CN110470609A - Complex water body multi-parameter based on microflow control technique examines device and method fastly - Google Patents

Complex water body multi-parameter based on microflow control technique examines device and method fastly Download PDF

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Publication number
CN110470609A
CN110470609A CN201810449086.4A CN201810449086A CN110470609A CN 110470609 A CN110470609 A CN 110470609A CN 201810449086 A CN201810449086 A CN 201810449086A CN 110470609 A CN110470609 A CN 110470609A
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chip
sample
water body
detection
parameter
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CN110470609B (en
Inventor
孙冰
姜慧芸
王林
朱红伟
石宁
徐伟
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China Petroleum and Chemical Corp
Sinopec Safety Engineering Research Institute Co Ltd
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China Petrochemical Corp
Sinopec Qingdao Safety Engineering Institute
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Priority to CN201810449086.4A priority Critical patent/CN110470609B/en
Priority claimed from CN201810449086.4A external-priority patent/CN110470609B/en
Publication of CN110470609A publication Critical patent/CN110470609A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/50Containers for the purpose of retaining a material to be analysed, e.g. test tubes
    • B01L3/502Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
    • B01L3/5027Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3577Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64Fluorescence; Phosphorescence
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65Raman scattering
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2200/00Solutions for specific problems relating to chemical or physical laboratory apparatus
    • B01L2200/10Integrating sample preparation and analysis in single entity, e.g. lab-on-a-chip concept
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00Additional constructional details
    • B01L2300/02Identification, exchange or storage of information
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00Additional constructional details
    • B01L2300/08Geometry, shape and general structure
    • B01L2300/0803Disc shape
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00Additional constructional details
    • B01L2300/08Geometry, shape and general structure
    • B01L2300/0809Geometry, shape and general structure rectangular shaped
    • B01L2300/0829Multi-well plates; Microtitration plates

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Abstract

The present invention relates to microfluidic art, discloses a kind of Complex water body multi-parameter based on microflow control technique and examine equipment and the fast detecting method of Complex water body multi-parameter fastly.It includes chip and detection device that the Complex water body multi-parameter examines equipment fastly;Wherein, the chip includes the reaction tank for example reaction;The detection device is used to detect the signal of the sample in the reaction tank.The detection speed that Complex water body multi-parameter of the invention examines equipment and detection method fastly is fast, flux is high, has good processing capacity for complex sample.

Description

Complex water body multi-parameter based on microflow control technique examines device and method fastly
Technical field
The present invention relates to microfluidic arts, and in particular to a kind of Complex water body multi-parameter based on microflow control technique is fast Examine equipment and the fast detecting method of Complex water body multi-parameter.
Background technique
While world economy and industrial expansion are that the mankind bring huge convenient, but also pollutant is emitted on quantity It is continuously increased in type, environmental issue is on the rise.Greatly developing all kinds of high-precision analysis instruments and detection technique Meanwhile the analytical technology of small portable, simple and fast also becomes a big research hotspot, it is numerous because operating to supplement large-scale instrument It is trivial, maintenance workload is larger, requires laboratory environment high, to be difficult to use in on-site test etc. deficiency.
Micro-total analysis system is also known as chip lab, be intended to by laboratory functional one be integrated on a chip Kind analytical technology, brilliant prospect is shown in terms of the miniaturization of analytical technology, portability, automation, is become in recent years One big research hotspot.
For micro-total analysis system at present also in developing stage, Shang Buneng actually realizes the function of chip lab, thus When involving the need for carrying out the analysis experiment of pre-treatment, pretreatment part experiment is usually first manually completed, enters back into micro- complete point Analysis system is analyzed, and micro-total analysis system automation, rapid, portability development are limited.
Summary of the invention
It is of the existing technology for the high-throughput quick test problems of complex sample the purpose of the invention is to overcome, it mentions Equipment and the fast detecting method of Complex water body multi-parameter are examined fastly for a kind of Complex water body multi-parameter based on microflow control technique, the complexity water Body multi-parameter examines that equipment detection speed is fast, and flux is high fastly, has good processing capacity for complex sample.
To achieve the goals above, it is fast to provide a kind of Complex water body multi-parameter based on microflow control technique for one aspect of the present invention Equipment is examined, it includes chip and detection device which examines equipment fastly;Wherein, the chip be rotary chip or Person's straight-line chip, the chip include the reaction tank for example reaction;The detection device is for detecting the reaction tank In sample signal.
Preferably, the label for determining detection signal, the label and the reaction tank pair are provided on the chip It should be arranged.
Preferably, the multiple reaction tank of the rotary chip is arranged in using the center of the chip as the circle in the center of circle Zhou Shang.
Preferably, the chip includes substrate and cover plate, and the substrate is fixedly connected with the cover plate, alternatively, the base Piece and the cover plate can be mutually shifted, to change the connected relation in the chip between reaction tank and/or runner.
Preferably, it further includes sample introduction component that the Complex water body multi-parameter examines equipment fastly, and the sample introduction component is used for sample Product sample introduction is into the chip.
It is highly preferred that the sample introduction component is manual injector;
It is highly preferred that the sample introduction component includes pretreatment portion, the pretreatment portion is for pre-processing sample.
Preferably, the detection device includes more than one detection part.
It is highly preferred that the detection part be chromaticity sensing section, absorbance detection component, fluorescence signal detection part, One of Raman signal detection component and infrared spectroscopy detection part are a variety of.
Preferably, the water quality many reference amounts detection device further includes the driving part for driving chip rotation, signal acquisition part One of part, data processor, data output component and data transfer component are a variety of.
Second aspect of the present invention provides a kind of fast detecting method of Complex water body multi-parameter, wherein utilizes answering for aforementioned present invention Miscellaneous water body multi-parameter is examined equipment fastly and is detected, and by sample feeding into the chip, and is examined by the detection device It surveys.
Preferably, it by rotating the chip or keeping the chip mobile relative to the detection device, completes different Sample detection in the reaction tank.
Preferably, by being arranged on the chip for determining the label of detection signal, determine what detection device used Detection part.
Through the above technical solutions, Complex water body multi-parameter of the invention examine device and method fastly can be according to the need of detection Appropriate chip selected to use, detection part, sampling device etc. are wanted, has the advantages that high-throughput, detection is fast, accuracy is high, needle Good detection effect is attained by various samples, pretreatment appropriate, reaction process can also be set as needed, more Quickly and easily complete detection.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of rotary chip of the invention;
Fig. 2 is a kind of structural schematic diagram of slidingtype chip of the invention;
Fig. 3 is a kind of structural schematic diagram of manual injector of the invention;
Fig. 4 is the structural schematic diagram of the manual injector with pretreatment component of the invention;
Fig. 5 is the structural schematic diagram of detection device of the invention.
Description of symbols
1, manual injector 2, chip
11, control unit 12, sample cell 13, out sample portion
14, pretreatment portion
21, runner 22, reaction tank 23, injection port
31, light source 32, branch optical fiber 33, spectroscopy equipment
Specific embodiment
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more New numberical range, these numberical ranges should be considered as specific open herein.
One aspect of the present invention provides a kind of Complex water body multi-parameter based on microflow control technique and examines equipment fastly, the Complex water body It includes chip and detection device that multi-parameter examines equipment fastly;Wherein, the chip be rotary chip or straight-line chip, it is described Chip includes the reaction tank for example reaction;The detection device is used to detect the signal of the sample in the reaction tank.
In the present invention, the Complex water body multi-parameter examines equipment by using microflow control technique fastly, can be by core Multiple reaction tanks are arranged on piece, so as to be completed in a short time the synchronous detection of a large amount of samples, and can pass through chip Interior structure design, completes the operation such as sample pretreatment, reaction, and detection process Highgrade integration is easy to operate, and precision is high.
According to the present invention, there is no particular limitation for the structure of the chip, can be rotary chip or straight-line core Piece can be the various well known shapes such as circle, rectangle.
As the rotary chip, refer to can on chip a little where chip rotation in surface.From From the point of view of rotation, the rotary chip is preferably circular or regular polygon, more preferably round.It is described rotary When chip is round, preferably rotated around its center of circle.
A preferred embodiment according to the present invention, as shown in Figure 1, the multiple reaction tank is arranged with the core The center of piece is on the circumference in the center of circle.Center of the i.e. the multiple reaction tank apart from the chip is equidistant.
Another preferred embodiment according to the present invention, the reaction tank is divided into multiple groups, and every group of reaction tank has Multiple reaction tanks, every group of multiple reaction tanks are separately positioned on using the center of the chip as one in one group of concentric circles in the center of circle Circumference on.That is center of every group of the multiple reaction tanks apart from the chip is equidistant.
There is no particular limitation for the rotating manner of the rotary chip, it is preferable that the rotary chip can pass through It drives either manually or by the driving part in detection device and is rotated in detection device, preferably around the rotary chip Center rotation.From detection device is simplified, cost is reduced, convenient for from the point of view of portable operation, the rotary chip is excellent Gating can be manually rotated.And from detection efficiency is improved, it is realized in the short time from the point of view of detecting on a large scale, the rotary core Piece preferably passes through the driving rotation of the driving part in detection device.
As the straight-line chip, refers to the chip that the reaction tank on chip is arranged in rows, is typically designed to rectangle, And with reaction tank more than a row.The reaction tank of straight-line chip, generally can be by making straight-line core due to marshalling Piece is mobile relative to the detection device and is detected, such as the pull straight-line chip in detection device.
In the present invention, the reaction tank on the chip can be 2 or more, preferably 5 or more, more preferably 10- 50.It can also include runner on the chip for the ease of reaction, the runner flows between differential responses pond for sample It is dynamic.The set-up mode of the runner needs to cooperate chip detection demand to carry out, such as when needing to carry out multistep reaction in the chips, It can be set to include successively reaction tank-runner-reaction tank-runner-reaction tank structure, to complete in multiple reaction tanks Different reactions.In order to control the flowing of sample, various promotion mixed structures, micro-valve etc. can also be set in the chips, Whether for controlling the mixing and flowing of sample.
A preferred embodiment according to the present invention is provided with the mark for determining detection signal on the chip Note, the label are correspondingly arranged with the reaction tank.
A preferred embodiment according to the present invention, as shown in Figure 1, the chip has multiple reaction tanks, Duo Gesuo Reaction tank is stated to be arranged in using the center of the chip to be correspondingly arranged with the reaction tank useful on more than one circumference in the center of circle In the label for determining detection signal.In the use process of chip, by rotary chip, so that the reaction tank in chip is located at inspection The corresponding inspection positions of device are surveyed, while can determine corresponding detection part.Preferably, it is respectively corresponded with each reaction tank It is provided with the label for determining detection signal, thus a chip can be completed in a short time a variety of different Testing index Detection.And detection process is easy to operate, and accuracy is high, and can be suitable for various detection methods.
In the present invention, the label can be the label with specific color or shape, such as can pass through printing Or the modes such as stickup are formed on the chip, the groove with specific shape, the notch etc. being also possible on chip.It is described There is no particular limitation for the shape of label, achievees the purpose that identify and distinguish between, such as can be triangle, square, just Pentagon, star, naturally it is also possible to for number, letter or various irregular shapes.Can only it be arranged on 1 on chip Label is stated, the label is for determining that the detection signal of chip (can be same detection signal, be also possible in multiple reaction tanks not With the detection ordering of signal), thus when carrying out different tests with different chips convenient for determining detection mode;It can also on chip With corresponding one group even each corresponding detection signal of reaction tank setting, to complete the detection of unlike signal in a chip.
In the present invention, as long as differential responses pond can be with after the set-up mode of the multiple reaction tank rotates chip Positioned at the detection zone of detection device.By the multiple reaction tank being arranged in the center center of circle of the chip On more than one circumference, so as to complete the detection of multiple reaction tanks on chip with single detection part, reaches batch and examine The purpose of survey.
According to the present invention, the chip includes substrate and cover plate, and the substrate is fixedly connected (also referred to as with the cover plate " fixed chip "), alternatively, the substrate and the cover plate can be mutually shifted, thus change in the chip reaction tank and/ Or the connected relation (also referred to as " slidingtype chip ") between runner.It is set in general, being examined fastly in Complex water body multi-parameter of the invention It is above-mentioned fixed chip used in standby, slidingtype chip also can be used as needed.
As the slidingtype chip, can have reaction tank and/or runner on the substrate, and in the cover plate It is upper that there is reaction tank and/or runner, by being mutually shifted for the substrate and the cover plate, can make between runner and reaction tank Connected relation change, such as form two disconnected reaction tanks on substrate, form runner on cover plate, it is mobile before runner Two reaction tanks cannot be connected to;And being mutually shifted by cover plate and cover plate, runner can be connected to two reaction tanks, so that Sample and/or preset reagent in two reaction tanks can react to each other, consequently facilitating the progress reacted in control chip.It is described Can according to need on slidingtype chip and multiple reaction tanks and multiple runners be set, adapt to Complex water body multi-parameter examine fastly in it is various Complicated, high pass quantitative response demand.Above-mentioned movement can be sliding or rotation etc. in plane.
A preferred embodiment according to the present invention, as shown in the a-d in Fig. 2, the rotatable chip 1 includes base Piece and cover plate, the reaction tank setting on the substrate, are provided with reagent, the substrate and the cover plate on the cover plate Relative movement, so that the reaction tank is interconnected or separates with the reagent.A in Fig. 2 shows rotatable chip 1 Substrate, be provided with reaction tank thereon, b shows the cover plate of rotatable chip 1, is provided with reagent thereon.C, d in Fig. 2 Two kinds of rotation status figures of the respectively described rotatable chip 1 show the state that reaction tank is connected to from different reagents.
According to the present invention, it further includes sample introduction component that the Complex water body multi-parameter examines equipment fastly, and the sample introduction component is used for By sample feeding into the chip.There is no particular limitation for the sample introduction component, can complete above-mentioned sample feeding operation i.e. Can, existing any sampling device can be used.From the point of view of convenient for operation and portability, it is preferable that described Sample introduction component is manual injector.
As a kind of manual injector of the invention, as shown in figure 3, the manual injector 1 includes sample cell 12, control Portion 11 and out sample portion 13, the control unit 11 are connected with the sample cell 12, for entering sample and being maintained at the sample In product pond 12 or sample is made to release the sample cell 12 through the sample portion 13 out, the sample portion 13 out is located at the sample cell 12 The side opposite with the control unit 11;The injection port 23 of the manual injector 1 and chip 2 is tightly connected.
The manual injector 1 can cooperate with the chip 2, realize sample introduction and control sample in the chip 2 Flow process purpose, the manual injector 1 can be used for sampling, thus the dress that the very big operation simplified needs It sets, is highly convenient for the use of sampling device under various application scenarios.Flow process of the above-mentioned control sample in chip 2, simultaneously Including the process for pushing sample to move forward or back, so as to so that the function of chip is more diversified, such as sample can be made anti- Again by some reaction tank to accelerate the mixing of sample, or after first being mixed with the sample in some chamber, then with it is other The sample of reaction tank mixes.
As needed, the injection port 23 can protrude from the outside of chip, also can be set in the inside of chip, preferably The injection port 23 is provided with screw thread, to be screwed on sample portion 13 out.
According to the present invention, the manual injector 1 can be according to different hand samplings from the connection relationship of the chip 2 Device is selected.
A preferred embodiment according to the present invention takes for the ease of the completion of manual injector 1 is used alone Sample process, sample portion 13 and the injection port 23 of chip 2 out of the manual injector 1 are removably tightly connected.It, can be with when sampling The manual injector 1 is removed, enter sample by the operation control unit 11 and is maintained in the sample cell 12, then By going out after sample portion 13 connect with the injection port 23 of chip 2 for manual injector 1, operate the control unit 11 will sample described in out Release the injection port that the sample cell 12 enters the chip 11 in sample portion 13.
It can be to be screwed on or connected by elastic sealing element as the above-mentioned concrete mode being removably tightly connected It connects, the bottom in the preferably described sample portion 13 out has helicitic texture or flexible seal member, is preferably screwed on.The helicitic texture can Think internal thread structure or external thread structure;The flexible seal member can be rubber stopper.
Another preferred embodiment according to the present invention, in order to be further simplified device, the manual injector 1 Sample portion 13 is fixedly connected with the injection port 23 of the chip 2 out.It is highly preferred that the sample cell 12 of the manual injector 1, out sample The injection port 23 of portion 13 and the chip 2 is formed as one, in use, sample can directly be added in sample cell 12, then will The control unit 11 is coupled with sample cell 12, by operation control portion 11, controls the flow process of sample in the chips.
A further preferred embodiment according to the present invention, the control unit 11 control the inner cavity of sample cell 12 The range of (i.e. the chamber for sample storage of sample cell 12 and the formation of control unit 11) volume change is according in the chip 2 Portion's structure is selected.As long as the sample of specified amount is packed into sample cell as a result, so that it may which accurate control sample is in chip 2 Each runner, the mobility status in reaction tank, facilitate the control that sample flow in experimentation is repeated several times, improve experiment Repeatability.
In accordance with the present invention it is preferred that the control unit 11 and the sample cell 12 are detachably connected.By by the control Portion 11 processed and the sample cell 12 are detachably connected, the two can be separated, convenient for adding sample in sample cell.
According to the present invention, there is no particular limitation for the shape of the sample cell 12 and the control unit 11, and the two can phase Mutually cooperation, realization enter sample and are maintained in the sample cell 12 or sample is made to go out sample portion 13 described in release the sample Product pond 12.Specifically, the sample cell 12 and the control unit 11 are preferably all cylindricality.The control unit 11 and the sample Also there is no particular limitation for the connection type in product pond 12, such as can be connected and sealed, be screwed on by seal member etc., from From the aspect of operating the control unit 11, the preferably described control unit 11 is screwed on the sample cell 12.
A preferred embodiment according to the present invention, the process that the control unit 11 controls sample flow pass through described The cavity volume of sample cell 12 caused by relative motion between control unit 11 and the sample cell 12, which changes, to be completed.
Preferably, the sample cell 12 and control unit 11 can be set to tube-in-tube structure.Wherein, the control unit 11 can be with As outer cylinder or inner cylinder.It is highly preferred that the inside of the sample cell 12 is arranged in the control unit 11.Specifically, the sample Product pond 12 can be the outer cylinder of upper opening, and the control unit 11 can be the inner cylinder of sealed bottom.Preferably, the control unit 11 may be set to be telescopic piston.By setting piston for control unit 11, can be relatively moved in sample cell 12.It is logical Crossing makes control unit 11 and sample cell 12 cooperate, and control unit 11 relatively moves inside sample cell 12, makes the interior of sample cell 12 Chamber size changes, and control sample enters or outflow sample cell 12.
In order to complete control unit 11 and sample cell 12 and be tightly connected, preferably set in the lateral wall bottom of the control unit 11 It is equipped with sealing ring, the sealing ring is for sealing gap between the control unit 11 and the sample cell 12.
Another preferred embodiment according to the present invention, the process that the control unit 11 controls sample flow pass through institute The deformation process for stating control unit 11 itself is completed.The control unit 11 have can deformation part, and can deformation part by this Deformation changes the volume of 12 inner cavity of sample cell.It is described can deformation part shape and set-up mode there is no particular limitation, Preferably, the control unit 11 can deformations be divided into the scalable side wall of alterable height.It is specifically as follows folding side wall, For example formed as longitudinal section be continuous N font tubular or middle part can deformation part connection up and down two can not deformations Point structure (wherein, can deformation part can be made of flexible material, by can deformation part deformation change up and down two not Can deformation part mutual alignment relation, such as by horizontal connection structure variation be mutual insert structure) etc..The control unit 11 Side wall as can deformations timesharing, preferably deformation occurs at top, and when use can apply pressure or pulling force at the top of this, Manipulate the Sidewall Height variation of the control unit 11.
As above-mentioned control unit 11 can deformation part material, preferably flexible material, more preferably flexible macromolecule Polymer is specifically as follows one of polyethylene, polypropylene, polytetrafluoroethylene (PTFE), polytetrafluoroethylene (PTFE) or a variety of, wherein being preferably Polyethylene and/or polypropylene.
The material of the manual injector 1, it is however preferred to have translucency and chemically inert material.For the ease of observe into Sample process, the preferably described sample cell 12 are transparent or semitransparent sample cell.As the material of the sample cell 12, preferably high score Sub- polymer is specifically as follows polyethylene, polypropylene, polystyrene, polyvinyl chloride, polytetrafluoroethylene (PTFE), polycarbonate, poly- methyl One of methyl acrylate, ABS plastic, phenolic resin, epoxy resin, glass and quartz are a variety of, wherein preferably poly- second One of alkene, polypropylene, polystyrene and polyvinyl chloride are a variety of.In addition, the control unit 11 is except can be in addition to deformation part Part and it is described go out sample portion 13 it is also preferred that using above-mentioned material.
If Fig. 3 shows, it includes manual injector 1 and chip 2 that Complex water body multi-parameter of the invention examines equipment fastly.G shows in Fig. 3 The structure of chip 2 is gone out, the chip 2 is round dispersion shape multiple flow passages chip, including 1 injection port 23 and 6 and injection port 23 22,6 runners 21 of the reaction tank being equally spaced are respectively communicated with each reaction tank 22 and injection port 23;It is only shown in a-d in Fig. 3 The injection port 23 of chip 2 illustrates only the one group of runner 21 and reaction tank 22 of chip 2 in e-f;The manual injector 1 wraps It includes the sample cell 12 of the tubular of polyethylene, the control unit 11 of cupuliform and sample portion 13, the control unit 11 is arranged in the sample out The inside in product pond 12, and be removably tightly connected with the sample cell 12, for entering sample and being maintained at the sample In pond 12 or sample is made to release the sample cell 12, and the lateral wall bottom setting of the control 11 through the sample portion 13 out There is the sealing ring of rubber system, sample portion 13 is located at the bottom of the sample cell 12 out;The manual injector 1 and the chip 2 The injection port 23 is formed as one.Fluid sample is added in sample cell 12 first when sample introduction, control unit 11 is placed in sample In pond 12, the sealing ring is contacted with the inner sidewall of sample cell 12, pushes control unit 11 until touching interface bottom.Sample exists In the lower runner 21 for entering chip 2 of pressure effect, sample flow rate is gradually reduced in flow process, in a period of time (such as 10- Liquid fills up first reaction tank after 60s), enters liquid release reaction tank 22 since 23 end pressure of injection port at this time is less than The pressure in gap between two layers of chip, sample will not continue to overflow, and all reaction tanks are filled out after a period of time (such as 10-60s) Full, sample stops flowing.
A preferred embodiment according to the present invention, as shown in figure 4, the sample introduction component can also include pretreatment Portion 14, the pretreatment portion 14 is for pre-processing sample.It is described go out sample portion 13 be located at the pretreatment portion 14 with control The opposite side in portion 11 processed is forced out described again after the processing for making sample pass through pretreatment portion by the movement of the control unit 11 Manual injector.
According to the present invention, for a variety of pretreatment operations for cooperating sample to need, the pretreatment portion 14 preferably includes 1 Above preprocessing module (14a, 14b, 14c), preferably 2 or more, more preferably 2-5, further preferably 2-3.
As the pretreatment operation carried out in each preprocessing module, can be selected according to the sample of institute's sample introduction.Tool Body, the preprocessing module in filtering module, enrichment module, separation module, pH adjustment module and the reaction module one Kind is a variety of.As filtering module, wherein fiber, porous solid, accumulation medium etc. can be set, such as polypropylene is fine One of dimension, glass fibre, active carbon, gravel are a variety of, wherein preferably polypropylene fibre, glass fibre;As enrichment Module, wherein aluminium oxide, silica, targeting vector can be set;As reaction module, wherein may include the reaction needed Object, such as the mercuric sulfate with chloride progress precipitation reaction.For example, when carrying out the pretreatment of phosphate from sewage measurement sample, The preprocessing module includes filtering module, pH adjustment module and pre-reaction module;Carry out polycyclic aromatic hydrocarbon measurement sample in water When pretreatment, the preprocessing module includes filtering module and enrichment module.
According to the present invention, by the way that the pretreatment portion 14 and the sample cell 12 is detachably connected, it can be convenient and set Different preprocessing modules is set, so that manual injector be made to meet the needs of different sample pretreatments and sample introduction.As detachable The mode of ground connection, the sample cell 12 can pass through plug division, screw thread, buckle or the detachably connected pretreatment of groove Portion 14.
In order to improve the leakproofness of sample cell 12 and pretreatment portion 14, such as can be in sample cell 12 and pretreatment portion 14 Sealing performance between interconnecting piece can according to need between further setting sealing accessory, such as gasket Piece etc. guarantees that carry out process is gone on smoothly to improve the leakproofness of sample injector.
As shown in figure 4, the manual injector used includes control unit 11, sample cell 12, pretreatment portion 14 and sample portion 13 out, Control unit 11, sample cell 12 and pretreatment portion 14 are cylindrical, transparent glass material.The pretreatment portion 14 is filter module Block.The filtering module is internally provided with polypropylene fibre filter disc;Sample inlet is arranged in its top, on the side wall of the sample inlet It is provided with internal screw thread.Sample export is set in the bottom of sample cell 12, external screw thread is provided on the side wall of the sample export, it will The sample inlet of pretreatment portion 14 and the sample export of sample cell 12 are screwed on, and keep pretreatment portion 14 removably close with sample cell 12 Envelope connection.The sample export of pretreatment portion 14 is as sample portion 13 is gone out, and sample portion 13 is located at the middle part of 14 bottom of pretreatment portion out, The external screw thread for being screwed on micro-total analysis chip is provided on side wall.Control unit 11 can form sample with sealed sample pond 12 Chamber makes the mobile volume that can change sample cavity of control unit 11 by pushing manually, and makes the sample in sample cavity by pre- place Reason portion 14 is simultaneously extruded by going out sample portion 13.Before starting sample introduction, control unit 11 is opened, sample is injected into sample injector, closes control The injection port of the sample injector and chip is screwed on by portion 11, and control unit 11 is then pushed to make the smaller volume of sample cavity, and sample passes through Enter chip after the filter disc filtering of pretreatment portion 14.Observation enters the water sample of chip, has no grainless impurity.
According to the present invention, the detection device includes more than one detection part.The detection part is used for detection chip The signal of upper sample.
In the present invention, there is no particular limitation for the detection part, can be used for the various detection parts of chip detection, Such as the detection part can be chromaticity sensing section, absorbance detection component, fluorescence signal detection part, Raman signal inspection Survey one of component and infrared spectroscopy detection part or a variety of.It is wherein preferably absorbance detection component and fluorescence detection component One of or it is a variety of.
A preferred embodiment according to the present invention, as shown in figure 5, the detection part is by light source 31, branch light Fibre 32 and spectroscopy equipment 33 are constituted.The light source 31 is used for generating the light for carrying out testing required wavelength, the branch optical fiber 32 In detecting optical signalling in multiple reaction tanks simultaneously, the spectroscopy equipment 33 is for collecting the optical signal after reaction tank.When When being provided with the more than two reaction tanks not waited with the centre distance of the chip on chip, the branch optical fiber 32 can will be used It is divided into multichannel in the incident light of detection, to realize the detection for the reaction tank not waited with the centre distance of the chip.
According to the present invention, in order to realize data processing, data transmission the effects of, the water quality many reference amounts detection device also wraps Including can also include the mechanical part for driving chip rotation, signal acquisition component, data processor, data output component, number According to one of transmission part or a variety of.It further include number as a kind of preferred embodiment of water quality many reference amounts detection device According to processing component, data output component, data transfer component.As the data processor, such as can be including control Device, arithmetic unit and central processing unit of register etc.;It may include having the function of images outputting as the data output component Display screen, touch screen, voice output etc.;As the data transfer component, initial data can be uploaded to remote service Device is remotely handled, then result is returned directly to designated terminal, can also by data processor generate treated Information remote transmitting to cloud carries out information collection.
According to the present invention, in order to cooperate the markd chip of tool, the detection of many kinds of parameters is realized, the Complex water body multi-parameter There is identification component and more than one test section fastly, the identification part is used to detect to be used to determine on the chip in inspection equipment The label of signal is detected, the test section is used to determine that the detection label of signal to be corresponding on the chip.In chip In rotary course, the identification part identifies the label that each reaction tank setting is corresponded on the chip, then determines respectively each anti- The detection mode for answering pond to need to use, to realize the detection respectively to unlike signal object.
Second aspect of the present invention provides a kind of fast detecting method of Complex water body multi-parameter, utilizes the Complex water body of aforementioned present invention Multi-parameter is examined equipment fastly and is detected, and by sample feeding into the chip, and is detected by the detection device.
In order to which the detection of multi-parameter is rapidly completed, in the present invention it is possible to by rotating the chip or making the core Piece is mobile relative to the detection device, completes the sample detection in the different reaction tanks.For rotary chip, Ke Yitong It crosses rotary chip and completes detection;For straight-line chip, can complete to detect by pull chip.
A preferred embodiment according to the present invention, by being arranged on the chip for determining detection signal Label, determines the detection part that detection device uses.By with the use of having a markd chip, method of the invention can be Short time handles the detection process of multiple types sample signal, to improve detection speed.
The index that method of the invention can detecte includes COD, total nitrogen, sulfide, total phosphorus etc., specifically be can be used corresponding Reagent sample is handled after detect., can be preset in the chips by reagent for the reaction for needing to be added reagent, thus Detection accuracy is improved, and easily facilitates operation.
Method of the invention can according to the needs chip suitably selected to use, detection part, sampling device etc. of detection, To be attained by good detection effect for various samples, pretreatment appropriate can also be set as needed, reacted Journey more quickly and easily completes detection.It is especially suitable for being detected for water sample.
The present invention will be described in detail by way of examples below.In following embodiment, specific detection agents difference The commercially available product for being WAK for the Japanese physical and chemical company trade mark vertical altogether, sample COD, total nitrogen, sulfide, the mixing of total phosphorus titer are molten Liquid.
Embodiment 1
It includes manual injector 1, chip 2 and such as Fig. 3 institute that Complex water body multi-parameter used in the present embodiment examines equipment fastly The built-in hand-held spectrophotometer of rotary fixing frame shown.
Sample introduction is carried out using manual injector 1 as shown in Figure 3;Using band, there are four types of the circles of not isolabeling to have label Rotary chip, all 12 reaction tanks be averaged scattering device on the circumference of the center of circle equidistance R away from chip (in Fig. 3 12 reaction tanks are set on the basis of middle g signal).The chip 2 is round dispersion shape multiple flow passages chip, including 1 injection port 23 and 12 reaction tanks being equally spaced with injection port 23,22,12 runners 21 are respectively communicated with each reaction tank 22 and injection port 23;The injection port 23 of chip 2 is illustrated only in Fig. 3 in a-d, the one group of runner 21 and reaction tank of chip 2 are illustrated only in e-f 22;
The sample cell 12 of tubular of the manual injector 1 including polyethylene, the control unit 11 of cupuliform and sample portion 13 out, The inside of the sample cell 12 is arranged in the control unit 11, and is removably tightly connected with the sample cell 12, for making Sample enters and is maintained in the sample cell 12 or sample is made to release the sample cell 12, and institute through the sample portion 13 out The lateral wall bottom for stating control 11 is provided with the sealing ring of rubber system, and sample portion 13 is located at the bottom of the sample cell 2 out;
The injection port 23 of the manual injector 1 and the chip 2 is formed as one.
Fluid sample is added in sample cell 12 first, control unit 11 is placed in sample cell 12, the sealing ring and sample The inner sidewall in product pond 12 contacts, and pushes control unit 11 until touching interface bottom.Sample enters chip 2 under pressure In runner 21, sample flow rate is gradually reduced in flow process, and liquid fills up first reaction tank after 32s, due at this time 23 end pressure of injection port, which is less than, releases the pressure that reaction tank 22 enters gap between two layers of chip for liquid, and sample will not continue to overflow Out, all reaction tanks are filled after 19s, and sample stops flowing.
The hand-held spectrophotometer of the built-in rotary fixing frame is by light source 31, branch optical fiber 32 and spectroscopy equipment 33 It constitutes, and it is (total for optional 410nm (total nitrogen), 620nm (COD), 665nm (sulfide), 880nm to be prefixed measurement wavelength Phosphorus).Hand rotary process is used when test, rotates chip around the center of circle.Specific detection examination is prefixed on it can recognize chip Agent reacts with preset reaction reagent after sample solution is introduced reaction tank, absorption values is read after 30min.
1-3 is total nitrogen detection cell in 12 reaction tanks, and 4-6 is COD detection cell, and 7-9 is sulfide detection cell, and 10-12 is Total phosphorus detection cell corresponds to reaction tank in 4 groups and different labels is respectively set.It can be manually rotated chip and pass through above-mentioned reaction tank one by one, Spectrophotometer determines that the corresponding measurement wavelength of index to be detected, the wavelength for then changing light source are gone forward side by side after detecting above-mentioned label Row measurement.The corresponding concentration measured is respectively such as the following table 1.
Table 1
Embodiment 2
It includes round recognizable chip and as shown in Figure 3 that Complex water body multi-parameter used in the present embodiment examines equipment fastly The built-in hand-held spectrophotometer of rotary fixing frame.
Using band, there are four types of the circles of not isolabeling can recognize that chip, 4 reaction tanks are averaged scattering device away from chip The distance in the center of circle is the circle that distance of the scattering device in the center of circle away from chip is R2 in addition, 4 reaction tanks are averaged on the circumference of R1 Zhou Shang.The hand-held spectrophotometer of this is built-in rotary fixing frame is made of light source 31, branch optical fiber 32 and spectroscopy equipment 33, And being prefixed measurement wavelength is optional 410nm (total nitrogen), 620nm (COD), 665nm (sulfide), 880nm (total phosphorus).It surveys Hand rotary process is used when examination, rotates chip around the center of circle.Specific detection agents are prefixed on it can recognize chip, are being incited somebody to action After sample solution introduces reaction tank, reacts with preset reaction reagent, absorption values are read after 30min.
It 1,2 is total nitrogen detection cell that the distance in the center of circle away from chip, which is on the circumference of R1, in 8 reaction tanks, and 3,4 detect for COD Pond, it 5,6 is sulfide detection cell that distance, which is on the circumference of R2,7,8 is total phosphorus detection cell.Reaction tank is corresponded in 4 groups to be respectively set Different labels.It can be manually rotated chip and pass through above-mentioned reaction tank one by one, determination is to be checked after spectrophotometer detects above-mentioned label The corresponding measurement wavelength of index is surveyed, is then measured.The corresponding concentration measured is respectively such as the following table 2:
Table 2
The preferred embodiment of the present invention has been described above in detail, and still, the present invention is not limited thereto.In skill of the invention In art conception range, can with various simple variants of the technical solution of the present invention are made, including each technical characteristic with it is any its Its suitable method is combined, and it should also be regarded as the disclosure of the present invention for these simple variants and combination, is belonged to Protection scope of the present invention.

Claims (10)

1. a kind of Complex water body multi-parameter based on microflow control technique examines equipment fastly, which is characterized in that the Complex water body multi-parameter Fast inspection equipment includes chip and detection device;
Wherein, the chip is rotary chip or straight-line chip, and the chip includes the reaction tank for example reaction;
The detection device is used to detect the signal of the sample in the reaction tank.
2. Complex water body multi-parameter according to claim 1 examines equipment fastly, wherein be provided on the chip for determining The label of signal is detected, the label is correspondingly arranged with the reaction tank.
3. Complex water body multi-parameter according to claim 1 examines equipment fastly, wherein the rotary chip it is the multiple Reaction tank is arranged in using the center of the chip as on the circumference in the center of circle.
4. Complex water body multi-parameter according to claim 1 examines equipment fastly, wherein the chip includes substrate and cover plate, The substrate is fixedly connected with the cover plate, alternatively, the substrate and the cover plate can be mutually shifted, to change the core Connected relation in piece between reaction tank and/or runner.
5. Complex water body multi-parameter described in any one of -4 examines equipment fastly according to claim 1, wherein the Complex water body It further includes sample introduction component that multi-parameter examines equipment fastly, and the sample introduction component is used for sample feeding into the chip;
Preferably, the sample introduction component is manual injector;
Preferably, the sample introduction component includes pretreatment portion, and the pretreatment portion is for pre-processing sample.
6. Complex water body multi-parameter described in any one of -4 examines equipment fastly according to claim 1, wherein the detection device Including more than one detection part;
Preferably, the detection part is chromaticity sensing section, absorbance detection component, fluorescence signal detection part, Raman letter One of number detection part and infrared spectroscopy detection part are a variety of.
7. Complex water body multi-parameter described in any one of -4 examines equipment fastly according to claim 1, wherein the water quality is joined more Amount detection device further includes the driving part for driving chip rotation, signal acquisition component, data processor, data output component With one of data transfer component or a variety of.
8. a kind of fast detecting method of Complex water body multi-parameter, which is characterized in that using being answered described in any one of claim 1-7 Miscellaneous water body multi-parameter is examined equipment fastly and is detected, and by sample feeding into the chip, and is examined by the detection device It surveys.
9. the fast detecting method of Complex water body multi-parameter according to claim 8, wherein by rotating the chip or making institute State the sample detection that chip is mobile relative to the detection device, in the different reaction tanks of completion.
10. the fast detecting method of Complex water body multi-parameter according to claim 8 or claim 9, wherein pass through what is be arranged on the chip For determining the label of detection signal, the detection part that detection device uses is determined.
CN201810449086.4A 2018-05-11 Complex water body multi-parameter quick detection equipment and method based on microfluidic technology Active CN110470609B (en)

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