve are to input reaction solution, control in optical flow cell
The port closing that 3rd magnetic valve is communicated with waste fluid container, blocks the path that reaction solution enters waste fluid container from the 3rd magnetic valve.
In above-mentioned technical proposal, the angle of inclination of the light path system box of the fluorescence detector should make to be arranged on light path system
The optical detecting channel of the optical flow cell in box is 25~45 ° with the angle α of horizontal plane.
In above-mentioned technical proposal, also including debubbler, the debubbler is closed vessel, and one end of the closed vessel is provided with
The blast pipe of feed tube and with closure, the other end is provided with drain pipe；The debubbler is at least 1, when debubbler is 1
When, on the liquid outlet of connection low-lift pump with a branch line of the inlet of six-way injection valve, it is preferably mounted at low
Press pump is pumped on the pipeline between the liquid outlet of the pump line of sample or standard specimen and the inlet of six-way injection valve；When debubbler is
Two or more when, be separately mounted to connect low-lift pump liquid outlet and the inlet of six-way injection valve different branched pipes
Lu Shang, or be separately mounted to connect the liquid outlet of low-lift pump and on the different branch lines of the inlet of six-way injection valve and connect
The liquid outlet of low-lift pump from the different branch lines of the first blender；Debubbler should be located at the feed tube of debubbler when installing
The top of drain pipe.
The debubbler can play a part of to reduce because sample introduction is as follows to bubble, its working method is introduced in stream：Enter
During the sample of sample instills closed vessel from the feed tube of closed vessel upper end, then through the drain pipe of closed vessel lower end through pipe fitting
Into in six-way injection valve or the first blender, the bottom of closed vessel is hydraulically full, and top is full of air, if being introduced during sample introduction
Bubble, then during closed vessel bottom is instilled from feed tube, bubble can enter closed vessel to sample with drop separation
Top, so as to play a part of reduce bubble, it is necessary to open the sealing on blast pipe when the gas in container to be closed is excessive
Lid discharge part gas.
In above-mentioned technical proposal, it is to ensure when the first electromagnetism that the first magnetic valve is arranged on above optical flow cell
Valve can successfully to input air in optical flow cell when being communicated with air, it is preferable that the installation site of first magnetic valve
Higher than the entrance location at least 20cm of the feed pathway of optical flow cell.
In above-mentioned technical proposal, low-lift pump is Multichannel constant-current pump, the quantity of the stream that low-lift pump is specifically used and each
Individual liquid outlet needs to be configured with the annexation of six-way injection valve or the first blender according to actual analysis.
In above-mentioned technical proposal, the time relay is the timing automatic powered off and on time relay of energy, preferably
It is circulation time-delay relay.
Method for exhausting of the device of above-mentioned the first structure in Flow Injection Analysis be：The time relay is set to hand
Dynamic to open the pattern powered off after energization, 20~60s of energization, during Flow Injection Analysis, the time relay is not powered on,
When entering bubble in finding optical flow cell and cannot exclude, close low-lift pump and stop sample introduction, the manually opened time relay
Power supply, make the first magnetic valve to input air in optical flow cell, the time relay is powered after 20~60s and automatically powers off, and opens
Low-lift pump sample introduction is opened, the air being completely exhausted out in optical flow cell to input reaction solution in optical flow cell completes exhaust behaviour
Make, be further continued for carrying out Flow Injection Analysis.
The device of above-mentioned second structure can realize manual exhaust and on-line automatic exhaust in Flow Injection Analysis, its
In, the method for manual exhaust is：The pattern powered off after the time relay is set into manually opened energization, 20~60s of energization,
During Flow Injection Analysis, the time relay is not powered on, and bubble is entered in optical flow cell is found and cannot be excluded
When, reaction solution is input into waste fluid container, the first magnetic valve to light by the power supply of the manually opened time relay, the second magnetic valve of control
Learn input air in flow cell, the time relay is powered after 20~60s and automatically powers off, the second closed electromagnetic valve import of control, the
One magnetic valve is after question response liquid excludes the air in optical flow cell completely, i.e., complete to reaction solution is input into optical flow cell
Into bleeding, it is further continued for carrying out Flow Injection Analysis；
The method of on-line automatic exhaust is：The time relay is set to be powered after 10~90min of time delay, is powered 20~
The circulation pattern powered off after 60s, after 10~90min of Flow Injection Analysis, the time relay is auto-power on, controls the second magnetic valve
Reaction solution is input into waste fluid container, the first magnetic valve to input air in optical flow cell, the time relay is powered after 20~60s
Automatically power off, the second closed electromagnetic valve import of control, the first magnetic valve are incited somebody to action to reaction solution, question response liquid is input into optical flow cell
After air in optical flow cell is excluded completely, that is, a bleeding is completed, flowing is hereafter proceeded in the manner previously described
Injection Analysis and bleeding.
The device of above-mentioned the third type can realize manual exhaust and on-line automatic exhaust in Flow Injection Analysis, its
In, the method for manual exhaust is：The pattern powered off after the time relay is set into manually opened energization, 20~60s of energization,
During Flow Injection Analysis, the time relay is not powered on, and bubble is entered in optical flow cell is found and cannot be excluded
When, reaction solution is input into waste fluid container, the first magnetic valve to light by the power supply of the manually opened time relay, the 3rd magnetic valve of control
Input air in flow cell is learned, is automatically powered off after 20~60s of time relay energization, control the 3rd magnetic valve and waste fluid container phase
To being input into reaction solution in optical flow cell, question response liquid is by optical flow for logical port closing, the 3rd magnetic valve and the first magnetic valve
After air in logical pond is excluded completely, that is, bleeding is completed, be further continued for carrying out Flow Injection Analysis；
The circulation pattern for the time relay being set to after 10~90min of time delay to be powered, being powered off after the 20~60s that is powered, stream
After dynamic 10~90min of Injection Analysis, the time relay is auto-power on, the 3rd magnetic valve of control by reaction solution be input into waste fluid container,
First magnetic valve is automatically powered off to input air in optical flow cell after 20~60s of time relay energization, controls the 3rd electromagnetism
Port closing, the 3rd magnetic valve and the first magnetic valve that valve is communicated with waste fluid container are treated to reaction solution is input into optical flow cell
After reaction solution excludes the air in optical flow cell completely, that is, complete once to arrange time operation, that is, complete a bleeding, this
Proceed Flow Injection Analysis and bleeding in the manner previously described afterwards.
The venting principleand of the Flow Injection Analysis device with degassing function of the present invention is as follows：In Flow Injection Analysis
During, the bubble produced during introducing or analyze from stream, particularly minute bubbles are easily rested in optical flow cell
Cannot discharge, because air pocket is easier discharge than minute bubbles, device of the present invention is by the time relay and magnetic valve
Coordinate, manually or automatically control the first magnetic valve to be communicated with air and by, full of air, this is equivalent to light in optical flow cell
One air pocket of introducing in flow cell is learned, and the optical flow cell is obliquely installed, the time relay is located at optical flow cell
Top, this is conducive to air smoothly into optical flow cell and being rapidly filled with, then by time relay magnetic valve
Cooperation, air pocket is discharged to reaction solution is passed through in optical flow cell, thus realize exhaust.
Compared with prior art, the invention has the advantages that：
1., the invention provides a kind of Flow Injection Analysis device with degassing function, it is a kind of flowing of new structure
Injection analyzer, is provided with the time relay, the first magnetic valve, the second magnetic valve or the 3rd magnetic valve, optical flow in the device
Logical pond is obliquely installed and the first magnetic valve is located at the top of optical flow cell, by the time relay and the second magnetic valve/3rd
The cooperation of magnetic valve and the first magnetic valve, can periodically or manually control the first magnetic valve to be passed through in optical flow cell air and by
Optical flow cell is full of, and, equivalent to an air pocket is introduced in optical flow cell, air pocket is easier discharge than minute bubbles for this,
Again by the cooperation of the time relay and the second magnetic valve/the 3rd magnetic valve and the first magnetic valve, to being passed through in optical flow cell
Reaction solution discharges air therein, you can the purpose of the whole bubbles in discharge optical flow cell is realized, with prior art phase
Than Flow Injection Analysis device of the present invention has simplified bleeding, good exhaust effect, is conducive to saving flow injection point
The advantage of the manpower of analysis.
2. optical flow cell is obliquely installed due to the Flow Injection Analysis device with degassing function of the present invention and
First magnetic valve is arranged on the top of optical flow cell, this be not only advantageous to air smoothly enter optical flow cell in and by its
Be rapidly filled with, and help avoid analysis during minute bubbles be trapped in optical flow cell, so as to ensure de-soak effect.
3. because the Flow Injection Analysis device with degassing function of the present invention also can be set debubbler, the debubbler
Can play a part of to reduce because sample introduction is to bubble is introduced in stream, can as far as possible be reduced to Flow Injection Analysis stream from source
In bubble, this advantageously reduces the frequency being vented during Flow Injection Analysis.
4. because the Flow Injection Analysis device with automatic ventilating function of the present invention can not only realize manual exhaust,
And on-line automatic exhaust can be realized, manual exhaust is applied to Flow Injection Analysis amount less and analysis is not allowed to be also easy to produce bubble
Sample situation, on-line automatic exhaust is particularly well-suited to the sample that batch-automated analysis and analysis easily produce bubble
Situation, with it is applied widely the characteristics of.
5. due to the simple structure of the Flow Injection Analysis device with automatic ventilating function of the present invention, for production
For new Flow Injection Analysis device, the advantage with easy to manufacture, for the repacking to existing Flow Injection Analysis device
For, with convenient advantage is reequiped, bleeding is simple in addition, good exhaust effect, thus application easy to spread.
Brief description of the drawings
Fig. 1 is the first structural representation of the Flow Injection Analysis device with automatic ventilating function of the present invention；
Fig. 2 is optical flow cell and the light path system of the Flow Injection Analysis device with automatic ventilating function of the present invention
The scheme of installation of system box；
Fig. 3 is second structural representation of the Flow Injection Analysis device with automatic ventilating function of the present invention；
Fig. 4 is the structural representation of the debubbler of the Flow Injection Analysis device with automatic ventilating function of the present invention
Figure；
Fig. 5 is the third structural representation of the Flow Injection Analysis device with automatic ventilating function of the present invention；
Fig. 6 is the 4th kind of structural representation of the Flow Injection Analysis device with automatic ventilating function of the present invention；
In figure, 1-low-lift pump, 2-six-way injection valve, the 3-the first blender, 4-reactor, 5-optical flow cell, 5-
1-feed pathway, 5-2-liquid outlet channel, 5-3-optical detecting channel, 6-fluorescence detector, 6-1-light path system box, 7-
Computer processing system, 8-waste fluid container, the 9-the first magnetic valve, 10-time relay, 11-support, the 12-the second mixing
Device, the 13-the second magnetic valve, the 14-the three magnetic valve, 15-debubbler, 15-1-feed tube, 15-2-closure, 15-3-
The angle of blast pipe, 15-4-drain pipe, the optical detecting channel of α-optical flow cell and horizontal plane, S-sample, C-promotion
Liquid, R-nitrite ion.
Specific embodiment
By the following examples with reference to accompanying drawing to the Flow Injection Analysis device with automatic ventilating function of the present invention
And its method for exhausting in Flow Injection Analysis is described further.
Embodiment 1
In the present embodiment, the structure of the Flow Injection Analysis device with degassing function as shown in figure 1, including low-lift pump 1,
Six-way injection valve 2, the first blender 3, reactor 4, optical flow cell 5, fluorescence detector 6, computer processing system 7 and waste liquid
Container 8, the optical flow cell 5 is U-shaped optical flow cell, including optical detecting channel 5-3 and is communicated with optical detecting channel
Feed pathway 5-1, liquid outlet channel 5-2, the fluorescence detector 6 include light path system box 6-1 and light signal collection processing system
System, the optical detecting channel 5-3 of optical flow cell is arranged in the light path system box of fluorescence detector, the detection of fluorescence detector
Optical detecting channel 5-3 and with the optical detecting channel of optical flow cell parallel, the low pressure of the light path through optical flow cell
Pump 1 is Multichannel constant-current pump, including sample S pump lines, promotes liquid C pump lines, nitrite ion R pump lines, and the device also includes the first electromagnetism
Valve 9, the time relay 10 and support 11, first magnetic valve 9 are three-way magnetic valve.
The support slant setting that the light path system box 6-1 of fluorescence detector 6 passes through support 11, the light of the fluorescence detector
The angle of inclination of road system box 6-1 should make the optical detecting channel 5-3 and water of the optical flow cell being arranged in light path system box
The angle α of plane is 25 °, the outlet port of the entrance location less than liquid outlet channel 5-2 of the feed pathway 5-1 of optical flow cell,
As shown in Figure 2.
The sample pump line of low-lift pump 1 and the liquid outlet of promotion liquid pump pipe are respectively by pipe fitting through six-way injection valve 2 and first
The entrance connection of blender 3, the liquid outlet of the nitrite ion pump line of low-lift pump 1 by pipe fitting directly with the entrance of the first blender 3
Connection, the outlet of the first blender 3 is connected by pipe fitting with the entrance of reactor 4, and the outlet of reactor 4 passes through pipe fitting and first
One inlet communication of magnetic valve 9, another import of the first magnetic valve 9 is communicated with air, and the outlet of the first magnetic valve 9 passes through
Pipe fitting is connected with the feed pathway 5-1 of optical flow cell, and the liquid outlet channel 5-2 of optical flow cell is by pipe fitting and waste fluid container 8
Connection, the light signal collection processing system of fluorescence detector 6 is connected with computer processing system 7, the time relay 10 and first
Magnetic valve 9 is connected, and the first magnetic valve 9 of control to input air or reaction solution in optical flow cell 5, pacify by first magnetic valve 9
Mounted in the top of optical flow cell, the entrance location of the installation site higher than the feed pathway of optical flow cell of the first magnetic valve
20cm。
It is using method for exhausting of the said apparatus in Flow Injection Analysis：
The pattern powered off after the time relay is set into manually opened energization, 20~60s of energization, in Flow Injection Analysis
During, the time relay 10 is not powered on, and when entering bubble in finding optical flow cell 5 and cannot exclude, closes low
Press pump 1 stops sample introduction, and the power supply of the manually opened time relay 10 makes the first magnetic valve 9 be communicated to optical flow cell with air
Middle input air, automatically powers off after 20~60s of time relay energization, and now optical flow cell has been filled entirely with air, the first electricity
Magnet valve 9 and the outlet of reactor, are then turned on the sample introduction of low-lift pump 1, are completely exhausted out to reaction solution is input into optical flow cell
Air therein is to complete bleeding, is further continued for carrying out Flow Injection Analysis.
Embodiment 2
In the present embodiment, the structure of the Flow Injection Analysis device with degassing function as shown in figure 3, including low-lift pump 1,
Six-way injection valve 2, the first blender 3, reactor 4, optical flow cell 5, fluorescence detector 6, computer processing system 7 and waste liquid
Container 8, the optical flow cell 5 is U-shaped optical flow cell, including optical detecting channel 5-3 and is communicated with optical detecting channel
Feed pathway 5-1, liquid outlet channel 5-2, the fluorescence detector 6 include light path system box 6-1 and light signal collection processing system
System, the optical detecting channel 5-3 of optical flow cell is arranged in the light path system box of fluorescence detector, the detection of fluorescence detector
Optical detecting channel 5-3 and with the optical detecting channel of optical flow cell parallel, the low pressure of the light path through optical flow cell
Pump 1 is Multichannel constant-current pump, including sample S pump lines, promotes liquid C pump lines, nitrite ion R pump lines, and the device also includes the first electromagnetism
Valve 9, the time relay 10, support 11 and a debubbler 15, first magnetic valve 9 are three-way magnetic valve, the debubbler
15 is closed vessel, and one end of the closed vessel is provided with the blast pipe 15-3 of feed tube 15-1 and with closure 15-2, another
End is provided with drain pipe 15-4, as shown in Figure 4.
The support slant setting that the light path system box 6-1 of fluorescence detector 6 passes through support 11, the light of the fluorescence detector
The angle of inclination of road system box 6-1 should make the optical detecting channel 5-3 and water of the optical flow cell being arranged in light path system box
The angle α of plane is 30 °, the outlet port of the entrance location less than liquid outlet channel 5-2 of the feed pathway 5-1 of optical flow cell,
As shown in Figure 2.
The outlet of the sample pump line of low-lift pump 1 connected by pipe fitting with the feed tube 15-1 of debubbler, and debubbler goes out liquid
Pipe 15-2 is connected through six-way injection valve 2 by pipe fitting with the entrance of the first blender 3, and the feed tube 15-1 of debubbler is located at out liquid
The top of pipe 15-2, the liquid outlet of the promotion liquid pump pipe of low-lift pump 1 passes through pipe fitting through the blender 3 of six-way injection valve 2 and first
Entrance is connected, and the liquid outlet of the nitrite ion pump line of low-lift pump 1 is connected by entrance of the pipe fitting directly with the first blender 3, and first
The outlet of blender 3 is connected by pipe fitting with the entrance of reactor 4, and the outlet of reactor 4 is by pipe fitting and the first magnetic valve 9
One inlet communication, another import of the first magnetic valve 9 is communicated with air, and the outlet of the first magnetic valve 9 passes through pipe fitting and light
The feed pathway 5-1 connections of flow cell are learned, the liquid outlet channel 5-2 of optical flow cell is connected by pipe fitting with waste fluid container 8, optics
The light signal collection processing system of detector 6 is connected with computer processing system 7, and the time relay 10 connects with the first magnetic valve 9
Connect, the first magnetic valve 9 of control is arranged on optical flow to input air or reaction solution in optical flow cell 5, first magnetic valve 9
The top in logical pond, the entrance location 30cm of the installation site higher than the feed pathway of optical flow cell of the first magnetic valve.
It is same as Example 1 using method for exhausting of the said apparatus in Flow Injection Analysis.
Embodiment 3
In the present embodiment, the structure of the Flow Injection Analysis device with degassing function as shown in figure 5, including low-lift pump 1,
Six-way injection valve 2, the first blender 3, reactor 4, optical flow cell 5, fluorescence detector 6, computer processing system 7 and waste liquid
Container 8, the optical flow cell 5 is U-shaped optical flow cell, including optical detecting channel 5-3 and is communicated with optical detecting channel
Feed pathway 5-1, liquid outlet channel 5-2, the fluorescence detector 6 include light path system box 6-1 and light signal collection processing system
System, the optical detecting channel 5-3 of optical flow cell is arranged in the light path system box of fluorescence detector, the detection of fluorescence detector
Optical detecting channel 5-3 and with the optical detecting channel of optical flow cell parallel, the low pressure of the light path through optical flow cell
Pump 1 is Multichannel constant-current pump, including sample S pump lines, promotes liquid C pump lines, nitrite ion R pump lines, and the device also includes the first electromagnetism
Valve 9, the time relay 10, support 11, the second blender 12, the second magnetic valve 13 and three debubblers 15, first electromagnetism
Valve 9 is three-way magnetic valve, the second magnetic valve 13 is two three-way electromagnetic valves, and the debubbler 15 is closed vessel, the closed vessel
One end is provided with the blast pipe 15-3 of feed tube 15-1 and with closure 15-2, and the other end is provided with drain pipe 15-4, such as Fig. 4 institutes
Show.
The support slant setting that the light path system box 6-1 of fluorescence detector 6 passes through support 11, the light of the fluorescence detector
The angle of inclination of road system box 6-1 should make the optical detecting channel 5-3 and water of the optical flow cell being arranged in light path system box
The angle α of plane is 45 °, the outlet port of the entrance location less than liquid outlet channel 5-2 of the feed pathway 5-1 of optical flow cell,
As shown in Figure 2.
The outlet of the sample pump line of low-lift pump 1 is connected by pipe fitting with the feed tube 15-1 of a debubbler, debubbler
Drain pipe 15-2 is connected through six-way injection valve 2 by pipe fitting with the entrance of the first blender 3, the promotion liquid pump pipe of low-lift pump 1
Liquid outlet is connected by pipe fitting with the feed tube 15-1 of a debubbler, the drain pipe 15-2 of debubbler by pipe fitting through six lead into
Sample valve 2 is connected with the entrance of the first blender 3, and the liquid outlet of the nitrite ion pump line of low-lift pump 1 passes through pipe fitting and a debubbler
Feed tube 15-1 connections, the drain pipe 15-2 of debubbler connected by pipe fitting with the entrance of the first blender 3, and above three is gone
Bubbler makes the feed tube 15-1 of debubbler be located at the top of drain pipe 15-2 when mounted.The outlet of the first blender 3 passes through
Pipe fitting is connected with the entrance of reactor 4, and the outlet of reactor 4 is connected by pipe fitting with the entrance of the second blender, the second mixing
The outlet of device passes through a pipe fitting import, the inlet communication of the second magnetic valve respectively with the first magnetic valve 8, the second magnetic valve
Outlet is connected by pipe fitting with waste fluid container 8, light signal collection processing system and the computer processing system 7 of fluorescence detector 6
Connection, the time relay 10 is connected with the first magnetic valve and the second magnetic valve respectively, controls the second magnetic valve by reaction solution
Input waste fluid container, the first magnetic valve of control are to input air in optical flow cell, or the first magnetic valve of control is to optical flow
Reaction solution, the second closed electromagnetic valve import of control are input into logical pond 5, reaction solution into the path of the second magnetic valve is blocked, it is described
First magnetic valve 9 is arranged on the top of optical flow cell, and the installation site of the first magnetic valve is led to higher than the feed liquor of optical flow cell
The entrance location 40cm in road.
The method being exhausted in Flow Injection Analysis using said apparatus is as follows：
1. method one：Manual exhaust
The pattern powered off after the time relay is set into manually opened energization, 20~60s of energization, in Flow Injection Analysis
During, the time relay is not powered on, manually opened when entering bubble in finding optical flow cell 5 and cannot exclude
The power supply of the time relay 10, it is useless that the second magnetic valve 13 of control connects the reaction solution input that will be exported by reactor with waste fluid container
In liquid container 8, while controlling the air inlet of the first magnetic valve 9 to be communicated with air to optical flow cell input air, time relay
Automatically powered off after 20~60s of device energization, now optical flow cell has been filled entirely with air, and reaction solution enters the path of the second magnetic valve
It is truncated, the outlet of the first magnetic valve 9 and reactor, the reaction solution exported by reactor enters optics through the first magnetic valve
Flow cell, after question response liquid excludes the air in optical flow cell completely, that is, completes bleeding, is further continued for carrying out flowing note
Penetrate analysis.
2. method two：On-line automatic exhaust
The circulation pattern for the time relay being set to after 10~90min of time delay to be powered, being powered off after the 20~60s that is powered, stream
After dynamic 10~90min of Injection Analysis, the time relay 10 is auto-power on, and the second magnetic valve 13 of control is connected with waste fluid container will be by
In the reaction solution input waste fluid container 8 of reactor output, while it is defeated to optical flow cell to control the first magnetic valve 9 to be communicated with air
Enter air, automatically powered off after 20~60s of time relay energization, now optical flow cell has been filled entirely with air, and reaction solution enters
The path of the second magnetic valve is truncated, the outlet of the first magnetic valve 9 and reactor, and the reaction solution exported by reactor is through the
One magnetic valve 9 enters in optical flow cell, after question response liquid excludes the air in optical flow cell completely, that is, completes once to arrange
Gas is operated, and Flow Injection Analysis and bleeding are hereafter proceeded in the manner previously described.
Embodiment 4
In the present embodiment, the structure of the Flow Injection Analysis device with degassing function as shown in fig. 6, including low-lift pump 1,
Six-way injection valve 2, the first blender 3, reactor 4, optical flow cell 5, fluorescence detector 6, computer processing system 7 and waste liquid
Container 8, the optical flow cell 5 is U-shaped optical flow cell, including optical detecting channel 5-3 and is communicated with optical detecting channel
Feed pathway 5-1, liquid outlet channel 5-2, the fluorescence detector 6 include light path system box 6-1 and light signal collection processing system
System, the optical detecting channel 5-3 of optical flow cell is arranged in the light path system box of fluorescence detector, the detection of fluorescence detector
Optical detecting channel 5-3 and with the optical detecting channel of optical flow cell parallel, the low pressure of the light path through optical flow cell
Pump 1 is Multichannel constant-current pump, including sample S pump lines, promotes liquid C pump lines, nitrite ion R pump lines, and the device also includes the first electromagnetism
Valve 9, the time relay 10, support 11, the 3rd magnetic valve 14 and three debubblers 15, first magnetic valve and the 3rd magnetic valve
Three-way magnetic valve is, the debubbler 15 is closed vessel, and one end of the closed vessel is provided with feed tube 15-1 and with close
The blast pipe 15-3 of 15-2 is covered, the other end is provided with drain pipe 15-4, as shown in Figure 4.
The support slant setting that the light path system box 6-1 of fluorescence detector 6 passes through support 11, the light of the fluorescence detector
The angle of inclination of road system box 6-1 should make the optical detecting channel 5-3 and water of the optical flow cell being arranged in light path system box
The angle α of plane is 35 °, the outlet port of the entrance location less than liquid outlet channel 5-2 of the feed pathway 5-1 of optical flow cell,
As shown in Figure 2.
The outlet of the sample pump line of low-lift pump 1 is connected by pipe fitting with the feed tube 15-1 of a debubbler, debubbler
Drain pipe 15-2 is connected through six-way injection valve 2 by pipe fitting with the entrance of the first blender 3, the promotion liquid pump pipe of low-lift pump 1
Liquid outlet is connected by pipe fitting with the feed tube 15-1 of a debubbler, the drain pipe 15-2 of debubbler by pipe fitting through six lead into
Sample valve 2 is connected with the entrance of the first blender 3, and the liquid outlet of the nitrite ion pump line of low-lift pump 1 passes through pipe fitting and a debubbler
Feed tube 15-1 connections, the drain pipe 15-2 of debubbler connected by pipe fitting with the entrance of the first blender 3, and above three is gone
Bubbler makes the feed tube 15-1 of debubbler be located at the top of drain pipe 15-2 when mounted.The outlet of the first blender 3 passes through
Pipe fitting is connected with the entrance of reactor 4, and the outlet of reactor 4 is by pipe fitting and the inlet communication of the 3rd magnetic valve, the 3rd electromagnetism
The one outlet of valve passes through pipe fitting by pipe fitting and an inlet communication of the first magnetic valve, another outlet of the 3rd magnetic valve
Connected with waste fluid container 8, the light signal collection processing system of fluorescence detector 6 is connected with computer processing system 7, the time
Relay 10 is connected with the first magnetic valve and the 3rd magnetic valve respectively, control the 3rd magnetic valve by reaction solution be input into waste fluid container,
The first magnetic valve is controlled to be circulated to optics to input air in optical flow cell, or the 3rd magnetic valve of control and the first magnetic valve
Reaction solution, the port closing for controlling the 3rd magnetic valve to be communicated with waste fluid container are input into pond 5, reaction solution from the 3rd magnetic valve is blocked
Into the path of waste fluid container 8, first magnetic valve 9 is arranged on the top of optical flow cell, the installation position of the first magnetic valve
Put the entrance location 35cm of the feed pathway higher than optical flow cell.
The method being exhausted in Flow Injection Analysis using said apparatus is as follows：
1. method one：Manual exhaust
The pattern powered off after the time relay is set into manually opened energization, 20~60s of energization, in Flow Injection Analysis
During, the time relay is not powered on, manually opened when entering bubble in finding optical flow cell 5 and cannot exclude
The power supply of the time relay 10, it is useless that the 3rd magnetic valve 14 of control connects the reaction solution input that will be exported by reactor with waste fluid container
In liquid container 8, while controlling the first magnetic valve 9 to be communicated with air to optical flow cell input air, time relay energization 20
Automatically powered off after~60s, now optical flow cell has been filled entirely with air, the outlet that the 3rd magnetic valve is communicated with waste fluid container is closed
Close, the first magnetic valve is connected with the 3rd magnetic valve, the reaction solution exported by reactor enters optical flow cell through the first magnetic valve
In, after question response liquid excludes the air in optical flow cell completely, that is, bleeding is completed, it is further continued for carrying out flow injection point
Analysis.
2. method two：On-line automatic exhaust
The circulation pattern for the time relay being set to after 10~90min of time delay to be powered, being powered off after the 20~60s that is powered, stream
After dynamic 10~90min of Injection Analysis, the time relay 10 is auto-power on, and the 3rd magnetic valve 14 of control is connected with waste fluid container will be by
In the reaction solution input waste fluid container 8 of reactor output, while it is defeated to optical flow cell to control the first magnetic valve 9 to be communicated with air
Enter air, automatically powered off after 20~60s of time relay energization, now optical flow cell has been filled entirely with air, the 3rd magnetic valve
The port closing communicated with waste fluid container, the first magnetic valve is connected with the 3rd magnetic valve, and the reaction solution exported by reactor is through the
One magnetic valve enters in optical flow cell, after question response liquid excludes the air in optical flow cell completely, that is, completes once to arrange
Secondary operation, hereafter proceeds Flow Injection Analysis and bleeding in the manner previously described.
Claims (8)
1. there is the Flow Injection Analysis device of degassing function, including low-lift pump (1), six-way injection valve (2), the first blender
(3), reactor (4), optical flow cell (5), fluorescence detector (6), computer processing system (7) and waste fluid container (8), described
Optical flow cell (5) including optical detecting channel (5-3) and the feed pathway (5-1) communicated with optical detecting channel, go out liquid lead to
Road (5-2), the fluorescence detector (6) includes light path system box (6-1) and light signal collection processing system, optical flow cell
Optical detecting channel (5-3) is arranged in the light path system box of fluorescence detector, and the detection light path of fluorescence detector is described in
Optical detecting channel (5-3) is simultaneously parallel with the optical detecting channel, it is characterised in that also including the first magnetic valve (9), time
Relay (10), support (11), the second blender (12) and the second magnetic valve (13), first magnetic valve (9) are powered for three
Magnet valve, the second magnetic valve are two three-way electromagnetic valves；
The support slant setting that the light path system box (6-1) of fluorescence detector passes through support (11), the feed liquor of optical flow cell leads to
Outlet port of the entrance location in road (5-1) less than liquid outlet channel (5-2)；The part liquid outlet of low-lift pump (1) is passed through by pipe fitting
Six-way injection valve (2) is connected with the entrance of the first blender (3), and the part liquid outlet of low-lift pump (1) is by pipe fitting directly with the
The entrance connection of one blender (3), the outlet of the first blender (3) is connected by pipe fitting with the entrance of reactor (4), reactor
(4) outlet is connected by pipe fitting with the entrance of the second blender, and the outlet of the second blender is electric with first respectively by pipe fitting
One import of magnet valve (9), the inlet communication of the second magnetic valve, the outlet of the second magnetic valve is by pipe fitting and waste fluid container (8)
Connection, another import of the first magnetic valve (9) is communicated with air, and the outlet of the first magnetic valve (9) passes through pipe fitting and optical flow
Feed pathway (5-1) connection in logical pond, the liquid outlet channel (5-2) of optical flow cell is connected by pipe fitting with waste fluid container (8), light
The light signal collection processing system for learning detector (6) is connected with computer processing system (7), and the time relay (10) is respectively
It is connected with the first magnetic valve and the second magnetic valve, reaction solution is input into waste fluid container, the first electromagnetism of control by the second magnetic valve of control
Valve is to input air in optical flow cell, or the first magnetic valve of control is to input reaction solution in optical flow cell (5), control the
Two closed electromagnetic valve imports, block reaction solution into the path of the second magnetic valve, and first magnetic valve (9) is installed in optical flow
The top in logical pond.
2. there is the Flow Injection Analysis device of degassing function, including low-lift pump (1), six-way injection valve (2), the first blender
(3), reactor (4), optical flow cell (5), fluorescence detector (6), computer processing system (7) and waste fluid container (8), described
Optical flow cell (5) including optical detecting channel (5-3) and the feed pathway (5-1) communicated with optical detecting channel, go out liquid lead to
Road (5-2), the fluorescence detector (6) includes light path system box (6-1) and light signal collection processing system, optical flow cell
Optical detecting channel (5-3) is arranged in the light path system box of fluorescence detector, and the detection light path of fluorescence detector is described in
Optical detecting channel (5-3) is simultaneously parallel with the optical detecting channel, it is characterised in that also including the first magnetic valve (9), time
Relay (10), support (11) and the 3rd magnetic valve (14), first magnetic valve (9) and the 3rd magnetic valve (14) are threeway
Magnetic valve；
The support slant setting that the light path system box (6-1) of fluorescence detector passes through support (11), the feed liquor of optical flow cell leads to
Outlet port of the entrance location in road (5-1) less than liquid outlet channel (5-2)；The part liquid outlet of low-lift pump (1) is passed through by pipe fitting
Six-way injection valve (2) is connected with the entrance of the first blender (3), and the part liquid outlet of low-lift pump (1) is by pipe fitting directly with the
The entrance connection of one blender (3), the outlet of the first blender (3) is connected by pipe fitting with the entrance of reactor (4), reactor
(4) by pipe fitting and the inlet communication of the 3rd magnetic valve, the one outlet of the 3rd magnetic valve is by pipe fitting and the first electricity for outlet
One inlet communication of magnet valve, another outlet of the 3rd magnetic valve is connected by pipe fitting with waste fluid container (8), the first magnetic valve
(9) another import is communicated with air, and the outlet of the first magnetic valve (9) is by pipe fitting and the feed pathway of optical flow cell
(5-1) is connected, and the liquid outlet channel (5-2) of optical flow cell is connected by pipe fitting with waste fluid container (8), fluorescence detector (6)
Light signal collection processing system is connected with computer processing system (7), the time relay (10) respectively with the first magnetic valve
With the connection of the 3rd magnetic valve, control the 3rd magnetic valve that reaction solution is input into waste fluid container, the first magnetic valve of control and circulated to optics
Input air in pond, or the 3rd magnetic valve of control and the first magnetic valve are to input reaction solution in optical flow cell (5), control the
The port closing that three magnetic valves are communicated with waste fluid container, blocks the path that reaction solution enters waste fluid container (8) from the 3rd magnetic valve,
First magnetic valve (9) is installed in the top of optical flow cell.
3. the Flow Injection Analysis device with degassing function according to claim 1 or claim 2, it is characterised in that the optics inspection
Surveying the angle of inclination of the light path system box (6-1) of device should lead to the optical detection of the optical flow cell being arranged in light path system box
Road (5-3) is 25~45 ° with the angle (α) of horizontal plane.
4. the Flow Injection Analysis device with degassing function according to claim 1 or claim 2, it is characterised in that also including de-soak
Device (15), the debubbler (15) is closed vessel, and one end of the closed vessel is provided with feed tube (15-1) and with closure
The blast pipe (15-3) of (15-2), the other end is provided with drain pipe (15-4)；
The debubbler (15) is at least 1, when debubbler (15) for 1 when, installed in connection low-lift pump (1) liquid outlet with
On one branch line of the inlet of six-way injection valve (2)；When debubbler (15) for two or more when, be respectively mounted
Connection low-lift pump (1) liquid outlet from the different branch lines of the inlet of six-way injection valve (2), or the company of being separately mounted to
The liquid outlet of low-lift pump (1) is connect to go out with connection low-lift pump (1) from the different branch lines of the inlet of six-way injection valve (2)
Liquid mouthful from the different branch lines of the first blender；Debubbler (15) should be located at the feed tube (15-1) of debubbler when installing
The top of drain pipe (15-4).
5. the Flow Injection Analysis device with degassing function according to claim 1 or claim 2, it is characterised in that first electricity
Entrance location at least 20cm of the installation site of magnet valve higher than the feed pathway of optical flow cell.
6. the Flow Injection Analysis device with degassing function according to claim 1 or claim 2, it is characterised in that the time after
Electrical equipment (10) is can the timing automatic powered off and on time relay.
7. a kind of method for exhausting during Flow Injection Analysis, it is characterised in that usage right 1 described device of requirement, operates as follows：
The pattern powered off after the time relay (10) is set into manually opened energization, 20~60s of energization, in Flow Injection Analysis
During, the time relay is not powered on, and when entering bubble in finding optical flow cell (5) and cannot exclude, opens manually
Open the power supply of the time relay, the second magnetic valve of control (13) by reaction solution be input into waste fluid container (8), the first magnetic valve (9) to
Input air in optical flow cell, automatically powers off after 20~60s of time relay energization, the second closed electromagnetic valve import of control,
First magnetic valve to reaction solution is input into optical flow cell, after question response liquid excludes the air in optical flow cell completely, i.e.,
Bleeding is completed, is further continued for carrying out Flow Injection Analysis；
Or the cyclic module for being set to after 10~90min of time delay to be powered by the time relay (10), powering off after the 20~60s that is powered
Formula, after 10~90min of Flow Injection Analysis, the time relay is auto-power on, and be input into for reaction solution by the second magnetic valve of control (13)
Waste fluid container (8), the first magnetic valve (9) to input air in optical flow cell (5), the time relay be powered after 20~60s from
Dynamic circuit breaker electricity, to being input into reaction solution in optical flow cell, question response liquid is by light for the second closed electromagnetic valve import of control, the first magnetic valve
After air in flow cell is excluded completely, that is, a bleeding is completed, flowing note is hereafter proceeded in the manner previously described
Penetrate analysis and bleeding.
8. a kind of method for exhausting during Flow Injection Analysis, it is characterised in that usage right 2 described devices of requirement, operates as follows：
The pattern powered off after the time relay is set into manually opened energization, 20~60s of energization, in Flow Injection Analysis process
In, the time relay is not powered on, and bubble is entered in optical flow cell is found and when cannot exclude, the manually opened time after
Reaction solution is input into waste fluid container (8), the first magnetic valve (9) and is circulated to optics by the power supply of electrical equipment, the 3rd magnetic valve (14) of control
Input air in pond (5), is automatically powered off after 20~60s of time relay energization, and the 3rd magnetic valve of control is communicated with waste fluid container
Port closing, the 3rd magnetic valve and the first magnetic valve circulate optics to reaction solution, question response liquid is input into optical flow cell
After air in pond is excluded completely, that is, bleeding is completed, be further continued for carrying out Flow Injection Analysis；
Or the circulation pattern for being set to after 10~90min of time delay to be powered by the time relay, powering off after the 20~60s that is powered, stream
After 10~90min of dynamic Injection Analysis, the time relay is auto-power on, and the 3rd magnetic valve (14) of control holds reaction solution input waste liquid
Device (8), the first magnetic valve (9) are automatically powered off to input air in optical flow cell (5) after 20~60s of time relay energization,
Port closing, the 3rd magnetic valve and the first magnetic valve that the 3rd magnetic valve is communicated with waste fluid container are controlled to defeated in optical flow cell
Enter reaction solution, after question response liquid excludes the air in optical flow cell completely, that is, complete once to arrange time operation, that is, complete once
Bleeding, hereafter proceeds Flow Injection Analysis and bleeding in the manner previously described.
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| CN108593834B (en) * | 2018-04-26 | 2020-04-07 | 深圳市华星光电半导体显示技术有限公司 | Ion chromatograph and sample injection method thereof |
| CN110646560B (en) * | 2019-10-10 | 2022-02-11 | 杭州浅海科技有限责任公司 | Flow injection method for uniformly distributing reagent |
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| CN201508363U (en) * | 2009-08-10 | 2010-06-16 | 国家海洋局第一海洋研究所 | A device for eliminating fine bubble from water in a total phosphorus analyzing flowing system |
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