CN107957414A - A kind of method with potassium bromide quenching fluorescence in Raman spectrum - Google Patents
A kind of method with potassium bromide quenching fluorescence in Raman spectrum Download PDFInfo
- Publication number
- CN107957414A CN107957414A CN201711019040.0A CN201711019040A CN107957414A CN 107957414 A CN107957414 A CN 107957414A CN 201711019040 A CN201711019040 A CN 201711019040A CN 107957414 A CN107957414 A CN 107957414A
- Authority
- CN
- China
- Prior art keywords
- sample
- kbr tablet
- indentation
- raman spectrum
- mesh
- 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
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
Landscapes
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention belongs to technical field of analysis and detection, discloses a kind of method with potassium bromide quenching fluorescence in Raman spectrum.Using general infrared mould compacting kbr tablet, then using the sand paper or diamond disk of 220~320 mesh as instrument, with hand kbr tablet is promoted on sand paper or mill, indentation is made on kbr tablet, sample is effectively dispersed in the scored areas of kbr tablet, is then made on specimen face side, puts Upper gasket, then tabletting, the kbr tablet for being pressed with sample of gained is placed in the reflected light path of Raman spectrometer to take a little is detected.The fluorescence of any intensity in big absolutely most solid and fluid sample can be quenched in the present invention, laboratory is set to possess the Raman spectrum detection that a laser can complete most solids and fluid sample, and special consumptive material need not be used, there is highly important practical value.
Description
Technical field
The invention belongs to technical field of analysis and detection, and in particular to a kind of side with potassium bromide quenching fluorescence in Raman spectrum
Method.
Background technology
India's physicist's Raman (C.V.Raman) exists with his student's Clichy southern (K.S.Krishnan) in nineteen twenty-eight
A kind of new visible light scattering phenomenon is reported on Nature magazines, the frequency of light is scattered when this scattering occurs to be become
Change, this phenomenon is known as Raman scattering.Because it is found that Ramam effect and Raman scattering, Raman obtain Nobel in nineteen thirty
Physics is encouraged.In addition, it have also discovered similar phenomenon in nineteen twenty-eight Liang Wei former Soviet Union scientist.Raman phenomenon is a kind of non-ballistic of light
Property scattering phenomenon.When photon collides with material molecule, molecule produces induced dipole square under the action of electromagnetic field causes pole
Change, energy transfer occurs between molecule and photon, this process can be explained with " virtual energy level " of a Raman.Frequency reduces
Scattering light be known as stokes scattering, the elevated scattering light of frequency is known as anti-Stokes scattering.The energy comparison of incident light
When low, the scattering of generation is known as normal Raman scattering, is a kind of linear phenomena, at this moment stockes line is typically much stronger than anti-stoke
This line.What is studied herein is such a scattering.
In vibration processes, the change of molecular polarizability belongs to Raman active, and the generally vibration of non-polar group is drawn
Graceful spectral peak is stronger.Being of wide application for Raman spectrum is general, in new material, new energy, biomedicine, physics, geology, the administration of justice
There is very important application Deng ambit, such as graphene, carbonitride, chitosan, rare-earth mineral research field are all using drawing
Graceful spectrum is as important characterization method.Raman spectrum effectively promotes the development in these fields.
But Raman spectrum is often disturbed be subject to fluorescence in an experiment.Fluorescence is Electron absorption photon and launches again
Process, the wavelength of fluorescence is more than the wavelength of incident light and several orders of magnitude higher than the intensity of Raman diffused light.Work as Raman scattering
Virtual energy level and electronics true energy level it is close when, fluorescence will interfere the detection of Raman spectrum, sometimes even so that point
Analysis can not carry out completely.And fluorescence interference phenomenon can all occur for the material being much studied, therefore avoid fluorescence interference very heavy
Will.The method used at present has very much, for example, change excitation wavelength (generally use long wavelength), shorten acquisition time, change it is small narrow
Seam, photobleaching, and add quencher etc..When fluorescence interference is especially strong, it is necessary to using the method for adding quencher.It is quenched
Agent has many kinds, and potassium bromide is common quencher, but sample can not generally be had with potassium bromide mixing or tabletting merely
Strong fluorescence is quenched in effect.Therefore in real work, overcoming for fluorescence is still one of Raman detection most thorny issue.
The content of the invention
For more than in place of shortcoming and defect existing in the prior art, it is an object of the invention to provide in Raman spectrum one
The method of kind potassium bromide quenching fluorescence.
The object of the invention is achieved through the following technical solutions：
A kind of method with potassium bromide quenching fluorescence in Raman spectrum, includes the following steps：
(1) using general infrared mould compacting kbr tablet；
It is first noted that infrared mould is made choice.Traditional moulds can easily be removed kbr tablet, and some new classes
The mould of type is then that kbr tablet is inlayed wherein, it is more difficult to removes, therefore should select the mould for easily removing kbr tablet.Potassium bromide
Potassium bromide used during using infrared sample preparation, without in addition processing.The kbr tablet pressed can not have to protect in drier
Deposit, because the Raman peaks of water are natively weaker, the slight moisture absorption of kbr tablet will not have any impact experiment；Certainly also not
It should preserve in a humid environment.
(2) indentation is made on kbr tablet；
The making of indentation is particularly important, because only that the indentation for obtaining one fixed width could meet the bar of experiment in next step
Part.It is not all right with common pocket knife scribing, because indentation is too wide.And sand paper and disc surface are stained with abrasive material, the grain of abrasive material
Degree (mesh number) has many specifications, therefore is effectively to select with sand paper and mill polishing.The optimization of abrasive material mesh number is discussed further below
Journey.The result shows that 220 mesh~320 mesh can obtain ideal band, can obtain optimum efficiency using 320 mesh abrasive materials.Can
To be used as the instrument for making indentation using the carborundum paper of 320 mesh or the diamond disk of 320 mesh.During operation, according to
Sand paper, then first stretch sand paper, and then forefinger and thumb are held the both ends of kbr tablet and slided on sand paper to a direction, sliding
Dynamic distance about 3cm, is slided once.It according to mill, can use and the same method of sand paper, or bromination is pushed down with middle finger
Potassium piece promotes on mill, and firmly appropriateness can (such as 1 kilogram).Sand paper can be cleaned after with ear washing bulb, and mill needs after
Naturally dry is rinsed well with water, and unavailable paper wipes.
(3) loading and final film-making；
Loading uses proper method in having made on the kbr tablet of indentation, to be effectively dispersed in sample sample distribution
In scored areas.This is equally one of committed step.First by kbr tablet indentation upward, it is placed on clean pan paper.If
Indoor light is not very bright, need to prepare flashlight or infrared lamp in case observation.For the sample of different shape, the tool taken
Body method is different.
1. powder sample and fine granularity sample：The sample of 0.2mg or so is taken with spoon, is gently shaken, makes it appropriate equal
It is distributed in evenly on kbr tablet.To powdered samples, gently stirred with the pan paper rolled well, open the sample dispersion of reunion.
If fine granularity sample, is pressed lightly on spoon, make its crushing.Then, sample is stirred along indentation direction, sample is tried one's best
It is dispersed in scored areas.At this moment observation sample is paid attention to, being more than must gently being dialled with pan paper for kerf width for diameter removes,
Until no obvious above-mentioned particle in sample.There cannot be the region of the sample collection of sheet on kbr tablet at the same time.If in addition,
It is the sample of large grained, should be ground first in agate mortar certainly.
2. thick liquid：A little sample is dipped with capillary glass tube, is moved along indentation direction, makes sample along indentation direction point
Cloth.The libation at an ancient wedding ceremony takes three or four samples.Being brandished with hand makes evaporation of the solvent.
3. solution example：With capillary glass tube pipette samples, dubbed on kbr tablet, optional diverse location dubs four
It is secondary.Wherein allow liquid runs down indentation free movement (capillary moving) twice, stir liquid along indentation direction with capillary twice
Body, should once dial to kbr tablet edge.Being brandished with hand makes evaporation of the solvent.
It is preferably to lack unsuitable more to pay attention to Key Principles during loading, otherwise will be dispersed with hyperfluorescence area on kbr tablet everywhere
Domain, may make the failure of an experiment.After completion of the sample, sample is gently placed on mould with tweezers, on specimen face side, puts pad
Piece, presses upperpush rod with tablet press machine, Upper gasket and sample strip is entered in mould by upperpush rod.The same positive normal pressure of subsequent step
Piece is consistent.
(4) Raman spectrum detects；
Purpose using above-mentioned method for making sample is to obtain the sample area of given shape, has and only this region can just be obtained
Preferable Raman spectrogram is obtained, other shapes of region can not be realized.The region of this given shape is exactly ribbon region
(stripe area), the typical sizes in this region are that length is more than 100 μm, 5~10 μm of width, it is certainly more narrower can be more
It is good.The band spectrogram quality for meeting typical sizes can be especially good, and fluorescent base originally can be quenched；But it is careful that atypia band passes through
Reconnaissance can generally also obtain preferable spectrogram.It should be noted that the following conditions, method and skill during detection.
Observe and adopt time spectrum and use 50 times of camera lenses.Since band is smaller, can not be observed with 10 times of object lens；If with 100 times of things
Mirror, since the visual field is smaller, then observing speed can be slack-off.With normal 50 times of camera lenses and 50 times of telephoto lenses, to observing without shadow
Ring.But consider from signal strength, it is preferable with normal 50 times of camera lenses.Find ribbon region and reconnaissance is highly dependent on skill.Most
Noteworthy point is that banded zone is higher in the frequency that the edge of kbr tablet and outer region occur, this should be weight
The region of point concern.Observational technique to piece is that object lens are first navigated to one end (such as the edge on the most left side) of kbr tablet,
Then object lens are moved along Y-axis to be observed and found.Object lens are kept to move along the x-axis, until the observation for completing full sheet is (necessary
Words).One kbr tablet usually has 1~2 exemplary ribbon, there is 3~4 sometimes.Sometimes phase negative side of the band in initial position
To, therefore it is patient during searching.For exemplary ribbon, in the reconnaissance of band center.For atypia band it is noted that choosing
Appropriate point is detected.If band is wide, the end stenosis reconnaissance in band may be selected；If without suitable band only
There is discrete point, the point in ribbon arrangement may be selected.The point of selection may not be all suitable, if fluorescence still can nearby go more by force again
Find, or even replace region.The fluorescence of sample is stronger, and strip width should be thinner.Laser usually selects 532nm, if still
Old hypofluorescence exists, and 633nm may be selected, generally can all obtain high quality spectrogram., usually must choosing if sample does not have standard spectrogram
Two different point collection spectrograms are selected, two times result needs unanimously just to can confirm that spectrogram；, should be in standard spectrogram if there is standard spectrogram
Unanimously.As long as actually band is preferable, spectrogram is usually all ideal.
Present method be advantageous in that even if a kind of lasers of laboratory only 532nm or 633nm, pass through above-mentioned sample preparation
Various types of solids and fluid sample can be also handled with spectral method is adopted, especially with the sample of fluorescence, without purchasing
The laser of specific wavelength is put, greatly facilitates the Raman experiments room of general type.Some samples are even using replacement laser
Method can not also obtain preferable spectrogram, this method is exactly to obtain the powerful approach of Raman spectrogram, even unique method.
On the other hand, although preferable spectrogram can be obtained by replacing laser sometimes, in different excitation wavelength conditions
Under, the spectrogram of same sample may be different.Using the method for surface enhanced, although can be with quenching fluorescence, after surface enhanced
Spectrogram often with not strengthening when have different.Therefore under the conditions of hyperfluorescence, to study some excitation wavelength normal
Raman spectrogram during experiment condition, process provides a strong means.
Brief description of the drawings
Fig. 1 is to be made the chitosan obtained after indentation in the embodiment of the present invention 1 on kbr tablet of 320 mesh sand paper
The photo figure (C) of Raman spectrogram (A), the Raman spectrogram (B) of bibliography and exemplary ribbon.
Fig. 2 is the standard spectrogram (A) of calcium carbonate in the embodiment of the present invention 2, the standard spectrogram (B) of starch, gained sample
The photo figure (D) of Raman spectrogram (C) and the band chosen.
Fig. 3 is the photo figure (B) of the Raman spectrogram (A) of gained sample and the band chosen in the embodiment of the present invention 3.
Fig. 4 is the Raman spectrogram (C) of carbonitride sample in carbonitride spectrogram reported in the literature (A and B), embodiment 4
With the photo figure (D) of the floating screed band of selection.
Fig. 5 is rhodamine 6G reported in the literature (R6G) spectrogram (A), the Raman spectrogram of 5 gained R6G samples of embodiment
(B) and choose floating screed band photo figure (C).
Fig. 6 is the photograph of the Raman spectrogram (A) of glucide and the band chosen in sample obtained by the embodiment of the present invention 6
Piece figure (B)；The photo figure (D) of the Raman spectrogram of lipid and protein substance (C) and the floating screed band chosen.
Embodiment
With reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Embodiment 1
(1) using general infrared mould (diameter 13mm) compacting kbr tablet；
(2) indentation is made on kbr tablet：
The good kbr tablet of pressure, the both ends of piece are held with forefinger and thumb, respectively in 120 mesh, 220 mesh, 280 mesh, 320
Mesh, 360 mesh, slide on 7 kinds of mesh number carborundum papers of 400 mesh and 500 mesh, and sliding distance about 3cm, obtains impressed potassium bromide
Piece.
(3) loading and final film-making (preparation of chitosan sample is the sample making course of very typical powdered samples)：
Kbr tablet indentation is face-up, it is placed on clean pan paper.About 0.2mg Chitosan powders are taken (to go with spoon
95%) acetyl degree, which is more than, to be uniformly sprinkling upon on kbr tablet, further disperseed powder with a pan paper, then along indentation side
To powder is stirred, it is set to be distributed in as far as possible in indentation.Dial again except indivedual larger particles, for the in blocks coloured of on piece
Region, is also dialled except clean.Kbr tablet is positioned on infrared mould with tweezers, puts Upper gasket, then tabletting, pressure is
12MPa。
(4) Raman spectrum detects：
Sample is placed in the reflected light path of Raman spectrometer after the completion of film-making and is detected.Instrument condition is：Excitation wave
Long 532nm, to sample on power 6mW, 50X camera lens, grating 600gr/mm, 200 μm of slit, 100 μm of pin hole, accumulated time
30s, accumulates 2 times.
Observation and result of the test are as follows.
(1) 120 mesh：The irregular region in kbr tablet surface is more, it is difficult to find band.Have that a rule bandwidth is very wide,
About 50 μm, and there are many bulk particles in centre.The band (5~10 μm) of suitable width only has one, and very short (~25 μ of length
m).Preferable spectrogram can not be obtained.
(2) 220 mesh：A suitable band can be respectively found at the edge of kbr tablet and periphery, the μ of a width~10
M, another width is 8 μm and 15 μm, and length is~500 μm, can obtain preferable spectrogram.But still have in band more much
Block particle.The another band for having a length to be 250 μm, but width~20 μm, are unsatisfactory for requiring.
(3) 280 mesh：It can be found that on piece has many thin indentations, 3 μm or 8 μm of width.Two are found that in the periphery of piece
Almost parallel band, 12 μm of width, length is respectively 900 μm and 400 μm, and spectrogram is fine.Another discovery band two, length/
Width is respectively：350 μm/8 μm and 250 μm/12 μm.Although using the sand paper band number showed increased of 280 mesh, width is still
It is aobvious slightly wide.
(4) 320 mesh：On piece has many thin indentations, 3 μm of width.The band that length is 150 μm is found that at the edge of piece,
4~5 μm of width, spectrogram is very good.Separately finding one band of each discovery at edge and periphery, length/width is respectively 350 μm/
10 μm~15 μm and 200 μm/5 μm, the latter's spectrogram is good.The strip width of 320 mesh sand paper is decreased obviously than 280 mesh.This method
The Raman spectrogram of the chitosan of acquisition is as shown in A in Fig. 1, (B in Fig. 1) basically identical with bibliography.The photograph of exemplary ribbon
Piece is as shown in Figure 1 C.
(5) 360 mesh：On piece has many thin indentations, 3 μm of width.A band is only found, length/width is 150 μm/7 μ
M, but have strong fluorescence in spectrogram, spectrogram is poor.
(6) 400 mesh：On piece has many thin indentations, 3 μm of width.A band is only found, length/width is 120 μm/8 μ
M, but have strong fluorescence in spectrogram, spectrogram is poor.
(7) 500 mesh：On piece has very more thin indentations, 2 μm of width, and depth is shallower.Only find a very short bar
Band, length/width are 80 μm/8 μm, have strong fluorescence in spectrogram, appearance is weaker, and spectrogram is poor.
By above optimization process as it can be seen that the band number of 320 mesh sand paper is more, narrower width, the non-convention of spectrogram of acquisition
Think, therefore 320 mesh are optimal mesh number.120 mesh are difficult to obtain band.Although 220 mesh and 280 mesh can obtain ideal bar
Band, but strip width is still wider, is typically larger than 10 μm.It is not especially strong sample for fluorescence, 10~15 μm of band is fine
Obtain preferable spectrogram, but for hyperfluorescence and the very sample of hyperfluorescence, strip width must narrow (such as 5 μm or smaller)
Good spectrogram can be obtained.Therefore 220 mesh and 280 mesh have compared with big limitation, and 220 purpose bands and irregular.For 360
Mesh, 400 mesh and 500 mesh sand paper, bin number is seldom, only one.Although size is substantially suitable, fluorescence is all stronger, it is difficult to
Obtain preferable spectrogram, it may be possible to because band is shallower.Therefore 320 mesh are optimal mesh numbers, to the sample of various fluorescence intensities
Product well adapting to property.
Sample preparation is repeated to chitosan using 320 mesh sand paper, can obtain preferable band, length is more than 100 μm, the μ of width~5
M, spectrogram are ideal and basically identical.Therefore the method for making sample has good stability.
Compare 320 mesh carborundum papers of domestic and international different brands, stripe size, quantity and spectrogram quality basic one
Cause, thus different brands on sample quality without influence.
Compare the common sand paper of 320 mesh (into kermesinus, main abrasive material is carborundum and aluminium oxide in abrasive material face), 320 mesh carbon
The sample quality of SiClx sand paper and 320 mesh diamond disks.The band spectrogram quality that the common sand paper of 320 mesh is formed is general, and holds
Tend to have abrasive material to come off to form pollution, therefore common sand paper is not easy to select.The effect of diamond disk and carborundum paper is suitable, because
This can also be selected.
Embodiment 2
The present embodiment sample (sample 1) is pale pink powder, is prepared by following methods：Weigh calcium carbonate and starch is each
1.0g, stirs evenly.Rhodamine 6G (R6G) aqueous solution 1mL of 10 μ g/mL is added, then be sufficiently stirred and makes to be uniformly mixed.By
In the presence of R6G, sample shows intense fluorescence.Calcium carbonate does not have fluorescence, its characteristic peak is in 1089cm-1、716cm-1And 283cm-1.Starch does not also show fluorescence, its characteristic peak appears in 2916cm-1、1339cm-1And 1131cm-1。
(1) using general infrared mould (diameter 13mm) compacting kbr tablet；
(2) indentation is made on kbr tablet：
The good kbr tablet of pressure, the both ends of piece are held with forefinger and thumb, are slided on 320 mesh carborundum papers, sliding
Dynamic distance about 3cm, obtains impressed kbr tablet.
(3) (calcium carbonate and starch is respectively inorganic and organic dust, the mixture that they are formed is for loading and final film-making
The representative configuration of powder sample, operating process also represent the During typical operation of powdered samples)：
Kbr tablet indentation is face-up, it is placed on clean pan paper.About 0.2mg samples are taken uniformly to be sprinkling upon bromine with spoon
Change potassium on piece, powder is further disperseed with a pan paper, then powder is stirred along indentation direction, it is distributed as far as possible
In indentation.Dial except indivedual larger particles, for the coloured region in blocks of on piece, also dial except clean again.By potassium bromide
Piece is positioned on infrared mould with tweezers, puts Upper gasket, then tabletting, pressure 12MPa.
(4) Raman spectrum detects：
After the completion of sample is placed in the reflected light path of Raman spectrometer and is detected.Instrument condition is：Excitation wavelength
532nm, to sample on power 6mW, 50X camera lens, grating 600gr/mm, 200 μm of slit, 100 μm, accumulated time 30s of pin hole,
Accumulation 2 times.Find 5 bands altogether on kbr tablet, wherein most suitable band occurs in the middle part of piece, length/wide
Degree is respectively 300 μm/6 μm, and obtained spectrogram is good.The standard spectrogram (A) of calcium carbonate, standard spectrogram (B), the sample spectra of starch
The photo figure (D) of figure (C) and band is shown in Fig. 2.Band takes a position as at tracking cross.
Embodiment 3
The sample (sample 2) of the present embodiment is commercially available roll paper.Roll paper shows intense fluorescence, and possible cause is wherein to contain
Fluorescent whitening agent.Roll paper is soft two-dimentional sample, is made of fiber, can take following methods sample preparation.By roll paper in 320 mesh gold
Dabbed on hard rock mill, form thin fiber powder, larger chip is blown away with ear washing bulb.
(1) using general infrared mould (diameter 13mm) compacting kbr tablet；
(2) indentation is made on kbr tablet：
The good kbr tablet of pressure, is pinned with middle finger, is promoted in the position for forming fine fibre powder on diamond disk before,
Actuating length about 3cm, obtains impressed kbr tablet, while the fine fibre powder of roll paper is uniformly distributed in indentation.
(3) loading and final film-making：
Kbr tablet indentation is face-up, Upper gasket is put, then tabletting, pressure 12MPa.
(4) Raman spectrum detects：
After the completion of sample is placed in the reflected light path of Raman spectrometer and is detected.Instrument condition is：Excitation wavelength
532nm, to sample on power 6mW, 50X camera lens, grating 600gr/mm, 200 μm of slit, 100 μm, accumulated time 30s of pin hole,
Accumulation 2 times.Find 6 bands altogether on kbr tablet, wherein having, 4 spectrograms are good, length/width is respectively 800 μm/8 μm,
400 μm/8 μm, 100 μm/8 μm and 200 μm/8 μm.Because roll paper is made of fiber in itself, therefore easily forms high-quality band.Sample
The photo figure (B) of product spectrogram (A) and band is shown in Fig. 3.Band takes a position as at tracking cross.
Embodiment 4
The sample (sample 3) of the present embodiment is carbonitride (C3N4), voluntarily prepared by laboratory.Method is：By dicyandiamide plus
Enter into porcelain crucible, be positioned over calcination under the conditions of 500 DEG C in Muffle furnace.Carbonitride is a kind of new material, is had to visible ray good
It is good to absorb, can be as photochemical catalyst and the material of manufacture fluorescent optical sensor.But during using excited by visible light, there is very hyperfluorescence to go out
It is existing.Method for making sample is as follows.
(1) using general infrared mould (diameter 13mm) compacting kbr tablet；
(2) indentation is made on kbr tablet：
The good kbr tablet of pressure, the both ends of piece are held with forefinger and thumb, are slided on 320 mesh carborundum papers, sliding
Dynamic distance about 3cm, obtains impressed kbr tablet.
(3) loading and final film-making：
Kbr tablet indentation is face-up, it is placed on clean pan paper.About 0.2mg samples are taken uniformly to be sprinkling upon bromine with spoon
Change potassium on piece, powder is further disperseed with a pan paper, then powder is stirred along indentation direction, it is distributed as far as possible
In indentation.Dial except indivedual larger particles, for the coloured region in blocks of on piece, also dial except clean again.Due to nitridation
The particle of carbon is thinner, therefore should remove more.Kbr tablet is positioned on infrared mould with tweezers, puts Upper gasket, so
Tabletting afterwards, pressure 12MPa.
(4) Raman spectrum detects：
After the completion of sample is placed in the reflected light path of Raman spectrometer and is detected.Instrument condition is：Excitation wavelength
532nm, to sample on power 10mW, 50X camera lens, resolution ratio 4cm-1, 50 μm, time for exposure 0.25s of pin hole, accumulates 200 times.
Carbonitride sample is more special, it is more difficult to effective band is formed, can only be in a manner of discrete point or interrupted mode forms floating screed
Band.Although the more effective band of fluorescence is strong, the main spectral peak of carbonitride still clearly, disclosure satisfy that analysis needs.Text
The carbonitride spectrogram (A and B), the sample spectrogram (C) of carbonitride and the photo figure (D) of floating screed band for offering middle report are shown in Fig. 4, band
A position is taken as at tracking cross.By photo as it can be seen that carbonitride forms a floating screed band from top to bottom.The nitridation obtained herein
Carbon spectrogram and document are basically identical, and wherein A is with reference to wherein " block g-C3N4" spectrogram (main spectral peak is 1236cm-1And 704cm-1~708cm-1), spectrograms (excitation wavelength 244nm) of the B with reference to wherein " a ".
Embodiment 5
The sample (sample 4) of the present embodiment is the aqueous solution of rhodamine 6G (R6G), and concentration 1%, solution takes on a red color.R6G
It is a kind of organic dyestuff, available for biological stain and imaging.
(1) using general infrared mould (diameter 13mm) compacting kbr tablet；
(2) indentation is made on kbr tablet：
The good kbr tablet of pressure, the both ends of piece are held with forefinger and thumb, are slided on 320 mesh carborundum papers, sliding
Dynamic distance about 3cm, obtains impressed kbr tablet.
(3) loading and final film-making：
Kbr tablet indentation is face-up, it is placed on clean pan paper.Sample is diluted 10 times, obtains concentration as 0.1%
Test solution.Suitable test solution is drawn with capillary glass tube, is dubbed at the center of kbr tablet, is made a small amount of
Solution is transferred on kbr tablet, then along indentation direction stroke liquid, until the edge of piece.One is also selected in the periphery of piece
Position equally operates.Selected else a bit in the periphery of piece, solution is flowed along indentation after point sample, be actually the capillary work of indentation
With caused.It can also be dubbed if necessary in the edge of piece.Brandished with hand, volatilize solvent, then tabletting, pressure 12MPa.
(4) Raman spectrum detects：
After the completion of sample is placed in the reflected light path of Raman spectrometer and is detected.Instrument condition is：Excitation wavelength
532nm, to sample on power 6mW, 50X camera lens, grating 600gr/mm, 200 μm of slit, 100 μm, accumulated time 20s of pin hole,
Accumulation 2 times.R6G samples are also more special, it is also difficult to effective band is formed, can only be in a manner of discrete point or embedded thin indentation
Floating screed band is formed, but can also have preferable spectrogram.R6G spectrograms (A) reported in the literature, the sample spectrogram (B) of R6G and floating screed band
Photo figure (C) is shown in Fig. 5, and band takes a position as at tracking cross.By the C of Fig. 5 as it can be seen that on piece is formd is made of discrete point
Floating screed band, end embedded in thin indentation (2 μm of width).The reconnaissance at the thin indentation of band, obtains good spectrogram, main
Spectrum peak position is wanted in 1364cm-1、1307cm-1、1189cm-1、1773cm-1、613cm-1And 1649cm-1Place.Provided in document
Spectrogram is shown in A (a) in Fig. 5, is excited using 1064nm wavelength.The spectrogram obtained herein and document are basically identical.
Embodiment 6
The sample (sample 5) of the present embodiment is commercially available baby formula milk powder, white powdered.The component of milk powder is very
Complexity, is formed by pure milk and multiple additives formula, and main component is the compounds such as carbohydrate, fat and protein.
(1) using general infrared mould (diameter 13mm) compacting kbr tablet；
(2) indentation is made on kbr tablet：
The good kbr tablet of pressure, the both ends of piece are held with forefinger and thumb, are slided on 320 mesh carborundum papers, sliding
Dynamic distance about 3cm, obtains impressed kbr tablet.
(3) loading and final film-making：
Kbr tablet indentation is face-up, it is placed on clean pan paper.About 0.2mg samples are taken uniformly to be sprinkling upon bromine with spoon
Change potassium on piece, powder is further disperseed with a pan paper, then powder is stirred along indentation direction, it is distributed as far as possible
In indentation.Dial again except indivedual larger particles.Kbr tablet is positioned on infrared mould with tweezers, puts Upper gasket, so
Tabletting afterwards, pressure 12MPa.
(4) Raman spectrum detects：
After the completion of sample is placed in the reflected light path of Raman spectrometer and is detected.Instrument condition is：Excitation wavelength
633nm, to sample on power 3mW, 50X camera lens, grating 600gr/mm, 200 μm of slit, 100 μm, accumulated time 30s of pin hole,
Accumulation 2 times.Experiment shows, more preferable with 633nm rate of induced polarization 532nm effects for powdered milk sample, therefore selects 633nm excitations.
A very short lustrous band (see Fig. 6 B) is found on sample, after testing differentiate for glucide formed band (spectrogram is shown in figure
6A), 1094cm-1And 1122cm-1For the characteristic peak of glucide.Projection, " smooth " standard is found in other regions of piece again
Band (see Fig. 6 D), differentiates to be lipid and protein substance (spectrogram is shown in Fig. 6 C), wherein 1748cm after testing-1For lipid material
Characteristic peak, 1656cm-1For the characteristic peak of protein substance.It is more difficult for the extremely complex material of the components such as milk powder, this method
The averaged spectrum of sample is obtained, but the spectrum of special component can be obtained, also has valuable help to analysis.Especially, when in sample
When the content of certain component is very low can not to obtain Raman spectrum using conventional method, this method can realize the richness of low content component
Collection, separation, so as to fulfill detection.A position that takes for band is at tracking cross.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention and from above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (5)
1. a kind of method with potassium bromide quenching fluorescence in Raman spectrum, it is characterised in that include the following steps：
(1) using general infrared mould compacting kbr tablet；
(2) indentation is made on kbr tablet：Using the sand paper or diamond disk of 220~320 mesh as instrument, existed with hand
Kbr tablet is promoted on sand paper or mill；
(3) loading and final film-making：By sample distribution in having made on the kbr tablet of indentation, sample is set to be effectively dispersed in indentation
In region, then make on specimen face side, put Upper gasket, then tabletting；
(4) Raman spectrum detects：The kbr tablet for being pressed with sample of step (3) is placed in the reflected light path of Raman spectrometer and is taken
Point is detected.
A kind of 2. method with potassium bromide quenching fluorescence in Raman spectrum according to claim 1, it is characterised in that：In bromine
When changing potassium on piece making indentation, using the sand paper or diamond disk of 320 mesh as instrument.
3. a kind of method with potassium bromide quenching fluorescence in Raman spectrum according to claim 1, it is characterised in that make sample
The method that product are effectively dispersed in scored areas is：For powder sample, first it is uniformly distributed on kbr tablet, then along indentation
Sample is stirred in direction, sample is distributed in as far as possible in indentation, and removes particle of the diameter more than kerf width and large stretch of concentration
Particle；For thick liquid sample, sample is dipped with capillary glass tube, is moved along indentation direction；For solution example, glass is used
Capillary pipette samples, dub on kbr tablet, either along indentation direction stir liquid or allow liquid runs down indentation direction
Free movement.
A kind of 4. method with potassium bromide quenching fluorescence in Raman spectrum according to claim 1, it is characterised in that：Step
(4) taking described in, which is a little detected, refers to that choosing length is more than 100 μm, and width is that 5~10 μm of ribbon region is examined
Survey；Or choose the floating screed region that in a manner of discrete point or interrupted mode is formed and be detected.
A kind of 5. method with potassium bromide quenching fluorescence in Raman spectrum according to claim 1, it is characterised in that：It is described
Raman spectrometer uses the laser of 532nm or 633nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711019040.0A CN107957414B (en) | 2017-10-27 | 2017-10-27 | Method for quenching fluorescence by using potassium bromide in Raman spectrum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711019040.0A CN107957414B (en) | 2017-10-27 | 2017-10-27 | Method for quenching fluorescence by using potassium bromide in Raman spectrum |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107957414A true CN107957414A (en) | 2018-04-24 |
| CN107957414B CN107957414B (en) | 2020-09-22 |
Family
ID=61964008
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711019040.0A Active CN107957414B (en) | 2017-10-27 | 2017-10-27 | Method for quenching fluorescence by using potassium bromide in Raman spectrum |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107957414B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1425911A (en) * | 2003-01-17 | 2003-06-25 | 南京师范大学 | Raman test method for quick eliminating biologichal molecular fluorescence |
| CN101191771A (en) * | 2007-12-21 | 2008-06-04 | 辽宁大学 | Raman spectra detection process |
| CN102706854A (en) * | 2012-06-11 | 2012-10-03 | 上海化工研究院 | Portable system for rapidly recognizing chemical fertilizer |
| CN103664958A (en) * | 2012-09-26 | 2014-03-26 | 四川海思科制药有限公司 | Crystal form of ticagrelor and preparation method for crystal form |
| CN106950215A (en) * | 2017-03-22 | 2017-07-14 | 武汉大学 | A kind of method of sodium carbonate or sodium acid carbonate content in measure solid sample |
-
2017
- 2017-10-27 CN CN201711019040.0A patent/CN107957414B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1425911A (en) * | 2003-01-17 | 2003-06-25 | 南京师范大学 | Raman test method for quick eliminating biologichal molecular fluorescence |
| CN101191771A (en) * | 2007-12-21 | 2008-06-04 | 辽宁大学 | Raman spectra detection process |
| CN102706854A (en) * | 2012-06-11 | 2012-10-03 | 上海化工研究院 | Portable system for rapidly recognizing chemical fertilizer |
| CN103664958A (en) * | 2012-09-26 | 2014-03-26 | 四川海思科制药有限公司 | Crystal form of ticagrelor and preparation method for crystal form |
| CN106950215A (en) * | 2017-03-22 | 2017-07-14 | 武汉大学 | A kind of method of sodium carbonate or sodium acid carbonate content in measure solid sample |
Non-Patent Citations (1)
| Title |
|---|
| 黎雯: "类水滑石/碳纳米管复合材料的构建及其对双酚A的催化降解研究", 《中国博士学位论文全文数据库 工程科技I辑》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107957414B (en) | 2020-09-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Duran et al. | Determination of pigments and binders in Pompeian wall paintings using synchrotron radiation–high‐resolution X‐ray powder diffraction and conventional spectroscopy–chromatography | |
| Esposito et al. | Analysis of single bacterial spores by micro-Raman spectroscopy | |
| Schopf et al. | Laser–Raman imagery of Earth's earliest fossils | |
| Vandenabeele et al. | Non‐destructive analysis of paintings using Fourier transform Raman spectroscopy with fibre optics | |
| Raza et al. | Application of Raman spectroscopy in forensic investigation of questioned documents involving stamp inks | |
| Zhang et al. | Practical implementation, characterization and applications of a multi-colour time-gated luminescence microscope | |
| Pessanha et al. | Application of spectroscopic techniques to the study of illuminated manuscripts: a survey | |
| Zhang et al. | Surface-enhanced Raman spectroscopy with Au-nanoparticle substrate fabricated by using femtosecond pulse | |
| Kikawada et al. | Enhanced multicolor fluorescence in bioimaging using deep-ultraviolet surface plasmon resonance | |
| Wang et al. | Innovative ochre processing and tool use in China 40,000 years ago | |
| Shahbazi et al. | Preparation, characterization, and application of a lipophilic coated exfoliated Egyptian blue for near-infrared luminescent latent fingermark detection | |
| Mancini et al. | Testing of Raman spectroscopy as a non‐invasive tool for the investigation of glass‐protected miniature portraits | |
| Klisińska‐Kopacz | Non‐destructive characterization of 17th century painted silk banner by the combined use of Raman and XRF portable systems | |
| Prati et al. | Evaluation of the effect of six different paint cross section preparation methods on the performances of Fourier Transformed Infrared microscopy in attenuated total reflection mode | |
| Campanella et al. | The shining brightness of daylight fluorescent pigments: Raman and SERS study of a modern class of painting materials | |
| Alyami et al. | Identification of dye content in colored BIC ballpoint pen inks by Raman spectroscopy and surface‐enhanced Raman scattering | |
| Retko et al. | Surface‐enhanced Raman spectroscopy (SERS) analysis of organic colourants utilising a new UV‐photoreduced substrate | |
| Gullu et al. | Use of tourmaline as a potential petrogenetic indicator in the determination of host magma: CRS, XRD and PED-XRF methods | |
| Xu et al. | Mineralogical characteristics of Mn coatings from different weathering environments in China: clues on their formation | |
| Sciutto et al. | A new integrated TLC/MU-ATR/SERS advanced approach for the identification of trace amounts of dyes in mixtures | |
| Saviello et al. | Plasmonic colloidal pastes for surface-enhanced Raman spectroscopy (SERS) of historical felt-tip pens | |
| Guilherme et al. | Synchrotron micro-XRF with Compound Refractive Lenses (CRLs) for tracing key elements on Portuguese glazed ceramics | |
| CN107957414A (en) | A kind of method with potassium bromide quenching fluorescence in Raman spectrum | |
| King et al. | The use of longwave reflected UV imaging for the enhancement of cyanoacrylate developed fingermarks: A simple, safe and effective imaging tool | |
| Worobiec et al. | Damage and molecular changes under a laser beam in SEM‐EDX/MRS interface: a case study on iron‐rich particles |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |