CN209148482U - A kind of capillary viscosity instrument based on micro-example measurement - Google Patents

A kind of capillary viscosity instrument based on micro-example measurement Download PDF

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CN209148482U
CN209148482U CN201821749199.8U CN201821749199U CN209148482U CN 209148482 U CN209148482 U CN 209148482U CN 201821749199 U CN201821749199 U CN 201821749199U CN 209148482 U CN209148482 U CN 209148482U
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capillary
sample
temperature
pressure sensor
pressure
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孙亮
王鹏辉
张志林
王德双
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Chengdu Ke Rui Technology Co Ltd
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Chengdu Ke Rui Technology Co Ltd
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Abstract

The utility model discloses a kind of capillary viscosity instrument based on micro-example measurement, including constant current transfusion system, sample injector, temperature-controlling system, capillary, first pressure sensor, the constant current transfusion system is connect with sample injector, the sample injector is connect with capillary, is provided with first pressure sensor between the capillary and sample injector;The first pressure sensor and capillary are arranged in temperature-controlling system;The constant current transfusion system includes liquid storage bottle, degasser, constant flow high pressure pump, and the constant flow high pressure pump is connect by degasser with liquid storage bottle, and the constant flow high pressure pump is connect with sample injector.This practical measuring accuracy is preferable, while reducing the dosage of sample, without calibration, has widened the sample measurement range of viscosity apparatus, has had preferable practicability.

Description

A kind of capillary viscosity instrument based on micro-example measurement
Technical field
The utility model belongs to the technical field of liquid viscosity measurement, and in particular to a kind of hair based on micro-example measurement Tubule viscosity apparatus.
Background technique
Viscosity is the important physical parameter of fluid, and common viscosity is viscous in respect of rotational viscometer, falling ball viscometer, oscillatory type Spend meter, capillary viscometer etc..First three realizes viscosity measurement using the resistance of motion of fluid, and sample requirements are big, viscosimeter Calculation method is complicated.And most widely used capillary viscometer is calculated as representing with Ubbelohde (Ubbelohde) viscosity, working principle For the fluid flow at the capillary both ends of statistics constant pressure difference, i.e. constant-voltage method.Its structure is simple, and precision is preferable and easy to operate, It is widely used in the viscosity measurements of the liquid such as Polymer Solution, blood plasma, gasoline, diesel oil.But the control of its temperature generally uses water-bath Slot, bulky, heating and cooling are slow, and test takes a long time and manual operation is complicated, it is crucial that non-newtonian flow can not be measured Viscosity of the body (viscosity changes with flow velocity) under different shear rate.And constant speed method capillary tube method measures viscosity, is more common in height Molecule rheometer, although viscosity of the non-newtonian fluid under different shear rate can be measured, but its structure is complex, bulky, Sample consumption is more, and is difficult to clean after.
Existing viscosity measurements means greatest drawback is that required sample size is larger, temperature control is inaccurate, can not measure Non-newtonian fluid and detection efficiency are low.There is presently no the fluids that accurately can quickly measure a small amount of or even micro (< 1ml) sample Viscosity measurements equipment, is still that there are blank especially for the viscosimetric analysis under the different shear rate of non-newtonian fluid.
Utility model content
The purpose of this utility model is to provide a kind of capillary viscosity instrument based on micro-example measurement, this practical surveys Measure accuracy it is preferable, while reduce sample dosage, without calibration, widened the sample measurement range of viscosity apparatus, have compared with Good practicability.
The utility model is achieved through the following technical solutions: a kind of capillary viscosity based on micro-example measurement Instrument, including constant current transfusion system, sample injector, temperature-controlling system, capillary, first pressure sensor, the constant current transfusion system with Sample injector connection, the sample injector are connect with capillary, are provided with first pressure sensor between the capillary and sample injector; The first pressure sensor and capillary are arranged in temperature-controlling system;The constant current transfusion system include liquid storage bottle, degasser, Constant flow high pressure pump, the constant flow high pressure pump are connect by degasser with liquid storage bottle, and the constant flow high pressure pump is connect with sample injector.
It further include second pressure sensor, back pressure regulator device further to preferably realize the utility model, The outlet end of the capillary is disposed with second pressure sensor, back pressure regulator device, and the second pressure sensor is set It sets in temperature-controlling system.
Further include controller further to preferably realize the utility model, the controller respectively with sample introduction Device, temperature-controlling system, first pressure sensor, second pressure sensor, back pressure regulator device, constant flow high pressure pump connection.
The controller be the prior art and be not the utility model improvement, so it will not be repeated.The controller can Think the PCL controller of the AFPX-C40T model of Panasonic/ Panasonic Corporation production, can be Mitsubishi/ Mitsubishi public affairs It takes charge of the PCL controller of the FX3SA-30MT-CM model of production, can be the 30MR model of Mitsubishi/ Mitsubishi production Singlechip controller.The first pressure sensor and second pressure sensor can be the HM22 of Nanjing Hong Mu company production Type high accuracy pressure transmitter can be the T27M01RMF24000#G type high-precision pressure pick-up of Ashcroft company production Device.
In order to preferably realize the utility model, further, temperature is additionally provided between the temperature-controlling system and sample injector Adjusting device is spent, the temperature adjusting device is preheating apparatus or pre- refrigerating plant.
In order to preferably realize the utility model, further, the temperature-controlling system is insulating box or water bath.
In order to preferably realize the utility model, further, the material of the capillary can for stainless steel, PEEK, Any one in quartz glass;The internal diameter of the capillary is 0.1~2mm, 0.1~20m of length.
The utility model includes that constant current transfusion system, sampling system, temperature-controlling system, capillary, pressure detecting and control are System, control and record system and other appurtenances are constituted.Wherein constant current transfusion system is responsible for providing the high-pressure spray of constant flow rate Body mainly includes liquid storage bottle, degasser, constant flow high pressure pump and high-pressure liquid line.Sampling system is responsible for the sample of designated volume Product are introduced into high-pressure liquid line, can be selected liquid chromatogram in widely used six-way injection valve or other with identity function Structure realize.Temperature-controlling system is for guaranteeing that temperature when sample passes through capillary is constant, the constant temperature that can be used temperature-controlled precision high Case or water bath are realized.Pressure detecting and control system are responsible for monitoring the pressure at capillary both ends and adjust the pressure in entire flow path Power is made of pressure sensor and back pressure regulator device.Control is responsible for controlling coordinated scheduling, the number of each subsystem with record system According to record and analysis etc..
Flow media is stored in liquid storage bottle, is entered constant flow high pressure after the gas that degassed machine removing is wherein dissolved and is pumped, high Constant flow pump is pressed to export to after flow media pressurization with constant flow velocity.After being completely filled with flow media in system, capillary enters Pressure at mouthful is stablized constant.After sampling system introduces the sample fluid of certain volume into flow path, flow media can be pushed away Dynamic sample flows through capillary, monitors the pressure difference at capillary both ends, draws pressure drop-time graph, thus can calculate sample Viscosity.In order to preferably measure the viscosity of different samples, above-mentioned test macro can be suitably modified.
It improves 1: in order to reduce error caused by diffusion, the not liquid miscible with sample solution can be filled at sample both ends As spacer medium.For example, perfluoro solvent, paraffin oil, silicone oil etc..
Improve 2: according to the viscosity of different samples, the replaceable different length of test temperature, internal diameter capillary.To avoid inhaling Attached equal disturbing factors, take into account different samples, workable capillary material includes but is not limited to stainless steel, PEEK, quartz glass.
Improve 3: the simple resistance by capillary generates back pressure, and the pressure limit that instrument can be provided is relatively narrow, thus may be used Following improvement is done on original structure.As shown in Fig. 2, increase second pressure sensor and backpressure regulation at capillary outlet end Device, the reading average value of first pressure sensor second pressure sensor should be subject to by so then testing pressure, and calculate viscosity When, it is drawn with the reading difference of first pressure sensor second pressure sensorCurve.
Improve 4: in order to improve testing efficiency, six-way valve sample injector can be replaced with sampling, dilution etc. functions from Dynamic sampling device.The autosampler that conventional high-performance liquid chromatogram (HPLC) can be used directly according to sample volume size or replacement are more The quantitative loop of large volume.
It improves 5: to guarantee that second pressure working sensor is stablized, second pressure sensor can be placed in insulating box.
Improvement 6: error additional caused by temperature difference when entering insulating box in order to avoid room temperature fluid, six-way valve sample introduction Preheating/refrigeration module can be increased between device and first pressure sensor.
Improve 7:, can be right before sample introduction to avoid the influence of the gas dissolved in sample and finely ground particles to viscosimetric analysis Sample is de-gassed and uses filtering with microporous membrane.
The utility model has the beneficial effects that
(1) the constant current transfusion system is connect with sample injector, and the sample injector is connect with capillary, the capillary with into First pressure sensor is provided between sample device;The first pressure sensor and capillary are arranged in temperature-controlling system;It is described Constant current transfusion system includes liquid storage bottle, degasser, constant flow high pressure pump, and the constant flow high pressure pump is connected by degasser and liquid storage bottle It connects, the constant flow high pressure pump is connect with sample injector.This practical measuring accuracy is preferable, while reducing the dosage of sample, nothing It needs to demarcate, has widened the sample measurement range of viscosity apparatus, there is preferable practicability.The utility model passes through constant current transfusion system Flow media is inputted, to realize that constant flow high pressure pushes sample to enter capillary and measures, the dosage of sample is reduced, widens The sample measurement range of viscosity apparatus has preferable practicability.
It (2) further include second pressure sensor, back pressure regulator device, the outlet end of the capillary is disposed with second Pressure sensor, back pressure regulator device, the second pressure sensor are arranged in temperature-controlling system.The utility model passes through back pressure Regulating device can produce specified flow resistance, improve the control accuracy of the utility model, have preferable practicability.Second Pressure sensor setting improves job stability in temperature-controlling system, reduces error, has preferable practicability.
It (3) further include controller, the controller is pressed with sample injector, temperature-controlling system, first pressure sensor, second respectively Force snesor, back pressure regulator device, constant flow high pressure pump connection.The utility model realizes automation control by the setting of controller System improves the accuracy of procedure operation, improves working efficiency, has preferable practicability.
(4) temperature adjusting device is additionally provided between the temperature-controlling system and sample injector, the temperature adjusting device is pre- Heating device or pre- refrigerating plant.The utility model effectively prevents when room temperature fluid enters insulating box caused by temperature difference Additional error has preferable practicability.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the utility model;
Fig. 2 is the attachment structure schematic diagram of back pressure regulator device and capillary.
Wherein: 1- degasser, 2- constant flow high pressure pump, 3- sample injector, 4- first pressure sensor, 5- capillary, 6- constant temperature Case, 7- controller, 8- liquid storage bottle, 9- waste liquid bottle, 10- second pressure sensor, 11- back pressure regulator device.
Specific embodiment
Embodiment 1:
A kind of capillary viscosity instrument based on micro-example measurement, as shown in Figure 1, including constant current transfusion system, sample injector 3, temperature-controlling system, capillary 5, first pressure sensor 4, the constant current transfusion system are connect with sample injector 3, the sample injector 3 It is connect with capillary 5, is provided with first pressure sensor 4 between the capillary 5 and sample injector 3;The first pressure sensing Device 4 and capillary 5 are arranged in temperature-controlling system;The constant current transfusion system include liquid storage bottle 8, degasser 1, constant flow high pressure pump 2, The constant flow high pressure pump 2 is connect by degasser 1 with liquid storage bottle 8, and the constant flow high pressure pump 2 is connect with sample injector 3.
Flow media is stored in liquid storage bottle 8, and degassed machine 1 enters constant flow high pressure pump 2 after removing the gas wherein dissolved, High pressure constant flow pump is exported after pressurizeing to flow media with constant flow velocity.After being completely filled with flow media in system, capillary 5 The pressure of inlet is stablized constant.After sampling system introduces the sample fluid of certain volume into flow path, flow media meeting It pushes sample to flow through capillary 5, monitors the pressure difference at 5 both ends of capillary, draw pressure drop-time graph, thus can calculate sample The viscosity of product.
The utility model in use, places flow media in liquid storage bottle 8, flow media after degasser 1, into Enter constant flow high pressure pump 2, constant flow high pressure pump 2 by controller 7 regulate and control, flow media pressurize in high-pressure pump after with constant flow velocity Q Output, subsequently enters sample injector 3.After flow media is completely filled with flow path, the sample of certain volume, sample are injected by sample injector 3 Product, by first pressure sensor 4, into capillary 5, finally flow through capillary 5 into waste liquid bottle under the promotion of flow media 9.First pressure sensor 4 and capillary 5 are placed in insulating box 5, and controlled temperature device 7 is adjusted.First pressure sensor 4 With certain sampling rate in real time to 7 returning pressure value of controller.Program prepared in advance is stored in controller 7 and is calculated public Formula controls entire testing process, records measurement data and calculate final result.
The utility model test operation method is as follows:
1, instrument prepares.High pressure constant flow pump is perfused, after flow velocity is set, the temperature and pressure of whole system is waited to stablize.
2, sample introduction and data are acquired.After the pressure for recording a bit of time, sample is injected into system from sampling device.Note Record pressure-time curve flows completely out capillary 5 until sample, and pressure replys initial value completely.
3, cleaning is closed.According to sample pollution condition, sampling device is cleaned.It is 0 that constant current flow rate pump, which is arranged, closes insulating box 5 temperature control.
This practical measuring accuracy is preferable, while reducing the dosage of sample, without calibration, has widened the sample of viscosity apparatus Product measurement range has preferable practicability.The utility model inputs flow media by constant current transfusion system, to realize perseverance Stream pushed at high pressure sample enters capillary 5 and measures, and reduces the dosage of sample, has widened the sample measurement model of viscosity apparatus It encloses, there is preferable practicability.
Embodiment 2:
The present embodiment be improve on the basis of embodiment 1, as shown in Fig. 2, further include second pressure sensor 10, Back pressure regulator device 11, the outlet end of the capillary 5 are disposed with second pressure sensor 10, back pressure regulator device 11, The second pressure sensor 10 is arranged in temperature-controlling system.Further include controller 7, the controller 7 respectively with sample injector 3, Temperature-controlling system, first pressure sensor 4, second pressure sensor 10, back pressure regulator device 11,2 connection of constant flow high pressure pump.
For the pressure limit for expanding test macro, a second pressure sensor 10 and back pressure regulator device can be further added by 11, it is connected to 5 outlet side of capillary.Back pressure regulator device 11 is controlled by controller 7, can produce specified flow resistance.Second Pressure sensor 10 is with certain sampling rate in real time to 7 returning pressure value of controller.
The simple resistance by capillary 5 generates back pressure, and the pressure limit that instrument can be provided is relatively narrow, can tie thus in original Following improvement is done on structure.As shown in Fig. 2, increase second pressure sensor 10 and back pressure regulator in 5 outlet end of capillary, such as This, which then tests pressure, should be subject to the reading average value of 4 second pressure sensor 10 of first pressure sensor, and when calculating viscosity, It is drawn with the reading difference of 4 second pressure sensor 10 of first pressure sensorCurve.
Wherein constant current transfusion system is responsible for providing the high-pressure fluid of constant flow rate, mainly includes liquid storage bottle 8, degasser 1, perseverance Flow high-pressure pump 2 and high-pressure liquid line.Sample injector 3 is responsible for for the sample of designated volume being introduced into high-pressure liquid line, optional It is realized with six-way injection valve widely used in liquid chromatogram or other structures with identity function.Temperature-controlling system is for guaranteeing Temperature when sample is by capillary 5 is constant, and the insulating box 5 or water bath that can be used temperature-controlled precision high are realized.Pressure detecting with Control system is responsible for monitoring the pressure at 5 both ends of capillary and adjusts the pressure in entire flow path, by pressure sensor and back pressure tune Regulating device 11 is constituted.Controller 7 is responsible for the coordinated scheduling of each subsystem of control, the record of data and analysis etc..
The utility model can produce specified flow resistance by back pressure regulator device 11, improve the tune of the utility model Precision is controlled, there is preferable practicability.The setting of second pressure sensor 10 improves job stability in temperature-controlling system, reduces Error has preferable practicability.The utility model realizes automation control by the setting of controller 7, improves program The accuracy of operation improves working efficiency, has preferable practicability.The utility model passes through the input flowing of constant current transfusion system Medium reduces the dosage of sample, has widened viscosity to realize that constant flow high pressure pushes sample to enter capillary 5 and measures The sample measurement range of instrument has preferable practicability.
Device for measuring viscosity described in the utility model has the advantage that
(1) even under high pressure using constant flow high-pressure plunger pump, capillary 5 and backpressure control device control compressible fluid Speed flowing, the limitation of compressible fluid can not accurately be measured by overcoming 5 viscosimeter of conventional capillaries;
(2) it directly controls flow and measures pressure difference, to obtain the shear stress and shear rate of fluid, be suitable for non-ox The viscosimetric analysis of fluid;
(3) accurate control is carried out to temperature, pressure, flow, sample volume etc. using full-automatic control system, reduces artificial behaviour Make factor, improve testing efficiency and experimental precision, reduces experimental error
(4) cooperation autosampler 3 can realize continuous and automatic testing different temperatures difference pressure with automatic backpressure control device Under power fluid viscosity with shear rate variation relation.
(5) sample consumption few (only needing 20~500uL), sample are small to the pollution of test device, easy to clean, it is ensured that survey Test result it is accurate.It is particularly suitable for the biological samples such as sample size few precious sample, such as blood, tissue fluid.
(6) test macro is demarcated without standard sample, and sample viscosity can directly be calculated.
5 viscosity determinator of the utility model capillary can measure most of fluids in assigned temperature, pressure and different shearings Viscosity when speed, determination efficiency are high, and measurement range is wide, and measurement accuracy is high, and repeatable accuracy is high, without standard sample calibration and Consumed sample is considerably less, it is only necessary to 20~500uL.This practical measuring accuracy is preferable, while reducing the use of sample Amount is not necessarily to calibration, has widened the sample measurement range of viscosity apparatus, has preferable practicability.
The other parts of the present embodiment are same as Example 1, and so it will not be repeated.
Embodiment 3:
The present embodiment is improved on the basis of embodiment 1 or 2, is also set between the temperature-controlling system and sample injector 3 It is equipped with temperature adjusting device, the temperature adjusting device is preheating apparatus or pre- refrigerating plant.The temperature-controlling system is perseverance Incubator 5 or water bath.The material of the capillary 5 can be any one in stainless steel, PEEK, quartz glass;The hair The internal diameter of tubule 5 is 0.1~2mm, 0.1~20m of length.
Many components and technical solution can continue to use existing high-efficient liquid phase chromatogram technology, such as constant current in the utility model Flow rate pump range is 50 μ L/min~5mL/min, precision 0.001ml/min, and pressure resistance is up to 150MPa.The temperature control essence of insulating box 5 Degree can reach 0.1 DEG C.Pressure difference 0~80MPa of measurement range, precision 0.01kPa.Backpressure control device adjustable extent 3~ 50MPa.0.1~2mm of internal diameter of capillary 5,0.1~20m of length.
The utility model effectively prevents error additional caused by temperature difference when room temperature fluid enters insulating box 5, tool There is preferable practicability.The utility model inputs flow media by constant current transfusion system, to realize that constant flow high pressure pushes sample Product enter capillary 5 and measure, and reduce the dosage of sample, have widened the sample measurement range of viscosity apparatus, have preferable Practicability.This practical measuring accuracy is preferable, while reducing the dosage of sample, without calibration, has widened the sample of viscosity apparatus Product measurement range has preferable practicability.
The other parts of the present embodiment are identical as above-described embodiment 1 or 2, and so it will not be repeated.
The above is only the preferred embodiment of the utility model, not does limit in any form to the utility model System, any simple modification made by the above technical examples according to the technical essence of the present invention, equivalent variations, each falls within Within the protection scope of the utility model.

Claims (7)

1. a kind of capillary viscosity instrument based on micro-example measurement, which is characterized in that including constant current transfusion system, sample injector (3), temperature-controlling system, capillary (5), first pressure sensor (4), the constant current transfusion system is connect with sample injector (3), described Sample injector (3) is connect with capillary (5), is provided with first pressure sensor (4) between the capillary (5) and sample injector (3); The first pressure sensor (4) and capillary (5) are arranged in temperature-controlling system;The constant current transfusion system includes liquid storage bottle (8), degasser (1), constant flow high pressure pump (2), the constant flow high pressure pump (2) are connect by degasser (1) with liquid storage bottle (8), institute Constant flow high pressure pump (2) is stated to connect with sample injector (3).
2. a kind of capillary viscosity instrument based on micro-example measurement according to claim 1, which is characterized in that further include Second pressure sensor (10), back pressure regulator device (11), the outlet end of the capillary (5) are disposed with second pressure biography Sensor (10), back pressure regulator device (11), the second pressure sensor (10) are arranged in temperature-controlling system.
3. a kind of capillary viscosity instrument based on micro-example measurement according to claim 2, which is characterized in that further include Controller (7), the controller (7) pass with sample injector (3), temperature-controlling system, first pressure sensor (4), second pressure respectively Sensor (10), back pressure regulator device (11), constant flow high pressure pump (2) connection.
4. a kind of capillary viscosity instrument based on micro-example measurement according to claim 2, which is characterized in that the back Pressure control device adjustable extent 3MPa ~ 50 MPa.
5. a kind of capillary viscosity instrument based on micro-example measurement according to claim 1, which is characterized in that the control Temperature adjusting device is additionally provided between warm system and sample injector (3), the temperature adjusting device is for preheating apparatus or in advance Refrigerating plant.
6. a kind of capillary viscosity instrument based on micro-example measurement according to claim 1-5, feature exist In the temperature-controlling system is insulating box (6) or water bath.
7. a kind of capillary viscosity instrument based on micro-example measurement according to claim 1, which is characterized in that the hair The material of tubule (5) can be any one in stainless steel, PEEK, quartz glass;The internal diameter of the capillary (5) be 0.1 ~ 2mm, 0.1 ~ 20m of length.
CN201821749199.8U 2018-10-26 2018-10-26 A kind of capillary viscosity instrument based on micro-example measurement Active CN209148482U (en)

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Application Number Priority Date Filing Date Title
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CN209148482U true CN209148482U (en) 2019-07-23

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