CN106644669B - A kind of cigarette combustion cone fixing means and device - Google Patents
A kind of cigarette combustion cone fixing means and device Download PDFInfo
- Publication number
- CN106644669B CN106644669B CN201611127086.XA CN201611127086A CN106644669B CN 106644669 B CN106644669 B CN 106644669B CN 201611127086 A CN201611127086 A CN 201611127086A CN 106644669 B CN106644669 B CN 106644669B
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- Prior art keywords
- cigarette
- combustion cone
- dodecenylsuccinic anhydride
- embedding
- dehydration
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/36—Embedding or analogous mounting of samples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/42—Low-temperature sample treatment, e.g. cryofixation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2873—Cutting or cleaving
Abstract
The invention discloses a kind of cigarette combustion cone fixing means and devices.The present invention obtains cigarette combustion cone internal structure by situ, the defect of in-situ observation can not be carried out to cigarette combustion cone partial interior microstructure by overcoming conventional method, the microstructure for remaining cigarette combustion cone to the maximum extent, the mechanism generated for further investigation cigarette burning process and harmful substance provide foundation.
Description
Technical field
The present invention relates to a kind of cigarette combustion cone fixing means and devices, belong to cigarette field.
Background technique
The aroma source of cigarette is burnt and also produces a large amount of harmful components simultaneously in combustion process, these it is harmful at
The generation and combustion state divided is closely related, therefore has for the research of combustion state for tobacco business reducing tar and reducing harm important
Directiveness effect.
For a long time, slow for the microstructure change progress during cigarette burning, essentially consist in cigarette knot
The particularity of structure, burning wimble fraction pipe tobacco brittleness is very big, and burning poppet surface and internal structure are highly vulnerable to breakage during cutting, therefore
And it is difficult to carry out the internal structure of combustion cone anatomy observation in situ.Therefore it finds a kind of simple and effective and can see in situ
Examine internal microstructure changes during cigarette burning Method means very it is necessary to.
Summary of the invention
It is simple, efficient, accurate that the object of the present invention is to provide one kind, retains the form knot of cigarette combustion cone to greatest extent
Structure, the cigarette combustion cone fixing means in situ for obtaining cigarette combustion cone internal structure.
Simply retain the morphosis of cigarette combustion cone to greatest extent another object of the present invention is to provide a kind of, and
Efficiently, accurately the cigarette combustion cone in situ for obtaining cigarette combustion cone internal structure fixes device.
A method of it is in situ to obtain cigarette combustion cone internal structure, the cigarette of combustion state is not being influenced into combustion cone knot
Extinguish rapidly under the premise of structure, go to grey part of exchanging, is subsequently placed in -10 DEG C~-5 DEG C freezen protectives;Burning tapered end is placed in packet
In pipe laying, embedding medium I is slowly added dropwise under the premise of not influencing to burn wimble structure, stands infiltration, embedding is then further added dropwise
Agent II is heated to 40-80 DEG C, solidifies 6-48h, cutting, observation;
The ingredient of the embedding medium I are as follows: 1,2,3- means of dehydration of glycerol glycerin ether, dodecenylsuccinic anhydride, N- methylol
Acrylamide;
Each component molar ratio are as follows: 1,2,3- means of dehydration of glycerol glycerin ether/(dodecenylsuccinic anhydride+N- methylol propylene
Amide)=1/0.69, wherein dodecenylsuccinic anhydride/N hydroxymethyl acrylamide ratio range is 0.1-0.5;
The ingredient of the embedding medium II are as follows: 1,2,3- means of dehydration of glycerol glycerin ether, dodecenylsuccinic anhydride, N- methylol
Acrylamide and 2,4,6- tri- (dimethylamino methyl) phenol;
Each component molar ratio are as follows: 1,2,3- means of dehydration of glycerol glycerin ether/(dodecenylsuccinic anhydride+N- methylol propylene
Amide)/2,4,6- tri- (dimethylamino methyl) phenol=1:0.69:0.01, wherein dodecenylsuccinic anhydride/N- methylol third
Acrylamide=0.1-0.5.
The molar ratio of the dodecenylsuccinic anhydride and N hydroxymethyl acrylamide is preferably 0.25-0.45.
Preferably, burning tapered end is placed in embedding pipe in the case where cigarette vertically being fixed.
The cigarette of combustion state is preferably placed in small-sized closed container by the method extinguished rapidly.
It can not only quickly extinguish in this way, and be conducive to maintain original burning wimble structure.
The small-sized closed container is preferably glass bushing.
By using glass bushing, help quickly to extinguish.
The time of penetration is preferably 1-4 hours.
By the way that within the above range, optimal osmotic effect can be reached, reduces the generation of bubble time of penetration control,
And the burning wimble structure of cigarette is not destroyed simultaneously.
The solidification temperature is preferably 60-80 DEG C.
The curing time is preferably 6-12 hours.
By control solidification temperature and curing time, the embedding effect that can have further obtained.
Preferably rectangular in shape, square, the round or triangle of used embedding pipe.
The mode of the observation includes directly observing combustion cone cross-section structure, passing through optical microscopy, scanning electron microscopy
Mirror, transmission electron microscope or confocal laser scanning microscope.
Device, including pedestal are fixed used in above-mentioned cigarette combustion cone fixing means, the pedestal is equipped with embedding pipe
Bracket;Embedding pipe is installed on the embedding pipe holder;The embedding tube opening is vertically arranged upward;It is also installed on the pedestal
There is the cigarette clamper that can steadily move up and down;Make after the cigarette clamper clamping cigarette cigarette be located at embedding pipe just on
Side, and combustion cone is rectified to embedding tube opening end.
The embedding pipe holder can stretch up and down, to adjust cigarette embedding length, meanwhile, in same sample displacement embedding medium
In the process, also facilitate adjusting embedding pipe height or replacement embedding pipe.
The embedding pipe preferably has the structure for adapting to cigarette shape.
Facilitate to agree with cigarette and glass bushing preferably in this way.
The outer shape of the embedding pipe is preferably rectangle, square, circle or triangle.
The internal diameter of the embedding pipe is preferably 8mm~12mm.
It is defined by the internal diameter to embedding pipe, can further match cigarette dimension, while reducing the use of embedding medium
Amount.
Advantages of the present invention essentially consists in:
The problem of can not carrying out in-situ observation to cigarette combustion cone partial internal structure the invention avoids conventional method, most
The microstructure for remaining to limits cigarette combustion cone, the machine generated for further investigation cigarette burning process and harmful substance
System provides foundation.
By means of the present invention, the microstructure for each position of combustion cone during home position observation cigarette burning provides
Feasibility, avoids the disadvantages of direct cutting process of combustion cone is frangible, during remaining cigarette burning to the maximum extent
Actual physical state.Meanwhile obtained sample can be further sliced, polishing treatment, directly be observed, or transmission electricity
The means such as mirror, scanning electron microscope, laser confocal microscope are observed and are analyzed with carrying out high-resolution, to fire from microcosmic angle to cigarette
Burning process carries out analysis and provides necessary means.
In specific scheme, by carrying out strict control to whole process and parameter, including the selection to embedding medium, ingeniously
Two steps of application embed wonderfully, and composition proportion and entire sampling, embedding, solidification process are continued to optimize, and just obtain this hair
It is bright that efficiently, accurately original position obtains the effect of cigarette combustion cone internal structure.
The solidification effect especially of the invention just obtained in a short period of time, can largely shorten preparation
Period improves efficiency.
As shown in attached drawing of the invention, observed by the slice that microscope obtains the present invention, various sections
Structure is all very clear.And it can accurately measure the Areal porosity of gained combustion cone.
The device of the invention is simple, and structure is simple and convenient to operate, and is each position during home position observation cigarette burning
Microstructure provides feasibility, avoids the disadvantages of combustion cone cutting process is frangible, remains cigarette burning to the maximum extent
Actual physical state in the process;Meanwhile cigarette and embedding pipe are relatively fixed, avoid since cigarette density is small, can not be complete
Immerse phenomena such as embedding caused by embedding medium is incomplete;Obtained sample can further be sliced, polishing treatment, be transmitted
The means such as Electronic Speculum, scanning electron microscope, laser confocal microscope are observed and are analyzed with carrying out high-resolution, can be from microcosmic angle pair
Cigarette burning process carries out analysis and provides necessary means.
Detailed description of the invention
Fig. 1 is the cigarette combustion cone slice along the axially cutting acquisition of cigarette.
Fig. 2 is the cigarette combustion cone slice that transverse cuts obtain.
Fig. 3 is cigarette combustion cone center axial slice.
Can be seen that the present invention from Fig. 1-Fig. 3 can obtain the structure of gem-pure each section.Including charred portion
The structure of non-charred portion is very clear.
Fig. 4 is the schematic diagram of the fixed device of cigarette combustion cone used in the present invention.
Specific embodiment
Following embodiment is intended to illustrate invention, rather than further limits to the scope of the present invention.
Embodiment 1
It is as follows that cigarette combustion cone embeds fixing step:
(1) it samples: taking a cigarette sample to light, third mouth is pumped under mode standard, cigarette is put into circle rapidly
In glass bushing, extinguish cigarette rapidly.Grey part of exchanging carefully is gone to, cigarette is placed in freezen protective at -10 DEG C~-5 DEG C and is waited for
With.
(2) it embeds: by embedding medium I:1,2,3- means of dehydration of glycerol glycerin ether, dodecenylsuccinic anhydride, N- methylol third
Acrylamide is uniformly mixed according to molar ratio for 1:0.2:0.49, and cigarette is vertically fixed, and burning tapered end is placed in embedding pipe.Slowly
Embedding medium I is instilled, permeate 2 hours under room temperature, is then slowly dropped into embedding medium II, is respectively formulated and ratio is as follows: 1,2,3- the third three
Dehydration of alcohols glycerin ether, dodecenylsuccinic anhydride, N hydroxymethyl acrylamide and 2,4,6- tri- (dimethylamino methyl) phenol
Molar ratio be 1:0.2:0.49:1.
(3) solidify: being placed in baking oven, solidify 12 hours at 60 DEG C.
(4) it cuts: the cigarette sample after solidification being taken out from embedding pipe, removes and does not embed part.Use precision slicer
Cutting is carried out, the axial cross section of cigarette combustion cone is obtained.
The microscope observation analysis of cigarette combustion cone
The cigarette combustion cone embedded samples of acquisition are subjected to axially cutting, slice thickness 0.1mm (Fig. 3).It is aobvious to be placed in optics
Micro- microscopic observation combustion cone internal structure distinguishes its combustion state and distribution by pipe tobacco color.Combustion cone length is measured simultaneously
11.58mm, area of section 56.22mm2, and the volume for calculating combustion cone is about 512.36mm3.Pass through the images such as Image J
Processing software, the Areal porosity for calculating the cigarette sample combustion cone is 33.2%, significantly less than the Areal porosity of unburned part
50.1%.
Embodiment 2
As shown in figure 4, the fixed device of cigarette combustion cone of the invention, including pedestal 1, the pedestal 1 are equipped with embedding pipe
Bracket 6;Outer shape is installed for round, square or triangle on the embedding pipe holder 6, internal diameter is 8mm~12mm's
Embed pipe 5;The embedding pipe 5 is opening up to be vertically arranged;The cigarette folder that can steadily move up and down is also equipped on the pedestal 1
Holder 2;The cigarette clamper clamps the surface for making cigarette 3 be located at embedding pipe after cigarette 3, and combustion cone is rectified to embedding pipe
5 open ends.
In use, a cigarette sample is taken to light first, it is pumped to third mouth under mode standard, cigarette is put into circle rapidly
In shape glass bushing, extinguish cigarette rapidly;Grey part of exchanging carefully is gone to, cigarette 3 is fixed on vertically in cigarette clamper 2,
And height is regulated, protrude into combustion cone 4 integrally in embedding pipe 5;It is slowly dropped into the embedding medium for being not added with curing agent, is seeped under room temperature
Saturating 2 hours;Then the height of embedding pipe holder 6 is adjusted, the embedding pipe more renewed makes combustion cone 4 integrally protrude into the packet after replacement
In pipe laying, and fill the embedding medium containing curing agent of brand-new;After standing eliminates bubble, whole device is placed in baking oven, 60
Solidify 24 hours at DEG C;The cigarette sample after solidification is taken out from embedding pipe finally, removes and does not embed part;Use precision slicing
Machine carries out cutting, obtains the axial cross section of cigarette combustion cone, and carry out subsequent analysis.
Comparative example 1
It in step (2), is directly handled with embedding medium II, is not used embedding medium I, remaining step is with embodiment 1, as a result
Generate a large amount of bubbles, can not accurate observation combustion cone structure.
Claims (6)
1. a kind of cigarette combustion cone fixing means, which is characterized in that extinguish the cigarette of combustion state rapidly, go to grey portion of exchanging
Point, it is subsequently placed in -10 DEG C~-5 DEG C freezen protectives;Embedding medium I is added dropwise, stands infiltration, embedding medium II is then further added dropwise, adds
Heat solidifies 6-48h, cutting, observation to 40-80 DEG C;
The ingredient of the embedding medium I are as follows: 1,2,3- means of dehydration of glycerol glycerin ether, dodecenylsuccinic anhydride, N- methylol propylene
Amide;
Each component molar ratio are as follows: 1,2,3- means of dehydration of glycerol glycerin ether/(dodecenylsuccinic anhydride+N hydroxymethyl acrylamide)
=1/0.69, wherein dodecenylsuccinic anhydride/N hydroxymethyl acrylamide=0.1-0.5;
The ingredient of the embedding medium II are as follows: 1,2,3- means of dehydration of glycerol glycerin ether, dodecenylsuccinic anhydride, N- methylol propylene
Amide and 2,4,6- tri- (dimethylamino methyl) phenol;
Each component molar ratio are as follows: 1,2,3- means of dehydration of glycerol glycerin ether/(dodecenylsuccinic anhydride+N- methylol acryloyl
Amine)/2,4,6- tri- (dimethylamino methyl) phenol=1:0.69:0.01, wherein dodecenylsuccinic anhydride/N- methylol propylene
Amide=0.1-0.5.
2. according to the method described in claim 1, it is characterized by: the dodecenylsuccinic anhydride and N- methylol acryloyl
The molar ratio of amine is 0.25-0.45.
3. method according to claim 1 or 2, it is characterised in that: the time of the infiltration is 1-4 hours.
4. method according to claim 1 or 2, it is characterised in that: the cured temperature is 60-80 DEG C, when cured
Between be 6-12 hours.
5. the method according to claim 1, it is characterised in that: burning tapered end is placed in embedding in the case where cigarette is vertically fixed
Guan Zhong.
6. the method according to claim 1, it is characterised in that: the method extinguished rapidly is small-sized for the cigarette of combustion state to be placed in
In closed container, the small-sized closed container is glass bushing.
Priority Applications (1)
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CN201611127086.XA CN106644669B (en) | 2016-12-09 | 2016-12-09 | A kind of cigarette combustion cone fixing means and device |
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CN201611127086.XA CN106644669B (en) | 2016-12-09 | 2016-12-09 | A kind of cigarette combustion cone fixing means and device |
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CN106644669B true CN106644669B (en) | 2019-06-11 |
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CN108303344B (en) * | 2017-12-20 | 2020-04-17 | 红云红河烟草(集团)有限责任公司 | Method for judging falling of cigarette combustion cone |
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