CN105067648A - Pretreatment method of soot structure morphology tests under different working conditions - Google Patents
Pretreatment method of soot structure morphology tests under different working conditions Download PDFInfo
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- CN105067648A CN105067648A CN201510452802.0A CN201510452802A CN105067648A CN 105067648 A CN105067648 A CN 105067648A CN 201510452802 A CN201510452802 A CN 201510452802A CN 105067648 A CN105067648 A CN 105067648A
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Abstract
The invention provides a pretreatment method of soot structure morphology tests under different working conditions. The pretreatment method comprises the following steps: collecting a proper amount of diesel engine particles (PM) from the tail gas from a diesel engine, drying the particles at a constant temperature, weighing part of the PM sample, pouring the weighed PM sample into a test tube, adding a proper amount of dichloromethane into the test tube; vibrating the test tube by ultrasonic waves, then subjecting the test tube to a centrifugation treatment; pouring out the upper-layer solution, adding a proper amount of dichloromethane for another time; repeating the previous steps for several times, pouring out the upper-layer solution, placing the test tube on a test tube rack; dropwise adding the solution in the test tube onto a silicon sheet or cooper net by a pipette so as to obtain a sample, and finally detecting the sample on the silicon sheet or copper net to obtain the structure morphology of DS. According to the method, SOF and inorganic salts in DS can be effectively removed, moreover, the particle agglomeration and layering phenomenon are reduced, and the pretreatment method has the advantages that the operation is simple and is easy to control, and the repeatability is high.
Description
Technical field
The present invention relates to the detection analysis field of diesel emission, relate generally to a kind of preprocess method to soot (DS) tissue topography test under different operating mode.
Background technology
Having the features such as low oil consumption, high thermal efficiency and good reliability due to diesel engine, there is dieselization trend in worldwide vehicular engine; Due to the inherent characteristics of diesel engine mixed Daqu and burning, noxious emission main in exhaust is NO
xwith particulate PM, compare with gasoline engine, diesel engine NO
xdischarge capacity and gasoline engine be substantially in same order, and the discharge capacity of PM is about 30 ~ 50 times of gasoline engine; Diesel engine PM is then primarily of 3 fractions compositions, i.e. soot (DS), soluble organic (SOF), inorganic salts and other some polymkeric substance, SOF is the high boiling point organic compound be adsorbed on soot, the inorganic salts sulfide that mainly sulphur composition produces in diesel oil.
Because the particle in diesel engine vent gas has very large harm to health, affect the growth of teenager's pulmonary function, the weight of ewborn infant, neuronal function, shorten the life-span etc. of crowd; The particularly diameter particle (PM10) that is less than 10 μm, stop because it is tiny not by people's nasal cavity, directly can enter human body, the particle that particle diameter is less than 1 μm, can at deep lung extended stationary periods, not easily be excluded external, and each organ of whole body can be entered with blood circulation, be, in particle, a maximum class is threatened to health, therefore, Abgasgesetz is put into effect in succession in countries in the world, the discharge of restriction diesel particulate.
According to correlative study, diesel engine carbon black and particle have very strong correlativity, therefore often set about studying from the test of soot; And due to the liquids and gases (being mainly SOF and inorganic salts) in soot meeting absorption tail gas, the tissue topography of soot can be made to analyze and produce comparatively big error, it is very necessary for therefore carrying out effective pre-service to soot before the study; The difference of load condition can affect SOF and inorganic salt content that soot adsorbs, and SOF discharge capacity when middle Smaller load is comparatively large, and when large load, discharge is less; And DS to be emitted on middle Smaller load less, during large load, discharge is larger; In order to reflect the tissue topography of soot more really, corresponding pre-service need be carried out according to different load operating mode, SOF in soot and inorganic salts can be eliminated by pre-service, reduce particle agglomeration and stratification, improve the sharpness of soot tissue topography.
Summary of the invention
The object of the present invention is to provide one effectively can to remove under different operating mode SOF and inorganic salts ingredients in soot, alleviate particle agglomeration and stratification, improve the preprocess method of soot tissue topography measuring resolution.
1. according to an aspect of the present invention, provide a kind of preprocess method to soot (DS) tissue topography test under different operating mode.Described preprocess method comprises:
(1) from diesel engine vent gas, gather PM, freeze-day with constant temperature, take part PM sample, be poured in test tube, add q. s. methylene chloride solution;
(2) ultrasonic vibration, hydro-extractor is separated;
(3) pour out upper solution, again add q. s. methylene chloride;
(4) after repeating above-mentioned (2) (3) step several times, pour out upper solution, test tube is statically placed on test tube rack, utilize liquid-transfering gun solution in test tube to be dripped obtained sample on silicon chip or copper mesh.
Utilize scanning electron microscope (SEM), transmission electron microscope (TEM) tests to the sample on silicon chip or copper mesh the tissue topography's feature obtaining DS.
2. according to an aspect of the present invention, baking temperature is at 35 ~ 50 DEG C at 20 ~ 35h drying time in drying box for PM.
3. according to an aspect of the present invention, described test tube capacity is 10 ~ 15ml test tube, and PM sample quality is 0.06 ~ 0.10mg.
4. according to an aspect of the present invention, described methylene chloride purity>=99%, methylene chloride is PM/CH
2cl
2=0.1mg/9ml ~ 0.1mg/12ml.
5. according to an aspect of the present invention, under small load condition (0 ~ 85%), under high load working condition (85 ~ 100%), the ultrasonic vibration time is at 23 ~ 30min at 18 ~ 23min the ultrasonic vibration time.
6. according to an aspect of the present invention, centrifuge speed is at 18000 ~ 23000r/min, and centrifugation time is at 4 ~ 5min.
7. according to an aspect of the present invention, pour out upper solution, surplus solution, at 0.5 ~ 1ml, adds methylene chloride again.
8. according to an aspect of the present invention, at 6 ~ 10 times under multiplicity requirement small load condition (0 ~ 25%), at 4 ~ 6 times under moderate duty operating mode (25 ~ 85%), under high load working condition (85 ~ 100%), multiplicity is at 3 ~ 4 times.
9. according to an aspect of the present invention, liquid-transfering gun drips the solution on silicon chip or TEM copper mesh is 1 ~ 3.
10. according to an aspect of the present invention, a kind of preprocess method to soot (DS) tissue topography test under different operating mode is provided, described method comprises the steps: to carry out pre-service by above-mentioned preprocess method to diesel particulate (PM) sample, obtain supernatant as sample, utilize scanning electron microscope (SEM), transmission electron microscope (TEM) measures the tissue topography of DS.
11. according to an aspect of the present invention, and the ultrasonic vibration time is too short, and soot agglomeration can not get effective improvement, ultrasonic vibration overlong time, easily causes soot too to disperse, be unfavorable for the observation to tissue topography; Under high load working condition, in PM, soot proportion is comparatively large, during concussion that need be longer chien shih its obtain good dispersion.
12. according to an aspect of the present invention, low repetition, then the SOF in soot is too much residual, and reaching described multiplicity can effectively eliminate SOF and inorganic salts; Along with load increases, in PM, SOF proportion reduces, and only needs less multiplicity just effectively can remove SOF in soot and inorganic salts.
Accompanying drawing explanation
Fig. 1 is the SEM figure of untreated samples.
Fig. 2 is the SEM figure of sample after process.
Fig. 3 is the TEM of untreated samples.
Fig. 4 is the TEM figure of sample after process.
Embodiment
Below by embodiment in detail the present invention is described in detail, but the invention is not restricted to down describe embodiment.
embodiment 1
1 ~ 2mgPM is gathered from diesel engine vent gas, preserved in double dish, put into drying box 40 DEG C of dry 24h, from double dish, take 0.08mgPM sample, be poured in 10ml test tube, add dichloromethane solution to 9ml, then ultrasonic vibration 20min, with the centrifugal 5min of hydro-extractor 20000r/min, pours out upper solution, until surplus solution 1ml, again add methylene chloride to 9mL; Repeat above-mentioned steps 5 times, pour out upper solution, test tube is statically placed on test tube rack, utilize liquid-transfering gun solution in test tube to be dripped 2 obtained samples on silicon chip or copper mesh, utilize scanning electron microscope (SEM), the tissue topography of transmission electron microscope (TEM) working sample.
comparative example 1
1 ~ 2mgPM is gathered from from diesel engine vent gas, take 0.08mgPM sample, be poured in 10ml test tube, add dichloromethane solution to 9ml, shake test tube 5min, is statically placed in test tube on test tube rack, utilizes liquid-transfering gun solution in test tube to be dripped 2 obtained samples on silicon chip or copper mesh, utilize scanning electron microscope (SEM), the tissue topography of transmission electron microscope (TEM) working sample.
From Fig. 1,2, untreated front oily matter is bonded together, and surface profile is fuzzy.After process, PM bonding shape phenomenon alleviates, and present a kind of loose porous form, surface structure also becomes more obvious.
From Fig. 3,4, after process, agglomeration and stratification effectively alleviate, and image is more clear.
Claims (10)
1., to a preprocess method for soot tissue topography test under different operating mode, it is characterized in that described preprocess method comprises the steps:
(1) from diesel engine vent gas, gather PM, freeze-day with constant temperature, take part PM sample, be poured in test tube, add q. s. methylene chloride solution;
(2) ultrasonic vibration, hydro-extractor is separated;
(3) pour out upper solution, again add q. s. methylene chloride;
(4) after repeating above-mentioned (2) (3) step several times, pour out upper solution, utilize liquid-transfering gun solution in test tube to be dripped obtained sample on silicon chip or copper mesh.
2. pre-service way according to claim 1, is characterized in that: PM freeze-day with constant temperature 20 ~ 35h, baking temperature 35 ~ 50 DEG C.
3. pre-service way according to claim 1, is characterized in that: described test tube capacity is 10 ~ 15ml, PM sample quality is 0.06-0.10mg.
4. pre-service way according to claim 1, is characterized in that: described methylene chloride purity>=99%, and methylene chloride is PM/CH
2cl
2=0.1mg/9ml ~ 0.1mg/12ml.
5. pre-service way according to claim 1, is characterized in that: in, under small load condition (0 ~ 85%), under high load working condition (85 ~ 100%), the ultrasonic vibration time is at 23 ~ 30min at 18 ~ 23min the ultrasonic vibration time.
6. pre-service way according to claim 1, is characterized in that: centrifuge speed is at 18000 ~ 23000r/min, and centrifugation time is at 4 ~ 5min.
7. pre-service way according to claim 1, is characterized in that: pour out upper solution, and surplus solution, at 0.5 ~ 1ml, adds methylene chloride again.
8. pre-service way according to claim 1, it is characterized in that: at 6 ~ 10 times under multiplicity requirement small load condition (0 ~ 25%), at 4 ~ 6 times under moderate duty operating mode (25 ~ 85%), under high load working condition (85 ~ 100%), multiplicity is at 3 ~ 4 times.
9. pre-service way according to claim 1, is characterized in that: the liquid-transfering gun solution dripped on silicon chip or copper mesh is 1 ~ 3.
10. the preprocess method to soot (DS) tissue topography test under different operating mode, it is characterized in that described method comprises the steps: to carry out pre-service by the preprocess method described in claim arbitrary in claim 1 ~ 9 to diesel particulate (PM) sample, obtain supernatant drop in silicon chip or copper mesh as test sample, utilize scanning electron microscope (SEM), transmission electron microscope (TEM) tests to the sample on silicon chip or copper mesh the tissue topography's feature obtaining DS.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106596357A (en) * | 2016-11-28 | 2017-04-26 | 江苏大学 | Method for characterizing morphologies of particulate matters in diesel |
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| US20060108535A1 (en) * | 2002-12-20 | 2006-05-25 | Pedersen Niels H | Apparatus and a method of determining hydrogen by use of a neutron source |
| CN103630471A (en) * | 2013-11-20 | 2014-03-12 | 江苏大学 | Method for measuring median particle diameter of particles in exhaust gas of diesel engine |
| CN203745204U (en) * | 2013-07-12 | 2014-07-30 | 江苏大学 | Visual testing device for spraying and combustion dynamic conditions in diesel engine cylinder |
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2015
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060108535A1 (en) * | 2002-12-20 | 2006-05-25 | Pedersen Niels H | Apparatus and a method of determining hydrogen by use of a neutron source |
| CN203745204U (en) * | 2013-07-12 | 2014-07-30 | 江苏大学 | Visual testing device for spraying and combustion dynamic conditions in diesel engine cylinder |
| CN103630471A (en) * | 2013-11-20 | 2014-03-12 | 江苏大学 | Method for measuring median particle diameter of particles in exhaust gas of diesel engine |
Non-Patent Citations (2)
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| 李芳: "柴油发动机颗粒排放物的组分研究", 《南京信息工程大学硕士学位论文》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106596357A (en) * | 2016-11-28 | 2017-04-26 | 江苏大学 | Method for characterizing morphologies of particulate matters in diesel |
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Application publication date: 20151118 |