CN103808660A - Gas cell for ultraviolet-visible spectrum analysis - Google Patents

Gas cell for ultraviolet-visible spectrum analysis Download PDF

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Publication number
CN103808660A
CN103808660A CN201410090851.XA CN201410090851A CN103808660A CN 103808660 A CN103808660 A CN 103808660A CN 201410090851 A CN201410090851 A CN 201410090851A CN 103808660 A CN103808660 A CN 103808660A
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China
Prior art keywords
pond
ultraviolet
visible light
cell
gas cell
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CN201410090851.XA
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CN103808660B (en
Inventor
姜波
胡文忠
刘长建
权春善
郑维
姜爱丽
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Dalian Minzu University
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Dalian Nationalities University
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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

A kind of ultraviolet-visible light analysis of spectrum gas cell
Technical field
The present invention is applicable to ultraviolet-visible light analysis of spectrum use, specifically for mensurated gas composition sample, have certain volatile liquid and a solid sample at a certain temperature.
Background technology
Current existing technology also do not have uv-visible absorption spectra method to organism the qualitative checking method with gaseous state.The material that prior art can only exist with liquid or solid state organism detects.Liquid solvent dilution, solid is with detecting after dissolution with solvents.When under some specific conditions, can only obtain organic gas, and while can not get producing thus the liquid or solid of corresponding gas, just cannot detect by prior art.
Uv-visible absorption spectra (UV-Vis) can provide organic important structure information, and it is supplying wave spectrum equally important with infrared absorption spectrum, mass spectrum, nuclear-magnetism, and to determining of compound structure, this four large 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, cost is low, convenient, measure the detection method of analyzing accurately oil and the organic matter's steam based on uv-visible absorption spectra, be the technical issues that need to address in the testing process of oil and the organic matter's at present.
Summary of the invention
For solving the method that lacks uv-visible absorption spectra instrument mensurated gas composition in prior art, the invention provides a kind of uv-visible absorption spectra analysis gas cell, gas cell window of the present invention is replaceable, can facilitate, noresidue, pollution-free, multiduty Accurate Determining gaseous sample, have certain volatile liquid and a SOLID ORGANIC sample at a certain temperature.
Technical scheme of the present invention is as follows:
A kind of ultraviolet-visible light analysis of spectrum gas cell, comprise pond body, two pond windows, two nuts and geometrical clamp, in the middle of described pond body, have for holding gaseous sample and doubling as the pond heart of light path, body top, pond is provided with the bleeding point communicating with the pond heart, and below, side, pond is also provided with an outwardly bottom interface communicating with the pond heart; Body two ends, described pond have the outer of protrusion, and described outer has external thread, and described nut has the internal thread being mated, and described geometrical clamp is located at any one end, body top, pond.
Further, described pond window is polyethylene film or quartz.
Further, described polyethylene film should meet one of following two conditions:
1. the pouch made from polyethylene film carries out in scanning obtains after instrument zeroing ultraviolet-visible light spectrogram, in 190nm to 900nm scope without absorption peak;
2. the pouch made from polyethylene film carries out scanning in the ultraviolet-visible light spectrogram obtaining after instrument zeroing, in 190nm to 900nm scope, only between 190nm to 217nm, have absorption, and absorbance answers≤0.1.
Described polyethylene film meets the requirement of DB44/T926-2011 and standard GB/T 9687, is selected from the one in density polyethylene film with high, low-density polyethylene film and ultra-low density polyethylene film.
The selected polyethylene film of the present invention does not contain affects the composition that organic vapo(u)r detects.
The available scope of described polyethylene film is wider, for example food preserving bag, the food bag etc. of commercial tygon material.The present invention's point used breaks formula polyethylene film food bag in 190nm to 900nm scope, carry out after instrument zeroing with double-layer polyethylene film, except be tending towards gradually strengthening at absorbance between 217nm to 190nm, final beyond the absorbance less than 0.1 at 190nm place, all without other absorption peaks.Testing result is not affected substantially, all can guarantee the reappearance of mensuration, detect and can verify by the repeatability of repeatedly measuring of the present invention.
The present invention is that commodity food preserving bag by name and food bag more than ten brands of tygon and high density polyethylene are tested to being purchased from the material in large supermarket simultaneously, all between 190nm to 900nm, carry out after instrument zeroing with double-layer polyethylene film, except be tending towards gradually strengthening at absorbance between 217nm to 190nm, final beyond the equal less than 0.1 of absorbance at 190nm place, all, without other absorption 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 light spectrogram of food fresh keeping membrane and commercialization food preserving bag, the ultraviolet-visible light spectrogram of food bag etc. is very approaching, even the transmittance of the ultraviolet-visible light spectrogram of preservative film in 220nm to 900nm scope is better than polyethylene film, but after returning to zero with double-layer food preservative film instrument, uv-visible absorption spectra figure absorbance between 363nm to 190nm of scanning gained declines gradually, so that be finally reduced to closely-0.2 at 190nm place absorbance, so large negative value can affect testing result, make the intensity major part of the absorption peak in this wavelength coverage be tending towards on the low side.
Further, described ultraviolet-visible light analysis of spectrum also comprises 4 silica gel pieces with gas cell, and described silica gel piece is hollow, and formation path channels matches with the pond heart of pond body; In described outer, lay successively silica gel piece, pond window and silica gel piece, then fix with nut.
Further, the described nut not female one end of tool end face is annular hollow, blocks pond window and silica gel piece when installing, is fixed in outer.Hollow space is preferably not less than the cross section of pond body hollow space, in order to form path channels.
Further, the degree of depth of described outer equals 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, and the correspondence position of described silica gel piece and pond window has two openings.
Further, the bottom interface lower end of preferred described pond body is ground.Can connect in use sample bottle, described sample bottle should have the ground matching with bottom interface lower end, is connected with pond body is detachable.In use, can manually be sealingly fastened in Chi Tishang by geometrical clamp or alternate manner, prevent that it from coming off, bottle clip coming off that avoids evaporating that is similar to Rotary Evaporators as available is fixed; Also available silica gel plug is connected to bottom interface and is sealed.
Further, preferred described pond body and sample bottle are glass or tygon material.
Ultraviolet-visible light analysis of spectrum of the present invention is the application in ultraviolet-visible light analysis of spectrum with gas cell.For sample for thering is volatile liquid, thering is volatile solid or gaseous sample.
When detection has volatile liquid and has volatile solid, packing sample into sample bottle receives on gas cell by bottom interface, the aspirating hole of pond body top is covered tightly with silica gel plug, by aspirating hole, the air of Chi Tizhong is extracted out with instruments such as syringes, form certain negative pressure and be beneficial to gaseous volatilization in sample bottle to body inside, pond, adopt again type of heating to promote that sample further volatilizees, be full of the whole gas cell pond heart etc. sample vapor, utilize geometrical clamp that gas cell is fixed in light path and is detected.
And in the time detecting gaseous sample, separately getting a silica gel plug clogs gas cell bottom interface, the nut of body both sides, pond is unscrewed, silica gel plug place above the body of pond is filled with the gaseous sample of pre-detection through aspirating hole, estimate that in the body of pond, air is replaced by sample gas substantially, the nut of body both sides, pond is tightened, and with silica gel plug by the aspirating hole jam-pack of pond body top, pond body is put into light path and detects.
Beneficial effect of the present invention:
1. the present invention adopts, at gas cell side-lower, a bottom interface is set, while measuring volatile solid and fluid sample, can directly connect sample bottle, the pond that makes solid or fluid sample evaporate into pond body is detected in the heart, that has avoided that steam injects is loaded down with trivial details, has also avoided getting in gas process vapor components and has met cold liquefaction and adhere to get on gas device and cause the steam in injecting gas pond there is no representational problem;
2. the pond window of gas cell of the present invention is detachable, is convenient to the cleaning in the body of pond;
3. the pond window of gas cell of the present invention can adopt polyethylene film material, polyethylene film material is easy to get, the food preserving bag in supermarket can meet experiment demand, do once and can directly change a slice polyethylene film after experiment, cost is very low, without pond window is cleaned, avoid, because cleaning the sample room cross pollution that thoroughly do not cause, guaranteeing the accuracy of testing result.
Accompanying drawing explanation
Accompanying drawing 4 width of the present invention,
Fig. 1. ultraviolet-visible light analysis of spectrum gas cell main structure chart of the present invention;
Fig. 2. nut structure schematic diagram of the present invention;
Fig. 3. silica gel piece structural representation of the present invention;
Fig. 4. carry out scanning obtains after instrument zeroing ultraviolet-visible spectrum (UV-Vis) figure and carry out with double-deck preservative film the UV-Vis that scanning obtains after instrument zeroing and scheme with polyethylene film pouch.Spectrogram horizontal ordinate is wavelength (unit: nm), and ordinate is absorbance (without unit).In spectrogram: 1---carries out with polyethylene film pouch the UV-Vis figure that the rear scanning of instrument zeroing obtains, 2---carries out scanning the UV-Vis figure obtaining after instrument zeroing with double-deck preservative film.
Wherein: 1. pond body, 2. nut, 3. silica gel piece, 4. geometrical clamp, the 11. pond hearts, 12. bleeding points, 13. bottom interface, 14. outers, 15. draw-in grooves, 16. grounds.
Embodiment
Following non-limiting example can make the present invention of those of ordinary skill in the art's comprehend, but does not limit the present invention in any way.
Embodiment 1
Ultraviolet-visible light analysis of spectrum gas cell, as shown in Figure 1, comprise pond body 1, two pond windows, two nuts 2 and geometrical clamp 4, described pond body 1 has for holding gaseous sample and doubling as the pond heart 11 of light path, body 1 top in pond is provided with the bleeding point 12 communicating with the pond heart 11, and body 1 side-lower in pond is also provided with an outwardly bottom interface 13 communicating with the pond heart 11; Body 1 two ends, described pond have the outer 14 of protrusion, and described outer 14 has external thread, and described nut 2 has the internal thread being mated.The inside side in described outer 14 has two draw-in grooves 15.Described pond body 1 is tygon material (also can be glass material).
Described gas cell also comprises 4 silica gel pieces 3, and as shown in Figure 3, silica gel piece 3 is hollow, and formation path channels matches with the pond heart 11 of pond body 1; Upper and lower two ends also have two openings, corresponding with two draw-in grooves 15 in outer 14, lay successively silica gel piece 3, pond window and silica gel piece 3 in described outer 14, more fixing with nut 2.As shown in Figure 2, one end has internal thread to described nut 2 structures, and the female one end of tool end face is not annular hollow, blocks pond window and silica gel piece 3 when installing, is fixed in outer 14.The diameter of hollow space is identical with the long limit of the pond heart 11, in order to form path channels.
Described pond window is polyethylene film, and described polyethylene film is made up of the disconnected formula food bag of hard your the US business's punctuate by name of the commodity purchased from supermarket.As shown in Figure 4, in figure, 1 is that described polyethylene film carries out ultraviolet-visible spectrum (UV-Vis) figure after instrument zeroing with polyethylene film pouch, in figure, baseline is steady, the small peak that just has absorbance to raise gradually between 217nm to 190nm, enhancing at 208.01nm peak is obvious, and the final absorbance at 190nm place is below 0.1.Testing result is not affected substantially.And the 2 UV-Vis figure that obtain for carry out the rear scanning of instrument zeroing with double-deck preservative film in figure, between 363nm to 190nm, absorbance declines gradually, reduction at 268.46nm peak is obvious, so that be finally reduced to closely-0.2 at 190nm place absorbance, so large negative value can affect testing result.
Adopt above gas cell, in the time thering is the sample detection of volatile liquid or solid, get one and there is the ground sample bottle matching with the ground 16 of pond body bottom interface 13, pack sample into, receive on pond body 1 by bottom interface 13, body 1 top bleeding point 12 in pond is covered tightly with silica gel plug, the air of Chi Tizhong is extracted out with instruments such as syringes, form the liquid or solid that certain negative pressure is beneficial in sample bottle and evaporate into pond body 1 inside, adopt again type of heating to promote that sample further volatilizees, treat that sample vapor is full of the pond heart 11 of whole pond body 1, utilize geometrical clamp that gas cell is fixed in light path and is detected.
Adopt above gas cell, in the time carrying out gaseous sample detection, with silica gel plug by gas cell bottom interface 13 jam-packs, the nut 2 of pond body 1 both sides is unscrewed, be filled with the gaseous sample of pre-detection by the bleeding point 12 at body top, pond, in the pond heart 11 of expectation pond body 1, air is replaced by sample gas substantially, and the nut 2 of pond body 1 both sides is tightened, and with silica gel plug by aspirating hole 12 jam-packs, put into light path detect.

Claims (10)

1. a ultraviolet-visible light analysis of spectrum gas cell, it is characterized in that: comprise pond body (1), two pond windows, two nuts (2) and geometrical clamps (4), have in the middle of described pond body (1) for holding gaseous sample and doubling as the pond heart (11) of light path, body top, pond is provided with the bleeding point (12) communicating with the pond heart (11), and pond body (1) side-lower is also 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) have external thread, and described nut (2) has the internal thread being mated, and described geometrical clamp (4) is located at any one end, body top, pond.
2. ultraviolet-visible light analysis of spectrum gas cell according to claim 1, is characterized in that described pond window is polyethylene film or quartz.
3. ultraviolet-visible light analysis of spectrum gas cell according to claim 2, is characterized in that described polyethylene film should meet one of following two conditions:
1. the pouch made from polyethylene film carries out in scanning obtains after instrument zeroing ultraviolet-visible light spectrogram, in 190nm to 900nm scope without absorption peak;
2. the pouch made from polyethylene film carries out scanning in the ultraviolet-visible light spectrogram obtaining after instrument zeroing, in 190nm to 900nm scope, only between 190nm to 217nm, have absorption, and absorbance answers≤0.1.
4. ultraviolet-visible light analysis of spectrum gas cell according to claim 1, characterized by further comprising 4 silica gel pieces (3), and described silica gel piece (3) is hollow, and formation path channels matches with the pond heart (11) of pond body; In described outer (14), lay successively silica gel piece (3), pond window and silica gel piece (3), more fixing with nut (2).
5. according to the ultraviolet-visible light analysis of spectrum gas cell described in claim 1 or 4, it is characterized in that described nut (2) not the female one end of tool end face be annular hollow.
6. ultraviolet-visible light analysis of spectrum gas cell according to claim 4, is characterized in that the degree of depth of described outer (14) equals the thickness of two silica gel pieces (3) and 1 pond window.
7. ultraviolet-visible light analysis of spectrum gas cell according to claim 4, the inner side that it is characterized in that described outer (14) has two symmetrical draw-in grooves (15) in order to fixing silica gel piece (3) and pond window, and the correspondence position of described silica gel piece (3) and pond window has two openings.
8. ultraviolet-visible light analysis of spectrum gas cell according to claim 1, is characterized in that described sidepiece interface (13) lower end is ground (16).
9. the application in ultraviolet-visible light analysis of spectrum with gas cell of the ultraviolet-visible light analysis of spectrum described in claim 1~8 any one.
10. the ultraviolet-visible light analysis of spectrum according to claim 9 application in ultraviolet-visible light analysis of spectrum with gas cell, it is characterized in that for sample for thering is volatile liquid, thering is volatile solid or gaseous sample.
CN201410090851.XA 2014-03-12 2014-03-12 Gas cell for ultraviolet-visible spectrum analysis Expired - Fee Related CN103808660B (en)

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CN101097182A (en) * 2006-06-29 2008-01-02 中国石油化工股份有限公司 Dynamic rotating sample pool and infrared spectrum analysis general purpose accessory
JP2011058804A (en) * 2009-09-04 2011-03-24 Nippon Telegr & Teleph Corp <Ntt> Gas detector and method of detecting gas, and method of identifying benzene concentration and toluene concentration within liquid sample
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

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5116759A (en) * 1990-06-27 1992-05-26 Fiberchem Inc. Reservoir chemical sensors
CN1167165A (en) * 1996-03-27 1997-12-10 日新制钢株式会社 Atomic absorption analysis for measuring and controlling amount of metal vapor in vapor deposition coating line and apparatus therefor
US20020154299A1 (en) * 1999-08-20 2002-10-24 Robertson Charles William Liquid photometer using surface tension to contain sample
CN101097182A (en) * 2006-06-29 2008-01-02 中国石油化工股份有限公司 Dynamic rotating sample pool and infrared spectrum analysis general purpose accessory
JP2011058804A (en) * 2009-09-04 2011-03-24 Nippon Telegr & Teleph Corp <Ntt> Gas detector and method of detecting gas, and method of identifying benzene concentration and toluene concentration within liquid sample
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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Title
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