CN109580439A - A kind of Ultrafast spectrum experimental method of microparticle - Google Patents
A kind of Ultrafast spectrum experimental method of microparticle Download PDFInfo
- Publication number
- CN109580439A CN109580439A CN201811220629.1A CN201811220629A CN109580439A CN 109580439 A CN109580439 A CN 109580439A CN 201811220629 A CN201811220629 A CN 201811220629A CN 109580439 A CN109580439 A CN 109580439A
- Authority
- CN
- China
- Prior art keywords
- sample
- laser
- lens
- microparticle
- cavity
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000011859 microparticle Substances 0.000 title claims abstract description 52
- 238000001228 spectrum Methods 0.000 title claims abstract description 30
- 238000002474 experimental method Methods 0.000 title claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 80
- 238000006073 displacement reaction Methods 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 23
- 230000003287 optical effect Effects 0.000 claims abstract description 19
- 238000001514 detection method Methods 0.000 claims abstract description 8
- 238000011160 research Methods 0.000 claims abstract description 5
- 238000005086 pumping Methods 0.000 claims description 24
- 239000012530 fluid Substances 0.000 claims description 15
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 8
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 8
- 210000001367 artery Anatomy 0.000 claims description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims description 4
- 238000004080 punching Methods 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 210000003462 vein Anatomy 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 230000000737 periodic effect Effects 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 2
- 238000004611 spectroscopical analysis Methods 0.000 abstract description 2
- 238000010586 diagram Methods 0.000 description 16
- 239000007788 liquid Substances 0.000 description 6
- 239000007850 fluorescent dye Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000001917 fluorescence detection Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 230000000886 photobiology Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000013519 translation Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/06—Investigating concentration of particle suspensions
-
- G01N15/075—
Abstract
The present invention relates to material engineering fields, a kind of Ultrafast spectrum experimental method of microparticle, the Ultrafast spectrum research device of microparticle includes displacement platform I, rotation motor, rotary shaft, magnet, displacement platform II, sample cavity, stirring sheet, lens I, beam splitter, laser, optical filter, lens II, aperture, lens III, detector and computer, the microparticle sample of low concentration is studied using Ultrafast spectrum method, using the sample cavity and stirring means of special designing, so that the sample of different zones has faster exchange velocity to meet the needs of Ultrafast spectrum experiment in sample cavity, and it can be avoided mechanical noise and enter spectrum, also avoid the periodic refraction of laser in the sample, improve the quality of spectroscopic data, high-precision counting is carried out to the microparticle in the sample cavity of rotation using fluorescent detection method, no sample Loss, operating process are easy.
Description
Technical field
The present invention relates to material engineering field, especially a kind of microparticle that low concentration is studied using Ultrafast spectrum method
A kind of Ultrafast spectrum experimental method of microparticle of sample.
Background technique
Ultrafast spectrum be it is a kind of using ultrafast laser come the method for study sample characteristic, can obtain with femtosecond resolution ratio
Time-resolved spectrum, the laser for needing to focus commonly used in the ultrafast process in research photochemistry or photobiology, in experiment
It is mapped to the partial region in sample, the laser repetition rate of the laser system of the prior art can reach kHz magnitude, this just needs sample
There is sufficiently fast exchange velocity between the part of laser excitation and unawakened part in product, to avoid sample by laser
Repeat excitation and experimental result impacted, certain prior arts using the method for circulating pump come so that part in sample into
Row exchange, the sample size not only needed is larger, and can introduce mechanical noise, or even will cause specimen breakdown；Other are existing
Technology carries out the sample exchange of different zones using the blender at the uniform velocity rotated, but in the sample cavity of certain small volumes
It is smaller to stir range, i.e., can only be stirred mixing to the sample around stirring sheet, and sample can be made to generate laser
Periodically refraction, causes to introduce periodic noise in Ultrafast spectrum, have an impact to the result of Ultrafast spectrum.Certain
It in, needs to count the numbers of particles in liquid, count measurement in the prior art takes a long time, and can only be to list
The biggish sample of amounts of particles in the volume of liquid of position measures, and a kind of Ultrafast spectrum experimental method of microparticle can
It solves the problems, such as.
Summary of the invention
To solve the above-mentioned problems, the method for the present invention uses the sample cavity and stirring means of special designing, so that sample cavity
The sample of middle different zones has faster exchange velocity to meet the needs of Ultrafast spectrum experiment, in addition, using fluorescence detection side
Method carries out high-precision counting, no sample loss, operating process simplicity to the microparticle in the sample cavity of rotation.
The technical scheme adopted by the invention is that:
The Ultrafast spectrum research device of microparticle includes displacement platform I, rotation motor, rotary shaft, magnet, displacement platform II, sample
Product chamber, stirring sheet, lens I, beam splitter, laser, optical filter, lens II, aperture, lens III, detector and computer, xyZ
For three-dimensional coordinate system, rotation motor is fixed on displacement platform I, and the laser, beam splitter, lens I and sample cavity are successively
Form input path, the sample cavity, lens I, beam splitter, optical filter, lens II, aperture, lens III and detector successively group
At emitting light path, laser can the adjustable continuous laser of launch wavelength and laser pulse, laser pulse include pumping pulse and
Direct impulse, the pumping pulse and direct impulse have different power, frequency and duration, direct impulse and pumping arteries and veins
Time interval between punching can be adjusted；Magnet is parallel to z coordinate axis by rotation axis connection rotation motor, rotary shaft, is displaced
Platform I can be three-dimensional mobile, and rotation motor is able to drive magnet rotation, and sample cavity is fixed on displacement platform II, and displacement platform II can
Three-dimensional is mobile, and displacement platform II is able to drive sample cavity and rotates around the y direction center line of sample cavity, and sample cavity top half is rectangular
Body cavity, lower half portion are the cylinder barrel of axis in the y-direction, have aperture plate, the length between the top half and lower half portion
Cube chamber is 30 millimeters a height of, 10 millimeters a length of, width is 2 millimeters, and the cylinder barrel is 20 millimeters a height of, basal diameter is 10 millimeters,
The y direction center line of the rectangular body cavity and the axis collinear of the cylinder barrel, stirring sheet is by having outside magnetic stainless steel
Package polytetrafluoroethylene (PTFE) is made, and the diameter of stirring sheet is 1.2 millimeters, length is 13 millimeters, and stirring sheet is located at the sample cavity upper half
Point, the aperture plate can prevent stirring sheet from falling into cylinder barrel；The rotation motor, laser and detector distinguish cable connection meter
Calculation machine can adjust the time difference between the laser pulse of laser sending and rotation motor rotation angle by computer；It is small
The size in hole can be adjusted, and the detection resolution of detector can be adjusted according to various sizes of microparticle to be measured.
Stirring sheet makes the principle of the sample part progress fast exchange of the different zones in sample cavity are as follows:
Adjusting displacement platform II makes the width direction of the rectangular body cavity of the top half of sample cavity parallel with z-axis, adjusts position
Moving stage I makes the axis extended line of rotary shaft be located at the center of rectangular body cavity, opens rotation motor and makes magnet around rotary shaft
Axis at the uniform velocity rotates, and revolving speed representative value is 0.5 revolutions per second, and due to the magnetic torque effect by magnet, stirring sheet will be revolved with magnet
Turn, stirring sheet is rotated up both ends and contacts and be limited with the inner wall of rectangular body cavity, and magnet continues to rotate at this time, stirring sheet still by
Magnetic torque to magnet acts on, but stirring sheet position is constant, when magnet is rotated to a certain angle, magnetic of the stirring sheet by magnet
Torque is reversed, and stirring sheet can quickly be overturn to the opposite direction that magnet rotates at this time, and stirring sheet is overturn until both ends and rectangular body cavity
Inner wall contact and be limited, in conclusion stirring sheet is rotated twice during magnet at the uniform velocity rotates a circle, once
It is stirring sheet as magnet direction of rotation rotates at a slow speed, is that the opposite direction that stirring sheet is rotated to magnet is quickly overturn again, stirs
The quick switching process for mixing piece makes the sample of stirring sheet near zone and the sample fast exchange of sample cavity other parts.Technology
Advantage is: stirring sheet will not introduce noise with the rotary course at a slow speed of magnet direction of rotation, by adjusting laser pulse and stirring
The time interval for mixing the quick switching process of opposite direction that piece is rotated to magnet, can be effectively prevented from mechanical noise in sample into
Enter spectrum, also avoids the periodic refraction of laser in the sample.
The principle of count measurement is carried out to the microparticle in fluid sample are as follows:
Fluid sample containing microparticle to be measured is placed in sample cavity, according to the type of microparticle to be measured, to fluid sample
Middle addition fluorescent dye enables the microparticle surfaces under the laser irradiation of specific wavelength to launch fluorescence, laser hair
The laser irradiation sample penetrated makes microparticle launch fluorescence, and the fluorescence is recorded by emitting light path by detector；Laser
The laser of transmitting is focused in the cylinder barrel of sample cavity lower half portion after the deviation of beam splitter by lens I, displacement platform II band
Dynamic sample cavity is rotated around the y direction center line of sample cavity, and the microparticle to suspend in fluid sample is moved together with solvent, and is passed through
The focus of sample endovenous laser is to launch fluorescence；In the non-rotary situation of sample cavity, wherein the part being irradiated with a laser
This partial volume that the fluorescence that microparticle in volume is launched can be detected by detector, is defined as detectable volume, estimates
The method for calculating detectable volume is as follows: the fluorescence reference for the fluorescence that will launch is fixed in sample cavity, and is made
Detector can identify that laser beam is along negative z direction incidence sample cavity, when sample cavity is fixed, detector record
The intensity of fluorescence signal is(formula one), wherein w0It is sharp
Beam waist diameter of the light beam in the direction x, z0For the beam waist diameter of laser beam in the z-direction, adjusts displacement platform II and make sample cavity along the side x
To translation, detector is recorded the fluorescence signal of fluorescence reference, obtains w after being fitted using dimensional gaussian distribution to data0,
Adjusting displacement platform II translates sample cavity in the z-direction, and detector records the fluorescence signal of fluorescence reference, using dimensional Gaussian
Distribution obtains z after being fitted to data0, it is fitted using formula a pair of the data obtained, estimates detectable volume, representative value
It is 0.5 nanoliter；Detector continuously records the intensity for the fluorescence that the microparticle in a period of time T in detectable volume is launched, and obtains
To the signal data of some varying strengths, computer obtains detectable volume in T time after handling the signal data
The quantity of interior microparticle, and the revolving speed of sample cavity is combined, the quantity of microparticle in unit liquid volume can be obtained.
Microparticle quick counter measurement method in fluid sample are as follows:
Fluid sample containing microparticle to be measured is placed in sample cavity by step 1；
Step 2 adds fluorescent dye into fluid sample according to the type of microparticle to be measured, so that in respective wavelength
Laser irradiation under microparticle surfaces can launch fluorescence；
Step 3 adjusts the position of lens I, beam splitter, laser, optical filter, lens II, aperture, lens III and detector
It sets, so that the laser of laser transmitting is focused to the cylinder barrel of sample cavity lower half portion by lens I after the deviation of beam splitter
In, and make after passing sequentially through lens I, beam splitter, optical filter, lens II, aperture and lens III by the light of sample reflection, into
Enter detector；
Step 4, displacement platform II drive sample cavity to rotate around the y direction center line of sample cavity, and revolving speed a typical range of from 50 arrives
400 revs/min；
Step 5, the continuous laser that laser is launched are incident on the sample in sample cavity, the wave of the continuous laser
Length is determined according to the type of the fluorescent dye added in fluid sample；
Step 6 adjusts the size of aperture, and detector is enabled clearly to record the fluorescence of single microparticle transmitting；
Step 7, detector records the light projected from sample and generates corresponding data, after computer analyzes the data,
The quantity information for obtaining the microparticle sample to be measured in the detectable volume of fluid sample can be obtained in conjunction with the revolving speed of sample cavity
The quantity of microparticle in unit liquid volume, it is micro- in the unit volume liquid that can detect for 2 microns of microparticle of diameter
The minimum value of the quantity of particle is 50/milliliter.
A kind of the step of Ultrafast spectrum experimental method of microparticle are as follows:
Step 1, the fluid sample containing microparticle to be measured is placed in sample cavity；
Step 2, adjusting displacement platform II makes the width direction of the rectangular body cavity of the top half of sample cavity and z coordinate axis flat
Row adjusts the center for the rectangular body cavity that displacement platform I makes the axis extended line of rotary shaft be located at sample cavity top half；
Step 3, the position of lens I, beam splitter, laser, optical filter, lens II, aperture, lens III and detector is adjusted
It sets, so that the laser of laser transmitting is focused to the cuboid of sample cavity top half by lens I after the deviation of beam splitter
In chamber, and make after passing sequentially through lens I, beam splitter, optical filter, lens II, aperture and lens III by the light of sample reflection,
Into detector；
Step 4, open rotation motor magnet is at the uniform velocity rotated around the axis of rotary shaft, revolving speed representative value be 0.5 turn/
Second, so that stirring sheet is stirred sample；
Step 5, laser periodically launches pumping pulse and direct impulse sequence, pumping pulse and direct impulse week
It is incident in sample to phase property；
Step 6, it according to the rotation angle of the corresponding rotation motor in stirring sheet position, is issued by computer regulated laser
Pumping pulse and direct impulse interval time so that the quick switching process of opposite direction that stirring sheet is rotated to magnet is pumping
Pulse and direct impulse are incident in the time slot of sample；
Step 7, detector records the light projected from sample and generates corresponding data, and computer obtains after analyzing the data
To the Ultrafast spectrum of sample.
The beneficial effects of the present invention are:
The method of the present invention uses novel sample stirring means, so that the exchange velocity of sample is comparatively fast to meet in sample cavity
The needs of Ultrafast spectrum experiment, and can be avoided mechanical noise and enter spectrum, also avoid laser in the sample periodic
Refraction, improves the quality of spectroscopic data.
Detailed description of the invention
It is further illustrated below with reference to figure of the invention:
Fig. 1 is schematic diagram of the present invention；Fig. 2 is sample cavity side enlarged diagram；Fig. 3 is the top view of Fig. 2；
Fig. 4 is schematic diagram one of of the stirring sheet with magnet rotary course；
Fig. 5 is stirring sheet with the two of the schematic diagram of magnet rotary course；
Fig. 6 is stirring sheet with the three of the schematic diagram of magnet rotary course；
Fig. 7 is stirring sheet with the four of the schematic diagram of magnet rotary course；
Fig. 8 is stirring sheet with the five of the schematic diagram of magnet rotary course；
Fig. 9 is stirring sheet with the six of the schematic diagram of magnet rotary course.
In figure, 1. displacement platform I, 2. rotation motors, 3. rotary shafts, 4. magnet, 5. displacement platform II, 6. sample cavities, 7. stirrings
Piece, 8. lens I, 9. beam splitters, 10. lasers, 11. optical filters, 12. lens II, 13. apertures, 14. lens III, 15. detections
Device.
Specific embodiment
If Fig. 1 is schematic diagram of the present invention, xyz is three-dimensional coordinate system, including displacement platform I (1), rotation motor (2), rotation
Shaft (3), magnet (4), displacement platform II (5), sample cavity (6), stirring sheet (7), lens I (8), beam splitter (9), laser
(10), optical filter (11), lens II (12), aperture (13), lens III (14), detector (15) and computer, rotation motor
(2) it is fixed on displacement platform I (1), for magnet (4) by rotary shaft (3) connection rotation motor (2), rotary shaft (3) is parallel to z seat
Parameter, displacement platform I (1) can be three-dimensional mobile, and rotation motor (2) is able to drive magnet (4) rotation, and sample cavity (6) is fixed on position
On moving stage II (5), displacement platform II (5) can be three-dimensional mobile, and displacement platform II (5) is able to drive sample cavity (6) around sample cavity (6)
Y direction center line rotation, sample cavity (6) top half be rectangular body cavity, lower half portion be the cylinder barrel of axis in the y-direction, institute
Stating has aperture plate between top half and lower half portion, the rectangular body cavity is 30 millimeters a height of, 10 millimeters a length of, width is 2 millimeters,
The cylinder barrel is 20 millimeters a height of, basal diameter is 10 millimeters, y direction center line and the cylinder barrel of the rectangular body cavity
Axis collinear, by having magnetic stainless steel, package polytetrafluoroethylene (PTFE) is made stirring sheet (7) outside, and the diameter of stirring sheet (7) is
1.2 millimeters, length be 13 millimeters, stirring sheet (7) is located at sample cavity (6) top half, and the aperture plate can prevent stirring sheet (7)
Cylinder barrel is fallen into, the laser (10), beam splitter (9), lens I (8) and sample cavity (6) successively form input path, described
Sample cavity (6), lens I (8), beam splitter (9), optical filter (11), lens II (12), aperture (13), lens III (14) and detection
Device (15) successively forms emitting light path, laser (10) can the adjustable continuous laser of launch wavelength and laser pulse, laser arteries and veins
Punching includes pumping pulse and direct impulse, and the pumping pulse and direct impulse have different power, frequency and duration,
Time interval between direct impulse and pumping pulse can be adjusted, the rotation motor (2), laser (10) and detector
(15) difference cable connection computer can adjust the laser pulse and rotation motor of laser (10) sending by computer
(2) time difference between angle is rotated；The size of aperture (13) can be adjusted, can according to various sizes of microparticle to be measured come
Adjust the detection resolution of detector (15).
If Fig. 2 is sample cavity side enlarged diagram, if Fig. 3 is the top view of Fig. 2, sample cavity (6) top half is long
Cube chamber, lower half portion are the cylinder barrel of axis in the y-direction, y direction center line and the cylinder barrel of the rectangular body cavity
Axis collinear.
If Fig. 4 is schematic diagram one of of the stirring sheet with magnet rotary course, if Fig. 5 is stirring sheet with magnet rotary course
The two of schematic diagram, as Fig. 6 be stirring sheet with magnet rotary course schematic diagram three, if Fig. 7 is that stirring sheet is rotated through with magnet
The four of the schematic diagram of journey, as Fig. 8 be stirring sheet with magnet rotary course schematic diagram five, if Fig. 9 is that stirring sheet is revolved with magnet
The six of the schematic diagram of journey are turned over, arrow is direction of rotation in figure, and rotation motor (2) is able to drive magnet (4) rotation, magnet (4)
Position of magnetic pole change, stirring sheet (7) with magnet (4) rotate.
The Ultrafast spectrum research device of microparticle include displacement platform I (1), rotation motor (2), rotary shaft (3), magnet (4),
Displacement platform II (5), sample cavity (6), stirring sheet (7), lens I (8), beam splitter (9), laser (10), optical filter (11), lens
II (12), aperture (13), lens III (14), detector (15) and computer, xyz are three-dimensional coordinate system, rotation motor
(2) be fixed on displacement platform I (1), the laser (10), beam splitter (9), lens I (8) and sample cavity (6) successively form into
Penetrate optical path, the sample cavity (6), lens I (8), beam splitter (9), optical filter (11), lens II (12), aperture (13), lens
III (14) and detector (15) successively form emitting light path, and laser (10) the adjustable continuous laser of launch wavelength and can swash
Light pulse, laser pulse include pumping pulse and direct impulse, and the pumping pulse and direct impulse have different power, frequency
Rate and duration, the time interval between direct impulse and pumping pulse can be adjusted；Magnet (4) is connected by rotary shaft (3)
It connects rotation motor (2), rotary shaft (3) is parallel to z coordinate axis, and displacement platform I (1) can be three-dimensional mobile, and rotation motor (2) being capable of band
Moving magnet (4) rotation, sample cavity (6) are fixed on displacement platform II (5), and displacement platform II (5) can be three-dimensional mobile, displacement platform II
(5) be able to drive sample cavity (6) around sample cavity (6) y direction center line rotate, sample cavity (6) top half be rectangular body cavity,
Lower half portion is the cylinder barrel of axis in the y-direction, has aperture plate, the rectangular body cavity between the top half and lower half portion
A height of 30 millimeters, 10 millimeters a length of, width be 2 millimeters, the cylinder barrel is 20 millimeters a height of, basal diameter is 10 millimeters, the length
The y direction center line of cube chamber and the axis collinear of the cylinder barrel, stirring sheet (7) are wrapped up outside magnetic stainless steel by having
Polytetrafluoroethylene (PTFE) is made, and the diameter of stirring sheet (7) is 1.2 millimeters, length is 13 millimeters, and stirring sheet (7) is located on sample cavity (6)
Half part, the aperture plate can prevent stirring sheet (7) from falling into cylinder barrel；The rotation motor (2), laser (10) and detector
(15) difference cable connection computer can adjust the laser pulse and rotation motor of laser (10) sending by computer
(2) time difference between angle is rotated；The size of aperture (13) can be adjusted, can according to various sizes of microparticle to be measured come
Adjust the detection resolution of detector (15).
Stirring sheet (7) makes the principle of the sample part progress fast exchange of the different zones in sample cavity (6) are as follows:
Such as Fig. 1, adjusting displacement platform II (5) makes the width direction and z-axis of the rectangular body cavity of the top half of sample cavity (6)
In parallel, the center that displacement platform I (1) makes the axis extended line of rotary shaft (3) be located at rectangular body cavity is adjusted, rotation motor is opened
(2) rotate magnet (4) at the uniform velocity around the axis of rotary shaft (3), revolving speed representative value is 0.5 revolutions per second, such as Fig. 4, Fig. 5, due to by
Magnetic torque to magnet (4) acts on, and stirring sheet (7) will be rotated with magnet (4), and such as Fig. 6, stirring sheet (7) is rotated up both ends
It contacts and is limited with the inner wall of rectangular body cavity, such as Fig. 7, magnet (4) continues to rotate at this time, and stirring sheet (7) is still by magnet (4)
Magnetic torque effect, but stirring sheet (7) position is constant, such as Fig. 8, when magnet (4) rotation to a certain angle, stirring sheet (7) by
Magnetic torque to magnet (4) is reversed, and stirring sheet (7) can quickly be overturn to the opposite direction that magnet (4) rotate at this time, such as Fig. 9, stirring
Piece (7) is overturn until both ends contact and are limited with the inner wall of rectangular body cavity, in conclusion the process that magnet at the uniform velocity rotates a circle
In, stirring sheet (7) is rotated twice, is once stirring sheet (7) as magnet (4) direction of rotation rotates at a slow speed, is again
Stirring sheet (7) is quickly overturn to the opposite direction that magnet (4) rotates, and the quick switching process of stirring sheet (7) makes stirring sheet (7) attached
The sample of near field and the sample fast exchange of sample cavity (6) other parts.Technological merit is: stirring sheet (7) is with magnet (4)
The rotary course at a slow speed of direction of rotation will not introduce noise, be rotated by adjusting laser pulse and stirring sheet (7) to magnet (4)
The time interval of the quick switching process of opposite direction, the mechanical noise that can be effectively prevented from sample enter spectrum, also avoid
The periodic refraction of laser in the sample.
The principle of count measurement is carried out to the microparticle in fluid sample are as follows:
Fluid sample containing microparticle to be measured is placed in sample cavity (6), according to the type of microparticle to be measured, to liquid-like
Fluorescent dye is added in product, and the microparticle surfaces under the laser irradiation of specific wavelength is enabled to launch fluorescence, laser
(10) the laser irradiation sample emitted makes microparticle launch fluorescence, and the fluorescence is remembered by emitting light path by detector (15)
Record；The laser of laser (10) transmitting focuses to sample cavity (6) lower half by lens I (8) after the deviation of beam splitter (9)
In the cylinder barrel divided, displacement platform II (5) drives sample cavity (6) to rotate around the y direction center line of sample cavity (6), in fluid sample
The microparticle of suspension is moved together with solvent, and by the focus of sample cavity (6) interior laser to launch fluorescence；In sample cavity
(6) in non-rotary situation, wherein the fluorescence that the microparticle in the partial volume being irradiated with a laser is launched can be by detector
(15) this partial volume detected, is defined as detectable volume, and the method for estimating detectable volume is as follows: will launch
The fluorescence reference of fluorescence be fixed in sample cavity (6), and make detector (15) that can identify that laser beam is along the negative side Z
To incident sample cavity (6), when sample cavity is fixed, the intensity of the fluorescence signal of detector (15) record is(formula one), wherein w0It is laser beam in the with a tight waist of the direction x
Diameter, z0For the beam waist diameter of laser beam in the z-direction, adjusts displacement platform II (5) and sample cavity (6) is translated in the x-direction, detect
Device (15) records the fluorescence signal of fluorescence reference, obtains w after being fitted using dimensional gaussian distribution to data0, adjust position
Moving stage II (5) translates sample cavity (6) in the z-direction, and detector (15) records the fluorescence signal of fluorescence reference, using two dimension
Gaussian Profile obtains z after being fitted to data0, it is fitted using formula a pair of the data obtained, estimates detectable volume, allusion quotation
Offset is 0.5 nanoliter；Detector (15) continuously records the fluorescence that the microparticle in a period of time T in detectable volume is launched
Intensity, obtains the signal data of some varying strengths, and computer obtains to visit in T time after handling the signal data
The quantity of the microparticle in volume is surveyed, and combines the revolving speed of sample cavity (6), the number of microparticle in unit liquid volume can be obtained
Amount.
A kind of the step of Ultrafast spectrum experimental method of microparticle are as follows:
Step 1, the fluid sample containing microparticle to be measured is placed in sample cavity (6)；
Step 2, adjusting displacement platform II (5) sits the width direction of the rectangular body cavity of the top half of sample cavity (6) and z
Parameter is parallel, adjusts the cuboid that displacement platform I (1) makes the axis extended line of rotary shaft (3) be located at sample cavity (6) top half
The center of chamber；
Step 3, lens I (8), beam splitter (9), laser (10), optical filter (11), lens II (12), aperture are adjusted
(13), the position of lens III (14) and detector (15), so that the laser of laser (10) transmitting is by the inclined of beam splitter (9)
Backward, it is focused to by lens I (8) in the rectangular body cavity of sample cavity (6) top half, and the light reflected by sample is successively led to
After crossing lens I (8), beam splitter (9), optical filter (11), lens II (12), aperture (13) and lens III (14), into detector
(15)；
Step 4, opening rotation motor (2) rotates magnet (4) at the uniform velocity around the axis of rotary shaft (3), revolving speed representative value
It is 0.5 revolutions per second, so that stirring sheet (7) is stirred sample；
Step 5, laser (10) periodically launches pumping pulse and direct impulse sequence, pumping pulse and detection arteries and veins
Punching is periodically incident in sample；
Step 6, according to the rotation angle of the corresponding rotation motor (2) in stirring sheet (7) position, pass through computer regulated laser
The interval time of pumping pulse and direct impulse that device (10) issues, so that the opposite direction that stirring sheet (7) is rotated to magnet (4) is fast
Fast switching process is in the time slot that sample is incident in pumping pulse and direct impulse；
Step 7, detector (15) records the light projected from sample and generates corresponding data, and computer analyzes the data
The Ultrafast spectrum of sample is obtained afterwards.
The method of the present invention uses special sample cavity and stirring means, so that when carrying out Ultrafast spectrum experiment in sample cavity
Sample have faster exchange velocity, noise is small, and spectral quality is high, and operating process is easy.
Claims (1)
1. a kind of Ultrafast spectrum experimental method of microparticle, the Ultrafast spectrum research device of microparticle includes displacement platform I (1), rotation
Turn motor (2), rotary shaft (3), magnet (4), displacement platform II (5), sample cavity (6), stirring sheet (7), lens I (8), beam splitter
(9), laser (10), optical filter (11), lens II (12), aperture (13), lens III (14), detector (15) and computer,
Xyz is three-dimensional coordinate system, and rotation motor (2) is fixed on displacement platform I (1), the laser (10), beam splitter (9), thoroughly
Mirror I (8) and sample cavity (6) successively form input path, the sample cavity (6), lens I (8), beam splitter (9), optical filter
(11), lens II (12), aperture (13), lens III (14) and detector (15) successively form emitting light path, laser (10) energy
Enough adjustable continuous lasers of launch wavelength and laser pulse, laser pulse include pumping pulse and direct impulse, the pumping arteries and veins
Punching and direct impulse have different power, frequency and duration, the time interval energy between direct impulse and pumping pulse
It is enough to adjust；Magnet (4) is parallel to z coordinate axis, displacement platform I (1) by rotary shaft (3) connection rotation motor (2), rotary shaft (3)
Can be three-dimensional mobile, rotation motor (2) is able to drive magnet (4) rotation, and sample cavity (6) is fixed on displacement platform II (5), is displaced
Platform II (5) can be three-dimensional mobile, and displacement platform II (5) is able to drive sample cavity (6) and rotates around the y direction center line of sample cavity (6),
Sample cavity (6) top half be rectangular body cavity, lower half portion be the cylinder barrel of axis in the y-direction, the top half and lower half
There is aperture plate, the rectangular body cavity is 30 millimeters a height of, 10 millimeters a length of, width is 2 millimeters, the cylinder barrel a height of 20 between part
Millimeter, basal diameter are 10 millimeters, the y direction center line of the rectangular body cavity and the axis collinear of the cylinder barrel, stirring sheet
(7) polytetrafluoroethylene (PTFE) is wrapped up outside magnetic stainless steel being made, the diameter of stirring sheet (7) is 1.2 millimeters, length 13 by having
Millimeter, stirring sheet (7) are located at sample cavity (6) top half, and the aperture plate can prevent stirring sheet (7) from falling into cylinder barrel；It is described
Rotation motor (2), laser (10) and detector (15) difference cable connection computer, can adjust laser by computer
(10) time difference between the laser pulse issued and rotation motor (2) rotation angle；The size of aperture (13) can be adjusted, energy
Enough detection resolutions that detector (15) are adjusted according to various sizes of microparticle to be measured,
It is characterized in that: a kind of the step of Ultrafast spectrum experimental method of microparticle are as follows:
Step 1, the fluid sample containing microparticle to be measured is placed in sample cavity (6)；
Step 2, adjusting displacement platform II (5) makes the width direction and z coordinate axis of the rectangular body cavity of the top half of sample cavity (6)
In parallel, the rectangular body cavity that displacement platform I (1) makes the axis extended line of rotary shaft (3) be located at sample cavity (6) top half is adjusted
Center；
Step 3, adjust lens I (8), beam splitter (9), laser (10), optical filter (11), lens II (12), aperture (13), thoroughly
The position of mirror III (14) and detector (15) so that laser (10) transmitting laser after the deviation of beam splitter (9), quilt
Lens I (8) is focused in the rectangular body cavity of sample cavity (6) top half, and the light reflected by sample is made to pass sequentially through lens I
(8), after beam splitter (9), optical filter (11), lens II (12), aperture (13) and lens III (14), into detector (15)；
Step 4, opening rotation motor (2) rotates magnet (4) at the uniform velocity around the axis of rotary shaft (3), and revolving speed representative value is 0.5
Revolutions per second, so that stirring sheet (7) is stirred sample；
Step 5, laser (10) periodically launches pumping pulse and direct impulse sequence, pumping pulse and direct impulse week
It is incident in sample to phase property；
Step 6, according to the rotation angle of the corresponding rotation motor (2) in stirring sheet (7) position, pass through computer regulated laser
(10) interval time of the pumping pulse and direct impulse that issue, so that the opposite direction that stirring sheet (7) is rotated to magnet (4) is quick
Switching process is in the time slot that sample is incident in pumping pulse and direct impulse；
Step 7, detector (15) records the light projected from sample and generates corresponding data, and computer obtains after analyzing the data
To the Ultrafast spectrum of sample.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811220629.1A CN109580439B (en) | 2018-10-10 | 2018-10-10 | Ultra-fast spectrum experiment method for microparticles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811220629.1A CN109580439B (en) | 2018-10-10 | 2018-10-10 | Ultra-fast spectrum experiment method for microparticles |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109580439A true CN109580439A (en) | 2019-04-05 |
| CN109580439B CN109580439B (en) | 2023-12-22 |
Family
ID=65920200
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811220629.1A Active CN109580439B (en) | 2018-10-10 | 2018-10-10 | Ultra-fast spectrum experiment method for microparticles |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109580439B (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040085540A1 (en) * | 2000-12-28 | 2004-05-06 | Lapotko Dmitri Olegovich | Method and device for photothermal examination of microinhomogeneities |
| US20080186477A1 (en) * | 2007-01-19 | 2008-08-07 | Xuefeng Wang | System with extended range of molecular sensing through integrated multi-modal data acquisition |
| CN101271025A (en) * | 2007-03-20 | 2008-09-24 | 北京大学 | Method and device for ultrafast time discrimination measurement of seed photo-signal |
| CN101587074A (en) * | 2009-06-23 | 2009-11-25 | 华中科技大学 | Component analyzer for laser probe micro-area |
| CN101816552A (en) * | 2010-05-11 | 2010-09-01 | 天津大学 | Imitating CT scanning mode multispectral time domain fluorescence molecular tomography measuring system |
| DE102010005723A1 (en) * | 2010-01-26 | 2011-07-28 | WITec Wissenschaftliche Instrumente und Technologie GmbH, 89081 | Raman device i.e. Raman microscope, for recording sample surface, has time difference measuring device measuring photons and Raman and/or fluorescence photons emitted by sample based on effect of photons of light source |
| CN107532333A (en) * | 2015-02-22 | 2018-01-02 | 里兰斯坦福初级大学理事会 | Microtraps screening device, method and product |
-
2018
- 2018-10-10 CN CN201811220629.1A patent/CN109580439B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040085540A1 (en) * | 2000-12-28 | 2004-05-06 | Lapotko Dmitri Olegovich | Method and device for photothermal examination of microinhomogeneities |
| US20080186477A1 (en) * | 2007-01-19 | 2008-08-07 | Xuefeng Wang | System with extended range of molecular sensing through integrated multi-modal data acquisition |
| CN101271025A (en) * | 2007-03-20 | 2008-09-24 | 北京大学 | Method and device for ultrafast time discrimination measurement of seed photo-signal |
| CN101587074A (en) * | 2009-06-23 | 2009-11-25 | 华中科技大学 | Component analyzer for laser probe micro-area |
| DE102010005723A1 (en) * | 2010-01-26 | 2011-07-28 | WITec Wissenschaftliche Instrumente und Technologie GmbH, 89081 | Raman device i.e. Raman microscope, for recording sample surface, has time difference measuring device measuring photons and Raman and/or fluorescence photons emitted by sample based on effect of photons of light source |
| CN101816552A (en) * | 2010-05-11 | 2010-09-01 | 天津大学 | Imitating CT scanning mode multispectral time domain fluorescence molecular tomography measuring system |
| CN107532333A (en) * | 2015-02-22 | 2018-01-02 | 里兰斯坦福初级大学理事会 | Microtraps screening device, method and product |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109580439B (en) | 2023-12-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US10724957B2 (en) | Micro-droplet fluorescence detection system | |
| US9435727B2 (en) | Optical analysis device, optical analysis method and computer program for optical analysis using single light-emitting particle detection | |
| JPH04500274A (en) | Highly sensitive fluorescent single particle and single molecule detection device and method | |
| CN107478630B (en) | Device and method for improving single-molecule optical imaging contrast | |
| CN105259132A (en) | Terahertz wave transmission imaging system | |
| US20140170760A1 (en) | Optical anaylsis device, optical analysis method and computer program for optical analysis using single light-emitting particle detection | |
| JP2007538243A (en) | Apparatus and method for investigating a sample | |
| CN116577317B (en) | Combined detection device and combined detection method for Raman-laser ablation-mass spectrum | |
| CN209416867U (en) | A kind of Ultrafast spectrum research device of microparticle | |
| CN109374487A (en) | A kind of Ultrafast spectrum research device of microparticle | |
| CN106290277B (en) | The device and method in conversion nano fluorescent particle service life on a kind of measurement monodisperse | |
| US20220228969A1 (en) | Low-noise vibrational spectroscopy | |
| CN109580439A (en) | A kind of Ultrafast spectrum experimental method of microparticle | |
| US9528923B2 (en) | Optical analysis device, optical analysis method and computer program for optical analysis using single light-emitting particle detection | |
| GB2482908A (en) | Rheometer with optical interferometer | |
| CN109580440A (en) | A kind of microparticle quick counter measurement method in fluid sample | |
| WO2017144619A1 (en) | Method and device for high throughput imaging | |
| CN209342750U (en) | A kind of experimental facilities using Laser Doppler speed | |
| CN1815187A (en) | THz detecting system and method for oscillating mirror rapid scanning electro-optic sampling | |
| EP3059577A1 (en) | Photometric analysis device employing single light-emitting particle detection, photometric analysis method, and computer program for photometric analysis | |
| US11579091B2 (en) | Non-contact spatial super-resolution coherent Raman spectrometric imaging method | |
| CN106681015B (en) | A kind of automatic focusing mechanism and method suitable for reflective THz wave system | |
| CN103994973A (en) | Raman spectrum detection head and detection method | |
| Hattori et al. | Fluorescence correlation spectroscopy with traveling interference fringe excitation | |
| CN110907420B (en) | Device for measuring mass transfer equilibrium time between immiscible solution and liquid phase and measuring method using device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB03 | Change of inventor or designer information |
Inventor after: Xu Jingjing Inventor after: Zhang Xiangping Inventor after: Fang Xiaohua Inventor after: Zhao Yongjian Inventor before: Zhang Xiangping Inventor before: Fang Xiaohua Inventor before: Zhao Yongjian |
|
| CB03 | Change of inventor or designer information | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |