CN104407083B - Full-automatic piece-rate system and the application in edible oil polar compound separates thereof - Google Patents
Full-automatic piece-rate system and the application in edible oil polar compound separates thereof Download PDFInfo
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- CN104407083B CN104407083B CN201410709516.3A CN201410709516A CN104407083B CN 104407083 B CN104407083 B CN 104407083B CN 201410709516 A CN201410709516 A CN 201410709516A CN 104407083 B CN104407083 B CN 104407083B
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Abstract
The present invention provides a kind of full-automatic segregation apparatus and the application in edible oil polar compound separates thereof, and described full-automatic segregation apparatus includes automatic sample handling system 100, post switched system 200, automatic separation system 300 and temperature control system 400.When using assembly of the invention that edible oil polar compound is separated, auto injection can be realized and chromatographic column automatically switches, the multiple sample of continuous processing, it is achieved high flux sharp separation；Meanwhile, sample introduction, post switching, separation component are collected and are used full Mechanical course, it is to avoid the anthropic factor impact on experiment, on-line ultraviolet monitoring, flow velocity from dynamic(al) correction, make testing result accurately, stable.
Description
Technical field
The present invention relates to Chemical Decomposition detection field, particularly relate to a kind of full-automatic piece-rate system and at edible oil
Application in polar compound separation.
Technical background
Use the artificial mode that separate currently for separating of polar compound in detection sample more, such as, be used for examining
Survey the method for edible oil polar compound mainly according to " GB/T 5009.202-2003 edible vegetable oil frying process
In the mensuration of polar compound (PC) ", separated by silica gel column chromatography, the polarity group in TLC detection oils and fats
Point.Its principle is: the oils and fats of frying is by equipped with when having adsorbed the silicagel column of certain moisture, washing of flowing phase
Taking off, triglyceride therein (i.e. through frying unchanged oils and fats) is first eluted and flows out spectrum post；Fling to
Eluant, weighs, is the quality of non-polar component, deducts the matter of non-polar component by the quality of upper prop sample
Amount is exactly the quality (there occurs the oils and fats of chemical change after frying) of polar compound.But, conventional post chromatography by
In fully relying on manual operations, the not only waste of manpower of staff coutroi velocity, also result in unstable result simultaneously,
Poor reproducibility；After column chromatography for separation terminates, needing dependence TLC to verify separating effect, so operation is the most numerous
Trivial, generally require through being repeated several times operation, can be only achieved desired separated effect, cause separating effect checking stagnant
After；Additionally, traditional method dress post pre-treatment, need to spend 1 day by silicon particle drying and control water content, then
People frock post half an hour, column chromatography for separation process-field controls to need 1 hour, also wants TLC checking separating effect to need partly
Hour, the most time-consuming.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, it is provided that a kind of full-automatic segregation apparatus, it is possible to accurate, real-time,
Quickly component, particularly polar compound in sample are separated.
The present invention a further object is a kind of method providing edible oil polar compound to separate, it is to avoid existing people
Accuracy and the problem of poor reproducibility in work operational approach.
For achieving the above object, the present invention provides a kind of full-automatic segregation apparatus, including automatic sample handling system, post
Switched system and automatic separation system；
Described automatic sample handling system includes the first pump machanism, six-way injection valve, the first multiplexer channel selector valve and
First electrical control mechanism, described six-way injection valve with quantitative loop, described first pump machanism and six-way injection valve pipeline
Connect；
Described post switched system includes the second multiplexer channel selector valve, the 3rd multiplexer channel selector valve, column holder machine
Structure and the second electrical control mechanism, described column holder mechanism is used for placing chromatographic column, and described second multiplexer channel selects
Valve and the 3rd multiplexer channel selector valve lay respectively at the first upper and lower both sides of column holder mechanism, and the second multiplexer channel selects
Valve is connected with six-way injection valve pipeline；
Described automatic separation system include the second pump machanism, detector, automatic collector, the 3rd electrical control mechanism with
And industrial computer, described second pump machanism is connected with six-way injection valve and the 3rd multiplexer channel selector valve pipeline respectively.
Preferably, described full-automatic segregation apparatus also includes temperature control system, described temperature control system bag
Include refrigeration mechanism and the 4th electrical control mechanism.
Preferably, described refrigeration mechanism includes semiconductor chilling plate, cold temperature groove and fan, described semiconductor refrigerating
Cold temperature groove is freezed by sheet, and the radiating surface of cooling piece is dispelled the heat by described fan.
Preferably, described full-automatic segregation apparatus also includes motor, by motor drive pump machanism,
Six-way injection valve, multiplexer channel selector valve.
Preferably, described first pump machanism includes that syringe pump and three-way valve, described syringe pump and three-way valve pipeline are even
Connecing, described three-way valve is connected with waste liquid barrel pipeline.
Preferably, described second pump machanism includes valveless metering pump.
Preferably, described detector is UV-detector.
Preferably, described first column holder mechanism is slide rail type upper and lower scalable column holder.
Preferably, described automatic collector includes X/Y axle two dimension autonomous movement positioner, arrangement for adjusting height
With catcher pallet, described catcher pallet arranges liquid leakage tank and flow-guiding channel.
Preferably, described full-automatic segregation apparatus also includes earth leakage circuit-breaker.
Preferably, described full-automatic segregation apparatus also includes that solvent barrel detects device.When nothing in solvent barrel being detected
During solvent, system halt runs, and audio alert.
In a kind of specific embodiment, described solvent barrel detection device includes photoelectric sensor, described photoelectricity
Sensor includes light source transmitting terminal and light source receiving terminal, and described light source transmitting terminal and light source receiving terminal are positioned at solvent
Pipeline two ends above Tong.When there being liquid in pipeline, photoelectric sensor output high level, when not having in pipeline
During liquid, photoelectric sensor output low level.
In a kind of specific embodiment, described solvent barrel detection device includes pressure transducer, the first pressure
Sensor communicates with air, and the second pressure transducer accesses pipeline and stretches in solvent barrel.Pass through pressure transducer
Relatively two pressure sensor signal values judge whether have solvent in solvent barrel.
Preferably, described full-automatic segregation apparatus also includes that waste liquid barrel detects device, described waste liquid barrel detection device
For capacitance sensor, described capacitance sensor is fixed on waste liquid bottleneck.When waste liquid liquid level reach a certain height,
Capacitance sensor generation switching signal, system halt runs, and audio alert.
Preferably, described entirely also include that apparatus for testing weeping, described apparatus for testing weeping include two from segregation apparatus
The critesistor of individual identical characteristics, described critesistor is connected a resistance respectively.Gather resistance two ends respectively
Magnitude of voltage, when there being liquid to contact, the magnitude of voltage of liquid contact jaw becomes big, and system halt runs, and voice reporting
Alert.
Preferably, described full-automatic piece-rate system also includes that pressure-detecting device, described pressure-detecting device include
Piezoresistive pressure transmitter.Piezoresistive pressure transmitter is pressure oscillation and whether superpressure in the signal piping.
Preferably, described full-automatic piece-rate system also includes flow velocity automatic correction device.Described flow velocity is from dynamic(al) correction
Device includes Pitot tube and pressure reduction pressure transducer, and described Pitot tube includes inner tube, trocar sheath, baroport and complete
Pressure hole, described pitot hole is positioned at the head of Pitot tube, and described baroport is positioned at Pitot tube side surface.In device,
The head of Pitot tube is accessed pipeline, accesses pressure reduction pressure transducer in inner tube and trocar sheath, by measuring total head
Measure with the difference of static pressure and flow through the flow velocity in pipeline；When the actual flow velocity determined is inconsistent with setting flow velocity
Time, it is automatically adjusted revolution speed, thus flow velocity is carried out from dynamic(al) correction.
Preferably, described Pitot tube embeds thermocouple, for measuring the temperature in pipeline.
Full-automatic segregation apparatus of the present invention is the separation of polar compound in sample, more has the present invention of choosing
Described full-automatic segregation apparatus is for the separation of edible oil polar compound.
Therefore, further, the present invention also provides for a kind of food using full-automatic segregation apparatus of the present invention
With oil pole component separation method, specifically comprise the following steps that
Step 1, is prepared as clarification, without the liquid fat sample precipitated by edible oil；
Step 2, uses nonpolar eluent to be carried out pipeline in full-automatic segregation apparatus；
Concrete, described step 2 includes: the first multiplexer channel selector valve connection non-polar component eluent,
Non-polar component eluent enters the public pipeline of six-way injection valve, is inhaled into the first pump machine through six-way injection valve
Structure, carries out rinse to public pipeline, drains the gas in pipeline after cleaning；
Step 3, weighs the grease sample prepared by step 1, dissolves with solvent, obtains sample solution；
Step 4, chromatographic column is placed on column holder, and sample solution step 3 prepared injects full-automatic segregation apparatus
In six-way injection valve, bring sample solution into chromatographic column by nonpolar eluent, complete sample introduction, and continue into
Row eluting；
Concrete, described step 4 includes: chromatographic column is placed on column holder, the first multiplexer channel selector valve
The sample solution that connection is prepared by step 3, sample solution is by entering quantitative loop after six-way injection valve；Six-way injection valve
Carrying out gear switch, quantitative loop connects with the second pump machanism and chromatographic column, accesses nonpolar eluent, nonpolar
Eluent is entered quantitative loop by six-way injection valve, and the sample solution in quantitative loop is taken to chromatograph by nonpolar eluent
Post, completes sample introduction, and proceeds eluting；
Step 5, start-up detector, monitor in real time, it is thus achieved that elution chromatography figure；
Step 6, the elution chromatography figure obtained according to step 5 judges eluent acquisition time, and automatic collector is collected
All of eluent in this time；
Step 7, collects step 6 the eluent rotation obtained and steams, weigh the quality of non-polar component.
Preferably, described non-polar component eluent flow rate is 25mL/min, and non-polar component Eluant temperature is
10℃。
Preferably, detector is ultraviolet deuterium lamp detector, and detection wavelength is 200nm.
Beneficial effects of the present invention:
Full-automatic segregation apparatus the most of the present invention can realize auto injection and chromatographic column automatically switches, and locates continuously
Manage multiple sample, automatically collect, it is achieved high flux sharp separation, it is ensured that process stability and result accuracy.
2. use the online ultraviolet detection of detector, monitor separation component in real time, it is ensured that polar compound and nonpolar group
That divides is kept completely separate, and solves separating effect checking delayed.
3. full-automatic operation avoids the anthropic factor impact on result；Use valveless metering pump, flow velocity is steady,
Precision is high, resistance tocrocking is strong, it is ensured that the collimation of separating resulting and repeatability；Automatic sample handling system uses quantitatively
Environmental protection card sample introduction is mentioned accurately, is reappeared.
The separation method of edible oil polar compound the most of the present invention chooses existing or commercially available detached dowel, exempts
Front preparation filled out by manual dress post, time saving and energy saving, stability and favorable reproducibility.
5. possess flow velocity zero offset capability, make result more accurate, stable, operator can be saved simultaneously
Carry out manual synchronizing, it is to avoid waste unnecessary time and reagent.
Accompanying drawing explanation
Fig. 1 is the structural representation of a detailed description of the invention of the full-automatic segregation apparatus of the present invention
Fig. 2 is the annexation schematic diagram of a detailed description of the invention of the full-automatic segregation apparatus of the present invention
Fig. 3 is the structural representation of automatic sample handling system in the full-automatic segregation apparatus of the present invention
Fig. 4 is the structural representation of the present invention full-automatic segregation apparatus center pillar switched system
Fig. 5 is the structural representation of automatic separation system in the full-automatic segregation apparatus of the present invention
Fig. 6 is the structural representation of temperature control system in the full-automatic segregation apparatus of the present invention
Fig. 7 is that the full-automatic segregation apparatus of the present invention cleans fluid path figure
Fig. 8 is the present invention full-automatic segregation apparatus sample introduction fluid path figure
Fig. 9 is that the present invention full-automatic segregation apparatus profit sample/sample enters post fluid path figure
Figure 10 A and Figure 10 B is a specific embodiment party of solvent barrel detection device in the full-automatic segregation apparatus of the present invention
Formula schematic diagram
Figure 11 is another detailed description of the invention signal of solvent barrel detection device in the full-automatic segregation apparatus of the present invention
Figure
Figure 12 A and 12B is a detailed description of the invention of waste liquid barrel detection device in the full-automatic segregation apparatus of the present invention
Schematic diagram
Figure 13 is a detailed description of the invention schematic diagram of apparatus for testing weeping in the full-automatic segregation apparatus of the present invention
Figure 14 A and Figure 14 B is the one of flow velocity automatic correction device to be embodied as in the full-automatic segregation apparatus of the present invention
Mode schematic diagram
Detailed description of the invention
Below in conjunction with accompanying drawing, embodiment of the present invention is clearly and completely described.
Fig. 1-6 is a detailed description of the invention of the full-automatic segregation apparatus of the present invention.
Referring to the drawings 1, full-automatic segregation apparatus includes automatic sample handling system 100, post switched system 200, automatically
Piece-rate system 300 and temperature control system 400.
Referring to the drawings 203, automatic sample handling system 100 includes the first pump machanism 101, six-way injection valve 102, first
Multiplexer channel selector valve 103 and the first electrical control mechanism 104, wherein, six-way injection valve 102 with quantitative loop 105,
First pump machanism 101 is connected with six-way injection valve 102 pipeline.Optionally, the first pump machanism 101 includes syringe pump
106 and three-way valve 107, syringe pump 106 and three-way valve 107 pipeline connect, and three-way valve and waste liquid barrel 108 pipeline are even
Connect；First multiplexer channel selector valve 103 can be selected for six-way valve, including 6 sample intake passages, wherein passage 103-1
May be configured as sample channel to 103-5, be connected with sample liquid 110 pipeline, 103-6 passage is set to flushing channel,
It is connected with cleanout fluid 111 pipeline.The reagent of automatic sample handling system 100 is placed in reagent rack 109.
Referring to the drawings 2, accompanying drawing 4, post switched system 200 includes the second multiplexer channel selector valve the 201, the 3rd multichannel
Channel selector valve 202, column holder mechanism 203 and the second electrical control mechanism 204, described column holder mechanism is arranged
Chromatographic column 205, the second multiplexer channel selector valve 201 and the 3rd multiplexer channel selector valve 202 is had to lay respectively at first
Column holder mechanism about 203 both sides, the second multiplexer channel selector valve 201 is connected with six-way injection valve 102 pipeline.
Optionally, column holder mechanism 203 is high to adapt to different post for slide rail type upper and lower scalable column holder, widens pillar
Range.
Referring to the drawings 2, accompanying drawing 5, automatic separation system 300 include the second pump machanism 301, detector 302, from
Dynamic catcher the 303, the 3rd electrical control mechanism 304 and industrial computer 305, the second pump machanism 301 respectively with clematis stem sample introduction
Valve 102 and the 3rd multiplexer channel selector valve 202 pipeline connect.Optionally, the second pump machanism 301 can be pottery nothing
Valve dosing pump, supports binary solvent conveying, and mobile phase solvent A and solvent B enters valveless meter after electromagnetic valve 306
Amount pump, easy cleaning maintenance, change in flow is 1-200ml/min, maximum pressure for 200psi (14bar/1.4M
Pa), the most also including blender 307, blender 307 is for fully mixing solvent orange 2 A and solvent B, and pressure
Force checking device 308, when beyond setting pressure, system alarm.Also include the second column holder mechanism 309, bag
Include different model liner, to adapt to multiple column type.Optionally, detector uses wavelength to be 200nm-400nm's
Deuterium lamp UV-detector, can coordinate with control system and realizes smartphone in detection simultaneously in process of the test.
Optionally, automatic collector has X/Y axle two dimension telecontrol equipment, height adjuster, catcher pallet automatically,
Wherein catcher pallet is provided with liquid leakage tank and leakage diversion Design, can leakage be drawn.Industrial computer 305 is adopted
With built-in industrial control machine and chromatographic analysis system, operating intuitive and convenient, data are transmitted accurately and timely.
Referring to the drawings 2, accompanying drawing 6, temperature control system 400 includes refrigeration mechanism 401, touch screen 402 and the
Four electrical control mechanisms 404.Wherein, the operations such as touch screen 402 carries out temperature control and regulation, temperature data shows are used；
Solvent barrel 405 and 406 is respectively used to store the solvent orange 2 A as flowing phase and solvent B.Due to the easy gas of petroleum ether
Changing, in order to prevent pump gasification when drawing petroleum ether, cause fluid flow inaccurate, design refrigeration mechanism ensures
Petroleum ether is under low temperature environment, improves system accuracy.In the present invention, refrigeration mechanism 401 is according to quasiconductor system
Cold principle, uses PID temperature control regulation system to export as temperature as input, semiconductor chilling plate, multiple systems
Cold carries out transmitting cryogenic temperature, and then freezes solvent bottle cold temperature groove, and carries out cooling piece heat radiation with fan
The heat radiation action in face, carries out Rapid Thermal exchange.
Above-mentioned first electrical control mechanism the 104, second electrical control mechanism the 204, the 3rd electrical control mechanism 304 and the 4th is automatically controlled
Mechanism 404 is integrated by automatically controlled original paper, it is provided that slave computer guarantee, and its rear end includes communication interface, is connect by communication
Mouth electrically connects with industrial computer 305 respectively, and electrical control mechanism rear end also includes that on and off switch and other interface are (as power-off is protected
Protect).
Optionally, use motor, if motor is as actuator, utilize motor drive control pump,
Six-way injection valve, multiplexer channel selector valve, height adjuster etc. run, it is achieved mechanical automation controls.
The fluid path figure of 7-9 segregation apparatus full-automatic to the present invention is described further below in conjunction with the accompanying drawings.
Clean
Referring to the drawings 7, before sample introduction, syringe pump 106 is existing to be carried out pipeline (now quantitative loop 105 with point
Communicate from stream), first passage selects six-way valve 103 to open, and cleanout fluid 111 is inhaled into six-way injection valve 102
Public pipeline, six-way injection valve 102-6 position entered from the right side mouth of three-way valve 107 by 1, be inhaled into
In syringe pump 106, to reach the purpose that public pipeline, syringe pump 106 are cleaned, after reaching to clean capacity, three
Logical valve 107 switches, and waste liquid is discharged by syringe pump 106 through three-way valve 107.
Sample introduction
Referring to the drawings 8, cleaned after, automatic sampling apparatus 100 carries out sample introduction (now quantitative loop 105 and sampling
Stream communicates), on the first multiplexer channel selector valve 103, respective channel is opened, and sample liquid 111 is inhaled into second and leads to
The public pipeline of road selector valve, is entered quantitative loop by six-way injection valve 102-6 position through 5, original in quantitative loop
Liquid is entered from the right side mouth of three-way valve 107 by 1 through 2, is inhaled in syringe pump 106, reaches to set and holds
After amount, three-way valve 107 switches, and waste liquid is discharged by syringe pump 106 through three-way valve 107.
Profit sample/sample enters post
Referring to the drawings 9, six-way injection valve 102 carries out gear switch, quantitative loop 105 and the second pump machanism 301 and color
Spectrum post 205 is connected, and flows and is entered quantitative loop 105, quantitative loop 105 by six-way injection valve 102-3 position through 2
In sample flowed through 4 by 5 and taken to chromatographic column 205 mutually, complete sample introduction.After having run sampling step,
Injector is gradually completing profit post-sample introduction-operation gradient according to the step arranged automatically, it is achieved most 5 kinds of samples
Automatic switchover sample introduction.
In an optional embodiment, full-automatic segregation apparatus also includes earth leakage circuit-breaker.Due to chemistry
Experiment contacts with solvent a lot, when the hands contact instrument of experiment operator humidity or plug power supply, especially
It is the instrument of metal shell, it is more likely that electric shock phenomenon can occur, therefore, add band electric leakage and protect in instrument
The air switch protected, when instrument is short-circuited, air switch automatic trip；Or instrument generation leaky,
Will trip, protect the life safety of operator to a great extent.Concrete, in the present invention, will leakage
Electric protective circuit breaker is received on zero line and the live wire of power supply (such as: 220V/50Hz alternating current) input, zero
Line and fire wire output end access earth leakage protective device end (such as: 24V Switching Power Supply, 48V Switching Power Supply, industrial computer
Adapter and detector etc.), selection rated current is 2A, and leakage current is the earth leakage circuit-breaker of 30mA,
When system being short-circuited or load current is more than 2A, or system generation leaky, leakage current is more than
During 30mA, earth leakage circuit-breaker will automatically cut off main circuit, it is achieved earth leakage circuit-breaker is to instrument and personnel
Safeguard protection.
In an optional embodiment, full-automatic segregation apparatus also includes that solvent barrel detects device, works as detection
In solvent barrel solvent-free time, system halt runs, and audio alert.Instrument is in the case of unmanned
During operation, when the solvent in solvent barrel is finished, instrument can detect do not had solvent, and now instrument is certainly
Body enters halted state, and points out user with voice, when operator add molten in solvent barrel
After agent, click continues to run with, and instrument, if be detected that there is solvent in solvent barrel, eliminates language alarm and continues
The continuous experiment carrying out being not fully complete.
Solvent barrel detection device can be Photoelectric Detection, referring to the drawings 10A, according to air 11 and liquid 12 to light
The different principle of refractive index, due to air 11 to light almost without refraction, when the light of light source 13 is by air 11
After, receiving terminal 14 can all receive the energy of light, when by liquid 12, owing to liquid 12 has certain folding
Penetrate, the energy dropoff of the light that receiving terminal 14 receives, i.e. can determine whether whether pipeline has liquid flow through, to work as pipeline
In when there is no liquid, i.e. can determine whether solvent barrel does not has solvent, otherwise solvent barrel have solvent.Concrete, ginseng
According to accompanying drawing 10B, photoelectric sensor includes light source transmitting terminal 13 and light source receiving terminal 14, and light source transmitting terminal 13 He
Light source receiving terminal 14 is positioned at pipeline 15 two ends above solvent barrel, and control line is linked on control circuit plate, works as pipe
When having liquid in road, photoelectric sensor output high level, when not having liquid in pipeline, photoelectric sensor exports
Low level, after panel receives low level, suspends valveless metering pump, starts speech ciphering equipment, send voice and carry
Show, send out communication command to industrial computer simultaneously, after industrial computer receives order, show warning information at software interface.
Solvent barrel detection device can also be pressure detecting, and after liquid compression air, air pressure becomes big
Principle, utilizes the pressure in two micropressure sensor signal pipings, a micropressure sensor and air contact,
Detection air pressure is held as a comparison, and the pressure in a micropressure sensor signal piping is as test side, pipe
Road one terminates micropressure sensor, and one end is accessed in solvent barrel, the liquid when there being liquid in solvent barrel, in pipeline
Body compressed air, the pressure ratio air pressure in pipeline is big, the force value comparison ratio of the pressure transducer of test side
The force value of end is big, i.e. detects in solvent barrel have pressure, along with the solvent in solvent barrel reduces, and liquid in pipeline
The compressed-air actuated pressure of body reduces.When not having liquid in solvent barrel, the pressure in pipeline is air pressure,
Now the pressure of two micropressure sensors is of substantially equal, now detects that solvent barrel is empty, otherwise, test side
Pressure ratio contrast end pressure big, i.e. solvent barrel has solvent.Concrete, referring to the drawings 11, pacify in instrument
Filling two micropressure sensors, a sensor (not shown on figure) communicates with air, a sensor 16
Access one section of pipeline 17 and stretch in solvent barrel 406, the AD conversion of the holding wire Access Control plate of two sensors
Device interface, panel detects the numerical values recited of two holding wires in real time, by comparing two pressure sensor signals
Value judges whether have solvent in solvent barrel.Utilize this device to detect, whether be possible not only to detect in solvent barrel
There is solvent, it is also possible to the height of solvent liquid level in solvent barrel detected.
In an optional embodiment, described full-automatic segregation apparatus also includes that waste liquid barrel detects device.Instrument
Device is when unattended operation, when the waste liquid in waste liquid barrel is full, and operation suspension together, and carry out voice message,
After changing empty waste liquid barrel, click continues to run with, and instrument proceeds the experiment being not fully complete.This function can be kept away
Exempt from overflow waste liquor contamination operating board, and can avoid waste liquid overflow after, be evaporated to air, to experimenter
Health damages.Wherein, waste liquid barrel detection device can be capacitance sensor, 12A referring to the drawings, due to
Any material all can have certain dielectric constant, therefore can use capacitive approach switch as detection waste liquid be
The fullest no sensor.The probe of capacitive approach switch is the concussion loop with certain frequency, when there being material
During close to this probe, the frequency of oscillation circuit there occurs change, can judge have object proximity to visit according to this change
Head.Concrete, 12B, is fixed on waste liquid barrel 22 mouthfuls by described capacitance sensor 21, when waste liquid liquid referring to the drawings
Face reach a certain height, and capacitance sensor detects solvent liquid level, and capacitance sensor generation switching signal is given and controlled
Plate, after panel receives switching signal, suspends valveless metering pump, starts speech ciphering equipment, send voice message,
Send out communication command to industrial computer simultaneously, after industrial computer receives order, show warning information at software interface.
In an optional embodiment, full-automatic segregation apparatus also includes apparatus for testing weeping.Instrument is in fortune
During row, often there will be pipe joint leakage, or the situation that pipeline bursts apart, owing to instrument internal has electricity
Gas element, if finding leakage not in time, can cause the waste of experimental period and reagent, and serious likely can
Causing instrument damage and personal safety injury, therefore instrument internal needs to add apparatus for testing weeping, when in instrument
When portion has liquid to leak, instrument can detect, and stops the operation of pump in time, it is to avoid loses time and reagent.
Critesistor is the resistance that a kind of resistance value changes along with ambient temperature, and leakage detection uses critesistor conduct
Leakage detection probe, when make use of liquid gasification, liquid absorbs heat, the principle that temperature reduces.Concrete,
Apparatus for testing weeping can be located at automatic separation system bottom, detection fluid path original paper (such as pipeline, pump machanism, valve etc.)
The leakage that region is likely to occur.Fluidic leak detector has two critesistor as detection probe, and logical direct current or
Alternating current, when not having liquid to contact, two critesistor are in the same space, equal by electric current, therefore
The temperature of two critesistor is in the state of phase isoequilibrium.When one of them critesistor has liquid to contact,
Critesistor generates heat, and makes liquid gasification, takes away heat simultaneously, and thermistor temp reduces, two critesistor
Temperature disequilibrium, now instrument has been detected as leakage.Concrete, referring to the drawings 13, apparatus for testing weeping
Including the critesistor of two identical characteristics, a small resistor (10 ohms) that critesistor is connected respectively
Forming temperature sensor A and temperature sensor B, two temperature sensor circuits are separately added into the DC voltage of 24V,
Utilize the magnitude of voltage being gathered small resistor two ends by Chip Microcomputer A/D interface, when temperature is not changed in, two little electricity
Resistance direct voltage is equal, and when there being liquid to contact, the critesistor of test side reduces, and electric current increases, and collects
Magnitude of voltage become big, now Instrumental results is leakage.
In an optional embodiment, described full-automatic segregation apparatus also includes pressure-detecting device, is used for
Detecting instrument in running, pressure oscillation situation and pipeline whether superpressure in pipeline.Wherein, pressure detecting
Device can be located at automatic separation system top, is connected on the pipeline between blender and chromatographic column, senses pipe in real time
Road pressure.When there being liquid to flow in pipeline, liquid has certain pressure to pipeline arm, available pressure resistance type
The solvent in the pressure transmitter signal piping pressure to pipeline arm.Concrete, piezoresistive pressure transmitter according to
The size of probe pressure, the current signal of output 4mA-20mA, utilize Chip Microcomputer A/D outfan, 4mA-20mA
The digital signal that analog-signal transitions is 0V-3.3V, further according to reduction formula, force value is shown at screen
On.
In an optional embodiment, described full-automatic segregation apparatus also includes flow velocity automatic correction device.
Owing to infusion pump is in running, owing to pipe joint does not connect, or solvent density, temperature are the most equal
Various subjectivities or odjective cause cause the flow velocity of pump not meet with the flow velocity of setting, and now, instrument itself can root
According to the flow velocity size flow through in pipeline with arrange flow velocity and contrast, carry out from dynamic(al) correction, operator can be saved
Carry out manual synchronizing, it is to avoid waste unnecessary time and reagent.
Actual flow velocity in pipeline, from dynamic(al) correction, can be measured by flow rate pump according to Pitot tube measuring principle.
Pitot tube is the dress that the total head pressure by measurement fluid and the difference of hydrostatic head, i.e. dynamic head measure flow rate of liquid
Putting, also referred to as dynamic pressure measurement pipe, referring to the drawings 14A, its front end center aperture 41 is used for measuring the total head pressure of fluid,
Row's aperture 42 on side surface is used for measuring hydrostatic pressure head, and Pitot tube head has ellipse, taper and spherical
Structure, when measuring rate of flow of fluid, inserts the head of Pitot tube at the mensuration of runner, referring to the drawings 14B, finishes
The central small hole of trustship head to be met to fluid, and wherein positive axis should be parallel with fluid flowing path direction.Pitot tube is stretched
The inner sleeve 43 gone out and trocar sheath 44 access differential pressure micropressure sensor 45, output total head and the difference of static pressure:
hDynamic=hEntirely-hQuiet
Record hDynamicAfter, according to the relation of flow velocity Yu dynamic pressure, the flow velocity of fluid can be obtained:
Because
So
Thus obtain flow further
Q=ω Fm3/s
In formula: rate of flow of fluid in ω-pipeline, unit m/s；Q-pipeline section amasss, unit m2。
Further, it is also possible to add thermocouple between Pitot tube trocar sheath and inner sleeve, and draw holding wire, can
To measure the temperature of liquid in pipeline simultaneously.
Concrete, the present invention accesses in pipeline one section of Pitot tube 46 with thermocouple, at trocar sheath 44
Differential pressure micro-pressure transmitter 45, thermocouple signal end and pressure transmitter signal end is added with inner sleeve 43 air end
Access Chip Microcomputer A/D input interface, be digital signal by AD conversion, contrast with arranging flow velocity, according to right
Rotating speed than structure regulation pump, it is achieved the zero offset capability of flow velocity.
It addition, this flow velocity automatic correction device is not limited only to full-automatic segregation apparatus disclosed in the embodiment of the present invention
In, it is also possible to relate to the instrument such as chromatograph of liquid, gas chromatograph of fluid path, Chemical Decomposition system for other
Deng.
Additionally, the present invention also provides for a kind of edible oil polar compound separation method, it is below a concrete enforcement
Mode:
1 sample prepares
1.1 the removal of impurity
Sample as sample should be liquid, clarification, without precipitation and fully mixes.If sample is not clarified, is had
Precipitation, then must be placed in oils and fats in water-bath or the thermostatic drying chamber of 50 DEG C, the temperature of oils and fats is heated to 50 DEG C
And shake well is to melt possible fat crystals.If now oil sample becomes clarification, nothing precipitation, then can make
For sample, otherwise oils and fats should be placed in the thermostatic drying chamber of 50 DEG C, with the insoluble impurity of filter paper filtering,
Taking the supernatant liquid oils and fats after filtration as sample, for preventing Oxidation of Fat and Oils, filter process should complete as early as possible.
Freezing point higher than 50 DEG C or is higher than to the sample of 50 DEG C of lubricant components containing freezing point, then must be by oil
Fat is placed in water-bath or the thermostatic drying chamber of higher than its freezing point about 10 DEG C, by oils and fats heating shake well
To melt possible fat crystals.If also needing to filter, then oils and fats is placed in higher than its freezing point about 10 DEG C
In thermostatic drying chamber, with the insoluble impurity of filter paper filtering, take the supernatant liquid oils and fats after filtration as sample,
For preventing Oxidation of Fat and Oils, filter process should complete as early as possible.
1.2 drying and dehydrating
If containing moisture in oils and fats, dehydration must be dried.To being liquid at room temperature, crystallizing or solidifying without obvious
Gu the oils and fats of phenomenon, and through the process of " 1.1 " and after being cooled to room temperature for liquid, without substantially crystallization or
The oils and fats of solidification phenomenon, can be added the ratio anhydrous sulfur of addition of 1g～2g anhydrous sodium sulfate in every 10g oils and fats
Acid sodium, and it is thoroughly mixed adsorption dewatering, then with filter paper filtering, take the supernatant liquid oils and fats after filtration and make
For sample.
To having crystallization or the oils and fats of solidification phenomenon at room temperature, and pass through the process of " 1.1 " and be cooled to room
Wen Houyou substantially crystallizes or the oils and fats of solidification phenomenon, after can being completely dissolved with appropriate petroleum ether by oil sample again
Using anhydrous sodium sulfate adsorption dewatering, then filter paper filtering collects filtrate, and it is 45 DEG C that filtrate is placed in bath temperature
Rotary Evaporators in, under condition of negative pressure, by solvent therein rotate be evaporated, take the supernatant liquid oils and fats of residual
As sample.
The activation of 2 chromatographic columns
Moisten with non-polar component eluent for the flowing phase pipeline of the relatively full-automatic segregation apparatus of flowing
Wash, drain the gas in flowing phase pipeline.Take 1 chromatographic column, connect into the stream of full-automatic segregation apparatus
Dynamic phase pipeline, rinses chromatographic column 10 with non-polar component eluent for flowing phase, the flow velocity of 25mL/min
Min, makes chromatographic column be infiltrated by solvent completely.
The separation of 3 non-polar component
Take 1 clean 10mL glass beaker, accurately weigh the oil sample of 1g (being accurate to 0.001g)
M (), then fully dissolves oil sample with the petroleum ether (30 DEG C～60 DEG C of boiling ranges) of 5mL, becomes
Sample solution.First FLASH chromatographic column being disconnected with flowing phase pipeline, the upper end that sample solution is injected into chromatographic column enters
At Kou, then wash the interior residual of 10mL glass beaker with the petroleum ether (30 DEG C～60 DEG C of boiling ranges) of 3mL
Sample solution, cleaning mixture is also with being injected into the porch, upper end of chromatographic column, then by the upper end of FLASH chromatographic column and stream
Dynamic phase pipeline connects, and carries out the separation of non-polar component by following parameter:
A) flowing phase: non-polar component eluent；
B) flow rate of mobile phase: 25mL/min；
C) fraction collector: with 1000mL osculum glass receiving flask, for collecting container, from eluting start with
Full collection mode is collected；
D) UV-detector monitoring wavelength: 200nm；
E) real-time monitoring system is enabled, it is thus achieved that elution chromatography figure；
F) solvent temperature control system temperature: 10 DEG C；
G) elution time: 11min.
When carrying out lock out operation, the ambient temperature of experiment should control between 10 DEG C～25 DEG C.
The collection of 4 non-polar component, concentration and quantitatively
Take 1 clean 500mL flask and put into the thermostatic drying chamber of (103 ± 2) DEG C, dry about 1h,
Then taking out in being immediately placed in glass desicator and be cooled to room temperature, then weigh (M0).Separate according to " 3 "
The Real-time Monitoring Data that operation is obtained, the end time point of the chromatographic peak that non-polar component is maximum should control
In 4.5min～6.8min interval, it is now all collections in 0min～11min by elution time interval
Eluent (in 1000mL osculum glass receiving flask) pour in this 500mL round-bottomed flask.
Then this is placed in, equipped with the 500mL flask collecting eluent, the rotary evaporation that bath temperature is 60 DEG C
In instrument, under condition of normal pressure, solvent major part therein is evaporated, the most again under condition of negative pressure, residue is few
Amount solvent rotary evaporation, near dry, take out this flask and dries the water of flask outer wall.Then this 500mL is burnt
The vacuum constant temperature drying baker of 40 DEG C put into by bottle, under the condition of negative pressure of 0.1MPa, dries 20min～30min,
Putting into glass desicator after end and be cooled to room temperature, then weigh (M1), and (M1-M0) is nonpolar
The quality of component.
Above-described embodiment is only for illustrating technology design and the feature of the present invention, not in order to limit the present invention, all
Within the spirit and principles in the present invention, any amendment of being made, equivalent etc., should be included in the present invention
Protection domain within.
Claims (14)
1. a full-automatic segregation apparatus, it is characterised in that: include automatic sample handling system, post switched system, from
Dynamic piece-rate system；
Described automatic sample handling system include the first pump machanism, six-way injection valve, the first multiplexer channel selector valve and
First electrical control mechanism, described six-way injection valve with quantitative loop, described first pump machanism and six-way injection valve pipeline
Connect；
Described post switched system includes that the second multiplexer channel selector valve, the 3rd multiplexer channel selector valve, the first post prop up
Frame mechanism and the second electrical control mechanism, described first column holder mechanism is used for placing chromatographic column, described second multichannel
Channel selector valve and the 3rd multiplexer channel selector valve lay respectively at the first upper and lower both sides of column holder mechanism, the second multichannel
Channel selector valve is connected with six-way injection valve pipeline；
Described automatic separation system include the second pump machanism, detector, automatic collector, the 3rd electrical control mechanism with
And industrial computer, described second pump machanism is connected with six-way injection valve and the 3rd multiplexer channel selector valve pipeline respectively；
Described full-automatic segregation apparatus also includes that flow velocity automatic correction device, described flow velocity automatic correction device include
Pitot tube and pressure reduction pressure transducer, wherein, described Pitot tube includes inner sleeve, trocar sheath, baroport and complete
Pressure hole, described pitot hole is positioned at the head of Pitot tube, and described baroport is positioned at Pitot tube side surface, at inner sleeve
Pressure reduction pressure transducer is accessed with trocar sheath.
2. full-automatic segregation apparatus as claimed in claim 1, it is characterised in that described automatically separates dress
Also including temperature control system in putting, described temperature control system includes refrigeration mechanism and the 4th electrical control mechanism.
3. full-automatic segregation apparatus as claimed in claim 2, it is characterised in that: described refrigeration mechanism includes half
Conductor cooling piece, cold temperature groove and fan.
4. the full-automatic segregation apparatus as described in any one of claim 1-3, it is characterised in that: described automatically
Segregation apparatus also includes motor, drives pump machanism, six-way injection valve, multiplexer channel to select by motor
Select valve.
5. the full-automatic segregation apparatus as described in any one of claim 1-3, it is characterised in that: described first pump
Mechanism includes that syringe pump and three-way valve, described syringe pump and three-way valve pipeline connect, described three-way valve and waste liquid barrel
Pipeline connects.
6. the full-automatic segregation apparatus as described in any one of claim 1-3, it is characterised in that: described second pump
Mechanism includes valveless metering pump.
7. full-automatic segregation apparatus as claimed in claim 1, it is characterised in that: described automatic collector includes
X/Y axle two dimension autonomous movement positioner, arrangement for adjusting height and catcher pallet, on described catcher pallet
Liquid leakage tank and flow-guiding channel are set.
8. full-automatic segregation apparatus as claimed in claim 1, it is characterised in that: described full-automatic segregation apparatus
Also include earth leakage circuit-breaker.
9. full-automatic segregation apparatus as claimed in claim 1, it is characterised in that: described full-automatic segregation apparatus
Also include that solvent barrel detects device.
10. full-automatic segregation apparatus as claimed in claim 9, it is characterised in that: described solvent barrel detection device
Including photoelectric sensor or pressure transducer.
11. full-automatic segregation apparatuss as claimed in claim 1, it is characterised in that: described full-automatic segregation apparatus
Also including that waste liquid barrel detects device, described waste liquid barrel detection device is capacitance sensor.
12. full-automatic segregation apparatuss as claimed in claim 1, it is characterised in that: described full-automatic segregation apparatus
Also include that apparatus for testing weeping, described apparatus for testing weeping include the critesistor of two identical characteristics.
13. full-automatic segregation apparatuss as claimed in claim 1, it is characterised in that: described full-automatic segregation apparatus
Also include that pressure-detecting device, described pressure-detecting device include piezoresistive pressure transmitter.
14. full-automatic segregation apparatuss as claimed in claim 1, it is characterised in that: described Pitot tube arranges heat
Galvanic couple.
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| CN104655768B (en) * | 2015-03-11 | 2016-08-17 | 天津博纳艾杰尔科技有限公司 | Oil component automatic separation equipment and the application in wax, colloid separation in crude oil thereof |
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| CN109459462B (en) * | 2018-10-31 | 2021-03-19 | 泉州市全通光电科技有限公司 | Automatic freezing point tester and testing method thereof |
| CN109499095A (en) * | 2018-11-30 | 2019-03-22 | 南京浦世环境科技发展有限公司 | Full-automatic element sepatation purification devices |
| CN110161257A (en) * | 2019-06-18 | 2019-08-23 | 广东优尼德生物科技有限公司 | A kind of glycolated hemoglobin analysis |
| CN212207226U (en) * | 2020-06-10 | 2020-12-22 | 上海贝高医疗科技有限公司 | Static sample introduction and flow fraction collection device matched with liquid chromatograph |
| CN112666293B (en) * | 2020-12-19 | 2022-05-13 | 北京大学 | Liquid phase automatic synthesizer |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6415670B1 (en) * | 1999-03-26 | 2002-07-09 | Yamazen Corporation | Injection apparatus |
| CN101191790A (en) * | 2006-12-01 | 2008-06-04 | 株式会社日立高新技术 | Liquid chromatographic analysis apparatus |
| CN101614711A (en) * | 2009-04-03 | 2009-12-30 | 天津博纳艾杰尔科技有限公司 | A kind of automatic three-stage chromatograph |
| CN102008837A (en) * | 2010-09-30 | 2011-04-13 | 中国科学院昆明植物研究所 | Separating preparative chromatography apparatus comprising serial preparative chromatography column |
| CN102648409A (en) * | 2009-10-08 | 2012-08-22 | 通用电气健康护理有限公司 | Multi-stream high-pressure liquid chromatography module |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2892795B2 (en) * | 1989-09-12 | 1999-05-17 | エーザイ株式会社 | Mobile phase conversion method and apparatus in high performance liquid chromatography mass spectrometry |
| US6812030B2 (en) * | 2001-04-25 | 2004-11-02 | Biotrove, Inc. | System and method for high throughput sample preparation and analysis using column chromatography |
| JP5533805B2 (en) * | 2011-07-15 | 2014-06-25 | 株式会社島津製作所 | Liquid chromatograph and program |
-
2014
- 2014-11-28 CN CN201410709516.3A patent/CN104407083B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6415670B1 (en) * | 1999-03-26 | 2002-07-09 | Yamazen Corporation | Injection apparatus |
| CN101191790A (en) * | 2006-12-01 | 2008-06-04 | 株式会社日立高新技术 | Liquid chromatographic analysis apparatus |
| CN101614711A (en) * | 2009-04-03 | 2009-12-30 | 天津博纳艾杰尔科技有限公司 | A kind of automatic three-stage chromatograph |
| CN102648409A (en) * | 2009-10-08 | 2012-08-22 | 通用电气健康护理有限公司 | Multi-stream high-pressure liquid chromatography module |
| CN102008837A (en) * | 2010-09-30 | 2011-04-13 | 中国科学院昆明植物研究所 | Separating preparative chromatography apparatus comprising serial preparative chromatography column |
Non-Patent Citations (1)
| Title |
|---|
| 食品安全国家标准 食用油中极性组分（PC）的测定;中华人民共和国国家卫生和计划生育委员会 发布;《道客巴巴》;20141117;第2页"5.1 试样的制备"小节、第4-5页"11 分析步骤"小节 * |
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