CN105527224B - A device and method for analyzing a sample - Google Patents
A device and method for analyzing a sample Download PDFInfo
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- CN105527224B CN105527224B CN201410514959.7A CN201410514959A CN105527224B CN 105527224 B CN105527224 B CN 105527224B CN 201410514959 A CN201410514959 A CN 201410514959A CN 105527224 B CN105527224 B CN 105527224B
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Abstract
A kind of equipment (20) for analyzing sample, comprising: electromagnetic radiation source (1) is configured to generate incidence electromagnetic radiation beam (2)；Sample container (5), it is configured to receive the sample to be analyzed, shape the sample container (5), with symmetry axis (25), arrange the sample container (5), to receive incidence electromagnetic radiation beam (2), to travel in sample container (5), it interacts with sample, and the sample container (5) is arranged, so that the scattered electromagnetic radiation beam (6) to be detected travels to the outside of sample container (5)；And electromagnetic radiation detector (12), it is configured to detect the scattered electromagnetic radiation beam (6) to be detected received from sample container (5), wherein the direction relative to incidence electromagnetic radiation beam (2) determines the orientation of sample container (5), so that incidence electromagnetic radiation beam (2) just in traveling to sample container (5) before to the incident track of symmetry axis (25) relative to the scattered electromagnetic radiation beam (6) to be detected from symmetry axis (25) just leave sample container (5) to scattered electromagnetic radiation beam (6) after position Scattering Trajectories it is symmetrical, so that the Scattering Trajectories of sample container (5) outside are unrelated with sample container (5) and sample refractive index.
Description
Technical field
The present invention relates to a kind of equipment for analyzing sample.
In addition, the present invention relates to a kind of methods for analyzing sample.
Background technique
In order to analyze fluid sample, fluid sample can be injected in sample container.Then, make electromagnetic radiation beam and liquid
Sample interaction, wherein scattered electromagnetic radiation Shu Ranhou can carry the physical property and chemical property for indicating fluid sample
Information.
Refer to US 2004/100630, GB 2,494,734, DE 102008007743, US 2004/251134, GB
2,494,735 and US 4,710,643.
WO 2011/092510 discloses a kind of by the small of static and/or dynamic light scattering characterization fluid sample
Cup, the cuvette have the main body that fluid sample is kept merely with surface tension.In addition, it is scattered to additionally provide a kind of light including cuvette
Penetrate instrument.Further it is provided that a kind of method for being used to prepare the cuvette including fluid sample, this method include to cuvette loading liquid
The step of body sample.Further it is provided that a kind of method for characterizing fluid sample, the method includes analysis be included in it is small
Cup in fluid sample the step of.Cuvette can be used for keeping fluid sample, and can be also used for light scattering experiments.
US 5,572,321 is related to a kind of for measuring the device of the luminous density of the thin films scattering of colloidal medium.More specifically
It says on ground, it is intended that carry out submicron particle size analysis using photon correlation, and including the thin films scattering for measuring colloidal medium
The device of luminous density.The device includes: monochromatic source；Convergent optical system, for making light-resource fousing in the film to be analyzed；
At least one photosensitive detector, for detecting thin films scattering or backscattering light；And for handling from one or
The system of the signal of the multiple photoelectric detectors of person.
Surge light scattering (ELS) equipment for measuring boundary up to the current potential of particle in dispersion can use interferometer to arrange,
In interferometer arrangement, the light of the particle scattering in sample is Chong Die with reference beam.Dynamic can also be determined using corresponding arrangement
Light scatters the granular size of (DLS).
This equipment can be equipped with the detection system using optical fiber.For specific sample, optical means tune can use
The equipment is saved, and then, other samples which can be used to have identical dispersive medium.However, if utilizing it
His solvent, the especially solvent with other refractive index values analyze sample, then need to adjust optical element again.
Such as the commercial equipment of Malvern Zetasizer is equipped with various compensating modules, compensating module counteracting has
This variation caused by the solvent of another refractive index value.Make customer analysis that there is the sample of different refractivity value in this way.
Therefore, in traditional equipment, the variation of the refractive index of specimen holder and sample leads to the scattering electromagnetism for leaving specimen holder
The track of radiation beam changes, or needs to compensate by increasing Additional optical unit.Former instance leads to measurement not
Accurately, the complex appts that latter instance causes area occupied big, and/or for user's inconvenience.
Summary of the invention
The object of the present invention is to provide a kind of unrelated with used sample container and sample, based on simple electromagnetic radiation
High-precision sample measurement system.
To achieve the goals above, the device and method according to independent claims are provided.
Exemplary embodiment in accordance with the present invention, provides a kind of equipment for analyzing sample, which includes: electromagnetism spoke
Source is penetrated, the electromagnetic radiation source is constructed, to generate incidence electromagnetic radiation beam；Sample container constructs the sample container, to be divided with accommodating
The sample of analysis shapes the sample container, to arrange the sample container with symmetry axis, to receive incidence electromagnetic radiation beam, thus
It travels in sample container, interacts with sample, and arrange the sample container, so that the scattered electromagnetic radiation beam to be detected
Travel to the outside of sample container；And electromagnetic radiation detector, the electromagnetic radiation detector is constructed, to detect from sample container
The scattered electromagnetic radiation beam to be detected received, wherein the direction relative to incidence electromagnetic radiation beam determines the orientation of sample container
(especially tilt sample container, more particularly operate using inclined twice makes sample container incline with two different inclined shafts
Tiltedly), so that incidence electromagnetic radiation beam (especially along from) just before traveling in sample container (position) to symmetrical
The incident track of axis (path) is relative to the scattered electromagnetic radiation beam (especially along) to be detected from symmetry axis to scattering electricity
The Scattering Trajectories that magnetic radiation beam just leaves the position (path) after sample container are symmetrical, so that the scattering outside sample container
Track is unrelated with sample container and sample refractive index.
Another exemplary embodiments according to the present invention provide a kind of method for analyzing sample, wherein this method comprises:
Make incidence electromagnetic radiation beam to the sample container for accommodating the sample to be analyzed and shapes the sample container with symmetry axis
(25)；Incidence electromagnetic radiation beam is received by sample container, to travel in sample container, to interact with sample；Make to want
The scattered electromagnetic radiation beam of detection travels to sample container；Detect the scattered electromagnetic radiation to be detected received from sample container
Beam；And the direction relative to incidence electromagnetic radiation beam determines the orientation of sample container, so that incidence electromagnetic radiation beam just exists
Before traveling in sample container to the incident track of symmetry axis relative to the scattered electromagnetic radiation beam to be detected from symmetry axis to
The Scattering Trajectories that scattered electromagnetic radiation beam just leaves the position after sample container are symmetrical, so that the Scattering Trajectories outside sample container
It is unrelated with sample container and sample refractive index.
In the description of the present application, term " symmetry axis of sample container " can refer in particular to extend along sample container straight
Axis, wherein the section of sample container is relative between end bearing and respective planes in each section perpendicular to symmetry axis
Intersect point symmetry (or at least substantially symmetrical).In particular, the symmetry axis of tubular sample container is made of its drum shaft.
In the description of the present application, term " symmetrical footprint " can be refered in particular to, and by executing symmetry operation, (such as mirror image becomes
Change), track (that is, incident track or Scattering Trajectories) may map to another track (that is, Scattering Trajectories or entering
Penetrate track), vice versa.In particular, the symmetrical footprint can be mutually symmetrical in the axial direction, and more particularly, at two
In space protection, which can be mutually symmetrical in the axial direction (especially when watching from two orthogonal directions).
In the description of the present application, statement " Scattering Trajectories and sample container outside sample container and sample refraction
Rate is unrelated " the scattered electromagnetic radiation beam direction of propagation outside sample container can be refered in particular to (more precisely, directive electromagnet radiation detection
The direction of propagation of a part of scattered electromagnetic radiation of device) be not dependent on sample container material and/or sample in it
The refractive index of material.It can also refer to, in the different materials and/or difference by the different sample containers with different refractivity value
Between the different scattered electromagnetic radiation beams of the different materials scattering of sample, space displacement does not occur.
In the description of the present application, term " the scattered electromagnetic radiation beam to be detected " can be refered in particular to, by incoming electromagnetic spoke
The specific part for the scattered electromagnetic radiation that fluid sample interaction in beam and sample container generates, specific part scattering
To predetermined direction and enter in spatial volume box, so that its electromagnetic radiation sensitivity region for hitting electromagnetic radiation detector.It is general
Lead to it is clear for the skilled person that will permitted as to the response using the fluid sample in incidence electromagnetic radiation beam irradiating sample container
Multi-direction scattered electromagnetic radiation.Because of the detector arranged using space filtering, selection is unidirectional.Additionally or as one kind
Selection, can use single mode optical fiber.However, because constructing optical path between sample container and electromagnetic radiation sensitivity area, only
It needs to be arranged symmetrically the partial dispersion electromagnetic radiation beam to be detected selectively relative to incidence electromagnetic radiation beam.
According to exemplary embodiments, the accurate directive electromagnetism of the scattered electromagnetic radiation beam that electromagnetic radiation detector can be made to will test
Radiation detector, and it is unrelated with the refractive index value of material of fluid sample that is sample container and/or being contained within.This is
By adjusting the relative bearing between incidence electromagnetic radiation beam and sample container (in particular, by making electromagnetic radiation beam phase twice
Sample container is suitably tilted, vice versa) realize, specifically, the adjusting is able to carry out, so that in sample container
The upstream and downstream at (geometry or scattering) center realizes symmetrical beam geometry.Therefore, it can be realized to sample
The influence based on refractive index of the material of the material of container and/or in sample container sample compensates.Therefore, lead to
Only progress geometrical orientation adjusting is crossed, and does not therefore need any additional firmware or adjusts work, realizes analytical equipment and folding
It penetrates rate offset or changes unrelated.Therefore, user using the sample container of any requirement and any can want in analytical equipment
The sample (in the solvent that can decompose and/or be dispersed in any requirement) asked, without exclusively carrying out refraction before the use
Rate is adjusted.
Other exemplary embodiments of the device and method are described below.
In the preferred embodiment it is assumed that the elongation relative to its wall (especially the first wall and the second wall) and sample container
The vertical line of first wall of (or extension) parallel sample container of axis has fixed incidence angle, positions electromagnetic radiation detector,
To detect the scattered electromagnetic radiation beam by second wall parallel and opposed with incident wall, so that electromagnetic radiation detector be made to receive
The scattered-out beam direction arrived is identical as above-mentioned fixed incidence angle relative to the angle of the vertical line of the second opposed walls so that sample or
Any variation of the refractive index of sample container wall all will make refraction angle and the first wall and the second wall generate identical and opposite variation,
So that the detection direction of scattered electromagnetic radiation beam remains unchanged.
In a preferred embodiment, the intersection point and scattered electromagnetic radiation beam of incidence electromagnetic radiation beam and sample container and sample hold
The intersection point of device essentially forms isosceles triangle together with the region scattered, and scattering region is center angle.
In a preferred embodiment, sample container is tilted relative to the direction of incidence electromagnetic radiation beam, so that incoming electromagnetic spoke
Beam is before just traveling in sample container to the incident track of symmetry axis relative to the scattered electromagnetic radiation beam to be detected
The Scattering Trajectories of the position after sample container axially and symmetrically (or mirror image pair is just left from symmetry axis to scattered electromagnetic radiation
Claim) so that the Scattering Trajectories outside sample container are unrelated with sample container and sample refractive index.This is especially suitable for various shapes
The sample container of shape, for example, tubular or cubic shaped.It therefore, there is no need to the sample container rotational symmetry around axis.
In a preferred embodiment, relative to incidence electromagnetic radiation beam direction arrange sample container so that with include sample
On vertical the first visual direction (for example, with reference to Fig. 3) of the plane (that is, symmetry axis is located in the plane) of the symmetry axis of product container, phase
For the symmetry axis of sample container, be mutually substantially axisymmetrically arrange incidence electromagnetic radiation beam and scattered electromagnetic radiation beam (because
This, when watching from the first visual direction, the projection of the incidence electromagnetic radiation beam of symmetry axis upstream on this plane can be mapped to pair
Claim the projection of the scattered electromagnetic radiation beam in axis downstream on this plane)；And the second view in the symmetry axis along sample container
To on (for example, with reference to Fig. 4), axisymmetrically arrange incidence electromagnetic radiation beam and scattered electromagnetic radiation beam (therefore, when from the mutually
When two visual directions are watched, projection of the incidence electromagnetic radiation beam of symmetry axis upstream on the plane perpendicular to the symmetry axis of sample container
Projection of the scattered electromagnetic radiation beam in symmetry axis downstream on the plane perpendicular to the symmetry axis of sample container can be mapped to).
On the first visual direction, the symmetry axis of sample container can constitute the symmetry axis of axial symmetry map operation simultaneously, utilize the axial symmetry
The incidence electromagnetic radiation beam of map operation, symmetry axis upstream can be mapped to the scattered electromagnetic radiation beam in symmetry axis downstream.?
On two visual directions, can perpendicular to axial symmetry map operation symmetry axis and the symmetry axis of determining sample container can be intersected with it
Orientation, using the axial symmetry map operation, the incidence electromagnetic radiation beam of symmetry axis upstream can be mapped to symmetry axis downstream
Scattered electromagnetic radiation beam.By corresponding deflection or obliquely (and advantageously, pass through also relative to incidence electromagnetic radiation beam
The incident window of its sample container for entering sample container) be arranged in incidence electromagnetic radiation beam and sample container symmetry axis it
Between, it is unrelated with sample container and/or institute direction the refractive index of material of sample that detection may be implemented, because the result is that dissipating
It penetrates electromagnetic radiation beam (that is, electromagnetic radiation detector partial dispersion electromagnetic radiation to be detected) and sample is being left by its exit window
Substantially the same direction of directive and there is no space displacement always after product container, and with it is sample container and sample
Refractive index value is unrelated.
In a preferred embodiment, sample container is arranged, so that on the first visual direction (for example, with reference to Fig. 3), sample container
First inclination angle 90 °-a of the symmetry axis relative to the direction acute rake angle (that is, angle less than 90 °) of incidence electromagnetic radiation beam.?
In preferred embodiment, sample container is arranged, so that on the second visual direction (for example, with reference to Fig. 4), relative to incidence electromagnetic radiation
Scattered electromagnetic radiation beam is obliquely arranged at the second inclination angle (b+b) for the acute angle (that is, angle less than 90 °) that the direction of beam is formed
Direction.As a result, inclined twice in this way, it can be unrelated with sample and sample container refractive index, reproduction will detect
Scattered electromagnetic radiation beam.The exact value at two inclination angles depends on the geometry of analytical equipment.However, suitably select this two
When a inclination angle, it is no longer necessary to do hardware based compensation to the influence based on refractive index.Inclined twice in this way, sample container
Symmetrical plane normal direction relative to especially along incident beam axis and perpendicular to its two axis tilt so that realize refractive index
Compensation.First inclined shaft can be the incident direction of electromagnetic radiation beam, that is, Guangzhou.Second inclined shaft can be perpendicular to the incident beam side
To.
In embodiment, the first inclination angle (90 ° of-a) in the range of about 75 ° with about 89 °, especially in about 80 ° and about 87 °
In the range of.In embodiment, in the range of about 2 ° with about 30 °, second especially is selected in the range of about 6 ° with about 20 °
Inclination angle (b+b).When the value of adjustable inclination, a criterion is to need to avoid in the fully reflective electromagnetic radiation beam of sample container.It adjusts
Another criterion at section inclination angle is to maintain electromagnetic radiation beam sufficiently smallly by the body of its sample container including sample propagated
Product.As a result, the inclination angle of above-mentioned value is particularly suitable as the small of sample container for ELS analytical equipment or DLS analytical equipment
Cup.Typically for the common angle of scattering (with reference to " c " in Figure 13) (for example, 20 °) in the range of 10 ° with 40 °, as a result
It is, respectively appropriate selection " a " and " b ", to use between 1 ° and 15 °, particularly between the range between 3 ° and 10 °.
In embodiment, sample container is that especially have rectangular section, more particularly with the multi-panel of square-section
Shape, be also possible on the symmetrical plane perpendicular to symmetry axis with circular cross-section cylindrical shape, wherein polygon or
The circular center of gravity of person is located on symmetry axis.It, being capable of top of the reasonable definition corresponding to sample container for all these geometries
The symmetrical plane in face and bottom surface.The incident window of sample container can be the cross of (especially parallel) sample container with exit window
To the face in face.In addition to this, there is no geometry limitation for the shape of sample container.
In embodiment, at least the volume fractiion of sample container has perpendicular to the constant cross-section shape of symmetry axis and section
Product, arranges the volume fractiion, to penetrate electromagnetic radiation beam.It is, therefore, possible to provide very symmetrical arrangement.
In embodiment, from including forward scattered electromagnetic beam, backward scattered electromagnetic radiation beam and lateral scattering electromagnetism
Selection travels to the scattered electromagnetic radiation beam of electromagnetic radiation detector in the group of radiation beam.In a preferred embodiment, forward scattering
Electromagnetic radiation beam for analyzing because its with sufficiently high intensity and carrying indicate the sample to be analyzed property it is intentional
Adopted information.However, can also be measured in back scattering geometry (for example, please referring to Fig. 8) as a kind of selection,
So that scattered electromagnetic radiation beam (then, constituting the measurement beam for wanting directive electromagnetic radiation detector) travels to sample container upstream
Direction, that is, opposite with forward scattered electromagnetic beam.Furthermore, it is possible to lateral scattering (for example, with reference to Fig. 7).In addition, for this
A little situations, can reproduction detection unrelated with sample container and specimen material refractive index.
In embodiment, which includes mounting platform, constructs the mounting platform, to install sample container, wherein constructing
Mounting platform and sample container, so that the orientation of symmetry axis is parallel to gravity when sample container to be mounted on mounting platform.
The advantages of embodiment, is that sample container is mounted on not inclined plane earth, and with incidence electromagnetic radiation beam in sample
Inclined direction on container realizes the inclined twice of requirement.Therefore, even if when injecting fluid sample in sample container, still
It can prevent the fluid sample and be flowed out from sample container because of being tilted relative to g vector.
In embodiment, which includes beam splitter, constructs the beam splitter, the electromagnetic radiation that electromagnetic radiation source is generated
It is split into forming the first part of incidence electromagnetic radiation beam and forms the second part of reference beam, wherein the equipment is constructed, so that
Reference beam directive electromagnetic radiation detector without interacting with sample, and constructs the equipment, so that scattered electromagnetic radiation beam
Interference is generated in the upstream of electromagnetic radiation detector with reference beam.In particular, for this analysis method based on interference, it can
With the geometry of very high position precision prediction scattered electromagnetic radiation beam, so that reference beam and scattered electromagnetic radiation beam are certain
It can be realized and interfere with each other, it is extremely important.This is can be obtained to indicate the liquid to be analyzed according to the interference of reference beam and scattered-out beam
The basis of the information of the property of body sample.
In embodiment, which is not used to compensate the different rails for the scattered electromagnetic radiation beam for being located at sample container downstream
Any compensating optical element and any regulating mechanism of mark, the different tracks are the different foldings by sample container and/or sample
It penetrates caused by rate.Therefore, the equipment can be manufactured with miniature manner, and the equipment can work in a user-friendly manner.
In embodiment, which is configured to include one in following group: surge light scatters (ELS) equipment, uses
The boundary of particle in the surge mobility and sample of measurement sample reaches at least one of potential；And dynamic light scattering
(DLS) equipment, for measuring the size of the particle in sample.In particular, in these measuring systems based on interference, reference beam
Space precise overlay between scattered electromagnetic radiation beam is most important.
In embodiment, which includes source beam controlling element, which is arranged in electromagnetism spoke
Penetrate between source and sample container, for regulating and controlling the electromagnetic radiation beam of sample container upstream, thus make incidence electromagnetic radiation beam to
Sample container.The source beam controlling element can be lens, for incidence electromagnetic radiation beam to be focused on sample container.It can be with
The orientation of the lens is determined, so that incidence electromagnetic radiation beam is propagated from the center of lens by lens, to make incoming electromagnetic spoke
Beam is downward or is bent upwards.It is then possible to above-mentioned oblique structure be realized, without the sample container phase for making to be filled with liquid
For ground inclination.
In embodiment, which includes detector lateral bundle controlling element, which is arranged in sample
Between product container and electromagnetic radiation detector, for regulating and controlling the electromagnetic radiation beam in sample container downstream, to make to scatter electromagnetism spoke
Beam directive electromagnetic radiation detector.The detector lateral bundle controlling element can be lens, for keeping scattered electromagnetic radiation beam poly-
Coke arrives detector.
In embodiment, which includes back scattering detector, constructs the back scattering detector, to detect by sample
The electromagnetic radiation of container back scattering.It especially can be with relative to 120 ° to 180 ° of incident beam, preferably with about 170 °
Angle detects the radiation.
In embodiment, electromagnetic radiation source is constructed, to generate incident beam.It is therefore possible to use (example in visual range
Such as, the electromagnetic radiation of 400nm to 800nm).However, as a kind of selection, it also can be such as infrared in other wave-length coverages
Or it is ultraviolet, it measures.
In embodiment, electromagnetic radiation source is constructed, to generate incident coherent electromagnetic radiation beam.The coherent electromagnetic radiation beam exists
Based on phase relation is determined within the scope of large space, to keep the electromagnetic radiation beam and another electromagnetic radiation beam relevant.Laser is
The appropriate selection of corresponding electromagnetic radiation source.
In embodiment, electromagnetic radiation detector is configured to photoelectric detector.This is a very simple detector,
The significant letter of the property about the sample to be analyzed can be obtained from the relevant result of scattered electromagnetic radiation beam and reference beam
Breath.
In embodiment, sample container is configured to cuvette.According to exemplary embodiments, it might even be possible to using lower quality
Cuvette, without losing high spatial angle.For example, the height (along the direction of symmetry axis) of the cuvette as sample container can be with
Between 1cm and 5cm, 3cm especially can be.Length, width or the diameter of the sample container are (perpendicular to right
Claim the direction of axis) it can especially can be 0.5cm in the range of 0.2cm and 1cm.
In embodiment, sample container has sample receiving volume, constructs the sample receiving volume, to accommodate the sample of analysis
Product, and by the top surface in sample container, the sample receiving volume can be entered.Therefore, sample container has at top and opens
Mouthful, and therefore there is cup-shaped geometry.Then, for example, can use suction pipe, sample is injected a sample into from upper position and is held
In device.
According to the example of embodiment described here, aforementioned aspect of the present invention and other aspects are it is clear that and join
These examples for examining embodiment describe aforementioned aspect of the present invention and other aspects.
The present invention is described in more detail below with reference to the example of embodiment, the invention is not limited to the examples of embodiment.
Detailed description of the invention
It is inclined relative to the incidence electromagnetic radiation beam for compensation of refractive index that Fig. 1 shows exemplary embodiments according to the present invention
For analyze include sample in sample container equipment side view.
Fig. 2 shows the top views of equipment shown in Fig. 1.
Fig. 3 shows the side view of the beam geometry shape for the electromagnetic radiation beam propagated by equipment shown in Fig. 1 and Fig. 2.
Fig. 4 shows the top view of the beam geometry shape for the electromagnetic radiation beam propagated by equipment shown in Fig. 1 and Fig. 2.
Fig. 5 shows the electromagnetism that exemplary embodiments according to the present invention are used for cube sample container and forward scattering operating mode
Radiation beam geometry.
Fig. 6 shows the electromagnetism that exemplary embodiments according to the present invention are used for cylindrical sample container and forward scattering operating mode
Radiation beam geometry.
Fig. 7 shows the electromagnetism that exemplary embodiments according to the present invention are used for cube sample container and lateral scattering operating mode
Radiation beam geometry.
Fig. 8 shows the electromagnetism that exemplary embodiments according to the present invention are used for cube sample container and backscattering operating mode
Radiation beam geometry.
Fig. 9 to Figure 13 shows the electromagnetic radiation beam and sample that exemplary embodiments according to the present invention are used to analyze the equipment of sample
The different views of relative bearing between container.
Specific embodiment
View in attached drawing is schematic diagram.In different figures, benefit is denoted by the same reference numerals similar or like
Unit.
Before exemplary embodiments of the invention are described with reference to the drawings, this hair that exemplary embodiments are based on is developed into description
Bright some basic considerations.
In the light scattering tool with the detection system based on single mode optical fiber (for example, surge light scattering ELS or dynamic optical
Scatter DLS) in, the electromagnetic radiation being only from one very small space angular region is connected to optical fiber.Therefore, only along very special
This part light for determining direction propagation is transmitted to detector from optical fiber.This characteristic of optical fiber is usually required, because of drop significant in this way
The interference effect of the reflection of low environment light and optical fiber part.In the case where correction adjusts the equipment, only selectively examine
It surveys from the scattering light for wanting cube.
However, carrying out analysis to the sample of different refractivity value is a kind of challenge according to above-mentioned boundary condition.According to sample
Refractive index, incident and outgoing light wave reflects in different ways.Therefore, it is necessary to the sample tune respectively to each refractive index value
Save the equipment.On the contrary, scattered photon is now as refraction angle changes without reaching detector, because these photons are no longer able to join
Enter optical fiber.Therefore, with the increase of variations in refractive index, measuring signal may lose.However, in practice requiring that the analytical equipment energy
Enough measurements have the sample of different refractivity value.
Using the different sample containers of window wall being made from a different material and/or with different thickness (such as not
Same cuvette) when, spatial excursions occur for Shu Keneng, and the measuring signal on detector is also caused to be lost in this way.
Traditionally, compensating plate can be inserted into Shu Tonglu, the compensating plate can be selected according to the refractive index of sample (especially
It is to be related to plate thickness).For example, this motor driving that can use the different compensating plates with many different-thickness changes wheel in fact
Existing, it is heavy that motor driving changes wheel.
As described above, traditionally, being used to solve above-mentioned optics problem for the additional optical fiber part of such as compensating plate, and should
Additional optical fiber part has the thickness of the refractive index based on sample.This can use the horse of the compensating plate with many different-thickness
Change wheel up to driving to realize.
The defect that above-mentioned conventional method has is to need additional optical to compensate the optical distortion based on refractive index.
In addition, larger drift may occur for effective scattering volume on Shu Fangxiang, for example, 1mm or bigger.Compensating plate is used also to make
It compensates in a step-wise manner, causes precision inadequate.This equipment is manufactured including motor, electronic component and space and with miniature manner
Trend is disagreed.
In order to overcome at least part defect in these defects, exemplary embodiments of the invention provide a kind of pair of electromagnetism
The equipment of radiating scattering instrument progress compensation of refractive index.For this purpose, specific bundle sample container orientation geometry can be used.Pass through
The measurement is carried out, can be realized the autobalance of doubling firing angle variation (particularly because sample of different refractivity).It is advantageous
It is that this can be real in the case where not needing an example an example and carrying out optics adjusting respectively or use independent optical compensation unit
It is existing.
In embodiment, using the sample container by using the fluid sample with variable refractive index value, automotive resistance
The space displacement of electromagnetic radiation beam or the specific bundle geometry of drift.When the refraction of sample container and/or fluid sample
When rate value changes, does not need user and adjust the equipment.Also the variable optical component of such as compensating plate need not be used.Relative to
The electromagnetic radiation beam that sample container (especially its center) is arranged symmetrically incidence electromagnetic radiation beam and scatters from sample container.Electricity
Refractive index when refractive index and scattered electromagnetic radiation beam when magnetic radiation beam travels in sample container come out from sample container is mutual
It balances each other.
According to exemplary embodiments, this can be by making sample container (more precisely, the geometirc symmetry axis of sample container)
It is realized relative to the specific inclined twice of electromagnetic radiation beam.With the incident window of incidence electromagnetic radiation beam vertical transmission to sample container
In compare, be able to carry out for the first time tilt, make incidence electromagnetic radiation beam relative to incident window normal vector towards sample hold
The symmetry axis of device rotates first jiao (" a ").In addition, with the incident window of incidence electromagnetic radiation beam vertical transmission to sample container
It compares, is able to carry out second of inclination, make incidence electromagnetic radiation beam relative to the normal vector of incident window perpendicular to sample
Second jiao (" b ") is rotated in the plane of the symmetry axis of container.
Make the electromagnetism on direction on its direction towards the center of sample container and that it leaves sample container in this way
The propagation path of radiation is symmetrical.Therefore, the optical effect to its center two sides based on refractive index compensates mutually.In other words,
In order to realize full symmetric image (in particular, incidence angle and the angle of emergence can be in the source portion of propagation path and detector side
It is identical), sample container inclination can be made twice.
The advantages of embodiment, is that any sample for requiring refractive index value can be measured.In addition, the embodiment only results in
The scattering volume for being parallel to the incident window of sample container generates very small space displacement and (is less than 0.1mm, and in certain feelings
Under condition, significantly less than 0.1mm).On Shu Fangxiang, effective scattering volume is accurately retained between incident window and exit window
Center.In addition, the case where with the independent optical fiber part of conventionally used such as compensating plate is identical, each refractive index can be realized
Accurate and continuous or stepless compensation, rather than only grading compensation.Furthermore it is possible to the embodiment is implemented with miniature manner,
Because the individual component (motor changes wheel, compensating plate) that traditionally refractive index compensation requires is not required, and need not be spent
Time-consuming adjusting optical path.
Fig. 1 shows fluid sample that exemplary embodiments according to the present invention are used to analyze include in sample container 5 to carry out
The equipment 20 (can be realized by the surge light scattering ELS equipment of the boundary for measuring sample particle up to potential) of compensation of refractive index,
The sample container 5 surrounds two tilt axis relative to electromagnetic radiation beam 2.Fig. 2 shows the top views of equipment 20 shown in Fig. 1.It is right
It is measured in DLS (dynamic light scattering), it is convenient to omit (however, as a kind of selection, reference beam 9 can be used for DLS to reference beam 9
Measurement).
Electromagnetic radiation source 1 generates electromagnetic radiation in a manner of collimation laser, here, electromagnetic radiation source 1 is configured to laser
Source.Electromagnetic radiation beam is split into two parts by beam splitter 3.
Source beam controlling element 4 by being configured to lens guides its first part, and the source beam controlling element 4 is by first
Part focuses on the center for constituting the sample container 5 of sample box as incidence electromagnetic radiation beam 2.In addition, the lens make first
Divide downwards (laser beam is not beaten in the center of lens).The first part adjusted for generating electromagnetic radiation beam, which enters, to be had
The sample container 5 (Fig. 2 diagram is shown) of transparent window and electrode, the electrode is in the fluid sample being contained in sample container 5
Generate electric field.Then, the more detailed description done as follows, the fluid sample in sample container 5 dissipate incidence electromagnetic radiation beam 2
It penetrates.Fluid sample in sample container 5 makes all directions scattering of the light in space.The electromagnetic radiation of scattering is from sample container 5
It projects.It will be indicated as the scattered electromagnetic radiation beam 6 to be detected (being detected because to send it to electromagnetic radiation detector 12)
A part of scattered electromagnetic radiation be directed to detector side controlling element 7, here, the detector side controlling element 7 is by another
Lens are realized.Here, will test device lateral bundle controlling element 7 is configured to the condenser lens that focus is located at the center of sample container 5, and
And the scattered electromagnetic radiation beam 6 that will detect of the detector lateral bundle controlling element 7 is redirected to the optical flat of interferometer, below
It will be described in more detail.
After interacting with detector lateral bundle controlling element 7, scattered electromagnetic radiation beam 6 is reflected by reflector 8, so that dissipating
Penetrate 6 directive electromagnetic radiation detector 12 of electromagnetic radiation beam.However, the optical fiber for being arranged in the entrance of electromagnetic radiation detector 12 is only adopted
Collection scatters to the light of a special angle, and the light is sent to electromagnetic radiation detector 12.Dotted line in Fig. 1 and Fig. 2 projects
The specific optical path, and the specific optical path seeks to the scattered electromagnetic radiation beam 6 of detection.Fluid sample in sample container 5
Scattering particles when moving in one direction together, Doppler effect makes the frequency drift of scattered electromagnetic radiation beam 6.The movement
Be as in sample container 5 electrode generate electric field caused by, and to the boundary of particle surface up to potential it is directly proportional.
Beam splitter 3 divides and non-directive sample container 5 is (and therefore, not along its entire propagation path and liquid
The interaction of body sample) second part electromagnetic radiation beam can be the reference beam 9 separated from remaining former laser beam.Reflector
10 reflected fudicial beams 9.Can use optical modulator (not shown) makes the frequency shift (FS) of reference beam 9.
Beam combination device 11 is combined reference beam 9 with the scattered electromagnetic radiation beam 6 to be detected with interference mode, so that electromagnetism spoke
It penetrates detector 12 and is able to detect the beam obtained by reference beam 9 and the interference of scattered electromagnetic radiation beam 6.Electromagnetic radiation detector 12 is examined
The detection signal measured is sent to analysis processor (not shown), and then, utilizes technology well known to those of ordinary skill, analysis
Processor determines that (such as boundary reaches potential, electromobility, media particle at least one property of the fluid sample in sample container 5
Size etc.).
As described above, electromagnetic radiation detector 12 is configured to optic fibre detector, which only acquires and detects
Light from a specific direction, because only that the light is connected to single mode optical fiber.Detection signal be exactly scattered electromagnetic radiation beam 6 with
The result that reference beam 9 is interfered.As a result the frequency of beat is the difference of the two frequencies.Analysis processor is determined for difference frequency
(that is, phase change rate) and the boundary for calculating the particle being contained in the fluid sample in sample container 5 reach potential, can this point
Analysis processor is configured to digital signal processing unit.
Ref. No. 22 indicates to propagate the part not scattered by entire sample container 5 in electromagnetic radiation.With reference to
The expression of number 13 does not reach the reference beam 9 and/or scattered electromagnetic radiation of electromagnetic radiation detector 12 for absorbing or subsideing
The absorber (or ligh trap) of the electromagnetic radiation of beam 6.The laser of incident window of the expression of Ref. No. 14 from sample container 5
The back of beam is anti-.From sample when Ref. No. 16 is indicated for absorbing or being trapped in 2 irradiating sample container 5 of incidence electromagnetic radiation beam
Another light absorber (or ligh trap) of the electromagnetic radiation of the incident window reflection of product container 5.The expression of Ref. No. 24, visually
Pair of the symmetry of the incidence electromagnetic radiation beam 2 and scattered electromagnetic radiation beam 6 on path between enhanced beam controlling element 4,7
Claim plane.
DLS measurement (but reference beam 9 can also be used for DLS measurement) for no reference beam 9, detects and divides
Analyse the scattered electromagnetic radiation beam 6 projected from sample box or sample container 5.
According to the embodiment of the present invention, the following special characteristic of optical layout is explicitly pointed out:
I) source beam controlling element 4 (being configured to lens herein) makes electromagnetic radiation beam through the sample in sample container 5, no
On optical flat in interferometer, but it is bent downwardly.Refer to the back at the incident window of sample container 5 instead (
Ref. No. 14) directive require destination.
Ii) with the symmetrical arrangement scattered electromagnetic radiation beam 6 and incidence electromagnetic radiation beam 2 relative to sample container 5.This
It is meant that the incidence electromagnetic radiation beam 2 of the incident window in sample container 5 and the scattered electromagnetic radiation 6 in exit window
Refraction it is full symmetric.This argument is for the sample of all possible refractive index and for the sample of all box wall materials and box wall thickness
Product container 5 (its incident window and exit window are designed identical) is all effectively.
It is shaped to accommodate the sample container 5 of the sample to be analyzed, with symmetry axis 25, to arrange the sample container 5, to receive
Incidence electromagnetic radiation beam 2 (passes through incident window), to travel in sample container 5, interacts with sample, and arranging should
Sample container 5, so that scattered electromagnetic radiation beam 6 travels to except sample container 5 and (passes through exit window).
Advantageously, the direction relative to incidence electromagnetic radiation beam 2 determines the orientation of sample container 5, so that incoming electromagnetic
Radiation beam 2 at least along from the position just before traveling to sample container 5 to the path of symmetry axis 25 incident track with
Path of the scattered electromagnetic radiation beam 6 at least along the position for just leaving sample container 5 from symmetry axis 25 to scattered electromagnetic radiation 6
Scattering Trajectories it is symmetrical.It is symmetrical that these can be designed according only to the proper orientation between sample container 5 and incidence electromagnetic radiation beam 2
Path, so that the Scattering Trajectories (that is, the radiation to be detected) come out from sample container 5 and sample container 5 and sample refraction
Rate is unrelated.In other words, even if using different samples and different sample containers 5 in equipment 20, scattered electromagnetic radiation
The side that interesting part (that is, that electromagnetic radiation detector 12 is spatially aligned and therefore the only part sensitive to its) is propagated
To still constant always, and it is unrelated with the refractive index of sample container 5 and sample.
More specifically, in order to realize above-mentioned symmetry and therefore realize refraction with sample and/or sample container 5
Rate is unrelated, and sample container 5 is arranged in the direction of propagation relative to incidence electromagnetic radiation beam 2, so that:
First vertical with including plane (that is, the paper of Fig. 1) of symmetry axis 25 of sample container 5 shown in Fig. 1
On visual direction 30, relative to the symmetry axis 25 (this also forms the symmetry axis of axial symmetry operation) of sample container 5, axisymmetrically cloth mutually
The scattered electromagnetic radiation setting incidence electromagnetic radiation beam 2 (more precisely its projection on the first visual direction 30) and being detected
Beam 6 (more precisely its projection on the first visual direction 30)；And
The second visual direction 40 that symmetry axis 25 (perpendicular to the paper of Fig. 2) along sample container shown in Fig. 2 extends
On, incidence electromagnetic radiation beam 2 (more precisely its projection on the second visual direction 40) is axisymmetrically arranged mutually and to be examined
The scattered electromagnetic radiation beam 6 (more precisely its projection on the second visual direction 40) of survey.
It will be with reference to Fig. 3 and Fig. 4 more detailed description only by obtaining incidence electromagnetic radiation beam 2 relative to the inclination of sample container 5
Obtain these symmetric cases.Equipment 20 includes the mounting platform 18 for installing sample container 5, wherein construction mounting platform 18 and sample
Product container 5, so that the orientation of symmetry axis 25 is parallel to gravity g when sample container 5 to be mounted on mounting platform 18.Therefore,
Without accommodate fluid sample sample container 5 orientation relative to gravity and therefore relative to ground inclination, and by not
Sample container 5 is tilted, and tilts incidence electromagnetic radiation beam 2, can be realized the well azimuth of requirement.
Advantageously, equipment 20 is not for compensating the difference of the scattered electromagnetic radiation beam 6 positioned at the downstream of sample container 5
Any compensating optical element and any regulating mechanism of track, the different tracks are usually by sample container 5 and/or sample
Caused by different refractivity.
Fig. 3 shows the side view of the beam geometry shape of the electromagnetic radiation beam by propagating according to the equipment 20 of Fig. 1 and Fig. 2.
Fig. 4 shows the top view of the beam geometry shape for the electromagnetic radiation beam propagated by equipment 20 shown in Fig. 1 and Fig. 2.
From figure 3, it can be seen that arrangement sample container 5, so that symmetry axis 25 is relative to incoming electromagnetic on the first visual direction 30
90 ° of the first inclination angle-a of the direction acute rake angle of radiation beam 2.First 90 ° of inclination angle-a can be in the range of 80 ° to 87 °.
From fig. 4, it can be seen that arrangement sample container 5, so that on the second visual direction 40, relative to incidence electromagnetic radiation beam 2
Direction acute rake angle the second inclination angle b+b arrange the direction of propagation of scattered electromagnetic radiation beam 6.In the range of 6 ° with 20 °
Select the second inclination angle b+b.
It is above-mentioned to make incidence electromagnetic radiation beam 2 twice relative to the inclination of sample container 5 there are two advantageous effects: on the one hand, this
Sample prevents the undesirable position of part directive of incidence electromagnetic radiation beam 2 reflected at the incident window of sample container 5.Even
Importantly, the mutually symmetrical with structure (while on two visual directions 30 and 40) of incident track and Scattering Trajectories is achieved,
The mutually symmetrical with structure, which is constituted, does not require the sample because leading to the sample container of variations in refractive index and/or being accommodated within
Change and readjust the basis of the remarkable advantage of the optical path in 5 downstream of sample container.Along visual direction 30, sample container 5 it is symmetrical
Axis 25 constitutes incidence electromagnetic radiation beam 2 according to its symmetry axis of the symmetrical mapping to scattered electromagnetic radiation beam 6 in the axial direction simultaneously.Edge
Visual direction 40, another symmetry axis 26 for intersecting with the symmetry axis 25 of sample container 5 constitute incidence electromagnetic radiation beam 2 according to it
It is symmetrically mapped the symmetry axis of scattered electromagnetic radiation beam 6 in the axial direction.
Construction shown in Fig. 3 is returned to, arranges vertically rather than obliquely sample container 5.In order to realize above-mentioned inclination arrangement,
It is not straightened laser in level, but generates the electromagnetic radiation beam relative to transverse axis.It is identical as conventional method, refractive index
Variation leads to beam displacement.For different refractive index values (n=1.3, n=1.6), this is shown in Figure 3.In the described embodiment,
It is not detected on laser plane, and is symmetrically examined (in the mapping of chain-dotted line/symmetry axis 26 or mirror image) with incident laser
It surveys.Detection scattering light in an upward direction.Therefore, incidence electromagnetic radiation beam 2 and the scattered electromagnetic radiation beam 6 to be detected are in sample
Refraction situation at two windows of container 5 is identical.For different refractive index values, the angle inspection to be slightly displaced in the sample
It surveys scattered-out beam (the case where different refractivity value (n=1.3, n=1.6) is shown in Fig. 3).However, in the outside of sample container 5,
Two scattered electromagnetic radiation beams 6 good alignment again (this is symmetrical result).Uniquely become as caused by the refractive index changed
Change is the slightly displacement because of effective scattering volume.Effective scattering volume is defined as incidence electromagnetic radiation beam 2 and scattering electromagnetism
The overlapping volume (in Fig. 3, intersection point) between two lines of the different value of n of radiation beam 6.All possibility intersection points are all placed exactly in
The middle part of sample container 5, and it (is two refractive index values at 7o in the angle of incidence electromagnetic radiation beam 2 that vertical displacement is very small
Displacement between (n=1.3, n=1.6) is less than 0.1mm).
Fig. 4 is returned, the horizontal alignment of incident window is not orthogonal to the direction of propagation of incidence electromagnetic radiation beam 2.In addition,
On second visual direction 40 shown in Fig. 4, the arrangement of incidence electromagnetic radiation beam 2 and the scattered electromagnetic radiation beam 6 to be detected is relative to sample
Product container 5 is symmetrical.Therefore, for each refractive index of fluid sample, effective scattering volume is all located just at sample container 5
Center or middle part between incident window and exit window.The very a little displacement of incident window generation is only parallel to (to be less than
0.1mm)。
Fig. 5 shows the electricity that exemplary embodiments according to the present invention are used for cube sample container 5 and forward scattering operating mode
Magnetic radiation beam geometry shape.Fig. 6 shows exemplary embodiments according to the present invention and works for cylindrical sample container 5 and forward scattering
The electromagnetic radiation beam geometry of mode.Fig. 7 show according to the present invention exemplary embodiments for cube sample container 5 and lateral
Scatter the electromagnetic radiation beam geometry of operating mode.Fig. 8 shows exemplary embodiments according to the present invention to be held for cube sample
The electromagnetic radiation beam geometry of device 5 and backscattering operating mode.Fig. 5 to Fig. 8 is clearly shown above with reference to Fig. 1 to Fig. 4
The principle of description can be applied to the sample container 5 and/or different scattering detection bodies of different geometries by necessary modification
Architecture (i.e., it is possible to detection is measured in transmission, backscattering or lateral scattering).
Fig. 9 to Figure 13 show exemplary embodiments according to the present invention be used to analyze sample equipment 20 electromagnetic radiation beam with
The different views of relative bearing between sample container 5.
It should be noted that term " includes " is not excluded for other units or step, and the article " one " is not excluded for majority.This
Outside, it can be combined in conjunction with the unit that different embodiments describe.
It shall also be noted that the reference symbol in claims should not be regarded as to the limit to the scope of the claims
System.
Implementation of the invention is not limited to shown in the drawings and preferred embodiments described above.On the contrary, even for
Different embodiment, solution and principle according to the present invention shown in utilization, can there is various modifications.
Claims (15)
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| US5572321A (en) * | 1993-11-24 | 1996-11-05 | Institut Francais Du Petrole | Detector for measuring the luminous intensity scattered by thin films of colloidal media |
| JP3258889B2 (en) * | 1996-01-11 | 2002-02-18 | 株式会社堀場製作所 | Optical axis adjustment method in scattering particle size distribution analyzer |
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