CN103808661A - Gas cell for infrared spectroscopy analysis - Google Patents
Gas cell for infrared spectroscopy analysis Download PDFInfo
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- CN103808661A CN103808661A CN201410090917.5A CN201410090917A CN103808661A CN 103808661 A CN103808661 A CN 103808661A CN 201410090917 A CN201410090917 A CN 201410090917A CN 103808661 A CN103808661 A CN 103808661A
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- infrared spectroscopy
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Abstract
The invention discloses a gas cell for infrared spectroscopy analysis, comprising a cell body and two cell windows, wherein the cell windows are detachably connected with the cell body; a bleeder hole is formed at the top of the cell body; a bottom interface is arranged at the bottom of the cell body; each cell window comprises a window frame, a window and a gasket; the window is a polyethylene film or a potassium bromide sheet. By adopting the gas cell disclosed by the invention, solid, liquid and gas samples with volatility can be determined, a gas taking process of the solid or liquid sample is avoided, and the cell windows are detachable and convenient to clean, 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 relates to infrared spectrum detection field, relate in particular to a kind of infrared analysis gas cell for sample detection.
Background technology
Current existing infrared spectrum gas cell can only detect gaseous sample, or the steam importing that fluid sample volatilization is produced wherein detects.Existing gas cell is generally fixed the salt windows such as KBr at body two ends, pond, top has the piston of inflation/deflation, in the time detecting, the gas or the liquid vapors that are filled with in gas cell can be residual on salt window, and salt window is not to test to change once at every turn, can only clean with volatile low boiling point organic solvent, if do not washed clean clearly, can form interference to subsequent measurements, cause the inaccurate of subsequent measurements result.
The for example analysis to oil samples, existing infrared spectrum gas cell detects oil vapour, if oil samples is first heated, get again in its steam injecting gas pond, oil vapour adheres on collector owing to meeting cold liquefaction on the one hand, make the oil sample vapor volume deficiency in be injected into gas cell, or because meeting cold liquefaction and adhere to get on gas device and make the steam in injecting gas pond there is no representativeness getting in gas process certain component of steam; On the other hand, the oil vapour in injecting gas pond also can be on its salt window can form and adheres to and residual, if do not washed clean clearly after experiment, and then in different sample detection, on salt window, can form multiple contaminates, causes the inaccurate of subsequent sample measurement result.If oil samples is directly injected in gas cell, because oil samples volatility is low, need heating produce steam, like this gas cell inwall especially the salt window of gas cell can be subject to serious irreversible membrane fouling, so that cannot clean up, cause thus the inaccurate of subsequent sample measurement result.
In addition liquid or solid sample can not directly be packed in existing infrared spectrum gas cell and be detected, liquid or solid sample directly can not be packed in gas cell and detect after heating.
Summary of the invention
For residual impurity on the window of above gas cell of the prior art pond not in easy cleaning, gas replenishment process part vapor components easily adhere to collector and cause measurement result there is no the problems such as representative, the invention provides a kind of convenience, noresidue, pollution-free, multiduty more Accurate Determining gaseous sample, there is the Infrared spectroscopy gas cell of certain volatile liquid and solid sample.Adopt gas cell of the present invention, after experiment finishes, replaceable pond window.Lower end at gas cell can connect the bottle that fills volatile liquid or solid sample.Before experiment, the sample bottle that liquid or solid is housed can be connected in to gas cell and heat at a certain temperature, then put into IR instrument light path and carry out IR analysis.After once experiment finishes, pull down pond window, with effumability solvent cleaning pond body inwall, until in the body of pond, clean up dry after, install new pond window, test next time.
Technical purpose of the present invention is achieved through the following technical solutions:
A kind of Infrared spectroscopy gas cell, comprises pond body and two pond windows, it is characterized in that the relative both sides of body, described pond are respectively equipped with coaxial port I and port II, and described two pond windows are connected with pond body detachable-type sealed with port II by port I respectively; Body top, described pond is provided with bleeding point, and body bottom in described pond is also provided with an outwardly bottom interface.
Infrared spectroscopy gas cell of the present invention, described pond window comprises window, described window is polyethylene film or kbr tablet.
Further, described polyethylene film should meet one of following two conditions:
1. in Infrared spectroscopy, in the infrared spectrogram after double-layer polyethylene film buckle back scape, at 4000cm
-1to 400cm
-1scope is interior without absorption peak;
2. in Infrared spectroscopy, in the infrared spectrogram after double-layer polyethylene film buckle back scape, at 4000cm
-1to 400cm
-1in scope, only at 2930cm
-1to 2845cm
-1between have the absorption peak of two light transmittance values>=94.0%.
Describedly refer to polyethylene film and make pouch with the infrared spectrogram after double-layer polyethylene film buckle back scape, put into light path buckle back scape, should meet only at 2930cm
-1to 2845cm
-1between have the absorption peak of two light transmittance values>=94.0%.
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 available scope of described polyethylene film is wider, for example food preserving bag, the food bag etc. of commercial tygon material.The disconnected formula polyethylene film food bag of the present invention's point used, as Fig. 4 be as described in the infrared spectrogram of polyethylene film after with air buckle back scape, Fig. 5 is with the infrared spectrogram after double-layer polyethylene film buckle back scape, in Fig. 5, at 4000cm
-1to 400cm
-1in scope, except at 2929.87cm
-1and 2846.93cm
-1have outside two peaks, all without other absorption peaks.And its peak intensity is very weak, the light transmittance values at two peaks all, up to more than 94.0%, does not affect testing result substantially, all can guarantee the reappearance of measuring.
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 at 2929.87cm
-1and 2846.93cm
-1between only have Huo Wu peak, two peaks, the intensity at its peak, light transmittance values is all higher, the light transmittance values at peak all, up to more than 94.0%, does not affect testing result.
And it is pointed out that food fresh keeping membrane is not suitable for the present invention.Although the infrared spectrogram of the infrared spectrogram of food fresh keeping membrane and commercialization food preserving bag, food bag etc. is very approaching, using after double-layer food preservative film buckle back scape, at 2937.59cm
-1to 2843.07cm
-1between peak more, and at 2937.59cm
-1the peak at place is strong, and light transmittance values is only 78%, and so large numerical value has had a strong impact on testing result.
Infrared spectroscopy gas cell of the present invention, preferred described pond window also comprises that window-frame and packing ring, described window-frame one end have internal thread, the end face of the other end has the interior edge of annular, when edge is used for installing in annular, blocks window, is fixed in window-frame.Described port I and port II have the external thread matching with window-frame, and when connection, packing ring is placed between port and window.
Infrared spectroscopy gas cell of the present invention, preferred described packing ring is that the material that can play sealing function is made, as silica gel.
Infrared spectroscopy gas cell of the present invention, on the body of preferred described pond, at least one side external stability of porose I or hole II is provided with several magnet pieces.Preferred described magnet piece has 6, is symmetrically distributed in the both sides of edges of hole I or hole II.
Infrared spectroscopy gas cell of the present invention, preferred described bottom interface lower end 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.
Infrared spectroscopy gas cell of the present invention, preferred described pond body and sample bottle are glass or tygon material.
Infrared spectroscopy of the present invention is the application in Infrared spectroscopy 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, aspirating hole 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 whole gas cell etc. sample vapor, put into light path and detect.
And in the time detecting gaseous sample, separately getting a silica gel plug clogs gas cell bottom interface, the pond window 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 pond window of body both sides, pond is tightened, pond body is put into light path and detect.
Beneficial effect of the present invention:
1. the present invention adopts in gas cell bottom a bottom interface is set, while measuring volatile solid and fluid sample, can directly connect sample bottle, making solid or fluid sample evaporate into Chi Tizhong detects, 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 clean;
3. described in gas cell of the present invention, the window of pond window 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 5 width of the present invention,
Fig. 1. gas cell main structure chart of the present invention;
Fig. 2. the structural representation of pond window;
Fig. 3. the each several part composition structural drawing of pond window;
Fig. 4. the infrared scan spectrogram of polyethylene film after with air buckle back scape;
Fig. 5. the infrared scan spectrogram of polyethylene film after with double-layer polyethylene film buckle back scape;
Wherein: 1. pond body, 2. pond window, 11. port I, 12. port II, 13. bleeding points, 14. bottom interface, 15. magnet pieces, 21. window-frames, 22. windows, 23. packing rings.
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.
Infrared spectroscopy gas cell, as depicted in figs. 1 and 2, comprise pond body 1 and two pond windows 2, the both sides that pond body 1 is relative are respectively equipped with coaxial port I 11 and port II 12, and body 1 top in pond is provided with bleeding point 13, and silica gel plug 4 matches with bleeding point 13, the bottom of described pond body 1 is also provided with an outside outstanding bottom interface 14, bottom interface 14 has outer grinding port, and described gas cell also comprises a sample bottle 5 with interior ground, matches with bottom interface 14.The one side outside with hole I 11 of pond body 1 is also installed with 6 magnet pieces, is symmetrically distributed in the both sides of edges of hole I 11.Described pond body 1 and sample bottle are glass material.
As shown in Figure 3, described pond window 2 comprises window-frame 21, window 22 and packing ring 23, described window-frame 21 one end have internal thread, described port I 11 and port II 12 have the external thread coordinating with it, the end face of window-frame 21 other ends has the interior edge of annular, when connection, packing ring 23 is placed between port and window 22, then window-frame is tightened to sealing.
Described window 22 is polyethylene film material, 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 Fig. 4 be as described in the infrared spectrogram of polyethylene film after with air buckle back scape, Fig. 5 is with the infrared spectrogram after double-layer polyethylene film buckle back scape, in Fig. 5, at 4000cm
-1to 400cm
-1in scope, except at 2929.87cm
-1and 2846.93cm
-1have outside two peaks, all without other absorption peaks.And its peak intensity is very weak, the light transmittance values at two peaks all, up to more than 94.0%, does not affect testing result substantially.
Adopt above Infrared spectroscopy gas cell, in the time thering is the sample detection of volatile liquid or solid, get a sample bottle with the interior ground matching with the outer grinding port of pond body bottom interface 14, pack sample into, receive on gas cell by bottom interface 14, aspirating hole 13 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 whole pond body 1, putting into light path detects.
Adopt above Infrared spectroscopy gas cell, in the time carrying out gaseous sample detection, with silica gel plug by gas cell bottom interface 14 jam-packs, the pond window of pond body 1 both sides is unscrewed, be filled with the gaseous sample of pre-detection by the aspirating hole 13 at pond body 1 top, estimate that in the body 1 of pond, air is replaced by sample gas substantially, by tightening of pond, the both sides window of pond body 1, and with silica gel plug by aspirating hole 13 jam-packs, put into light path detect.
Claims (8)
1. an Infrared spectroscopy gas cell, comprise pond body (1) and two pond windows (2), it is characterized in that the relative both sides of described pond body (1) are respectively equipped with coaxial port I (11) and port II (12), described two pond windows (2) are connected with pond body (1) detachable-type sealed with port II (12) by port I (11) respectively; Described pond body (1) top is provided with bleeding point (13), and described pond body (1) bottom is also provided with an outwardly bottom interface (14).
2. Infrared spectroscopy gas cell according to claim 1, is characterized in that described pond window (2) comprises window (22), and described window (22) is polyethylene film or kbr tablet.
3. Infrared spectroscopy gas cell according to claim 2, is characterized in that described polyethylene film should meet one of following two conditions:
1. in Infrared spectroscopy, in the infrared spectrogram after double-layer polyethylene film buckle back scape, at 4000cm
-1to 400cm
-1scope is interior without absorption peak;
2. in Infrared spectroscopy, in the infrared spectrogram after double-layer polyethylene film buckle back scape, at 4000cm
-1to 400cm
-1in scope, only at 2930cm
-1to 2845cm
-1between have the absorption peak of two light transmittance values>=94.0%.
4. Infrared spectroscopy gas cell according to claim 2, it is characterized in that described pond window (2) also comprises that window-frame (21) and packing ring (23), described window-frame (21) one end have internal thread, described port I (11) and port II (12) have the external thread matching with it, the end face of described window-frame (21) other end has the interior edge of annular, when connection, packing ring (23) is placed between port and window (22).
5. Infrared spectroscopy gas cell according to claim 1, is characterized in that described bottom interface (14) lower end is ground.
6. Infrared spectroscopy gas cell according to claim 1, is characterized in that at least one side outside of the upper ports having I (11) of described pond body (1) and port II (12) is also installed with several magnet pieces (15).
7. the application in Infrared spectroscopy with gas cell of the Infrared spectroscopy described in claim 1~6 any one.
8. the Infrared spectroscopy according to claim 7 application in Infrared spectroscopy with gas cell, it is characterized in that for sample for thering is volatile liquid, thering is volatile solid or gaseous sample.
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CN201410090917.5A CN103808661A (en) | 2014-03-12 | 2014-03-12 | Gas cell for infrared spectroscopy analysis |
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CN201410090917.5A CN103808661A (en) | 2014-03-12 | 2014-03-12 | Gas cell for infrared spectroscopy analysis |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104614316A (en) * | 2015-02-11 | 2015-05-13 | 中国科学技术大学 | Infrared spectrometer and reaction tank thereof |
CN105572041A (en) * | 2014-10-16 | 2016-05-11 | 北京普利生仪器有限公司 | Optical detecting equipment, optical detecting method and device and reaction cup |
CN114323819A (en) * | 2021-12-17 | 2022-04-12 | 上海航天化工应用研究所 | Device and method for collecting precipitated gas in solid propellant aging process |
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