CN209215064U - A kind of separation of close and distant water component and collection device based on on-line checking - Google Patents

A kind of separation of close and distant water component and collection device based on on-line checking Download PDF

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Publication number
CN209215064U
CN209215064U CN201821610930.9U CN201821610930U CN209215064U CN 209215064 U CN209215064 U CN 209215064U CN 201821610930 U CN201821610930 U CN 201821610930U CN 209215064 U CN209215064 U CN 209215064U
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bottle
chromatographic column
separation
detector
magnetic valve
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张学治
刘青玲
潘波
李静
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Institute of Hydrobiology of CAS
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Institute of Hydrobiology of CAS
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Abstract

A kind of separation of close and distant water component and collection device based on on-line checking, including the water bottle, sample bottle, group sub-bottle, backwash liquor bottle being connected respectively with six logical selection valves, six logical selection valves pass sequentially through on-line degassing device and peristaltic pump is connected with chromatographic column, chromatographic column is linked in sequence again UV detector and fluorescence detector, fluorescence detector is connected separately with full-automatic collector and three-way magnetic valve, and two outlets of three-way magnetic valve are respectively connected to waste liquid bottle and group sub-bottle.The plant automation degree of the utility model is high, it is easy to operate, separating rate is fast, each component can be collected automatically, equipment takes up space small, it solves the problems, such as to automate during existing separation and collection, can not judge to elute terminal, and pass through the concentration of real-time monitoring elution fraction, realization is efficiently separated and collected.

Description

A kind of separation of close and distant water component and collection device based on on-line checking
Technical field
The utility model belongs to water treatment field, and in particular to a kind of separation of close and distant water component and receipts based on on-line checking Acquisition means.
Background technique
With the worsening shortages of water resource and the continuous improvement of water standard, at the advanced treating of drinking water and reusing sewage The problems such as reason, is increasingly prominent.The complicated multiplicity of organic matter, separation method are also varied in water environment.Hydrophilic and hydrophobic separation and receipts Collection is mainly adsorbed and is eluted using macroreticular resin.The suction-operated of macroreticular resin be by it and the molecule that is adsorbed it Between Van der Waals force and the hydrogen bond of formation etc..Simultaneously because the object that the cellular structure of resin keeps it different to molecular size Matter has screening effect.Therefore, organic compound is according to the difference of adsorption capacity and the size of molecular weight, in the adsorption mechanism of resin It is separated with lower realize of screening principle effect.
The hydrophobe separation of organic matter mainly uses manual separation and collection in the prior art.For example, Journal of Secondary sewage quilt of the Environmental Sciences (environmental science magazine) in the 520-527 pages report of volume 20 in 2008 XAD series plastics are separated into each component, and the method for only describing secondary sewage classification, this method is manual separation, is separated Journey does not use detector, cannot achieve judging automatically for elution terminal.The process does not use on-line degassing device, can not solve Certainly interference of the bubble to separation process.Patent " a kind of integral type protein chromatographic device ", can detecte ultraviolet suction by detector Luminosity, conductivity, pH value etc., but can not judge to elute terminal, also without specific separation application;Patent " dissolves in water Property organic constituents separation automation device and method ", the degree of automation is lower, such as the first feed liquor liquid storage bottle need manual switching, It can not achieve the continuous separation of multiple components and the undetectable eluate concentration of backwash.
In conclusion method and apparatus in the prior art, cannot achieve the automation of separation and collection, and backwash process In be unable to real-time monitoring backwash and go out the concentration feature of sample, thus can not judge to elute terminal, can not realize automatic collection Function, equipment are taken up too much space, and are operated relatively complicated.
Summary of the invention
The separation of close and distant water component and collection device that the purpose of the utility model is to provide a kind of based on on-line checking, the dress High degree of automation is set, easy to operate, separating rate is fast, can collect each component automatically, and equipment takes up space small, solves existing There is separation and cannot be automated during collecting, can not judge the problem of eluting terminal, and passes through real-time monitoring elution fraction Concentration, realization are efficiently separated and are collected.
The technical solution that the utility model is taken is as follows:
A kind of separation of close and distant water component and collection device based on on-line checking, including what is be connected respectively with six logical selection valves Water bottle, sample bottle, group sub-bottle, backwash liquor bottle, six logical selection valves pass sequentially through on-line degassing device and peristaltic pump is connected with chromatography Column, chromatographic column is linked in sequence again UV detector and fluorescence detector, and fluorescence detector is connected separately with full-automatic collector And three-way magnetic valve, two outlets of three-way magnetic valve are respectively connected to waste liquid bottle and group sub-bottle.
Further, the chromatographic column has 2~3, and each chromatographic column is respectively connected with pressure sensor and two three-way electromagnetic valves, Chromatographic column needed for being connected by two three-way electromagnetic valves.
Further, described six logical selection valves, three-way magnetic valve and two three-way electromagnetic valves are connected with control system, the control System processed is also electrically connected with on-line degassing device, peristaltic pump, pressure sensor, UV detector, fluorescence detector respectively.
Further, the control system includes wriggling pump control module, solenoid valve control module, detector control mould Block, on-line degassing device control module, pressure sensor control module, flow chart of tube (PID) display module and LCD touch Control module.
The utility model has the beneficial effects that
Utility model device high degree of automation, easy to operate, separating rate is fast, and equipment takes up space small, and backwash can Real-time monitoring judges automatically elution terminal according to the concentration signal intensity of component to be separated in eluent, realizes different component It efficiently separates and collects automatically, reduce system separating liquid resid vol;By the control system of setting, each component can be carried out Flexibly and easily switch and starts, high degree of automation.
Detailed description of the invention
Fig. 1 is utility model device connection schematic diagram;
In figure: 1, water bottle;2, sample bottle;3, sub-bottle is organized;4, A backwash liquor bottle;5, B backwash liquor bottle;6, six logical selection valve;7, On-line degassing device;8, peristaltic pump;9, two three-way electromagnetic valve A;10, two three-way electromagnetic valve B;11, two three-way electromagnetic valve C;12, pressure sensing Device;13, A chromatographic column;14, two three-way electromagnetic valve D;15, two three-way electromagnetic valve E;16, B chromatographic column;17, two three-way electromagnetic valve F;18, two is logical Solenoid valve G;19, two three-way electromagnetic valve H;20, UV detector;21, fluorescence detector;22, full-automatic collector;23, it three is powered Magnet valve;24, waste liquid bottle.
Specific embodiment
The utility model is described in further detail with reference to the accompanying drawing.
As shown in Figure 1, a kind of separation of close and distant water component and collection device based on on-line checking, including lead to choosing with six respectively Water bottle 1, sample bottle 2, group sub-bottle 3, A backwash liquor bottle 4 and B backwash liquor bottle 5, the two backwash bottles being connected to valve 6 fill difference Backwash solvent, six logical selection valves 6 pass sequentially through on-line degassing device 7 and the connection of peristaltic pump 8, and there are two A chromatographic columns 13 in parallel With B chromatographic column 16, each chromatographic column is connected with several two three-way electromagnetic valves and a pressure sensor, and chromatographic column is linked in sequence again to be had UV detector 20 and fluorescence detector 21, fluorescence detector 21 are connected separately with full-automatic collector 22 and three-way magnetic valve 23, two outlets of three-way magnetic valve 23 are respectively connected to waste liquid bottle 24 and group sub-bottle 3.
The six logical selection valve 6, three-way magnetic valve 24 and each two three-way electromagnetic valve are respectively connected with control system, control system By controlling six logical selection valves 6, water bottle 1, sample bottle 2, the switching for organizing sub-bottle 3, A backwash liquor bottle 4 and B backwash liquor bottle 5 are realized;It can By control three-way magnetic valve 23, to realize waste liquid bottle 24 and organize the switching of sub-bottle 3;Also it can control automatic sample collector 22 rotate clockwise or counterclockwise, realizes the collection of different samples;The control system also respectively with on-line degassing device 7, compacted Dynamic pump 8, pressure sensor 12, UV detector 20, fluorescence detector 21 are electrically connected, and need to control respective channel according to experiment It opens or closes.
The six logical selection valve 6 goes out valve for five into one, and five into water bottle 1 is separately connected, and sample bottle 2 organizes sub-bottle 3, A backwash liquor Bottle 4 and B backwash liquor bottle 5, the selection valve can open corresponding channel according to the needs of actual experiment;The automatic sample is received Storage 22 is programmable, can rotate collector automatically according to the numerical value change of UV detector 20, and mobile syringe needle realizes sample It is automatic to collect.
The control system includes wriggling pump control module, solenoid valve control module, detector control module, pipeline process Scheme (PID) display module, on-line degassing device control module, pressure sensor control module and LCD touch control module, In:
LCD touch control module, for receiving the operational order issued from contact control module, to the operational order It is processed and displayed, can also input corresponding operation instruction with the application software of operation support MATLAB;
Wriggling pump module, for receiving the operational order issued from contact control module, at the operational order Reason, and processing result is shown on liquid crystal touch screen;
Solenoid valve control module, for receive from contact control module issue operational order, to the operational order into Row processing, carrys out the on or off of electromagnetic valve for adjusting.
The sample of the utility model separates and collection method are as follows:
Organic matter in water sample to be separated is divided into strong dredge using macroporous absorbent resin XAD7HP and XAD4 by the utility model Aqueous acidic substance, strong-hydrophobicity neutral substance, weak hydrophobicity acidic materials, weak hydrophobicity neutral substance, strongly hydrophilic substance Five components.
One, the pretreatment of sample: 0.45 μm of membrane filtration of sample to be separated, and it is acidified to pH 2.0 with HCl, it is placed in In sample bottle.
Two, the filling of resin: strong-hydrophobicity resin XAD7HP is fitted into A chromatographic column 13, by weak hydrophobic resin XAD4 It is fitted into B chromatographic column 16, resin has to tamp, and column interior cannot be allowed cavity or bubble occur, be again if occurring Filling.
Three, the cleaning of resin: new resin contains the organic matters such as crosslinking agent during the preparation process, when being loaded into chromatographic column In after, need to be cleaned repeatedly with organic solvent, be cleaned later with clear water, finally separate sample, detailed process again are as follows:
The cleaning of XAD7HP resin: the access of six logical selection valves 6 and A backwash liquor bottle 4 of connection, on-line degassing device 7 carry out Backwash liquor sodium hydroxide is flowed into A chromatographic column 13 by two three-way electromagnetic valves 9, two three-way electromagnetic valves 11, flows through two by degassing, peristaltic pump 8 Three-way electromagnetic valve 14, two three-way electromagnetic valves 19 flow through three-way magnetic valve 23 using UV detector 20, fluorescence detector 21, enter Waste liquid bottle 24;It is cleaned again using same process using the backwash liquor acetonitrile in B backwash liquor bottle 5;Finally in water bottle 1 Water carry out forward and reverse clean twice (first by water by two three-way electromagnetic valves 9, two three-way electromagnetic valves 11 inflow A chromatographic column 13, Waste liquid bottle 24 is finally flowed into, then, water A chromatographic column 13 is reversely flowed into, then is passed through by two three-way electromagnetic valves 10, two three-way electromagnetic valves 14 Two three-way electromagnetic valves 11, two three-way electromagnetic valves 18 are crossed, waste liquid bottle 24 is finally flowed into), complete cleaning;In the behaviour unrelated with B chromatographic column 16 Two three-way electromagnetic valves 15 being attached thereto when making and two three-way electromagnetic valves 17 are closed;
The cleaning of XAD4 resin: XAD4 resin is cleaned using the above method.
Four, sample separates
The absorption of A chromatographic column 13: the access of six logical selection valves 6 and sample bottle 2 of connection, on-line degassing device 7 are de-gassed, Sample is flowed into A chromatographic column 13 by two three-way electromagnetic valves 9, two three-way electromagnetic valves 11 by peristaltic pump 8, and it is logical to flow through two three-way electromagnetic valves 14, two Solenoid valve 19 flows through three-way magnetic valve 23 using UV detector 20, fluorescence detector 21, into group sub-bottle 3, Qiang Shushui Property substance adsorbed by XAD7HP, into group sub-bottle 3 being weak hydrophobicity acidic materials, weak hydrophobicity neutral substance and strong parent The mixed component of aqueous substance.
The absorption of B chromatographic column 16: the access of connection six logical selection valve 6 and group sub-bottle 3, on-line degassing device 7 are de-gassed, Sample is flowed into B chromatographic column 16 by two three-way electromagnetic valves 9, two three-way electromagnetic valves 15 by peristaltic pump 8, and it is logical to flow through two three-way electromagnetic valves 17, two Solenoid valve 19 obtains strongly hydrophilic substance into sample automatic collector using UV detector 20, fluorescence detector 21 Component (enter sample divider at this time is a kind of purer component).
What A chromatographic column 13 adsorbed is substance (including the strong-hydrophobicity acidic materials, strong-hydrophobicity neutrals of strong-hydrophobicity Matter), what B chromatographic column 16 adsorbed is weak hydrophobic substance (including weak hydrophobicity acidic materials, weak hydrophobicity neutral substance), warp It is adsorbed after twice, the efflux into sample divider is strongly hydrophilic material composition.
Five, chromatographic column backwash is de-
13 backwash of A chromatographic column: the access of six logical selection valves 6 and A backwash liquor bottle 4 of connection, on-line degassing device 7 are taken off Backwash liquor sodium hydroxide is reversely flowed into A chromatographic column 13 by two three-way electromagnetic valves 10, two three-way electromagnetic valves 14, flowed through by gas, peristaltic pump 8 Two three-way electromagnetic valves 11, two three-way electromagnetic valves 18, using UV detector 20, fluorescence detector 21, strong-hydrophobicity acidic materials into Enter automatic collector;It is connected to the access of six logical selection valves 6 and B backwash liquor bottle 5, benefit is in the same way, anti-by backwash liquor acetonitrile To A chromatographic column 13 is flowed into, strong-hydrophobicity neutral substance is finally made to enter automatic collector.
16 backwash of B chromatographic column: the access of six logical selection valves 6 and A backwash liquor bottle 4 of connection, on-line degassing device 7 are taken off Backwash liquor sodium hydroxide is flowed into B chromatographic column 16 by two three-way electromagnetic valves 10, two three-way electromagnetic valves 17, it is logical to flow through two by gas, peristaltic pump 8 Solenoid valve 15, two three-way electromagnetic valves 18, using UV detector 20, fluorescence detector 21, weak hydrophobicity acidic materials enter certainly Dynamic collector;It is connected to the access of six logical selection valves 6 and B backwash liquor bottle 5, on-line degassing device 7 is de-gassed, and peristaltic pump 8 will be anti- Washing lotion acetonitrile flows into B chromatographic column 16 by two three-way electromagnetic valves 10, two three-way electromagnetic valves 17, flows through two three-way electromagnetic valves 15, two energization magnetic Valve 18, using UV detector 20, fluorescence detector 21, weak hydrophobicity neutral substance enters automatic collector.
Backwash again after resin adsorption, backwash liquor is different, and the substance being eluted out is also different, and A chromatographic column 13 is anti-using two kinds Washing lotion obtains strong-hydrophobicity acidic materials and strong-hydrophobicity neutral substance, and B chromatographic column 16 is obtained weak hydrophobic using two kinds of backwash liquors The substance of sample bottle 2, is finally separated and enters sample divider not by property neutral substance and weak hydrophobicity acidic materials With in receiving flask.
After each sample separation into, dotted portion in Fig. 1 need to only be changed to required sample bottle and group sub-bottle.The dress Resin cleaning, cleaning systems, sample separation and chromatographic column backwash can be executed automatically by, which setting, takes off, and then reaches and continuously separate multiple samples Purpose.
A kind of method and apparatus of separation of close and distant water component and collection based on on-line checking provided by the utility model, from Dynamicization degree is high, and easy to operate, separating rate is fast, equipment take up space it is small, backwash can real-time monitoring, according in eluent wait divide Concentration signal intensity from component judges automatically elution terminal, realizes the separation and collection of different component.
The de- automated procedures table of the cleaning of 1 resin of table, cleaning systems, sample separation, chromatographic column backwash
1, the automated procedures can reach resin by the on or off of the automatic execution part solenoid valve of computer controlled interface The purpose that cleaning, cleaning systems, sample separation and chromatographic column backwash take off.Wherein:
1. water bottle, sample bottle, organize sub-bottle, A backwash liquor bottle, B backwash liquor bottle by six logical selection valves realize automation cleaning, Sample introduction and backwash.
2. by the on or off of two three-way electromagnetic valves of control, to realize upper sample introduction or lower backwash, to reach backwash automation.
3. can achieve the purpose that collect automatically by the full-automatic collector of Programmable Multifunction.The self-reacting device can root According to the concentration signal intensity of component to be collected in eluent, test tube corresponding to collector is automatically selected, reaches and collect automatically Purpose.The collector is programmable, can according to detector whether appearance, to realize the collection of different test tubes.
4. the automation instrument device can realize that multiple samples continuously separate.It, only need to will be in Fig. 1 after the separation of each sample Dotted portion changes required sample bottle and group sub-bottle into.The device can execute resin cleaning, cleaning systems, sample separation automatically It is de- with chromatographic column backwash, and then achieve the purpose that continuously to separate multiple samples.
2, each component is collected automatically.The self-reacting device can be strong according to the concentration signal of component to be collected in eluent Degree, automatically selects test tube corresponding to collector (receiving flask), achievees the purpose that collect automatically.The collector is programmable, can root According to detector whether appearance, to realize the collection of different test tubes.The UV detector of eluent module after testing, just starts to wash When de-, the concentration signal intensity of component to be collected is stronger, has a very strong ultraviolet absorption peak, these Fraction collections to one In test tube, with the progress of elution, and there is another ultraviolet absorption peak, in these Fraction collections to another test tube, To realize the collection of different test tubes.
3, elution terminal is judged automatically.The accurate judgement of elution terminal is realized by the series connection of multiple on-line checking devices.Inspection Surveying module includes the detectors such as the UV detector being sequentially connected in series, fluorescence detector.The ultraviolet inspection of eluent module after testing Survey device, just start elution when, the concentration signal intensity of component to be collected is stronger, with the progress of elution, component to be collected it is dense It is more and more weaker to spend signal, when concentration signal is less than setting numerical value (common water sample is eluted to absorbance less than 0.06), elution is completed.
4, on-line degassing device.The use of on-line degassing device can increase the separative efficiency of chromatographic column.
5, system separating liquid resid vol is reduced.The introducing of six logical selection valves, three-way magnetic valve, reduces separation system Dead volume (separating liquid resid vol), and reduce the device space.

Claims (4)

1. a kind of separation of close and distant water component and collection device based on on-line checking, which is characterized in that including leading to choosing with six respectively Water bottle (1), the sample bottle (2), group sub-bottle (3), backwash liquor bottle being connected to valve (6), six logical selection valves (6) pass sequentially through online de- Device of air (7) and peristaltic pump (8) are connected with chromatographic column, and chromatographic column is linked in sequence again UV detector (20) and fluorescence detector (21), fluorescence detector (21) is connected separately with full-automatic collector (22) and three-way magnetic valve (23), three-way magnetic valve (23) Two outlet be respectively connected to waste liquid bottle (24) and organize sub-bottle (3).
2. a kind of separation of close and distant water component and collection device based on on-line checking as described in claim 1, which is characterized in that The chromatographic column has 2~3, and each chromatographic column is respectively connected with pressure sensor (12) and two three-way electromagnetic valves, passes through two energization magnetic Valve connects required chromatographic column.
3. a kind of separation of close and distant water component and collection device based on on-line checking as claimed in claim 2, which is characterized in that The six logical selection valve (6), three-way magnetic valve (23) and two three-way electromagnetic valves are connected with control system, and the control system is also divided It is not electric with on-line degassing device (7), peristaltic pump (8), pressure sensor (12), UV detector (20), fluorescence detector (21) Connection.
4. a kind of separation of close and distant water component and collection device based on on-line checking as claimed in claim 3, which is characterized in that The control system includes wriggling pump control module, solenoid valve control module, detector control module, the control of on-line degassing device Module, pressure sensor control module, flow chart of tube display module and LCD touch control module.
CN201821610930.9U 2018-09-30 2018-09-30 A kind of separation of close and distant water component and collection device based on on-line checking Active CN209215064U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109342159A (en) * 2018-09-30 2019-02-15 中国科学院水生生物研究所 A kind of separation of close and distant water component and collection device and method based on on-line checking

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109342159A (en) * 2018-09-30 2019-02-15 中国科学院水生生物研究所 A kind of separation of close and distant water component and collection device and method based on on-line checking

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