CN206057137U - Using sessile drop method all automatic measurement liquid surface or the device of interfacial tension - Google Patents
Using sessile drop method all automatic measurement liquid surface or the device of interfacial tension Download PDFInfo
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Abstract
The utility model discloses a kind of device of employing sessile drop method all automatic measurement liquid surface/interfacial tension.This utility model includes the capillary tube to form hanging drop, and the both sides of capillary tube are provided with background light source and image unit；Described the first pipelines of capillary tube Jing are connected with the first liquid feeding unit, and the first liquid feeding unit and image unit are connected with computer；Described fluid valve of the first liquid feeding unit configuration with ingress port and outlet port, the outlet port of fluid valve are connected with the first pipeline, and the ingress port of fluid valve is connected with the second pipeline, and the second pipeline is connected with second container.This utility model not only realizes all automatic measurement of liquid/fluid system surface/interface tension value, and improve certainty of measurement and stability, the impact of anthropic factor is reduced, is that the application of the surface/interface tension measurement techniques for expanding liquid/fluid system is laid a good foundation.
Description
Technical field
This utility model is related to a kind of employing sessile drop method all automatic measurement liquid/stream-system surface tension or interfacial tension
Device, belongs to the fields of measurement of liquid/stream-system.
Background technology
The surface tension or interfacial tension of liquid/stream-system is caused by mutual (attraction) active force between molecule.Table
Face/interfacial tension not still important material basic physical parameters, and in commercial production, daily life and natural process
In all play an important role.If no matter the development and production of surfactant be in commercial Application or in daily life
In, it is quite important, and its Main Function is that the surface tension or interfacial tension for effectively and in time reducing system, this is right
The performance of the ink that such as ink-jet printer is used have very crucial impact, determine generation ink droplet sprawl attribute,
So as to the quality for printing.The foam frequently encountered in industrial processes and in daily life and foaming phenomena, similarly
With the use of surfactant or intervention and thus caused surface/interface tension value is closely related.Surface tension also with the earth
On many life and natural phenomena be closely related：The Surfactant of human lung's alveolar secretion can be effectively reduced alveolar
Surface tension (to close to 0), ensure that human body respiration it is normal, effectively carry out；And the high surface tension that water has
Value maintains plant and up conveys water and nutrient from rhizome.
The measurement of liquid surface/interfacial tension can be used conventional methods, such as based on weigh dynamometry flat band method and hang
(extension) around-France (force tensiometer) and the bubble pressure method (pressure based on measure differences in pressure
Tensiometer), and the modern times method, sessile drop method (the optical pendant drop such as based on optical image security
tensiometer).The latter is based on its table the characteristics of the aspects such as measurement accuracy, ease-to-operate and having wide range of applications property
Reveal in following many many advantages：
The accuracy and reliability of measurement
Measured value range
Under extreme conditions, such as high temperature, under high pressure, measurement
Required amount of liquid (more few better)
Both to static measurement, and fitness to kinetic measurement
Both to liquid/gas-stalagmometry, and fitness to the measurement of liquid liquid-interfacial tension
The fitness of surface/interface tension force of the measurement containing surfactant solution
Fitness of the measurement containing various different chemical substance (including various different types of surfactants) systems
The fitness of measurement viscosity higher solution or liquid
Total time needed for measurement
The integrated cost of measurement
Due to due to historical development, although current sessile drop method is also popularized, it possesses enough potentiality completely,
In most applications, replace or supplement (or most) traditional measuring method.But the hanging drop with current commodity
Method is compared, and traditional still possesses advantage in one aspect based on the flat band method and suspension ring method e measurement technology that weigh dynamometry, and that is just
It is its all automatic measurement ability.After testing sample is ready, these traditional methods fully automatically can complete single measurement,
Long-time kinetic measurement (when using flat band method) or the measurement of entire series, the latter can be used to fully automatically complete surface
The measurement of the critical micelle concentration (CMC) of activator solution.And current sessile drop method does not also possess so high automaticity.
In the market device as shown in Figure 1 is relied on based on the optics sessile drop method of image procossing, obtain hanging drop
Positive side (two dimension) profile (orthogonal silhouette) image.When hanging drop is in hydrostatic equilibrium state,
Its shape can be described by Laplace-Young equations.But the latter is only under some special boundary conditions, such as drop is presented center
During axle rotational symmetry (rotational axis symmetry), can just pass through numerical solution.One is only subject to outside gravity
Power the is acted on, shape of hanging drop under hydrostatic equilibrium state is by its volume (v), the density contrast (Δ between two-phase
ρ) with its surface/interface tension force (γ), and the contact diameter (d) between hanging drop and solid support surface is determined.Surface/
Interfacial tension compares generally by capillary tube parameter (a) to represent with the strength of gravity, when it only depends on the attribute of system and measurement
Temperature and pressure.
In above formula, g is the acceleration of gravity on measurement ground.For a given system and measuring condition (temperature/pressure), its
Though capillary tube parameter (a) is certain value, different droplet sizes (v) and contact diameter (d) will affect and cause final liquid
Drop shape (see Fig. 2).As long as in principle, it is possible to from the hanging drop of a random size and dimension-its deviation is spherical and center is presented
Axle rotational symmetry-positive side profile image determine capillary tube parameter (a) value of system.From the latter, in the close of known architectures
In the case of degree difference and acceleration of gravity, surface/interface tension force (γ) value can be further calculated again.
The positive side profile image of hanging drop that experiment is obtained, as any the same by testing the physical quantity that obtains of measurement, always
It is by measuring system and the measurement error of conditional decision with certain.And this measurement error will be finally reflected and be calculated
Surface/interface tension force (γ) value measurement error on.But during this error propagation, the enlargement range of error is and liquid
The shape of drop is significantly correlated：Under normal circumstances, drop shape more deviates spherical, and the enlargement range of error is also less.So
When being measured using sessile drop method, for (absolute) direct measurement error of the contour images of given size, calculated surface/
The precision (or error) of interfacial tension measured value is relevant with the shape of drop；And liquid/the stream to certain capillary tube parameter (a) value-
Use when system and measurement, certain size (capillary tube for forming hanging drop of external diameter or internal diameter d), the shape of drop only with
The volume (or size) of drop is relevant.Therefore in order to improve the precision of surface/interface tension value measurement as far as possible in actual measurement,
It is necessary to ensure that the hanging drop to form " appropriate " size or/and shape so as to deviate spherical as far as possible.Here " appropriate " refers to as far as possible
Ground is big, but can not be too big so that hanging drop is unstable, be susceptible to come off or occur acutely to rock.But this measure equally also can
Bring the difficulty in practical operation：It is susceptible to come off when hanging drop is too big first；Even if secondly at the beginning when quite stable
Hanging drop, when the surface/interface tension force of system becomes hour over time, the surface/interface tension value of decline will certain moment without
Method supports the effect of gravity again and causes hanging drop to fall off.Furthermore, if the surface/interface tension value of system, either for
Which kind of reason, is elevated over time, then one hanging drop of size " appropriate " during beginning, after a certain time, it is also possible to no
Size " appropriate " again.
After necessary preparation is completed, the measuring process of current hanging drop measurement method is typically：In operator
Close observation under, the appropriate hanging drop of a size is produced by (manually or automatically) liquid feeding.The hanging drop of generation can not be too big, no
Then it can come off；But can not be too little, because this can cause the precision for measuring not high.And start when " appropriate " volume or
By the experience of operator, or determined by attempting.In the case of the latter, operator is by being constantly increasing drop
Volume till it comes off, thereby determine that the maximum of drop comes off front volume.Then a less volume is selected, such as most
The about 70-90% of the front volume that comes off greatly, forms the drop for measuring.In body of the measurement containing surfactant component
When being, as the surface/interface tension value of this kind of system generally declines over time, and often decline in the incipient stage
Speed and amplitude all highly significants, at this moment just must additionally carefully continuous observation hanging drop change over time, in case system
The surface/interface tension force for constantly declining cannot support the action of gravity of hanging drop again and cause droplet detachment.For such system,
The hanging drop size formed when starting can not be too big, or the body of hanging drop must be reduced during carefully monitoring every now and then
Product, to ensure which unlikely falls off；After drop comes off in measurement process, a less drop of volume is re-formed
Proceed measurement to start anew, it is reciprocal with this, until completing required measuring task.It is all these all to cause to need behaviour
Make getting involved deeply for personnel and the required time is measured with attentively putting into, extending, also so that measuring method cannot be applied to nobody
With the field with treatment.Therefore, researching and developing a high precision, good stability, anthropic factor affects few based on the complete of sessile drop method
The device of automatic measurement liquid surface/interfacial tension, becomes industry problem urgently to be resolved hurrily.
Utility model content
Technical problem to be solved in the utility model is to provide using sessile drop method all automatic measurement liquid surface/interface
The device of tension force.This utility model not only realizes all automatic measurement of liquid/stream-system surface/interfacial tension value, and improves
Certainty of measurement and stability, reduce the impact of anthropic factor, are the surface/interface tonometry skill for expanding liquid/stream-system
The application of art is laid a good foundation.
To solve above-mentioned technical problem, the technical solution of the utility model is as follows：Using sessile drop method all automatic measurement liquid
The device of surface/interface tension force, including the capillary tube for forming hanging drop, the both sides of capillary tube are provided with background light source and image unit；
Described the first pipelines of capillary tube Jing are connected with the first liquid feeding unit, and the first liquid feeding unit and image unit are connected with computer；
Described fluid valve of the first liquid feeding unit configuration with ingress port and outlet port, the outlet port and first pipe of fluid valve
Road is connected, and the ingress port of fluid valve is connected with the second pipeline, and the second pipeline is connected with second container.
The device of aforesaid employing sessile drop method all automatic measurement liquid surface/interfacial tension, sets in described second container
There is the 4th pipeline, the 4th pipeline is connected with the second liquid feeding unit, and the second liquid feeding unit is connected with the 3rd pipeline, the connection of the 3rd pipeline
There is the 3rd container.
The device of aforesaid employing sessile drop method all automatic measurement liquid surface/interfacial tension, the outlet of described capillary tube
The first container of printing opacity is provided with the outside of end, below the first container, regulating platform is provided with.
The device of aforesaid employing sessile drop method all automatic measurement liquid surface/interfacial tension, sets in the first described container
There is the 5th pipeline, the 5th pipeline is connected with the 3rd liquid feeding unit, and the 3rd liquid feeding unit is connected with the 6th pipeline, the connection of the 6th pipeline
There is the 4th container.
The device of aforesaid employing sessile drop method all automatic measurement liquid surface/interfacial tension, described second container and/or
Agitating device is provided with below first container.
The beneficial effects of the utility model：Compared with prior art, this utility model has the characteristics that：(1) this practicality
It is new in the case where being not required to very important person's monitoring or intervening, to be automatically completed under conditions of corresponding preparation is ready
The measurement of the surface/interface tension force or capillary tube parameter of a series of single or batch samples.(2) this utility model can be given
Under the conditions of automatically determine limiting volume VrSo as to form the hanging drop of proper volume, this process is without the need in advance by being input into one
Product value is specifying；Nor depend on gradually increasing the advance trial knot till hanging drop falls off by forming a volume
Fruit which thereby enhances automaticity, the precision and stability of measurement, reduces the impact of anthropic factor determining.(3) this reality
Real-time detection and adjustment are carried out to drop shape with new, to ensure in whole measurement process, even if surface/interface tension value
There is violent change, can ensure that hanging drop, in an appropriate size, both ensure that the precision of measurement, and can prevent drop again all the time
Fall off in measurement process.(4) this utility model not only compensate for surface/interface tonometry so far based on sessile drop method
The shortcoming of technology, and further improve and extend automaticity, reduce impact of the anthropic factor to certainty of measurement,
Popularization for sessile drop method and solid foundation has been established in most application alternative/complement traditional measurement methods, and
Further extend the range of application of sessile drop method, including online fully-automated synthesis/monitoring, surfactant system it is complete from
Dynamic screening/optimization etc., to fields such as scientific research, improved product/exploitation and the raisings of industrial processes automaticity
Have great importance.
Description of the drawings
Fig. 1 is the structural representation of existing sessile drop method measurement apparatus；
Fig. 2 is the hanging drop dimensionless theoretical profile schematic diagram of the different shape factor；
Fig. 3 is two various sizes of hanging drop images and digital simulation curve：A () small size hanging drop, shape are close to sphere；
B () large scale hanging drop, image do not include drop bottom apex (apex)；
Fig. 4 is the coordinate schematic diagram of hanging drop theoretical contour；
Fig. 5 is the structural representation of measurement apparatus in embodiment 1 and 2；
Fig. 6 is the structural representation of measurement apparatus in embodiment 1 and 4；
Fig. 7 is to implement preferred measurement apparatus structural representation in row 1；
Fig. 8 is the measurement result of embodiment 2；
Fig. 9 is the measurement result of embodiment 3；
Figure 10 is the measurement result of embodiment 4；
Figure 11 is the structural representation of preferred measurement apparatus in embodiment 1.
This utility model is further described with reference to specific embodiment.
Specific embodiment
With reference to embodiment, the utility model is described in further detail, but not as to limit of the present utility model
System.
Embodiment 1：It is a kind of based on it is full-automatic formed/control appropriate size hanging drop, so as to realize all automatic measurement liquid/stream-
The device of system surface/interfacial tension value, as shown in Figure 5, including the capillary tube 1 for forming hanging drop 2, the outlet of the capillary tube
End vertically downward, is exposed in gas phase, and the both sides of capillary tube 1 are provided with background light source 4 and image unit 6, and image unit 6 is just included
Camera lens 5 to hanging drop, the image unit are horizontal that (image unit can also be in upright position, as long as before which
Place one can make light path occur 90 ° transformation prisms), normal alignment capillary tube port and as reference position setting liquid
Drop detection image region；Described 1 the first pipelines of Jing 13 of capillary tube are connected with the first liquid feeding unit 3, the first liquid feeding unit 3 and take the photograph
As unit 6 is connected with computer 7；Described fluid of the configuration of the first liquid feeding unit 3 with ingress port 12 and outlet port 11
Valve 26, the outlet port 11 of fluid valve 26 are connected with the first pipeline 13, and the ingress port 12 of fluid valve 26 is connected with the second pipeline
15, the second pipeline 15 is connected with second container 10, is loaded with outstanding in prepare liquid/stream-system two-phase in the second container 10
Drop phase (drop phase), when the fluid in the first liquid feeding unit 3 exhausts or when needing replacing whne fluid measured phase, passes through
Second pipeline by second container treat fluid measured phase (or update/change treat fluid measured phase), be delivered to the first liquid feeding unit
It is interior for measuring, so as to realize batch or successional all automatic measurement.The computer obtains capillary tube by image unit
The image information of the drop that port is formed, and by being analyzed to which and being calculated relevant current drop, including volume
With capillary tube parameter (according to a preliminary estimate be worth) etc. in interior, parameter value；Obtain right according to these parameter values and by further calculating
The limiting volume Vr for answering, according to the liquid volume added of output control the first liquid feeding unit, adjusts hanging drop to proper volume, then by this
The analysis of the hanging drop that sample is formed, calculating, fully automatically determine the surface tension of liquid/gas-system.
It is when the first liquid feeding unit 3 is equipped with the higher phase of prepare liquid/stream-two-phase system Midst density and logical with capillary tube 1
Cross the first infusion pipeline 13 to be connected, the port of export of the capillary tube 1 is vertically downward, close in prepare liquid/stream-two-phase system
In the relatively low gas phase of degree or another liquid phase, the latter is placed in one by made by optical glass, the first container 8 of optical path direction printing opacity
In.
When the first liquid feeding unit fills 3 phase for having prepare liquid/stream-two-phase system Midst density relatively low (gas phase or liquid phase),
And be connected by the first infusion pipeline 13 with capillary tube 1, the port of export of the capillary tube 1 vertically upward, located at prepare liquid/
In the higher another liquid phase of stream-two-phase system Midst density, the latter is placed in one by made by optical glass, the of optical path direction printing opacity
In one container 8.At this moment the drop for being formed is the rising hanging drop (rising dropor bubble) of a reversing, but its analysis, meter
Calculate identical with normal (sagging) hanging drop.For convenience's sake, hanging drop hereinafter referred to as, unless specifically stated otherwise beyond,
Both normal (sagging) hanging drop had been included, also including rising hanging drop (or bubble).
The first described liquid feeding unit 3 is two-way (bidirectional) liquid feeding unit：Both can be (passing through
Infusion/dispense) increase, it is also possible to which (by withdrawal/aspirate) reduces the volume of drop.In this feelings
Under condition, the hanging drop that computer 7 can not only be formed in a suitably dimensioned, and can take appropriate measures if necessary, to prevent from hanging
Drip excessive and fall off before being measured, so that the time dependent body of the similarly suitable surface/interface tension force of method
The measurement of system, can track dynamic change of the surface/interfacial tension with the time for a long time, until it reaches balance.
Described computer 3 by image unit 6 in real time, constantly formed, or presence, the image of drop
Information, and by its analytical calculation is constantly obtained the volume and system of current drop capillary tube parameter (or with these ginseng
The proportional value of number).Then the limiting volume of current drop is extrapolated according to computational methods corresponding above, is thus constantly supervised
Depending on and control drop size to remain at which corresponding with current capillary tube parameter value (or surface/interface tension value)
Appropriate size：It is allowed on the one hand to keep the precision to guarantee to measure as large as possible；On the other hand it is again sufficiently stable, to prevent which
Fall off as volume is excessive；Another further aspect, also should reduce the frequency or number of times for changing droplet size, as far as possible with to table
The impact of face/interface equalization process is maintained at minimum level.
The ingress port 12 of liquid (distribution) valve of the first above-mentioned liquid feeding unit 3 by the second pipeline 15 directly with needs
The liquid phase of detection/monitoring is connected.The latter is regularly loaded into the first liquid feeding by ingress port 12 under the control of computer 7
In unit, for measuring use, so as to realize the fully-automated synthesis/monitoring to (with the second pipeline) liquid phase that is connected.
As shown in Figure 6, further preferred version is：Also include possessing ingress port (inlet port) and the port of export
(automatic, controllable) second liquid feeding unit 18 of mouth (outlet port) fluid (distribution) valve (valve).Second liquid feeding unit
The ingress port of 18 fluid (distribution) valve is connected with the liquid phase in the 3rd container 19 by the 3rd pipeline 21, its outlet port
Connect with above-mentioned second container 10 via the 4th pipeline 20.When measurement starts, volume and a certain in second container 10, is loaded with
Specified ingredients content (concentration C0) known liquid phase, (same specified ingredients) content (concentration C is loaded with the 3rd container 19s)
Known, but content (concentration Cs) with second container in the liquid phase liquid phase that there were significant differences.The second container is configured with
(magnetic) agitating device (16,17), for promoting and keeping the mix homogeneously of solution.In measurement process, the computer 7 passes through
The first liquid feeding unit 3 is controlled, the liquid phase in second container 10 can be quantitatively removed (reduce) when necessary；By control the
Two liquid feeding units 18, the fluid that when necessary fluid in the 3rd container 19 mutually quantitatively can be injected in second container 10
Phase.So can automatically realize the specified ingredients concentration contained by the 10 interior liquid phase for containing of second container from C0To being close to CsChange
Change, changed with fully automatically carrying out surface/interface tension force (or capillary tube parameter) to change with the specified ingredients content (concentration)
Dependence linearity curve measurement.Facing containing surface active agent composition system can further be realized from described dependence linearity curve
The all automatic measurement of boundary's micellar concentration.
As shown in Figure 7, another preferred version is：Including the 3rd liquid feeding unit 24, the fluid of the 3rd liquid feeding unit 24
The outlet port of (distribution) valve (valve) is connected with the first above-mentioned container 8 via the 5th pipeline 22, and ingress port is via
Six pipelines 26 are connected with the 4th container 25.Liquid phase (or the liquid of prepare liquid/stream-system is loaded with 4th container 25
One of body phase) solvent or (high concentration) mother solution, can the computer unit control under pass through the 3rd liquid feeding unit
24 the 6th pipelines 26 of fluid (distribution) valve Jing are quantitatively injected in the first container 8 from the 4th container 25, to change first
The composition of liquid phase in container.First container 8 is configured with (magnetic) agitating device 23 of computer control, for promoting and keeping molten
The mix homogeneously of liquid.
As shown in Figure 11, further preferred version is：Further include equipped with possessing ingress port (inlet
Port) and outlet port (outlet port) fluid (distribution) valve (valve) the 4th liquid feeding unit 24, its fluid valve enters
Mouthful port is connected with the liquid phase in the 4th container 25 by the 6th pipeline 26, its outlet port via the 7th pipeline 27 with it is above-mentioned
The first container 8 or second container 10 be connected.4th container, 25 interior to be measured system auxiliary agent of the splendid attire containing debita spissitudo/
The mother solution of additive, can be under computer unit control by fluid (distribution) the valve quilt of the 4th liquid feeding unit 24
Quantitatively it is injected in the prepare liquid body phase of the first container 8 or second container 10, to change the composition of prepare liquid body phase.Described
One or second container be configured with agitating device, for promoting and keeping the mix homogeneously of solution.The stirring dress of the first container configuration
The startup and stopping put be able to must be controlled by computer.By the composition for automatically changing liquid phase in first or second container, can
Fully automatically to complete the dependence measurement that surface/interface tension force changes with composition (or a certain concentration of component), so as to enter one
Step fully automatically realizes the such as compositional optimization containing surfactant system or screening.
Embodiment 2：Tap water capillary all automatic measurement in atmosphere：
It is a kind of to form/control appropriate size hanging drop, so as to (realize) all automatic measurement liquid/stream-diagram of system based on full-automatic
The device of face/interfacial tension value, as shown in Figure 5, including the capillary tube 1 for forming hanging drop 2, the port of export of described capillary tube 1
Outside be provided with the first container 8 of printing opacity, be provided with regulating platform 25 below the first container 8；The both sides of capillary tube 1 are provided with bias light
Source 4 and image unit 6, described background light source, regulating platform and image unit are each attached on platform 9；Described 1 Jing of capillary tube
First pipeline 13 is connected with the first liquid feeding unit 3, and the first liquid feeding unit 3 and image unit 6 are connected with computer 7；Described
One liquid feeding unit 3 is configured with the fluid with ingress port (inlet port) 11 and outlet port (outlet port) 12 and (divides
With) valve (valve), the outlet port 11 of fluid valve is connected with the first pipeline 13, and the ingress port 12 of fluid valve is connected with second
Pipeline 15, the second pipeline 15 are connected with second container 10.The port of the wherein capillary tube 1 is immersed in gas phase, described hair
Tubule 1 is between the light-emitting area and the camera lens 5 of image unit 6 of background light source 4.Wherein, the first liquid feeding unit 3 is driven by motor
And equipped with precision glass syringe 26 (0.05-10.0ml), its operating can be controlled by computer unit 7 by control system
The on-position of (syringe piston displacement), rotation direction and running speed and fluid (distribution) valve.
Additionally, the first liquid feeding unit 3 that this utility model embodiment is provided also includes adding via the second pipeline 15 and first
The second container 10 that the ingress port of fluid (distribution) valve of liquid unit 3 connects.(shape to be measured is loaded with the second container 10
Into hanging drop) liquid, wherein the gas phase is positioned at by made by optical glass, in the first container 8 of optical path direction printing opacity.Specifically
Ground, places the first container 8 for receiving the drop that comes off in the lower section of 1 port of capillary tube, stable to drop 2 in order to reduce air flow
Property impact, while reduce drop droplet formation, measurement waiting process in volatilization, preferably 1 port of capillary tube is extend into
In first container 8, and plus appropriate lid sealing as far as possible.Further, first container 8 is carried by regulating platform 25, described
Regulating platform 25 is placed on platform 9, wherein the first and second containers and the first liquid feeding unit periphery can be all provided with temperature control folder if necessary
Cover unit to maintain certain measurement temperature.
The method that this utility model embodiment also provides the surface/interface tension force that liquid is measured based on above-mentioned measurement apparatus,
Comprise the steps：
A, computer unit 7 start control program, to computer input or specified measurement of correlation parameter：The caliber of capillary tube
(external diameter is adopted in this utility model embodiment) or the density or density difference of image magnification, drop phase and surrounding phase,
The acceleration of gravity on measurement ground, forms the speed of drop, drop size index or scope, and the stopping criterion of measurement (includes every time
Rate of change and/or most long measurement persistent period), number of repetition is measured, extra exclusion before being met again measurement next time, is needed
Need before drop number, and measurement using liquid sample to wash number of liquid feeding unit and pipeline etc.；
B, the upper and lower, left and right position under real time imaging state, adjusting capillary tube 1 so as to which there is part (about 0.2- port
It is 1mm) visible in the top of image, and the left and right centre position of image is approximately in, as shown in Figure 3.Adjust image focusing and
Related image parameter so that capillary tube port image clearly, brightness and contrast grade are suitable, measures image times magnification if necessary
Number；
C, the testing liquid of q.s is added (or connecting line 15 is inserted into be loaded with q.s and treat toward second container 10
In the liquid phase of the second container for surveying liquid), start measurement；
After d, measurement start, computer unit 7 will be detected to current image first, to determine 1 port of capillary tube
Whether occur in the picture, whether its imaging is clear, whether position is appropriate, if it find that any problem will remind user to be changed
Enter；
E, according to setting, computer unit 7 uses 3 pairs of the first liquid feeding units of the first liquid feeding unit and connecting line if necessary
And capillary tube is cleaned, the liquid for cleaning is received by the first container 8, makes certain liquid steaming is formed in the first container
Vapour phase；
F, computer unit 7 are loaded into testing liquid the syringe of the first liquid feeding unit, according to the formation drop of setting
Speed adds testing liquid toward capillary tube 1, starts simultaneously at the forming process and state for persistently monitoring drop.When computer unit is examined
When measuring the port of capillary tube 1 and initially forming drop 2, constantly the Liquid particle image to obtaining is analyzed calculatings, and tracking is currently
Drop parameter, including current volume, capillary tube parameter value (or its correlative) and its variation tendency, and thereby (according to above
The method of description) calculate the limiting volume of drop.According to calculated drop limiting volume, capillary tube parameter (or its phase
Measure pass) variation tendency, and the measurement parameter (drop size index) for arranging, computer unit make corresponding judgement, automatically
Ground control liquid volume added increases to an appropriate size by drop, starts measurement, and gathers measurement data；
G, in whole measurement process, computer unit persistently monitor the state of drop, analytical calculation obtain drop figure
Picture, according to newest capillary tube parameter (or its correlative) value and its variation tendency that obtain, and the drop size index for arranging,
Be made whether to be necessary the decision of the size and amplitude of accommodation size that adjust drop；Period should consider that the size of drop is fitted
When to take the drop size index of setting, the precision of measurement into account, the stability of drop and prevent which from coming off, reducing again as far as possible
Interference to drop.After the single measurement stopping criterion for arranging meets, computer unit stops the measurement to current drop；
H, next, the repeated measure number of times according to measure setup is repeated by computer unit to same sample
Measurement, till specified measuring task is completed.Before each repeated measure is performed, computer unit will be by Rapid Freon-feeding
Promote current droplet detachment, and more drops can be forced quickly to leave capillary tube port according to arranging.Then (in acquiescence
Under setting) it forms drop using final droplet size during last measurement is adopted as initial droplet volume this time,
Start to remeasure.
Fig. 8 gives the measurement result that continuous 5 drops are carried out to above-mentioned tap water/gas phase-system (at room temperature).Liquid
The meansigma methodss and standard deviation of drop volume are 28.49 ± 0.06 μ l, and the surface tension value for measuring is 72.41 ± 0.02mN/m
(0.03%).As the surface tension of tap water for adopting is little with time change, so work as computer unit, the is being carried out
Droplet formation initial stage during one-shot measurement, it is determined that appropriate drop size, and phase is defined by controlling the first liquid feeding unit
After answering the drop of size, the size of drop remains unchanged in whole measurement process.In ensuing repeated measure, computer
Unit forms drop as initial droplet volume using final droplet size during last measurement, starts to remeasure, institute
Also there is repeatability well with the droplet size of each measurement.
Embodiment 3：Aqueous surfactant solution capillary all automatic measurement in atmosphere
It is a kind of to form/control appropriate size hanging drop, so as to (realize) all automatic measurement liquid/stream-diagram of system based on full-automatic
The device of face/interfacial tension value, construction is with implementation with the description in above-described embodiment two.Described device is used to measurement
Containing the aerial surface tension value of aqueous surfactant solution.The Size Indices range set of drop is 85-90%, is repeated
Pendulous frequency is 3, and every time the stopping criterion of measurement is most long time of measuring 2000 seconds.According in embodiment one description input or
After specifying related measurement parameter, aqueous surfactant solution to be measured is added in second container, starts measurement.Fig. 9 is given
The result that measurement is obtained.
Different from the surface tension of the tap water in embodiment two, measure here containing aqueous surfactant solution in sky
Surface tension value in gas shows the time dependence of highly significant, its value from newly formed drop when about 70mN/m in starting
About 51mN/m is just quickly fallen in 50s, and continues to drop to about 47.5mN/m in back to back about 100s.This numerical value exists
About 45.5mN/m is further lowered into after ensuing about 350s, its last equilibrium valve～44.7mN/m is close to.From Fig. 9 simultaneously
Corresponding first droplet size for being given can be seen that droplet size about 27 μ l from the outset over time with table
The decline of face tension value is progressively correspondingly adjusted to about 16.7 last μ l, is remained in the volume range specified, both
The precision of measurement is ensure that, also ensures that drop is in what is do not fallen off during so violent surface tension variations all the time
Steady statue so that prolonged dynamic surface tension measurement or the measurement of equilibrium surface tension value fully automatically can be realized.
In ensuing repeated measure, because being same liquid sample system, when computer unit directly employs last measurement
Final droplet size form drop as initial droplet volume, start to remeasure.Do not have in whole measurement process yet
Again the volume of drop is adjusted, unless the volume of drop exceedes the upper limit of the scope of setting or/and faces the danger for coming off.
The all automatic measurement of embodiment 4, aqueous surfactant solution critical micelle concentration (CMC)
It is a kind of to form/control appropriate size hanging drop, so as to (realize) all automatic measurement liquid/stream-diagram of system based on full-automatic
The device of face/interfacial tension value, as shown in Figure 6, possesses ingress port (inlet port) and outlet port including configuration
The two-way first liquid feeding unit 3 of (outlet port) fluid (distribution) valve (valve) and the second liquid feeding unit 18, via first
The capillary tube 1 that pipeline 13 is connected with the outlet port of fluid (distribution) valve of the first liquid feeding unit 3, background light source 4 and shooting list
Unit 6, and to control the computer unit 7 of image unit and first, second liquid feeding cell operation, wherein the capillary tube 1
Port be immersed in by made by optical glass, in the gas phase in the first container 8 of optical path direction printing opacity, described capillary tube 1
Light-emitting area in background light source 4 and between the camera lens 5 of image unit 6.Wherein, first, second liquid feeding unit be equipped with
The syringe pump (syringe pump) of precision glass syringe 26,27 (0.05-10.0ml), can be by control system by computer
Unit 7 controls the on-position of its operating (syringe piston displacement), rotation direction and running speed and fluid (distribution) valve.
In addition the inlet ports of 3 fluid of the first liquid feeding unit (distribution) valve are connected with the liquid phase in second container 10 via the second pipeline 15
Connect, the second container 10 is loaded with the water phase of known volume when measurement starts, and is configured with (magnetic) agitating device 16,17,
For promoting and keeping the mix homogeneously of liquid phase.The inlet ports of fluid (distribution) valve of the second liquid feeding unit are by the 3rd pipe
Road 21 is connected with the liquid in the 3rd container 19, and its outlet port is connected with above-mentioned second container 10 via the 4th pipeline 20
Connect.The surface to be measured containing concentration known (its value is significantly higher than the critical micelle concentration of expectation) is loaded with 3rd container
Activator solution (mother solution).The first liquid feeding unit 3 can be passed through in the case where the computer unit 7 is controlled in measurement process
Fluid valve quantitatively remove liquid phase in second container 10 into the first container 8 and by the stream of the second liquid feeding unit 18
Body valve injects the liquid phase mother solution to be measured of metering toward second container 10, to change the composition (surfactant of liquid phase in second container
Concentration).Further, first container 8 is carried by regulating platform 25, and the regulating platform 25 is placed on instrument platform, wherein the
One and second container and the first liquid feeding unit periphery can be all provided with temperature control chuck unit 14 if necessary to maintain certain measurement temperature
Degree.Furthermore, in order to reduce impact of the air flow to 2 stability of drop, while reducing droplet liquid in droplet formation, measurement etc.
Volatilize during treating, the first container 8 can add appropriate lid to seal as far as possible.
This utility model embodiment is also provided and measures the surface/interface tension force of liquid with liquid phase group based on above-mentioned measurement apparatus
Into the method for change, comprise the steps：
A, start computer unit 7 control/application program, under real time imaging state, adjust capillary tube 1 it is upper and lower,
Left and right position so as to which port has part (about 0.2-1mm) visible in the top of image, and is approximately in the middle of the left and right of image
Position, as shown in Figure 3.Adjust the focusing of image and related image parameter so that capillary tube port image clearly, brightness and anti-
Margin is suitable, remeasures image magnification if necessary；
B, add toward second container 10 metering, the prepare liquid body phase of known (starting) concentration (as neat solvent or certain together
The solution of beginning concentration；The present embodiment adopts neat solvent water), past 3rd container 19 adds the known of the prepare liquid body phase of q.s
(the present embodiment is female using the higher aqueous solution containing surfactant to be measured of concentration for the mother solution or neat solvent of (higher) concentration
Liquid)；
C, to computer input or specified measurement of correlation parameter：Caliber or image including systematic parameter such as capillary tube amplifies
The density or density difference of multiple, drop phase and surrounding phase, measures the acceleration of gravity on ground, forms the speed of drop, drop chi
Very little index or scope, the stopping criterion (including rate of change and/or most long measurement persistent period) of measurement every time, and it is critical with measuring
The concentration range and concentration change pattern (or concentration point set) of the related measurement parameter of micellar concentration (CMC) such as measurement, works as concentration
The wash number to the first liquid feeding unit 3, connecting line 13,15 and capillary tube 1 with new concentration samples is needed during change, each
The measurement number of repetition of concentration point, meeting again needs the drop number of extra exclusion between measurement；Measurement is attached to second before starting
Liquid phase in container 10 (the present embodiment adopts neat solvent water) volume and concentration (the present embodiment because adopting neat solvent water,
So initial concentration is for 0), (the present embodiment is adopted and contains surfactant the concentration of the liquid phase being contained in the 3rd container 19
, concentration be higher by expectation several times of CMC value mother solution)；
D, startup measurement.Computer unit 7 will be detected to current image first, to determine that 1 port of capillary tube is
In the picture, whether its imaging is clear for no appearance, and whether position is appropriate, if it find that any problem will remind user to be changed
Enter；
E, according to setting, computer unit 7 determines the concentration value of next measurement point, and by control first, second plus
The quantitative plus/minus liquid function of liquid unit, realizes this concentration value in the liquid phase of second container 10.Then it is dense with this according to arranging
The liquid phase of degree cleans the first liquid feeding unit, connecting line 13,15 and capillary tube 1, and the liquid phase for cleaning is connect by the first container 8
Receive, make in the first container, to form certain liquid vapour phase.
F, computer unit 7 are loaded into the first liquid feeding unit (for the present embodiment is filled the testing liquid in second container
It is downloaded in the glass syringe of the first liquid feeding unit), testing liquid is added toward capillary tube 1 according to the formation liquid drop speed of setting,
Start simultaneously at the forming process and state for persistently monitoring drop.When the port that computer unit detects capillary tube 1 initially forms
During drop 2, constantly the Liquid particle image to obtaining is analyzed calculating, persistently tracks current drop parameter, including working as precursor
Product, capillary tube parameter value (or its correlative) and its variation tendency, and thereby (according to method described above) calculates drop
Limiting volume.According to calculated drop limiting volume, the variation tendency of capillary tube parameter (or its correlative), Yi Jishe
The measurement parameter (drop size index range) put, computer unit make corresponding judgement, automatically control liquid volume added by drop
An appropriate size is increased to, is started measurement, and is gathered measurement data；
G, in whole measurement process, computer unit persistently monitors the state of drop, is obtained most according to analytical calculation
New capillaries parameter (or its correlative) value and its variation tendency, and the drop size index range for arranging, be made whether
The decision of the necessary size and amplitude of accommodation size for adjusting drop；Period should consider that the size of drop is appropriate, to guarantee to survey
The precision of amount, the stability of drop and prevent which from coming off, reduce the interference to drop again as far as possible.When the single measurement for arranging stops
After only criterion meets, computer unit stops the measurement to current drop；
H, next, computer unit is by the repeated measure number of times according to measure setup, the sample to same concentration point
Carry out repeated measure.Before each repeated measure is performed, computer unit will promote current droplet detachment by Rapid Freon-feeding, and
And more drops can be forced quickly to leave capillary tube port according to arranging, to reduce surfactant in capillary tube port
Impact of the adsorption effect to follow-up repeated measure.Then it will adopt final droplet size during last measurement as this time
Initial droplet volume forming drop, start to remeasure, till specified repeated measure task is completed.
I, repeat the above steps e-h, till the concentration range or concentration point set specified is fully completed.
Figure 10 gives the result that measurement is obtained.From the dependence of surfactant concentration in this surface tension value with solution
Curve, computer unit determine critical micelle concentration of the surfactant to be measured in this system according to corresponding analysis method
For about 0.047g/l.
Embodiment of the present utility model is not limited to above-described embodiment, does on the premise of without departing from this utility model objective
The various change for going out is belonged within protection domain of the present utility model.
Claims (5)
1. using the device of sessile drop method all automatic measurement liquid surface/interfacial tension, it is characterised in that：Including the hair for forming hanging drop
Tubule, the both sides of capillary tube are provided with background light source and image unit；Described the first pipelines of capillary tube Jing are connected with the first liquid feeding
Unit, the first liquid feeding unit and image unit are connected with computer；Described first liquid feeding unit configuration with ingress port and
The fluid valve of outlet port, the outlet port of fluid valve are connected with the first pipeline, and the ingress port of fluid valve is connected with second pipe
Road, the second pipeline are connected with second container.
2. the device of employing sessile drop method all automatic measurement liquid surface/interfacial tension according to claim 1, its feature exist
In：The 4th pipeline is provided with described second container, the 4th pipeline is connected with the second liquid feeding unit, and the second liquid feeding unit is connected with
3rd pipeline, the 3rd pipeline are connected with the 3rd container.
3. the device of employing sessile drop method all automatic measurement liquid surface/interfacial tension according to claim 1, its feature exist
In：The first container of printing opacity is provided with the outside of the port of export of described capillary tube, below the first container, regulating platform is provided with.
4. the device of employing sessile drop method all automatic measurement liquid surface/interfacial tension according to claim 3, its feature exist
In：The 5th pipeline is provided with the first described container, the 5th pipeline is connected with the 3rd liquid feeding unit, and the 3rd liquid feeding unit is connected with
6th pipeline, the 6th pipeline are connected with the 4th container.
5. the device of employing sessile drop method all automatic measurement liquid surface/interfacial tension according to claim 3, its feature exist
In：Agitating device is provided with below described second container and/or the first container.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109668939A (en) * | 2017-10-17 | 2019-04-23 | 上海宝钢钢材贸易有限公司 | A kind of liquid foam liquid phase fraction measuring device and dynamic measurement method |
| CN109709001A (en) * | 2017-10-25 | 2019-05-03 | 河北工业大学 | Based on optical Contact-angle measurement system |
| CN110376103A (en) * | 2019-07-10 | 2019-10-25 | 金华职业技术学院 | A kind of Surface Tension of Liquid Drops test device |
| WO2021247062A1 (en) * | 2020-06-04 | 2021-12-09 | Saudi Arabian Oil Company | Method of measurement of interfacial tension (ift) of two immiscible fluids at reservoir conditions |
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- 2016-08-28 CN CN201620974022.2U patent/CN206057137U/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109668939A (en) * | 2017-10-17 | 2019-04-23 | 上海宝钢钢材贸易有限公司 | A kind of liquid foam liquid phase fraction measuring device and dynamic measurement method |
| CN109709001A (en) * | 2017-10-25 | 2019-05-03 | 河北工业大学 | Based on optical Contact-angle measurement system |
| CN110376103A (en) * | 2019-07-10 | 2019-10-25 | 金华职业技术学院 | A kind of Surface Tension of Liquid Drops test device |
| CN110376103B (en) * | 2019-07-10 | 2024-04-09 | 金华职业技术学院 | Liquid drop surface tension testing device |
| WO2021247062A1 (en) * | 2020-06-04 | 2021-12-09 | Saudi Arabian Oil Company | Method of measurement of interfacial tension (ift) of two immiscible fluids at reservoir conditions |
| US11649708B2 (en) | 2020-06-04 | 2023-05-16 | Saudi Arabian Oil Company | Method of measurement of interfacial tension (IFT) of two immiscible fluids at reservoir conditions: an in situ gas buffered injection |
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