CN106872386A - A kind of solid-phase extraction device suitable for the measurement of online transmission mode - Google Patents
A kind of solid-phase extraction device suitable for the measurement of online transmission mode Download PDFInfo
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- CN106872386A CN106872386A CN201710038406.2A CN201710038406A CN106872386A CN 106872386 A CN106872386 A CN 106872386A CN 201710038406 A CN201710038406 A CN 201710038406A CN 106872386 A CN106872386 A CN 106872386A
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- solid
- container
- extraction device
- phase extraction
- glass
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- 238000002414 normal-phase solid-phase extraction Methods 0.000 title claims abstract description 42
- 230000005540 biological transmission Effects 0.000 title claims abstract description 27
- 238000005259 measurement Methods 0.000 title claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 43
- 238000001514 detection method Methods 0.000 claims abstract description 23
- 239000011521 glass Substances 0.000 claims abstract description 22
- 238000001228 spectrum Methods 0.000 claims abstract description 19
- 239000007790 solid phase Substances 0.000 claims abstract description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000003595 spectral effect Effects 0.000 claims description 14
- 239000012488 sample solution Substances 0.000 claims description 7
- 239000003365 glass fiber Substances 0.000 claims description 5
- 239000012611 container material Substances 0.000 claims 1
- 230000035945 sensitivity Effects 0.000 abstract description 5
- 238000002211 ultraviolet spectrum Methods 0.000 abstract description 5
- 239000000243 solution Substances 0.000 description 7
- 239000000741 silica gel Substances 0.000 description 6
- 229910002027 silica gel Inorganic materials 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000000862 absorption spectrum Methods 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 229920001429 chelating resin Polymers 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- CQPFMGBJSMSXLP-UHFFFAOYSA-M acid orange 7 Chemical compound [Na+].OC1=CC=C2C=CC=CC2=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 CQPFMGBJSMSXLP-UHFFFAOYSA-M 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- SIXWIUJQBBANGK-UHFFFAOYSA-N 4-(4-fluorophenyl)-1h-pyrazol-5-amine Chemical compound N1N=CC(C=2C=CC(F)=CC=2)=C1N SIXWIUJQBBANGK-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 230000002452 interceptive effect Effects 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N monobenzene Natural products C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 2
- 239000013307 optical fiber Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 238000000411 transmission spectrum Methods 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- ZTKQHJHANLVEBM-UHFFFAOYSA-N 2-[3-(ethylamino)-6-ethylimino-2,7-dimethylxanthen-9-yl]benzoic acid Chemical compound C1=2C=C(C)C(NCC)=CC=2OC2=CC(=NCC)C(C)=CC2=C1C1=CC=CC=C1C(O)=O ZTKQHJHANLVEBM-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- RVPVRDXYQKGNMQ-UHFFFAOYSA-N lead(2+) Chemical compound [Pb+2] RVPVRDXYQKGNMQ-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 125000005498 phthalate group Chemical class 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
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
- G01N21/17—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
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
-
- 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
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
-
- 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
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
- G01N2001/4061—Solvent extraction
Abstract
The invention discloses a kind of solid-phase extraction device suitable for the measurement of online transmission mode.The solid-phase extraction device includes a container；The upper end of the container is set for opening；The lower surface of the container is provided with several through holes；The material of a pair of opposite flanks of the container is glass；The glass can be quartz glass, with adapt to ultraviolet spectra detect the need for.Spectrum is directly determined on enrichment material after carrying out SPE using solid-phase extraction device of the present invention, detection sensitivity and selectivity is improve, operation is simplified.Transmitted spectrum is detected on solid phase material, detection sensitivity is further increased, detection precision is also improved.SPE material source enriches, it is easy to select, applied widely.
Description
Technical field
The present invention relates to a kind of solid-phase extraction device suitable for the measurement of online transmission mode, belong to the sample of analytical chemistry
Pretreatment and field of spectral analysis technology.
Background technology
In technical field of analytical chemistry, solid phase extraction techniques are widely used in sample pre-treatments, its simple to operate, cost
Sensitivity low, that analysis method can be effectively improved and selectivity.Using solid phase material to detected components and interfering component energy of adsorption
The difference of power, solid phase extraction techniques can reach and detected components are enriched with, the purpose for interfering component separate.Under normal circumstances,
Solid phase extraction method is also eluted absorbed component with suitable solvent after concentration and separation operation is completed, and is carried out follow-up
Analysis detection.Therefore need to be improved existing detection method.
The content of the invention
It is an object of the invention to provide a kind of solid-phase extraction device suitable for the measurement of online transmission mode, using the present invention
Solid-phase extraction device, to the measurement of the absorption spectrum of solid phase sample, and with diffusing reflection and can transmit both of which, Transmission Modes
Formula is diffusing transmission pattern, and the spectrum of measurement is diffusing transmission spectrum.
After solid-phase extraction device of the present invention carries out SPE, to solid phase material without its diffuse transmission light of wash-out direct measurement
Spectrum.
Solid-phase extraction device suitable for the measurement of online transmission mode provided by the present invention, it includes a container；
The upper end of the container is set for opening；
The lower surface of the container is provided with several through holes；
The material of a pair of opposite flanks of the container is glass.
In above-mentioned solid-phase extraction device, the container is cube shaped.
In above-mentioned solid-phase extraction device, the glass can be quartz glass, with adapt to ultraviolet spectra detect the need for.
In above-mentioned solid-phase extraction device, the material of other two sides is not limited, and stainless steel or other corrosion resistants such as may be selected
Erosion metal material, glass, ceramics or plastics etc..
In above-mentioned solid-phase extraction device, the spacing between the top and bottom of the container is 50~200mm, i.e., described
The height of container.
In above-mentioned solid-phase extraction device, spacing before with glass as material two sides of the container for 1~
10mm (i.e. inventive container is flat cube shaped), i.e. light path.
In above-mentioned solid-phase extraction device, the material of the lower surface of the container is glass fibre, filter paper or core.
Transmission mode diffuse transmission light spectrum detection method is carried out using the solid-phase extraction device, is comprised the following steps：
SPE material is placed with the container；
The sample solution that component to be measured is contained in the opening set by the upper surface of the container to addition in the container；
After the sample solution flows through the SPE material, the through hole outflow from the lower surface of the container；
Diffusing transmission spectral detection is carried out between with glass as material two sides of the container.
When the sample solution flows through the SPE material, it is tested component and adsorbs on the SPE material,
Other compositions flow out with filtrate, reach the purpose of concentration and separation；After enrichment terminates, you can realize solid phase in the port of clear glass
The measurement of absorption spectrum.
After spectral detection terminates, the SPE material is eluted with suitable solvent, just can be continuing with.
In above-mentioned detection method, the SPE material can use existing conventional fiber material, such as silica gel, resin
Deng.
The above-mentioned tested component of detection method requirement has absorption light property, can be to enrichment on the SPE material
Component carries out UV, visible light, near-infrared diffusing transmission spectral detection.
The invention has the advantages that：
(1) spectrum is directly determined on enrichment material after carrying out SPE using solid-phase extraction device of the present invention, is improved
Detection sensitivity and selectivity, simplify operation.
(2) transmitted spectrum is detected on solid phase material, detection sensitivity is further increased, detection is also improved accurate
Degree.
(3) SPE material source enriches, it is easy to select, applied widely.
Brief description of the drawings
Front when Fig. 1 is structural representation and the work of the solid-phase extraction device of online transmitted spectrum detection of the invention regards
Figure and lateral plan.
Marked in figure as follows：1 through hole.
Fig. 2 is absorbed for the diffusing transmission of the dyestuff orange II determined using solid-phase extraction device of the present invention in embodiment 1
Spectrum.
Specific embodiment
Experimental technique used in following embodiments is conventional method unless otherwise specified.
Material used, reagent etc. in following embodiments, unless otherwise specified, commercially obtain.
It is structural representation of the present invention for the solid-phase extraction device of transmission mode solid phase spectra measurement as shown in Fig. 1 (a)
Figure, it includes a cube shaped container, and its upper surface sets for opening, for the injection of sample solution, set on lower surface
Have several through holes 1, can make filtrate flow out and SPE material is not lost in, the material of lower surface can be glass fibre, filter paper
Or core.The side at left and right two ends is made up of transparent smooth glass, for the measurement of diffusing transmission spectrum.Two other end face does not have
Particular/special requirement, may be selected the material such as stainless steel or other corrosion-resistant metal materials, glass, ceramics or plastics.
The height of above-mentioned three-dimensional body container is 50~200mm, and interior spacing is 1~10mm (light between transparent smooth glass
Journey).
Two ends for spectral measurement must be with smooth glass system into if must use quartzy glass for ultraviolet spectra measurement
Glass.
When transmission mode diffusing transmission spectral detection is carried out on above-mentioned solid phase extraction equipment, can carry out as steps described below：
The SPE material of suitable powder is added in container, the height for inserting material should ensure that light path can be completely
By material layer.Sample solution is injected from the opening of upper end, through hole 1 of the filtrate from lower surface flows out, such as Fig. 1 (b) and Fig. 1
Shown in (c), component absorption is tested on SPE material, other compositions flow out with filtrate.Enrichment terminates, without eluting, directly
It is connected on the diffusing transmission absorption spectrum that transparent smooth glass port measures solid phase material.Spectral measurement terminates, and is washed with suitable solvent
After de- material, for testing next time.
Tested component requirements have and absorb light property, and UV, visible light, near red can be carried out to the component that is enriched with solid phase material
Outer diffusing transmission spectral detection.
Embodiment 1,
The solid-phase extraction device detected using online transmitted spectrum, with reference to orange in UV, visible light diffusing transmission spectral detection solution
The content of yellow II, concrete operation step is as follows：
(1) made using glass, be highly 50mm, spacing 2mm, lower exit port are glass fibre in spectral measurement two ends
Solid-phase extraction device, chromatographic silica gel is filled inside it, be highly 30mm.
(2) 10mL orange IIs are injected the upper port of said apparatus, solution is flowed through silica gel material by vavuum pump,
Orange II is attracted on material.
(3) spectrum is determined using optical fiber ultraviolet-visual spectrometer.Light source and spectrometer are connected respectively to by light by optical fiber
Two end faces of spectrometry, notice that light path should completely pass through layer of silica gel.Light source and spectrometer are opened, directly determines unrestrained saturating after stabilization
Absorption spectrum is penetrated, its diffusing transmission absorption spectrum is as shown in Figure 2.
Spectral measurement terminates, and the orange II of removal is eluted with alcohol solvent, so that the device is used to test next time.
Embodiment 2,
The solid-phase extraction device detected using online transmitted spectrum, with reference to adjacent benzene two in diffusing transmission ultraviolet spectra detection solution
The content of formic acid di-isooctyl, concrete operation step is as follows：
(1) using glass make solid-phase extraction device, be highly 44mm, broadband 12mm, thickness 3.5mm, spectral measurement
Spacing 1mm in two ends, lower exit port is glass fibre, and chromatographic silica gel is filled inside it, is highly 30mm.
(2) 100mL diisooctyl phthalates solution is injected the upper end open of said apparatus, is made by vavuum pump molten
Liquid flows through silica gel material, and diisooctyl phthalate is attracted on material.
(3) enriching apparatus are inserted the cuvette slot of ultraviolet-visible spectrophotometer, instrument is opened, by transmitted spectrum
Pattern determines diffusing transmission ultraviolet spectra.
Spectral measurement terminates, and removal diisooctyl phthalate is eluted with solvent hexane, under being used for so as to the device
Once test.
Embodiment 3,
The solid-phase extraction device detected using online transmitted spectrum, with reference to lead metal ion near infrared spectrum detection solution
Content, concrete operation step is as follows：
(1) using glass make solid-phase extraction device, be highly 44mm, broadband 12mm, thickness 3.5mm, spectral measurement
Spacing 2mm in two ends, lower exit port is filter paper.
(2) SPE material is chelating resin D401.The pre-treatment step of chelating resin D401：1. resin is first used 50
~60 DEG C of hot water is embathed, and embathes and often stirs, and water is changed once every 15~30min, is embathed to embathing water without brown, foam
Untill seldom.2. after resin being soaked into 3h with the HCl of 1mol/L, then it is 4 or so to clean to pH with deionized water.3. 1mol/L is used
NaOH treatment 3h after, be flushed to pH for 10 or so with deionized water.4. after resin being soaked into 3h with the HCl of 1mol/L, spend
It is more than 6 that ionized water cleans to pH, then is cleaned with ultra-pure water 3 times.
(3) the chelating resin D401 after treatment is filled into solid-phase extraction device, is highly 30mm.
(4) 30mL lead solutions injection solid-phase extraction device is taken, solution is flowed through chelating resin material by vavuum pump, adsorbed
Lead ion.
Enriching apparatus are inserted the cuvette slot of near infrared spectrometer, instrument is opened, determines unrestrained by transmitted spectrum pattern
Ultraviolet transmissive spectrum.
Claims (8)
1. it is a kind of suitable for online transmission mode measurement solid-phase extraction device, it is characterised in that：The solid-phase extraction device bag
Include a container；
The upper end of the container is set for opening；
The lower surface of the container is provided with several through holes；
The material of a pair of opposite flanks of the container is glass.
2. solid-phase extraction device according to claim 1, it is characterised in that：The container is cube shaped.
3. solid-phase extraction device according to claim 1 and 2, it is characterised in that：The glass is quartz glass.
4. the solid-phase extraction device according to any one of claim 1-3, it is characterised in that：The upper end of the container is with
Spacing between end is 50~200mm.
5. the solid-phase extraction device according to any one of claim 1-4, it is characterised in that：The container is with glass
Spacing before two sides of material is 1~10mm.
6. the solid-phase extraction device according to any one of claim 1-5, it is characterised in that：The lower surface of the container
Material is glass fibre, filter paper or core.
7. transmission mode diffuse transmission light spectrum detection method is carried out using solid-phase extraction device any one of claim 1-6,
Comprise the following steps：
SPE material is placed with the container；
The sample solution that component to be measured is contained in the opening set by the upper surface of the container to addition in the container；It is described
After sample solution flows through the SPE material, the through hole outflow from the lower surface of the container；
Diffusing transmission spectral detection is carried out between with glass as material two sides of the container.
8. solid-phase extraction device any one of claim 1-6 in the original location solid phase spectra detection in application.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710038406.2A CN106872386A (en) | 2017-01-19 | 2017-01-19 | A kind of solid-phase extraction device suitable for the measurement of online transmission mode |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710038406.2A CN106872386A (en) | 2017-01-19 | 2017-01-19 | A kind of solid-phase extraction device suitable for the measurement of online transmission mode |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106872386A true CN106872386A (en) | 2017-06-20 |
Family
ID=59158520
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710038406.2A Pending CN106872386A (en) | 2017-01-19 | 2017-01-19 | A kind of solid-phase extraction device suitable for the measurement of online transmission mode |
Country Status (1)
| Country | Link |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109916700A (en) * | 2019-03-26 | 2019-06-21 | 华东理工大学 | A kind of small-sized Solid Phase Extraction and solid phase spectra detect aggregate device |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2415488A (en) * | 2004-05-13 | 2005-12-28 | Bruker Biospin Gmbh | Dividing a gas flow for drying solid phase extraction samples |
| CN101303279A (en) * | 2008-06-26 | 2008-11-12 | 华东理工大学 | On-line enriching apparatus for near-infrared testing low abundance components and use method thereof |
| CN101660999A (en) * | 2009-09-11 | 2010-03-03 | 华东理工大学 | Micro near-infrared spectral analytical method based on enrichment of integrated material |
| CN105784441A (en) * | 2016-03-15 | 2016-07-20 | 华东理工大学 | Magnetic membrane enrichment and separation device and using method thereof in solid phase spectrum detection |
-
2017
- 2017-01-19 CN CN201710038406.2A patent/CN106872386A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2415488A (en) * | 2004-05-13 | 2005-12-28 | Bruker Biospin Gmbh | Dividing a gas flow for drying solid phase extraction samples |
| CN101303279A (en) * | 2008-06-26 | 2008-11-12 | 华东理工大学 | On-line enriching apparatus for near-infrared testing low abundance components and use method thereof |
| CN101660999A (en) * | 2009-09-11 | 2010-03-03 | 华东理工大学 | Micro near-infrared spectral analytical method based on enrichment of integrated material |
| CN105784441A (en) * | 2016-03-15 | 2016-07-20 | 华东理工大学 | Magnetic membrane enrichment and separation device and using method thereof in solid phase spectrum detection |
Non-Patent Citations (1)
| Title |
|---|
| 杜一平 等: "固相萃取光谱（SPES）及其在光谱快检中的应用", 《光谱学与光谱分析》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109916700A (en) * | 2019-03-26 | 2019-06-21 | 华东理工大学 | A kind of small-sized Solid Phase Extraction and solid phase spectra detect aggregate device |
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170620 |
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