CN105987866A - Heterogeneous liquid settlement automatic-monitoring method and device - Google Patents
Heterogeneous liquid settlement automatic-monitoring method and device Download PDFInfo
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Abstract
The invention discloses a heterogeneous liquid settlement automatic-monitoring method and device and concretely discloses a heterogeneous liquid settlement automatic-monitoring device and a heterogeneous liquid settlement automatic-monitoring method using the device. The device comprises a sample bearing device, an image acquisition device, a control device and an optional data processing device. The device has a simple structure and can be operated easily. Compared with the traditional artificial measurement method, the method provided by the invention has the advantages of time saving, continuity, reliability and accuracy. The device and method have an important latent application value in the scientific research and production application fields of pharmaceutics, chemistry and chemical engineering, materials science and food processing.
Description
Technical field
The present invention relates to field of medicine and chemical technology, more particularly to a kind of heterogeneous liquid Monitoring method of the subsidence and set
Standby.
Background technology
Sedimentation refers to microgranule in a fluid under gravity, and the motion of deposition, refers generally in a liquid downwards
The sedimentation of solid particle.Sedimentation speed and the particle diameter of microgranule, the density of microgranule, the density of fluid and viscosity,
Temperature, fluid the factor such as kinestate relevant, in different field, for different application, can be by adding table
Face activating agent, suspending agent, stabilizer, flocculant, flocculating agent, deflocculant, regulate the heavy of heterogeneous system
Fall feature.The mensuration of sedimentation dynamic process, important in inhibiting in the fields such as medicament, chemical industry, food.
In art of pharmacy, the heterogeneous formulation such as sol, Emulsion, suspensoid as regular dosage form in clinic
On be widely used, with incompatible liquid, Solid drug particles as dispersed substance, with gaseous state, liquid continuous phase for point
Dispersion media and the heterogeneous system that constitutes.The sedimentation of heterogeneous formulation system is to affect its physical stability and clinical treatment
The principal element of effect, is also the major criterion weighing preparation product quality, and therefore state-promulgated pharmacopoeia regulation suspensoid is in matter
Measuring and need in checking to check sedimentation volume ratio, be to weigh one of the most qualified major criterion of product, sedimentation is too much, mistake
Hurry up, the meaning that medicine is made suspensoid will be lost, so sedimentation volume ratio must be up to standard, its product of guarantee
Quality.Formulation process is widely present the operation of the process to heterogeneous system simultaneously, such as: dispersion, mistake
Filter, centrifugal, clean system etc., study its sedimentation dynamic characteristic, processed at heterogeneous formulation Formulation, medicine
Important in inhibiting in journey.
For mixed suspension preparation, according to 2010 editions Chinese Pharmacopoeias, its assay method: test sample 50 contained by apparatus plug graduated cylinder
ML, close plug, firmly shaking 1 minute, write down the beginning height H of suspended matter0, stand 3 hours, write down suspended matter
Final height H, be calculated as follows:
With sedimentation volumn ratio as vertical coordinate, the sedimentation time is abscissa mapping, can obtain subsidence curve, according to sedimentation
The shape of curve may determine that the quality of suspensoid Formulation.The more gentle slow reduction of subsidence curve is it is believed that locate
Side's excellent in design.
In chemical material field, along with being widely used of macromolecular material, particularly at building, traffic and electricity
A large amount of uses of the aspects such as sub-electrical equipment, danger and the hazardness of fire considerably increase.Use and add magnesium hydroxide
The polymeric material of fire retardant, can improve tradition halogen containing flame-retardant material due to thermal decomposition and burning produce a large amount of smog and
Poisonous, the shortcoming of corrosive hydrogen halides gas, for overcoming the shortcoming of magnesium hydroxide dispersibility, poor compatibility, improves
Serviceability, it is necessary to it is carried out surface modification treatment and eliminates surface polarity, change the surface nature of magnesium hydroxide,
To solve the compatibility and the problem of bad dispersibility.With surface modifier, magnesium hydroxide is carried out wet process surface treatment, logical
Cross the magnesium hydrate powder after sedimentation velocity test before modified and it is characterized, so that it is determined that modifying agent kind,
The process conditions of the surface modifications such as amount of modifier, modification temperature and modification time.
In food processing field, the finished product of food processing field and intermediate major part are with heterogeneous suspending system
Presented in, as acidic milk drink can be divided into fermented type and the big class of layout type two by its machining process.This
The protein beverage planting trophism is difficult to keep uniform stability status, and easily how layering and precipitation, ensure
In beverage, the stability of protein is one of numerous food product producer urgent problem.Lactic acid beverage to be made exists
Do not produce layering or precipitation in shelf-life, improve stability, i.e. to reduce the sedimentation velocity of granule as much as possible, make
It is substantially equal to zero.
Existing sedimentation dynamic process assay method rests essentially within artificial sxemiquantitative observation, trend contrast, lacks
Quantitative dynamic analysis, in actual application, different system sedimentation spans cycle time are big, and reading sampling interval is each not
Identical, when sample to be tested is too much, the resources costs such as manpower, time is high, and the relatively big directly shadow of artificial error in reading
Ring the accuracy of result.A small amount of/micro-example, multiple batches of parallel control, essence in preparation R&D process cannot be met
The amount of determination, the mensuration demand of long time period.
Summary of the invention
It is an object of the invention to provide a kind of heterogeneous liquid settlement automatic monitoring method and device.
A first aspect of the present invention, it is provided that the settlement automatic monitoring equipment of a kind of heterogeneous liquid, described equipment
Including:
Sample bearing device, described sample bearing device contains the container of testing sample, Qi Zhongsuo for laying
Stating testing sample is the heterogeneous liquid that sedimentation can occur；
Image collecting device, described image collecting device is arranged to be used for gathering the image letter of described sample
Breath；
Controlling device, described control device is arranged to be used for controlling the work of described image collecting device；With
Optional data processing equipment, described data processing equipment is arranged to be used for identifying described image information
In liquid level demarcation line, and/or identify liquid level boundary line further over time.
In another preference, described image collecting device is arranged to gather the image of sample in different time points
Obtain the sample image information comprising many hardwoods image.
In another preference, the image information of described sample is selected from lower group: the intensity of reflected light or glimmering of sample
Light intensity.
In another preference, described sample bearing device can lay one or more (such as 2,3,4,5,
6,7,8,9,10) contain testing sample container.
In another preference, described data processing equipment includes that data processing module and result derive module,
Described data processing module for processing the image information that collects, and store brightness value, positional information and time
Between information；Described result derives module and is used for deriving sedimentation kinetics equation and drawing subsidence curve.
In another preference, the settlement automatic monitoring equipment of described heterogeneous liquid also includes casing and luminous dress
Putting, described sample bearing device, described image collecting device and described light-emitting device are placed in described casing,
Described light-emitting device provides light source for described image collecting device；Preferably, described light-emitting device is luminous strong
Degree is for adjustable.
In another preference, one or more in lower group of described light source: the micro-light source of LED, LED
Array light source, LED area light source, shadowless lamp, cold light source bulb (xenon lamp), laser diode and gas swash
Light device.
In another preference, described equipment also includes that temperature-adjusting device, described temperature-adjusting device are set
It is set to the temperature for regulating sample.
In another preference, described control device is additionally operable to control described temperature-adjusting device and/or luminous dress
Put.
In another preference, described " control " includes the image setting and/or changing described image collecting device
Frequency acquisition, image acquisition quantity；And/or
Set and/or change described thermostatic target temperature；And/or
Set and/or change light intensity and/or the light application time of described light-emitting device.
In another preference, described sample bearing device includes liquid container and fixes described liquid container
Support.
In another preference, described support is provided with the hole corresponding with described liquid container, and described liquid holds
Device is laid on the bracket by described hole, and described support is provided with longitudinal window, when equipped with treating test sample
When the described liquid container of product is laid on the bracket, described image collecting device passes through described window collection
The image information of described sample.In another preference, described container is transparent or semitransparent.Described
Hole has the space of accommodating described liquid container, when the described liquid container equipped with testing sample is placed in described
Time on support, the part equipped with testing sample of the most described liquid container is positioned at described hole, in described hole
On the window offered allow the state from external observation to testing sample.
In another preference, the material of described liquid container is selected from: acrylic, quartz glass, simple glass,
Phenolic resin and silica gel, preferably quartz glass.
In another preference, described liquid container is flat based tubes.
In another preference, described image collecting device includes that image acquisition device and guide rail, described image are adopted
Storage is movably arranged on described guide rail.
In another preference, one or more in lower group of described image acquisition device: line array CCD, face
Battle array CCD, industrial CCD/CMOS, high resolution CCD/CMOS and fluorescent probe.
In another preference, described temperature-adjusting device includes temperature sensor, heater and radiator.
In another preference, described temperature-adjusting device uses water-bath, metal bath or gas bath to control described sample
Temperature.In another preference, described support is that (preferably copper, copper alloy, aluminum or aluminum closes metal rack
Gold support), described temperature-adjusting device controls the temperature of described sample to be tested by described metal rack.
In another preference, described heater is positioned at the lower section of described support.
In another preference, described casing is provided with vent.
In another preference, described casing is camera bellows.
In another preference, described device also includes background board.
A second aspect of the present invention, it is provided that a kind of method monitoring heterogeneous liquid sedimentation, described method includes
Step:
A () provides heterogeneous liquid sample and gathers the image information of described sample
The image using image collecting device to gather sample in different time points obtains the sample drawing comprising many hardwoods image
As information；
B () processes image information
(b1) uniformity extracting every hardwood image target area after each hardwood image gray processing gathered step (a) is special
Reference breath (preferably, described uniformity characteristic information is brightness value), draws characteristic curve；
(b2) formed after the characteristic curve of each hardwood image being merged according to image acquisition time and comprise the three of temporal information
Dimension sedimentation kinetics surface model.By analyze this this three-dimensional sedimentation kinetics surface model, i.e. can obtain non-all
The sedimentation dynamic information of phase fluid sample, including sedimentation kinetic curve and sedimentation kinetics equation.
In another preference, described method further comprises the steps of:
(b3) the three-dimensional sedimentation kinetics surface model obtained in step (b2) is processed
On reservation three-dimensional sedimentation kinetics surface model, region at sedimentation boundary, removes other region, builds through matching
Mould obtains sedimentation kinetic curve and the sedimentation kinetics equation of described sample.
In another preference, in described step (b3), at described sedimentation boundary, the determination method in region is: institute
State characteristic curve and occur that the position suddenlyd change is liquid level boundary region；Preferably, at curve sudden change, described curve
Slope be liquid level boundary curve at change in the range of 20 °～90 °.
In another preference, in described step (a), under specified time interval, described sample is carried out image and adopt
Collection obtains the sample image information comprising many hardwoods sample image.Described specified time interval can be 0.1s-1h,
I.e., it is possible to carry out an image acquisition every 0.1s, it is also possible to carry out an image acquisition every 1h, concrete
Interval time is depending on sample.
In another preference, in described step (b1), described characteristic curve is bright to liquid bottom for reflection liquid level
The curve of degree Strength Changes.
In another preference, described sedimentation kinetic curve is the reaction time dependent curve of sedimentation volume ratio.
In another preference, described method further comprises the steps of:
The stability of heterogeneous liquid sample is entered by c sedimentation kinetic curve and equation that () obtains according to step (b)
Row quantitative assessment also exports mensuration report.
In another preference, in described step (b1), after each hardwood image gray processing that will obtain in step (a)
Carry out Image semantic classification, extract characteristic area, store brightness value and time point information, and draw described characteristic curve.
In another preference, in described step (b1), described Image semantic classification includes:
(i) image enhaucament: use Space domain and/or frequency domain method to improve visual quality of images；
(ii) filtering: use the method for wave filter and/or Wiener filtering to extract echo signal from noise (bright
Angle value)；
(iii) limb recognition: use Roberts operator, Kirsch operator to detect step change type edge, use
Laplacian operator detection ridge or edge effect type picture element, use threshold value responsive type Sobel and
Prewitt operator detection fuzzy edge, it is achieved non-threshold values detects；
(iv) image segmentation: the image partition method of use includes image partition method (threshold value based on region
Method, region-growing method, split degree method), image partition method (Robert operator, Sobel of based on edge
Operator, Pre-witt operator, Canny operator, Laplace operator, method of differential operator, frontier tracing method)
And mixed type image partition method (genetic algorithm, wavelet transformation, Snake model), divide the image into
Several regions specific, with unique properties also propose interesting target (e.g., settling zone), based on
The area in this calculated settlement region.
In another preference, in described step (b), the image collected is carried out pretreatment, reduce noise
Interference, improves the image quality of image；Image is carried out gray processing, finds out ash by target recognition, image segmentation
The edge feature of degree image, determines liquid level demarcation line, and then draws the level change in every hardwood image；Never simultaneously
Between put the image of collection extract sedimentation boundary feature point set, obtain subsidence curve through matching.
In should be understood that within the scope of the present invention, above-mentioned each technical characteristic of the present invention and below (as implemented
Example) in can be combined with each other between each technical characteristic of specifically describing, thus constitute new or preferred skill
Art scheme.As space is limited, the most tired at this state.
Accompanying drawing explanation
Figure 1A shows the structural representation of preferably apparatus of the present invention；
Figure 1B shows the perspective view of preferably apparatus of the present invention；
Fig. 1 C shows the sectional structure schematic diagram of preferably apparatus of the present invention；
Fig. 1 D shows the sample bearing device structural representation of preferably apparatus of the present invention；
Fig. 1 E shows the preferably sample bearing device of apparatus of the present invention and a temperature-adjusting device structure
Schematic diagram；
Fig. 1 F shows the preferably sample bearing device of apparatus of the present invention and a temperature-adjusting device structure
Schematic diagram；
Fig. 1 G shows the supporting structure schematic diagram of preferably apparatus of the present invention；
Fig. 1 H shows the plan structure schematic diagram of preferably apparatus of the present invention；
Fig. 2 shows single image and the characteristic curve thereof of embodiment 2；
Fig. 3 shows three typical images and characteristic curve thereof in the infall process of embodiment 2；
Fig. 4 shows the settling characteristics information time sequence three-dimensional surface model of embodiment 2；
Fig. 5 shows the sedimentation boundary detection figure after the settling characteristics information retrieval of embodiment 2；
Fig. 6 shows that the sedimentation boundary of embodiment 2 determines method；
Fig. 7 shows the sedimentation kinetics equation matched curve of embodiment 2；
Fig. 8 A shows the sedimentation kinetics equation in Fig. 7；
Fig. 8 B shows the different interval acquired results difference analysis of embodiment 2, dynamic including sedimentation
Mechanical equation matched curve and sedimentation kinetics equation；
Fig. 9 shows three typical images and characteristic curve thereof in the infall process of embodiment 3；
Figure 10 shows the settling characteristics information time sequence three-dimension curved surface of embodiment 3；
Figure 11 shows that the sedimentation boundary after the settling characteristics information retrieval of embodiment 3 detects；
Figure 12 shows that the sedimentation boundary of embodiment 3 determines method；
Figure 13 shows the sedimentation kinetics equation matched curve of embodiment 3；
Figure 14 shows the sedimentation kinetics equation of embodiment 3；
Figure 15 shows three typical images and characteristic curve thereof in the infall process of embodiment 4；
Figure 16 shows the settling characteristics information time sequence three-dimension curved surface of embodiment 4；
Figure 17 shows that the sedimentation boundary after the settling characteristics information retrieval of embodiment 4 detects；
Figure 18 shows that the sedimentation boundary of embodiment 4 determines method.
Detailed description of the invention
The present inventor is by extensively in-depth study, it is thus achieved that a kind of heterogeneous liquid settlement automatic monitoring method
And device, use the method for the present invention to be capable of the automatic monitoring to heterogeneous liquid sedimentation, can be to suspendible
The stability of system carries out quantitative assessment, has intellectuality, automatization, precision height, sensitivity advantages of higher.
One of the present invention preferred embodiment in, the method for described monitoring heterogeneous liquid sedimentation includes
Following steps:
A the heterogeneous system to be measured in () loading sedimentation pipe fully shakes up after, put in monitoring device,
The parameters such as light-source brightness, focal length, amplification are adjusted to optimum efficiency；
(b) programmable interval, image acquisition quantity；
C () gathers the uniformity characteristic information of target area setting time point；
D () sets up sedimentation kinetics surface model；
E interference region is rejected in the compacting of () threshold value, segmentation, extract sedimentation boundary eigenvalue and obtain sedimentation
Kinetics point set data；
(f) numerical fitting output sedimentation kinetics equation and sedimentation kinetic curve.
One of the present invention preferred embodiment in, the settlement automatic monitoring of described heterogeneous liquid sets
For including: imaging system, environmental control system and quantitative kinetic analysis system.
(1) imaging system described in comprises light source module and image capture module.
Light source module provides light stable, uniform, adjustable for sedimentation kinetics image information collecting process
According to condition, thus obtaining high quality graphic data, described light-source system should meet claimed below: flat
Face, cold light source, stable, anti-interference, brightness is adjustable, homogenous diffusion light type；Brightness is high, the life-span is long,
Heating is less, temperature is low, light is soft natural without stroboscopic, energy saving, easy for installation.Described light
Origin system is selected from the micro-light source of LED, LED line array light source, LED area light source, shadowless lamp, cold light source
Bulb (xenon lamp), laser diode, gas laser one or more, and be not limited only to these,
For required precision the highest time the micro-light source of preferred LED；During laser-induced fluorescence (LIF) is tested, preferably
Laser diode.
Described image capture module is used for gathering settling characteristics information, comprise image acquisition detector and
Image acquisition control system.
Described image acquisition detector should meet claimed below: big panel CMOS or CCD panel,
High-resolution 10～15M, programmability, focal length, brightness, contrast, white balance, amplification
Can program calling and controlling, low distortion, can long-time stable collection；Self-scanning, high sensitivity, lightweight,
Volume is little, location of pixels is accurate, little power consumption, life-span length, good reliability, convenient signal treatment, connect
Mouth is abundant to be easily programmed.Described detector is selected from line array CCD, area array CCD, industry
CCD/CMOS, high resolution CCD/CMOS camera, fluorescent probe (coordinating fluorescent agent to use)
One or more.
Technical grade image acquisition detector good stability, each photosensitive unit of CMOS photo-sensitive cell
Being independent, also not interfering with other unit even if damaging, therefore price is relatively low；Secondly as
Each unit independently carries out signal amplification and analog/digital conversion, and the most not only power consumption is the lowest, and whole
The volume of module is the least.But, owing to part bigger in photosensitive unit is exaggerated device and analog
Converting unit occupies, and the aperture opening ratio of traditional cmos element is the lowest, thus causes light utilization ratio poor；
Additionally, due to each unit independently exports, the amplification of initial signal is difficult to accomplish strict unification, because of
The noise problem ratio of this image is more serious.
The advantage of line array CCD is that one-dimensional pixel number can be made a lot, and total pixel number angle relatively face battle array
CCD camera is few, and pixel dimension is relatively more flexible, and frame width number is high, is particularly well-suited to one-dimensional dynamic mesh
Target is measured.And line array CCD resolving power is high, cheap, great majority can be met and measure visual field
Requirement, but obtain two dimensional image with line array CCD, it is necessary to be equipped with scanning motion, and in order to enable
Determine image each pixel correspondence position on measured piece, it is necessary to be equipped with the devices such as grating with note
The coordinate of the record every one scan line of line array CCD.Supposedly, the requirement of these two aspects causes using linear array
CCD obtains image following deficiency: image acquisition time is long, measures efficiency low；Due to scanning motion
And the existence of corresponding position feedback element, add system complexity and cost；The precision of images may
Affected by scanning motion precision and reduced, finally affected certainty of measurement.
The fluorescent characteristic that laser Induced Fluorescence Technology is excited by Study of Laser is come qualitatively or quantitatively
Determine the character of test substances.Owing to the fluorescence of numerous organic and inorganic compound own endogenous is imitated
Rate is low, in order to distinguish various different sample or the different piece of same sample, must be aided with all kinds of glimmering
Light probe or fluorometric reagent carry out specific binding with testing sample.Mainly consider during selection following because of
Element: excitation wavelength and fluorescence emission wavelengths；Light stability and photobleaching；Fluorescence qualitative and quantitative；
Toxicity；The pH environment being suitable for.
When less demanding to certainty of measurement, monitoring the time longer time, preferably industry cmos image detection
Device；When certainty of measurement requires that high, the monitoring time is shorter, preferably industrial CCD image detector.When
When certainty of measurement requires granule water white transparency in higher, testing sample, preferably fluorescent probe (coordinates glimmering
Photo etching uses).
Described image acquisition control system, is used for regulating and controlling image acquisition detector, regulates optimal imaging
Parameter, foundation high speed, high-resolution, the image-pickup method of low distortion, set up controlled infall process
Detection environment, it is ensured that the concordance of measurement result, repeatability.
(2) it is different that the environmental control system described in comprises temperature control module, standardization settling module, camera bellows
Change background module.
It is setting value that described temperature control module is used for keeping sedimentation to measure ambient temperature, can programme-control liter
Cooling.Following condition need to be met: temperature-15～100 DEG C of continuously adjustabe, temperature control sensitivity and error symbol
Standardization.Selecting the one in water-bath, metal bath, gas bath according to operation principle, bath temperature balances
Hurry up, but temperature control scope is narrower, when water circulates, imaging effect can be produced impact, dress can be increased
Put size；Metal bath uses micro computer and semiconductor refrigerating/thermal technology to realize temperature control, utilizes metal pattern
Block heats, and faster, temperature control is accurate for warming and cooling rate, and device also becomes the exquisitest small and exquisite, metal
Module need not add water, clean easy to clean；Gas bath is easy to use, but hygral equilibrium is slow, accuracy of temperature control
Relatively low.Therefore preferred metal bath.
Described standardization settling module is for ensureing the most controlled sedimentation environment, and core component is heavy
Fall measures pipe, and sedimentation measures pipe (preferably standard size) should meet following condition: high transmission rate, low
Reflecting rate, to lead hot/cold performance good.Material is selected from acrylic, quartz glass, simple glass, phenolic aldehyde
Resin, the one in silica gel, preferably quartz glass.
Described camera bellows alienation background module, during being used for keeping settlement monitoring, environment is consistent, core
Parts refer to differentiation background and camera bellows.For reduce later image analyze workload, background need to meet with
Lower requirement: primary colours are adjustable, sub-light exquisiteness backboard, aberration strengthen.Camera bellows is used for keeping settlement monitoring mistake
In journey, environment is consistent, it is to avoid extraneous light intensity change, affects image acquisition effect；Keep box house temperature
Spend constant, need to meet claimed below: sealing, light tight, shielding external interference, insulation.Material selects
From: rustless steel, acrylic, ferrum, extruded polystyrene foam plastics, mold pressing type polystyrene steep
One or more in foam plastics.
(3) the image quantitative kinetic analysis system described in, including: visualization exports mould with result
Block, image optimization strengthen module, characteristic extracting module, image analysis module, quantitative analysis module.
Utilize visualization with output object module, set image acquisition quantity, interval time, temperature,
Adjust detector focal length, adjust light intensity；Utilize image optimization to strengthen module, reduce the interference of noise,
Improve the image quality of image；Utilize characteristic extracting module, find out the edge feature of gray level image, really
Determine liquid level demarcation line, and then draw the level change in each image；Utilize image analysis module, from
Time series sedimentation result extracts sedimentation boundary feature point set, sets up sedimentation kinetics three-dimension curved surface mould
Type；Utilize quantitative analysis module, can obtain settling kinetics equation and subsidence curve.Image kinetics
The workflow of quantified system analysis is as follows:
The present invention preferred embodiment in, the operation that described characteristic extracting module performs includes:
1) image enhaucament: main target is that image passes through image procossing so that it is visual quality of images is carried
High, it is simple to identify, improve the visual effect of image so that it is be more suitable for a certain specific occasion than original image
Application, it is simple to for computer disposal.According to processing the difference in territory, image enhaucament is broadly divided into two kinds of methods:
Space domain and frequency domain method.
2) filtering: purpose is to extract echo signal from noise.When the frequency spectrum of signal and noise is mutual
Time the most overlapping, band filter is separated, and otherwise needs the method using Wiener filtering to obtain the line of signal
Property Minimum Mean Squared Error estimation.Test wavelet transformation, wavelet soft-threshold, based on mathematical morphology, nerve net
Network theory, fuzzy theory, Anisotropic diffusion equation, high-order statistic and utilize Image Priori Knowledge to design
The noise-reduction method such as wave filter.
3) limb recognition: the extractive technique at edge is a key technology in sedimentation image procossing, Roberts
Operator, Kirsch operator are for detecting the edge of step change type, and Laplacian operator is used for detecting ridge or limit
The picture element of edge effect type, threshold value responsive type Sobel and Prewitt operator have stronger noise resisting ability,
Blurring edge detector realizes the detection of non-threshold values.
4) image segmentation: conventional dividing method be broadly divided into dividing method based on region (threshold method,
Region-growing method, split degree method), dividing method based on edge (Robert operator, Sobel operator,
Pre-witt operator, Canny operator, Laplace operator, method of differential operator, frontier tracing method) and
Mixed type (genetic algorithm, wavelet transformation, Snake model).
Main advantages of the present invention are:
(1) the heterogeneous liquid settlement automatic monitoring equipment of the present invention, it is possible to the heterogeneous liquid of monitoring of automatization
Body settles, and can be continuously monitored sample, highly sensitive, can to different settling behavior (rise, sink,
Layering etc.) it is monitored evaluating, can monitor multiple sample simultaneously, simple in construction, be easy to safeguard；
(2) the heterogeneous liquid settlement automatic monitoring method of the present invention, favorable reproducibility, digital image-wise is protected
The measurement result deposited records infall process truly, facilitates subsequent analysis, can review, will not because of the storage of image,
Transmission or a series of map functions such as duplication and change, can at any time history testing result be carried out reprocessing and
Analyse in depth；Processing accuracy is high, motility is high, the infall process information preserved with digital image form, joins
Close image optimization, analytical technology can complete feature information extraction, modeling analysis with high efficiency, with Traditional Man
Metering system compare have save time, continuously, reliably, the advantage such as accurately.
Below in conjunction with specific embodiment, state the present invention further.Should be understood that these embodiments are only used for
The bright present invention rather than restriction the scope of the present invention.The experiment side of unreceipted detailed conditions in the following example
Method, is generally carried out according to normal condition, or according to the condition proposed by manufacturer.
Embodiment 1 heterogeneous liquid settlement automatic monitoring equipment
As shown in Figure 1A, the settlement automatic monitoring equipment of the heterogeneous liquid in the present embodiment, including:
Sample bearing device 1, described sample bearing device 1 is used for laying the container containing testing sample, its
Described in testing sample be can occur sedimentation heterogeneous liquid；Image collecting device 2, described image acquisition
Device 2 is arranged to be used for gathering the image information of described sample；Control device 3, described control device 3
It is arranged to be used for controlling the work of described image collecting device 2；With data processing equipment 4, at described data
Reason device 4 is arranged to be used for the liquid level demarcation line identifying in described image information, and identifies liquid further
Boundary line, face is over time.Data processing equipment described in the present embodiment is computer.
Image collecting device 2 is arranged to gather the image of sample in different time points, it is thus achieved that comprise many hardwoods image
Sample image information.The image information of described sample can be intensity of reflected light or the fluorescence intensity of sample.
Sample bearing device 1 can lay one or more (such as 2,3,4,5,6,7,8,9,10)
Containing the container 11 of testing sample, in Figure 1B, the sample bearing device 1 of display can lay 6 Shengs simultaneously
The container 11 of dress testing sample, and detect in same batch.
Data processing equipment 4 includes that data processing module 41 and result derive module 42, and described data process
Module 41 is for processing the image information collected, and stores brightness value, positional information and temporal information；
Described result derives module 42 and is used for deriving sedimentation kinetics equation and drawing subsidence curve.
As shown in Figure 1B, the settlement automatic monitoring equipment of the heterogeneous liquid in the present embodiment also includes casing 6
With light-emitting device 5, described sample bearing device 1, described image collecting device 2 and described light-emitting device 5
Being placed in described casing 6, described light-emitting device 5 provides light source for described image collecting device 2；Described
The luminous intensity of electro-optical device 5 is adjustable, can regulate the luminescence of light-emitting device 5 by controlling device 3
Intensity.In the both sides of light-emitting device 5, reflector 51 can be set.
The light source of light-emitting device 5 can be: the micro-light source of LED, LED line array light source, LED area light source, nothing
Shadow lamp, cold light source bulb (xenon lamp), laser diode and gas laser etc..
Equipment in the present embodiment also includes that temperature-adjusting device 7, described temperature-adjusting device 7 are arranged to
For regulating the temperature of testing sample.Described temperature-adjusting device 7 can use water-bath, metal bath or gas bath
Control described sample temperature.
Described control device 3 can also control temperature-adjusting device 7 and light-emitting device 5, can set and/or
Change the picture-taken frequency of described image collecting device 2, image acquisition quantity；Set and/or change described temperature
The target temperature of degree adjusting means 7；Set and/or change light intensity and/or the illumination of described light-emitting device 5
Time.Control device 3 and can include display floater, show the occurrence of setting on a display panel.
Described sample bearing device 1 includes liquid container 11 and the support 12 of fixing described liquid container 11.
Support 12 can be common test tube support, it is also possible to be arranged to the form shown in Fig. 1 D, G, at support
12 are provided with the hole 121 corresponding with described liquid container 11, and described liquid container 11 is by described hole 121
Being placed on described support 12, described support is provided with longitudinal window 122, when the institute equipped with testing sample
Stating liquid container 11 when being placed on described support 12, described image collecting device 2 is through described window 122
Gather the image information of described sample.Liquid container 11 described in the present embodiment is transparent or semitransparent
Flat based tubes.
The material of liquid container 11 can be acrylic, quartz glass, simple glass, phenolic resin and silica gel,
It is preferably quartz glass.
Described image collecting device 2 includes image acquisition device 21 and guide rail 22, and described image acquisition device 21 can
Being arranged on described guide rail 22 of movement.In the present embodiment, it is provided with two guide rails, image acquisition device 21
Position can move with back and forth or left and right, to obtain optimal image capture position.
Image acquisition device 21 can be selected from: line array CCD, area array CCD, industrial CCD/CMOS, high-resolution
CCD/CMOS and fluorescent probe.
In the present embodiment, described support 12 is metal rack (preferably copper, copper alloy, aluminum or aluminum alloy
Support), described temperature-adjusting device 3 controls the temperature of described sample to be tested by described metal rack 12.
As referring to figure 1e, temperature-adjusting device 7 includes temperature sensor (not shown), radiator 71 and adds
Hot device 72.Heater 72 is placed in the lower section of support 12.In the present embodiment, casing 6 is camera bellows, Ke Yi
Can arrange vent on casing 6, radiator 71 is relative with the vent on casing 6.
In other embodiments, if using common support (such as test tube rack), can set after support
Put background board.
Embodiment 2 settling behavior is monitored
In monitoring standard test tube (flat based tubes), (microcrystalline Cellulose and colloidal microcrystalline cellulose are by certain for sample
Ratio mix) sedimentation (downwards) behavior.This experimental provision and method is utilized to be monitored, available essence
True subsidence curve and sedimentation kinetics equation.
Step 1: use the heterogeneous liquid settlement automatic monitoring device in embodiment 1, fills testing liquid
Entering in flat based tubes, adjusting light-source brightness is optimal imaging effect；Set image acquisition interval, adopt
Collection quantity, is monitored.
Step 2: combine Fig. 2, gathers after terminating, reads in whole picture, carry out automated graphics process (gray scale
Change), the uniformity characteristic information extracting target area in every pictures (i.e. flat based tubes) (includes test tube
And the brightness brightness between background, interface, clarifying area, sedimentation boundary and white suspendible part and test tube
Value), draw Line profile (characteristic curve), brightness between background area and flat based tubes, suspended matter
All there is sudden change in value.
Analyzing line profile to understand, there is sudden change i.e. ripple with flat based tubes upper end brightness value in liquid level position
At paddy a.Due to the accumulation of suspended matter in infall process, density increases, and causes brightness value to increase.In sample
Estimate so-called clarifying area and also there is solid particle, therefore cause curve brightness value the most slowly to increase, until
During the sedimentation face of arrival, at the appearance sudden change i.e. b that advances the speed.
C region between distance about 300-540 pixel is suspendible region (that is, the height of suspended matter),
Due to the instability of the condition such as illumination condition, CCD, cause the brightness value in c region that fluctuation occurs.
Image can be made to be distorted during due to CCD imaging, so it is quick to there is brightness value between region c, d
Declining region, d is suspendible sections bottom position, and e is bottom test tube, and f is black background region.
Step 3: when formation comprises after being merged according to image acquisition time by all characteristic curves (curve in Fig. 3)
Between the three-dimensional sedimentation kinetics surface model of information, as shown in Figure 4, Fig. 4 shows settling characteristics information time
Sequence three-dimension curved surface.Fig. 4 i.e. picture target area uniformity characteristic information stack result in time.Along with
The carrying out of infall process, Line profile (sedimentation separating surface) gradually turns right skew.By analyzing this this three
Dimension sedimentation kinetics surface model, i.e. can obtain the sedimentation dynamic information of heterogeneous liquid sample.
Step 4: Fig. 5 be obtain from the three-dimensional sedimentation kinetics surface model of Fig. 4 about position and time
Two dimension sedimentation information, has reflected out the position (yellow curve) over time of sedimentation boundary.In conjunction with Fig. 5,
After in test tube, sample has settled, at highs and lows, (target area is in Fig. 3 in suspendible region
White suspendible part) will appear from two and stablize separating surface (this two interfacial brightness values approximation, shows in Fig. 5
Two yellow area shown): left side yellow area is sedimentation boundary, and the right yellow area is bottom interference
Region (two yellow area have identical brightness value).In subsequent treatment, can be by interception position
Bottom interference region is removed (X1=520) by mode.
Step 5: Fig. 6 be obtain from the three-dimensional sedimentation kinetics surface model of Fig. 4 about position and brightness
The two-dimentional sedimentation information of value, it is possible to reflect the brightness value at sedimentation boundary, i.e. the brightness value at sedimentation boundary is about
In g region.In conjunction with Fig. 6, select appropriate brightness scope (in g region, brightness value span is 85-165,
For making matched curve more accurate, choosing brightness value is 118-119 scope), remove brightness value not in Figure 5
Region in the range of selected, (green in Fig. 7 is discontinuous to obtain sedimentation boundary key feature point set data
Curve), i.e. can obtain settling kinetics matched curve (Fig. 7) and equation (Fig. 8) through matching.
In the present embodiment, different brightness value spans is verified, as shown in Figure 8 B, in figure
Respectively to different intervals (in the g interval of Fig. 6), brightness value take respectively 90-100,100-110,
The sedimentation kinetics equation that 110-120,120-130,130-140,140-150,90-150 obtain is the most right
Should in fresult1 (x), fresult2 (x), fresult3 (x), fresult4 (x), fresult5 (x),
fresult6(x)、fresult7(x).Can draw from figure, in the g interval range of Fig. 6, take not
Same range of luminance values, obtained sedimentation kinetics equation matched curve (subsidence curve) difference is the least, says
The method of the bright present invention has good stability and repeatability.
Embodiment 3 monitors sedimentation (upwards) behavior of pik woods breast in cillin bottle
Sedimentation (upwards) behavior of pik woods breast in monitoring cillin bottle.The sedimentation of this sample is (the most attached at 200s
Closely settle), sample size few (putting into effective dimensions in cillin bottle is 150 pixels), liquid level sedimentation becomes
Changing little, artificial reading cannot obtain subsidence curve accurately.Therefore utilize this experimental provision and method to be monitored,
After difference is changed, available conventional subsidence curve (gradually successively decreasing) and sedimentation kinetics equation thereof.
Step 1: use the heterogeneous liquid settlement automatic monitoring device in embodiment 1, fills testing liquid
Entering in flat based tubes, adjusting light-source brightness is optimal imaging effect；Set time interval, collecting quantity,
It is monitored.
Step 2: combine Fig. 9,10,11,12, draws settling characteristics information time sequence three-dimension curved surface.
Figure 10 i.e. stack result of picture target area uniformity characteristic information.
Step 3: combine Figure 11, after in test tube, sample has settled, target area is at highs and lows
Place will appear from two and stablizes separating surface, two yellow area: right area is sedimentation boundary, left area
For upper end interference region.Choose suitable parameters to remove it.
Step 4: combine Figure 12,13,14, selects appropriate brightness scope, removable interference region,
Obtain settling kinetics equation and matched curve.
Embodiment 4 monitors the settling behavior of different prescription pik woods breasts in cillin bottle
The settling behavior (layering) of different prescription pik woods breasts in monitoring cillin bottle, this sample is the most significantly
Sedimentation boundary change procedure upwardly or downwardly, belongs to lamination.Utilize this experimental provision and method,
Available sample realizes correct time during layering.
Step 1: use the heterogeneous liquid settlement automatic monitoring device in embodiment 1, fills testing liquid
Entering in flat based tubes, adjusting light-source brightness is optimal imaging effect；Set time interval, collecting quantity,
It is monitored.
Step 2: combine Figure 15,16,17,18, draws settling characteristics information time sequence three-dimension curved surface.
Figure 16 i.e. stack result of picture target area uniformity characteristic information.As shown in figure 17, sample is the brightest
Aobvious rising or downward trend, belong to lamination.The matrix obtained is analyzed, obtains derivative
The data point of value correspondence, and then available sample greatly starts to occur the correct time of layering.
The all documents mentioned in the present invention are incorporated as reference the most in this application, just as each document
It is individually recited as with reference to like that.In addition, it is to be understood that after the above-mentioned teachings having read the present invention,
The present invention can be made various changes or modifications by those skilled in the art, and these equivalent form of values fall within this Shen equally
Please appended claims limited range.
Claims (10)
1. the settlement automatic monitoring equipment of a heterogeneous liquid, it is characterised in that described equipment includes:
Sample bearing device, described sample bearing device contains the container of testing sample, Qi Zhongsuo for laying
Stating testing sample is the heterogeneous liquid that sedimentation can occur；
Image collecting device, described image collecting device is arranged to be used for gathering the image letter of described sample
Breath；
Controlling device, described control device is arranged to be used for controlling the work of described image collecting device；With
Optional data processing equipment, described data processing equipment is arranged to be used for identifying described image information
In liquid level demarcation line, and/or identify liquid level boundary line further over time.
2. the settlement automatic monitoring equipment of heterogeneous liquid as claimed in claim 1, it is characterised in that institute
State image collecting device to be arranged to gather, in different time points, the sample that the image acquisition of sample comprises many hardwoods image
Image information.
3. the settlement automatic monitoring equipment of heterogeneous liquid as claimed in claim 1, it is characterised in that
The settlement automatic monitoring equipment of described heterogeneous liquid also includes casing and light-emitting device, and described sample carries
Device, described image collecting device and described light-emitting device are placed in described casing, and described light-emitting device is institute
State image collecting device and light source is provided；Preferably, the luminous intensity of described light-emitting device is adjustable.
4. the settlement automatic monitoring equipment of heterogeneous liquid as claimed in claim 1, it is characterised in that
The settlement automatic monitoring equipment of described heterogeneous liquid also includes temperature-adjusting device, described temperature regulation dress
Put the temperature being arranged to be used for regulating sample.
5. the settlement automatic monitoring equipment of heterogeneous liquid as claimed in claim 1, it is characterised in that
Described sample bearing device includes liquid container and the support of fixing described liquid container；Preferably, described
Support is provided with the hole corresponding with described liquid container, and described liquid container is placed in described by described hole
On frame, described support is provided with longitudinal window, when the described liquid container equipped with testing sample is placed in institute
When stating on support, described image collecting device gathers the image information of described sample through described window.
6. the settlement automatic monitoring equipment of heterogeneous liquid as claimed in claim 1, it is characterised in that
Described image collecting device includes that image acquisition device and guide rail, described image acquisition device are movably arranged at institute
State on guide rail.
7. the method monitoring heterogeneous liquid sedimentation, it is characterised in that described method includes step:
A () provides heterogeneous liquid sample and gathers the image information of described sample
The image using image collecting device to gather sample in different time points obtains the sample drawing comprising many hardwoods image
As information；
B () processes image information
(b1) uniformity extracting every hardwood image target area after each hardwood image gray processing gathered step (a) is special
Reference breath (preferably, described uniformity characteristic information is brightness value), draws characteristic curve；
(b2) formed after the characteristic curve of each hardwood image being merged according to image acquisition time and comprise the three of temporal information
Dimension sedimentation kinetics surface model.
8. method as claimed in claim 7, it is characterised in that described method further comprises the steps of:
(b3) the three-dimensional sedimentation kinetics surface model obtained in step (b2) is processed
On reservation three-dimensional sedimentation kinetics surface model, region at sedimentation boundary, removes other region, builds through matching
Mould obtains sedimentation kinetic curve and the sedimentation kinetics equation of described sample.
9. method as claimed in claim 8, it is characterised in that in described step (b3), described sedimentation boundary
The determination method in region, place is: described characteristic curve occurs that the position of sudden change is liquid level boundary region；Preferably,
At curve sudden change, described slope of a curve is liquid level boundary curve in the range of 20 °～90 ° at change.
10. method as claimed in claim 8, it is characterised in that described method further comprises the steps of:
The stability of heterogeneous liquid sample is entered by c sedimentation kinetic curve and equation that () obtains according to step (b)
Row quantitative assessment also exports mensuration report.
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| CN109085098A (en) * | 2017-06-14 | 2018-12-25 | 北京精微视觉科技有限公司 | A kind of detection method and detection device of cell settlement progress |
| CN111610173A (en) * | 2020-05-27 | 2020-09-01 | 中国水利水电科学研究院 | Three-dimensional fluid concentration field calibration device and calibration method |
| CN117871353A (en) * | 2024-03-11 | 2024-04-12 | 天津美腾科技股份有限公司 | Coal slime water sedimentation detection method and system |
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