CN109954297A - Washing device and application thereof - Google Patents
Washing device and application thereof Download PDFInfo
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- CN109954297A CN109954297A CN201910221251.5A CN201910221251A CN109954297A CN 109954297 A CN109954297 A CN 109954297A CN 201910221251 A CN201910221251 A CN 201910221251A CN 109954297 A CN109954297 A CN 109954297A
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- eluent
- triple valve
- washing device
- elution
- storage tank
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/42—Selective adsorption, e.g. chromatography characterised by the development mode, e.g. by displacement or by elution
- B01D15/424—Elution mode
-
- 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
- G01N1/4005—Concentrating samples by transferring a selected component through a membrane
-
- 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
- G01N1/4005—Concentrating samples by transferring a selected component through a membrane
- G01N2001/4011—Concentrating samples by transferring a selected component through a membrane being a ion-exchange membrane
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The present invention provides a kind of washing device and application thereof.Washing device of the invention includes sequentially connected the first storage tank of eluent, accurate liquid feeding pump, elution column, the first triple valve, discharge liquor force (forcing) pump, the second triple valve and sample receiver, wherein the second triple valve further connects the second storage tank of eluent, first triple valve is provided with pressure balance interface, and elution column is provided with charging interface.In this washing device, eluent to be pumped into rate equal with the discharge rate of eluate.This washing device is applied to separation and the analysis field of object, the accuracy for dividing object the analysis of variance using elution method can be improved.
Description
Technical field
The present invention relates to separator technical fields, more particularly, to a kind of washing device and application thereof.
Background technique
Elution method is also known as elution method, and sample is added in one end of elution column, and mobile phase continues through the stationary phase in elution column,
Each component successively washes out from stationary phase and obtains enrichment and separation in sample.
Elution is widely used in the fields such as biochemistry, nuclear energy, chemical industry, drug testing, not only can be used for preparing product, but also can be with
For analyzing sample.When for example, by using ion exchange resin separating zirconium, hafnium, two-phase partitioning system of the zirconium in separation resin and solution
Number is different, then is separated using the method eluted to ion exchange resin to the mixed solution of zirconium, hafnium；Pseudoephedrine
It is the raw material for preparing crystal methamphetamine, using the pseudoephedrine in the method analysis suspicious specimen of column chromatography；Grape wine and white wine
In there are many flavor substance, these flavor substances are separated and are measured using the method for column chromatography.When elution, eluent exists
Pressure drop in elution column changes with the progress of elution, and eluent will occur from flow when eluting the outflow in column
Variation or even eluent discharge rate are less than the feed rate of eluent, lead to elution process failure and then lead to object
Dividing the analysis of variance, there are comparable errors, mistake that is unsuccessful when perhaps leading to amplify separation equipment or leading to analysis result.
The discharge rate matched requirement of the feed rate and eluent of eluent when dividing the analysis of variance to elution to meet,
The stability of eluent discharge rate from elution column is improved, the present invention is specifically proposed.
Summary of the invention
One of the objects of the present invention is to provide a kind of washing devices, to match eluent to greatest extent from elution column
The feed rate of discharge rate and eluent into elution column, improves the stability of eluent flow velocity rate from elution column, into
And improve the accuracy for dividing object the analysis of variance.
Washing device of the invention includes sequentially connected the first storage tank of eluent, accurate liquid feeding pump, elution column, the one or three
Port valve, discharge liquor force (forcing) pump, the second triple valve and sample receiver, wherein second triple valve further connects eluent
Two storage tanks, first triple valve are provided with pressure balance interface, and the elution column is provided with charging interface.Each portion of the invention
It can be connected by associated ping between part.
In certain embodiments, first storage tank of eluent elutes preceding liquid for storing.
In certain embodiments, the accurate liquid feeding pump is used to adjust pressure and stream of the eluent when entering elution column
Amount；Preferably, accurate liquid feeding pump uses the pump of stability of flow.
In certain embodiments, it is the equipment used that the elution column, which is for eluting target components, and it includes be used for
Elute the filler of target components.And the charging interface is set to the top of the elution column, for loading liquid to be separated
Body.
In certain embodiments, first triple valve is eluted for adjusting the eluent rate of outflow, and for eliminating
Siphonic effect in the process.
In certain embodiments, the pressurization when discharge liquor force (forcing) pump is for eluent outflow elution column；Preferably,
Discharge liquor force (forcing) pump uses the pump of stability of flow；Preferably, discharge liquor force (forcing) pump uses peristaltic pump；Preferably, discharge liquor is pressurizeed
The flow of pump is more than or equal to the flow of accurate liquid feeding pump；Preferably, the flow of discharge liquor force (forcing) pump is equal to the stream of accurate liquid feeding pump
Amount.
In certain embodiments, second triple valve is used for respectively to the second storage tank of eluent and/or sample reception
Device imports eluent；Preferably, the second triple valve is solenoid valve；Preferably, the second triple valve is in the state of no power, elution
Liquid is exported through the second triple valve to the second storage tank of eluent, and is not exported to sample receiver；Preferably, the second triple valve is logical
In the state of electricity, eluent is exported through the second triple valve to sample receiver, and is not exported to the second storage tank of eluent.
In certain embodiments, the sample receiver is used to collect the eluent as sample.
In certain embodiments, second storage tank of eluent is used to collect the eluent not as sample.
The second object of the present invention is to provide purposes of the mentioned-above washing device in terms of dividing the analysis of variance.Invention
People's discovery, the apparatus structure is simple, at low cost, in separation and analytic process, it is easy to realize eluent discharge rate and wash
The feed rate of de- liquid is equal, and is able to maintain elution rate and stablizes.
Compared with prior art, the present invention obtains at least one of following beneficial effect:
1, washing device of the present invention can effectively realize eluent discharge rate and eluent from elution column
Feed rate it is equal.
2, washing device of the present invention can effectively realize the stability of eluent discharge rate from elution column.
Detailed description of the invention
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art
Embodiment or attached drawing needed to be used in the description of the prior art be briefly described, it should be apparent that, it is described below
Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor
It puts, is also possible to obtain other drawings based on these drawings.
Fig. 1 is a kind of washing device schematic diagram proposed by the present invention.
The elution curve (elution rate 2.0mL/min) of Fig. 2 LaCePrNd.
The elution curve (elution rate 3.0mL/min) of Fig. 3 zirconium, hafnium.
The elution curve (elution rate 4.0mL/min) of Fig. 4 zirconium, hafnium.
The elution curve (elution rate 1.0mL/min) of Fig. 5 LaCePrNd.
Description of symbols: the first storage tank of 1- eluent；2- precision liquid feeding pump；3- elutes column；The first triple valve of 4-；5- row
Liquid force (forcing) pump out；The second triple valve of 6-；The second storage tank of 7- eluent；8- sample receiver；9- pressure balance interface；10- charging
Interface.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific
Condition person carries out according to conventional conditions or manufacturer's recommended conditions.
In the present invention, if without particularly illustrating, all embodiments mentioned in this article and preferred implementation method
It can be combined with each other to form new technical solution.
In the present invention, if without particularly illustrating, all technical characteristics and preferred feature mentioned in this article can be with
Intercombination forms new technical solution.
In the present invention, if percentage (%) or part refer to the weight relative to composition without particularly illustrating
Percentage or parts by weight.
In the present invention, if related each component or its preferred ingredient can be combined with each other shape without particularly illustrating
The technical solution of Cheng Xin.
In the present invention, unless otherwise indicated, numberical range " a~b " indicates the contracting of any real combinings between a to b
Sketch form shows that wherein a and b is real number.Such as numberical range " 6~22 " indicate herein all listed " 6~22 " it
Between whole real numbers, " 6~22 " be these combinations of values breviary indicate.
" range " disclosed in this invention can be respectively one or more lower limits and one in the form of lower and upper limit
A or multiple upper limits.
Unless otherwise indicated, profession used herein and meaning phase known to scientific term and one skilled in the art
Together.In addition, any method similar to or equal to what is recorded or material can also be applied in the present invention.
Washing device
In one aspect of the invention, the present invention provides a kind of washing device, which includes being sequentially connected ground eluent
First storage tank 1, accurate liquid feeding pump 2, elution column 3, the first triple valve 4, discharge liquor force (forcing) pump 5, the second triple valve 6 and sample reception
Device 8, the second triple valve 6 further connect the second storage tank of eluent 7.It is provided with pressure balance interface 9 on the first triple valve 4,
Charging interface 10 is provided on elution column 3 simultaneously.Inventors have found that being pumped into rate and washing for eluent can be made using the device
The discharge rate of de- liquid is completely the same, to improve the stability of eluent discharge rate to greatest extent, raising is separated, analyzed
As a result accuracy is conducive to propose that separation equipment accurately amplifies requirement, is conducive to propose the differentiation to the data of analysis.
In certain embodiments of the present invention, the eluent is determined according to the property of system to be separated.As a result,
Eluent is pumped into elution column from the entrance of elution column, and eluent is from the outlet outflow elution column of elution column, in eluent from elution
Column outlet outflow elution column when, in such a way that discharge liquor force (forcing) pump and the first triple valve combine, maintain eluent from
Elute the stability when outlet outflow of column.
In certain embodiments of the present invention, the elution column is determined according to the property of system to be separated.It is all
The material that physics, chemical action does not occur with the filler and eluent eluted in column is used equally for manufacture elution column.Ordinary circumstance
Under, glass, PVC, PMMA, stainless steel etc. are used equally for manufacture elution column.Flow direction of the eluent in elution column both can be with
It from top to down, and can be from below to up.
It in certain embodiments of the present invention, include filler in the elution column, these fillers are according to be separated
What the property of system determined.For example, for the separation of elements multiple for rare earth, it is general to be made using the substance with extraction ability
It is different from filler binding ability according to the different elements of rare earth for filler, rare earth element is eluted using corresponding strip liquor；It is right
In zirconium, hafnium separation for, can using D296 strong-base anion-exchange resin be used as filler, using sulfuric acid solution conduct wash
The separation of zirconium, hafnium may be implemented according to the difference that zirconium, hafnium and D296 strong-base anion-exchange resin interact in de- liquid.
The precision liquid feeding pump refers to an accurate feed liquor pumping system, can be by conventional pump, flow measurement device, pressure
Metering device composition, accurate feed liquor pumping system are capable of providing accurate flow and accurate pressure.In implementation of the invention
In example, accurate liquid feeding pump is using Sanotac pump (model: MPF0102C), this pump can control flow, to the liquid of outlet
Body carries out pressure measurement, and has over-voltage protecting function.But this is not indicated, can only implement this hair using the pump of this model
It is bright.
Gear pump, plunger pump, peristaltic pump etc. can be used in the discharge liquor force (forcing) pump.In operating process, discharge liquor pressurization
The flow of pump is more than or equal to the flow of accurate liquid feeding pump.In an embodiment of the present invention, using peristaltic pump (longer,
BT100-2J).But this is not indicated, can only implement the present invention using the peristaltic pump of this model.
Three-way solenoid valve can be used in second triple valve, and manually-operated triple valve also can be used.In the present invention
Embodiment in, use three-way solenoid valve (Jinan Yun Cheng instrument, FQY22).When no power, the entrance of solenoid valve, with eluent
Second storage tank communicates, and is not communicated with sample receiver；When energization, the entrance of solenoid valve is communicated with sample receiver, with eluent
Second storage tank is not communicated with.But this is not indicated, can only implement the present invention using the solenoid valve of this model.
The sample receiver refers to utensil at the appointed time with sample reception function.It can use and manually exist
The specified time carries out reception sample from sample outlet, can also carry out reception sample in conjunction with existing instrument and equipment.At this
In the embodiment of invention, sample receiver uses automatic fraction collector (the limited public affairs of Shanghai fine jade spy's analysis instrument of simple reformation
Department, BSZ-100-LCD).But this is not indicated, can only implement the present invention using the sample receiver of this model.
The purposes of washing device
In another aspect of this invention, the purposes the present invention provides a kind of washing device in terms of dividing the analysis of variance.This
The purposes of invention preferably can be regarded as the method for separating using washing device and analyzing substance or mixture.Inventors have found that should
Apparatus structure is simple, at low cost, and the discharge rate of eluent is stablized during elution, especially suitable for research elution process
The data of amplification rule and accurate discriminant analysis.
Present invention will be further explained by specific examples below, it should be understood, however, that, these embodiments are only
It is used, is but should not be understood as present invention is limited in any form for being described in more detail.
Embodiment 1
A set of washing device is assembled according to Fig. 1.Elution column material is transparent PVC pipe, pvc pipe diameter 50mm, high 1600mm.
The filler in column is eluted using the microballoon of four kinds of rare earth elements (lanthanum: cerium: praseodymium: neodymium (molar ratio)=1:1:1:1) of load.Eluent
For the hydrochloric acid solution of 3.0mol/L.Operating condition is set as the feed rate 2.0mL/min of hydrochloric acid solution, and sample receiver is every
6.0mL sample (the second triple valve energization 3.0min) is received every 10min.Under conditions of 25 ± 1 DEG C, by the elution of 2.0hr
Afterwards, above-mentioned four kinds of rare earths are totally separated from, and the separating resulting of above-mentioned four kinds of rare earth elements is as shown in Figure 2.
Embodiment 2
A set of washing device is assembled according to Fig. 1.Elution column material is transparent PVC pipe, pvc pipe diameter 50mm, high 1600mm.
Filler in elution column is using the D296 strong-base anion-exchange resin for having loaded two kinds of zirconium, hafnium elements to be separated.Eluent
For 20% sulfuric acid solution.Operating condition is set as the feed rate 3.0mL/min of sulfuric acid solution, sample receiver be every
10min receives 6.0mL sample (the second triple valve energization 2.0min).Under conditions of 25 ± 1 DEG C, after the elution of 5.0hr,
Zirconium, hafnium are totally separated from, and in eluent flow rate 3.0mL/min, zirconium, the elution result of hafnium are as shown in Figure 3.
Embodiment 3
A set of washing device is assembled according to Fig. 1.Elution column material is transparent PVC pipe, pvc pipe diameter 50mm, high 1600mm.
Filler in elution column is using the D296 strong-base anion-exchange resin for having loaded two kinds of zirconium, hafnium elements to be separated.Eluent
For 20% sulfuric acid solution.The base buret that first pressure-measuring pipe and the second pressure-measuring pipe are all made of 50mL is vertically arranged, and is surveyed pressure and is situated between
Matter uses pure water (density 0.98).Operating condition is set as the feed rate 4.0mL/min of sulfuric acid solution, and sample receiver is
4.0mL sample (the second triple valve energization 1.0min) is received every 10min.It is steady in the flow that eluent entrance and eluent export
Periodically, eluent inlet pressure 24.0cm water column higher than eluent outlet pressure is measured.In eluent flow rate 4.0mL/min,
Zirconium, the elution result of hafnium are as shown in Figure 4.
Embodiment 4
A set of washing device with drop measurement function is assembled according to Fig. 1.Elution column material is transparent PVC pipe, pvc pipe
Diameter 50mm, high 1600mm.The base buret that first pressure-measuring pipe and the second pressure-measuring pipe are all made of 50mL is vertically arranged, and is surveyed pressure and is situated between
Matter uses pure water (density 0.98).The filler in column is eluted using four kinds of rare earth element (lanthanums: cerium: praseodymium: neodymium (molar ratio) of load
=1:1:1:1) microballoon.Eluent is the hydrochloric acid solution of 3mol/L.Operating condition is set as the feed rate of hydrochloric acid solution
1.0mL/min, sample receiver are to receive 6.0mL sample (the second triple valve energization 6.0min) every 10min.Enter in eluent
When mouth and the stability of flow of eluent outlet, eluent inlet pressure 10.0cm water column higher than eluent outlet pressure is measured.?
When eluent flow rate 1.0mL/min, lanthanum, cerium, praseodymium, the elution result of neodymium are as shown in Figure 5.
Although illustrate and describing the present invention with specific embodiment, it will be appreciated that without departing substantially from of the invention
Many other change and modification can be made in the case where spirit and scope.It is, therefore, intended that in the following claims
Including belonging to all such changes and modifications in the scope of the invention.
Claims (10)
1. a kind of washing device, which is characterized in that it includes sequentially connected the first storage tank of eluent, accurate liquid feeding pump, elution
Column, the first triple valve, discharge liquor force (forcing) pump, the second triple valve and sample receiver, wherein second triple valve further connects
The second storage tank of eluent is connect, first triple valve is provided with pressure balance interface, and the elution column is provided with charging interface.
2. washing device according to claim 1, which is characterized in that before first storage tank of eluent is for storing elution
Liquid.
3. washing device according to claim 1, which is characterized in that it is described precision liquid feeding pump for adjust eluent into
Pressure and flow when entering to elute column；
Preferably, the accurate liquid feeding pump uses the pump of stability of flow.
4. washing device according to claim 1, which is characterized in that the elution column includes for eluting target components
Filler, and the charging interface is set to the top of the elution column, for loading liquid to be separated.
5. washing device according to claim 1, which is characterized in that first triple valve is used to adjust the stream of eluent
Speed out, and for eliminating the siphonic effect in elution process.
6. washing device according to claim 1, which is characterized in that the discharge liquor force (forcing) pump is washed for eluent outflow
Pressurization when de- column.
7. washing device according to claim 1, which is characterized in that second triple valve is used for respectively to the elution
The second storage tank of liquid and/or the sample receiver import eluent；
Preferably, second triple valve is solenoid valve；
Preferably, in the state of no power, eluent is exported through second triple valve to described and is washed second triple valve
De- the second storage tank of liquid, and do not export to the sample receiver；
Preferably, in the state of energization, eluent is exported through second triple valve to the sample second triple valve
Receiver, and do not export to second storage tank of eluent.
8. washing device according to claim 1, which is characterized in that the sample receiver is for collecting as sample
Eluent.
9. washing device according to claim 1, which is characterized in that second storage tank of eluent for collect not as
The eluent of sample.
10. purposes of -9 described in any item washing devices in substance separation and analysis field according to claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910221251.5A CN109954297B (en) | 2019-03-22 | 2019-03-22 | Elution device and use thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910221251.5A CN109954297B (en) | 2019-03-22 | 2019-03-22 | Elution device and use thereof |
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| Publication Number | Publication Date |
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| CN109954297A true CN109954297A (en) | 2019-07-02 |
| CN109954297B CN109954297B (en) | 2021-12-14 |
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| CN201910221251.5A Active CN109954297B (en) | 2019-03-22 | 2019-03-22 | Elution device and use thereof |
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Citations (5)
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| US20090186374A1 (en) * | 2008-01-23 | 2009-07-23 | Etogen Scientific | Apparatus for measuring effect of test compounds on biological objects |
| CN103694311A (en) * | 2013-12-05 | 2014-04-02 | 成都雅途生物技术有限公司 | Chromatography device for purifying protein |
| CN203941163U (en) * | 2014-06-19 | 2014-11-12 | 深圳市凯特生物医疗电子科技有限公司 | A kind of glycolated hemoglobin analysis liquid road |
| CN205435056U (en) * | 2016-02-05 | 2016-08-10 | 北京创新通恒科技有限公司 | Chromatographically pure piece -rate system |
| CN205656174U (en) * | 2016-05-25 | 2016-10-19 | 中南大学 | System for be used for detecting trace metal ion content |
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2019
- 2019-03-22 CN CN201910221251.5A patent/CN109954297B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090186374A1 (en) * | 2008-01-23 | 2009-07-23 | Etogen Scientific | Apparatus for measuring effect of test compounds on biological objects |
| CN103694311A (en) * | 2013-12-05 | 2014-04-02 | 成都雅途生物技术有限公司 | Chromatography device for purifying protein |
| CN203941163U (en) * | 2014-06-19 | 2014-11-12 | 深圳市凯特生物医疗电子科技有限公司 | A kind of glycolated hemoglobin analysis liquid road |
| CN205435056U (en) * | 2016-02-05 | 2016-08-10 | 北京创新通恒科技有限公司 | Chromatographically pure piece -rate system |
| CN205656174U (en) * | 2016-05-25 | 2016-10-19 | 中南大学 | System for be used for detecting trace metal ion content |
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