CN105445484A - Flow injection analysis apparatus with exhausting function and exhausting method for flow injection analysis - Google Patents
Flow injection analysis apparatus with exhausting function and exhausting method for flow injection analysis Download PDFInfo
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- CN105445484A CN105445484A CN201510976695.1A CN201510976695A CN105445484A CN 105445484 A CN105445484 A CN 105445484A CN 201510976695 A CN201510976695 A CN 201510976695A CN 105445484 A CN105445484 A CN 105445484A
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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 invention provides a flow injection analysis apparatus with exhausting function. The apparatus comprises a low pressure pump, a six-way injection valve, a first mixer, a reactor, an optical flow cell, an optical detector, a computer processing system, a waste liquid container, a solenoid valve and a time relay which is matched with the solenoid valve. The invention also provides an exhausting method for flow injection analysis; the method is used for the flow injection analysis apparatus with exhausting function, and can be used for realizing hand-operated exhaust or automatic on-line exhaust during the flow injection analysis process; the exhaust operation is simple, the exhaust effect is good, and the analysis efficiency is improved.
Description
Technical field
The invention belongs to Flow Injection Analysis field, particularly there is method for exhausting during Flow Injection Analysis device and the Flow Injection Analysis of degassing function.
Background technology
Time Flow Injection Analysis (FIA), sample or standard specimen are injected in the reagent current-carrying of pipeline with the form of sample plug and carry out analytical test.In Flow Injection Analysis process, because the joint impermeability of flow path system degree of closure that is bad, valve is poor, adopt the reasons such as peristaltic pump feed liquor, easily from stream system, suck bubble, or owing to needing heating in Flow Injection Analysis process, cause the solubleness of gas in sample or standard specimen solution and current-carrying decline and discharge the liquid evaporation formation bubble in bubble or flow path system, the decomposition of reagent instability produces the reasons such as bubble, reaction generation bubble or reagent volatilization generation bubble and produce bubble in flow path system.The detection of the introducing of bubble often Interference Flow Injection Analysis signal, affects the accuracy of measurement result, even makes mensuration carry out time serious, therefore should avoid producing bubble and managing to eliminate the bubble produced in Flow Injection Analysis process as far as possible.
In flow path system, bubble is introduced in order to the least possible when Flow Injection Analysis, usually liquid will be promoted before sample introduction, the vacuumize degassing such as nitrite ion and sample solution or ultrasonic oscillation process are to reduce wherein dissolved gases, but this operation can only reduce introduces bubble in flow path system, but the bubble produced in stream cannot be eliminated, when the minute bubbles produced in flow path system be trapped in optical flow cell disturb normally detect time, can only Flow Injection Analysis device out of service, optical flow cell is taken out, the outer wall of optical flow cell is flicked repeatedly with finger, flick while the angle of transform optics flow cell, the minute bubbles be trapped in wherein are up moved gradually, continue to analyze until optical flow cell loads after all being discharged in Flow Injection Analysis device by minute bubbles again, the operation of the mode of this exhaust bubble is very loaded down with trivial details, be unfavorable for the raising of analysis efficiency, also human cost when saving Flow Injection Analysis is an impediment to.Li Jinxin etc. improve existing Flow Injection Analysis device, the pressure increase that a back-pressure circle makes stream system is installed additional after optical flow cell, the pressure increase of stream system can reduce the volatilization of solution, increase the solubleness of gas in water, and then reduce bubble to the interference (rock and mineral testing analyzed, 1996, 15 (2): 104-106), the Flow Injection Analysis device of this improvement can only reduce and discharges bubble because of heating or produce bubble because of solution evaporation, but the bubble that other reasons produces in flow path system cannot be eliminated, restricted application, and back-pressure circle may cause the pressure of flow path system too high, flow cell is caused to damage.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, the method for exhausting when Flow Injection Analysis device and Flow Injection Analysis with degassing function is provided, to simplify bleeding during Flow Injection Analysis, improve analysis efficiency.
The Flow Injection Analysis device having degassing function of the present invention, has three kinds of structures, and they belong to a total inventive concept.
The Flow Injection Analysis device with degassing function of the first structure of the present invention, structure is as follows:
This device comprises low-lift pump, six-way injection valve, first mixer, reactor, optical flow cell, fluorescence detector, computer processing system and waste fluid container, the feed pathway that described optical flow cell comprises optical detecting channel and communicates with optical detecting channel, liquid outlet channel, described fluorescence detector comprises light path system box and light signal collection disposal system, the optical detecting channel of optical flow cell is arranged in the light path system box of fluorescence detector, the detection light path of fluorescence detector is parallel with described optical detecting channel through described optical detecting channel, also comprise the first solenoid valve, the time relay and support, described first solenoid valve is three-way solenoid valve,
The light path system box of fluorescence detector is by the support slant setting of support, and the entrance location of the feed pathway of optical flow cell is lower than the exit position of liquid outlet channel, the part liquid outlet of low-lift pump is communicated with through the entrance of six-way injection valve with the first mixer by pipe fitting, the part liquid outlet of low-lift pump is directly communicated with the entrance of the first mixer by pipe fitting, the outlet of the first mixer is communicated with the entrance of reactor by pipe fitting, the outlet of reactor is by an inlet communication of pipe fitting and the first solenoid valve, another import of first solenoid valve communicates with air, the outlet of the first solenoid valve is communicated with the feed pathway of optical flow cell by pipe fitting, the liquid outlet channel of optical flow cell is communicated with waste fluid container by pipe fitting, the light signal collection disposal system of fluorescence detector is connected with computer processing system, the time relay is connected with the first solenoid valve, control the first solenoid valve to input air in optical flow cell or reactant liquor, described first solenoid valve is arranged on the top of optical flow cell.
The Flow Injection Analysis device with degassing function of the second structure of the present invention, on the basis of the device of the first structure above-mentioned, add the second mixer and the second solenoid valve, described second solenoid valve is two three-way electromagnetic valves, the outlet of reactor is communicated with by the entrance of pipe fitting with the second mixer, the outlet of the second mixer by pipe fitting respectively with an import of the first solenoid valve, the inlet communication of the second solenoid valve, the outlet of the second solenoid valve is communicated with waste fluid container by pipe fitting, the described time relay is connected with the first solenoid valve and the second solenoid valve respectively, control the second solenoid valve and reactant liquor is inputted waste fluid container, control the first solenoid valve to input air in optical flow cell, or control the first solenoid valve and input reactant liquor in optical flow cell, control the second closed electromagnetic valve import, block the path that reactant liquor enters the second solenoid valve.
The Flow Injection Analysis device with degassing function of the third structure of the present invention, on the basis of the device of the first structure above-mentioned, add the 3rd solenoid valve, described 3rd solenoid valve is three-way solenoid valve, the outlet of reactor is by the inlet communication of pipe fitting and the 3rd solenoid valve, one of 3rd solenoid valve exports an inlet communication by pipe fitting and the first solenoid valve, another outlet of 3rd solenoid valve is communicated with waste fluid container by pipe fitting, the described time relay is connected with the first solenoid valve and the 3rd solenoid valve respectively, control the 3rd solenoid valve and reactant liquor is inputted waste fluid container, control the first solenoid valve to input air in optical flow cell, or control the 3rd solenoid valve and the first solenoid valve input reactant liquor in optical flow cell, control the port closing that the 3rd solenoid valve communicates with waste fluid container, block reactant liquor enters waste fluid container path from the 3rd solenoid valve.
In technique scheme, the angle of inclination of the light path system box of described fluorescence detector should make the optical detecting channel of the optical flow cell be arranged in light path system box and the angle α of surface level be 25 ~ 45 °.
In technique scheme, also comprise de-soak device, described de-soak device is closed container, and one end of this closed container is provided with the gas outlet of feed tube and with closure, and the other end is provided with drain pipe; Described de-soak device is at least 1, when de-soak device is 1, be arranged on connect the liquid outlet of low-lift pump and the inlet of six-way injection valve a branch line on, be preferably mounted on pipeline that low-lift pump pumps between the liquid outlet of the pump line of sample or standard specimen and the inlet of six-way injection valve; When de-soak device is two or more, be arranged on respectively connect the liquid outlet of low-lift pump from the different branch lines of the inlet of six-way injection valve, or be arranged on respectively connect the liquid outlet of low-lift pump from the different branch lines of the inlet of six-way injection valve with connect on the liquid outlet of low-lift pump and the different branch lines of the first mixer; De-soak device should make the feed tube of de-soak device be positioned at the top of drain pipe when installing.
Described de-soak device can play and reduce because sample introduction introduces the effect of bubble in stream, its working method is as follows: the sample of sample introduction is from the feed tube instillation closed container of closed container upper end, then the drain pipe through closed container lower end enters in six-way injection valve or the first mixer through pipe fitting, the bottom of closed container is full of liquid, top is full of air, if introduce bubble during sample introduction, then sample is in the process from feed tube instillation closed container bottom, bubble can enter the top of closed container with drop separation, thus play the effect reducing bubble, when gas in container to be closed is too much, need the gland bonnet discharge section gas opened on gas outlet.
In technique scheme, the top first solenoid valve being arranged on optical flow cell is in order to ensure can successfully to input air in optical flow cell when the first solenoid valve communicates with air, preferably, the installation site of described first solenoid valve is higher than the entrance location at least 20cm of the feed pathway of optical flow cell.
In technique scheme, low-lift pump is Multichannel constant-current pump, and the quantity of the stream that low-lift pump specifically adopts and the annexation of each liquid outlet and six-way injection valve or the first mixer need to arrange according to actual analysis.
In technique scheme, the described time relay is the time relay of energy timing automatic power-off and energising, and preferably circulate timing relay.
The method for exhausting of device when Flow Injection Analysis of the first structure above-mentioned is: the time relay is set to manually opened energising, the pattern of power-off after energising 20 ~ 60s, in Flow Injection Analysis process, the time relay is not energized, when finding enter bubble in optical flow cell and cannot get rid of, close low-lift pump and stop sample introduction, the power supply of the manually opened time relay, make the first solenoid valve to input air in optical flow cell, auto-breaking after time relay energising 20 ~ 60s, open low-lift pump sample introduction, in optical flow cell, input the air that reactant liquor discharges in optical flow cell completely namely complete bleeding, proceed Flow Injection Analysis again.
The device of above-mentioned the second structure can realize manual exhaust and on-line automatic exhaust when Flow Injection Analysis, wherein, the method of manual exhaust is: the time relay is set to manually opened energising, the pattern of power-off after energising 20 ~ 60s, in Flow Injection Analysis process, the time relay is not energized, when finding enter bubble in optical flow cell and cannot get rid of, the power supply of the manually opened time relay, control the second solenoid valve and reactant liquor is inputted waste fluid container, first solenoid valve is to input air in optical flow cell, auto-breaking after time relay energising 20 ~ 60s, control the second closed electromagnetic valve import, first solenoid valve inputs reactant liquor in optical flow cell, after air in optical flow cell is got rid of by question response liquid completely, namely bleeding is completed, proceed Flow Injection Analysis again,
The method of on-line automatic exhaust is: be energized after the time relay being set to time delay 10 ~ 90min, the circulation pattern of power-off after energising 20 ~ 60s, after Flow Injection Analysis 10 ~ 90min, the time relay is energized automatically, control the second solenoid valve and reactant liquor is inputted waste fluid container, first solenoid valve is to input air in optical flow cell, auto-breaking after time relay energising 20 ~ 60s, control the second closed electromagnetic valve import, first solenoid valve inputs reactant liquor in optical flow cell, after air in optical flow cell is got rid of by question response liquid completely, namely a bleeding is completed, after this Flow Injection Analysis and bleeding is proceeded according to aforementioned manner.
The device of the third type above-mentioned can realize manual exhaust and on-line automatic exhaust when Flow Injection Analysis, wherein, the method of manual exhaust is: the time relay is set to manually opened energising, the pattern of power-off after energising 20 ~ 60s, in Flow Injection Analysis process, the time relay is not energized, when finding enter bubble in optical flow cell and cannot get rid of, the power supply of the manually opened time relay, control the 3rd solenoid valve and reactant liquor is inputted waste fluid container, first solenoid valve is to input air in optical flow cell, auto-breaking after time relay energising 20 ~ 60s, control the port closing that the 3rd solenoid valve communicates with waste fluid container, 3rd solenoid valve and the first solenoid valve input reactant liquor in optical flow cell, after air in optical flow cell is got rid of by question response liquid completely, namely bleeding is completed, proceed Flow Injection Analysis again,
Be energized after the time relay being set to time delay 10 ~ 90min, the circulation pattern of power-off after energising 20 ~ 60s, after Flow Injection Analysis 10 ~ 90min, the time relay is energized automatically, control the 3rd solenoid valve and reactant liquor is inputted waste fluid container, first solenoid valve is to input air in optical flow cell, auto-breaking after time relay energising 20 ~ 60s, control the port closing that the 3rd solenoid valve communicates with waste fluid container, 3rd solenoid valve and the first solenoid valve input reactant liquor in optical flow cell, after air in optical flow cell is got rid of by question response liquid completely, namely row's time operation is completed once, namely a bleeding is completed, after this Flow Injection Analysis and bleeding is proceeded according to aforementioned manner.
The venting principleand with the Flow Injection Analysis device of degassing function of the present invention is as follows: in Flow Injection Analysis process, the bubble introduced from stream or produce in analytic process, particularly minute bubbles easily rest in optical flow cell and cannot discharge, discharge because air pocket is easier than minute bubbles, device of the present invention is coordinated by the time relay and solenoid valve, control the first solenoid valve manually or automatically communicate with air and be full of air by optical flow cell, this is equivalent to introduce an air pocket in optical flow cell, and described optical flow cell is obliquely installed, the time relay is positioned at the top of optical flow cell, this is conducive to air and enters smoothly in optical flow cell and it to be full of fast, again by the cooperation of time relay solenoid valve, in optical flow cell, pass into reactant liquor air pocket is discharged, thus realize exhaust.
Compared with prior art, the present invention has following beneficial effect:
1. the invention provides a kind of Flow Injection Analysis device with degassing function, it is a kind of Flow Injection Analysis device of new structure, the time relay is provided with in this device, first solenoid valve, second solenoid valve or the 3rd solenoid valve, optical flow cell is obliquely installed and the first solenoid valve is positioned at the top of optical flow cell, by coordinating of the time relay and the second solenoid valve/the 3rd solenoid valve and the first solenoid valve, can regularly or Non-follow control first solenoid valve in optical flow cell, pass into air and optical flow cell be full of, this is equivalent to introduce an air pocket in optical flow cell, air pocket is easier than minute bubbles discharges, coordinating again by the time relay and the second solenoid valve/the 3rd solenoid valve and the first solenoid valve, in optical flow cell, pass into reactant liquor air is wherein discharged, the object of whole bubbles of discharging in optical flow cell can be realized, compared with prior art, Flow Injection Analysis device of the present invention has simplification bleeding, good exhaust effect, be conducive to the advantage of the manpower saving Flow Injection Analysis.
2. because optical flow cell is obliquely installed by the Flow Injection Analysis device with degassing function of the present invention and the first solenoid valve is arranged on the top of optical flow cell, this is not only conducive to air and enters smoothly in optical flow cell and it to be full of fast, and help avoid the medium and small bubble residence of analytic process in optical flow cell, thus ensure de-soak effect.
3. because the Flow Injection Analysis device with degassing function of the present invention also can arrange de-soak device, this de-soak device can play and reduce because sample introduction introduces the effect of bubble in stream, can try one's best from source and reduce to the bubble in Flow Injection Analysis stream, this is conducive to the frequency be vented when reducing Flow Injection Analysis.
4. because the Flow Injection Analysis device with automatic ventilating function of the present invention not only can realize manual exhaust, and on-line automatic exhaust can be realized, it is little and analyze the situation being not easy the sample producing bubble that manual exhaust is applicable to Flow Injection Analysis amount, on-line automatic exhaust is specially adapted to batch-automated analysis and analyzes the situation of the sample easily producing bubble, has feature applied widely.
5. because the structure with the Flow Injection Analysis device of automatic ventilating function of the present invention is simple, for the Flow Injection Analysis device that production is new, there is the advantage easily manufactured, for the repacking for existing Flow Injection Analysis device, have and reequip advantage easily, in addition simple, the good exhaust effect of bleeding, is thus easy to apply.
Accompanying drawing explanation
Fig. 1 is the first structural representation with the Flow Injection Analysis device of automatic ventilating function of the present invention;
Fig. 2 of the present inventionly has the optical flow cell of the Flow Injection Analysis device of automatic ventilating function and the scheme of installation of light path system box;
Fig. 3 is the second structural representation with the Flow Injection Analysis device of automatic ventilating function of the present invention;
Fig. 4 is the structural representation with the de-soak device of the Flow Injection Analysis device of automatic ventilating function of the present invention;
Fig. 5 is the third structural representation with the Flow Injection Analysis device of automatic ventilating function of the present invention;
Fig. 6 is the 4th kind of structural representation with the Flow Injection Analysis device of automatic ventilating function of the present invention;
In figure, 1-low-lift pump, 2-six-way injection valve, 3-the first mixer, 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, 9-the first solenoid valve, 10-time relay, 11-support, 12-the second mixer, 13-the second solenoid valve, 14-the three solenoid valve, 15-de-soak device, 15-1-feed tube, 15-2-gland bonnet, 15-3-gas outlet, 15-4-drain pipe, the optical detecting channel of α-optical flow cell and the angle of surface level, S-sample, C-promotion liquid, R-nitrite ion.
Embodiment
The Flow Injection Analysis device having an automatic ventilating function to of the present invention by reference to the accompanying drawings by the following examples and the method for exhausting when Flow Injection Analysis thereof are described further.
Embodiment 1
In the present embodiment, the structure with the Flow Injection Analysis device of degassing function as shown in Figure 1, comprises low-lift pump 1, six-way injection valve 2, first mixer 3, reactor 4, optical flow cell 5, fluorescence detector 6, computer processing system 7 and waste fluid container 8, described optical flow cell 5 is U-shaped optical flow cell, the feed pathway 5-1 comprising optical detecting channel 5-3 and communicate with optical detecting channel, liquid outlet channel 5-2, described fluorescence detector 6 comprises light path system box 6-1 and light signal collection disposal system, the optical detecting channel 5-3 of optical flow cell is arranged in the light path system box of fluorescence detector, the detection light path of fluorescence detector is parallel with the optical detecting channel of optical flow cell through the optical detecting channel 5-3 of optical flow cell, described low-lift pump 1 is Multichannel constant-current pump, comprises sample S pump line, promote liquid C pump line, nitrite ion R pump line, this device also comprises the first solenoid valve 9, the time relay 10 and support 11, described first solenoid valve 9 is three-way solenoid valve.
The light path system box 6-1 of fluorescence detector 6 passes through the support slant setting of support 11, the angle of inclination of the light path system box 6-1 of described fluorescence detector should make the angle α of the optical detecting channel 5-3 and surface level being arranged on the optical flow cell in light path system box be 25 °, the entrance location of the feed pathway 5-1 of optical flow cell lower than the exit position of liquid outlet channel 5-2, as shown in Figure 2.
The sample pump line of low-lift pump 1 is communicated with through the entrance of six-way injection valve 2 with the first mixer 3 respectively by pipe fitting with the liquid outlet promoting liquid pump pipe, the liquid outlet of the nitrite ion pump line of low-lift pump 1 is directly communicated with the entrance of the first mixer 3 by pipe fitting, the outlet of the first mixer 3 is communicated with by the entrance of pipe fitting with reactor 4, the outlet of reactor 4 is by an inlet communication of pipe fitting and the first solenoid valve 9, another import of first solenoid valve 9 communicates with air, the outlet of the first solenoid valve 9 is communicated with the feed pathway 5-1 of optical flow cell by pipe fitting, the liquid outlet channel 5-2 of optical flow cell is communicated with waste fluid container 8 by pipe fitting, the light signal collection disposal system of fluorescence detector 6 is connected with computer processing system 7, the time relay 10 is connected with the first solenoid valve 9, control the first solenoid valve 9 to input air or reactant liquor in optical flow cell 5, described first solenoid valve 9 is arranged on the top of optical flow cell, the installation site of the first solenoid valve is higher than the entrance location 20cm of the feed pathway of optical flow cell.
The method for exhausting of use said apparatus when Flow Injection Analysis is:
The time relay is set to manually opened energising, the pattern of power-off after energising 20 ~ 60s, in Flow Injection Analysis process, the time relay 10 is not energized, when finding enter bubble in optical flow cell 5 and cannot get rid of, close low-lift pump 1 and stop sample introduction, the power supply of the manually opened time relay 10, first solenoid valve 9 is communicated with air input air in optical flow cell, auto-breaking after time relay energising 20 ~ 60s, now optical flow cell is filled entirely with air, the outlet of the first solenoid valve 9 and reactor, then low-lift pump 1 sample introduction is opened, in optical flow cell, input the air that reactant liquor discharges wherein completely namely complete bleeding, proceed Flow Injection Analysis again.
Embodiment 2
In the present embodiment, there is the structure of the Flow Injection Analysis device of degassing function as shown in Figure 3, comprise low-lift pump 1, six-way injection valve 2, first mixer 3, reactor 4, optical flow cell 5, fluorescence detector 6, computer processing system 7 and waste fluid container 8, described optical flow cell 5 is U-shaped optical flow cell, the feed pathway 5-1 comprising optical detecting channel 5-3 and communicate with optical detecting channel, liquid outlet channel 5-2, described fluorescence detector 6 comprises light path system box 6-1 and light signal collection disposal system, the optical detecting channel 5-3 of optical flow cell is arranged in the light path system box of fluorescence detector, the detection light path of fluorescence detector is parallel with the optical detecting channel of optical flow cell through the optical detecting channel 5-3 of optical flow cell, described low-lift pump 1 is Multichannel constant-current pump, comprise sample S pump line, promote liquid C pump line, nitrite ion R pump line, this device also comprises the first solenoid valve 9, the time relay 10, support 11 and a de-soak device 15, described first solenoid valve 9 is three-way solenoid valve, described de-soak device 15 is closed container, one end of this closed container is provided with the gas outlet 15-3 of feed tube 15-1 and with closure 15-2, the other end is provided with drain pipe 15-4, as shown in Figure 4.
The light path system box 6-1 of fluorescence detector 6 passes through the support slant setting of support 11, the angle of inclination of the light path system box 6-1 of described fluorescence detector should make the angle α of the optical detecting channel 5-3 and surface level being arranged on the optical flow cell in light path system box be 30 °, the entrance location of the feed pathway 5-1 of optical flow cell lower than the exit position of liquid outlet channel 5-2, as shown in Figure 2.
The outlet of the sample pump line of low-lift pump 1 is communicated with the feed tube 15-1 of de-soak device by pipe fitting, the drain pipe 15-2 of de-soak device is communicated with through the entrance of six-way injection valve 2 with the first mixer 3 by pipe fitting, the feed tube 15-1 of de-soak device is positioned at the top of drain pipe 15-2, the liquid outlet of the promotion liquid pump pipe of low-lift pump 1 is communicated with through the entrance of six-way injection valve 2 with the first mixer 3 by pipe fitting, the liquid outlet of the nitrite ion pump line of low-lift pump 1 is directly communicated with the entrance of the first mixer 3 by pipe fitting, the outlet of the first mixer 3 is communicated with by the entrance of pipe fitting with reactor 4, the outlet of reactor 4 is by an inlet communication of pipe fitting and the first solenoid valve 9, another import of first solenoid valve 9 communicates with air, the outlet of the first solenoid valve 9 is communicated with the feed pathway 5-1 of optical flow cell by pipe fitting, the liquid outlet channel 5-2 of optical flow cell is communicated with waste fluid container 8 by pipe fitting, the light signal collection disposal system of fluorescence detector 6 is connected with computer processing system 7, the time relay 10 is connected with the first solenoid valve 9, control the first solenoid valve 9 to input air or reactant liquor in optical flow cell 5, described first solenoid valve 9 is arranged on the top of optical flow cell, the installation site of the first solenoid valve is higher than the entrance location 30cm of the feed pathway of optical flow cell.
Use the method for exhausting of said apparatus when Flow Injection Analysis identical with embodiment 1.
Embodiment 3
In the present embodiment, the structure with the Flow Injection Analysis device of degassing function as shown in Figure 5, comprises low-lift pump 1, six-way injection valve 2, first mixer 3, reactor 4, optical flow cell 5, fluorescence detector 6, computer processing system 7 and waste fluid container 8, described optical flow cell 5 is U-shaped optical flow cell, the feed pathway 5-1 comprising optical detecting channel 5-3 and communicate with optical detecting channel, liquid outlet channel 5-2, described fluorescence detector 6 comprises light path system box 6-1 and light signal collection disposal system, the optical detecting channel 5-3 of optical flow cell is arranged in the light path system box of fluorescence detector, the detection light path of fluorescence detector is parallel with the optical detecting channel of optical flow cell through the optical detecting channel 5-3 of optical flow cell, described low-lift pump 1 is Multichannel constant-current pump, comprises sample S pump line, promote liquid C pump line, nitrite ion R pump line, this device also comprises the first solenoid valve 9, the time relay 10, support 11, second mixer 12, second solenoid valve 13 and three de-soak devices 15, described first solenoid valve 9 is three-way solenoid valve, second solenoid valve 13 is two three-way electromagnetic valves, and described de-soak device 15 is closed container, and one end of this closed container is provided with the gas outlet 15-3 of feed tube 15-1 and with closure 15-2, and the other end is provided with drain pipe 15-4, as shown in Figure 4.
The light path system box 6-1 of fluorescence detector 6 passes through the support slant setting of support 11, the angle of inclination of the light path system box 6-1 of described fluorescence detector should make the angle α of the optical detecting channel 5-3 and surface level being arranged on the optical flow cell in light path system box be 45 °, the entrance location of the feed pathway 5-1 of optical flow cell lower than the exit position of liquid outlet channel 5-2, as shown in Figure 2.
The outlet of the sample pump line of low-lift pump 1 is communicated with the feed tube 15-1 of a de-soak device by pipe fitting, the drain pipe 15-2 of de-soak device is communicated with through the entrance of six-way injection valve 2 with the first mixer 3 by pipe fitting, the liquid outlet of the promotion liquid pump pipe of low-lift pump 1 is communicated with the feed tube 15-1 of a de-soak device by pipe fitting, the drain pipe 15-2 of de-soak device is communicated with through the entrance of six-way injection valve 2 with the first mixer 3 by pipe fitting, the liquid outlet of the nitrite ion pump line of low-lift pump 1 is communicated with the feed tube 15-1 of a de-soak device by pipe fitting, the drain pipe 15-2 of de-soak device is communicated with by the entrance of pipe fitting with the first mixer 3, above-mentioned three de-soak devices all make the feed tube 15-1 of de-soak device be positioned at the top of drain pipe 15-2 when mounted.The outlet of the first mixer 3 is communicated with by the entrance of pipe fitting with reactor 4, the outlet of reactor 4 is communicated with by the entrance of pipe fitting with the second mixer, the outlet of the second mixer by pipe fitting respectively with an import of the first solenoid valve 8, the inlet communication of the second solenoid valve, the outlet of the second solenoid valve is communicated with waste fluid container 8 by pipe fitting, the light signal collection disposal system of fluorescence detector 6 is connected with computer processing system 7, the described time relay 10 is connected with the first solenoid valve and the second solenoid valve respectively, control the second solenoid valve and reactant liquor is inputted waste fluid container, control the first solenoid valve to input air in optical flow cell, or control the first solenoid valve and input reactant liquor in optical flow cell 5, control the second closed electromagnetic valve import, block the path that reactant liquor enters the second solenoid valve, described first solenoid valve 9 is arranged on the top of optical flow cell, the installation site of the first solenoid valve is higher than the entrance location 40cm of the feed pathway of optical flow cell.
The method using said apparatus to be exhausted when Flow Injection Analysis is as follows:
1. method one: manual exhaust
The time relay is set to manually opened energising, the pattern of power-off after energising 20 ~ 60s, in Flow Injection Analysis process, the time relay is not energized, when finding enter bubble in optical flow cell 5 and cannot get rid of, the power supply of the manually opened time relay 10, control the second solenoid valve 13 to be communicated with waste fluid container the reactant liquor exported by reactor is inputted in waste fluid container 8, the air intake opening simultaneously controlling the first solenoid valve 9 communicates with air to optical flow cell input air, auto-breaking after time relay energising 20 ~ 60s, now optical flow cell is filled entirely with air, the path that reactant liquor enters the second solenoid valve is truncated, the outlet of the first solenoid valve 9 and reactor, the reactant liquor exported by reactor enters optical flow cell through the first solenoid valve, after air in optical flow cell is got rid of by question response liquid completely, namely bleeding is completed, proceed Flow Injection Analysis again.
2. method two: on-line automatic exhaust
Be energized after the time relay being set to time delay 10 ~ 90min, the circulation pattern of power-off after energising 20 ~ 60s, after Flow Injection Analysis 10 ~ 90min, the time relay 10 is energized automatically, control the second solenoid valve 13 to be communicated with waste fluid container the reactant liquor exported by reactor is inputted in waste fluid container 8, control the first solenoid valve 9 to communicate with air to optical flow cell input air simultaneously, auto-breaking after time relay energising 20 ~ 60s, now optical flow cell is filled entirely with air, the path that reactant liquor enters the second solenoid valve is truncated, the outlet of the first solenoid valve 9 and reactor, the reactant liquor exported by reactor enters in optical flow cell through the first solenoid valve 9, after air in optical flow cell is got rid of by question response liquid completely, namely a bleeding is completed, after this Flow Injection Analysis and bleeding is proceeded according to aforementioned manner.
Embodiment 4
In the present embodiment, there is the structure of the Flow Injection Analysis device of degassing function as shown in Figure 6, comprise low-lift pump 1, six-way injection valve 2, first mixer 3, reactor 4, optical flow cell 5, fluorescence detector 6, computer processing system 7 and waste fluid container 8, described optical flow cell 5 is U-shaped optical flow cell, the feed pathway 5-1 comprising optical detecting channel 5-3 and communicate with optical detecting channel, liquid outlet channel 5-2, described fluorescence detector 6 comprises light path system box 6-1 and light signal collection disposal system, the optical detecting channel 5-3 of optical flow cell is arranged in the light path system box of fluorescence detector, the detection light path of fluorescence detector is parallel with the optical detecting channel of optical flow cell through the optical detecting channel 5-3 of optical flow cell, described low-lift pump 1 is Multichannel constant-current pump, comprise sample S pump line, promote liquid C pump line, nitrite ion R pump line, this device also comprises the first solenoid valve 9, the time relay 10, support 11, 3rd solenoid valve 14 and three de-soak devices 15, described first solenoid valve and the 3rd solenoid valve are three-way solenoid valve, described de-soak device 15 is closed container, one end of this closed container is provided with the gas outlet 15-3 of feed tube 15-1 and with closure 15-2, the other end is provided with drain pipe 15-4, as shown in Figure 4.
The light path system box 6-1 of fluorescence detector 6 passes through the support slant setting of support 11, the angle of inclination of the light path system box 6-1 of described fluorescence detector should make the angle α of the optical detecting channel 5-3 and surface level being arranged on the optical flow cell in light path system box be 35 °, the entrance location of the feed pathway 5-1 of optical flow cell lower than the exit position of liquid outlet channel 5-2, as shown in Figure 2.
The outlet of the sample pump line of low-lift pump 1 is communicated with the feed tube 15-1 of a de-soak device by pipe fitting, the drain pipe 15-2 of de-soak device is communicated with through the entrance of six-way injection valve 2 with the first mixer 3 by pipe fitting, the liquid outlet of the promotion liquid pump pipe of low-lift pump 1 is communicated with the feed tube 15-1 of a de-soak device by pipe fitting, the drain pipe 15-2 of de-soak device is communicated with through the entrance of six-way injection valve 2 with the first mixer 3 by pipe fitting, the liquid outlet of the nitrite ion pump line of low-lift pump 1 is communicated with the feed tube 15-1 of a de-soak device by pipe fitting, the drain pipe 15-2 of de-soak device is communicated with by the entrance of pipe fitting with the first mixer 3, above-mentioned three de-soak devices all make the feed tube 15-1 of de-soak device be positioned at the top of drain pipe 15-2 when mounted.The outlet of the first mixer 3 is communicated with by the entrance of pipe fitting with reactor 4, the outlet of reactor 4 is by the inlet communication of pipe fitting and the 3rd solenoid valve, one of 3rd solenoid valve exports an inlet communication by pipe fitting and the first solenoid valve, another outlet of 3rd solenoid valve is communicated with waste fluid container 8 by pipe fitting, the light signal collection disposal system of fluorescence detector 6 is connected with computer processing system 7, the described time relay 10 is connected with the first solenoid valve and the 3rd solenoid valve respectively, control the 3rd solenoid valve and reactant liquor is inputted waste fluid container, control the first solenoid valve to input air in optical flow cell, or control the 3rd solenoid valve and the first solenoid valve input reactant liquor in optical flow cell 5, control the port closing that the 3rd solenoid valve communicates with waste fluid container, block reactant liquor enters waste fluid container 8 path from the 3rd solenoid valve, described first solenoid valve 9 is arranged on the top of optical flow cell, the installation site of the first solenoid valve is higher than the entrance location 35cm of the feed pathway of optical flow cell.
The method adopting said apparatus to be exhausted when Flow Injection Analysis is as follows:
1. method one: manual exhaust
The time relay is set to manually opened energising, the pattern of power-off after energising 20 ~ 60s, in Flow Injection Analysis process, the time relay is not energized, when finding enter bubble in optical flow cell 5 and cannot get rid of, the power supply of the manually opened time relay 10, control the 3rd solenoid valve 14 to be communicated with waste fluid container the reactant liquor exported by reactor is inputted in waste fluid container 8, control the first solenoid valve 9 to communicate with air to optical flow cell input air simultaneously, auto-breaking after time relay energising 20 ~ 60s, now optical flow cell is filled entirely with air, the port closing that 3rd solenoid valve communicates with waste fluid container, first solenoid valve is communicated with the 3rd solenoid valve, the reactant liquor exported by reactor enters in optical flow cell through the first solenoid valve, after air in optical flow cell is got rid of by question response liquid completely, namely bleeding is completed, proceed Flow Injection Analysis again.
2. method two: on-line automatic exhaust
Be energized after the time relay being set to time delay 10 ~ 90min, the circulation pattern of power-off after energising 20 ~ 60s, after Flow Injection Analysis 10 ~ 90min, the time relay 10 is energized automatically, control the 3rd solenoid valve 14 to be communicated with waste fluid container the reactant liquor exported by reactor is inputted in waste fluid container 8, control the first solenoid valve 9 to communicate with air to optical flow cell input air simultaneously, auto-breaking after time relay energising 20 ~ 60s, now optical flow cell is filled entirely with air, the port closing that 3rd solenoid valve communicates with waste fluid container, first solenoid valve is communicated with the 3rd solenoid valve, the reactant liquor exported by reactor enters in optical flow cell through the first solenoid valve, after air in optical flow cell is got rid of by question response liquid completely, namely row's time operation is completed once, after this Flow Injection Analysis and bleeding is proceeded according to aforementioned manner.
Claims (10)
1. there is the Flow Injection Analysis device of degassing function, comprise low-lift pump (1), six-way injection valve (2), first mixer (3), reactor (4), optical flow cell (5), fluorescence detector (6), computer processing system (7) and waste fluid container (8), the feed pathway (5-1) that described optical flow cell (5) comprises optical detecting channel (5-3) and communicates with optical detecting channel, liquid outlet channel (5-2), described fluorescence detector (6) comprises light path system box (6-1) and light signal collection disposal system, the optical detecting channel (5-3) of optical flow cell is arranged in the light path system box of fluorescence detector, the detection light path of fluorescence detector is parallel with described optical detecting channel through described optical detecting channel (5-3), characterized by further comprising the first solenoid valve (9), the time relay (10) and support (11), described first solenoid valve (9) is three-way solenoid valve,
The light path system box (6-1) of fluorescence detector is by the support slant setting of support (11), and the entrance location of the feed pathway (5-1) of optical flow cell is lower than the exit position of liquid outlet channel (5-2); the part liquid outlet of low-lift pump (1) is communicated with through the entrance of six-way injection valve (2) with the first mixer (3) by pipe fitting, the part liquid outlet of low-lift pump (1) is directly communicated with the entrance of the first mixer (3) by pipe fitting, the outlet of the first mixer (3) is communicated with by the entrance of pipe fitting with reactor (4), the outlet of reactor (4) is by an inlet communication of pipe fitting and the first solenoid valve (9), another import of first solenoid valve (9) communicates with air, the outlet of the first solenoid valve (9) is communicated with the feed pathway (5-1) of optical flow cell by pipe fitting, the liquid outlet channel (5-2) of optical flow cell is communicated with waste fluid container (8) by pipe fitting, the light signal collection disposal system of fluorescence detector (6) is connected with computer processing system (7), the time relay (10) is connected with the first solenoid valve (9), control the first solenoid valve (9) to input air in optical flow cell (5) or reactant liquor, described first solenoid valve (9) is arranged on the top of optical flow cell.
2. there is the Flow Injection Analysis device of degassing function according to claim 1, it is characterized in that this device also comprises the second mixer (12) and the second solenoid valve (13), described second solenoid valve is two three-way electromagnetic valves, the outlet of reactor (4) is communicated with by the entrance of pipe fitting with the second mixer, the outlet of the second mixer by pipe fitting respectively with an import of the first solenoid valve (9), the inlet communication of the second solenoid valve, the outlet of the second solenoid valve is communicated with waste fluid container (8) by pipe fitting, the described time relay (10) is connected with the first solenoid valve and the second solenoid valve respectively, control the second solenoid valve and reactant liquor is inputted waste fluid container, control the first solenoid valve to input air in optical flow cell, or control the first solenoid valve input reactant liquor in optical flow cell (5), control the second closed electromagnetic valve import, block the path that reactant liquor enters the second solenoid valve.
3. there is the Flow Injection Analysis device of degassing function according to claim 1, it is characterized in that this device also comprises the 3rd solenoid valve (14), described 3rd solenoid valve is three-way solenoid valve, the outlet of reactor (4) is by the inlet communication of pipe fitting and the 3rd solenoid valve, one of 3rd solenoid valve exports an inlet communication by pipe fitting and the first solenoid valve, another outlet of 3rd solenoid valve is communicated with waste fluid container (8) by pipe fitting, the described time relay (10) is connected with the first solenoid valve and the 3rd solenoid valve respectively, control the 3rd solenoid valve and reactant liquor is inputted waste fluid container, control the first solenoid valve to input air in optical flow cell, or control the 3rd solenoid valve and the first solenoid valve input reactant liquor in optical flow cell (5), control the port closing that the 3rd solenoid valve communicates with waste fluid container, block reactant liquor enters waste fluid container (8) path from the 3rd solenoid valve.
4. there is the Flow Injection Analysis device of degassing function according to claim arbitrary in claims 1 to 3, it is characterized in that the angle of inclination of the light path system box (6-1) of described fluorescence detector should make the optical detecting channel (5-3) of the optical flow cell be arranged in light path system box and the angle (α) of surface level be 25 ~ 45 °.
5. there is the Flow Injection Analysis device of degassing function according to claim arbitrary in claims 1 to 3, characterized by further comprising de-soak device (15), described de-soak device (15) is closed container, one end of this closed container is provided with the gas outlet (15-3) of feed tube (15-1) and with closure (15-2), and the other end is provided with drain pipe (15-4);
Described de-soak device (15) is at least 1, when de-soak device (15) is 1, is arranged on a branch line of the liquid outlet of connection low-lift pump (1) and the inlet of six-way injection valve (2); When de-soak device (15) is for two or more, be arranged on respectively connect low-lift pump (1) liquid outlet from the different branch lines of the inlet of six-way injection valve (2), or be arranged on respectively connect low-lift pump (1) liquid outlet from the different branch lines of the inlet of six-way injection valve (2) with connect on the liquid outlet of low-lift pump (1) and the different branch lines of the first mixer; De-soak device (15) should make the feed tube of de-soak device (15-1) be positioned at the top of drain pipe (15-4) when installing.
6. there is the Flow Injection Analysis device of degassing function according to claim arbitrary in claims 1 to 3, it is characterized in that the entrance location at least 20cm of the installation site of described first solenoid valve higher than the feed pathway of optical flow cell.
7. there is the Flow Injection Analysis device of degassing function according to claim arbitrary in claims 1 to 3, it is characterized in that the described time relay (10) is the time relay of energy timing automatic power-off and energising.
8. a method for exhausting during Flow Injection Analysis, it is characterized in that using device described in claim 1, operate as follows: the time relay (10) is set to manually opened energising, the pattern of power-off after energising 20 ~ 60s, in Flow Injection Analysis process, the time relay is not energized, when finding enter bubble in optical flow cell (5) and cannot get rid of, close low-lift pump (1) and stop sample introduction, the power supply of the manually opened time relay, make the first solenoid valve (9) to input air in optical flow cell, auto-breaking after time relay energising 20 ~ 60s, open low-lift pump sample introduction, in optical flow cell, input the air that reactant liquor discharges in optical flow cell completely namely complete bleeding, proceed Flow Injection Analysis again.
9. method for exhausting during Flow Injection Analysis, is characterized in that using device described in claim 2, operates as follows:
The time relay (10) is set to manually opened energising, the pattern of power-off after energising 20 ~ 60s, in Flow Injection Analysis process, the time relay is not energized, when finding enter bubble in optical flow cell (5) and cannot get rid of, the power supply of the manually opened time relay, control the second solenoid valve (13) and reactant liquor is inputted waste fluid container (8), first solenoid valve (9) is to input air in optical flow cell, auto-breaking after time relay energising 20 ~ 60s, control the second closed electromagnetic valve import, first solenoid valve inputs reactant liquor in optical flow cell, after air in optical flow cell is got rid of by question response liquid completely, namely bleeding is completed, proceed Flow Injection Analysis again,
Or be energized after the time relay (10) is set to time delay 10 ~ 90min, the circulation pattern of power-off after energising 20 ~ 60s, after Flow Injection Analysis 10 ~ 90min, the time relay is energized automatically, control the second solenoid valve (13) and reactant liquor is inputted waste fluid container (8), first solenoid valve (9) is to input air in optical flow cell (5), auto-breaking after time relay energising 20 ~ 60s, control the second closed electromagnetic valve import, first solenoid valve inputs reactant liquor in optical flow cell, after air in optical flow cell is got rid of by question response liquid completely, namely a bleeding is completed, after this Flow Injection Analysis and bleeding is proceeded according to aforementioned manner.
10. method for exhausting during Flow Injection Analysis, is characterized in that using device described in claim 3, operates as follows:
The time relay is set to manually opened energising, the pattern of power-off after energising 20 ~ 60s, in Flow Injection Analysis process, the time relay is not energized, when finding enter bubble in optical flow cell and cannot get rid of, the power supply of the manually opened time relay, control the 3rd solenoid valve (14) and reactant liquor is inputted waste fluid container (8), first solenoid valve (9) is to input air in optical flow cell (5), auto-breaking after time relay energising 20 ~ 60s, control the port closing that the 3rd solenoid valve communicates with waste fluid container, 3rd solenoid valve and the first solenoid valve input reactant liquor in optical flow cell, after air in optical flow cell is got rid of by question response liquid completely, namely bleeding is completed, proceed Flow Injection Analysis again,
Or be energized after the time relay being set to time delay 10 ~ 90min, the circulation pattern of power-off after energising 20 ~ 60s, after Flow Injection Analysis 10 ~ 90min, the time relay is energized automatically, control the 3rd solenoid valve (14) and reactant liquor is inputted waste fluid container (8), first solenoid valve (9) is to input air in optical flow cell (5), auto-breaking after time relay energising 20 ~ 60s, control the port closing that the 3rd solenoid valve communicates with waste fluid container, 3rd solenoid valve and the first solenoid valve input reactant liquor in optical flow cell, after air in optical flow cell is got rid of by question response liquid completely, namely row's time operation is completed once, namely a bleeding is completed, after this Flow Injection Analysis and bleeding is proceeded according to aforementioned manner.
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