CN103954576B - A kind ofly measure the method for Chemical Components in Cigarette Smoke at the adsorption form on solid adsorption material surface - Google Patents
A kind ofly measure the method for Chemical Components in Cigarette Smoke at the adsorption form on solid adsorption material surface Download PDFInfo
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Abstract
The present invention relates to infrared spectrum chemical analysis technology field, be specifically related to a kind ofly measure the method for Chemical Components in Cigarette Smoke at the adsorption form on solid adsorption material surface.The present invention is by being filled in In-situ Infrared reaction tank by solid adsorption material, and cigarette smoke volatilization or semi-volatility component are introduced in In-situ Infrared reaction tank by carrier gas and pipeline, use determination of infrared spectroscopy, analyze is carried out to infrared spectrum, thus cigarette smoke volatilization or the adsorption form of semi-volatility component on solid adsorption material surface can be obtained.Provided by the inventionly a kind ofly measure the method for Chemical Components in Cigarette Smoke at the adsorption form on solid adsorption material surface, judge the adsorptive power of different solid adsorption material adsorption active sites, for modification and the more valuable information of exploitation proposition of cigarette filter solid adsorption material, meet the demand of Harm reduction techniques technical development, there is very important realistic meaning.
Description
Technical field
The present invention relates to infrared spectrum chemical analysis technology field, be specifically related to a kind ofly measure the method for Chemical Components in Cigarette Smoke at the adsorption form on solid adsorption material surface.
Background technology
That disputes on along with smoking and health problem becomes increasingly conspicuous, tobacco business faces enormous challenge, and reducing tar and reducing harm has become direction and the trend of the development of current tobacco business.Wherein, cigarette filter sorbing material as one of the important means of reducing tar and reducing harm, enjoys the concern of researchers for the adsorption applications of harmful smoke components always.Therefore, how to judge the characterization of adsorption of solid adsorption material, namely smoke components is at the adsorption form on solid adsorption material surface, has extremely important realistic meaning for the application of sorbing material on cigarette filter.
At present, in tobacco business, measure the characterization of adsorption of certain solid adsorption material, generally from flue gas, utilize relative method directly to measure the clearance of some volatile ingredient in Chemical Components in Cigarette Smoke, thus determine the absorption property of sorbing material.And the instruments such as XRD, XPS, TEM, SEM, BET also can only play the booster action analyzing the nature measuring solid adsorption material.For the sign of the interaction mode investigated between cigarette smoke and solid adsorption material, there is not been reported.As can be seen here, only solid adsorption material is researched and developed in one-sided consideration at present, and does not note the situation of the interaction relationship between flue gas and solid adsorption material, there is significant limitation, urgently to be resolved hurrily.
Infra-red sepectrometry utilizes material to the selective absorbing of the electromagnetic radiation in infrared light district to carry out structure analysis and the compound of various absorption infrared light to be carried out to the method for qualitative and quantitative analysis as a kind of.As key atom or chemical bond and solid adsorption material interact after there is adsorption reaction, the electron cloud around key atom is become to change, the vibrational energy level transition causing into key atom is subjected to displacement, adopt the vibrational energy level transition becoming key atom in infrared spectroscopic determination molecule, the characteristic present means judging organism specific functional groups can be used as.At present, what utilize infrared spectrum characterization is the adsorption forms of some non-reversible adsorbents at solid material surface, carries out Infrared spectroscopy after usually adopting conventional compressing tablet sample preparation.And it is infeasible at the adsorption form on solid adsorption material surface to characterize Chemical Components in Cigarette Smoke after volatilization or half volatile material adopt compressing tablet sample preparation in Chemical Components in Cigarette Smoke.
And in-situ ft-ir is as important tools of analysis interactional between a kind of learning gas and solid material, be widely used in catalytic reaction and characterized the adsorption form of gas molecule on solid adsorption material surface under in-situ condition, in catalytic reaction, particularly catch the material of some Intermediates, understand the mechanism of catalytic reaction from molecular atoms angle.But adopt in-situ ft-ir to investigate in cigarette smoke volatilization or semi-volatility component on solid adsorption material surface with physisorption and chemisorption and deposit time interaction mode there is not been reported.
Therefore, in-situ ft-ir how is adopted to investigate volatilization or the adsorption form of semi-volatility component on solid adsorption material surface in cigarette smoke, thus probe into solid adsorption material characterization of adsorption, meet the demand of Tar technical development, highly practitioner in the art's research and exploitation.
Summary of the invention
The shortcoming of prior art in view of the above, the object of the present invention is to provide and a kind ofly measure the method for Chemical Components in Cigarette Smoke at the adsorption form on solid adsorption material surface, adopt in-situ ft-ir, the adsorption form of non-reversible adsorbing species on solid adsorption material surface can only be measured for solving in prior art, overcome the deficiency measuring reversible adsorption and exist in solid adsorption material adsorption form characterization technique, and then volatilize or the adsorption form of semi-volatility component on solid adsorption material in research Chemical Components in Cigarette Smoke, simultaneously can the different adsorption activity position of qualitative analysis surface excess, for modification and the more valuable information of exploitation proposition of cigarette filter solid adsorption material, meet the problem of the demand of Harm reduction techniques technical development.
For achieving the above object, the invention provides and a kind ofly measure the method for Chemical Components in Cigarette Smoke at the adsorption form on solid adsorption material surface, comprise the following steps:
Described in-situ ft-ir refers in test process, the motionless reduction adsorption material of original position is when reality absorption environment, gather the data such as the infrared spectrum of the reactions change of microcosmic with infrared ray continuous sweep, and carry out the technology of quantitative and qualitative analysis according to the data gathered.
1) Chemical Components in Cigarette Smoke is mixed with carrier gas, and mixed gas and solid adsorption material are carried out adsorption reaction;
Preferably, described solid adsorption material is selected from activated charcoal, molecular sieve, white carbon, ion exchange resin etc.Further, described molecular screening is from molecular sieve 3a, 4A, 5A, 13X, 13Z, AA.
Preferably, the concrete grammar that mixed gas and solid adsorption material carry out adsorption reaction is: described solid adsorption material is filled in In-situ Infrared reaction tank, mixed gas is introduced in In-situ Infrared reaction tank by pipeline, and is arranged in In-situ Infrared reaction tank solid adsorption material and carries out adsorption reaction.
Further, described In-situ Infrared reaction tank is arranged in infrared spectrometer.
Further, described pipeline controls sample introduction by six-way valve, and controls gas flow rate by mass flowmeter.Concrete, as shown in fig. 1, gas is from steel cylinder reduction valve out, control gas flow rate by the mass flowmeter be connected on pipeline, and control sample introduction by six-way valve, wherein, when Pulsed Sampling, controlled the switching of sampling and sample introduction by first six-way valve; And second six-way valve be connected with In-situ Infrared reaction tank, be then the switching of gating pulse sample introduction and continuous sample introduction.
Described In-situ Infrared reaction tank refers to: a kind of placement pressed powder sorbing material, and can control infrared light path in the generation diffuse reflection of solid adsorption material surface, can lead to reacting gas simultaneously and control the device of temperature of reaction.
The infrared reaction tank of described high-temp in-situ refers to: temperature of reaction can control at room temperature and above In-situ Infrared reaction tank thereof.
Described In-situ Infrared reaction tank is arranged in infrared spectrometer and refers to: In-situ Infrared reaction tank is arranged in the infrared light path of infrared spectrometer, can make infrared light, on solid adsorption material (being filled in In-situ Infrared reaction tank) surface, diffuse reflection occur.
Preferably, described Chemical Components in Cigarette Smoke is selected from carbon monoxide, crotonaldehyde, acryl aldehyde, acetaldehyde.
Further, the concentration comparable in described mixed gas in the concentration of Chemical Components in Cigarette Smoke carbon monoxide, crotonaldehyde, acryl aldehyde, acetaldehyde and actual cigarette smoke.So that the effect performance of the solid adsorption material investigated when putting into practice use.
Preferably, described carrier gas is selected from helium, argon gas, nitrogen.
Described carrier gas is the inert gas that can not have absorption at region of ultra-red.
Preferably, need before described adsorption reaction the process of solid adsorption material surface desorption.Concrete, described desorption process is at a Temperature Treatment certain hour higher than adsorption temp, solid adsorption material surface is easily decomposed and volatile composition desorption, avoids affecting baseline stability in adsorption experiment process.
Further, described desorption treatment conditions are: logical carrier gas 30min, and flow rate of carrier gas is 20mL/min, by solid adsorption material with the heating rate to 120 DEG C of 10 DEG C/min, and keep 30min, make solid adsorption material adsorption species desorption, be cooled to 30-90 DEG C, stablize 30min.
Preferably, the reaction conditions of described adsorption reaction is: adsorption reaction probe temperature: 10-100 DEG C; In mixed gas, Chemical Components in Cigarette Smoke is 0.01 ~ 2%:98 ~ 99.99% with the ratio of the volumn concentration of carrier gas; The flow velocity of mixed gas is 20mL/min; Reaction time: 30min.Preferably, described adsorption reaction probe temperature: 30-90 DEG C.
The principle of described Chemical Components in Cigarette Smoke and solid adsorption material adsorption reaction is: solid adsorption material adsorbs and is mainly divided into dispersion absorption and polarity to adsorb.Dispersion is adsorbed as solid adsorption material and adsorbate is close to each other, and its dipole moment changes, thus the absorption behavior occurred, mostly be physisorption; Polarity is adsorbed as solid adsorption material and adsorbate due to polar interaction, electron cloud transfer and and the absorption behavior occurred, mostly be chemisorption.When the absorption of generation polarity is that adsorbate is at solid absorption surface enrichment, and the electron pair of functional group there occurs transfer simultaneously, be easy to utilize the interactional adsorption form between the method for infrared spectrum judgement functional group and solid adsorption material.
2) adopt determination of infrared spectroscopy solid adsorption material surface, obtain infrared spectrum;
Preferably, described infrared spectrometer is Fourier infrared spectrograph.
Described determination of infrared spectroscopy solid adsorption material surface, obtains infrared spectrum and refers to: adopt infrared spectrometer original position METHOD FOR CONTINUOUS DETERMINATION and gather the infrared spectrum of solid adsorption material surface species.
Preferably, when described mixed gas and solid adsorption material carry out adsorption reaction, the synchronous determination of infrared spectroscopy solid adsorption material that adopts is surperficial.
Further, described synchronous employing determination of infrared spectroscopy solid adsorption material surface, when described mixed gas and solid adsorption material carry out after adsorption reaction reaches capacity and adsorb, spectrum is adopted in stopping.
Concrete, described saturated adsorption refers to: when mixed gas and solid adsorption material carry out adsorption reaction, and the synchronous determination of infrared spectroscopy solid adsorption material that adopts is surperficial, adopts spectrum continuously.When measure peak intensity in the infrared spectrum obtained change in time no longer change time, namely gas molecule reaches capacity on solid adsorption material surface adsorbed state.
Preferably, described determination of infrared spectroscopy condition is: spectral range: 4000-650cm
-1; Highest resolution: 0.4cm
-1; Signal to noise ratio (S/N ratio): 20000:1 (P-P); Beam splitter: KBr; Detecting device: MCT; Light source: the long-life is cold infrared; Sensitivity: 10ppm; Continuous sampling interval: 6-60s; Adopt spectrum quantity: 73; Detection time: 30min; Sweep velocity: 24s scans a spectrogram.
3) to step 2) measure obtain infrared spectrum analyze, thus measure Chemical Components in Cigarette Smoke at solid adsorption material table
The adsorption form in face.
The described principle analyzed of infrared spectrum to obtaining is: adsorbate is when absorption occurs on solid adsorption material surface, its functional group is at solid adsorption material surface enrichment, shifted by the functional group's electron pair adsorbed simultaneously, now can according to the change of the infrared absorption wave number of some functional group, judge which sense and solid adsorption material create to interact and formed to adsorb, and according to the displacement of infrared absorption wave number, the interactional adsorption form between functional group and solid adsorption material can be judged.
Described Chemical Components in Cigarette Smoke refers at the adsorption form on solid adsorption material surface: there is certain space structure in functional group, and after they and solid adsorption material surface atom interact, its adsorption structure has very large difference.On same solid adsorption material surface, adsorbate molecule can be had an effect with of a solid adsorption material surface atom, and same also can have an effect with multiple atom.Above different adsorption form, its adsorption power has larger difference.On different solid adsorption material surface, adsorbate molecule and single solid adsorption material surface atom interact, and the transfer form of its electron pair also has difference.The absorption behavior more than occurred, utilizes infrared means, the absorption of observation functional group at infrared band place, can obtain judging by the concrete adsorption form of binding molecule on solid adsorption material surface.Facilitate the use the sorbing material of some cheapnesss, its finishing is had to the functional group of specific adsorptive power, reach, with price solid adsorption material costly, there is identical adsorptive power.
The infrared spectrum of described smoke components can (be commonly used infrared data storehouse from database and have NISTChemistryWebBook, the NIMC organism spectrogram storehouse of SDBS and ChemExper Chemicals Directory CDD etc.) to find, the different activities position of solid adsorption material can directly judge from the power of infrared absorption peak for the adsorbance of single functional group.
As mentioned above, of the present inventionly a kind ofly measure the method for Chemical Components in Cigarette Smoke at the adsorption form on solid adsorption material surface, utilize the assay method of in-situ ft-ir, cigarette smoke volatilization or the REAL TIME INFRARED THERMAL IMAGE spectrogram of semi-volatility component after solid adsorption material adsorption is directly read by FTIR spectrum, and analyze is carried out to infrared spectrum, to investigate in cigarette smoke volatilization or semi-volatility component on solid adsorption material surface with physisorption and chemisorption, reversible adsorption and non-reversible absorption interaction mode when depositing, the surface excess of the different adsorption activity position of energy qualitative analysis simultaneously.The adsorption form of non-reversible adsorbing species on solid adsorption material surface can only be measured with prior art, overcome the deficiency measuring reversible adsorption and exist in solid adsorption material adsorption form characterization technique, volatilization or the adsorption form of semi-volatility component on solid adsorption material in research Chemical Components in Cigarette Smoke can be expanded to, for modification and the more valuable information of exploitation proposition of cigarette filter solid adsorption material, meet the demand of Harm reduction techniques technical development.
Accompanying drawing explanation
Fig. 1 is shown as the single unit system connection diagram of in-situ ft-ir of the present invention, wherein, and 1: In-situ Infrared reaction tank; 2: infrared spectrometer; 3: six-way valve; 4: mass flowmeter
Fig. 2 is shown as 3A molecular sieve of the present invention under 30 DEG C, 60 DEG C and 90 DEG C of conditions, the infrared spectrum of CO saturated adsorption
Fig. 3 is shown as 3A, 4A, 5A, 13X, 13Z and AA molecular sieve of the present invention under 30 DEG C of conditions, the infrared spectrum of CO saturated adsorption
Fig. 4 is shown as 13X molecular sieve of the present invention under 30 DEG C of conditions, crotonaldehyde, the infrared spectrum of acryl aldehyde and acetaldehyde saturated adsorption
Embodiment
Set forth the present invention further below in conjunction with specific embodiment, should be understood that these embodiments are only not used in for illustration of the present invention and limit the scope of the invention.
In the present embodiment, to comprise instrument, sample and reagent as follows for the selection of material:
1 material
1.1 instrument
The infrared reaction tank of DRK-4-NI8 high-temp in-situ (HARRICK company of the U.S.); Nicolet5700 Fourier infrared spectrograph (THERMOFISHER company of the U.S.); C100L mass flowmeter (SIERRA company of the U.S.); PMF-1 six-way valve (Nanjing Ke Lihua instrument and meter company limited)
1.2 sample and reagent
Chemical Components in Cigarette Smoke: carbon monoxide, crotonaldehyde, acryl aldehyde, acetaldehyde (99.999%, Shanghai Jiliang Standard Gas Co., Ltd.); Carrier gas: helium, argon gas, nitrogen (99.9999%, Shanghai Jiliang Standard Gas Co., Ltd.); Solid adsorption material: activated charcoal (Jacobi carbon company), white carbon (winning wound industrial group), ion exchange resin (LG-DOW company), molecular sieve: 3A, 4A, 5A, 13X, 13Z, AA (Shanghai Lvqiang New Material Co., Ltd)
Embodiment 1
1. method
1.1 pre-treatment
By molecular sieve filled for solid adsorption material 3A in In-situ Infrared reaction tank, and In-situ Infrared reaction tank is arranged in infrared spectrometer.Pass into purity be 99.9999% nitrogen gas half an hour (flow velocity 20mL/min) carry out desorption program, by in reaction in-situ pond with the heating rate to 120 DEG C of 10 DEG C/min, and keep half an hour, make molecular sieve surface adsorbing species desorption, be cooled to 30,60,90 DEG C respectively, stablize half an hour.By Chemical Components in Cigarette Smoke CO and carrier gas N
2mixing, is introduced in In-situ Infrared reaction tank by pipeline, carries out adsorption reaction with solid adsorption material.
1.2 measure
For introducing the mixed gas carrying out adsorption reaction in In-situ Infrared reaction tank with solid adsorption material, the synchronous determination of infrared spectroscopy solid adsorption material that adopts is surperficial, adopts spectrum continuously, stops adopting spectrum after adsorption reaction reaches capacity.
The reaction conditions of In-situ Infrared reaction tank is: mixed gas CO and N
2the ratio of volumn concentration: 2%:98%; Mixed gas flow velocity: 20mL/min; Adsorption reaction probe temperature: 30,60,90 DEG C; Reaction time: 30min.
Determination of infrared spectroscopy condition is: spectral range: 4000-650cm
-1; Highest resolution: 0.4cm
-1; Signal to noise ratio (S/N ratio): 20000:1 (P-P); Beam splitter: KBr; Detecting device: MCT; Light source: the long-life is cold infrared; Sensitivity: 10ppm; Continuous sampling interval: 60s; Adopt spectrum quantity: 73; Detection time: 30min; Sweep velocity: 24s scans a spectrogram.
2 analysis results and discussion
Analyze measuring the infrared spectrum obtained, concrete spectrogram is shown in Fig. 2.According to Fig. 2, under the adsorption temp of 30 DEG C and 90 DEG C, 3A molecular sieve has good absorption to CO.Under 30 DEG C and 60 DEG C of conditions, major absorbance peak is at 2013cm
-1, be attributed to the interaction of CO and single Al atom.Under 90 DEG C of conditions, major absorbance peak is at 1920cm
-1and 1865cm
-1, be attributed to the interaction of CO and two Al atom respectively, and the interaction of CO and three Al atom.Here the concentration of CO is 2%, and measured data have very high sensitivity, and signal to noise ratio (S/N ratio) S/N is=2500 ~ 8100.
As can be seen here, for Chemical Components in Cigarette Smoke CO, under condition of different temperatures, sorbing material 3A molecular sieve adsorption ability is different, therefore, select the adsorption temp 25 ~ 30 DEG C close to room temperature or high temperature 90 DEG C, can effective CO absorption molecule, at different temperatures, the adsorption form of CO is also different simultaneously.At present, conventional sorbing material, absorption property reduces along with the rising of temperature, and we have found the sorbing material 3A molecular sieve that can have better absorption property at different temperatures to Chemical Components in Cigarette Smoke CO here, be conducive to development of new and have the sorbing material of better absorption property at different temperatures.
Embodiment 2
1. method
1.1 pre-treatment
Respectively by molecular sieve filled to solid adsorption material 4A, 5A, 13X, 13Z, AA in In-situ Infrared reaction tank, and In-situ Infrared reaction tank to be arranged in infrared spectrometer.Pass into purity be 99.9999% helium atmosphere half an hour (flow velocity 20mL/min) carry out desorption program, by in reaction in-situ pond with the heating rate to 120 DEG C of 10 DEG C/min, and keep half an hour, make molecular sieve surface adsorbing species desorption, be cooled to 30 DEG C respectively, stablize half an hour.Chemical Components in Cigarette Smoke CO is mixed with carrier gas He, is introduced in In-situ Infrared reaction tank by pipeline, carry out adsorption reaction with solid adsorption material.
1.2 measure
For introducing the mixed gas carrying out adsorption reaction in In-situ Infrared reaction tank with solid adsorption material, the synchronous determination of infrared spectroscopy solid adsorption material that adopts is surperficial, adopts spectrum continuously, stops adopting spectrum after adsorption reaction reaches capacity.
The reaction conditions of In-situ Infrared reaction tank is: the ratio of the volumn concentration of mixed gas CO and He: 2%:98%; Mixed gas flow velocity: 20mL/min; Adsorption reaction probe temperature: 30 DEG C; Reaction time: 30min.
Determination of infrared spectroscopy condition is: spectral range: 4000-650cm
-1; Highest resolution: 0.4cm
-1; Signal to noise ratio (S/N ratio): 20000:1 (P-P); Beam splitter: KBr; Detecting device: MCT; Light source: the long-life is cold infrared; Sensitivity: 10ppm; Continuous sampling interval: 6s; Adopt spectrum quantity: 73; Detection time: 30min; Sweep velocity: 24s scans a spectrogram.
2 analysis results and discussion
Analyze measuring the infrared spectrum obtained, concrete spectrogram is shown in Fig. 3.Stronger according to the adsorptive power of Fig. 3,13X and 13Z molecular sieve.The aperture of 13X and 13Z molecular sieve is 1nm, be applicable to CO molecular diffusion in hole, be conducive to internal surface of hole and CO interaction of molecules, simultaneously, other molecular sieve of the silica alumina ratio of 13X and 13Z molecular sieve are high, hydroxyl and the water on surface are more, and the CO molecule like this due to hydrogen bond action absorption is also more, and comprehensive above 2 13X and 13Z molecular sieve have showed superior CO adsorptive power.In Fig. 3,2046cm
-1and 2021cm
-1the infrared absorption peak at place can be attributed to the CO of OH group absorption, 2046cm
-1and 2021cm
-1the infrared absorption peak at place can be attributed to the CO of OH group absorption, 1994cm
-1and 1970cm
-1the infrared absorption peak at place can be attributed to the CO of adsorption of metal ions in molecular sieve.Here the concentration of CO is 2%, and measured data have very high sensitivity, signal to noise ratio (S/N ratio) S/N=270 ~ 45000.
As can be seen here, for Chemical Components in Cigarette Smoke CO, under identical temperature 30 DEG C of conditions, select different sorbing materials, therefrom select best sorbing material to replace the sorbing material of existing routine.Learn the lessons from this case, modify hydroxyl, carbonyl isopolarity group at conventional absorbtion material surface, more effectively can improve the ability of its CO absorption, improve the use value of conventional absorbtion material simultaneously.
Embodiment 3
1. method
1.1 pre-treatment
By molecular sieve filled for solid adsorption material 13X in In-situ Infrared reaction tank, and In-situ Infrared reaction tank is arranged in infrared spectrometer.Pass into purity be 99.9999% argon gas half an hour (flow velocity 20mL/min) carry out desorption program, by in reaction in-situ pond with the heating rate to 120 DEG C of 10 DEG C/min, and keep half an hour, make molecular sieve surface adsorbing species desorption, be cooled to 30 DEG C, stablize half an hour.Respectively Chemical Components in Cigarette Smoke crotonaldehyde, acryl aldehyde and acetaldehyde are mixed with carrier gas Ar, introduced in In-situ Infrared reaction tank by pipeline, carry out adsorption reaction with solid adsorption material.
1.2 measure
Carry out the mixed gas of adsorption reaction for solid adsorption material, synchronously adopt determination of infrared spectroscopy solid adsorption material surface, adopt spectrum continuously, stop adopting spectrum after adsorption reaction reaches capacity.
The reaction conditions of In-situ Infrared reaction tank is: the ratio of mixed gas crotonaldehyde and the volumn concentration of Ar: 0.01%:99.99%; Mixed gas acryl aldehyde and N
2the ratio of volumn concentration: 0.01%:99.99%; Mixed gas acetaldehyde and N
2the ratio of volumn concentration: 0.01%:99.99%; Mixed gas flow velocity: 20mL/min; Adsorption reaction probe temperature: 30 DEG C; Reaction time: 30min.
Determination of infrared spectroscopy condition is: spectral range: 4000-650cm
-1; Highest resolution: 0.4cm
-1; Signal to noise ratio (S/N ratio): 20000:1 (P-P); Beam splitter: KBr; Detecting device: MCT; Light source: the long-life is cold infrared; Sensitivity: 10ppm; Continuous sampling interval: 6-60s; Adopt spectrum quantity: 73; Detection time: 30min; Sweep velocity: 24s scans a spectrogram.
2 analysis results and discussion
Analyze measuring the infrared spectrum obtained, concrete spectrogram is shown in Fig. 4.According to Fig. 4, the position of concrete infrared absorption peak marks in the drawings, and in the absorption of 13X molecular sieve surface, comparatively crotonaldehyde and acetaldehyde absorption absorption by force, can find when 3 kinds of smoke components are after 13X molecular sieve surface adsorbs, 1654cm acryl aldehyde simultaneously
-1having there is negative peak in place, and belongs to the infrared absorption position of water and hydroxyl herein.So available information is, crotonaldehyde, acryl aldehyde and acetaldehyde at the adsorption form of 13X molecular sieve surface is, the oxygen atom on aldehyde radical and the water of molecular sieve surface and hydroxyl generation interaction of hydrogen bond.Measured data have very high sensitivity, signal to noise ratio (S/N ratio) S/N=400 ~ 1270.
As can be seen here, for gas with various composition in Chemical Components in Cigarette Smoke, under identical temperature 30 DEG C of conditions, select suitable sorbing material, existing conventional absorbtion material can be replaced.And in other more cheap Conventional solid sorbing material finishing hydroxyls, carbonyl isopolarity functional group, the adsorptive power identical with price solid adsorption material costly can be reached, improve its use value.
In sum, of the present inventionly a kind ofly measure the method for Chemical Components in Cigarette Smoke at the adsorption form on solid adsorption material surface, volatilization or the adsorption form of semi-volatility component on solid adsorption material in research Chemical Components in Cigarette Smoke, simultaneously can the different adsorption activity position of qualitative analysis surface excess, according to obtained experimental result, thus judge the adsorptive power of different solid adsorption material adsorption active sites, thus utilize the sorbing material of some cheapnesss, its finishing is had to the functional group of specific adsorptive power, reach, with price solid adsorption material costly, there is identical adsorptive power.For modification and the more valuable information of exploitation proposition of cigarette filter solid adsorption material, meet the demand of Harm reduction techniques technical development.So the present invention effectively overcomes various shortcoming of the prior art and tool high industrial utilization.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all without prejudice under spirit of the present invention and category, can modify above-described embodiment or changes.Therefore, such as have in art usually know the knowledgeable do not depart from complete under disclosed spirit and technological thought all equivalence modify or change, must be contained by claim of the present invention.
Claims (7)
1. measure the method for Chemical Components in Cigarette Smoke at the adsorption form on solid adsorption material surface, comprise the following steps:
1) Chemical Components in Cigarette Smoke is mixed with carrier gas, and mixed gas and solid adsorption material are carried out adsorption reaction;
Need the process of solid adsorption material surface desorption before described adsorption reaction; Described desorption treatment conditions are: logical carrier gas 30min, and flow rate of carrier gas is 20mL/min, by solid adsorption material with the heating rate to 120 DEG C of 10 DEG C/min, and keep 30min, make solid adsorption material adsorption species desorption, be cooled to 30-90 DEG C, stablize 30min;
The reaction conditions of described adsorption reaction is: adsorption reaction probe temperature: 10-100 DEG C; In mixed gas, Chemical Components in Cigarette Smoke is 0.01 ~ 2%:98 ~ 99.99% with the ratio of the volumn concentration of carrier gas; The flow velocity of mixed gas is 20mL/min; Reaction time: 30min;
2) adopt determination of infrared spectroscopy solid adsorption material surface, obtain infrared spectrum;
3) to step 2) measure the infrared spectrum obtained and analyze, thus measure the adsorption form of Chemical Components in Cigarette Smoke on solid adsorption material surface.
2. according to claim 1ly a kind ofly measure the method for Chemical Components in Cigarette Smoke at the adsorption form on solid adsorption material surface, it is characterized in that, the concrete grammar that mixed gas and solid adsorption material carry out adsorption reaction is: described solid adsorption material is filled in In-situ Infrared reaction tank, mixed gas is introduced in In-situ Infrared reaction tank by pipeline, and is arranged in In-situ Infrared reaction tank solid adsorption material and carries out adsorption reaction.
3. according to claim 2ly a kind ofly measure the method for Chemical Components in Cigarette Smoke at the adsorption form on solid adsorption material surface, it is characterized in that, described pipeline controls sample introduction by six-way valve, and controls gas flow rate by mass flowmeter.
4. according to claim 1ly a kind ofly measure the method for Chemical Components in Cigarette Smoke at the adsorption form on solid adsorption material surface, it is characterized in that, described carrier gas is selected from helium, argon gas, nitrogen.
5. according to claim 1ly a kind ofly measure the method for Chemical Components in Cigarette Smoke at the adsorption form on solid adsorption material surface, it is characterized in that, when described mixed gas and solid adsorption material carry out adsorption reaction, the synchronous determination of infrared spectroscopy solid adsorption material that adopts is surperficial.
6. according to claim 5ly a kind ofly measure the method for Chemical Components in Cigarette Smoke at the adsorption form on solid adsorption material surface, it is characterized in that, described synchronous employing determination of infrared spectroscopy solid adsorption material surface, when described mixed gas and solid adsorption material carry out after adsorption reaction reaches capacity and adsorb, stopping adopting spectrum.
7. described a kind ofly measure the method for Chemical Components in Cigarette Smoke at the adsorption form on solid adsorption material surface according to claim 1-6 is arbitrary, it is characterized in that, described determination of infrared spectroscopy condition is: spectral range: 4000-650cm
-1; Highest resolution: 0.4cm
-1; Signal to noise ratio (S/N ratio): 20000:1P-P; Beam splitter: KBr; Detecting device: MCT; Light source: the long-life is cold infrared; Sensitivity: 10ppm; Continuous sampling interval: 6-60s; Adopt spectrum quantity: 73; Detection time: 30min; Sweep velocity: 24s scans a spectrogram.
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| CN104749129B (en) * | 2015-03-19 | 2017-07-21 | 中国环境科学研究院 | A kind of amino acid adsorbed Mechanism Study method calculated based on infrared spectrum and DFT |
| CN105334179B (en) * | 2015-11-12 | 2018-04-27 | 中南林业科技大学 | The spectrum detection device and method of wood materials glue interface adhesive penetration depth |
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