CN106644669A - Cigarette combustion cone fixing method and device - Google Patents
Cigarette combustion cone fixing method and device Download PDFInfo
- Publication number
- CN106644669A CN106644669A CN201611127086.XA CN201611127086A CN106644669A CN 106644669 A CN106644669 A CN 106644669A CN 201611127086 A CN201611127086 A CN 201611127086A CN 106644669 A CN106644669 A CN 106644669A
- Authority
- CN
- China
- Prior art keywords
- cigarette
- embedding
- combustion cone
- dodecenylsuccinic anhydride
- embedding pipe
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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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 cigarette combustion cone fixing method and device. The cigarette combustion cone fixing method has the advantages that an internal structure of a cigarette combustion cone is obtained in situ, the defect of the traditional method that in situ observation can not be carried out on a microstructure inside a cigarette combustion cone part is overcome, the microstructure of the cigarette combustion cone is reserved to the utmost extent, and evidence is provided for intensively studying a cigarette combustion process and a harmful substance production mechanism.
Description
Technical field
The present invention relates to a kind of cigarette combustion cone fixing means and device, belong to cigarette field.
Background technology
The aroma source of cigarette burns while also generating substantial amounts of harmful components, these are harmful into combustion process
The generation for dividing is closely related with fired state therefore important for tobacco business reducing tar and reducing harm has for the research of fired state
Directiveness effect.
For a long time, it is slow for the microstructure change progress during cigarette burning, essentially consist in cigarette knot
The particularity of structure, burning wimble fraction pipe tobacco fragility greatly, is highly vulnerable to breakage burning poppet surface and internal structure during cutting, therefore
And be difficult to carry out the internal structure of combustion cone the anatomy observation of original position.Therefore find a kind of simple effective and in situ can see
The Method means for examining internal microstructure change during cigarette burning are extremely necessary.
The content of the invention
It is an object of the invention to provide it is a kind of simple, efficient, accurate, the form knot of cigarette combustion cone is retained to greatest extent
Structure, original position obtains the cigarette combustion cone fixing means of cigarette combustion cone internal structure.
Another object of the present invention is to provide a kind of simple, the morphosis of cigarette combustion cone is retained to greatest extent, and
Efficiently, accurately original position obtains the cigarette combustion cone fixing device of cigarette combustion cone internal structure.
A kind of method for obtaining cigarette combustion cone internal structure in situ, is not affecting combustion cone to tie the cigarette of fired state
Extinguish rapidly on the premise of structure, go to grey part of exchanging, be subsequently placed in -10 DEG C～-5 DEG C freezen protectives；Burning tapered end is placed in into bag
In pipe laying, embedding medium I is slowly added dropwise on the premise of burning wimble structure is not affected, stands infiltration, be then further added dropwise and embed
Agent II, is heated to 40-80 DEG C, solidifies 6-48h, cutting, observation；
The composition of the embedding medium I is：1,2,3- means of dehydration of glycerol glycerin ethers, dodecenylsuccinic anhydride, N- methylols
Acrylamide；
Each component mol ratio is：1,2,3- means of dehydration of glycerol glycerin ethers/(dodecenylsuccinic anhydride+N- methylol propylene
Acid amides)=1/0.69, the wherein ratio range of dodecenylsuccinic anhydride/N hydroxymethyl acrylamide is 0.1-0.5；
The composition of the embedding medium II is：1,2,3- means of dehydration of glycerol glycerin ethers, dodecenylsuccinic anhydride, N- methylols
Acrylamide and 2,4,6- tri- (dimethylamino methyl) phenol；
Each component mol ratio is：1,2,3- means of dehydration of glycerol glycerin ethers/(dodecenylsuccinic anhydride+N- methylol propylene
Acid amides)/2,4,6- tri- (dimethylamino methyl) phenol=1:0.69:0.01, wherein dodecenylsuccinic anhydride/N- methylols third
Acrylamide=0.1-0.5.
The dodecenylsuccinic anhydride is preferably 0.25-0.45 with the mol ratio of N hydroxymethyl acrylamide.
Preferably, burning tapered end is placed in embedding pipe in the case that is vertically fixed cigarette.
The rapid method extinguished is preferably and the cigarette of fired state is placed in small-sized closed container.
So can not only quickly extinguish, and be conducive to maintaining original burning wimble structure.
The small-sized closed container is preferably glass bushing.
By using glass bushing, contribute to quick extinguishing.
The time of penetration is preferably 1-4 hours.
By controlling time of penetration within the above range, optimal osmotic effect can be reached, reduce the generation of bubble,
And while do not destroy the burning wimble structure of cigarette.
The solidification temperature is preferably 60-80 DEG C.
The hardening time is preferably 6-12 hours.
By controlling solidification temperature and hardening time, the embedding effect that can further obtain.
Preferably rectangular in shape, square, the circular or triangle of the embedding pipe for being used.
The mode of the observation is including directly observation combustion cone cross-section structure, by light microscope, scanning electron microscopy
Mirror, transmission electron microscope or confocal laser scanning microscope.
Fixing device used in above-mentioned cigarette combustion cone fixing means, including base, the base is provided with embedding pipe
Support；Embedding pipe is installed on the embedding pipe holder；The embedding tube opening is vertically arranged upward；Also install on the base
There is the cigarette clamper that can steadily move up and down；Cigarette is set to be located at just going up for embedding pipe after the cigarette clamper clamping cigarette
Side, and combustion cone is proper to embedding tube opening end.
The embedding pipe holder can stretch up and down, to adjust cigarette embedding length, meanwhile, replace embedding medium in same sample
During, it is also convenient for adjusting embedding pipe height or changing embedding pipe.
The embedding pipe preferably has the structure for adapting to cigarette shape.
So contribute to making cigarette and glass bushing preferably agree with.
The embedding pipe outer shape is preferably rectangular, square, circular or triangle.
The internal diameter of the embedding pipe is preferably 8mm～12mm.
By being defined to the internal diameter for embedding pipe, cigarette dimension can be further matched, while reducing the use of embedding medium
Amount.
Advantages of the present invention is essentially consisted in：
Present invention, avoiding conventional method cannot carry out the problem of in-situ observation to cigarette combustion cone partial internal structure, most
The microstructure of cigarette combustion cone is remained to limits, for the machine that further investigation cigarette burning process and harmful substance are produced
System provides foundation.
By the method for the present invention, the microstructure for each position of combustion cone during home position observation cigarette burning is provided
Feasibility, it is to avoid the shortcomings of combustion cone direct cutting process is frangible, remains to greatest extent during cigarette burning
Actual physical state.Meanwhile, obtained sample can further cut into slices, polishing, directly be observed, or transmission electricity
The means such as mirror, ESEM, laser confocal microscope are observed and analyzed with carrying out high-resolution, are that cigarette is fired from microcosmic angle
Burning process is analyzed the necessary means of offer.
In specific scheme, by strictly being controlled whole process and parameter, including the selection to embedding medium, ingeniously
Embed using two steps wonderfully, its composition proportion and whole sampling, embedding, solidification process are continued to optimize, and just obtain this
It is bright that efficiently, accurately original position obtains the effect of cigarette combustion cone internal structure.
The solidification effect that particularly present invention is just obtained in a short period of time, can to a great extent shorten preparation
In the cycle, improve efficiency.
As shown in the accompanying drawing of the present invention, the section that the present invention is obtained is observed by microscope, its various section
Structure is all very clear.And the Areal porosity of combustion cone obtained by can accurately measuring.
The device of the present invention is simple, simple structure, easy to operate, is each position during home position observation cigarette burning
Microstructure provides feasibility, it is to avoid the shortcomings of combustion cone cutting process is frangible, and cigarette burning is remained to greatest extent
During actual physical state；Meanwhile, cigarette is relatively fixed with embedding pipe, it is to avoid because cigarette density is little, cannot be complete
Embedding caused by the immersion embedding medium phenomenon such as not exclusively；Obtained sample can further cut into slices, polishing, be transmitted
The means such as Electronic Speculum, ESEM, laser confocal microscope are observed and analyzed with carrying out high-resolution, can be from microcosmic angle pair
Cigarette burning process is analyzed the necessary means of offer.
Description of the drawings
Fig. 1 is the cigarette combustion cone section along the axially cutting acquisition of cigarette.
Fig. 2 is the cigarette combustion cone section that transverse cuts are obtained.
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 tangent plane.Including charred portion
The structure of non-charred portion is very clear.
Fig. 4 is the schematic diagram of cigarette combustion cone fixing device used in the present invention.
Specific embodiment
Following examples are intended to the explanation present invention, rather than to the further restriction of the scope of the present invention.
Embodiment 1
Cigarette combustion cone embedding fixing step is as follows：
(1) sample：Take a cigarette sample to light, the 3rd mouthful is pumped under mode standard, rapidly cigarette is put into circle
In glass bushing, cigarette is set to extinguish rapidly.Grey part of exchanging carefully is gone to, freezen protective is treated at cigarette is placed in into -10 DEG C～-5 DEG C
With.
(2) embed：By embedding medium I：1,2,3- means of dehydration of glycerol glycerin ethers, dodecenylsuccinic anhydride, N- methylols third
Acrylamide is 1 according to mol ratio：0.2：0.49 is well mixed, and cigarette is vertically fixed, and burning tapered end is placed in embedding pipe.Slowly
Embedding medium I is instilled, is permeated 2 hours under normal temperature, be then slowly dropped into embedding medium II, each formula and ratio are 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
Mol ratio be 1：0.2：0.49：1.
(3) solidify：In being placed in baking oven, solidify 12 hours at 60 DEG C.
(4) cut：Cigarette sample after solidification is taken out from embedding pipe, is removed and is not embedded 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 carried out axially cutting, slice thickness 0.1mm (Fig. 3).It is placed in optics to show
Micro- Microscopic observation combustion cone internal structure, by pipe tobacco color its fired state and distribution are distinguished.Combustion cone length is measured simultaneously
11.58mm, area of section are 56.22mm2, and calculate the volume of combustion cone and be about 512.36mm3.By images such as Image J
Software is processed, 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 cigarette combustion cone fixing device of the present invention, including base 1, the base 1 is provided with embedding pipe
Support 6；It is circular, square or triangle to be provided with outer shape on the embedding pipe holder 6, and internal diameter is 8mm～12mm's
Embedding pipe 5；Pipe 5 is opening up is vertically arranged for the embedding；The cigarette folder that can steadily move up and down is also equipped with the base 1
Holder 2；Cigarette 3 is set to be located at the surface of embedding pipe after the cigarette clamper clamping cigarette 3, and combustion cone is rectified to embedding pipe
5 openends.
When using, a cigarette sample is taken first and is lighted, the 3rd mouthful is pumped under mode standard, rapidly cigarette is put into circle
In shape glass bushing, cigarette is set to extinguish rapidly；Grey part of exchanging carefully is gone to, cigarette 3 is vertically fixed in cigarette clamper 2,
And height is regulated, overall the stretching into of combustion cone 4 is embedded in pipe 5；It is slowly dropped under the embedding medium for being not added with curing agent, normal temperature and oozes
Saturating 2 hours；Then the height of embedding pipe holder 6 is adjusted, the embedding pipe for more renewing makes the overall bag stretched into after changing of combustion cone 4
In pipe laying, and fill the embedding medium containing curing agent of brand-new；Standing is eliminated after bubble, whole device is placed in baking oven, 60
Solidify 24 hours at DEG C；Finally the cigarette sample after solidification is taken out from embedding pipe, is removed and is not embedded part；Use precision slicing
Machine carries out cutting, obtains the axial cross section of cigarette combustion cone, and carries out subsequent analysis.
Comparative example 1
In step (2), directly with embedding medium II process, do not use embedding medium I, remaining step with embodiment 1, as a result
Produce a large amount of bubbles, it is impossible to the structure of accurate observation combustion cone.
Claims (10)
1. a kind of cigarette combustion cone fixing means, it is characterised in that the cigarette of fired state is extinguished rapidly, grey portion of exchanging is gone to
Point, it is subsequently placed in -10 DEG C～-5 DEG C freezen protectives；Embedding medium I is added dropwise, infiltration is stood, embedding medium II is then further added dropwise, plus
Heat solidifies 6-48h, cutting, observation to 40-80 DEG C；
The composition of the embedding medium I is：1,2,3- means of dehydration of glycerol glycerin ethers, dodecenylsuccinic anhydride, N- methylol propylene
Acid amides；
Each component mol ratio is：1,2,3- means of dehydration of glycerol glycerin ethers/(dodecenylsuccinic anhydride+N hydroxymethyl acrylamide)
=1/0.69, wherein dodecenylsuccinic anhydride/N hydroxymethyl acrylamide=0.1-0.5；
The composition of the embedding medium II is：1,2,3- means of dehydration of glycerol glycerin ethers, dodecenylsuccinic anhydride, N- methylol propylene
Acid amides and 2,4,6- tri- (dimethylamino methyl) phenol；
Each component mol ratio is：1,2,3- means of dehydration of glycerol glycerin ethers/(dodecenylsuccinic anhydride+N- methylol acryloyls
Amine)/2,4,6- tri- (dimethylamino methyl) phenol=1:0.69:0.01, wherein dodecenylsuccinic anhydride/N- methylol propylene
Acid amides=0.1-0.5.
2. the method according to claims 1, it is characterised in that：The dodecenylsuccinic anhydride and N- methylol propylene
The mol ratio of acid amides is 0.25-0.45.
3. the method according to claims 1 or 2, it is characterised in that：The time of penetration is 1-4 hours.
4. the method according to claims 1 or 2, it is characterised in that：The solidification temperature is 60-80 DEG C, hardening time
For 6-12 hours.
5. according to the method for claims 1, it is characterised in that：Burning tapered end is placed in into bag in the case where cigarette is vertically fixed
In pipe laying.
6. according to the method for claims 1, it is characterised in that：The rapid method extinguished be the cigarette of fired state is placed in it is little
In type closed container, the small-sized closed container is glass bushing.
7. the fixing device used in the cigarette combustion cone fixing means described in any one of claim 1-6, it is characterised in that bag
Base (1) is included, the base (1) is provided with embedding pipe holder (6)；Embedding pipe (5) is installed on embedding pipe holder (6)；
(5) are opening up is vertically arranged for the embedding pipe；The cigarette clamper that can steadily move up and down is also equipped with the base (1)
(2)；Make cigarette (3) that the surface of (5), and combustion cone (4) are managed positioned at embedding after the cigarette clamper (2) clamping cigarette (3)
Just to embedding pipe (5) openend.
8. the device according to claims 7, it is characterised in that：Embedding pipe (5) is with the knot for adapting to cigarette shape
Structure；The outer shape of embedding pipe (5) is rectangle, square, circle or triangle.
9. the device according to claims 7, it is characterised in that：Embedding pipe holder (6) can stretch up and down.
10. the device according to claims any one of 7-9, it is characterised in that：The internal diameter of embedding pipe (5) is 8mm
～12mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611127086.XA CN106644669B (en) | 2016-12-09 | 2016-12-09 | A kind of cigarette combustion cone fixing means and device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611127086.XA CN106644669B (en) | 2016-12-09 | 2016-12-09 | A kind of cigarette combustion cone fixing means and device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106644669A true CN106644669A (en) | 2017-05-10 |
| CN106644669B CN106644669B (en) | 2019-06-11 |
Family
ID=58824071
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611127086.XA Active CN106644669B (en) | 2016-12-09 | 2016-12-09 | A kind of cigarette combustion cone fixing means and device |
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| Country | Link |
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| CN (1) | CN106644669B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108303344A (en) * | 2017-12-20 | 2018-07-20 | 红云红河烟草(集团)有限责任公司 | A method of it judging cigarette combustion cone and falls |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108303344A (en) * | 2017-12-20 | 2018-07-20 | 红云红河烟草(集团)有限责任公司 | A method of it judging cigarette combustion cone and falls |
| 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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| CN106644669B (en) | 2019-06-11 |
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