CN104407083A - Full-automatic separation system and application of full-automatic separation system in separation of polar components in edible oil - Google Patents
Full-automatic separation system and application of full-automatic separation system in separation of polar components in edible oil Download PDFInfo
- Publication number
- CN104407083A CN104407083A CN201410709516.3A CN201410709516A CN104407083A CN 104407083 A CN104407083 A CN 104407083A CN 201410709516 A CN201410709516 A CN 201410709516A CN 104407083 A CN104407083 A CN 104407083A
- Authority
- CN
- China
- Prior art keywords
- full
- automatic
- tripping device
- automatic tripping
- pipeline
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Sampling And Sample Adjustment (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The invention provides a full-automatic separation system and application of the full-automatic separation system in separation of polar components in edible oil. The full-automatic separation system comprises an automatic sample injection system 100, a column switching system 200, an automatic separation system 300 and a temperature control system 400. When the device disclosed by the invention is used for separating the polar components in the edible oil, automatic sample injection and automatic chromatographic column switching can be realized; multiple samples can be continuously treated, and high-flux quick separation is realized; meanwhile, full mechanical control is performed on sample injection, column switching and separated component collection, so that influence on an experiment due to manmade factors is avoided; by ultraviolet online monitoring and automatic flowing speed correction, a detection result is accurate and 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 the application in edible oil polar compound is separated thereof.
Technical background
At present, the artificial mode be separated is adopted more for the separation detecting sample Semi-polarity component, such as detecting the method for edible oil polar compound mainly according to " mensuration of the polar compound (PC) in GB/T 5009.202-2003 edible vegetable oil frying process ", be separated by silica gel column chromatography, TLC detects the polar compound in grease.Its principle is: when the grease of frying is by being equipped with the silicagel column having adsorbed certain moisture, and under the wash-out of mobile phase, first triglyceride (namely through frying unaltered grease) is wherein flowed out spectrum post by wash-out; Flinging to eluant, eluent, weigh, be the quality of non-polar component, is exactly the quality (there occurs the grease of chemical change after frying) of polar compound by the quality that the quality of upper prop sample deducts non-polar component.But conventional post chromatography is owing to relying on manual operations completely, and the not only waste of manpower of staff coutroi velocity, also can cause unstable result, poor reproducibility simultaneously; After column chromatography for separation terminates, need to rely on TLC to verify separating effect, operation is very loaded down with trivial details like this, often needs, through operation for several times repeatedly, just can reach desired separated effect, cause separating effect to be verified delayed; In addition, the post pre-treatment of classic method dress, needs cost 1 day to be dried by silicon particle and controls water cut, then people's frock post half an hour, and column chromatography for separation process-field controls to need 1 hour, also wants TLC checking separating effect to need half an hour, very time-consuming.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of full-automatic tripping device is provided, can accurate, real-time, fast component, particularly polar compound in sample be separated.
Also object of the present invention is to provide a kind of method that edible oil polar compound is separated, and avoids the problem of accuracy and poor reproducibility in existing manually operated alternative.
For achieving the above object, the invention provides a kind of full-automatic tripping device, comprise automatic sample handling system, post switched system and automatic separation system;
Described automatic sample handling system comprises the first pump machanism, six-way injection valve, the first multiplexer channel selector valve and the first electrical control mechanism, and described six-way injection valve is with quantitative loop, and described first pump machanism is connected with six-way injection valve pipeline;
Described post switched system comprises the second multiplexer channel selector valve, the 3rd multiplexer channel selector valve, column holder mechanism and the second electrical control mechanism, described column holder mechanism is for placing chromatographic column, described second multiplexer channel selector 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 selector valve is connected with six-way injection valve pipeline;
Described automatic separation system comprises the second pump machanism, detecting device, automatic collector, the 3rd electrical control mechanism and industrial computer, and described second pump machanism is connected with six-way injection valve and the 3rd multiplexer channel selector valve pipeline respectively.
Preferably, described full-automatic tripping device also comprises temperature control system, and described temperature control system comprises refrigeration mechanism and the 4th electrical control mechanism.
Preferably, described refrigeration mechanism comprises semiconductor chilling plate, cold temperature groove and fan, and described semiconductor chilling plate freezes to cold temperature groove, and the radiating surface of described fan to cooling piece dispels the heat.
Preferably, described full-automatic tripping device also comprises stepper motor, drives pump machanism, six-way injection valve, multiplexer channel selector valve by stepper motor.
Preferably, described first pump machanism comprises syringe pump and T-valve, and described syringe pump is connected with T-valve pipeline, and described T-valve is connected with waste liquid barrel pipeline.
Preferably, described second pump machanism comprises valveless metering pump.
Preferably, described detecting device is UV-detector.
Preferably, described first column holder mechanism is the upper and lower adjustable column holder of slide rail type.
Preferably, described automatic collector comprises X/Y axle two dimension autonomous movement locating device, arrangement for adjusting height and gatherer pallet, and described gatherer pallet arranges liquid leakage tank and flow-guiding channel.
Preferably, described full-automatic tripping device also comprises earth leakage circuit-breaker.
Preferably, described full-automatic tripping device also comprises solvent barrel pick-up unit.When detecting solvent-free in solvent barrel, system halt runs, and audio alert.
In a kind of concrete embodiment, described solvent barrel pick-up unit comprises photoelectric sensor, and described photoelectric sensor comprises light source transmitting terminal and light source receiving terminal, and described light source transmitting terminal and light source receiving end are positioned at the pipeline two ends above solvent barrel.When there being liquid in pipeline, photoelectric sensor exports high level, when there is no liquid in pipeline, and photoelectric sensor output low level.
In a kind of concrete embodiment, described solvent barrel pick-up unit comprises pressure transducer, and the first pressure transducer communicates with air, and the second pressure transducer access pipeline also stretches in solvent barrel.Compare two pressure sensor signal values by pressure transducer and judge whether have solvent in solvent barrel.
Preferably, described full-automatic tripping device also comprises waste liquid barrel pick-up unit, and described waste liquid barrel pick-up unit is capacitive transducer, and described capacitive transducer is fixed on waste liquid bottleneck.When waste liquid liquid level reach a certain height, capacitive transducer generation switching signal, system halt runs, and audio alert.
Preferably, described full self-separation device also comprises apparatus for testing weeping, and described apparatus for testing weeping comprises the thermistor of two identical characteristics, and described thermistor is connected a resistance respectively.Gather the magnitude of voltage at resistance two ends respectively, when there being liquid comes into contact, the magnitude of voltage of liquid comes into contact end becomes large, and system halt runs, and audio alert.
Preferably, described full-automatic piece-rate system also comprises pressure-detecting device, and described pressure-detecting device comprises piezoresistive pressure transmitter.Piezoresistive pressure transmitter to be used in signal piping pressure surge and whether superpressure.
Preferably, described full-automatic piece-rate system also comprises flow velocity automatic correction device.Described flow velocity automatic correction device comprises Pitot tube and pressure reduction pressure transducer, and described Pitot tube comprises interior pipe, outer tube, baroport and pitot hole, and described pitot hole is positioned at the head of Pitot tube, and described baroport is positioned at Pitot tube side surface.In device, by the head of Pitot tube access pipeline, at interior pipe and outer tube access pressure reduction pressure transducer, measure by the difference measuring total head and static pressure the flow velocity flow through in pipeline; When the actual flow velocity determined and setting flow velocity are inconsistent, automatically regulate revolution speed, thus automatic calibration is carried out to flow velocity.
Preferably, in described Pitot tube, embed thermopair, for measuring the temperature in pipeline.
Full-automatic tripping device of the present invention is used for the separation of sample Semi-polarity component, more has the separation of of the present invention full-automatic tripping device for edible oil polar compound of choosing.
Therefore, further, the present invention also provides a kind of edible oil polar compound separation method adopting full-automatic tripping device of the present invention, and concrete steps are as follows:
Step 1, is prepared into clarification, without the liquid fat sample precipitated by edible oil;
Step 2, uses nonpolar eluent to clean pipeline in full-automatic tripping device;
Concrete, described step 2 comprises: the first multiplexer channel selector valve is communicated with non-polar component eluent, non-polar component eluent enters the public pipeline of six-way injection valve, the first pump machanism is inhaled into through six-way injection valve, rinse is carried out to public pipeline, after cleaning, drains the gas in pipeline;
Step 3, takes the grease sample prepared by step 1, by dissolution with solvents, obtains sample solution;
Step 4, chromatographic column is placed on column holder, the sample solution that step 3 is obtained is injected the six-way injection valve of full-automatic tripping device, brings sample solution into chromatographic column, complete sample introduction, and proceed wash-out by nonpolar eluent;
Concrete, described step 4 comprises: chromatographic column is placed on column holder, and the first multiplexer channel selector valve is communicated with the sample solution obtained by step 3, and sample solution is by entering quantitative loop after six-way injection valve; Six-way injection valve carries out gear switch, and quantitative loop is communicated with chromatographic column with the second pump machanism, accesses nonpolar eluent, nonpolar eluent enters quantitative loop by six-way injection valve, sample solution in quantitative loop is taken to chromatographic column by nonpolar eluent, completes sample introduction, and proceeds wash-out;
Step 5, start-up detector, Real-Time Monitoring, obtains elution chromatography figure;
Step 6, judge eluent acquisition time according to the elution chromatography figure that step 5 obtains, eluents all in this time collected by automatic collector;
Step 7, collects step 6 eluent obtained and revolves steaming, weighs 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 DEG C.
Preferably, detecting device is ultraviolet deuterium lamp detecting device, and determined wavelength is 200nm.
Beneficial effect of the present invention:
1. full-automatic tripping device of the present invention can realize auto injection and chromatographic column automatic switchover, and the multiple sample of process, automatically collects, realize high flux quick separating continuously, ensures process stability and result accuracy.
2. adopt detecting device online UV detect, monitor separation component in real time, guarantee being separated completely of polar compound and non-polar component, it is delayed to solve separating effect checking.
3. full-automatic operation avoids the impact of human factor on result; Adopt valveless metering pump, flow velocity is steady, precision is high, resistance tocrocking is strong, ensures collimation and the reappearance of separating resulting; Automatic sample handling system adopts quantitative loop to ensure, and sample introduction is mentioned accurately, reproduction.
4. the separation method of edible oil polar compound of the present invention chooses existing or commercially available separating column, exempts manual dress post and fills out front preliminary work, time saving and energy saving, stability and favorable reproducibility.
5. possess flow velocity zero offset capability, make result more accurate, stable, can save operating personnel carries out manual synchronizing simultaneously, avoids waste unnecessary time and reagent.
Accompanying drawing explanation
Fig. 1 is the structural representation of an embodiment of the full-automatic tripping device of the present invention
Fig. 2 is the annexation schematic diagram of an embodiment of the full-automatic tripping device of the present invention
Fig. 3 is the structural representation of automatic sample handling system in the full-automatic tripping device of the present invention
Fig. 4 is the structural representation of the present invention's full-automatic tripping device center pillar switched system
Fig. 5 is the structural representation of automatic separation system in the full-automatic tripping device of the present invention
Fig. 6 is the structural representation of temperature control system in the full-automatic tripping device of the present invention
Fig. 7 is the present invention's full-automatic tripping device cleaning fluid path figure
Fig. 8 is the present invention's full-automatic tripping device sample introduction fluid path figure
Fig. 9 is that the present invention's full-automatic tripping device profit sample/sample enters post fluid path figure
Figure 10 A and Figure 10 B is an embodiment schematic diagram of solvent barrel pick-up unit in the full-automatic tripping device of the present invention
Figure 11 is another embodiment schematic diagram of solvent barrel pick-up unit in the full-automatic tripping device of the present invention
Figure 12 A and 12B is an embodiment schematic diagram of waste liquid barrel pick-up unit in the full-automatic tripping device of the present invention
Figure 13 is an embodiment schematic diagram of apparatus for testing weeping in the full-automatic tripping device of the present invention
Figure 14 A and Figure 14 B is an embodiment schematic diagram of flow velocity automatic correction device in the full-automatic tripping device of the present invention
Embodiment
Below in conjunction with accompanying drawing, embodiment of the present invention is clearly and completely described.
Fig. 1-6 is an embodiment of the full-automatic tripping device of the present invention.
With reference to accompanying drawing 1, full-automatic tripping device comprises automatic sample handling system 100, post switched system 200, automatic separation system 300 and temperature control system 400.
With reference to accompanying drawing 203, automatic sample handling system 100 comprises 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 is with quantitative loop 105, and the first pump machanism 101 is connected with six-way injection valve 102 pipeline.Optionally, the first pump machanism 101 comprises syringe pump 106 and T-valve 107, and syringe pump 106 is connected with T-valve 107 pipeline, and T-valve is connected with waste liquid barrel 108 pipeline; First multiplexer channel selector valve 103 can select six-way valve, and comprise 6 sample intake passages, wherein path 10 3-1 to 103-5 can be set to sample channel, is connected with sample liquid 110 pipeline, and 103-6 channel setting is flushing channel, is connected with cleaning fluid 111 pipeline.The reagent of automatic sample handling system 100 is placed in reagent rack 109.
With reference to accompanying drawing 2, accompanying drawing 4, post switched system 200 comprises the second multiplexer channel selector valve 201, the 3rd multiplexer channel selector valve 202, column holder mechanism 203 and the second electrical control mechanism 204, described column holder mechanism is provided with chromatographic column 205, second multiplexer channel selector valve 201 and the 3rd multiplexer channel selector valve 202 lay respectively at the first column holder mechanism about 203 both sides, and the second multiplexer channel selector valve 201 is connected with six-way injection valve 102 pipeline.Optionally, column holder mechanism 203 is that the upper and lower adjustable column holder of slide rail type is high to adapt to different post, widens the usable range of pillar.
With reference to accompanying drawing 2, accompanying drawing 5, automatic separation system 300 comprises the second pump machanism 301, detecting device 302, automatic collector 303, the 3rd electrical control mechanism 304 and industrial computer 305, second pump machanism 301 and is connected with six-way injection valve 102 and the 3rd multiplexer channel selector valve 202 pipeline respectively.Optionally, second pump machanism 301 can be ceramic valveless metering pump, and support binary solvent conveying, mobile phase solvent A and solvent B enters valveless metering pump after solenoid valve 306, easy cleaning is safeguarded, change in flow is 1-200ml/min, maximum withstand voltage be 200psi (14bar/1.4MPa), also comprise mixer 307 simultaneously, mixer 307 is for fully mixing solvent orange 2 A and solvent B, and pressure-detecting device 308, when exceeding set pressure, system alarm.Also comprise the second column holder mechanism 309, comprise different model liner, to adapt to multiple column type.Optionally, detecting device employing wavelength is the deuterium lamp UV-detector of 200nm-400nm, in detection simultaneously, can coordinate realize smartphone with control system in process of the test.Optionally, automatic collector has X/Y axle two dimension telecontrol equipment, height adjuster, gatherer pallet automatically, and wherein gatherer pallet is provided with liquid leakage tank and leakage diversion Design, leakage can be drawn.Industrial computer 305 have employed built-in industrial control machine and chromatographic analysis system, operation intuitive and convenient, and data transmission accurately and timely.
With reference to accompanying drawing 2, accompanying drawing 6, temperature control system 400 comprises refrigeration mechanism 401, touch-screen 402 and the 4th electrical control mechanism 404.Wherein, touch-screen 402 is adopted to carry out the operation such as temperature regulating and controlling, temperature data display; Solvent barrel 405 and 406 is respectively used to the solvent orange 2 A and the solvent B that are stored as mobile phase.Because sherwood oil easily gasifies, in order to prevent pump from gasifying when drawing sherwood oil, causing fluid flow inaccurate, under design refrigeration mechanism ensures that sherwood oil is in low temperature environment, improving system accuracy.In the present invention, refrigeration mechanism 401 is according to semiconductor refrigerating principle, use PID temperature control regulating system as input, semiconductor chilling plate exports as temperature, multiple cooling piece carries out transmission cryogenic temperature to cold temperature groove, and then solvent bottle is freezed, and the heat radiation action of cooling piece radiating surface is carried out with fan, carry out Rapid Thermal exchange.
Above-mentioned first electrical control mechanism 104, second electrical control mechanism 204, the 3rd electrical control mechanism 304 and the 4th electrical control mechanism 404 are integrated by automatically controlled original paper; slave computer guarantee is provided; its rear end comprises communication interface; electrically connected with industrial computer 305 respectively by communication interface, electrical control mechanism rear end also comprises power switch and other interface (as power-off protection etc.).
Optionally, use motor, if stepper motor is as topworks, utilize stepper motor to drive the operations such as control pump, six-way injection valve, multiplexer channel selector valve, height adjuster, realize mechanical automation and control.
Below in conjunction with accompanying drawing 7-9, the fluid path figure of the full-automatic tripping device of the present invention is described further.
Cleaning
With reference to accompanying drawing 7, before sample introduction, syringe pump 106 is existing to be cleaned (now quantitative loop 105 communicates with separation flow path) pipeline, first passage selects six-way valve 103 to open, cleaning fluid 111 is inhaled into the public pipeline of six-way injection valve 102, entered by 1 right side mouth from T-valve 107 by six-way injection valve 102-6 position, be inhaled in syringe pump 106, to reach the object of cleaning public pipeline, syringe pump 106, after reaching cleaning capacity, T-valve 107 switches, and waste liquid is discharged through T-valve 107 by syringe pump 106.
Sample introduction
With reference to accompanying drawing 8, after cleaned, automatic sampling apparatus 100 carries out sample introduction (now quantitative loop 105 communicates with sampling stream), on first multiplexer channel selector valve 103, respective channel is opened, sample liquid 111 is inhaled into the public pipeline of second channel selector valve, quantitative loop is entered through 5 by six-way injection valve 102-6 position, in quantitative loop, original liquid is entered by 1 right side mouth from T-valve 107 through 2, be inhaled in syringe pump 106, after reaching setting capacity, T-valve 107 switches, and waste liquid is discharged through T-valve 107 by syringe pump 106.
Profit sample/sample enters post
With reference to accompanying drawing 9, six-way injection valve 102 carries out gear switch, quantitative loop 105 is connected with chromatographic column 205 with the second pump machanism 301, mobile phase enters quantitative loop 105 by six-way injection valve 102-3 position through 2, sample in quantitative loop 105 is taken chromatographic column 205 through 4 by mobile phase by 5, completes sample introduction.After having run sampling step, injector progressively completes profit post-sample introduction-operation gradient according to the step arranged automatically, realizes the automatic switchover sample introduction of maximum 5 kinds of samples.
In an optional embodiment, full-automatic tripping device also comprises earth leakage circuit-breaker.Due to a lot of with solvent contacts in chemical experiment, when the hand contact instrument that experiment operator is moist or plug power supply, especially the instrument of metal shell, probably can there is electric shock phenomenon, therefore, the earth leakage protective air switch of band is added in instrument, 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, on zero line earth leakage circuit-breaker being received power supply (such as: 220V/50Hz alternating current) input end and live wire, zero line and fire wire output end are accessed earth leakage protective device end (such as: 24V Switching Power Supply, 48V Switching Power Supply, industrial computer adapter and detecting device etc.), selection rated current is 2A, leakage current is the earth leakage circuit-breaker of 30mA, when to be short-circuited in system or load current is greater than 2A, or system generation leaky, when leakage current is greater than 30mA, earth leakage circuit-breaker will cut off main circuit automatically, realize the safeguard protection of earth leakage circuit-breaker to instrument and personnel.
In an optional embodiment, full-automatic tripping device also comprises solvent barrel pick-up unit, and when detecting solvent-free in solvent barrel, system halt runs, and audio alert.When instrument runs in unattended situation, when the solvent in solvent barrel is finished, instrument can detect has not had solvent, now instrument self enters halted state, and with voice, user is pointed out, after operating personnel add solvent in solvent barrel, click and continue to run, if instrument detects in solvent barrel have solvent, eliminate the experiment that language alarm proceeding does not complete.
Solvent barrel pick-up unit can be Photoelectric Detection, with reference to accompanying drawing 10A, the principle different with the refractive index of liquid 12 to light according to air 11, because air 11 does not almost reflect light, when the light of light source 13 is by after air 11, receiving end 14 all can receive the energy of light, when by liquid 12, because liquid 12 has certain refraction, the energy dropoff of the light that receiving end 14 receives, can judge whether have liquid to flow through in pipeline, when not having liquid in pipeline, can judge there is no solvent in solvent barrel, otherwise have solvent in solvent barrel.Concrete, with reference to accompanying drawing 10B, photoelectric sensor comprises light source transmitting terminal 13 and light source receiving end 14, and light source transmitting terminal 13 and light source receiving end 14 are positioned at pipeline 15 two ends above solvent barrel, control line is linked on control circuit board, when there being liquid in pipeline, photoelectric sensor exports high level, when there is no liquid in pipeline, photoelectric sensor output low level, after control panel receives low level, suspend valveless metering pump, start speech ciphering equipment, send voice message, send out communication command to industrial computer simultaneously, after industrial computer receives order, at software interface display warning information.
Solvent barrel pick-up unit also can be pressure detection, after liquid compression air, air pressure becomes large principle, utilize the pressure in two micropressure sensor signal pipings, a micropressure sensor contacts with air, detect air pressure to hold as a comparison, pressure in a micropressure sensor signal piping is as test side, pipeline one termination micropressure sensor, in one end access solvent barrel, when there being liquid in solvent barrel, liquid compression air in pipeline, pressure ratio air pressure in pipeline is large, the force value comparison of the pressure transducer of test side is larger than the force value of end, namely detect in solvent barrel have pressure, along with the solvent in solvent barrel reduces, in pipeline, the pressure of liquid compression air reduces.When not having liquid in solvent barrel, the pressure in pipeline is air pressure, and now the pressure of two micropressure sensors is substantially equal, now detects that solvent barrel is empty, otherwise the pressure ratio contrast end pressure of test side is large, namely has solvent in solvent barrel.Concrete, with reference to accompanying drawing 11, in instrument, two micropressure sensors are installed, a sensor (not shown on figure) communicates with air, a sensor 16 accesses one section of pipeline 17 and stretches in solvent barrel 406, the AD converter interface of the signal wire Access Control plate of two sensors, control panel detects the numerical values recited of two signal wires in real time, judges whether have solvent in solvent barrel by comparing two pressure sensor signal values.Utilize this device to detect, not only can detect in solvent barrel whether have solvent, the height of the solvent liquid level in solvent barrel can also be detected.
In an optional embodiment, described full-automatic tripping device also comprises waste liquid barrel pick-up unit.Instrument is when unattended operation, and when the waste liquid in waste liquid barrel is full, operation suspension together, and carry out voice message, after changing empty waste liquid barrel, click and continue to run, instrument proceeds the experiment do not completed.This function can avoid the waste liquor contamination operator's console overflowed, and after waste liquid can be avoided to overflow, is evaporated to air, damages experimenter's health.Wherein, waste liquid barrel pick-up unit can be capacitive transducer, with reference to accompanying drawing 12A, because any material all can have certain specific inductive capacity, capacitive approach switch therefore can be adopted as detecting the whether full sensor of waste liquid.The probe of capacitive approach switch is the concussion loop with certain frequency, and when there being material close to this probe, the frequency of oscillation circuit there occurs change, can judge have object proximity to pop one's head according to this change.Concrete, with reference to accompanying drawing 12B, described capacitive transducer 21 is fixed on waste liquid barrel 22 mouthfuls, when waste liquid liquid level reach a certain height, capacitive transducer detects solvent liquid level, capacitive transducer generation switching signal to control panel, after control panel receives switching signal, suspend valveless metering pump, start speech ciphering equipment, send voice message, send out communication command to industrial computer simultaneously, after industrial computer receives order, at software interface display warning information.
In an optional embodiment, full-automatic tripping device also comprises apparatus for testing weeping.Instrument is in operational process; often there will be pipe joint leakage, or the situation that pipeline bursts apart, because instrument internal has electrical equipment; if find leakage not in time; can cause the waste of experimental period and reagent, serious likely can cause instrument damage and personal safety injury, and therefore instrument internal needs to add apparatus for testing weeping; when instrument internal has leak of liquid; instrument can detect, and stops the operation of pump in time, avoids losing time and reagent.Thermistor is the resistance that a kind of resistance value changes along with environment temperature, and leakage detects and adopts thermistor as leakage detection probe, when make use of liquid gasification, and liquid absorption heat, the principle that temperature reduces.Concrete, apparatus for testing weeping can be positioned at automatic separation system bottom, detects the leakage that fluid path original paper (as pipeline, pump machanism, valve etc.) region may occur.Fluidic leak detector has two thermistors as detection probe, and logical direct current or alternating current, when not having liquid comes into contact, two thermistors are in the same space, equal by electric current, and therefore the temperature of two thermistors is in the state of phase isoequilibrium.When one of them thermistor has liquid comes into contact, thermistor generates heat, and makes liquid gasification, takes away heat simultaneously, and thermistor temp reduces, and the temperature out of trim of two thermistors, now instrument has been detected as leakage.Concrete, with reference to accompanying drawing 13, apparatus for testing weeping comprises the thermistor of two identical characteristics, connect thermistor a small resistor (10 ohms) formation temperature sensors A and temperature sensor B respectively, two temperature sensor circuits add the DC voltage of 24V respectively, utilize the magnitude of voltage being gathered small resistor two ends by Chip Microcomputer A/D interface, when temperature does not change, two small resistor direct voltages are equal, when there being liquid comes into contact, the thermistor of test side reduces, electric current increases, the magnitude of voltage collected becomes large, now Instrumental results is leakage.
In an optional embodiment, described full-automatic tripping device also comprises pressure-detecting device, for detecting instrument in operational process, and pressure surge situation and pipeline whether superpressure in pipeline.Wherein, pressure-detecting device can be positioned at automatic separation system top, is connected on the pipeline between mixer and chromatographic column, senses line pressure in real time.When there being liquid flow in pipeline, liquid has certain pressure to pipeline arm, and solvent in piezoresistive pressure transmitter signal piping can be utilized the pressure of pipeline arm.Concrete, piezoresistive pressure transmitter, according to the size of probe pressure, exports the current signal of 4mA-20mA, utilize Chip Microcomputer A/D output terminal, be the digital signal of 0V-3.3V the analog-signal transitions of 4mA-20mA, then according to reduction formula, force value be presented on screen.
In an optional embodiment, described full-automatic tripping device also comprises flow velocity automatic correction device.Because infusion pump is in operational process, because pipe joint does not connect, or the not equal various subjectivity of solvent density, temperature or odjective cause cause the flow velocity of pump and the flow velocity of setting not to meet, now, instrument itself and can arrange flow velocity and contrasts according to the flow velocity size flow through in pipeline, carry out automatic calibration, operating personnel can be saved and carry out manual synchronizing, avoid waste unnecessary time and reagent.
Flow rate pump automatic calibration, can measure the actual flow velocity in pipeline according to Pitot tube measuring principle.Pitot tube is by measuring the total head pressure of fluid and the difference of statical head, namely the device of flow rate of liquid measured by dynamic head, also dynamic pressure measurement pipe is claimed, with reference to accompanying drawing 14A, its front end central small hole 41 is for measuring the total head pressure of fluid, row's aperture 42 on side surface is for measuring hydrostatic head, Pitot tube head has ellipse, taper and spherical structure, when measuring rate of flow of fluid, the head of Pitot tube is inserted the mensuration place of runner, with reference to accompanying drawing 14B, the central small hole of Pitot tube head will be met to fluid, and wherein positive axis should be parallel with fluid flowing path direction.The inner sleeve 43 that Pitot tube stretches out and outer tube 44 access differential pressure micropressure sensor 45, export the difference of total head and static pressure:
H
dynamic=h
entirely-h
quiet
Record h
dynamicafter, according to the relation of flow velocity and dynamic pressure, the flow velocity of fluid can be obtained:
Because
So
Thus obtain flow further
Q＝ω·Fm
3/s
In formula: rate of flow of fluid in ω-pipeline, unit m/s; Q-pipeline section amasss, unit m
2.
In addition, thermopair can also be added between Pitot tube outer tube and inner sleeve, and draw signal wire, the temperature of liquid in pipeline can be measured simultaneously.
Concrete, in pipeline, the Pitot tube 46 that a length of tape has thermopair is accessed in the present invention, differential pressure micro-pressure transmitter 45 is added at outer tube 44 and inner sleeve 43 air end, thermocouple signal end and pressure unit signal end access Chip Microcomputer A/D input interface, be digital signal by AD conversion, with flow velocity be set contrast, regulate the rotating speed of pump according to comparison structure, realize the zero offset capability of flow velocity.
In addition, this flow velocity automatic correction device is not limited only to, in the disclosed full-automatic tripping device of the embodiment of the present invention, also may be used for other instrument relating to fluid path as liquid chromatograph, gas chromatograph, Chemical Decomposition system etc.
In addition, the present invention also provides a kind of edible oil polar compound separation method, is below a concrete embodiment:
1 sample prepares
1.1 the removal of impurity
Sample as sample should be liquid, clarifies, also fully mixes without precipitation.If sample is not clarified, have precipitation, then in the water-bath that grease must be placed in 50 DEG C or thermostatic drying chamber, by the heating temperatures to 50 of grease DEG C and shake well to melt possible fat crystals.If now oil sample becomes clarification, without precipitation, then can be used as sample, otherwise grease should be placed in the thermostatic drying chamber of 50 DEG C, with the insoluble impurity of Filter paper filtering, get the supernatant liquid grease after filtration as sample, for preventing Oxidation of Fat and Oils, filter process should complete as early as possible.
For solidifying point higher than 50 DEG C or containing solidifying point higher than the sample of 50 DEG C of lubricant components, then in the water-bath that grease must be placed in higher than its solidifying point about 10 DEG C or thermostatic drying chamber, by grease heating and shake well to melt possible fat crystals.Filter if also need, be then placed in by grease in the thermostatic drying chamber of higher than its solidifying point about 10 DEG C, with the insoluble impurity of Filter paper filtering, get the supernatant liquid grease 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 grease, must drying and dehydrating be carried out.For under room temperature be liquid, without the grease of obvious crystallization or solidification phenomenon, and through " 1.1 " process and after being cooled to room temperature for liquid, without the grease of obvious crystallization or solidification phenomenon, the ratio that can add 1g ~ 2g anhydrous sodium sulfate in every 10g grease adds anhydrous sodium sulfate, and be fully uniformly mixed adsorption dewatering, then use Filter paper filtering, get the supernatant liquid grease after filtration as sample.
For the grease having crystallization or solidification phenomenon under room temperature, and through " 1.1 " process and have the grease of obvious crystallization or solidification phenomenon after being cooled to room temperature, anhydrous sodium sulfate adsorption dewatering is used again after oil sample can being dissolved completely with appropriate sherwood oil, then Filter paper filtering collects filtrate, filtrate being placed in bath temperature is in the Rotary Evaporators of 45 DEG C, under condition of negative pressure, solvent is wherein rotated evaporate to dryness, gets residual supernatant liquid grease as sample.
The activation of 2 chromatographic columns
Carry out rinse with non-polar component eluent for the mobile phase pipeline of mobile phase to full-automatic tripping device, drain the gas in mobile phase pipeline.Get 1 chromatographic column, connect into the mobile phase pipeline of full-automatic tripping device, with non-polar component eluent for mobile phase, the flow velocity of 25mL/min rinses chromatographic column 10min, make chromatographic column completely infiltrate by solvent.
The separation of 3 non-polar component
Get 1 clean 10mL glass beaker, accurately take the oil sample (m) of 1g (being accurate to 0.001g), then use the sherwood oil of 5mL (30 DEG C ~ 60 DEG C boiling ranges) fully to be dissolved by oil sample, become sample solution.First FLASH chromatographic column and mobile phase pipeline are disconnected, sample solution is injected into the porch, upper end of chromatographic column, the sherwood oil of 3mL (30 DEG C ~ 60 DEG C boiling ranges) is used to wash sample solution residual in 10mL glass beaker again, cleansing solution is also with the porch, upper end being injected into chromatographic column, again the upper end of FLASH chromatographic column is connected with mobile phase pipeline, carries out the separation of non-polar component by following parameter:
A) mobile phase: non-polar component eluent;
B) flow rate of mobile phase: 25mL/min;
C) fraction collector: with 1000mL osculum glass receiving flask, be collection container, collect with full collection mode from wash-out;
D) UV-detector monitoring wavelength: 200nm;
E) enable real-time monitoring system, obtain elution chromatography figure;
F) solvent temperature control system temperature: 10 DEG C;
G) elution time: 11min.
When carrying out lock out operation, the environment temperature of experiment should control between 10 DEG C ~ 25 DEG C.
The collection of 4 non-polar component, concentrated and quantitatively
Get the thermostatic drying chamber that 1 clean 500mL flask puts into (103 ± 2) DEG C, dry about 1h, then take out and put into glass desicator immediately and be cooled to room temperature, then weigh (M0).According to the Real-time Monitoring Data that " 3 " lock out operation obtains, the end time point of the chromatographic peak that non-polar component is maximum should control in 4.5min ~ 6.8min interval, is now that the eluent (in 1000mL osculum glass receiving flask) of all collections in 0min ~ 11min is poured in this 500mL round-bottomed flask by elution time interval.
Then this is equipped with and collects the 500mL flask of eluent to be placed in bath temperature be in the Rotary Evaporators of 60 DEG C, under condition of normal pressure, by solvent major part evaporation wherein, and then under condition of negative pressure, a small amount of solvent rotary evaporation will be remained near dry, and take out this flask and dry the water of flask outer wall.Then this 500mL flask is put into the vacuum constant temperature drying box of 40 DEG C, under the condition of negative pressure of 0.1MPa, dry 20min ~ 30min, put into glass desicator after terminating and be cooled to room temperature, then weigh (M1), and (M1-M0) is the quality of non-polar component.
Above-described embodiment is only for illustrating technical conceive of the present invention and feature, and not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement etc., all should be included within protection scope of the present invention.
Claims (21)
1. a full-automatic tripping device, is characterized in that: comprise automatic sample handling system, post switched system, automatic separation system;
Described automatic sample handling system comprises the first pump machanism, six-way injection valve, the first multiplexer channel selector valve and the first electrical control mechanism, and described six-way injection valve is with quantitative loop, and described first pump machanism is connected with six-way injection valve pipeline;
Described post switched system comprises the second multiplexer channel selector valve, the 3rd multiplexer channel selector valve, column holder mechanism and the second electrical control mechanism, described column holder mechanism is for placing chromatographic column, described second multiplexer channel selector 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 selector valve is connected with six-way injection valve pipeline;
Described automatic separation system comprises the second pump machanism, detecting device, automatic collector, the 3rd electrical control mechanism and industrial computer, and described second pump machanism is connected with six-way injection valve and the 3rd multiplexer channel selector valve pipeline respectively.
2. full-automatic tripping device as claimed in claim 1, it is characterized in that, also comprise temperature control system in described full-automatic tripping device, described temperature control system comprises refrigeration mechanism and the 4th electrical control mechanism.
3. full-automatic tripping device as claimed in claim 2, is characterized in that: described refrigeration mechanism comprises semiconductor chilling plate, cold temperature groove and fan.
4. the full-automatic tripping device as described in any one of claim 1-3, is characterized in that: described full-automatic tripping device also comprises stepper motor, drives pump machanism, six-way injection valve, multiplexer channel selector valve by stepper motor.
5. the full-automatic tripping device as described in any one of claim 1-3, is characterized in that: described first pump machanism comprises syringe pump and T-valve, and described syringe pump is connected with T-valve pipeline, and described T-valve is connected with waste liquid barrel pipeline.
6. the full-automatic tripping device as described in any one of claim 1-3, is characterized in that: described second pump machanism comprises valveless metering pump.
7. full-automatic tripping device as claimed in claim 1, is characterized in that: described automatic collector comprises X/Y axle two dimension autonomous movement locating device, arrangement for adjusting height and gatherer pallet, and described gatherer pallet arranges liquid leakage tank and flow-guiding channel.
8. full-automatic tripping device as claimed in claim 1, is characterized in that: described full-automatic tripping device also comprises earth leakage circuit-breaker.
9. full-automatic tripping device as claimed in claim 1, is characterized in that: described full-automatic tripping device also comprises solvent barrel pick-up unit.
10. full-automatic tripping device as claimed in claim 9, is characterized in that: described solvent barrel pick-up unit comprises photoelectric sensor or pressure transducer.
11. full-automatic tripping devices as claimed in claim 1, it is characterized in that: described full-automatic tripping device also comprises waste liquid barrel pick-up unit, described waste liquid barrel pick-up unit is capacitive transducer.
12. full-automatic tripping devices as claimed in claim 1, is characterized in that: described full-automatic tripping device also comprises apparatus for testing weeping, and described apparatus for testing weeping comprises the thermistor of two identical characteristics.
13. full-automatic tripping devices as claimed in claim 1, is characterized in that: described full-automatic tripping device also comprises pressure-detecting device, and described pressure-detecting device comprises piezoresistive pressure transmitter.
14. full-automatic tripping devices as claimed in claim 1, it is characterized in that: described full-automatic tripping device also comprises flow velocity automatic correction device, described flow velocity automatic correction device comprises Pitot tube and pressure reduction pressure transducer.
15. full-automatic tripping devices as claimed in claim 14, it is characterized in that: described Pitot tube comprises interior pipe, outer tube, baroport and pitot hole, described pitot hole is positioned at the head of Pitot tube, and described baroport is positioned at Pitot tube side surface, at interior pipe and outer tube access pressure reduction pressure transducer.
16. full-automatic polarity edible oil polar compound piece-rate systems as described in claims 14 or 15, is characterized in that: arrange thermopair in described Pitot tube.
17. 1 kinds of edible oil polar compound separation methods, is characterized in that: this separation method uses the full-automatic tripping device as described in any one of claim 1-16, and separation method concrete steps are as follows:
Step 1, is prepared into clarification, without the liquid fat sample precipitated by edible oil;
Step 2, uses nonpolar eluent to clean pipeline in full-automatic tripping device;
Step 3, takes the grease sample prepared by step 1, by dissolution with solvents, obtains sample solution;
Step 4, chromatographic column is placed on column holder, the sample solution that step 3 is obtained is injected the six-way injection valve of full-automatic tripping device, brings sample solution into chromatographic column, complete sample introduction, and proceed wash-out by nonpolar eluent;
Step 5, start-up detector, Real-Time Monitoring, obtains elution chromatography figure;
Step 6, judge eluent acquisition time according to the elution chromatography figure that step 5 obtains, eluents all in this time collected by automatic collector;
Step 7, collects step 6 eluent obtained and revolves steaming, weighs the quality of non-polar component.
18. separation methods as claimed in claim 17, it is characterized in that: described step 2 comprises: the first multiplexer channel selector valve is communicated with non-polar component eluent, non-polar component eluent enters the public pipeline of six-way injection valve, the first pump machanism is inhaled into through six-way injection valve, rinse is carried out to public pipeline, after cleaning, drains the gas in pipeline.
19. separation methods as claimed in claim 17, is characterized in that: described step 4 comprises: chromatographic column is placed on column holder, the first multiplexer channel selector valve is communicated with the sample solution obtained by step 3, and sample solution is by entering quantitative loop after six-way injection valve; Six-way injection valve carries out gear switch, and quantitative loop is communicated with chromatographic column with the second pump machanism, accesses nonpolar eluent, nonpolar eluent enters quantitative loop by six-way injection valve, sample solution in quantitative loop is taken to chromatographic column by nonpolar eluent, completes sample introduction, and proceeds wash-out.
20. separation methods as claimed in claim 17, described nonpolar eluent flow rate is 25mL/min, and mobile phase temperature is 10 DEG C.
21. separation methods as claimed in claim 17, described detecting device is ultraviolet deuterium lamp detecting device, and determined wavelength is 200nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410709516.3A CN104407083B (en) | 2014-11-28 | 2014-11-28 | Full-automatic piece-rate system and the application in edible oil polar compound separates thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410709516.3A CN104407083B (en) | 2014-11-28 | 2014-11-28 | Full-automatic piece-rate system and the application in edible oil polar compound separates thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104407083A true CN104407083A (en) | 2015-03-11 |
| CN104407083B CN104407083B (en) | 2016-08-31 |
Family
ID=52644730
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410709516.3A Active CN104407083B (en) | 2014-11-28 | 2014-11-28 | Full-automatic piece-rate system and the application in edible oil polar compound separates thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104407083B (en) |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104655768A (en) * | 2015-03-11 | 2015-05-27 | 天津博纳艾杰尔科技有限公司 | Automatic crude oil component separating device and application of automatic crude oil component separating device in separation wax and colloid in crude oil |
| CN105891391A (en) * | 2016-06-29 | 2016-08-24 | 天津博纳艾杰尔科技有限公司 | Automatic sampling device |
| CN108028154A (en) * | 2015-10-07 | 2018-05-11 | 迪睿合株式会社 | Liquid leaching sensor, switch element, battery system |
| CN108896690A (en) * | 2018-07-16 | 2018-11-27 | 中国矿业大学 | A kind of the HPLC sampling device and sample injection method of multi pass acquisition |
| CN109459462A (en) * | 2018-10-31 | 2019-03-12 | 泉州市全通光电科技有限公司 | A kind of automatic freezing point apparatus and its test method |
| 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 |
| CN109669033A (en) * | 2017-10-17 | 2019-04-23 | 普瑞邦（北京）科技有限公司 | A kind of immune affinity column operating device |
| CN109752532A (en) * | 2017-11-03 | 2019-05-14 | 中国人民解放军军事医学科学院放射与辐射医学研究所 | A kind of incubation sampling device based on the detection of multichannel immunochromatography |
| 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 |
| CN112666293A (en) * | 2020-12-19 | 2021-04-16 | 北京大学 | Liquid phase automatic synthesizer |
| WO2021249347A1 (en) * | 2020-06-10 | 2021-12-16 | 上海贝高医疗科技有限公司 | Static sample injection and fraction collection apparatus for use with liquid chromatograph |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03175355A (en) * | 1989-09-12 | 1991-07-30 | Eisai Co Ltd | Method and apparatus for converting mobile phase in high performance liquid chromatography mass analysis |
| US6415670B1 (en) * | 1999-03-26 | 2002-07-09 | Yamazen Corporation | Injection apparatus |
| US20040219071A1 (en) * | 2001-04-25 | 2004-11-04 | Can Ozbal | System and method for high throughput sample preparation and analysis using column chromatography |
| 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 |
| JP2013024601A (en) * | 2011-07-15 | 2013-02-04 | Shimadzu Corp | Liquid chromatograph and program |
-
2014
- 2014-11-28 CN CN201410709516.3A patent/CN104407083B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03175355A (en) * | 1989-09-12 | 1991-07-30 | Eisai Co Ltd | Method and apparatus for converting mobile phase in high performance liquid chromatography mass analysis |
| US6415670B1 (en) * | 1999-03-26 | 2002-07-09 | Yamazen Corporation | Injection apparatus |
| US20040219071A1 (en) * | 2001-04-25 | 2004-11-04 | Can Ozbal | System and method for high throughput sample preparation and analysis using column chromatography |
| 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 |
| JP2013024601A (en) * | 2011-07-15 | 2013-02-04 | Shimadzu Corp | Liquid chromatograph and program |
Non-Patent Citations (1)
| Title |
|---|
| 中华人民共和国国家卫生和计划生育委员会 发布: "食品安全国家标准 食用油中极性组分（PC）的测定", 《道客巴巴》, 17 November 2014 (2014-11-17) * |
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104655768A (en) * | 2015-03-11 | 2015-05-27 | 天津博纳艾杰尔科技有限公司 | Automatic crude oil component separating device and application of automatic crude oil component separating device in separation wax and colloid in crude oil |
| CN108028154A (en) * | 2015-10-07 | 2018-05-11 | 迪睿合株式会社 | Liquid leaching sensor, switch element, battery system |
| CN108028154B (en) * | 2015-10-07 | 2020-11-10 | 迪睿合株式会社 | Liquid immersion sensor, switching element, and battery system |
| CN105891391A (en) * | 2016-06-29 | 2016-08-24 | 天津博纳艾杰尔科技有限公司 | Automatic sampling device |
| CN105891391B (en) * | 2016-06-29 | 2019-02-12 | 天津博纳艾杰尔科技有限公司 | A kind of automatic sampling apparatus |
| CN109669033A (en) * | 2017-10-17 | 2019-04-23 | 普瑞邦（北京）科技有限公司 | A kind of immune affinity column operating device |
| CN109752532A (en) * | 2017-11-03 | 2019-05-14 | 中国人民解放军军事医学科学院放射与辐射医学研究所 | A kind of incubation sampling device based on the detection of multichannel immunochromatography |
| CN109752532B (en) * | 2017-11-03 | 2022-04-15 | 中国人民解放军军事医学科学院放射与辐射医学研究所 | Incubation sample loading device based on multi-channel immunochromatography detection |
| CN108896690A (en) * | 2018-07-16 | 2018-11-27 | 中国矿业大学 | A kind of the HPLC sampling device and sample injection method of multi pass acquisition |
| CN109459462A (en) * | 2018-10-31 | 2019-03-12 | 泉州市全通光电科技有限公司 | A kind of automatic freezing point apparatus and its test method |
| 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 |
| WO2021249347A1 (en) * | 2020-06-10 | 2021-12-16 | 上海贝高医疗科技有限公司 | Static sample injection and fraction collection apparatus for use with liquid chromatograph |
| CN112666293A (en) * | 2020-12-19 | 2021-04-16 | 北京大学 | Liquid phase automatic synthesizer |
| CN112666293B (en) * | 2020-12-19 | 2022-05-13 | 北京大学 | Liquid phase automatic synthesizer |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104407083B (en) | 2016-08-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104407083A (en) | Full-automatic separation system and application of full-automatic separation system in separation of polar components in edible oil | |
| CN101487806B (en) | DSC meter with visualization function | |
| CN102564783B (en) | Thermal performance test system of solar water heater | |
| CN209656638U (en) | A kind of VOCs on-line detector | |
| CN103604909A (en) | Multipath gas on-line real-time monitoring method and apparatus | |
| CN107748214A (en) | The pretreatment of volatile organic matter and analysis system | |
| CN204008081U (en) | A kind of faucet valve core detection system | |
| CN201331502Y (en) | Differential scanning calorimeter compatible with visible function | |
| CN208937372U (en) | A kind of water sampling equipment that can acquire multilayer water sample simultaneously | |
| CN103018780B (en) | A kind of Probe-type high-frequency-respoliquid liquid metal leakage detector | |
| CN220153688U (en) | High-temperature lubricating oil flow standard device | |
| CN107132157A (en) | The experimental provision of Crude viscosity and wax deposit under magnetic fields | |
| CN204495754U (en) | Trace self-flow pattern condensation point of diesel oil on-line determination device | |
| CN103344354B (en) | A kind of In-porous-medium fluid temperature visualization measurement mechanism | |
| CN103808820A (en) | Freon gas detection warning device and detection method thereof | |
| CN104237427B (en) | A kind of liquid chromatogram mobile phase prior-warning device | |
| CN204495682U (en) | RAPID VISCO meter | |
| CN107817264B (en) | Automatic inclination point detector by controllable temperature difference method | |
| CN206609530U (en) | Video image temperature superimposition aims at temp measuring system | |
| CN206696134U (en) | A kind of engine motor oil viscosity detecting device of detectable assigned temperature | |
| CN203965393U (en) | A kind of Freon gas detection alarm instrument | |
| CN212622072U (en) | Novel online viscosity detection system | |
| CN201852604U (en) | Thermal gas mass flow meter | |
| CN204065040U (en) | A kind of liquid chromatogram mobile phase prior-warning device | |
| CN205139252U (en) | On -line monitoring system of high temperature fused salt conductivity |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |