CN109991182A - A kind of total phosphorus detection system and total phosphorus detection method - Google Patents
A kind of total phosphorus detection system and total phosphorus detection method Download PDFInfo
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- CN109991182A CN109991182A CN201910355789.5A CN201910355789A CN109991182A CN 109991182 A CN109991182 A CN 109991182A CN 201910355789 A CN201910355789 A CN 201910355789A CN 109991182 A CN109991182 A CN 109991182A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4044—Concentrating samples by chemical techniques; Digestion; Chemical decomposition
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
Abstract
The present invention provides a kind of total phosphorus detection system, includes at least: preprocessing module, for reducing the particulate matter in fluid to be measured；Module is cleared up in photocatalysis, is connected to the preprocessing module, is cleared up based on light-catalyzed reaction, for converting Phos for organic phosphorus in fluid to be measured；Microfluid detection module, it is connected to photocatalysis resolution module, it successively include the Microfluidic Mixing component and microfluid detection components of connection, the Microfluidic Mixing component is used to fluid to be measured mixing colour developing with medicament with detection, and the microfluid detection components are used to detect the absorbance of the fluid to be measured after colour developing.Total phosphorus detection system volume of the invention is very small, and reaction rate is fast, and effect is good.Total phosphorus detection method is simple and efficient, and will not be resulted in blockage, and accuracy is high, may be reused, small in size, at low cost, high degree of automation, is prevented the wasting of resources, save the cost, and environmental protection, is not needed high-temperature high-pressure apparatus.
Description
Technical field
The present invention relates to field of fluid treatment, are based on total phosphorus detection system and total phosphorus detection method more particularly to one kind.
Background technique
Total phosphorus is the phosphoric acid that element phosphor, pyrophosphate, orthophosphates, condensed phosphate, metaphosphate and organic group combine
The general name of salt etc., the main pollution source of total phosphorus are sanitary sewage, chemical fertilizer, phosphoric acid used in organophosphorus pesticide and modern age detergent
Salt buider etc..Moreover, phosphorus is a kind of key element necessary to the growth of algae in water, but excessive phosphorus content can make water again
Body causes filthy Shenzhen smelly, so that water eutrophication, or even there is red tide.During phosphorous chemical industry develops, byproduct
But also a large amount of pollution is brought, such as the three wastes (dust, waste water, solid waste), these substances enter in environment, can make to environment
At great injury.Such as exhaust gas and dust, carbon monoxide, carbon dioxide, hydrogen fluoride, hydrogen phosphide, hydrogen sulfide etc. are mainly contained；It is useless
Contain the poisonous and harmful substances such as phosphorus, fluorine, sulphur, chlorine, arsenic, alkali, uranium in water；Contain mill tailings, barren rock in solid waste, yellow phosphorus is raw
Produce phosphorus slag, the muck, fine ore, phosphorus mud, ferrophosphorus of discharge, the ardealite generated in Wet-process Phosphoric Acid Production is discharged in gas washing in SA production
Pyrite slag, calcium magnesium phosphate blast furnace lime-ash etc..Removing the method for total phosphorus in water at present mainly has: chemical precipitation method, bioanalysis, from
Sub- exchange process, absorption method, membrane separating method etc., these methods play the role of different key in different field.
Before the water body processing polluted to phosphorus, it is thus necessary to determine that the content of total phosphorus in water can just be made best in this way
Resolution.
Summary of the invention
In view of the foregoing deficiencies of prior art, the purpose of the present invention is to provide a kind of total phosphorus detection system and total phosphorus
Detection method.
In order to achieve the above objects and other related objects, first aspect present invention provides a kind of total phosphorus detection system, described
Total phosphorus detection system includes at least:
Preprocessing module, for reducing the particulate matter in fluid to be measured；
Module is cleared up in photocatalysis, is connected to the preprocessing module, is cleared up based on light-catalyzed reaction, and being used for will be to be measured
Organic phosphorus in fluid is converted into Phos；
Microfluid detection module and the photocatalysis resolution module be connected tos, successively include connection Microfluidic Mixing component with
Microfluid detection components, the Microfluidic Mixing component are used to fluid to be measured mixing colour developing, the miniflow with medicament with detection
Body detection components are used to detect the absorbance of the fluid to be measured after colour developing.
Second aspect of the present invention provides the method for carrying out total phosphorus detection using aforementioned total phosphorus detection system, the method includes
Following steps:
(1) fluid to be measured is pre-processed using preprocessing module, reduces the particulate matter in fluid to be measured；
(2) photocatalysis resolution is carried out using photocatalysis resolution module to pretreated fluid to be measured, it will be in fluid to be measured
Organic phosphorus be converted into Phos；
(3) fluid to be measured after resolution is mixed with the Microfluidic Mixing component detection of microfluid detection module with medicament aobvious
Color, the absorbance of the fluid to be measured after the microfluid detection components detection colour developing of microfluid detection module, calculates according to absorbance
Obtain the total phosphorus concentration in fluid to be measured.
As described above, total phosphorus detection system and total phosphorus detection method of the invention, have the advantages that
Total phosphorus detection system volume of the invention is very small, and reaction rate is fast, and effect is good.Total phosphorus detection method is simply high
Effect, will not result in blockage, and accuracy is high, may be reused, small in size, at low cost, high degree of automation, prevent resource unrestrained
Take, save the cost, and environmental protection, does not need high-temperature high-pressure apparatus.
Detailed description of the invention
Fig. 1 is shown as total phosphorus detection system planar structure schematic diagram of the invention.
Fig. 1 .1 is shown as total phosphorus detection system (with electrolyte mixing module) planar structure schematic diagram of the invention
Fig. 2 is shown as the preprocessing module planar structure schematic diagram of total phosphorus detection system of the invention.
Fig. 3 is shown as the preprocessing module schematic perspective view of total phosphorus detection system of the invention.
Fig. 4 is shown as the explosive view of the photocatalysis resolution module of total phosphorus detection system of the invention.
Fig. 5 is shown as the reaction tank without cathode and anode of the photocatalysis resolution module of total phosphorus detection system of the invention
Schematic diagram.
Fig. 6 is shown as the reaction tank containing cathode and anode of the photocatalysis resolution module of total phosphorus detection system of the invention
Schematic diagram.
Fig. 7 is shown as the photocatalysis resolution module assembly completion figure of total phosphorus detection system of the invention.
Fig. 8 is shown as the microfluid detection module structural schematic diagram of total phosphorus detection system of the invention.
The microfluid detection module that Fig. 9 is shown as total phosphorus detection system of the invention overlooks figure structure schematic representation.
Figure 10 is shown as the cross section view (side B-B of the microfluid detection module top view of total phosphorus detection system of the invention
To).
Figure 11 is shown as the perspective view of the electrolyte mixing module of total phosphorus detection system of the invention.
Figure 12 is shown as the explosive view depression angle view of the electrolyte mixing module of total phosphorus detection system of the invention.
The explosive view that Figure 13 is shown as the electrolyte mixing module of total phosphorus detection system of the invention looks up angular views.
Figure 14 is shown as the perspective view of the top view of the electrolyte mixing module of total phosphorus detection system of the invention.
Figure 15 is shown as the cross-sectional view (section A-A) of the electrolyte mixing module of total phosphorus detection system of the invention.
Figure 16 is shown as preprocessing module in present example and is discharged turbid figure, wherein blue indicates the water outlet of the 4th outlet
(inner ring turbidity), green indicate the water outlet (outer ring turbidity) of third outlet.
Figure 17 is shown as the water outlet granularity graph that preprocessing module the 4th exports in present example.
Figure 18 is shown as the water outlet granularity graph that preprocessing module third exports in present example.
Figure 19 is shown as 0.45 micron membrane filter of preprocessing module in present example and filters effect picture.
Figure 20 is shown as heating the influence to light-catalyzed reaction, wherein effect of the red for heating, the effect that blue does not heat
Fruit.
Component label instructions
1 preprocessing module
1.1 pretreatment imports
1.2 first arc split tunnels
1.2.1 first outlet
1.2.2 second outlet
1.3 Power Component
1.3.1 the first transfer tube
1.3.2 the second transfer tube
1.4 second arc split tunnels
1.4.1 the second liquid inlet
1.4.2 third exports
1.4.3 the 4th outlet
1.5 primary filter components
1.6 clear water tanks
1.7 waste water tank
1.8 suction pump
Module is cleared up in 2 photocatalysis
Import is cleared up in 2.1 photocatalysis
2.2 reaction tank is cleared up in photocatalysis
2.2.1 anode
2.2.2 cathode
2.3 ultraviolet lamp
2.4 photocatalysis resolution outlet
2.5 transparent glass
2.6 ultraviolet lampshades
2.7 cathode can
2.8 electrode hole
3 microfluid detection modules
3.1 Microfluidic Mixing components
3.1.1 microfluid injection port
3.1.2 microfluid medicament mouth
3.1.3 Microfluidic Mixing chamber
3.1.3.1 venthole
3.1.4 vibrator
3.2 microfluid detection components
3.2.1 microfluid test chamber
3.2.2 optical element
3.3 flow control components
3.4 microfluid liquid outlets
4 electrolyte mixing modules
4.1 hybrid agent
4.2 electrolyte mixing inlets
4.3 electrolyte mixing liquid outlets
4.4 mixed cell
Specific embodiment
Embodiments of the present invention are illustrated by particular specific embodiment below, those skilled in the art can be by this explanation
Content disclosed by book is understood other advantages and efficacy of the present invention easily.
Fig. 1 is please referred to Figure 20.It should be clear that this specification structure depicted in this specification institute accompanying drawings, ratio, size etc., are only used
To cooperate the revealed content of specification, so that those skilled in the art understands and reads, being not intended to limit the invention can
The qualifications of implementation, therefore do not have technical essential meaning, the tune of the modification of any structure, the change of proportionate relationship or size
It is whole, in the case where not influencing the effect of present invention can be generated and the purpose that can reach, it should all still fall in disclosed skill
Art content obtains in the range of capable of covering.Meanwhile in this specification it is cited as "upper", "lower", "left", "right", " centre " and
The term of " one " etc. is merely convenient to being illustrated for narration, rather than to limit the scope of the invention, relativeness
It is altered or modified, under the content of no substantial changes in technology, when being also considered as the enforceable scope of the present invention.
As shown in Figure 1, being total phosphorus detection system provided by the invention, the total phosphorus detection system is included at least:
Preprocessing module 1, for reducing the particulate matter in fluid to be measured；
Module 2 is cleared up in photocatalysis, be connected to the preprocessing module, is cleared up based on light-catalyzed reaction, and being used for will be to
Organic phosphorus in fluid measured is converted into Phos；
Microfluid detection module 3 is connected to photocatalysis resolution module, successively includes the Microfluidic Mixing component of connection
3.1 and microfluid detection components 3.2, the Microfluidic Mixing component is used to fluid to be measured mixing colour developing with medicament with detection,
The microfluid detection components are used to detect the absorbance of the fluid to be measured after colour developing.
Further, as shown in Figures 2 and 3, the preprocessing module 1 includes:
Import 1.1 is pre-processed, for receiving fluid to be measured；
First arc split tunnel 1.2, including the first liquid inlet and the first liquid outlet, first liquid inlet are set to described
It one end of first arc split tunnel 1.2 and is connected to the pretreatment import 1.1, first liquid outlet is set to described first
The other end of arc split tunnel 1.2, including first outlet 1.2.1 and second outlet 1.2.2, wherein first outlet 1.2.1 phase
The arc center of circle remoter than second outlet 1.2.2；
Power Component 1.3, including the first transfer tube 1.3.1 and the second transfer tube 1.3.2, the first transfer tube 1.3.1
Fluid from the first outlet 1.2.1 is respectively driven with the second transfer tube 1.3.2 and from the second outlet 1.2.2's
Fluid flowing.
The maximum particle diameter for the particulate matter for including in the first outlet water outlet, which is greater than in second outlet water outlet, includes
The maximum particle diameter of particulate matter.
Further, in the Power Component, including controller, for controlling the first transfer tube and the second driving respectively
Pump.
The controller can be single-chip microcontroller, and single-chip microcontroller can be 8 minimum systems.The controller can also select
With the controller or processor of different brand and model, or more seniority top digit.Controller can be used for installing associated control procedures.
After installing associated control procedures, controller can control the pump speed of the first transfer tube and second transfer tube as needed.
Further, the first transfer tube 1.3.1 is different from the pump speed of the second transfer tube 1.3.2.
In one embodiment, the pump speed of the first transfer tube 1.3.1 is greater than the pump of the second transfer tube 1.3.2
Speed.
In one embodiment, the first pump speed for stating transfer tube 1.3.1 be 70-150mL/min, and/or, described the
The pump speed of two transfer tube 1.3.2 is 60-130mL/min.
In one embodiment, the preprocessing module further include: the second arc split tunnel 1.4, including second enter
Liquid mouth 1.4.1 and the second liquid outlet, the second liquid inlet 1.4.1 be set to the second arc split tunnel 1.4 one end and
It is connected to the second outlet 1.2.2, second liquid outlet is set to the other end of the second arc split tunnel 1.4, packet
Include third outlet 1.4.2 and the 4th outlet 1.4.3, wherein third exports the arc center of circle remote compared to the 4th outlet 1.4.3 1.4.2.
The second arc split tunnel is for further separating the particulate matter in fluid.
In one embodiment, the preprocessing module further includes primary filter component 1.5, is set to pretreatment import
1.1 and first between arc split tunnel 1.2, for filtering the large particle in fluid to be measured.
In one embodiment, the primary filter component 1.5 includes filter, the aperture of the strainer of the filter
No more than 120 mesh.It results in blockage for preventing excessive particulate matter from entering hollow cylinder split tunnel.
In one embodiment, the fluid system further includes clear water tanks 1.6, for storing the stream of the 4th outlet discharge
Body.
In one embodiment, the fluid system further includes waste water tank 1.7, is gone out for collecting first outlet and third
The fluid of mouth discharge.
In one embodiment, the central angle of the first arc split tunnel is 179 ° -181 °.Optionally, it is
179°,180°,181°.Guarantee that particulate matter there are enough road radially outer bands to spread, while excessive volume will not be occupied.
In one embodiment, the central angle of the second arc split tunnel is 179 ° -181 °.Optionally, it is
179°,180°,181°.Guarantee the standby sufficient distance of the second arc separator, so that purified through the first arc separator
Liquid can continue to be separated again by the second arc split tunnel.
In one embodiment, the cavity of the first arc split tunnel 1.2 is the cuboid of embowment, described
The cavity high 0.4-2mm, wide 5-15mm of first arc split tunnel 3.The cavity of the second arc split tunnel 1.4 is to curve
The cuboid of arc, the maximum inner diameter of the second arc split tunnel 9 are high 0.4-2mm, wide 5-15mm.Guarantee that particulate matter can
To move along wide direction outer ring, simultaneously as depth-width ratio is low, unordered disturbance will not be generated in portion in the cavity.
In one embodiment, as shown in Fig. 2, the pretreatment import 1.1 is driven by suction pump 1.8.
Further, as shown in figure 4, photocatalysis resolution module includes:
Import 2.1 is cleared up in photocatalysis, is connected to the preprocessing module 1, for receiving from the to be measured of preprocessing module 1
Fluid；
Reaction tank 2.2 is cleared up in photocatalysis, is connected to photocatalysis resolution import 2.1, for carrying out light-catalyzed reaction；Institute
It states and is equipped with anode 2.2.1 and cathode 2.2.2 in photocatalysis resolution reaction tank, the anode is laid in photocatalysis resolution reaction tank bottom
Portion, the cathode 2.2.2 are set to the side wall of photocatalysis resolution reaction tank and do not contact directly with the anode 2.2.1；
Ultraviolet lamp 2.3 provides light source for clearing up reaction tank 2.2 for the photocatalysis；
Photocatalysis resolution outlet 2.4 is connected to photocatalysis resolution reaction tank 2.2, to be measured after reacting for being discharged
Fluid.
Import 2.1 is cleared up in the photocatalysis, is connected to the clear water tanks 1.6 of the preprocessing module.
In one embodiment, the anode 2.2.1 is flake.It optionally, is thin slice cuboid.
As shown in figure 5, the side wall of the photocatalysis resolution reaction tank is equipped with cathode can 2.7, it to be used for fixed negative pole.
The cathode can reacts bottom of pond portion equipped with certain distance with photocatalysis resolution, prevents the cathode and anode straight
Contact.
In one embodiment, the cathode 2.2.2 circular side wall free of discontinuities, it is preferred that the cathode 2.2.2 is at least
Around the half of perimeter side wall.
In one embodiment, photocatalysis resolution reaction tank inner cavity is right prism.
In one embodiment, as shown in Figure 5 and Figure 6, the photocatalysis resolution reaction tank side wall is equipped with electrode hole
2.8, for cathode and anode to be drawn out to respectively outside the photocatalysis resolution reaction tank, for connecting power supply.In anode and
Apply a voltage between cathode so as to prevent the compound of electrons and holes pair, so that endlessly generation-OH is free
Base increases the efficiency of photoelectrocatalysis.
In one embodiment, supply voltage is in 0.5-1V.
In one embodiment, the volume of the photocatalysis resolution reaction tank 2.2 is 25-1500 microlitres.
The reaction tank 2 is the reaction tank with certain length.
In one embodiment, the maximum length of photocatalysis resolution reaction tank inner cavity is 10mm-50mm.
In one embodiment, the maximum width of photocatalysis resolution reaction tank inner cavity is 5mm-10mm.
In one embodiment, the maximum height of photocatalysis resolution reaction tank inner cavity is 0.5mm-3mm.
In one embodiment, the anode 2.2.1 is titanium dioxide electrodes.
In one embodiment, the cathode 2.2.2 is Ti electrode.
In one embodiment, as shown in fig. 7, being equipped with ultraviolet lampshade 2.6 above the ultraviolet lamp 2.3.
In one embodiment, the photocatalysis resolution module further includes photocatalysis resolution heating component, for institute
Photocatalysis resolution reaction tank is stated to be heated.
Further, the heating component includes heating plate, is set in the reaction tank.
In one embodiment, the heating component controls reaction tank temperature in 60 ± 15 DEG C of section.To mention
High reaction efficiency.
Further, photocatalysis resolution reaction tank side is equipped with light-transmitting opening, and the ultraviolet lamp is set to the light-transmitting opening
Top, transparent glass 2.5 is equipped at the light-transmitting opening.Guarantee that ultraviolet light can be taken in, while preventing the liquid in reaction tank
Ultraviolet lamp is polluted.
In one embodiment, the length of the ultraviolet lamp 2.3 is greater than the half of the light-transmitting opening length.Guarantee
Ultraviolet lamp has certain length, guarantees that the entire surface of anode is all illuminated.Preferably, the length of the ultraviolet lamp and described
Optical port equal length.
In one embodiment, the width of the ultraviolet lamp 2.3 is no more than the width of photocatalysis resolution reaction tank.
Reduce the volume of whole device, and reduces the waste of resource.
In one embodiment, the ultraviolet lamp 2.3 is bonded the transparent glass 2.5 and is arranged.Shine ultraviolet light directly
It is mapped to inside photocatalysis resolution reaction tank, reduces light path.
The photocatalysis resolution import 2.1 and photocatalysis resolution outlet 2.4 are set to photocatalysis resolution reaction tank
Bottom.Water body can be discharged by not needing external force.
Further, as Figure 8-Figure 10, the Microfluidic Mixing component 3.1 includes:
Microfluid injection port 3.1.1 is connected to photocatalysis resolution module, clears up module from photocatalysis for receiving
Fluid to be measured；
Microfluid medicament mouth 3.1.2, for receiving the medicament that can be reacted with fluid to be measured；
Microfluidic Mixing chamber 3.1.3 distinguishes with the microfluid injection port 3.1.1 and microfluid medicament mouth 3.1.2
Connection makes liquid stream sample to be measured react with medicament for mixing fluid to be measured and medicament, as shown in Figure 10, the miniflow
The body side mixing chamber 3.1.3 is equipped with venthole 3.1.3.1.
The microfluid injection port 3.1.1 is connected to the photocatalysis resolution outlet 2.4 of photocatalysis resolution module.
As shown in Figure 10, the microfluid detection components 3.2 include:
Microfluid test chamber 3.2.1 is connected to the Microfluidic Mixing chamber 3.1.3, for detecting the prepare liquid after reacting
Flow sample；
Optical element 3.2.2, for providing light source to the microfluid test chamber 3.2.1.Carry out absorbance detection.
The medicament mouth can set multiple.Such as 2.
When medicament and liquid stream sample to be measured mix, bubble can be generated, the venthole can make bubble escape into atmosphere
In, prevent influence of the bubble to subsequent detection.The venthole that setting connects atmosphere simultaneously is injecting a sample into Microfluidic Mixing chamber
When can generate resistance to avoid system, if being not provided with venthole, sample is by can not be into due to the air drag in cavity
Enter mixing chamber；During evacuation of liquid, due to the presence of stomata, liquid can be discharged rapidly, if being not provided with stomata,
Due to the effect of air pressure, liquid will be unable to be discharged.
In one embodiment, the diameter of the microfluid injection port 3.1.1 is 0.5-2mm.
In one embodiment, the diameter of the microfluid medicament mouth 3.1.2 is 0.5-2mm.
In one embodiment, the sectional area of the Microfluidic Mixing chamber 3.1.3 is 10-20mm2。
The sectional area of the mixing chamber refers to, the microfluid injection port to the section of the Microfluidic Mixing cavity direction a.
In one embodiment, the volume of the microfluid test chamber 3.2.1 is 50-100mm3。
In one embodiment, the venthole 3.1.3.1 be located at the Microfluidic Mixing chamber 3.1.3 side wall and/
Or top.
In one embodiment, the venthole 3.1.3.1 can be set to the side wall of the Microfluidic Mixing chamber 3.1.3.
The height of the venthole is the 30%-90% of the Microfluidic Mixing chamber 3.1.3 height.The venthole is in higher position
It sets, can prevent liquid from overflowing.
In one embodiment, the diameter of the venthole 3.1.3.1 is 1-5mm.
In one embodiment, the Microfluidic Mixing chamber is hollow cylinder.
In one embodiment, it is additionally provided with outside the microfluid injection port 3.1.1 and microfluid medicament mouth 3.1.2
Conduit fixation kit, for fixed to injection port or the conduit of medicament mouth feed liquor.In one embodiment, the conduit is fixed
Component is equipped with spiral lamination, for fixing.
In one embodiment, vibrator 3.1.4 is equipped with below the Microfluidic Mixing chamber 3.1.3.For mixing
Shi Jinhang vibration generates many small turbulent flows in a liquid, accelerates the mixing of liquid, while preventing the precipitating generated in reaction
Object prevents choke system in mixing chamber encrustation, keeps whole device reusable, substantially reduces cost.
In one embodiment, the vibrator 5 is selected from flat vibrator.For example, the enlightening science and technology that can shine for Shenzhen has
Limit company YDF1027L lead type flat mini vibrating motor；Or the female roc in Shenzhen reaches electromechanical Co., Ltd, KPD-FLAT-
0827。
In one embodiment, the vibration frequency of vibrator is 10000-15000 beats/min.
Further, the microfluid test chamber 3.2.1 light-permeable.
In one embodiment, the optical element 3.2.2 is located above the microfluid test chamber 3.2.1.
Further, the microfluidic test device further includes microfluid liquid outlet 3.4, is connected with the microfluid test chamber
Liquid that is logical, being finished for detection to be discharged.
In one embodiment, the microfluid detection module further includes flow control component 3.3, for driving liquid stream to be measured
Sample flows in microfluidic test device and/or controls the flow of fluid to be measured.
In one embodiment, the flow control component includes transfer tube and valve, for controlling microfluid sample introduction respectively
The fluid flow of mouth, microfluid liquid outlet and microfluid medicament mouth.
The flow control component further includes peristaltic pump, for liquid stream sample to be detected to be injected into microfluid test chamber.
In one embodiment, the transfer tube is piezoelectric pump.
In one embodiment, the valve is marmem micro-valve (SMA valve).Can by change temperature come
The deformation of the intracorporal memorial alloy of control valve, carrys out the opening and closing of control valve).
In one embodiment, the microfluidic module main body is made of PMMA material.Microfluidic module main body packet
Microfluid injection port, microfluid medicament mouth, Microfluidic Mixing chamber and microfluid test chamber are included, without including photoelectricity device assembly,
Such as flow control component, vibrator and optical element.
In one embodiment, the microfluidic test device is integrally formed.Microfluidic module main body includes microfluid
Injection port, microfluid medicament mouth, Microfluidic Mixing chamber and microfluid test chamber, without including photoelectricity device assembly, such as flow control group
Part, vibrator and optical element etc..
In one embodiment, as shown in Fig. 1 .1, the total phosphorus detection system further includes electrolyte mixing module 4, if
Between the preprocessing module 1 and photocatalysis resolution module 2, for carry out the addition of photocatalysis resolution electrolyte with
Mixing.
As shown in Figure 11 to Figure 13, the electrolyte mixing module includes: hollow hybrid agent 4.1, in the mixing
On the length direction of main body, it is equipped with electrolyte mixing inlet 4.2 and electrolyte mixing liquid outlet 4.3, the electrolyte mixing
Liquid outlet 4.3 is connected to photocatalysis resolution module 2, blends liquid in the electrolyte mixing inlet 4.2 to electrolyte
It between mouth 4.3, is sequentially communicated in the mixer main body and is provided with multiple mixed cells 4.4, the mixed cell 4.4 is hollow
Prism.
The electrolyte mixing inlet 4.2 is connected to the clear water tanks 1.6 of preprocessing module.
Inlet communication is cleared up in the photocatalysis of the electrolyte mixing liquid outlet and photocatalysis resolution module.
Further, the prism is right prism.
The electrolyte mixing inlet is used for feed liquor.
The electrolyte mixing liquid outlet is for being discharged mixed liquid.
The mixed cell is mixed for liquid.
The electrolyte mixing inlet is connected to the electrolyte mixing liquid outlet by the mixed cell.
The mixed cell series connection.
In one embodiment, the mixed cell 4.4 is in hollow quadrangular, hexagonal prisms or eight prisms
It is any one or more.For enhancing the turbulent flow of fluid, accelerate the radial mixing of fluid.
It preferably, is that hollow square prism, regular hexagonal prism or positive eight prism are any one or more of.
In one embodiment, adjacent mixed cell is connected to by communication port, and each communication port is located along the same line.
Advantageously reduce the loss of liquid kinetic energy.Guarantee that water resistance is minimum, liquid feeding pump is required lower.
In one embodiment, adjacent communication port is set on the opposite rib of mixed cell.Preferably, the communication port
Sectional area be S2 be 0.01-0.36mm2.For the turbulent flow of high current body, accelerate the radial mixing of fluid.
As shown in figure 15, the sectional area S2 of the communication port refers to, flat with the place length direction c of the mixer main body
On the vertical direction AA in face, the area S2 of the communication port.
As shown in figure 14, in one embodiment, the bottom surface of the mixed cell is zhou duicheng tuxing, and symmetry axis is
The line b of the intersection point of the bottom surface of rib and the mixed cell in the mixed cell equipped with communication port.
As shown in figure 15, in one embodiment, the height of the hollow cavity of each mixed cell 4.4 is equal, it is preferred that institute
The height h for stating hollow cavity is 0.1-0.6mm.Be conducive to liquid quickly to mix, while saving sample overall volume.
Preferably, in the same plane, each bottom surface is in the same plane for each upper bottom surface of the mixed cell.
In one embodiment, the floor space of the mixed cell 4.4 is 20-40mm2.It optionally, is 31mm2.Favorably
Whirlpool is quickly formed in the liquid being injected into cavity, enhances mixed effect.
In one embodiment, the base area of each mixed cell 4.4 is identical；
In one embodiment, each 4.4 shape of mixed cell and volume are consistent.Be conducive to keep entire runner water resistance
Consistency facilitates processing, while extending device service life.
In one embodiment, the quantity of the electrolyte mixing inlet 4.2 is 2 or more.Be optionally, 2,
3 or 4 or more.The amount of fluid that can be mixed as needed carries out flexible choice.
In one embodiment, the quantity of the electrolyte mixing liquid outlet 4.3 is 1.For guaranteeing mixed cell
Outlet it is unique, guarantee the flowing velocity in mixing chamber of fluid.
In one embodiment, the quantity of the mixed cell 4.4 is 2-8.It further, can be 2-6.Have
Mixed processing is carried out conducive to the liquid for different volumes.
In one embodiment, the electrolyte mixing inlet 4.2 and the electrolyte mixing liquid outlet 4.3 are in institute
State the side of hollow mixer main body.For reducing product entire length.
The total phosphorus detection system further includes master controller, and the master controller can be single-chip microcontroller, and single-chip microcontroller can be
One 8 minimum system.The master controller can also select different brand and model, or more seniority top digit controller or
Processor.Master controller can be used for installing associated control procedures.After installing associated control procedures, master controller can be controlled as needed
The operating of vibrator, transfer tube or valve in modules processed.
The present invention provides the method for carrying out total phosphorus detection using foregoing total phosphorus detection system, includes the following steps:
(1) fluid to be measured is pre-processed using preprocessing module, reduces the particulate matter in fluid to be measured；
(2) photocatalysis resolution is carried out using photocatalysis resolution module to pretreated fluid to be measured, it will be in fluid to be measured
Organic phosphorus be converted into Phos；
(3) fluid to be measured after resolution is mixed with the Microfluidic Mixing component detection of microfluid detection module with medicament aobvious
Color, the absorbance of the fluid to be measured after the microfluid detection components detection colour developing of microfluid detection module, calculates according to absorbance
Obtain the total phosphorus concentration in fluid to be measured.
In one embodiment, in step (1), the first transfer tube driving in preprocessing module is controlled from described the
The fluid of one outlet controls the second transfer tube in preprocessing module and drives the fluid flowing from second outlet.
Preferably, first transfer tube is different from the pump speed of second transfer tube.
Further, in the Power Component, including controller, for controlling the first transfer tube and the second driving respectively
Pump.
Further, first transfer tube is different from the pump speed of second transfer tube.
In one embodiment, the pump speed of first transfer tube is greater than the pump speed of second transfer tube.
In one embodiment, first state transfer tube pump speed be 70-150mL/min, and/or, it is described second drive
The pump speed of dynamic pump is 60-130mL/min.
In one embodiment, step (2) the following steps are included:
A. react: ultraviolet light irradiation applies voltage, carries out light-catalyzed reaction；
B. drain: the fluid after discharge reaction；
C. electrode regeneration: after reaction, flushing liquor is added, applies backward voltage, then by electric pole short circuit, make electrode again
It is raw；
D. flushing liquor is discharged.
In one embodiment, the light radiation intensity of ultraviolet lamp is 300-500 microwatt/square centimeter.
In one embodiment, supply voltage 0.5-1V.The electronics and hole-recombination that generation can be effectively prevented, mention
High photocatalysis efficiency, while preventing the generation of additional electrochemical reaction.
In one embodiment, the feed liquor is interval feed liquor.Guarantee that fluid sufficiently reacts.
In one embodiment, the hydraulic detention time of the light-catalyzed reaction is 10-40min.Guarantee that fluid is abundant
Reaction.
In one embodiment, in step c, the time for applying backward voltage is 10-30s, electric pole short circuit time
For 10-60s.
In one embodiment, in step c, the flushing liquor is selected from deionized water, sodium hydrate aqueous solution or ethyl alcohol
Aqueous solution.
In one embodiment, the mass concentration of the sodium hydrate aqueous solution is 1%-5%, the ethanol water
Mass concentration be 10%-50%.
In one embodiment, in step a, further include to it is described need to be added in fluid to be reacted the concentrated sulfuric acid and/or
Aqueous sodium persulfate solution.Reinforce electric conductivity and oxidisability.
The concentrated sulfuric acid refers to the aqueous sulfuric acid that mass fraction is greater than or equal to 70%.
In one embodiment, the concentrated sulfuric acid accounts for the 2%-10% of feed liquor volume, and/or, the aqueous sodium sulfate
Liquid accounts for the 5%-10% of feed liquor volume, and the sodium sulfate concentration is 10-200mg/mL.
When carrying out electrode regeneration, apply backward voltage, the electric double layer of cathode and anode surface is caused to deconstruct, the double electricity of cathode
In layer in remaining phosphate anion and anode electric double layer remaining cation can the quick desorption from electric double layer, into flushing
In liquid, then keeps anode and cathode short-circuit by circuit control, so that phosphate radical is continued desorption, and reach stable.At this moment electrode surface
The remaining phosphate anion overwhelming majority enters in flushing liquor, then flushing liquor is emptied, and reaches regenerated purpose.
Backward voltage refers to the voltage contrary with the supply voltage in step a.
In one embodiment, photocatalysis resolution reaction tank is heated when reaction.Heating and temperature control 60 ±
In 15 DEG C of section.Improve reaction efficiency.For example, leading to for phosphorus-containing matter in the experiment of the resolution efficiency in 20 minutes
About 10 percentage points can be improved for resolution efficiency by crossing heating, as a result as shown in figure 20.
In one embodiment, electrolyte is added before carrying out photocatalysis resolution.The electrolyte can be sodium sulphate.
In step (3) the following steps are included:
1) microfluid medicament mouth valve is opened simultaneously, medicament is quantified into injection Microfluidic Mixing chamber；
2) it opens vibrator to mix medicament, vibrator and microfluid medicament mouth valve is closed after mixing；
3) sample is quantified into injection Microfluidic Mixing chamber；
4) vibrator is opened, medicament is made to be sufficiently mixed and be reacted with sample；
5) medicament after reaction microfluid test chamber is injected into detect.
This device is controlled by pump valve to be passed through miniflow physical examination by resolution or the liquid containing phosphate radical without resolution
Device is surveyed, first addition medicament, carries out mixing and chromogenic reaction, tested in judgement sample by the absorbance to liquid after colour developing
The concentration of phosphate radical.Medicament addition is controlled by pump valve, is ammonium molybdate solution and ascorbic acid respectively.Ammonium molybdate solution can be with
Phosphate radical stroke complex compound in sample.Main reactional equation is as follows:
PO43-+12MoO4 2-+27H+→H3PO4(MoO3)12+12H2O (1)
H3PMo(VI)12O40+Reductant→[H4PMo(VI)8Mo(V)4O40]3- (2)
Such reaction is famous molybdenum blue reaction, and reaction includes two steps, and first step is as shown in formula one, phosphoric acid
Radical ion is reacted with molybdenum acid ion in acid condition generates heteropoly acid H3PO4(MoO3)12In second step, first step
The heteropoly acid formed in rapid is reduced into as blue product.The absorbance of this blue product can in sample phosphate radical it is dense
Degree generates a certain range of linear relationship.So as to by obtaining the concentration of phosphate radical to the measurement of absorbance.
In one embodiment, step (3) the following steps are included:
1) microfluid medicament mouth valve is opened simultaneously, then by piezoelectric pump by quantitative medicament (molybdate solution and anti-
Bad hematic acid) injection Microfluidic Mixing chamber.
2) the vibration motor for opening Microfluidic Mixing bottom of chamber portion mixes medicament, incorporation time 10-30s, then
Close vibrating motor.
3) valve of microfluid medicament mouth is closed.
4) it opens sample pump (solenoid pump) and quantitative sample is injected into Microfluidic Mixing chamber, be then shut off sample
Pump.
5) it is again turned on vibration motor, mixes 10-20s.
6) it waits ten minutes, allows medicament and sample that molybdenum blue chromogenic reaction occurs.
7) vibrator test chamber is pumped by the solution that the peristaltic pump in vibrator test chamber downstream completes mixing.
8) it opens light source and detector is detected, be collected into current signal.
9) evacuation of liquid can carry out the detection of next sample.
Example
A kind of 1.1 total phosphorus detection systems, the system comprises preprocessing module, the preprocessing module includes:
Import, for receiving fluid；
Primary filter component includes filter, the hole of the strainer of the filter for filtering the large particle in fluid
Diameter is 120 mesh；
First arc split tunnel, including the first liquid inlet and the first liquid outlet, first liquid inlet are set to described the
One end of one arc split tunnel and with the inlet communication, first liquid outlet is set to the first arc split tunnel
The other end, including first outlet and second outlet, wherein first outlet compares the remote arc center of circle of second outlet；
Power Component, including controller, the first transfer tube and the second transfer tube, first transfer tube and the second transfer tube
Respectively drive the fluid from the first outlet and the fluid flowing from the second outlet.Guarantee the water flow velocity in channel
Degree.Controller controls the pump speed of the first transfer tube and the second transfer tube respectively, and the pump speed of first transfer tube is 100mL/
Min, and, the pump speed of second transfer tube is 85mL/min.
Second arc split tunnel, including the second liquid inlet and the second liquid outlet, second liquid inlet are set to described the
It one end of two arc split tunnels and is connected to the second outlet, it is logical that second liquid outlet is set to second arc separation
The other end in road, including third outlet and the 4th outlet, wherein the third outlet arc center of circle remote compared to the 4th outlet.
The central angle of the first arc split tunnel is 180 °.
The central angle of the second arc split tunnel is 180 °.
Cavity high 1mm, the wide 15mm of the first arc split tunnel, the cavity of the second arc split tunnel are a height of
0.4mm, width 5mm.
1.2. water filtering is carried out using fluid system described in 1.1.
1.3. the delivery turbidity of the outlet of measurement third and the 4th outlet divides water outlet granularity using Particle Size Analyzer
Analysis.Believe that TN100 transmissometer, by specification are operated in Particle Size Analyzer model Shanghai three.
1.4. interpretation of result
As shown in figure 16, green is that third exports turbidity value, and blue is the 4th outlet turbidity value, in different total flow items
Under part, we can be found that 185mL/min can achieve optimal effectiveness, and third exports turbidity value maximum, the 4th outlet turbidity value
Minimum reaches best separating effect.
The water outlet grain size analysis of 4th outlet is as shown in figure 17, it is seen that most of particulate matters are located at 20 microns, third
Outlet water outlet grain size analysis is as shown in figure 18, and most of particulate matters are located at 1000 microns of section.It can achieve the effect of separation.
It is as shown in figure 19 that 0.45 micron membrane filter filters effect picture.Dark color is first outlet water outlet filtering figure, and light color is the 4th
Water outlet filtering figure in outlet indicates to add up after longtime running effect naked eyes as it can be seen that most of particulate matter all goes out from first
Mouth is separated, and only a small amount of particle is flowed out from the 4th outlet.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology all without departing from the spirit and scope of the present invention, carries out modifications and changes to above-described embodiment.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should be covered by the claims of the present invention.
Claims (15)
1. a kind of total phosphorus detection system, which is characterized in that the total phosphorus detection system includes at least:
Preprocessing module (1), for reducing the particulate matter in fluid to be measured；
Module (2) are cleared up in photocatalysis, are connected to the preprocessing module, are cleared up based on light-catalyzed reaction, and being used for will be to be measured
Organic phosphorus in fluid is converted into Phos；
Microfluid detection module (3) is connected to photocatalysis resolution module, successively includes the Microfluidic Mixing component of connection
(3.1) and microfluid detection components (3.2), the Microfluidic Mixing component are used to mix fluid to be measured with detection with medicament aobvious
Color, the microfluid detection components are used to detect the absorbance of the fluid to be measured after colour developing.
2. total phosphorus detection system as described in claim 1, which is characterized in that the preprocessing module (1) includes:
It pre-processes import (1.1), for receiving fluid to be measured；
First arc split tunnel (1.2), including the first liquid inlet and the first liquid outlet, first liquid inlet are set to described the
It one end of one arc split tunnel (1.2) and is connected to the pretreatment import (1.1), first liquid outlet is set to described the
The other end of one arc split tunnel (1.2), including first outlet (1.2.1) and second outlet (1.2.2), wherein first goes out
Mouth (1.2.1) arc center of circle remote compared to second outlet (1.2.2)；
Power Component (1.3), including the first transfer tube (1.3.1) and the second transfer tube (1.3.2), first transfer tube
(1.3.1) and the second transfer tube (1.3.2) respectively drive fluid from the first outlet (1.2.1) and from described second
Export the fluid flowing of (1.2.2).
3. total phosphorus detection system as claimed in claim 2, which is characterized in that further include one or more in following characteristics:
1) Power Component (1.3) further includes controller, for controlling first transfer tube (1.3.1) and described the respectively
Two transfer tubes (1.3.2)；
2) preprocessing module further include: the second arc split tunnel (1.4), including the second liquid inlet (1.4.1) and second
Liquid outlet, second liquid inlet (1.4.1) are set to one end of the second arc split tunnel (1.4) and go out with described second
Mouth (1.2.2) connection, second liquid outlet are set to the other end of the second arc split tunnel (1.4), including third goes out
Mouth (1.4.2) and the 4th outlet (1.4.3), wherein third exports (1.4.2) compared to the 4th outlet (1.4.3) far arc center of circle；
3) preprocessing module further includes primary filter component (1.5), is set to pretreatment import (1.1) and separates with the first arc
Between channel (1.2), for filtering the large particle in fluid to be measured.
4. total phosphorus detection system as described in claim 1, which is characterized in that the photocatalysis clears up module and includes:
Photocatalysis clear up import (2.1), be connected to the preprocessing module (1), for receive come from preprocessing module (1) to
Fluid measured；
Reaction tank (2.2) are cleared up in photocatalysis, are connected to photocatalysis resolution import (2.1), for carrying out light-catalyzed reaction；
It is equipped with anode (2.2.1) and cathode (2.2.2) in the photocatalysis resolution reaction tank, the anode is laid in photocatalysis and disappears
Solution reaction bottom of pond portion, the cathode (2.2.2) be set to the photocatalysis resolution reaction tank side wall and not with the anode
(2.2.1) is directly contacted；
Ultraviolet lamp (2.3) provides light source for clearing up reaction tank (2.2) for the photocatalysis；
Photocatalysis resolution outlet (2.4) is connected to photocatalysis resolution reaction tank (2.2), to be measured after reacting for being discharged
Fluid.
5. total phosphorus detection system as claimed in claim 4, which is characterized in that further include one or more in following characteristics:
In the photocatalysis resolution module,
1) anode (2.2.1) is flake；
2) cathode (2.2.2) the circular side wall free of discontinuities, it is preferred that the cathode (2.2.2) is at least around perimeter side wall
Half；
3) volume of photocatalysis resolution reaction tank (2.2) is 25-1500 microlitres；
4) cathode (2.2.2) is Ti electrode；
5) photocatalysis resolution module further includes photocatalysis resolution heating component, for the photocatalysis clear up reaction tank into
Row heating；
6) photocatalysis resolution reaction tank side is equipped with light-transmitting opening, and the ultraviolet lamp is set to the top of the light-transmitting opening, described
Transparent glass (2.5) are equipped at light-transmitting opening.
6. total phosphorus detection system as claimed in claim 5, which is characterized in that further include one or more in following characteristics:
7) feature 6) in, the length of the ultraviolet lamp (2.3) is greater than the half of the light-transmitting opening length；
8) feature 6) in, the width of the ultraviolet lamp (2.3) is no more than the width of photocatalysis resolution reaction tank；
9) feature 6) in, the ultraviolet lamp (2.3) is bonded transparent glass (2.5) setting.
7. total phosphorus detection system as described in claim 1, which is characterized in that the Microfluidic Mixing component (3.1) includes:
Microfluid injection port (3.1.1) is connected to photocatalysis resolution module, for receiving from photocatalysis resolution module
Fluid to be measured；
Microfluid medicament mouth (3.1.2), for receiving the medicament that can be reacted with fluid to be measured；
Microfluidic Mixing chamber (3.1.3), with the microfluid injection port (3.1.1) and the microfluid medicament mouth (3.1.2) point
It is not connected to, for mixing fluid to be measured and medicament, so that liquid stream sample to be measured is reacted with medicament, the Microfluidic Mixing chamber
The side (3.1.3) is equipped with venthole (3.1.3.1)；
The microfluid detection components (3.2) include:
Microfluid test chamber (3.2.1) is connected to the Microfluidic Mixing chamber (3.1.3), for detecting the prepare liquid after reacting
Flow sample；
Optical element (3.2.2), for providing light source to the microfluid test chamber (3.2.1).
8. total phosphorus detection system as claimed in claim 7, which is characterized in that further include one or more in following characteristics:
1) venthole (3.1.3.1) is located at side wall and/or the top of the mixing chamber (3.1.3)；
2) diameter of the venthole (3.1.3.1) is 1-5mm；
3) vibrator (3.1.4) is equipped with below the Microfluidic Mixing chamber (3.1.3)；
4) the microfluid detection module further includes flow control component (3.3), for driving liquid stream sample to be measured to detect in microfluid
The flow of fluid to be measured is flowed and/or controlled in device.
9. total phosphorus detection system as described in claim 1, which is characterized in that further include electrolyte mixing module (4), be set to institute
State between preprocessing module (1) and photocatalysis resolution module (2), for carry out the addition of photocatalysis resolution electrolyte with
Mixing.
10. total phosphorus detection system as claimed in claim 9, which is characterized in that the electrolyte mixing module includes: hollow
Hybrid agent (4.1) is equipped with electrolyte mixing inlet (4.2) and electrolyte is mixed on the length direction of the hybrid agent
It closes liquid outlet (4.3), the electrolyte mixing liquid outlet (4.3) is connected to photocatalysis resolution module (2), in the electrolysis
Matter mix inlet (4.2) between electrolyte mixing liquid outlet (4.3), be sequentially communicated in the mixer main body be provided with it is more
A mixed cell (4.4), the mixed cell (4.4) are hollow prism.
11. total phosphorus detection system as claimed in claim 10, which is characterized in that further include one or more in following characteristics
: in the electrolyte mixing module,
1) mixed cell (4.4) is any one or more of selected from hollow quadrangular, hexagonal prisms or eight prisms, preferably
, it is that hollow square prism, regular hexagonal prism or positive eight prism are any one or more of；
2) adjacent mixed cell is connected to by communication port, and each communication port is located along the same line；
3) height of the hollow cavity of each mixed cell (4.4) is equal, it is preferred that the height of the hollow cavity is 0.1-0.6mm；
4) floor space of the mixed cell (4.4) is 20-40mm2；
5) base area of each mixed cell (4.4) is identical；
6) each mixed cell (4.4) shape and volume are consistent.
12. the method for carrying out total phosphorus detection using any total phosphorus detection system of claim 1-11, which is characterized in that packet
Include following steps:
(1) fluid to be measured is pre-processed using preprocessing module, reduces the particulate matter in fluid to be measured；
(2) photocatalysis resolution is carried out using photocatalysis resolution module to pretreated fluid to be measured, by having in fluid to be measured
Machine phosphorus is converted into Phos；
(3) fluid to be measured after resolution is mixed into colour developing with medicament with the Microfluidic Mixing component detection of microfluid detection module,
Microfluid detection module microfluid detection components detection colour developing after fluid to be measured absorbance, according to absorbance calculate to
Total phosphorus concentration in fluid measured.
13. the method for total phosphorus detection as claimed in claim 12, which is characterized in that in step (1), control in preprocessing module
The first transfer tube drive the fluid from the first outlet, control the second transfer tube driving in preprocessing module from the
The fluid flowing of two outlets；Preferably, first transfer tube is different from the pump speed of second transfer tube.
14. the method for total phosphorus detection as claimed in claim 13, which is characterized in that the pump speed of first transfer tube is greater than institute
State the pump speed of the second transfer tube.
15. the method for total phosphorus detection as claimed in claim 14, which is characterized in that the pump speed of first transfer tube is 70-
150mL/min, and/or, the pump speed of second transfer tube is 60-130mL/min.
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