CN108786179A - A kind of full-automatic part collection device of column chromatography for separation and method - Google Patents
A kind of full-automatic part collection device of column chromatography for separation and method Download PDFInfo
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- CN108786179A CN108786179A CN201811015091.0A CN201811015091A CN108786179A CN 108786179 A CN108786179 A CN 108786179A CN 201811015091 A CN201811015091 A CN 201811015091A CN 108786179 A CN108786179 A CN 108786179A
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- test tube
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- waste liquid
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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
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/24—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the treatment of the fractions to be distributed
- B01D15/247—Fraction collectors
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/80—Fraction collectors
- G01N30/82—Automatic means therefor
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- Biochemistry (AREA)
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- General Physics & Mathematics (AREA)
- Immunology (AREA)
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- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The invention discloses a kind of full-automatic part collection device of column chromatography for separation and method, including bottom plate, there is test tube disk above bottom plate, rack for test tube is placed with above test tube disk, waste liquid tank is equipped on the left of rack for test tube.Bottom plate and babinet vertical connection, box house is equipped with X-axis slideway, X-axis slideway and Y-axis suspension arm vertical connection, Y-axis slideway is equipped on the right side of Y-axis suspension arm, electromagnetism time switch is connected on Y-axis slideway, the left back top of babinet is equipped with triple valve, and triple valve is equipped with triple valve input terminal, effective liquid output nozzle, waste liquid and exports nozzle.The present invention is designed using square and underslung X-Y move modes, changes pipe registration；It collects solution to detach with circuit, use is safer.By triple valve and control program, waste liquid is automatically flowed into waste liquid tank.By solenoid valve control, prevent from changing the phenomenon of leakage in pipe handoff procedure.The present invention can replace manually to the collection of sample, easy to operate, improve work quality and efficiency, and reduce harm of the organic solvent to experimenter.
Description
Technical field
The invention belongs to full-automatic part assembling sphere more particularly to a kind of full-automatic part collection devices of column chromatography for separation
And method.
Background technology
When the departments such as scientific research, medical treatment, institution of higher learning and industrial enterprise laboratory carry out liquid chromatogram layer analysis；In oil
Chemical field：To just/isoparaffin, paraxylene/other xylene isomers, meta-xylene/other xylene isomers
Separation；In sugar, alcohol separation：Fructose/glucose sugar, sorbitol, mannitol, glucose/oligosaccharide, maltose/oligosaccharide, sucrose/
Fructose, glucose, sucrose/molasses, the separation of xylose/arabinose；In pharmaceuticals industry：Chiral object separation；In Food Chemistry：Fat
Fat acid detaches；In biochemistry：Citric acid, phenylalanine separation；Use column chromatography for separation.When column chromatography for separation is tested,
Generally requiring the interval short time continuously takes many samples, if the frequent condition experiment needs that do manually look at always sampling, sampling
Interval time is shorter, and people's timing sampling error is bigger, cross contamination, or sequence confusion is often caused, to experimental result shadow
Sound is very big.Task efficiency is limited, and people's Long Term Contact organic solvent increases the harm of body.
Invention content
It is an object of the invention to provide a kind of column chromatography for separation to solve the above-mentioned problems and automatically partly collect dress
It sets and method.The technical solution is as follows：
A kind of full-automatic part collection device of column chromatography for separation, including bottom plate, are placed with test tube disk above bottom plate, on test tube disk
Fang Fangyou rack for test tubes, rack for test tube left side are equipped with waste liquid tank.Bottom plate and babinet vertical connection, babinet surface are equipped with liquid crystal display
And button, box house are equipped with X-axis slideway, X-axis slideway and Y-axis suspension arm vertical connection, being equipped with Y-axis on the right side of Y-axis suspension arm slides
Road, connects electromagnetism time switch on Y-axis slideway, and electromagnetism time switch is equipped with that electromagnetism time switch is suitable for reading, under electromagnetism time switch
Mouthful, the left back top of babinet is equipped with triple valve, and triple valve is equipped with triple valve input terminal, effective liquid output nozzle, waste liquid efferent duct
Mouthful, the right back lower place of babinet is equipped with power supply and switch.
The triple valve input terminal waits for that collection liquid body mouth is connected by hose with column chromatography for separation.
The electromagnetism time switch that the electromagnetism time switch is controlled by program；The effective liquid output nozzle by hose with
Electromagnetism time switch is suitable for reading to be connected；Mouth is connected with test tube is collected under the electromagnetism time switch.
The waste liquid output nozzle is connected by hose with waste liquid tank.
The rack for test tube both ends are equipped with handle.
The X-axis slideway includes X lead screws and sliding rail, and X lead screws one end connection X-axis holds piece, and the other end connects X shaft couplings
Device, the X shaft couplings are connected with X stepper motors, and the sliding rail both ends are fixed on X-axis and hold on piece and X shaft couplings, the X lead screws
X sliding blocks are equipped with, the X sliding blocks are equipped with X threaded holes.
The Y-axis suspension arm is fixed on by X threaded holes on X sliding blocks, and sliding rail plays Auxiliary support to Y-axis suspension arm.
The Y-axis slideway includes Y lead screws, and Y lead screws one end connection Y-axis holds piece, and the other end connects Y shaft couplings, the Y
Shaft coupling is connected with Y stepping motor, and the Y lead screws are equipped with Y sliding blocks, and the Y sliding blocks are equipped with Y threaded holes.
The electromagnetism time switch is fixed on by Y threaded holes on Y sliding blocks.
The present invention provides a kind of method that column chromatography for separation is automatically partly collected, using above-mentioned apparatus, including following step
Suddenly：
1. by the power outlet of power-line plug insertion apparatus rear panel, rack for test tube and waste liquid tank are put into test tube disk
In, test tube disk is placed on bottom plate, and it is leaned on into foot to babinet.Column chromatography for separation is waited for that collection liquid body mouth passes through hose and threeway
Valve input terminal is connected, by effective liquid export nozzle by hose with electromagnetism time switch is suitable for reading is connected, waste liquid is exported into nozzle company
Hose is connect to be put into waste liquid tank.
2. turning on the switch, mouth setting first test tube of alignment, setting program under electromagnetism time switch are set gradually into waste liquid
Section time, the acquisition time of each test tube, the test tube quantity collected altogether.
3. starting to collect after setting, what is first started is waste liquid section, at this time triple valve switching three-way valve input terminal with it is useless
Liquid exports nozzle connection, and the waste liquid section time is mainly discharged into including emptying time early period and the early period useless waste collection time
To waste liquid tank.
4. being collection section after waste liquid section, triple valve switching three-way valve input terminal connects with effective liquid output nozzle at this time
Logical, collection liquid instills first test tube from mouth under electromagnetism time switch, after the acquisition time for setting each test tube, electromagnetism
Time switch is moved along Y-axis slideway to second, babinet direction test tube, and so on, until completing Y direction, the last one is tried
Pipe is collected, and then Y-axis suspension arm is moved to second row test tube along X-axis slideway, and mouth alignment second row is last under electromagnetism time switch
One test tube starts to collect from back to front, and electromagnetism time switch running track is serpentine track.When the test tube for completing setting collection
After quantity, collection is automatically stopped, and closes power supply.
Good effect using the above scheme：The present invention can replace manually to the collection of sample, and collect sample more
Precisely, while harm of the organic solvent to experimenter is reduced.
Description of the drawings
This patent is further described with reference to the accompanying drawings and embodiments：
Attached drawing 1 is the overall structure diagram of invention.
Attached drawing 2 is the rear panel schematic diagram of invention.
Attached drawing 3 is the X-axis slideway internal structure schematic diagram of invention.
Attached drawing 4 is the Y-axis slideway internal structure schematic diagram of invention.
In figure：1 button, 2 liquid crystal displays, 3 babinets, 4 bottom plates, 5X axis slideways, 6Y axle suspension hangers, 7Y axis slideways, 8 electromagnetism
Time switch, 9 electromagnetism time switches are suitable for reading, mouth under 10 electromagnetism time switches, 11 rack for test tubes, 12 waste liquid tanks, 13 test tube disks, 14
Hand, 15 triple valves, 16 triple valve input terminals, 17 effectively output nozzle, 18 waste liquids export nozzle, 19 power supplys, 20 switches, 21X steps
Stepper motor, 22X shaft couplings, 23X lead screws, 24 sliding rails, 25X sliding blocks, 26X threaded holes, 27X bearing plates, 28Y stepper motors, 29Y connection
Axis device, 30Y lead screws, 31Y threaded holes, 32Y sliding blocks, 33Y bearing plates.
Specific implementation mode
The invention will be further described below in conjunction with the accompanying drawings, but protection scope of the present invention is not limited to described in embodiment
Content.
Refering to fig. 1 shown in -4, a kind of full-automatic part collection device of column chromatography for separation and method, including bottom plate 4, bottom plate 4
Top is placed with test tube disk 13, and 13 top of test tube disk is placed with rack for test tube 11, and 11 left side of rack for test tube is equipped with waste liquid tank 12.Bottom plate 4 and case
3 vertical connection of body, 3 surface of babinet are equipped with liquid crystal display 2 and button 1, and babinet 3 is internally provided with X-axis slideway 5, X-axis slideway 5
With 6 vertical connection of Y-axis suspension arm, 6 right side of Y-axis suspension arm is equipped with Y-axis slideway 7, electromagnetism time switch 8 is connected on Y-axis slideway 7,
Electromagnetism time switch 8 is equipped with that electromagnetism time switch is suitable for reading 9, mouth 10 under electromagnetism time switch, and 3 left back top of babinet is equipped with triple valve
15, triple valve 15 is equipped with triple valve input terminal 16, effective liquid output nozzle 17, waste liquid and exports nozzle 18, the 3 right back lower place of babinet
Equipped with power supply 19 and switch 20.
The triple valve input terminal 16 waits for that collection liquid body mouth is connected by hose with column chromatography for separation.
The electromagnetism time switch 8 is the electromagnetism time switch controlled by program；Effective liquid output nozzle 17 passes through
Hose is connected with electromagnetism time switch suitable for reading 9；Mouth 10 is connected with test tube is collected under the electromagnetism time switch.
The waste liquid output nozzle 18 is connected by hose with waste liquid tank 12.
11 both ends of the rack for test tube are equipped with handle 14.
The X-axis slideway 5 includes X lead screws 23 and sliding rail 24, and 23 one end of X lead screws connection X-axis holds piece 27, and the other end connects
X shaft couplings 22 are connect, the X shaft couplings 22 are connected with X stepper motors 21, and 24 both ends of the sliding rail are fixed on X-axis and hold piece 27 and X connection
On axis device 22, the X lead screws 23 are equipped with X sliding blocks 25, and the X sliding blocks 25 are equipped with X threaded holes 26.
The Y-axis suspension arm 6 is fixed on by X threaded holes 26 on X sliding blocks 25, and sliding rail 24 plays auxiliary branch to Y-axis suspension arm 6
Support acts on.
The Y-axis slideway 7 includes Y lead screws 30, and 30 one end of Y lead screws connection Y-axis holds piece 33, and the other end connects Y shaft couplings
Device 29, the Y shaft couplings 29 are connected with Y stepping motor 28, and the Y lead screws 30 are equipped with Y sliding blocks 32, are set on the Y sliding blocks 32
There are Y threaded holes 31.
The electromagnetism time switch 8 is fixed on by Y threaded holes 31 on Y sliding blocks 32.
To detect accuracy of the device compared with manual time-keeping samples, column chromatography for separation experiment is carried out below, by Shandong
After more friend's Science and Technology Ltd. NaY types molecular sieves and Tianjin Nan Hua catalyst Co., Ltd NaY type molecular sieve spin dehydrations,
Numbered samples 1,2 respectively carry out the meta-xylene in column chromatography for separation mixed xylenes as adsorbent.
Embodiment 1
The method collected using the full-automatic part collection device of column chromatography for separation of the present invention, column chromatography for separation experiment are used
Meta-xylene in 1 separating mixed dimethyl of sample, experiment condition：165 DEG C, pressure 0.5Mpa of reaction temperature, parsing agent are first
Benzene, parsing agent flow velocity are 1ml/min.Specific implementation step is as follows：The power supply 19 of power-line plug insertion apparatus rear panel is inserted
In seat, rack for test tube 11 and waste liquid tank 12 are put into test tube disk 13, test tube disk 13 is placed on bottom plate 4, and it is leaned on to babinet 3
Foot.Column chromatography for separation is waited for that collection liquid body mouth is connected by hose with triple valve input terminal 16, effective liquid output nozzle 17 is led to
It crosses hose with electromagnetism time switch suitable for reading 9 to be connected, waste liquid output 18 connection flexible pipe of nozzle is put into waste liquid tank 12.It turns on the switch
20, by the setting of mouth 10 first test tube of alignment under electromagnetism time switch, setting program, it is 10min that the waste liquid section time is arranged first,
The time that each test tube is collected is 2min, sets 60 test tubes altogether, starts to collect after setting, and what is first started is waste liquid section,
15 switching three-way valve input terminal 16 of triple valve is connected to waste liquid output nozzle 18 at this time, and the waste liquid section time includes mainly emptying early period
Time and useless waste collection time early period, it is discharged into waste liquid tank 12.It is collection section after waste liquid section, triple valve at this time
15 switching three-way valve input terminals 16 are connected to effective liquid output nozzle 17, and collection liquid instills first from mouth 10 under electromagnetism time switch
A test tube, after 2min, electromagnetism time switch 8 is moved along Y-axis slideway 7 to second, 3 direction of babinet test tube, and so on, until
Y direction the last one test tube collection is completed, then Y-axis suspension arm 6 is moved to second row test tube, electromagnetism timing along X-axis slideway 5
The last one test tube of the lower alignment second row of mouth 10 of switch starts to collect from back to front, and 8 running track of electromagnetism time switch is snakelike
Track.After 60 test tubes have been collected, collection is automatically stopped, and is turned off the switch 20, is analyzed sample successively, disposes waste liquid, cleaning examination
Pipe, and separating degree is calculated by separating degree calculation formula R=2 (tR2-tR1)/(W1+W2), separating degree result of calculation is shown in Table 1.
Embodiment 2
Operating procedure is same as Example 1, and difference lies in parsing agent flow velocitys to be changed to 2ml/min；When the collection of each test tube
Between be changed to 1min.Separating degree result of calculation is shown in Table 1.
Embodiment 3
Operating procedure is same as Example 1, and difference lies in parsing agent flow velocitys to be changed to 4ml/min；When the collection of each test tube
Between be changed to 0.5min.Separating degree result of calculation is shown in Table 1.
Embodiment 4
Operating procedure is same as Example 1, and difference lies in samples 1 to change sample 2 into.Separating degree result of calculation is shown in Table 1.
Embodiment 5
Operating procedure is same as Example 2, and difference lies in samples 1 to change sample 2 into.Separating degree result of calculation is shown in Table 1.
Embodiment 6
Operating procedure is same as Example 3, and difference lies in samples 1 to change sample 2 into.Separating degree result of calculation is shown in Table 1.
Comparative example 1
The receiving time for testing reaction condition and each step is same as Example 1, and difference lies in received using manual time-keeping
Collect sample, separating degree result of calculation is shown in Table 1.
Comparative example 2
The receiving time for testing reaction condition and each step is same as Example 2, and difference lies in received using manual time-keeping
Collect sample, separating degree result of calculation is shown in Table 1.
Comparative example 3
The receiving time for testing reaction condition and each step is same as Example 3, and difference lies in received using manual time-keeping
Collect sample, separating degree result of calculation is shown in Table 1.
Comparative example 4
The receiving time for testing reaction condition and each step is same as Example 4, and difference lies in received using manual time-keeping
Collect sample, separating degree result of calculation is shown in Table 1.
Comparative example 5
The receiving time for testing reaction condition and each step is same as Example 5, and difference lies in received using manual time-keeping
Collect sample, separating degree result of calculation is shown in Table 1.
Comparative example 6
The receiving time for testing reaction condition and each step is same as Example 6, and difference lies in received using manual time-keeping
Collect sample, separating degree result of calculation is shown in Table 1.
Table 1
As can be seen from Table 1 under same experimental conditions, is automatically partly collected and filled using column chromatography for separation of the present invention
The method of collection is set than the method separating degree higher that manual time-keeping is collected, with the increase of parsing agent flow velocity, human error also exists
Increase, separating degree gap is also being continuously increased.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of full-automatic part collection device of column chromatography for separation, it is characterised in that：Including bottom plate (4), it is placed with above bottom plate (4)
Test tube disk (13), test tube disk (13) top are placed with rack for test tube (11), waste liquid tank (12) are equipped on the left of rack for test tube (11)；Bottom plate (4)
Side and babinet (3) bottom vertical connection, babinet (3) surface are equipped with liquid crystal display (2) and button (1), babinet (3) top
It is internally provided with X-axis slideway (5), X-axis slideway (5) and Y-axis suspension arm (6) vertical connection, being equipped with Y-axis on the right side of Y-axis suspension arm (6) slides
Road (7), connection electromagnetism time switch (8) on Y-axis slideway (7), electromagnetism time switch (8) be equipped with electromagnetism time switch (9) suitable for reading,
Mouth (10) under electromagnetism time switch, babinet (3) left back top are equipped with triple valve (15), and triple valve (15) is inputted equipped with triple valve
(16), effective liquid output nozzle (17), waste liquid output nozzle (18), babinet (3) right back lower place is held to be equipped with power supply (19) and switch
(20)。
2. the full-automatic part collection device of a kind of column chromatography for separation according to claim 1, it is characterised in that：The threeway
Valve input terminal (16) waits for that collection liquid body mouth is connected by hose with column chromatography for separation.
3. the full-automatic part collection device of a kind of column chromatography for separation according to claim 1, it is characterised in that：The electromagnetism
Time switch (8) is the electromagnetism time switch controlled by program；Effective liquid output nozzle (17) is fixed by hose and electromagnetism
Shi Kaiguan (9) suitable for reading is connected；Mouth (10) is connected with test tube is collected under the electromagnetism time switch.
4. the full-automatic part collection device of a kind of column chromatography for separation according to claim 1, it is characterised in that：The waste liquid
Output nozzle (18) is connected by hose with waste liquid tank (12).
5. the full-automatic part collection device of a kind of column chromatography for separation according to claim 1, it is characterised in that：The test tube
Frame (11) both ends are equipped with handle (14).
6. the full-automatic part collection device of a kind of column chromatography for separation according to claim 1, it is characterised in that：The X-axis
Slideway (5) includes X lead screws (23) and sliding rail (24), and X lead screws (23) one end connection X-axis holds piece (27), and the other end connects X connection
Axis device (22), the X shaft couplings (22) are connected with X stepper motors (21), and sliding rail (24) both ends are fixed on X-axis and hold piece (27)
On X shaft couplings (22), the X lead screws (23) are equipped with X sliding blocks (25), and the X sliding blocks (25) are equipped with X threaded holes (26).
7. the full-automatic part collection device of a kind of column chromatography for separation according to claim 7, it is characterised in that：The Y-axis
Suspension arm (6) is fixed on by X threaded holes (26) on X sliding blocks (25), and sliding rail (24) plays Auxiliary support to Y-axis suspension arm (6) and makees
With.
8. the full-automatic part collection device of a kind of column chromatography for separation according to claim 1, it is characterised in that：The Y-axis
Slideway (7) includes Y lead screws (30), and Y lead screws (30) one end connection Y-axis holds piece (33), and the other end connects Y shaft couplings (29),
The Y shaft couplings (29) are connected with Y stepping motor (28), and the Y lead screws (30) are equipped with Y sliding blocks (32), the Y sliding blocks (32)
It is equipped with Y threaded holes (31).
9. the full-automatic part collection device of a kind of column chromatography for separation according to claim 8, it is characterised in that：The electromagnetism
Time switch (8) is fixed on by Y threaded holes (31) on Y sliding blocks (32).
10. a kind of full-automatic part collection method of column chromatography for separation, which is characterized in that use claim 1-9 any one institute
The device stated, includes the following steps：
1. by power supply (19) socket of power-line plug insertion apparatus rear panel, rack for test tube (11) and waste liquid tank (12) are put into
In test tube disk (13), test tube disk (13) is placed on bottom plate (4), and it is leaned on into foot to babinet (3)；Column chromatography for separation is waited collecting
Liquid port is connected by hose with triple valve input terminal (16), and effective liquid output nozzle (17) is opened by hose and electromagnetism timing
It shuts mouth (9) to be connected, waste liquid output nozzle (18) connection flexible pipe is put into waste liquid tank (12)；
2. turning on the switch (20), mouth (10) setting first test tube of alignment, setting program under electromagnetism time switch are set gradually
Waste liquid section time, the acquisition time of each test tube, the test tube quantity collected altogether；
3. starting to collect after setting, what is first started is waste liquid section, at this time triple valve (15) switching three-way valve input terminal (16)
Be connected to waste liquid output nozzle (18), the waste liquid section time is mainly including emptying time early period and when useless waste collection early period
Between, it is discharged into waste liquid tank (12)；
4. being collection section after waste liquid section, triple valve (15) switching three-way valve input terminal (16) exports nozzle with effective liquid at this time
(17) it is connected to, collection liquid instills first test tube from mouth (10) under electromagnetism time switch, by the acquisition time for setting each test tube
After, electromagnetism time switch (8) is moved along Y-axis slideway (7) to second, babinet (3) direction test tube, and so on, until complete
It is collected at the last one test tube of Y direction, then Y-axis suspension arm (6) is moved to second row test tube along X-axis slideway (5), and electromagnetism is fixed
The last one test tube of mouth (10) alignment second row starts to collect from back to front under Shi Kaiguan, electromagnetism time switch (8) running track
For serpentine track；After completing the test tube quantity of setting collection, collection is automatically stopped, and closes power supply.
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| CN201811015091.0A CN108786179A (en) | 2018-08-31 | 2018-08-31 | A kind of full-automatic part collection device of column chromatography for separation and method |
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| CN201811015091.0A CN108786179A (en) | 2018-08-31 | 2018-08-31 | A kind of full-automatic part collection device of column chromatography for separation and method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111643928A (en) * | 2020-06-12 | 2020-09-11 | 中国地质大学（武汉） | Automatic solid phase extraction device |
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| CN207730517U (en) * | 2017-12-28 | 2018-08-14 | 上海屹尧仪器科技发展有限公司 | A kind of multichannel sample automatic classification collection and constant volume for large volume Solid Phase Extraction concentrates structure |
| CN207764244U (en) * | 2017-12-28 | 2018-08-24 | 北京同信天博科技发展有限公司 | A kind of automatic fluid injector |
| CN208823983U (en) * | 2018-08-31 | 2019-05-07 | 中触媒新材料股份有限公司 | A kind of full-automatic part collection device of column chromatography for separation |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111643928A (en) * | 2020-06-12 | 2020-09-11 | 中国地质大学（武汉） | Automatic solid phase extraction device |
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