CN113804678B - Method for detecting coke reaction depth - Google Patents
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- CN113804678B CN113804678B CN202010549787.2A CN202010549787A CN113804678B CN 113804678 B CN113804678 B CN 113804678B CN 202010549787 A CN202010549787 A CN 202010549787A CN 113804678 B CN113804678 B CN 113804678B
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- 239000000571 coke Substances 0.000 title claims abstract description 236
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 128
- 238000000034 method Methods 0.000 title claims abstract description 32
- 230000003287 optical effect Effects 0.000 claims description 14
- 230000004580 weight loss Effects 0.000 claims description 13
- 239000003822 epoxy resin Substances 0.000 claims description 12
- 238000000227 grinding Methods 0.000 claims description 12
- 229920000647 polyepoxide Polymers 0.000 claims description 12
- 238000004891 communication Methods 0.000 claims description 11
- 238000001514 detection method Methods 0.000 claims description 9
- 239000012780 transparent material Substances 0.000 claims description 2
- 239000011148 porous material Substances 0.000 description 26
- 208000016261 weight loss Diseases 0.000 description 12
- 230000009257 reactivity Effects 0.000 description 11
- 230000008859 change Effects 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 210000001015 abdomen Anatomy 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 238000010191 image analysis Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 208000020442 loss of weight Diseases 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
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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
- G01N1/286—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
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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
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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
- G01N1/286—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
- G01N2001/2866—Grinding or homogeneising
-
- 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
- G01N2001/366—Moulds; Demoulding
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
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- Length Measuring Devices By Optical Means (AREA)
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Abstract
The invention discloses a method for detecting coke reaction depth, which mainly solves the technical problem that the existing coke reaction depth cannot be accurately detected. The technical proposal is as follows: a method for characterizing coke reaction depth, comprising the steps of: 1) Preparing a sample after coke reaction; 2) Collecting an image of a sample after coke reaction; 3) Calculating the reaction depth of the coke, wherein the reaction depth of the coke is calculated according to a formula I, and p= (R-R)/R multiplied by 100 percent of formula I, wherein in the formula I, p is the reaction depth of the coke, and the unit is; r is the radius of the focal sphere sample before reaction, and the unit is mm; and r is the radial distance from the deepest position of the reacted coke communicating air hole to the center of the sample after the coke is reacted, and the unit is mm. The method can intuitively study the quality characteristics of the coke after the coke is reacted under different reaction conditions.
Description
Technical Field
The invention relates to a method for detecting coke performance after coke reaction, in particular to a method for detecting coke reaction depth, and belongs to the technical field of coking.
Background
Coke is an irregular porous body with a hard texture and carbon as a main component and containing cracks and defects, and is silver gray. The vertical and horizontal cracks can be seen by visual inspection of the coke. The coke pieces still contain microcracks, which break along the coarse longitudinal and transverse cracks. And separating the coke blocks along the microcracks to obtain a coke porous body, which is also called a coke body. The coke body is composed of air holes and air hole walls, which are also called Jiao Zhi, and the main components of the coke body are carbon and mineral substances.
Coke porosity determines coke strength and also determines the reactivity of coke in a blast furnace, so researchers have conducted a great deal of research on coke reactivity, and national standards have studied the quality characteristics of coke after reaction by coke reactivity and post-reaction strength.
The Chinese patent document with publication number CN101825548A discloses a method and a device for detecting the reactivity and the post-reaction heat-treatability of coke, and detects the start temperature, the reactivity and the post-reaction heat-treatability of coke. The detection method adopts an electric furnace as a heating furnace and adopts an electronic balance for weighing. The coke reactivity detection is carried out under isothermal conditions after the temperature rise, the weight loss of a coke sample is measured by an electronic balance, and when the coke weight loss rate reaches a specified value, the weight loss rate is detected as a reactivity index; and detecting the heat treatability after the coke reaction, and continuously heating under the protection of inert gas when the coke weight loss rate reaches a specified value, wherein the coke mass loss rate during the heat treatment is detected as a post-reaction heat treatability index. The method and the device provided by the invention have the advantages that the detection temperature reaches 1500-1600 ℃, and the thermal property characterization of the coke of the furnace belly (in front of the tuyere) and the furnace hearth can be displayed. The invention greatly improves the accuracy of measurement, shortens the measurement time and reduces the labor intensity of measurement operation. The method expands the coke reaction temperature and takes the coke mass loss rate as an evaluation index.
Paper (Wang Jieping, xie Quanan, sun Zhang, ji, liang Yinghua, iron and steel, 2015,50 (11) 8-13) is used for measuring the carbon dissolution reaction of coke at different temperatures by using a coke reactivity device, a specific surface area and aperture analyzer and SEM are used for representing pore structure parameters of the coke, a BET equation and a BJH method are used for calculating the specific surface area, the pore volume and the average aperture of the coke respectively, and an adsorption isotherm is used for calculating the fractal characteristic change of the coke surface, so as to examine the change rule of the pore structure in the carbon dissolution reaction process of the coke. Along with the temperature rise, the coke adsorption curve type is changed from the I-class to the II-class adsorption isotherm, the specific surface area and the pore volume are increased and then reduced, and the pore diameter change of 2-10 nm is obvious. The fractal dimension has a certain correlation with the pore structure, and can reflect the change of pores in the coke dissolution loss process. The method characterizes the pore structure change after the coke reaction by the pore fractal dimension.
In summary, the method characterizes the quality characteristics of the coke after the reaction, characterizes the coke by the weight loss rate, characterizes the coke by the fractal dimension of the air holes, can reflect the coke reaction quantity and the coke reaction, but cannot intuitively reflect the reaction depth of the coke.
For this purpose the invention proposes the use of an optical microscope for determining the depth of coke reaction by image analysis.
Disclosure of Invention
The invention aims to provide a method for detecting the reaction depth of coke, which mainly solves the technical problem that the existing coke reaction depth cannot be accurately detected, solves the problems that the existing coke reactivity can only be represented by the reaction weight loss rate and cannot react the weight loss position, and provides a novel method for quality description after the coke reaction.
The coke reaction depth refers to the ratio of the length of a coke communication air hole in the radial direction of the coke to the original coke radius after the reaction, which is expressed as the% of the coke reaction depth, when the coke ball with a certain radius reacts to a certain weight loss rate at a certain temperature. The method utilizes an optical microscope to observe the reacted coke communication air holes so as to determine the positions of the coke communication air holes.
The coke is a porous structure, and the coke pore structure determines the macroscopic properties of the coke. Different reaction depths of the coke reflect different damage degrees of the air holes to the coke, and reflect the shatter resistance and pulverization resistance of the coke after the coke reacts in the blast furnace. Because the coke mainly plays a skeleton role in the blast furnace, the coke is required to have good shatter resistance and pulverization resistance, and the lower the reaction depth of the coke is, the more complete the coke is, and the more beneficial to blast furnace ironmaking is.
The technical scheme adopted by the invention is that the method for detecting the reaction depth of the coke comprises the following steps:
1) Preparing a coke reaction sample, grinding the coke sample to be detected into a coke ball sample with the radius R of 12-15 mm, placing a Jiao Qiu sample in a coke reactor, and controlling a Jiao Qiu sample to react at 1050-1250 ℃ until the weight loss reaches 20-30% of the original mass; taking out the reacted coke ball sample from the coke reactor, transferring the reacted coke ball sample into a grinding tool in a vacuum chamber, controlling the vacuum degree of the vacuum chamber to be 50-60 kpa, pouring epoxy resin into the grinding tool in which the reacted coke ball sample is placed, and standing for 8-10 h until the epoxy resin on the surface of the reacted coke ball sample is hardened; taking out the reacted coke ball sample from the vacuum bin, cutting the reacted coke ball sample along the diameter direction, and throwing the reacted coke ball sample Jiao Qiumo until the reacted coke ball sample meets the detection requirement of an optical microscope to obtain a coke reacted sample:
2) Collecting an image of a sample after coke reaction, collecting an image of the sample after coke reaction by using an optical microscope, and obtaining an image overall view of the sample after coke reaction by image stitching, wherein the deepest part of the sample after coke reaction, which is the deepest position which can be reached by a coke communication air hole after reaction, is obtained by immersing epoxy resin displayed on the image of the sample after coke reaction into the deepest position of the sample after coke reaction, and the radial distance from the deepest position which can be reached by the coke communication air hole after reaction to the center of the sample after coke reaction is r;
3) Calculating the reaction depth of the coke, wherein the reaction depth of the coke is calculated according to a formula I, and p= (R-R)/R multiplied by 100 percent of formula I, wherein in the formula I, p is the reaction depth of the coke, and the unit is; r is the radius of the focal sphere sample before reaction, and the unit is mm; and r is the radial distance from the deepest position of the reacted coke communicating air hole to the center of the sample after the coke is reacted, and the unit is mm.
Further, in the step 1), the upper cover of the vacuum bin is made of transparent materials, and in the process of preparing the sample after the coke reaction, the sample can be observed.
Further, in the step 2), when an image of the sample after the coke reaction is collected by an optical microscope, the magnification of the optical microscope objective lens is 2.5 to 5.0 times.
The smaller the reaction depth of the coke, the less the damage to the coke, and if the coke r=12mm coke reacts at 1100 ℃, the higher the quality coke is if the reaction depth is less than 50% when the weight loss is 25%.
The method for detecting the coke reaction depth is based on the research of the coke reactivity and the coke pore structure. Since the coke reaction process is invisible, the intensity after the coke reaction is detected to infer the coke reaction process, and the research shows that apparent pores of the coke after the reaction are increased, namely, pores communicated with the surface are increased. The adhesive can be filled into the air inlet holes under a certain vacuum degree and identified by a microscope, so that the communicated air holes are distinguished. It is difficult to distinguish between the communicating pores and the closed pores without filling under a microscope, and it is difficult to fill the deep part of the pores without filling under a vacuum state, because of the crisscrossed three-dimensional structure of the coke pores, researches show that the communicating pores can be fully filled with the adhesive by filling under a vacuum state, and the communicating pores are distinguished from the closed pores under a microscope, the coke communicating pores are filled with the resin, and the coke closed pores are free of the resin.
In the prior art, a coke reaction depth characterization method is not available, which is mainly characterized in that the characterization macroscopic aspect after the coke reactivity is researched from the aspects of strength and coke pulverization, the microscopic aspect is researched on the aspects of coke porosity, coke pore fractal dimension and the like, only pore shape and pore structure are researched for an image method, the characteristic of the image method after the coke reaction is not combined with the pore of an adhesive filling and the coke reaction, and the microscopic image expression aspect of the characteristic after the coke reaction is not researched.
Compared with the prior art, the invention has the following positive effects: 1. a method for detecting the reaction depth of coke is developed. A method for detecting the reaction depth of coke is provided for researching the reaction process and the reaction depth of the coke by combining resin filling and characteristic research after the reaction of the coke under a certain vacuum state. 2. The method for detecting the coke reaction depth is an effective supplement to the characteristic evaluation after the coke reaction, overcomes the defect that the coke reaction process cannot be intuitively analyzed, and can intuitively study the quality characteristics after the coke reaction under different reaction conditions of different cokes.
Detailed Description
The invention will be further illustrated with reference to specific examples.
Example 1, a method for detecting depth of reaction of coke, comprising the steps of:
1) Preparing a coke reaction sample, grinding the coke sample to be detected into a coke ball sample with the radius R of 12mm, placing a Jiao Qiu sample in a coke reactor, and controlling Jiao Qiu sample to react at 1100 ℃ until the weight loss is 25% of the original mass; taking out the reacted coke ball sample from the coke reactor, transferring the reacted coke ball sample into a grinding tool in a vacuum chamber, controlling the vacuum degree of the vacuum chamber to be 55kpa, pouring epoxy resin with the model number of EpoThin & lt 2 & gt into the grinding tool in which the reacted coke ball sample is placed, and standing for 9 hours until the epoxy resin on the surface of the reacted coke ball sample is hardened; taking out the reacted coke ball sample from the vacuum bin, cutting the reacted coke ball sample along the diameter direction, and throwing the reacted coke ball sample Jiao Qiumo until the reacted coke ball sample meets the detection requirement of an optical microscope to obtain a coke reacted sample:
2) Collecting an image of a sample after coke reaction, collecting an image of the sample after coke reaction by using an optical microscope, scanning the whole sample after coke reaction according to 7 rows and 7 columns in the transverse direction under an objective lens of 2.5 times to obtain 49 images, and obtaining an image overall view of the sample after coke reaction by image stitching, wherein the deepest position which can be reached by epoxy resin displayed on the image of the sample after coke reaction is the deepest position which can be reached by a coke communication air hole after reaction, and the radius from the deepest position which can be reached by the coke communication air hole after reaction to the center of the sample after coke reaction is r;
3) Calculating the reaction depth of the coke, wherein the reaction depth of the coke is calculated according to a formula I, and p= (R-R)/R multiplied by 100 percent of formula I, wherein in the formula I, p is the reaction depth of the coke, and the unit is; r is the radius of the focal sphere sample before reaction, and the unit is mm; and r is the radial distance from the deepest position of the reacted coke communicating air hole to the center of the sample after the coke is reacted, and the unit is mm.
Example 2, a method for detecting depth of reaction of coke, comprising the steps of:
1) Preparing a coke reaction sample, grinding the coke sample to be detected into a coke ball sample with the radius R of 12mm, placing a Jiao Qiu sample in a coke reactor, and controlling Jiao Qiu sample to react at 1200 ℃ until the weight loss is 25% of the original mass; taking out the reacted coke ball sample from the coke reactor, transferring the reacted coke ball sample into a grinding tool in a vacuum chamber, controlling the vacuum degree of the vacuum chamber to be 55kpa, pouring epoxy resin with the model number of EpoThin & lt 2 & gt into the grinding tool in which the reacted coke ball sample is placed, and standing for 9 hours until the epoxy resin on the surface of the reacted coke ball sample is hardened; taking out the reacted coke ball sample from the vacuum bin, cutting the reacted coke ball sample along the diameter direction, and throwing the reacted coke ball sample Jiao Qiumo until the reacted coke ball sample meets the detection requirement of an optical microscope to obtain a coke reacted sample:
2) Collecting an image of a sample after coke reaction, collecting an image of the sample after coke reaction by using an optical microscope, scanning the whole sample after coke reaction according to 13 rows and 13 columns in the transverse direction under an objective lens of 5.0 times to obtain 169 images, and obtaining an image overall view of the sample after coke reaction by image stitching, wherein the deepest position which can be reached by epoxy resin displayed on the image of the sample after coke reaction is the deepest position which can be reached by a coke communication air hole after reaction, and the radius from the deepest position which can be reached by the coke communication air hole after reaction to the center of the sample after coke reaction is r;
3) Calculating the reaction depth of the coke, wherein the reaction depth of the coke is calculated according to a formula I, and p= (R-R)/R multiplied by 100 percent of formula I, wherein in the formula I, p is the reaction depth of the coke, and the unit is; r is the radius of the focal sphere sample before reaction, and the unit is mm; and r is the radial distance from the deepest position of the reacted coke communicating air hole to the center of the sample after the coke is reacted, and the unit is mm.
The accuracy and precision of the method are confirmed by comparing the adjustment test parameters and performing precision experiments.
The accuracy test of the depth of reaction of the coke was compared, and the test results are shown in table 1 below.
TABLE 1 depth of reaction detection of coke
| Category(s) | Reaction temperature, DEG C | Loss of weight, percent | Objective lens multiple | Depth of reaction,% |
| Sample 1 | 1100 | 25 | 2.5 | 62.4 |
| Sample 1 | 1100 | 25 | 5.0 | 64.3 |
| Sample 2 | 1200 | 25 | 2.5 | 48.2 |
| Sample 2 | 1200 | 25 | 5.0 | 46.8 |
Precision experiments, the reflectivities of the two groups of samples were subjected to 11 precision experiments, and the analysis results are shown in table 2.
TABLE 2 sample precision experiments in%
The experimental results show that the reaction depth of the coke is similar, the relative standard deviation RSD is less than 5%, the precision of the detection data is good, and the method is proved to be accurate and reliable and completely meets the coke reaction depth determination requirement.
In addition to the embodiments described above, other embodiments of the invention are possible. All technical schemes formed by equivalent substitution or equivalent transformation fall within the protection scope of the invention.
Claims (3)
1. A method for detecting the reaction depth of coke, which is characterized by comprising the following steps:
1) Preparing a coke reaction sample, grinding the coke sample to be detected into a coke ball sample with the radius R of 12-15 mm, placing a Jiao Qiu sample in a coke reactor, and controlling a Jiao Qiu sample to react at 1050-1250 ℃ until the weight loss reaches 20-30% of the original mass; taking out the reacted coke ball sample from the coke reactor, transferring the reacted coke ball sample into a grinding tool in a vacuum chamber, controlling the vacuum degree of the vacuum chamber to be 50-60 kpa, pouring epoxy resin into the grinding tool in which the reacted coke ball sample is placed, and standing for 8-10 h until the epoxy resin on the surface of the reacted coke ball sample is hardened; taking out the reacted coke ball sample from the vacuum bin, cutting the reacted coke ball sample along the diameter direction, and throwing the reacted coke ball sample Jiao Qiumo until the reacted coke ball sample meets the detection requirement of an optical microscope to obtain a coke reacted sample:
2) Collecting an image of a sample after coke reaction, collecting an image of the sample after coke reaction by using an optical microscope, and obtaining an image overall view of the sample after coke reaction by image stitching, wherein the deepest part of the sample after coke reaction, which is the deepest position which can be reached by a coke communication air hole after reaction, is obtained by immersing epoxy resin displayed on the image of the sample after coke reaction into the deepest position of the sample after coke reaction, and the radial distance from the deepest position which can be reached by the coke communication air hole after reaction to the center of the sample after coke reaction is r;
3) Calculating the reaction depth of the coke, wherein the reaction depth of the coke is calculated according to a formula I, and p= (R-R)/R multiplied by 100 percent of formula I, wherein in the formula I, p is the reaction depth of the coke, and the unit is; r is the radius of the focal sphere sample before reaction, and the unit is mm; and r is the radial distance from the deepest position of the reacted coke communicating air hole to the center of the sample after the coke is reacted, and the unit is mm.
2. The method for detecting the reaction depth of coke according to claim 1, wherein the vacuum chamber upper cover in the step 1) is made of a transparent material.
3. The method for detecting the depth of reaction of coke according to claim 1, wherein the magnification of the optical microscope objective lens is 2.5 to 5.0 times when the image of the sample after the coke reaction is collected by the optical microscope in the step 2).
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