CN102033005A - Preparation method of asphalt sample for microscopic analysis of reflected light - Google Patents
Preparation method of asphalt sample for microscopic analysis of reflected light Download PDFInfo
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- CN102033005A CN102033005A CN2009101968555A CN200910196855A CN102033005A CN 102033005 A CN102033005 A CN 102033005A CN 2009101968555 A CN2009101968555 A CN 2009101968555A CN 200910196855 A CN200910196855 A CN 200910196855A CN 102033005 A CN102033005 A CN 102033005A
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Abstract
The invention provides a preparation method of asphalt sample for microscopic analysis of reflected light, comprising the following steps of: taking typical asphalt sample to dry, heating and melting in an oven to eliminate bubble; then taking out the sample to pour in a rubber elastic module, cooling to cure in environmental temperature, demoulding a molded sample from the module; coarsely grinding the sample on an alumina waterproof abrasive paper, then finely grinding until there is no obvious scratch, taking water as lubricating agent and cooling agent, and spraying diamond-containing suspension on a polished cloth to finally polish the sample. The standardized and compact molded block can be obtained by heating-melting molding method without resin, curing agent and flake, which is good in flatness after polishing; the preparation method is convenient for manufacturing, low in cost and high in efficiency.
Description
Technical field
The present invention relates to the analytic sample preparation field, be specifically related to the preparation method of a kind of reflected light microscopic analysis with sample.
Background technology
Coal-tar pitch is the cementing agent during present raw material of wood-charcoal material is produced, carbon product by aggregate burntly pinch through mixing with cementing agent, die mould, roasting and make.External high-end user except traditional softening point (SP), toluene insolubles (TI), quinoline insolubles index requests such as (QI), also has clear and definite requirement to middle phase content to modified pitch.About 300～500 ℃, phase state in the middle of bitumen can occur in pyrolytic process forms optically anisotropic liquid crystal shape carbonaceous mutually from the parent phase matrix when molecular size, shape and distribution are favourable.Early stage what form, the centre shows as spheroidite mutually.Isoplanar molecule resembles to be arranged the equator.This equator sample is arranged can be high-visible under the polarized light that intersects.Adopt polarizing microscope, the middle phase spheroid (Mesophase beads) that has the delustring image is easy to see.
Existence mutually middle or secondary QI is unfavorable to the intensity of gained pitch coke, because it makes pitch generate cellular structure, wherein each anisotropy material is comprised in the isotropy parent, causes structural damage.It also hinders the infiltration of pitch to the coke micropore, brings defective for the structure of goods, causes aggregate Jiao to crack with the binder coke interface, reduces the intensity of carbon product.Therefore satisfying under the condition of other needs, the centre of pitch should reduced to minimum degree mutually.
GB/T 16773-1997 coal petrography analytic sample preparation method, fine coal must process mix, be pressed into briquet with cementing agent, and then grinds, is polished to mating plate; Lump coal is boiled glue, section, grinding, polishing make the lump coal mating plate; Lump coal by reinforcing, section, grinding, bonding die, grind again, operation such as modification, cover plate laminates.Its step is complicated, and efficient is low, cost is high, operation requires high.
Reflection microscopic analysis of the light of phase and assay method in the middle of ASTM D 4616-95 (2005) pitch adhere to the phenoplast ring on the thin card.For granulated samples, the potpourri of cover ring epoxy resins and hardening agent on the bonding particle in ring.Behind resin solidification, ring is filled up and solidify with the potpourri of epoxy resin and hardening agent.Also sample can be put into vacuum tank, remove gas; Sample for semi-molten after the pulverizing fills up annulus.Put into baking oven, allow pitch under this temperature, soften cohesion.It is fair with the top that cooling back is poured epoxy or plastics in the ring into, allows epoxy solidify; For the sample of fusing, sample is heated to is convenient to more than the softening point topple over, insert in the ring.A part is filled up with resin then with the pitch filling of fusing in the ring.
ASTMD 4616 also addresses a typical polishing order.On 240 order emery grinding wheels, the card face is ground off from plastic hoop, thereby expose the pitch particulate.Water is cooked lubricant and cooling medium.And then grind with 400 and 600 order emery grinding wheels respectively.With mark happy Grinding and polishing machine (loading the aluminium oxide of 0.3 μ m or the diamond compound of 3 μ m), do lubricant with adjuvant.To contain in the water of 0.05 μ m aluminium oxide suspending liquid places microcloth to go up as last brilliant polish card is polished at last.
As mentioned above, make asphalt sample in the prior art and need use auxiliary material such as resin, hardening agent, thin slice, operation is numerous and diverse, cost is higher, and the asphalt sample flatness after the moulding is bad, influences the microscopic analysis effect.
Summary of the invention
In order to solve above technical matters, the object of the present invention is to provide the preparation method of a kind of easy and simple to handle, with low cost, reflected light microscopic analysis that the gained sample surfaces is smooth with asphalt sample.
Technical scheme of the present invention is, a kind of reflected light microscopic analysis is with the preparation method of asphalt sample, and this method is carried out according to the following steps:
(1) gets asphalt sample dry below 60 ℃;
(2) be to heat melting in 110 ℃～150 ℃ baking oven or the air bath with dried asphalt sample in temperature, eliminate bubble;
(3) sample is taken out, pour the rubber elasticity mould into, cooling makes its full solidification under environment temperature, deviates from the moulding sample from mould;
(4) on pouncing paper that the sample corase grind is extremely smooth;
(5) further sample is finely ground to and does not have obvious cut;
(6) polish with polishing cloth;
(7) ultrasound wave washing sample will contain the adamantine suspending liquid of 0.05～0.1 μ m and be sprayed on and polish sample on the polishing cloth.
The drying steps of above-mentioned steps (1) can carry out in vacuum drying chamber or forced circulation watertight aircase, but also natural air drying (but the time of natural air drying is longer).As asphalt sample itself is dry, also can save step (1).
In the above-mentioned steps (2), the temperature of heating and melting will be higher than 30 ℃～50 ℃ of asphalt softening points.When heating and melting, the container of splendid attire pitch is generally steel or copper container, be convenient to beat cleaning after cold, and the pitch that shake falls to adhering to, preferably stainless.Other container also can, but can not influence asphalt quality, and cost is low.
In the above-mentioned steps (3), be about 20min～30min cool time at ambient temperature.
Above-mentioned steps (5) is finely ground to sample does not have cut, and the fine grinding process needs 3～5min.
Reflected light microscopic analysis according to the present invention in a preferred embodiment, in above-mentioned grinding, the polishing step, adopts water to do lubricant and cooling medium with the preparation method of asphalt sample.
Reflected light microscopic analysis according to the present invention is preferably with the preparation method of asphalt sample, and the described pouncing paper of step (4) is the aluminium oxide water-proof abrasive paper, and described aluminium oxide water-proof abrasive paper is 300～600 orders.
Reflected light microscopic analysis according to the present invention is preferably with the preparation method of asphalt sample, and described fine grinding step is carried out on aluminium oxide water-proof abrasive paper or emery paper.Described aluminium oxide water-proof abrasive paper or emery paper are 800 orders～1200 orders.
Reflected light microscopic analysis according to the present invention is preferably with the preparation method of asphalt sample, and in above-mentioned grinding, the polishing step, the rotating speed of used grinding and polishing dish is 150～300rpm.
The invention has the beneficial effects as follows that by the heating melting method of forming, must can not make regular, fine and close moulding asphalt blocks with resin, hardening agent, thin slice etc., flatness is good after the grinding and polishing, has advantage easy to make, that cost is low, efficient is high.The present invention adopts the rubber elasticity mould, can make the asphalt sample after the moulding both regular, deviates from easily again, and can reuse, and cost is low.In preparation method of the present invention, add thing owing to abandon, the sample homogeneous avoids heterogeneity hardness, shrinkage factor to differ and influence surface smoothness.Owing to do not add thing, when microexamination, the centre is added up mutually with quantitatively more convenient simultaneously.
Description of drawings
Fig. 1 adds the observation figure of asphalt moulding piece under polarizing microscope that resin is made.
Fig. 2 a is the observation figure of asphalt moulding sample of the present invention under 200 times of polarizing microscopes.
Fig. 2 b is the observation figure of asphalt moulding sample of the present invention under 500 times of polarizing microscopes.
Embodiment
Embodiment 1
Get representational asphalt sample 60 ℃ air-dry, get the 30g sample and put into copper molten sample spoon, be to heat melting in 150 ℃ the air bath in that temperature is set, observe until there not being obvious bubble.Then, take out sample and pour the rubber elasticity mould into, under environment temperature, cool off 20min, make its full solidification, deviate from the moulding sample from mould.On 300 order aluminium oxide water-proof abrasive papers that the sample corase grind is extremely smooth, the rotating speed number is 150rpm, and water is cooked lubricant and cooling medium.At 800 order aluminium oxide water-proof abrasive papers with sample fine grinding 3min to there not being obvious cut, rotating speed is 150rpm, water is cooked lubricant and cooling medium.With the polishing cloth polishing, rotating speed is 200rpm, and water is cooked clean-out system and cooling medium.Water cleans sample under ultrasound wave, will contain the adamantine suspending liquid of 0.1 μ m and be sprayed on the polishing cloth the last polishing of sample do.
Embodiment 2
Get representational sample 60 ℃ air-dry, get the 100g sample and put into molten sample spoon, be to heat melting in 140 ℃ the air bath in that temperature is set, observe until there not being obvious bubble.Then, take out sample and pour the rubber elasticity mould into, under environment temperature, cool off 25min, make its full solidification, deviate from the moulding sample from mould.On 400 order aluminium oxide water-proof abrasive papers that the sample corase grind is extremely smooth, rotating speed is 200rpm, and water is cooked lubricant and cooling medium.At 800 order aluminium oxide water-proof abrasive papers with sample fine grinding 3min to there not being obvious cut, rotating speed is 200rpm, water is cooked lubricant and cooling medium.With the polishing cloth polishing, rotating speed is 200rpm, and water is cooked clean-out system and cooling medium.Water cleans sample under ultrasound wave, will contain the adamantine suspending liquid of 0.1 μ m and be sprayed on the polishing cloth the last polishing of sample do.
Embodiment 3
Getting representational sample dries in 50 ℃ of drying boxes.Getting the 200g sample and put into stainless steel cup, is to heat melting in 130 ℃ the baking oven in that temperature is set, and observes until there not being obvious bubble.Then, take out sample and pour the rubber elasticity mould into, under environment temperature, cool off 30min, make its full solidification, deviate from the moulding sample from mould.On 500 order aluminium oxide water-proof abrasive papers that the sample corase grind is extremely smooth, rotating speed is 200rpm, and water is cooked lubricant and cooling medium.At 800 order aluminium oxide water-proof abrasive papers with sample fine grinding 5min to there not being obvious cut, rotating speed is 200rpm, water is cooked lubricant and cooling medium.With the polishing cloth polishing, rotating speed is 200rpm, and water is cooked clean-out system and cooling medium.Water cleans sample under ultrasound wave, will contain the adamantine suspending liquid of 0.05 μ m and be sprayed on the polishing cloth the last polishing of sample do.
Embodiment 4
Getting representational sample dries in 50 ℃ of drying boxes.Getting the 300g sample and put into stainless steel cup, is to heat melting in 130 ℃ the baking oven in that temperature is set, and observes until there not being obvious bubble.Then, take out sample and pour the rubber elasticity mould into, under environment temperature, cool off 30min, make its full solidification, deviate from the moulding sample from mould.On 600 order aluminium oxide water-proof abrasive papers that the sample corase grind is extremely smooth, rotating speed is 200rpm, and water is cooked lubricant and cooling medium.At 1200 order aluminium oxide water-proof abrasive papers with sample fine grinding 5min to there not being obvious cut, rotating speed is 300rpm, water is cooked lubricant and cooling medium.With the polishing cloth polishing, rotating speed is 300rpm, and water is cooked clean-out system and cooling medium.Water cleans sample under ultrasound wave, will contain the adamantine suspending liquid of 0.05 μ m and be sprayed on the polishing cloth the last polishing of sample do.
Embodiment 5
Getting representational sample dries in 60 ℃ drying box.Getting the 400g sample and put into stainless steel cup, is to heat melting in 110 ℃ the baking oven in that temperature is set, and observes until there not being obvious bubble.Then, take out sample and pour the rubber elasticity mould into, under environment temperature, cool off 30min, make its full solidification, deviate from the moulding sample from mould.On 600 order aluminium oxide water-proof abrasive papers that the sample corase grind is extremely smooth, rotating speed is 200rpm, and water is cooked lubricant and cooling medium.On 1200 order emery papers with sample fine grinding 5min to there not being obvious cut, rotating speed is 300rpm, water is cooked lubricant and cooling medium.With the polishing cloth polishing, rotating speed is 300rpm, and water is cooked clean-out system and cooling medium.Water cleans sample under ultrasound wave, will contain the adamantine suspending liquid of 0.05 μ m and be sprayed on the polishing cloth the last polishing of sample do.
From the contrast of Fig. 1 and Fig. 2 as can be known, compare with the asphalt sample of adding resin, the asphalt sample compact structure that the present invention prepares, the sample homogeneous is added up the centre when microexamination and quantitatively more convenient mutually.Preparation method of the present invention compares with technology in the past, has more advantage easy to make, that cost is low, efficient is high.
Claims (6)
1. a reflected light microscopic analysis is characterized in that this method is carried out according to the following steps with the preparation method of asphalt sample:
(1) gets asphalt sample dry below 60 ℃;
(2) be to heat melting in 110 ℃～150 ℃ baking oven or the air bath with dried asphalt sample in temperature, eliminate bubble;
(3) sample is taken out, pour the rubber elasticity mould into, cooling makes its full solidification under environment temperature, deviates from the moulding sample from mould;
(4) on pouncing paper that the sample corase grind is extremely smooth;
(5) further sample is finely ground to and does not have obvious cut;
(6) polish with polishing cloth;
(7) ultrasound wave washing sample will contain the adamantine suspending liquid of 0.05～0.1 μ m and be sprayed on and polish sample on the polishing cloth.
2. reflected light microscopic analysis according to claim 1 is characterized in that with the preparation method of asphalt sample, in above-mentioned grinding, the polishing step, adopts water to do lubricant and cooling medium.
3. reflected light microscopic analysis according to claim 1 is characterized in that with the preparation method of asphalt sample the described pouncing paper of step (4) is the aluminium oxide water-proof abrasive paper, and described aluminium oxide water-proof abrasive paper is 300～600 orders.
4. reflected light microscopic analysis according to claim 1 is characterized in that with the preparation method of asphalt sample described fine grinding step is carried out on aluminium oxide water-proof abrasive paper or emery paper.
5. reflected light microscopic analysis according to claim 4 is characterized in that with the preparation method of asphalt sample aluminium oxide water-proof abrasive paper or emery paper are 800 orders～1200 orders.
6. reflected light microscopic analysis according to claim 1 is characterized in that with the preparation method of asphalt sample in above-mentioned grinding, the polishing step, the rotating speed of used grinding and polishing dish is 150～300rpm.
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| CN 200910196855 CN102033005B (en) | 2009-09-30 | 2009-09-30 | Preparation method of asphalt sample for microscopic analysis of reflected light |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102680294A (en) * | 2012-05-17 | 2012-09-19 | 扬州大学 | Preparation method of modified asphalt fluorescent micro-morphological structure image source sample |
| CN103983486A (en) * | 2014-03-26 | 2014-08-13 | 江苏省沙钢钢铁研究院有限公司 | Apparatus and method of preparing micro coked sample for coke microstructure determination |
| CN104142261A (en) * | 2014-07-14 | 2014-11-12 | 中国矿业大学 | Method and device for rapidly manufacturing pulverized coal polished section by ultrasonic defoaming |
| CN104297432A (en) * | 2014-10-22 | 2015-01-21 | 中国石油天然气股份有限公司 | Method for determining resource quantity of deep crude oil cracking gas |
| CN108918230A (en) * | 2018-08-24 | 2018-11-30 | 河北工程大学 | A kind of preparation method of briquet |
| CN109001008A (en) * | 2018-09-07 | 2018-12-14 | 中国石油大学(华东) | A kind of mesophase pitch is used for sample preparation and the observation method of petrographic microscope detection |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102033004A (en) * | 2009-09-30 | 2011-04-27 | 上海宝钢化工有限公司 | Preparation method of pitch microsection |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62277491A (en) * | 1986-05-26 | 1987-12-02 | Maruzen Petrochem Co Ltd | Production of meso-phase pitch |
| JP3287227B2 (en) * | 1996-08-08 | 2002-06-04 | 三菱電機株式会社 | Micro foreign matter detection method and its detection device |
| CN101525543B (en) * | 2009-04-07 | 2013-02-06 | 汝南县东旭碳材塑料有限公司 | Preparation method for intermediate phase asphalt |
-
2009
- 2009-09-30 CN CN 200910196855 patent/CN102033005B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102033004A (en) * | 2009-09-30 | 2011-04-27 | 上海宝钢化工有限公司 | Preparation method of pitch microsection |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102680294A (en) * | 2012-05-17 | 2012-09-19 | 扬州大学 | Preparation method of modified asphalt fluorescent micro-morphological structure image source sample |
| CN103983486A (en) * | 2014-03-26 | 2014-08-13 | 江苏省沙钢钢铁研究院有限公司 | Apparatus and method of preparing micro coked sample for coke microstructure determination |
| CN103983486B (en) * | 2014-03-26 | 2017-03-08 | 江苏省沙钢钢铁研究院有限公司 | A kind of micro- coking sample preparation device for coke microscopic structure mensure and method |
| CN104142261A (en) * | 2014-07-14 | 2014-11-12 | 中国矿业大学 | Method and device for rapidly manufacturing pulverized coal polished section by ultrasonic defoaming |
| CN104297432A (en) * | 2014-10-22 | 2015-01-21 | 中国石油天然气股份有限公司 | Method for determining resource quantity of deep crude oil cracking gas |
| CN108918230A (en) * | 2018-08-24 | 2018-11-30 | 河北工程大学 | A kind of preparation method of briquet |
| CN109001008A (en) * | 2018-09-07 | 2018-12-14 | 中国石油大学(华东) | A kind of mesophase pitch is used for sample preparation and the observation method of petrographic microscope detection |
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| CN102033005B (en) | 2012-12-26 |
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