CN103808660B - Gas cell for ultraviolet-visible spectrum analysis - Google Patents
Gas cell for ultraviolet-visible spectrum analysis Download PDFInfo
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- CN103808660B CN103808660B CN201410090851.XA CN201410090851A CN103808660B CN 103808660 B CN103808660 B CN 103808660B CN 201410090851 A CN201410090851 A CN 201410090851A CN 103808660 B CN103808660 B CN 103808660B
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- cell
- cell body
- ultraviolet
- pond
- silica gel
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Abstract
The invention discloses a gas cell for ultraviolet-visible spectrum analysis. The gas cell comprises a cell body, two cell windows and two nuts, wherein the cell body comprises a cell center which is used for containing a gas sample and used as a light path; an extraction opening communicated with the cell center is formed at the upper part of the cell body; a bottom interface which is communicated with the cell center and protrudes outwards is also formed below the side of the cell body; convex outer edges are formed at two ends of the cell body; an outer thread is formed at the outer edge; each nut comprises an inner thread matched with the nut. By adopting the gas cell disclosed by the invention, solid, liquid and gas samples with volatility can be determined, the gas taking process of the solid or liquid sample is avoided, the cell windows are detachable, so that the cell windows and the cell body are convenient to clean, and the cell windows can adopt a polyethylene film material and can be directly replaced after each time of experiment. Thus, the gas cell is low in cost, cross contamination between the samples caused by halfway cleaning is avoided, and the accuracy of the detection result is ensured.
Description
Technical field
The present invention is applied to ultraviolet-visible light analysis of spectrum and uses, and is particularly used for measuring gaseous sample, has at a certain temperature
There are necessarily volatile liquid and solid sample.
Background technology
Existing technology does not also have the qualitative inspection that UV-Vis Spectrophotometry is existed with gaseous state to Organic substance at present
Survey method.Prior art can only be detected with the material that liquid or solid state exists to Organic substance.Liquid solvent dilution, solid
Detected with after solvent dissolving.Under the conditions of specific at some, the gas of Organic substance can only be obtained, and cannot thus produce phase
Answer gas liquid or solid when, just cannot be detected with prior art.
Uv-visible absorption spectra(UV-Vis)The important feature information of Organic substance can be provided, it is with INFRARED ABSORPTION light
Spectrum, mass spectrum, nuclear-magnetism supply wave spectrum equally important, the determination to compound structure, and this four big spectrum is indispensable.
To sum up, prior art does not have the detection method of organic vapo(u)r, therefore, how to obtain a kind of pollution-free, low cost,
Convenient, measure the detection method accurately analyzing oil and organic vapo(u)r based on uv-visible absorption spectra, be at present in oil and
The technical issues that need to address in the detection process of Organic substance.
Content of the invention
For solving to lack the method that uv-visible absorption spectra instrument measures gas in prior art, the present invention provides a kind of
Uv-visible absorption spectra analysis gas cell, the gas cell window of the present invention is replaceable, can facilitate, noresidue, pollution-free,
Multiduty Accurate Determining gaseous sample, there is necessarily volatile liquid and SOLID ORGANIC sample at a certain temperature.
Technical scheme is as follows:
A kind of ultraviolet-visible light analysis of spectrum gas cell, including cell body, two pond windows, two nuts and fixation clamp, institute
State and have in the middle of cell body for holding gaseous sample the pond heart as light path, cell body top is provided with the pumping communicating with the pond heart
Mouthful, cell body side-lower is additionally provided with an outwardly bottom interface communicating with the pond heart;Described cell body two ends have protrusion
Outer, described outer has external screw thread, and described nut has the female thread coordinating with it, and described fixation clamp is appointed located at cell body top
Meaning one end.
Further, described pond window is polyethylene film or quartz.
Further, described polyethylene film should meet one of following two conditions:
1. carried out with the pouch that polyethylene film is made in the UV-visible spectrum scan after instrument zeroing acquisition,
No absworption peak in the range of 190nm to 900nm;
2. carried out with the pouch that polyethylene film is made in the UV-visible spectrum scan after instrument zeroing acquisition,
In the range of 190nm to 900nm, only between 190nm to 217nm, there is absorption, and absorbance answers≤0.1.
Described polyethylene film meets DB44/T926-2011 and the requirement of standard GB/T 9687, selected from high density polyethylene (HDPE)
One of thin film, low-density polyethylene film and ultra-low density polyethylene thin film.
Polyethylene film selected by the present invention does not contain the composition having an impact organic vapo(u)r detection.
The available scope of described polyethylene film is wider, for example the food preserving bag of polyethylene material of commercialization, food
Product bag etc..Point used by the present invention breaks formula polyethylene film food bag in the range of 190nm to 900nm, is entered with double-layer polyethylene film
After the zeroing of row instrument, except between 217nm to 190nm, absorbance gradually tends to strengthening, the finally absorbance at 190nm
Beyond value is less than 0.1, all no other absworption peaks.Testing result is not affected substantially, all can guarantee that the repeatability of mensure, by this
The repeatability detection of the multiple mensure of invention can be verified.
The trade name food fresh keeping that the present invention is polyethylene and high density polyethylene (HDPE) to the material being purchased from big supermarket simultaneously
Bag and food bag more than ten brand are tested, and carry out instrument zeroing with double-layer polyethylene film all between 190nm to 900nm
Afterwards, except between 217nm to 190nm absorbance gradually tend to strengthen, finally the absorbance at 190nm is all not enough
Beyond 0.1, all no other absworption peaks, testing result is not affected.
And it is pointed out that food fresh keeping membrane is not suitable for the present invention.Although the ultraviolet-visible spectrum of food fresh keeping membrane
Figure and the UV-visible spectrum of commercial food products freshness protection package, food bag etc. are very close to or even the ultraviolet-visible light of preservative film
Light transmittance in the range of 220nm to 900nm for the spectrogram is better than polyethylene film, but after being returned to zero with double-layer food preservative film instrument,
The UV-visible absorption spectrum of scanning gained absorbance between 363nm to 190nm is gradually reduced, so that finally existing
At 190nm, absorbance is reduced to closely -0.2, and so big negative value can affect testing result, makes the absworption peak in this wave-length coverage
Intensity major part tend to low.
Further, described ultraviolet-visible light analysis of spectrum gas cell also includes 4 silica gel pieces, during described silica gel piece is
Sky, matched formation path channels with the pond heart of cell body;Silica gel piece, pond window and silica gel piece is laid successively in described outer,
Fixed with nut again.
Further, described nut does not have female one end end face is annular hollow, for blocking pond window when installing
Piece and silica gel piece, are fixed in outer.Hollow space is preferably not less than the section of cell body hollow space, in order to form light path
Passage.
Further, the depth of described outer is equal to the thickness of two silica gel pieces and 1 pond window.
Further, the inner side of described outer has two symmetrical draw-in grooves in order to fixing silica gel piece and pond window, institute
State silica gel piece and the correspondence position of pond window has two openings.
Further, it is preferable to the bottom interface lower end of described cell body is ground.Sample bottle can be connected when using, described sample
Product bottle should have the ground matching with bottom interface lower end, with cell body detachable connection.When using, can be either manually or by solid
Clamp or alternate manner are sealingly fastened on cell body, prevent it from coming off, and such as available prevent evaporative flask similar to Rotary Evaporators
The clip coming off is fixed;Also can use silica gel plug to be connected to bottom interface to be sealed against.
Further, it is preferable to described cell body and sample bottle are glass or polyethylene material.
Application in ultraviolet-visible light analysis of spectrum for the ultraviolet-visible light analysis of spectrum gas cell of the present invention.For
Sample is to have volatile liquid, have volatile solid or gaseous sample.
When detection has volatile liquid and has volatile solid, sample is loaded sample bottle and passes through bottom interface
It is connected on gas cell, with silica gel plug, the aspirating hole above cell body is covered tightly, pass through aspirating hole by cell body with instruments such as syringes
Air extract out, formed certain negative pressure be beneficial to sample bottle in gaseous volatilization to cell body, then using mode of heating promote sample
Product volatilize further, are full of the whole gas cell pond heart etc. sample vapor, using fixation clamp, gas cell are fixed on detection in light path
?.
And in detected gas sample, separately take a silica gel plug to clog gas cell bottom interface, by the spiral shell of cell body both sides
Cap is unscrewed, and is filled with the gaseous sample of pre-detection it is contemplated that air base in cell body through aspirating hole at the silica gel plug above cell body
This is replaced by sample gas, and the nut of cell body both sides is tightened, and is stoppered the aspirating hole above cell body with silica gel plug, by pond
Body is put into light path and is detected.
Beneficial effects of the present invention:
1. the present invention arranges a bottom interface using in gas cell side-lower, when measuring volatile solid and fluid sample
Sample bottle can directly be connected, make solid or fluid sample evaporate into and detects in the minds of the pond of cell body, it is to avoid steam injection loaded down with trivial details,
It also avoid taking vapor components during gas to liquefy to the cold to adhere to take and on gas device, lead to the steam injecting in gas cell there is no generation
The problem of table;
2. the pond window of the gas cell of the present invention is detachable, is easy to the cleaning in cell body;
3. the pond window of the gas cell of the present invention can adopt polyethylene film material, and polyethylene film material is easy to get, the food of supermarket
Product freshness protection package can meet experiment demand, can directly change a piece of polyethylene film, cost is very low, need not be to pond after doing once experiment
Window is carried out, it is to avoid because cleaning the sample room cross-contamination thoroughly not caused it is ensured that the accuracy of testing result.
Brief description
Accompanying drawing 4 width of the present invention,
Fig. 1. the ultraviolet-visible light analysis of spectrum gas cell main structure chart of the present invention;
Fig. 2. the nut structure schematic diagram of the present invention;
Fig. 3. the silica gel piece structural representation of the present invention;
Fig. 4. carry out scanning the ultraviolet-visible spectrum obtaining after instrument zeroing with polyethylene film pouch(UV-Vis)Figure and use
Double-deck preservative film scans the UV-Vis figure obtaining after carrying out instrument zeroing.Spectrogram abscissa is wavelength(Unit:nm), vertical coordinate is
Absorbance(No unit).In spectrogram:1--- polyethylene film pouch carries out scanning the UV-Vis figure obtaining after instrument zeroing,
The double-deck preservative film of 2--- carries out scanning the UV-Vis figure obtaining after instrument zeroing.
Wherein:1. cell body, 2. nut, 3. silica gel piece, 4. fixation clamp, the 11. pond hearts, 12. bleeding points, 13. bottom interface,
14. outers, 15. draw-in grooves, 16. grounds.
Specific embodiment
Following non-limiting examples can make those of ordinary skill in the art that the present invention is more fully understood, but not with
Any mode limits the present invention.
Embodiment 1
Ultraviolet-visible light analysis of spectrum gas cell, as shown in figure 1, include 1, two pond windows of cell body, two nut 2 and
Fixation clamp 4, described cell body 1 has for holding gaseous sample the pond heart 11 as light path, and cell body 1 top is provided with and the pond heart 11
The bleeding point 12 communicating, cell body 1 side-lower is additionally provided with an outwardly bottom interface 13 communicating with the pond heart 11;Described pond
Body 1 two ends have the outer 14 of protrusion, and described outer 14 has external screw thread, and described nut 2 has the female thread coordinating with it.Institute
State the inside side in outer 14 and there are two draw-in grooves 15.Described cell body 1 is polyethylene material(It is alternatively glass material).
Described gas cell also includes 4 silica gel pieces 3, as shown in figure 3, silica gel piece 3 is hollow, the pond heart 11 phase with cell body 1
Cooperatively form path channels;Upper and lower ends also have two openings, corresponding with two draw-in grooves 15 in outer 14, in described outer
Silica gel piece 3, pond window and silica gel piece 3 is laid successively in 14, more fixing with nut 2.Described nut 2 structure is as shown in Fig. 2 one end
There is female thread, not having female one end end face is annular hollow, for blocking pond window and silica gel piece 3 when installing, will
It is fixed in outer 14.The diameter of hollow space is identical with the long side of the pond heart 11, in order to form path channels.
Described pond window is polyethylene film, and described polyethylene film is by the disconnected formula of trade name your US business's punctuate hard purchased from supermarket
Food bag is made.As shown in figure 4, in figure 1 is described polyethylene film carries out the ultraviolet after instrument zeroing-can with polyethylene film pouch
See spectrum(UV-Vis)Figure, in figure baseline steadily, simply has the small peak that absorbance gradually rises between 217nm to 190nm,
Enhancing at 208.01nm peak is obvious, finally in the absorbance at 190nm below 0.1.Testing result is not had substantially
Have an impact.And in figure 2 is to be carried out with double-deck preservative film scanning the UV-Vis figure obtaining after instrument zeroing, 363nm to 190nm it
Between absorbance be gradually reduced, the reduction at 268.46nm peak is obvious so that final at 190nm absorbance be reduced to
Closely -0.2, so big negative value can affect testing result.
Using above gas cell, in the sample detection carrying out there is volatile liquid or solid, take one have with
The ground sample bottle that the ground 16 of cell body bottom interface 13 matches, is loaded sample, is connected on cell body 1 by bottom interface 13,
With silica gel plug, cell body 1 top bleeding point 12 is covered tightly, with instruments such as syringes, the air in cell body is extracted out, form certain negative pressure
It evaporate into inside cell body 1 beneficial to the liquid or solid in sample bottle, then promote sample to volatilize further using mode of heating, treat sample
Product steam is full of the pond heart 11 of whole cell body 1, using fixation clamp, gas cell is fixed on detection in light path.
Using above gas cell, when carrying out gaseous sample detection, with silica gel plug, gas cell bottom interface 13 is stoppered, will
The nut 2 of cell body 1 both sides is unscrewed, and is filled with the gaseous sample of pre-detection it is contemplated that the pond of cell body 1 by the bleeding point 12 at cell body top
In the heart 11, air is replaced by sample gas substantially, and the nut 2 of cell body 1 both sides is tightened, and with silica gel plug by aspirating hole 12
Stopper, put into light path detection.
Claims (7)
1. a kind of ultraviolet-visible light analysis of spectrum gas cell it is characterised in that:Including cell body(1), two pond window, two spiral shells
Cap(2)And fixation clamp(4), described cell body(1)Centre has for holding gaseous sample the pond heart as light path(11), cell body
Top is provided with and the pond heart(11)The bleeding point communicating(12), cell body(1)Side-lower is additionally provided with one and the pond heart(11)Communicate to
The bottom interface of outer protrusion(13);Described cell body(1)Two ends have the outer of protrusion(14), described outer(14)There is outer spiral shell
Stricture of vagina, described nut(2)There is the female thread coordinating with it, described fixation clamp(4)Located at any one end in cell body top;
Described pond window is polyethylene film or quartz;
Also include 4 silica gel pieces(3), described silica gel piece(3)For hollow, the pond heart with cell body(11)The formation light path that matches is led to
Road;In described outer(14)Inside lay silica gel piece successively(3), pond window and silica gel piece(3), then with nut(2)Fixing;
Described polyethylene film should meet one of following two conditions:
1. carried out in the UV-visible spectrum scan after instrument zeroing acquisition with the pouch that polyethylene film is made, in 190nm extremely
No absworption peak in the range of 900nm;
2. carried out in the UV-visible spectrum scan after instrument zeroing acquisition with the pouch that polyethylene film is made, in 190nm extremely
In the range of 900nm, only between 190nm to 217nm, there is absorption, and absorbance answers≤0.1.
2. ultraviolet-visible light analysis of spectrum gas cell according to claim 1 is it is characterised in that described nut(2)Do not have
Female one end end face is annular hollow.
3. ultraviolet-visible light analysis of spectrum gas cell according to claim 2 is it is characterised in that described outer(14)Depth
Degree is equal to two silica gel pieces(3)Thickness with 1 pond window.
4. ultraviolet-visible light analysis of spectrum gas cell according to claim 2 is it is characterised in that described outer(14)Interior
Side have two symmetrical in order to fixing silica gel piece(3)Draw-in groove with pond window(15), described silica gel piece(3)Right with pond window
Position is answered to have two openings.
5. ultraviolet-visible light analysis of spectrum gas cell according to claim 1 is it is characterised in that described bottom interface(13)
Lower end is ground(16).
6. the ultraviolet-visible light analysis of spectrum gas cell described in claim 1 ~ 5 any one is in ultraviolet-visible light analysis of spectrum
Application.
7. ultraviolet-visible light analysis of spectrum gas cell according to claim 6 answering in ultraviolet-visible light analysis of spectrum
With it is characterised in that the sample being directed to is to have volatile liquid, have volatile solid or gaseous sample.
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CN201410090851.XA CN103808660B (en) | 2014-03-12 | 2014-03-12 | Gas cell for ultraviolet-visible spectrum analysis |
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US5116759A (en) * | 1990-06-27 | 1992-05-26 | Fiberchem Inc. | Reservoir chemical sensors |
TW340876B (en) * | 1996-03-27 | 1998-09-21 | Nisshin Steel Co Ltd | Method and apparatus for controlling the deposition amount of a plating metal as well as method and apparatus for measuring the amount of a metal vapor |
WO2001014855A1 (en) * | 1999-08-20 | 2001-03-01 | Charles William Robertson | Liquid photometer using surface tension to contain sample |
CN101097182B (en) * | 2006-06-29 | 2011-06-15 | 中国石油化工股份有限公司 | Dynamic rotating sample pool and infrared spectrum analysis general purpose accessory |
JP5300668B2 (en) * | 2009-09-04 | 2013-09-25 | 日本電信電話株式会社 | Method for identifying benzene and toluene concentrations in liquid samples |
CN202126390U (en) * | 2011-06-22 | 2012-01-25 | 南京信息工程大学 | Absorption cell |
CN202393699U (en) * | 2011-11-08 | 2012-08-22 | 南京信息工程大学 | Sample pool |
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红外光谱中挥发性液体的气态样品取样技术;孙淑清 等;《光谱实验室》;20040531;第21卷(第3期);第445-446页 * |
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