CN107917893A - Load sample component and tera-hertz spectra test method for terahertz light spectrometry - Google Patents
Load sample component and tera-hertz spectra test method for terahertz light spectrometry Download PDFInfo
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- CN107917893A CN107917893A CN201711166183.4A CN201711166183A CN107917893A CN 107917893 A CN107917893 A CN 107917893A CN 201711166183 A CN201711166183 A CN 201711166183A CN 107917893 A CN107917893 A CN 107917893A
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- 238000010998 test method Methods 0.000 title claims abstract description 17
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- 238000001179 sorption measurement Methods 0.000 claims abstract description 106
- 239000012488 sample solution Substances 0.000 claims abstract description 39
- 239000000020 Nitrocellulose Substances 0.000 claims abstract description 29
- 229920001220 nitrocellulos Polymers 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000010521 absorption reaction Methods 0.000 claims abstract description 16
- 238000012360 testing method Methods 0.000 claims description 77
- FJWGYAHXMCUOOM-QHOUIDNNSA-N [(2s,3r,4s,5r,6r)-2-[(2r,3r,4s,5r,6s)-4,5-dinitrooxy-2-(nitrooxymethyl)-6-[(2r,3r,4s,5r,6s)-4,5,6-trinitrooxy-2-(nitrooxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-3,5-dinitrooxy-6-(nitrooxymethyl)oxan-4-yl] nitrate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O)O[C@H]1[C@@H]([C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@@H](CO[N+]([O-])=O)O1)O[N+]([O-])=O)CO[N+](=O)[O-])[C@@H]1[C@@H](CO[N+]([O-])=O)O[C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O FJWGYAHXMCUOOM-QHOUIDNNSA-N 0.000 claims description 26
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 13
- 229910052802 copper Inorganic materials 0.000 claims description 13
- 239000010949 copper Substances 0.000 claims description 13
- 238000000862 absorption spectrum Methods 0.000 claims description 10
- 230000005684 electric field Effects 0.000 claims description 10
- 229910052742 iron Inorganic materials 0.000 claims description 8
- 230000001681 protective effect Effects 0.000 claims description 8
- 238000012545 processing Methods 0.000 claims description 6
- 238000010926 purge Methods 0.000 claims description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 5
- 229910052737 gold Inorganic materials 0.000 claims description 5
- 239000010931 gold Substances 0.000 claims description 5
- 229910052709 silver Inorganic materials 0.000 claims description 5
- 239000004332 silver Substances 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 13
- 229920000573 polyethylene Polymers 0.000 abstract description 11
- 239000004698 Polyethylene Substances 0.000 abstract description 8
- -1 polyethylene Polymers 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 6
- 239000012528 membrane Substances 0.000 abstract description 6
- 239000000843 powder Substances 0.000 abstract description 5
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- 230000000712 assembly Effects 0.000 description 42
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- 229910021641 deionized water Inorganic materials 0.000 description 8
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- 239000000203 mixture Substances 0.000 description 8
- SPFMQWBKVUQXJV-BTVCFUMJSA-N (2r,3s,4r,5r)-2,3,4,5,6-pentahydroxyhexanal;hydrate Chemical compound O.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O SPFMQWBKVUQXJV-BTVCFUMJSA-N 0.000 description 6
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 description 6
- 229930091371 Fructose Natural products 0.000 description 6
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 238000001328 terahertz time-domain spectroscopy Methods 0.000 description 2
- YCIHPQHVWDULOY-FMZCEJRJSA-N (4s,4as,5as,6s,12ar)-4-(dimethylamino)-1,6,10,11,12a-pentahydroxy-6-methyl-3,12-dioxo-4,4a,5,5a-tetrahydrotetracene-2-carboxamide;hydrochloride Chemical compound Cl.C1=CC=C2[C@](O)(C)[C@H]3C[C@H]4[C@H](N(C)C)C(=O)C(C(N)=O)=C(O)[C@@]4(O)C(=O)C3=C(O)C2=C1O YCIHPQHVWDULOY-FMZCEJRJSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
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- 238000003818 flash chromatography Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000001471 micro-filtration Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012120 mounting media Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
Classifications
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- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3581—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using far infrared light; using Terahertz radiation
- G01N21/3586—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using far infrared light; using Terahertz radiation by Terahertz time domain spectroscopy [THz-TDS]
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- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (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)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The present invention relates to a kind of load sample component and tera-hertz spectra test method for terahertz light spectrometry.A kind of load sample component for terahertz light spectrometry includes：Supporting layer, first adsorption layer and the second adsorption layer；Supporting layer is located between first adsorption layer and the second adsorption layer so that first adsorption layer forms the gap of 0.2mm~0.5mm with the second adsorption layer；First adsorption layer and the second adsorption layer are nitrocellulose filter.Above-mentioned load sample component and tera-hertz spectra test method for terahertz light spectrometry is close due to the absorption coefficient of nitrocellulose filter and the absorption coefficient of polythene material, it can be adapted for terahertz light spectrometry completely, and use nitrocellulose filter need to only be added dropwise a small amount of sample solution as adsorption layer on adsorption layer and can be tested, avoid the method for making sample using polyethylene powders pressed disc method or polyvinylidene difluoride membrane impregnated sample solution, required sample size is few, sample consumption is small, can be adapted for detection during less sample.
Description
Technical field
The present invention relates to Terahertz detection technique field, more particularly to the load sample component for terahertz light spectrometry and
Tera-hertz spectra test method.
Background technology
THz wave refers to electromagnetic wave of the frequency in the range of 0.1-10THz, between microwave and it is infrared between, due to terahertz
Hereby vibration and rotation mode of the ripple to organic molecule is sensitive, and the tera-hertz spectra of material has fingerprint, and terahertz time-domain
The tera-hertz spectra that spectral technique can obtain amplitude and phase information, informative, and material at the same time is the fingerprint of material
Spectrum, has the characteristics that high permeability, low energy, instantaneity, acuteness, high s/n ratio, these features cause the lossless inspection of Terahertz
Survey technology has critically important application in many methods such as biomedicine, biochemistry, chemical industry.
At present, the method that Terahertz Technology prepares sample is mainly powder pressing method, and this method is although easy to operate, but powder
Broken sifting step spent time is longer, and sample size is larger needed for tabletting, at least needs 10mg samples to be mixed with polyethylene and presses
Piece (a diameter of round thin slices of 13mm), it is unsuitable for trace sample pressed disc method.
Terahertz Technology detection method for fluid sample is mainly liquid cell method.It is public disclosed in 2 days October in 2013
" using terahertz time-domain spectroscopy detecting the contet of sulphate, the method for nitrate solution concentration " patent that the number of opening is 103335976A, makes
It is polyethylene-liquid pond, detection sample concentration is 4%-18%；Disclosed in 1 day January in 2014, Publication No.
A kind of " terahertz time-domain spectroscopy method for quantitatively detecting quadracycline solution " patent of 103487399A, uses poly- inclined
Fluoride films, sample detection methods are immersed in solution example for polyvinylidene difluoride membrane, and detection sample concentration is
0.01%-2%.In summary, method for making sample limits in currently used Terahertz detection, and required sample is more, and sample consumes
Amount is big, be not suitable for sample it is less when detection.
The content of the invention
Based on this, it is necessary to which method for making sample limits in being detected for currently used Terahertz, and required sample is more, sample
A kind of the problem of consumption is big, there is provided load sample component and tera-hertz spectra test method for terahertz light spectrometry.
A kind of load sample component for terahertz light spectrometry, including：Supporting layer, first adsorption layer and the second adsorption layer；
The supporting layer is located between the first adsorption layer and second adsorption layer so that the first adsorption layer
The gap of 0.2mm~0.5mm is formed with second adsorption layer；
The first adsorption layer and second adsorption layer are nitrocellulose filter.
In a wherein embodiment, offered on the supporting layer sample well cause the first adsorption layer with it is described
Second adsorption layer is arranged at intervals.
In a wherein embodiment, the first fixed bed and the second fixed bed are further included, described first fixes layer stackup
In surface of the first adsorption layer away from the supporting layer, second fixed bed is laminated in second adsorption layer away from institute
State the surface of supporting layer；
The first test window is offered on first fixed bed, the second testing window is offered on second fixed bed
Mouthful, first test window is communicated with second test window with the sample well.
In a wherein embodiment, the thickness of first fixed bed and second fixed bed is respectively 0.2mm
~0.5mm.
In a wherein embodiment, the aperture of the nitrocellulose filter is 0.1 μm~0.65 μm.
In a wherein embodiment, the supporting layer is copper sheet, iron plate, silver strip or gold plaque.
A kind of tera-hertz spectra test method, comprises the following steps：
Weigh the sample preparation that is added to the water and obtain sample solution；
Above-mentioned load sample component is positioned in terahertz light spectrometer, and under the purging of protective gas, is carried out unloaded
Test obtains reference signal；
The sample solution is added drop-wise on the load sample component；
Under the purging of protective gas, had using terahertz light spectrometer to dropwise addition the load sample component of sample solution into
Row test obtains sample signal；
The Terahertz absorption spectra of the sample is obtained by the reference signal and the sample signal.
In a wherein embodiment, the terahertz light spectrometer is the model TPS-4000's of Teraview companies
Terahertz light spectrometer；Terahertz spectrum width is 0.06THz~4.0THz；In the scanning process of signal, scanning range for 0~
1200ps, acquisition rate 30scans/s, the resolution ratio of tera-hertz spectra is 1.2cm-1。
It is described that the sample is obtained by the reference signal and the sample signal in a wherein embodiment
The step of Terahertz absorption spectra, includes：
The progress Fast Fourier Transform (FFT) of the Time Domain Spectrum of the reference signal and the sample signal is obtained described with reference to letter
Number and the sample signal frequency domain spectra, the formula for carrying out the Fast Fourier Transform (FFT) is：
Er (ω)=Ar (ω) exp [- i φ r (ω)]=∫ Er (t) exp (- i ω t) dt；
Es (ω)=As (ω) exp [- i φ s (ω)]=∫ Es (t) exp (- i ω t) dt；
Wherein, ω is wave frequency, and t is the time, and i is imaginary unit；Er (t) be reference signal time-domain signal, Es
(t) it is the time-domain signal of sample signal；Er (ω) is the frequency-region signal of reference signal, and Es (ω) is that the frequency domain of sample signal is believed
Number；Ar (ω) is the amplitude of reference signal electric field, and As (ω) is the amplitude of sample signal electric field；φ r (ω) are reference signal electricity
The phase of field, φ s (ω) are the phase of sample signal electric field；
Again using the refractive index n (ω) and absorption coefficient of the data processing model extraction sample based on fresnel formula
(ω), the formula of the data processing model based on fresnel formula are：
Wherein, ρ (ω) is the ratio of sample signal and the amplitude of reference signal, and φ (ω) is sample signal and reference signal
Phase difference, d be sample thickness, c is the spread speed of electromagnetic wave in a vacuum.
In a wherein embodiment, the concentration of the sample solution is 0.1g/mL~2g/mL.
Above-mentioned load sample component and tera-hertz spectra test method for terahertz light spectrometry is spaced using two layers
The nitrocellulose filter of setting is used to adsorb test sample, due to the suction of the absorption coefficient and polythene material of nitrocellulose filter
Coefficient similar is received, can be adapted for terahertz light spectrometry completely, and uses two interlamellar spacings fine for the nitric acid of 0.2mm~0.5mm
The plain film of dimension, which combines, to be formed adsorption layer a small amount of sample solution need to only be added dropwise on adsorption layer, and sample solution can chromatograph cellulose nitrate
Between the hole of plain film or between the gap of two layers of nitrocellulose filter, you can tested, even if the concentration of sample solution or
Sample size is less, also can accurately be tested, and avoids using polyethylene powders pressed disc method or polyvinylidene difluoride membrane
The method for making sample of impregnated sample solution, required sample size is few, and sample consumption is small, can be adapted for detection during less sample.
Brief description of the drawings
Fig. 1 is the sectional view of the load sample component for terahertz light spectrometry of an embodiment；
Fig. 2 is the decomposition diagram of the load sample component for terahertz light spectrometry shown in Fig. 1；
Fig. 3 is the flow chart of the tera-hertz spectra test method of an embodiment；
Fig. 4 is the Terahertz absorption spectra of Sample assemblies A, Sample assemblies B, Sample assemblies C and Sample assemblies D；
The Terahertz that Fig. 5 is Sample assemblies E, Sample assemblies F, Sample assemblies G, Sample assemblies H and Sample assemblies I absorbs
Spectrum；
The Terahertz that Fig. 6 is Sample assemblies J, Sample assemblies K, Sample assemblies L, Sample assemblies M and Sample assemblies N absorbs
Spectrum.
Embodiment
Below in conjunction with embodiment and attached drawing to the load sample component and terahertz light for terahertz light spectrometry
Spectrum test method is described in further detail.
Please refer to Fig.1 and Fig. 2, the load sample component 100 for terahertz light spectrometry of an embodiment include first and inhale
Attached layer 110, the second adsorption layer 120, supporting layer 130, the first fixed bed 140 and the second fixed bed 150.
In the illustrated embodiment, 110 and second adsorption layer 120 of first adsorption layer is respectively laminated structure.First inhales
Attached 110 and second adsorption layer 120 of layer is nitrocellulose filter (nitrocellulose filter membrane, abbreviation NC
Film).
Nitrocellulose filter is a kind of microfiltration membranes of people's early start research.NC films have certain hydrophily but insoluble
Yu Shui, dissolves in some relatively common organic solvents (acetone etc.), and is slightly soluble in alcohols.It is with good property after film forming
Can, NC films have the characteristic of flash chromatography.
In a wherein embodiment, nitrocellulose filter is selected from the nothing of the Whatman brands of GE medical treatment life sciences
Bacterial type nitrocellulose filter or non-sterile type nitrocellulose filter.
In a wherein embodiment, the thickness of first adsorption layer 110 is 100 μm~110 μm, it is preferred that first inhales
The thickness of attached layer 110 is 100 μm.The aperture of first adsorption layer 110 is 0.1 μm~0.65 μm.Preferably, first adsorption layer 110
Aperture be 0.1 μm, 0.2 μm, 0.45 μm or 0.65 μm.It is furthermore preferred that the aperture of first adsorption layer 110 is 0.2 μm or 0.45 μ
m。
In a wherein embodiment, the thickness of the second adsorption layer 120 is 100 μm~110 μm, it is preferred that second inhales
The thickness of attached layer 120 is 100 μm.The aperture of second adsorption layer 120 is 0.1 μm~0.65 μm.Preferably, the second adsorption layer 120
Aperture be 0.1 μm, 0.2 μm, 0.45 μm or 0.65 μm.It is furthermore preferred that the aperture of the second adsorption layer 120 is 0.2 μm or 0.45 μ
m。
In the illustrated embodiment, supporting layer 130 is folded between 110 and second adsorption layer 120 of first adsorption layer, from
And cause 110 and second adsorption layer of first adsorption layer, 120 face and interval setting.
Further, in the illustrated embodiment, supporting layer 130 is also laminated structure, and sample is equipped with supporting layer 130
Sample wells 131, sample well 131 is through supporting layer 130 so that 110 and second adsorption layer of first adsorption layer, 120 face and interval setting.
The hole wall of first adsorption layer 110, the second adsorption layer 120 and sample well 131 forms a test position.
In the illustrated embodiment, 3 spaced sample wells are offered on supporting layer 130, corresponding first inhales
The quantity of attached 110 and second adsorption layer 120 of layer is also respectively 3, so as to form 3 test positions so that above-mentioned to be used for Terahertz
The load sample component of spectral measurement can once carry out the detection of 3 samples.Certainly, in other embodiments, sample well 131,
The quantity of 110 and second adsorption layer 120 of first adsorption layer can also be any amount that other are no less than 1.
In a wherein embodiment, supporting layer 130 is highly heat-conductive material, specifically, supporting layer 130 be selected from copper sheet,
Iron plate, silver strip or gold plaque.Consider from testing cost, it is preferred that supporting layer 130 is copper sheet or iron plate.
In a wherein embodiment, the thickness of supporting layer 130 is 0.2mm~0.5mm.
Further so that the spacing of 110 and second adsorption layer 120 of first adsorption layer is 0.2mm~0.5mm.
In a wherein embodiment, the sample well 131 on supporting layer 130 is circular hole, sample well 131 it is a diameter of
5mm~12mm.It is understood that in other embodiments, sample well 131 can also be square hole, or it is any other not
Regular shape.
In the illustrated embodiment, the first fixed bed 140 is laminated in table of the first adsorption layer 110 away from supporting layer 130
Face.
In a wherein embodiment, the first fixed bed 140 is sheet.First fixed bed 140 be selected from copper sheet, iron plate,
Silver strip or gold plaque.Preferably, the first fixed bed 140 is copper sheet or iron plate.
In a wherein embodiment, the thickness of the first fixed bed 140 is 0.2mm~0.5mm.
In a wherein embodiment, the first test window 141 is offered on the first fixed bed 140.First testing window
Mouth 141 runs through the first fixed bed 140.In the illustrated embodiment, the first test window 141 is circular hole, the first test window
141 a diameter of 5mm~12mm.It is understood that in other embodiments, the first test window 141 can also be side
Hole, or any other irregular shape.
In a wherein embodiment, the second fixed bed 150 is laminated in the second adsorption layer 120 away from supporting layer 130
Surface.
In a wherein embodiment, the second fixed bed 150 is sheet.Second fixed bed 150 be selected from copper sheet, iron plate,
Silver strip or gold plaque.Preferably, the second fixed bed 150 is copper sheet or iron plate.
In a wherein embodiment, the thickness of the second fixed bed 150 is 0.2mm~0.5mm.
In a wherein embodiment, the second test window 151 is offered on the second fixed bed 150.Second testing window
Mouth 151 runs through the second fixed bed 150.In the illustrated embodiment, the second test window 151 is circular hole, the second test window
151 a diameter of 5mm~12mm.It is understood that in other embodiments, the second test window 151 can also be side
Hole, or any other irregular shape.
In the illustrated embodiment, the first test window 141, the second test window 151 are set with 131 face of sample well
Put.Preferably, the positive throwing of the first test window mouth 141, the second test window 151 and sample well 131 in first adsorption layer 110
Shadow can be completely superposed.
It should be noted that in the illustrated embodiment, the number of the first test window 141 and the second test window 151
Amount is also respectively 3, and three sample wells 131, the first test window 141 and the second test window 151 are correspondingly formed three respectively
A test position.It is understood that the quantity of the first test window 141 and the second test window 151 can be no less than one
Any amount.
Above-mentioned load sample component and tera-hertz spectra test method for terahertz light spectrometry is spaced using two layers
The nitrocellulose filter of setting is used to adsorb test sample, due to the suction of the absorption coefficient and polythene material of nitrocellulose filter
Coefficient similar is received, can be adapted for terahertz light spectrometry completely, and uses two interlamellar spacings fine for the nitric acid of 0.2mm~0.5mm
The plain film of dimension, which combines, to be formed adsorption layer a small amount of sample solution need to only be added dropwise on adsorption layer, and solution can chromatograph nitrocellulose filter
Gap between or the gap of two layers of nitrocellulose filter between, you can tested, even if the concentration or sample of sample solution
Measure less, can accurately be tested, and avoid and impregnated using polyethylene powders pressed disc method or polyvinylidene difluoride membrane
The method for making sample of sample solution, required sample size is few, and sample consumption is small, can be adapted for detection during less sample.
It should be noted that in other embodiments, the first fixed bed 140 and the second fixed bed 150 can be omitted.
Further referring to Fig. 3, the tera-hertz spectra test method of an embodiment comprises the following steps：
S110, weigh the sample preparation that is added to the water and obtain sample solution.
In a wherein embodiment, sample can be the carbohydrate and other water-soluble substanceses of good water solubility.
In a wherein embodiment, after sample is added to the water using be vortexed stir by the way of stir it is complete to sample
Fully dissolved is in water.The rotating speed being vortexed when stirring is 2000rpm~2500rpm, and the time of vortex is 2min~3min.
In a wherein embodiment, the concentration of the sample solution of preparation is 0.1g/mL~2g/mL.
Load sample component, be positioned in terahertz light spectrometer by S120, and under the purging of protective gas, carries out unloaded survey
Examination obtains reference signal.
In a wherein embodiment, terahertz light spectrometer is the terahertz of the model TPS-4000 of Teraview companies
Hereby spectrometer；Terahertz spectrum width is 0.06THz~4.0THz；In the scanning process of signal, scanning range is 0~1200ps,
Acquisition rate is 30scans/s, and the resolution ratio of tera-hertz spectra is 1.2cm-1。
In a wherein embodiment, protective gas is selected from least one of nitrogen, argon gas and helium.
Sample solution, be added drop-wise on load sample component by S130.
In a wherein embodiment, the dosage of the sample solution being added drop-wise on load sample component is the μ L of 15 μ L~30.It is excellent
Choosing, it is added drop-wise to using micropipettor pipette samples solution on load sample component.
In a wherein embodiment, sample solution be added drop-wise to after load sample component at 15 DEG C~30 DEG C place 5min~
15min so that sample chromatography completely is into the gap of nitrocellulose filter.
S140, under the purging of protective gas, have the load sample component of sample solution to dropwise addition using terahertz light spectrometer
Tested to obtain sample signal.
In a wherein embodiment, terahertz light spectrometer is the terahertz of the model TPS-4000 of Teraview companies
Hereby spectrometer；Terahertz spectrum width is 0.06THz~4.0THz；In the scanning process of signal, scanning range is 0~1200ps,
Acquisition rate is 30scans/s, and the resolution ratio of tera-hertz spectra is 1.2cm-1。
In a wherein embodiment, protective gas is selected from least one of nitrogen, argon gas and helium.
S150, obtain the Terahertz absorption spectra of sample by reference to signal and sample signal.
In a wherein embodiment, the tool of the Terahertz absorption spectra of sample is obtained by reference to signal and sample signal
Body step includes：
S151, by the Time Domain Spectrum of reference signal and sample signal progress Fast Fourier Transform (FFT) obtain reference signal and sample
The frequency domain spectra of signal.
In a wherein embodiment, the formula for carrying out Fast Fourier Transform (FFT) is：
Er (ω)=Ar (ω) exp [- i φ r (ω)]=∫ Er (t) exp (- i ω t) dt；
Es (ω)=As (ω) exp [- i φ s (ω)]=∫ Es (t) exp (- i ω t) dt；
Wherein, ω is wave frequency, and t is the time, and i is imaginary unit；Er (t) be reference signal time-domain signal, Es
(t) it is the time-domain signal of sample signal；Er (ω) is the frequency-region signal of reference signal, and Es (ω) is that the frequency domain of sample signal is believed
Number；Ar (ω) is the amplitude of reference signal electric field, and As (ω) is the amplitude of sample signal electric field；φ r (ω) are reference signal electricity
The phase of field, φ s (ω) are the phase of sample signal electric field.
S152, again the refractive index n (ω) using the data processing model extraction sample based on fresnel formula and absorption system
Number α (ω).
In a wherein embodiment, the formula of the data processing model based on fresnel formula is：
Wherein, ρ (ω) is the ratio of sample signal and the amplitude of reference signal, and φ (ω) is sample signal and reference signal
Phase difference, d be sample thickness, c is the spread speed of electromagnetic wave in a vacuum.
Above-mentioned tera-hertz spectra test method, is used to adsorb and tests using the nitrocellulose filter of two layers of spaced setting
Sample, can be suitable for detection during less sample, and test accuracy is high, and detection limit is low.
Below in conjunction with specific embodiment to the load sample component for terahertz light spectrometry and tera-hertz spectra test side
Method illustrates.
Embodiment 1
(1) the Sample assemblies A for being used for tera-hertz spectra test is prepared, including：First adsorption layer, the second adsorption layer, sandwiched
Supporting layer between first adsorption layer and the second adsorption layer, surface stacking first of the first adsorption layer away from supporting layer are fixed
Layer, surface of second adsorption layer away from supporting layer are laminated the second fixed bed；Sample well is opened up on supporting layer, is opened on the first fixed bed
If the first test window, the second test window is opened up on the second fixed bed.
Wherein, supporting layer, the first fixed bed and the second fixed bed be thickness be 0.32mm copper sheet, first adsorption layer and
Second adsorption layer is that thickness is 100 μm, and aperture is 0.1 μm of nitrocellulose filter, sample well, the first test window and second
Test window is the circular hole of a diameter of 8mm, and sample well, the first test window and the second test window face are set.
(2) the Sample assemblies B for being used for tera-hertz spectra test is prepared, including：First adsorption layer, the second adsorption layer, sandwiched
Supporting layer between first adsorption layer and the second adsorption layer, surface stacking first of the first adsorption layer away from supporting layer are fixed
Layer, surface of second adsorption layer away from supporting layer are laminated the second fixed bed；Sample well is opened up on supporting layer, is opened on the first fixed bed
If the first test window, the second test window is opened up on the second fixed bed.
Wherein, supporting layer, the first fixed bed and the second fixed bed be thickness be 0.32mm copper sheet, first adsorption layer and
Second adsorption layer is that thickness is 100 μm, and aperture is 0.2 μm of nitrocellulose filter, sample well, the first test window and second
Test window is the circular hole of a diameter of 8mm, and sample well, the first test window and the second test window face are set.
(3) the Sample assemblies C for being used for tera-hertz spectra test is prepared, including：First adsorption layer, the second adsorption layer, sandwiched
Supporting layer between first adsorption layer and the second adsorption layer, surface stacking first of the first adsorption layer away from supporting layer are fixed
Layer, surface of second adsorption layer away from supporting layer are laminated the second fixed bed；Sample well is opened up on supporting layer, is opened on the first fixed bed
If the first test window, the second test window is opened up on the second fixed bed.
Wherein, supporting layer, the first fixed bed and the second fixed bed be thickness be 0.32mm copper sheet, first adsorption layer and
Second adsorption layer is that thickness is 100 μm, and aperture is 0.45 μm of nitrocellulose filter, sample well, the first test window and the
Two test windows are the circular hole of a diameter of 8mm, and sample well, the first test window and the second test window face are set.
(4) the Sample assemblies D for being used for tera-hertz spectra test is prepared, the polyethylene for accurately weighing 22mg is formed by tabletting
A diameter of 13mm, thickness are the disk of 0.2mm.
(5) Sample assemblies A, Sample assemblies B, Sample assemblies C and Sample assemblies D are put into terahertz light spectrometer and are surveyed
Examination obtains Terahertz absorption spectra, as shown in Figure 4.
From fig. 4, it can be seen that the absorption coefficient of nitrocellulose filter and polyethylene approaches, sample test is suitable as
Mounting medium.
Embodiment 2
(1) four load sample components are obtained, including：First adsorption layer, the second adsorption layer, be located in first adsorption layer and second
Supporting layer between adsorption layer, surface of the first adsorption layer away from supporting layer are laminated the first fixed bed, and the second adsorption layer is away from branch
The surface for supportting layer is laminated the second fixed bed；Sample well is opened up on supporting layer, opens up the first test window on the first fixed bed, second
The second test window is opened up on fixed bed.
Wherein, supporting layer, the first fixed bed and the second fixed bed be thickness be 0.5mm copper sheet, first adsorption layer and
Second adsorption layer is that thickness is 100 μm, and aperture is 0.2 μm of nitrocellulose filter, sample well, the first test window and second
Test window is the circular hole of a diameter of 12mm, and sample well, the first test window and the second test window face are set.
(2) the accurate Dextrose Monohydrate for weighing 2mg, the deionized water for adding 20 μ L thereto mix and prepared by the 30s that is vortexed
The sample solution that concentration is 0.1g/mL is obtained, the sample solution that 20 μ L are drawn with micropipettor is added drop-wise to a load sample component
On obtain Sample assemblies E.
(3) the accurate Dextrose Monohydrate for weighing 4mg, the deionized water for adding 20 μ L thereto mix and prepared by the 30s that is vortexed
The sample solution that concentration is 0.2g/mL is obtained, the sample solution that 20 μ L are drawn with micropipettor is added drop-wise to a load sample component
On obtain Sample assemblies F.
(4) the accurate Dextrose Monohydrate for weighing 6mg, the deionized water for adding 20 μ L thereto mix and prepared by the 30s that is vortexed
The sample solution that concentration is 0.3g/mL is obtained, the sample solution that 20 μ L are drawn with micropipettor is added drop-wise to a load sample component
On obtain Sample assemblies G.
(5) the accurate Dextrose Monohydrate for weighing 8mg, the deionized water for adding 20 μ L thereto mix and prepared by the 30s that is vortexed
The sample solution that concentration is 0.4g/mL is obtained, the sample solution that 20 μ L are drawn with micropipettor is added drop-wise to a load sample component
On obtain Sample assemblies H.
(6) the accurate polyethylene for weighing the Dextrose Monohydrate of 25mg and adding 175mg is formed by tabletting after mixing
A diameter of 13mm, thickness are the disk of 1.5mm, obtain Sample assemblies I.
(7) Sample assemblies E, Sample assemblies F, Sample assemblies G, Sample assemblies H and Sample assemblies I are put into tera-hertz spectra
Tested to obtain Terahertz absorption spectra in instrument, as shown in Figure 5.
NC films test result is consistent with tabletting result as can be seen from Figure 5, and Dextrose Monohydrate characteristic absorption peak is 1.80T
(59cm-1)、1.98T(65cm-1)、2.36T(78cm-1)、2.42T(81cm-1), sample absorption intensity with quality increase by
Gradually improve.
Embodiment 3
(1) four load sample components are obtained, including：First adsorption layer, the second adsorption layer, be located in first adsorption layer and second
Supporting layer between adsorption layer, surface of the first adsorption layer away from supporting layer are laminated the first fixed bed, and the second adsorption layer is away from branch
The surface for supportting layer is laminated the second fixed bed；Sample well is opened up on supporting layer, opens up the first test window on the first fixed bed, second
The second test window is opened up on fixed bed.
Wherein, supporting layer, the first fixed bed and the second fixed bed be thickness be 0.2mm copper sheet, first adsorption layer and
Second adsorption layer is that thickness is 100 μm, and aperture is 0.0.45 μm of nitrocellulose filter, sample well, the first test window and
Second test window is the circular hole of a diameter of 10mm, and sample well, the first test window and the second test window face are set.
(2) the accurate fructose for weighing 2mg, add thereto 20 μ L deionized water mix and the 30s that is vortexed be prepared it is dense
The sample solution for 0.1g/mL is spent, is added drop-wise on a load sample component and obtained with the sample solution of 20 μ L of micropipettor absorption
Sample assemblies J.
(3) the accurate fructose for weighing 4mg, add thereto 20 μ L deionized water mix and the 30s that is vortexed be prepared it is dense
The sample solution for 0.2g/mL is spent, is added drop-wise on a load sample component and obtained with the sample solution of 20 μ L of micropipettor absorption
Sample assemblies K.
(4) the accurate fructose for weighing 6mg, add thereto 20 μ L deionized water mix and the 30s that is vortexed be prepared it is dense
The sample solution for 0.3g/mL is spent, is added drop-wise on a load sample component and obtained with the sample solution of 20 μ L of micropipettor absorption
Sample assemblies L.
(5) the accurate fructose for weighing 8mg, add thereto 20 μ L deionized water mix and the 30s that is vortexed be prepared it is dense
The sample solution for 0.4g/mL is spent, is added drop-wise on a load sample component and obtained with the sample solution of 20 μ L of micropipettor absorption
Sample assemblies M.
(6) the accurate polyethylene for weighing the fructose of 50mg and adding 150mg is formed a diameter of by tabletting after mixing
13mm, thickness are the disk of 1.5mm, obtain Sample assemblies N.
(7) Sample assemblies J, Sample assemblies K, Sample assemblies L, Sample assemblies M and Sample assemblies N are put into tera-hertz spectra
Tested to obtain Terahertz absorption spectra in instrument, as shown in Figure 6.
For NC films test result with also consistent with tabletting result, fructose characteristic absorption peak is 1.68T as can be seen from Figure 6
(56cm-1)、2.12T(71cm-1), sample absorption intensity is gradually stepped up with the increase of quality.
Each technical characteristic of embodiment described above can be combined arbitrarily, to make description succinct, not to above-mentioned reality
Apply all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, the scope that this specification is recorded all is considered to be.
Embodiment described above only expresses the several embodiments of the present invention, its description is more specific and detailed, but simultaneously
Cannot therefore it be construed as limiting the scope of the patent.It should be pointed out that come for those of ordinary skill in the art
Say, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention
Scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
- A kind of 1. load sample component for terahertz light spectrometry, it is characterised in that including：Supporting layer, first adsorption layer and Two adsorption layers；The supporting layer is located between the first adsorption layer and second adsorption layer so that the first adsorption layer and institute State the gap that the second adsorption layer forms 0.2mm~0.5mm；The first adsorption layer and second adsorption layer are nitrocellulose filter.
- 2. the load sample component according to claim 1 for terahertz light spectrometry, it is characterised in that on the supporting layer Offering sample well causes the first adsorption layer to be arranged at intervals with second adsorption layer.
- 3. the load sample component according to claim 2 for terahertz light spectrometry, it is characterised in that it is solid to further include first Given layer and the second fixed bed, first fixed bed is laminated in surface of the first adsorption layer away from the supporting layer, described Second fixed bed is laminated in the surface of second adsorption layer away from the supporting layer；The first test window is offered on first fixed bed, the second test window, institute are offered on second fixed bed The first test window is stated to communicate with the sample well with second test window.
- 4. the load sample component according to claim 3 for terahertz light spectrometry, it is characterised in that described first fixes The thickness of layer and second fixed bed is respectively 0.2mm~0.5mm.
- 5. the load sample component according to claim 1 for terahertz light spectrometry, it is characterised in that the cellulose nitrate The aperture of plain film is 0.1 μm~0.65 μm.
- 6. the load sample component according to claim 1 for terahertz light spectrometry, it is characterised in that the supporting layer is Copper sheet, iron plate, silver strip or gold plaque.
- 7. a kind of tera-hertz spectra test method, it is characterised in that comprise the following steps：Weigh the sample preparation that is added to the water and obtain sample solution；It will be positioned over such as claim 1~6 any one of them load sample component in terahertz light spectrometer, and in protective gas Under purging, carry out no load test and obtain reference signal；The sample solution is added drop-wise on the load sample component；Under the purging of protective gas, the load sample component for having sample solution to dropwise addition using terahertz light spectrometer is surveyed Examination obtains sample signal；The Terahertz absorption spectra of the sample is obtained by the reference signal and the sample signal.
- 8. tera-hertz spectra test method according to claim 7, it is characterised in that the terahertz light spectrometer is The terahertz light spectrometer of the model TPS-4000 of Teraview companies；Terahertz spectrum width is 0.06THz~4.0THz；In signal Scanning process in, scanning range is 0~1200ps, acquisition rate 30scans/s, and the resolution ratio of tera-hertz spectra is 1.2cm-1。
- 9. tera-hertz spectra test method according to claim 7, it is characterised in that it is described by the reference signal and The sample signal, which obtains the step of Terahertz absorption spectra of the sample, to be included：By the Time Domain Spectrum of the reference signal and the sample signal progress Fast Fourier Transform (FFT) obtain the reference signal and The frequency domain spectra of the sample signal, the formula for carrying out the Fast Fourier Transform (FFT) are：Er (ω)=Ar (ω) exp [- i φ r (ω)]=∫ Er (t) exp (- i ω t) dt；Es (ω)=As (ω) exp [- i φ s (ω)]=∫ Es (t) exp (- i ω t) dt；Wherein, ω is wave frequency, and t is the time, and i is imaginary unit；Er (t) is the time-domain signal of reference signal, and Es (t) is The time-domain signal of sample signal；Er (ω) is the frequency-region signal of reference signal, and Es (ω) is the frequency-region signal of sample signal；Ar (ω) is the amplitude of reference signal electric field, and As (ω) is the amplitude of sample signal electric field；φ r (ω) are the phase of reference signal electric field Position, φ s (ω) are the phase of sample signal electric field；Again using the refractive index n (ω) and absorption coefficient (ω) of the data processing model extraction sample based on fresnel formula, institute The formula for stating the data processing model based on fresnel formula is：<mrow> <mi>n</mi> <mrow> <mo>(</mo> <mi>&omega;</mi> <mo>)</mo> </mrow> <mo>=</mo> <mfrac> <mrow> <mi>&phi;</mi> <mrow> <mo>(</mo> <mi>&omega;</mi> <mo>)</mo> </mrow> <mi>c</mi> </mrow> <mrow> <mi>&omega;</mi> <mi>d</mi> </mrow> </mfrac> <mo>+</mo> <mn>1</mn> <mo>;</mo> </mrow><mrow> <mi>&alpha;</mi> <mrow> <mo>(</mo> <mi>&omega;</mi> <mo>)</mo> </mrow> <mo>=</mo> <mfrac> <mn>2</mn> <mi>d</mi> </mfrac> <mi>l</mi> <mi>n</mi> <mo>{</mo> <mfrac> <mrow> <mn>4</mn> <mi>n</mi> <mrow> <mo>(</mo> <mi>&omega;</mi> <mo>)</mo> </mrow> </mrow> <mrow> <mi>&rho;</mi> <mrow> <mo>(</mo> <mi>&omega;</mi> <mo>)</mo> </mrow> <msup> <mrow> <mo>&lsqb;</mo> <mi>n</mi> <mrow> <mo>(</mo> <mi>&omega;</mi> <mo>)</mo> </mrow> <mo>+</mo> <mn>1</mn> <mo>&rsqb;</mo> </mrow> <mn>2</mn> </msup> </mrow> </mfrac> <mo>}</mo> <mo>;</mo> </mrow>Wherein, ρ (ω) is the ratio of sample signal and the amplitude of reference signal, and φ (ω) is the phase of sample signal and reference signal Potential difference, d are the thickness of sample, and c is the spread speed of electromagnetic wave in a vacuum.
- 10. tera-hertz spectra test method according to claim 7, it is characterised in that the concentration of the sample solution is 0.1g/mL~2g/mL.
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| PCT/CN2018/080594 WO2019100630A1 (en) | 2017-11-21 | 2018-03-27 | Sample loading assembly for terahertz spectroscopic measurement, and terahertz spectroscopic test method |
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| WO2019100630A1 (en) * | 2017-11-21 | 2019-05-31 | 深圳市太赫兹科技创新研究院 | Sample loading assembly for terahertz spectroscopic measurement, and terahertz spectroscopic test method |
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| CN112816434A (en) * | 2020-12-30 | 2021-05-18 | 首都师范大学 | Terahertz wave concentration detection kit |
| CN114264627A (en) * | 2021-12-20 | 2022-04-01 | 河南工业大学 | Terahertz sensor and using method thereof |
| CN114778481B (en) * | 2022-03-22 | 2024-01-09 | 首都师范大学 | Micrometer sensor based on terahertz metamaterial and detection method |
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