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CN101561403A - Three-dimensional orthogonality microscope image pick-up observation device and quantitative image method thereof - Google Patents

Three-dimensional orthogonality microscope image pick-up observation device and quantitative image method thereof Download PDF

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CN101561403A
CN101561403A CNA200910143878XA CN200910143878A CN101561403A CN 101561403 A CN101561403 A CN 101561403A CN A200910143878X A CNA200910143878X A CN A200910143878XA CN 200910143878 A CN200910143878 A CN 200910143878A CN 101561403 A CN101561403 A CN 101561403A
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高鸿
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Yanshan University
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Abstract

本发明公开一种三维正交显微镜摄像观测装置和图像定量方法。所述装置将三套配有CCD摄像机(4、5、6)的显微镜(1、2、3)三维正交配置,拍摄观测体三维图象。所述方法:a.用密度剃度离心分离法制备粒度、密度和成分均匀的试样(17);b.在选择的温度和压力下进行有溶液或无溶液观测;c.有溶液时,将试样(17)放入石英玻璃反应器(16)的溶液中后开始自动定时摄像;测量试样(17)三维方向的投影面积和周长,计算形状系数;d.无溶液时,测量试样(17)三维方向图象的投影面积和周长,计算形状系数;e.试样(17)体积及其变化率取三维数据的算术平均值。本发明提供了一种拍摄试样三维图像的装置和图像定量方法,特别是为溶液中高分子粒子和生物种子的三维行为的观测和定量评价提供了一种新的装置和方法。

Figure 200910143878

The invention discloses a three-dimensional orthogonal microscope imaging observation device and an image quantification method. The device arranges three sets of microscopes (1, 2, 3) equipped with CCD cameras (4, 5, 6) orthogonally in three dimensions to shoot three-dimensional images of the observation body. The method: a. prepare a sample (17) with uniform particle size, density and composition by density-gradient centrifugation; b. carry out observation with or without solution at a selected temperature and pressure; c. when there is a solution, put After the sample (17) is put into the solution of the quartz glass reactor (16), start automatic timing camera; measure the projected area and the circumference of the sample (17) three-dimensional direction, and calculate the shape factor; d. when there is no solution, measure the The projected area and the perimeter of the three-dimensional direction image of the sample (17) are used to calculate the shape factor; e. the volume of the sample (17) and its rate of change are the arithmetic mean of the three-dimensional data. The invention provides a device for taking three-dimensional images of a sample and an image quantitative method, especially provides a new device and method for the observation and quantitative evaluation of the three-dimensional behavior of polymer particles and biological seeds in a solution.

Figure 200910143878

Description

三维正交显微镜摄像观测装置及其图像定量方法 Three-dimensional orthogonal microscope camera observation device and its image quantification method

技术领域 technical field

本发明涉及一种三维正交显微镜摄像观测和图像定量的方法,尤其是用于对具有异方性高分子粒子在溶液中的膨胀和生物质种子在溶液中的膨胀发芽生长规律进行连续观测的三维正交显微镜摄像装置和图像定量方法。The invention relates to a three-dimensional orthogonal microscope camera observation and image quantification method, especially for continuous observation of the expansion of anisotropic polymer particles in solution and the expansion, germination and growth of biomass seeds in solution Three-dimensional orthogonal microscope camera device and image quantification method.

背景技术 Background technique

目前,公知的显微镜摄像系统都不能获得连续变化且不可移动的具有异方特性试样的三维图像。例如,用来测量溶液中高分子颗粒的溶胀特性的方法有四种:(1)基于填充床的体积测量法;(2)基于气相吸收的重量分析法;(3)基于测量颗粒尺寸分布得的马尔文激光散射法;(4)基于显微镜观测和图像解析相结合的方法。除了方法(4)之外的三种方法不能用于单一高分子颗粒的动态观测和定量。而通常只用一台显微镜的方法(4)不能获得单一高分子颗粒的三维连续图像。为了克服方法(4)的缺欠,中国和日本的研究者曾提出正交两台显微镜获取溶液中高分子颗粒膨胀特性图像的方法;美国研究者的方法也不能完全获得颗粒的三维图像。也有采用旋转试样,或倾斜试样,或旋转显微镜来获得三维图像的方法,但这些方法无法同时获得试样的同一时刻的三维图像。另外,有利用复杂和昂贵的共聚焦显微镜法三维观测的方法和基于数字全息摄像原理的显微镜法三维观测方法。因此,开发对具有异方性高分子颗粒进行三维显微镜摄像和图像定量解析的新方法意义重大。本发明就是一种用于对具有异方性的试样进行连续观测的三维正交显微镜摄像系统和相应的图像定量解析方法。At present, none of the known microscope camera systems can obtain a three-dimensional image of a continuously changing and immovable sample with anisotropic characteristics. For example, there are four methods used to measure the swelling characteristics of polymer particles in solution: (1) volumetric measurement based on packed bed; (2) gravimetric analysis based on gas phase absorption; (3) based on measurement of particle size distribution. Malvern laser scattering method; (4) A method based on the combination of microscope observation and image analysis. The three methods except method (4) cannot be used for dynamic observation and quantification of single polymer particles. However, the method (4) usually using only one microscope cannot obtain three-dimensional continuous images of a single polymer particle. In order to overcome the shortcomings of method (4), researchers in China and Japan have proposed a method to obtain images of the expansion characteristics of polymer particles in solution with two orthogonal microscopes; the method of American researchers cannot completely obtain three-dimensional images of particles. There are also methods of obtaining three-dimensional images by rotating the sample, tilting the sample, or rotating the microscope, but these methods cannot simultaneously obtain the three-dimensional image of the sample at the same moment. In addition, there are methods of three-dimensional observation using complicated and expensive confocal microscopy and three-dimensional observation methods of microscopy based on the principle of digital holography. Therefore, it is of great significance to develop new methods for three-dimensional microscopy imaging and image quantitative analysis of anisotropic polymer particles. The invention is a three-dimensional orthogonal microscope camera system and a corresponding image quantitative analysis method for continuous observation of samples with anisotropy.

发明内容 Contents of the invention

为了克服现有显微镜摄像系统不能获得连续变化且不可移动的具有异方特性观测体三维图象的问题,本发明提供一种三维正交显微镜摄像观测装置及其图像定量方法,该发明可连续获得随时间变化观测试样,特别是获得具有异方性变化观测试样的三维显微图像。In order to overcome the problem that the existing microscope camera system cannot obtain continuously changing and immovable three-dimensional images of an anisotropic observation body, the present invention provides a three-dimensional orthogonal microscope camera observation device and its image quantification method, which can continuously obtain Observing the sample over time, in particular, obtaining a three-dimensional microscopic image of the observed sample with anisotropy.

本发明解决其技术问题所采用的技术方案是:The technical solution adopted by the present invention to solve its technical problems is:

所述三维正交显微镜摄像观测装置用三台万能台架(11、12、13)三维正交固定三台显微镜(1、2、3),三台显微镜(1、2、3)与三台CCD摄像机(4、5、6)相连,三台CCD摄像机(4、5、6)的数据线(7、8、9)与计算机10相连接。三维位置可调的有透明窗的反应器台架14上放置石英玻璃反应器16,石英玻璃反应器16内放置试样17和溶液。设置在试样17上方和下方的多点光纤冷光源15调节照明方向并配合放置在石英玻璃透明反应器16后方的背景色板以获得清晰图像。The three-dimensional orthogonal microscope imaging observation device uses three universal stands (11, 12, 13) to fix three microscopes (1, 2, 3) three-dimensionally and orthogonally, three microscopes (1, 2, 3) and three microscopes (1, 2, 3) The CCD cameras (4, 5, 6) are connected, and the data lines (7, 8, 9) of the three CCD cameras (4, 5, 6) are connected with the computer 10. A three-dimensional position-adjustable reactor stand 14 with a transparent window is placed on a quartz glass reactor 16, and a sample 17 and a solution are placed in the quartz glass reactor 16. The multi-point optical fiber cold light source 15 arranged above and below the sample 17 adjusts the illumination direction and cooperates with the background color plate placed behind the quartz glass transparent reactor 16 to obtain a clear image.

根据试样颗粒尺寸大小选择显微镜聚焦距离di(i=1,2,3)的可调范围和显微镜目镜放大倍率fi(i=1,2,3)的可调范围;三台显微镜(1、2、3)的聚焦距离di(i=1,2,3)在40~110mm可调,三台显微镜(1、2、3)的目镜放大倍率fi(i=1,2,3)在0.68~4.5可调。Select the adjustable range of microscope focus distance d i (i=1, 2, 3) and the adjustable range of microscope eyepiece magnification f i (i=1, 2, 3) according to the sample particle size; three microscopes ( The focusing distance d i (i=1, 2, 3) of 1, 2, 3) is adjustable from 40 to 110mm, and the eyepiece magnification f i (i=1, 2, 3) Adjustable from 0.68 to 4.5.

显微镜1和显微镜2的镜头中心距支撑桌面的高度h1=h2=450mm,显微镜3的镜头中心距支撑桌面的高度h3=400mm。The height h 1 =h 2 =450mm between the lens center of the microscope 1 and the microscope 2 and the support table, and the height h 3 =400mm between the lens center of the microscope 3 and the support table.

计算机10的图象屏幕放大倍数为1100~8400。进行图象采集、存储,处理和分析的计算机10可使用商业或非商业或用户自编的图象采集、存储、处理的分析软件。The image screen magnification of the computer 10 is 1100-8400. The computer 10 for image acquisition, storage, processing and analysis can use commercial or non-commercial or user-edited image acquisition, storage, and analysis software for processing.

所述三维正交显微镜摄像观测装置的观测定量方法,其具体步骤如下:The observation quantitative method of described three-dimensional orthogonal microscope imaging observation device, its specific steps are as follows:

a.利用密度剃度离心分离方法获得粒度、密度和成分相对均匀、储存状态一致的2~6组观测用试样。a. Obtain 2 to 6 groups of observation samples with relatively uniform particle size, density and composition, and consistent storage state by using the density-gradient centrifugal separation method.

为获得粒度均匀和成分均匀的煤样,观测用代表性煤种破碎后进行密度剃度离心分离并按实验要求的粒度范围,如0.1~0.2mm、0.2~0.3mm等进行筛分,所得试样在105℃真空干燥24h后储存备用。In order to obtain coal samples with uniform particle size and uniform composition, the representative coal types used for observation are crushed and then subjected to density shaving centrifugation and sieved according to the particle size range required by the experiment, such as 0.1-0.2mm, 0.2-0.3mm, etc., and the obtained samples are After vacuum drying at 105°C for 24 h, it was stored for future use.

为获得粒度均匀和成分均匀的种子,无表皮破损的成熟的黄豆、绿豆、红豆、红小豆、黑豆等植物种子自然风干后,利用密度剃度离心法分离并按实验要求的粒度范围,如4×5×6mm、5×6×7mm等筛分,分离出的试样储存(温度23℃,湿度30-50%)备用。In order to obtain seeds with uniform particle size and composition, the mature soybean, mung bean, red bean, red bean, black bean and other plant seeds without skin damage are naturally air-dried, separated by density shaving centrifugation, and separated according to the particle size range required by the experiment, such as 4× Sieve at 5×6mm, 5×6×7mm, etc., and store the separated samples (temperature 23°C, humidity 30-50%) for future use.

b.观测可采用无溶液和有溶液两种方式,有溶液观测使用有机溶液或水。观测可在室温和环境压力下进行,也可在控制温度和控制压力条件下进行。b. Observation can be done in two ways: without solution and with solution. With solution, organic solution or water is used for observation. Observations can be performed at room temperature and ambient pressure, or under controlled temperature and controlled pressure conditions.

c.有溶液观测时,在观测温度和压力下,首先将3~5ml溶液注射进透明石英玻璃反应器16,然后将试样17放入石英玻璃反应器16的溶液中后开始按设定时间,三维正交显微镜摄像观测装置(三通道)自动定时摄像取样17。c. When there is solution observation, under the observation temperature and pressure, first inject 3-5ml solution into the transparent quartz glass reactor 16, then put the sample 17 into the solution in the quartz glass reactor 16 and start to press the set time , three-dimensional orthogonal microscope camera observation device (three channels) automatic timing camera sampling 17.

d.对无溶液试样17三维方向图象的投影面积、投影面积周长进行测量;然后计算同一试样三个方向的形状系数和体积;最后通过平均处理三维图像数据获得试样17的形状系数和体积。d. Measure the projected area and the perimeter of the projected area of the three-dimensional image of the solution-free sample 17; then calculate the shape factor and volume of the same sample in three directions; finally obtain the shape of the sample 17 by averaging the three-dimensional image data factor and volume.

试样的体积V按式(1)计算:The volume V of the sample is calculated according to formula (1):

VV == 44 33 ππ (( Ff 11 PP 11 ++ Ff 22 PP 22 ++ Ff 33 PP 33 )) 33 22 33 -- -- -- (( 11 ))

式(1)中,P1、P2、P3分别为三维直交显微镜观测得到的同一试样17三个方向的投影面积。F1、F2、F3分别为三维直交显微镜观测得到的同一试样17三个方向的形状系数,由式(2)计算:In formula (1), P 1 , P 2 , and P 3 are respectively the projected areas of the same sample 17 in three directions observed by a three-dimensional orthogonal microscope. F 1 , F 2 , and F 3 are the shape coefficients of the same sample 17 in three directions observed by a three-dimensional orthogonal microscope, calculated by formula (2):

Figure A20091014387800072
Figure A20091014387800072

e.对溶液中试样17三维方向图象的投影面积、投影面积周长进行测量;然后计算同一试样17三个方向的形状系数和体积变化率;最后通过平均处理三维图像数据获得试样17形状系数和体积变化率。e. Measure the projected area and the perimeter of the projected area of the sample 17 three-dimensional direction image in the solution; then calculate the shape coefficient and volume change rate of the same sample 17 in three directions; finally obtain the sample by averaging the three-dimensional image data 17 Shape factor and volume change rate.

试样17在t时刻的体积变化率(Qv,t)定义为t时刻的试样17体积(Vt)与零时刻的试样17体积(V0)之比,式(3);The volume change rate (Q v, t ) of sample 17 at time t is defined as the ratio of the volume of sample 17 (V t ) at time t to the volume of sample 17 (V 0 ) at time zero, formula (3);

QQ vv ,, tt == VV tt VV 00 -- -- -- (( 33 ))

考虑到试样17本身形状的不规则性和试样17体积变化的异方性特点,本发明将三个显微镜各自测得的t时刻试样17体积变化率的算术平均作为试样17在t时刻的体积变化率,式(4);Considering the irregularity of the shape of the sample 17 itself and the anisotropic characteristics of the volume change of the sample 17, the present invention uses the arithmetic mean of the volume change rate of the sample 17 measured by the three microscopes at time t as the sample 17 in Volume change rate at time t, formula (4);

QQ vv ,, tt == 11 33 {{ [[ Ff 11 ,, tt PP 11 ,, tt 33 // 22 Ff 1,01,0 PP 1,01,0 33 // 22 ]] ++ [[ Ff 22 ,, tt PP 22 ,, tt 33 // 22 Ff 2,02,0 PP 2,02,0 33 // 22 ]] ++ [[ Ff 33 ,, tt PP 33 ,, tt 33 // 22 Ff 3,03,0 PP 3,03,0 33 // 22 ]] }} -- -- -- (( 44 ))

式(4)中,Fi,t(i=1,2,3)是t时刻试样17在x,y,z三个方向的形状系数;Fi,0(i=1,2,3)是零时刻试样17在x,y,z三个方向的形状系数;Pi,t(i=1,2,3)是t时刻试样17在x,y,z三个方向的投影面积;Pi,0(i=1,2,3)是零时刻试样17在x,y,z三个方向的投影面积。式(4)可简写为式(5):In formula (4), F i, t (i=1, 2, 3) is the shape coefficient of sample 17 in x, y, z three directions at time t; F i, 0 (i=1, 2, 3 ) is the shape coefficient of the sample 17 in the three directions of x, y, and z at zero time; P i, t (i=1, 2, 3) is the projection of the sample 17 in the three directions of x, y, and z at the time t Area; P i,0 (i=1, 2, 3) is the projected area of the sample 17 in the three directions of x, y, and z at zero time. Formula (4) can be abbreviated as Formula (5):

QQ vv ,, tt == 11 33 (( QQ 11 vv ,, tt ++ QQ 22 vv ,, tt ++ QQ 33 vv ,, tt )) -- -- -- (( 55 ))

式(5)中,Qiv,t(i=1,2,3)是t时刻试样17在x,y,z三个方向的体积变化率。In formula (5), Q iv,t (i=1, 2, 3) is the volume change rate of the sample 17 in the three directions of x, y, and z at time t.

由于试样17中含有的体积不变物质,如矿物杂质等的体积应当从试样17体积中扣除;采用式(6)修正式(4)和式(5):Due to the volume-invariant substances contained in sample 17, such as the volume of mineral impurities, etc. should be deducted from the volume of sample 17; use formula (6) to modify formula (4) and formula (5):

QQ dmmfdmmf == (( QQ measuredmeasured -- ythe y )) (( 11 -- ythe y )) -- -- -- (( 66 ))

式(6)中,Qdmmf为干燥基无体积不变物质试样17的体积变化率,Qmeasured为观测的体积变化率。In formula (6), Q dmmf is the volume change rate of sample 17 without volume-invariant substance on a dry basis, and Q measured is the observed volume change rate.

Figure A20091014387800083
Figure A20091014387800083

修正后的式(4)和式(5)成为式(8)和式(9)。The revised formula (4) and formula (5) become formula (8) and formula (9).

QQ vv ,, tt == {{ 11 33 [[ (( Ff 11 ,, tt PP 11 ,, tt 33 // 22 Ff 1,01,0 PP 1,01,0 33 // 22 )) ++ (( Ff 22 ,, tt PP 22 ,, tt 33 // 22 Ff 2,02,0 PP 2,02,0 33 // 22 )) ++ (( Ff 33 ,, tt PP 33 ,, tt 33 // 22 Ff 3,03,0 PP 3,03,0 33 // 22 )) ]] -- ythe y }} (( 11 -- ythe y )) -- -- -- (( 88 ))

QQ vv ,, tt == {{ 11 33 (( QQ 11 vv ,, tt ++ QQ 22 vv ,, tt ++ QQ 33 vv ,, tt )) -- ythe y }} (( 11 -- ythe y )) -- -- -- (( 99 ))

式(8)和式(17)是本发明中试样体积变化率的通用计算式;当y=0时,即试样不含体积不变物质时,式(8)和式(9)成为式(4)和式(5)。Formula (8) and formula (17) are the general calculation formulas of sample volume change rate among the present invention; When y=0, promptly sample does not contain volume invariant substance, formula (8) and formula (9) become Formula (4) and Formula (5).

本发明的有益效果是:该发明可连续获得随时间变化观测试样,特别是具有异方性变化观测试样的三维显微图像;提供了一种能获得更加全面和准确的连续变化观测试样三维图像定量信息的方法;为具有异方性试样在溶液中或无溶液条件下的三维行为的观察和定量评价提供了一种新方法;特别是为三维显微观测和定量分析溶液中高分子粒子和植物种子等的行为和溶胀机理提供了一种新装置和新方法。该发明应用领域广泛,如矿物质粒子、金属和非金属材料粒子、生物质粒子、生物种子、生物细胞等。根据观测对象的不同,使用本发明提出的方法可以充分利用现有各类显微镜、摄像机和图像处理软件,观测广泛尺寸范围观测体的三维行为,获得观测体的三维动态图象信息。利用本发明生产的三维观测装置的成本低、有价格优势。另外,该发明装置具有结构简单,组合灵活、观测操作简单、观测质量好等优点。The beneficial effects of the present invention are: the invention can continuously obtain the three-dimensional microscopic image of the observation sample that changes with time, especially the three-dimensional microscopic image of the observation sample with anisotropic change; It provides a new method for the observation and quantitative evaluation of the three-dimensional behavior of samples with anisotropy in solution or without solution; especially for three-dimensional microscopic observation and quantitative analysis of high The behavior and swelling mechanism of molecular particles and plant seeds etc. provide a new device and new method. The invention has a wide range of applications, such as mineral particles, metal and non-metal material particles, biomass particles, biological seeds, biological cells and the like. According to different observation objects, using the method proposed by the present invention can make full use of various existing microscopes, cameras and image processing software to observe the three-dimensional behavior of the observation object in a wide range of sizes and obtain the three-dimensional dynamic image information of the observation object. The three-dimensional observation device produced by the invention has low cost and price advantage. In addition, the inventive device has the advantages of simple structure, flexible combination, simple observation operation, good observation quality and the like.

附图说明 Description of drawings

图1是三维正交显微镜摄像观测装置示意图;Fig. 1 is a schematic diagram of a three-dimensional orthogonal microscope imaging observation device;

图2是三个显微镜位置配置关系示意图;Figure 2 is a schematic diagram of the positional configuration relationship of three microscopes;

图3是0.6~0.9mm大同烟煤煤粒无溶液的三维图像;Figure 3 is a three-dimensional image of 0.6-0.9mm Datong bituminous coal particles without solution;

图4是0.6~0.9mm大同烟煤煤粒在水中的三维图像;Figure 4 is a three-dimensional image of 0.6-0.9mm Datong bituminous coal particles in water;

图5是0.6~0.9mm大同烟煤煤粒在砒啶溶液中的三维图像;Figure 5 is a three-dimensional image of 0.6-0.9mm Datong bituminous coal particles in pyridine solution;

图6是0.6~0.9mm大同烟煤煤粒在砒啶中的形状系数和体积溶胀率随时间的变化规律;Figure 6 shows the shape coefficient and volume swelling rate of 0.6-0.9mm Datong bituminous coal particles in pyridine as a function of time;

图7是水中黄豆吸水膨胀随时间变化的三维图像;Figure 7 is a three-dimensional image of the water swelling of soybeans in water as a function of time;

图8是水中黄豆形状系数和体积膨胀率随时间的变化规律。Fig. 8 is the changing rule of shape factor and volume expansion rate of soybean in water with time.

具体实施方式 Detailed ways

实施例1:溶液中煤粒溶解膨胀规律的观察和定量评价Example 1: Observation and quantitative evaluation of the dissolution and expansion of coal particles in the solution

其具体步骤如下:The specific steps are as follows:

a.实施例1中,观测用试样使用了温度为105℃真空干燥24小时,粒度范围为0.2~0.3mm、0.3~0.6mm、0.6~0.9mm、0.9~1.0mm的中国大同烟煤。a. In Example 1, China Datong bituminous coal with a particle size range of 0.2-0.3 mm, 0.3-0.6 mm, 0.6-0.9 mm, and 0.9-1.0 mm was used as the observation sample, which was vacuum-dried at 105° C. for 24 hours.

b.观测采用无溶液和有溶液两种方式,在室温(28℃)和环境压力下进行。b. Observations were carried out at room temperature (28° C.) and ambient pressure in two ways, without solution and with solution.

c.无溶液观测是在不使用溶液的情况下,实证系统的有效性。图3是无溶液大同烟煤颗粒的三维图像。图4是水中大同烟煤颗粒的三维图像。由图3和图4可见,煤粒具有显著的异方性,单纯地从一个方向评价煤粒体积不会得到准确的结果。c. No-solution observation is to demonstrate the effectiveness of the system without using a solution. Figure 3 is a three-dimensional image of a solution-free Datong bituminous coal particle. Figure 4 is a three-dimensional image of Datong bituminous coal particles in water. It can be seen from Figure 3 and Figure 4 that coal particles have significant anisotropy, and it is not possible to obtain accurate results simply by evaluating the volume of coal particles from one direction.

d.有溶液观测使用的有机溶液是试剂等级的吡碇(pyridine)。实验是在室温和环境压力下进行的,将3ml吡碇溶液注射进透明石英反应器16,然后将1~3粒试样放入反应器16的吡碇溶液中后开始自动定时摄像取样(三通道)。初期6小时取样时间间隔为10分钟,之后6小时取样时间间隔为30分钟,最后12小时取样时间间隔为60分钟,全部连续摄像取样时间为24小时。d. The organic solution used for the observation of the solution is pyridine of reagent grade. The experiment was carried out at room temperature and ambient pressure. 3ml of the pyridine solution was injected into the transparent quartz reactor 16, and then 1 to 3 samples were put into the pyridine solution of the reactor 16, and automatic timing camera sampling was started (three aisle). The sampling time interval for the first 6 hours is 10 minutes, the sampling time interval for the next 6 hours is 30 minutes, the sampling time interval for the last 12 hours is 60 minutes, and the sampling time for all continuous cameras is 24 hours.

吡碇溶液中大同无烟煤颗粒(0.6~0.9mm)在t=0min和t=180min时三个正交显微镜所摄同一粒子的三维图像见图5。由图5可见,吡碇溶液中煤粒溶胀具有显著的异方性,因此,只从一个方向观测和评价煤粒体积和溶胀率也不会得到准确和全面地信息。Figure 5 shows the three-dimensional images of Datong anthracite particles (0.6-0.9mm) in pyridine solution taken by three orthogonal microscopes at t=0min and t=180min. It can be seen from Figure 5 that the swelling of coal particles in the pyridin solution has significant anisotropy. Therefore, accurate and comprehensive information cannot be obtained by observing and evaluating the volume and swelling rate of coal particles only from one direction.

正是为了解决这个问题,提高测量精度,本发明采用三维正交配置的显微镜摄像观测和解析方法对无溶液和溶液中高分子煤粒的投影面积、相对投影面积、煤粒形状系数、体积和体积变化率进行定量解析,通过平均处理三维图像数据获得煤粒形状系数、煤粒体积和溶胀率变化规律。Just in order to solve this problem and improve the measurement accuracy, the present invention uses a three-dimensional orthogonally configured microscope camera observation and analysis method to analyze the projected area, relative projected area, coal particle shape factor, volume and volume of polymer coal particles in solution and solution. Quantitative analysis of the change rate is carried out, and the change law of the coal particle shape coefficient, coal particle volume and swelling rate is obtained by averaging the three-dimensional image data.

颗粒形状系数、颗粒体积溶胀率由式(2)计算,即Particle shape coefficient and particle volume swelling rate are calculated by formula (2), namely

颗粒体积溶胀率Qv,t由式(8)计算,即Particle volume swelling rate Qv ,t is calculated by formula (8), that is

QQ vv ,, tt == {{ 11 33 [[ (( Ff 11 ,, tt PP 11 ,, tt 33 // 22 Ff 1,01,0 PP 1,01,0 33 // 22 )) ++ (( Ff 22 ,, tt PP 22 ,, tt 33 // 22 Ff 2,02,0 PP 2,02,0 33 // 22 )) ++ (( Ff 33 ,, tt PP 33 ,, tt 33 // 22 Ff 3,03,0 PP 3,03,0 33 // 22 )) ]] -- ythe y }} (( 11 -- ythe y ))

对于大同烟煤,y=0.0152。For Datong bituminous coal, y=0.0152.

颗粒尺寸为0.6~0.9mm大同烟煤,在温度28℃砒啶溶液中,测量得到的三维方向的投影面积和投影面积周长随时间的变化数据见表1;测量得到的三维方向的形状系数和溶胀体积及其平均值的变化见表2;测量得到的砒啶溶液中大同烟煤颗粒的形状系数和体积溶胀率随时间的变化规律见图6。Datong bituminous coal with a particle size of 0.6-0.9mm, in a pyridine solution at a temperature of 28°C, the measured three-dimensional projected area and projected area perimeter change data with time are shown in Table 1; the measured three-dimensional shape coefficient and swelling volume Table 2 and the change of the average value are shown in Table 2; the measured shape coefficient and volume swelling rate of Datong bituminous coal particles in the pyridine solution are shown in Figure 6.

实施例2:生物质种子水中膨胀生长规律的观察和定量评价Embodiment 2: Observation and quantitative evaluation of the expansion and growth law of biomass seeds in water

其具体步骤如下:The specific steps are as follows:

a.实施例1中给出的式(1)~(5)完全适用于生物质种子在水中溶胀、发芽生长规律的动态观察和定量评价。a. The formulas (1)-(5) given in Example 1 are fully applicable to the dynamic observation and quantitative evaluation of the swelling and germination growth of biomass seeds in water.

b.实施例2中观测用试样使用了粒度为5.5×5.5×6.5mm的黄豆。b. The sample for observation in Example 2 used soybeans with a particle size of 5.5×5.5×6.5 mm.

c.观测使用的溶液是水,在室温(27℃)和环境压力下进行。将5ml纯净水注射进透明石英反应器16,然后将黄豆试样放入反应器16的水中后开始自动定时摄像(三通道)。自动摄像时间间隔为设定为1分钟,连续自动摄像时间为24小时。c. The solution used for the observations was water, carried out at room temperature (27° C.) and ambient pressure. 5ml of pure water is injected into the transparent quartz reactor 16, and then the soybean sample is put into the water in the reactor 16, and then the automatic timing camera (three channels) is started. The automatic camera time interval is set to 1 minute, and the continuous automatic camera time is 24 hours.

图7是水中黄豆吸水膨胀生长过程的三维图像。显著的异方性使只从一个方向观察和定量评价黄豆的溶胀生长过程不会得到准确和全面的信息,因此,三维观测和评价成为必然的选择。Fig. 7 is a three-dimensional image of the growth process of soybean absorbing water and swelling in water. Significant anisotropy makes it impossible to obtain accurate and comprehensive information from observing and quantitatively evaluating the swelling growth process of soybeans from only one direction. Therefore, three-dimensional observation and evaluation becomes an inevitable choice.

颗粒形状系数由式(2)计算,即Particle shape coefficient is calculated by formula (2), namely

Figure A20091014387800111
Figure A20091014387800111

颗粒体积溶胀率由式(4)计算,即The particle volume swelling rate is calculated by formula (4), namely

QQ vv ,, tt == 11 33 {{ [[ Ff 11 ,, tt PP 11 ,, tt 33 // 22 Ff 1,01,0 PP 1,01,0 33 // 22 ]] ++ [[ Ff 22 ,, tt PP 22 ,, tt 33 // 22 Ff 2,02,0 PP 2,02,0 33 // 22 ]] ++ [[ Ff 33 ,, tt PP 33 ,, tt 33 // 22 Ff 3,03,0 PP 3,03,0 33 // 22 ]] }}

测量得到的三方向投影面积和周长随时间的变化数据见表3;测量得到的三方向形状系数和三方向溶胀体积及其平均值的变化见表4;测量得到的水中黄豆的形状系数和体积溶胀率随时间的变化规律见图8。The measured three-direction projected area and perimeter change data over time are shown in Table 3; the measured three-direction shape coefficient and three-direction swelling volume and their average changes are shown in Table 4; the measured shape coefficient and volume swelling of soybeans in water The rate change over time can be seen in Figure 8.

表1.测量的煤粒试样的三方向投影面积和周长随时间的变化(图7使用的数据,0.6~0.9mm大同烟煤,28℃砒啶溶液)Table 1. Changes in the three-direction projected area and perimeter of the measured coal particle samples over time (data used in Figure 7, 0.6-0.9 mm Datong bituminous coal, 28 ° C pyridine solution)

  时间(分) Time (minutes)   P1(μm2)P 1 (μm 2 )   P2(μm2)P 2 (μm 2 )   P3(μm2)P 3 (μm 2 )   周长1(μm) Circumference 1(μm)   周长2(μm) Circumference 2 (μm)   周长3(μm) Circumference3(μm)   0 0   10430 10430   10269 10269   13924 13924   408.8 408.8   439.1 439.1   486.6 486.6   10 10   14254 14254   13883 13883   20473 20473   483.9 483.9   511.9 511.9   592.6 592.6   20 20   16191 16191   14319 14319   23354 23354   514.9 514.9   519.7 519.7   630.6 630.6   30 30   17338 17338   15742 15742   24774 24774   526.9 526.9   561.9 561.9   657.2 657.2   40 40   18298 18298   16483 16483   26181 26181   548.0 548.0   574.5 574.5   694.3 694.3   50 50   18566 18566   17149 17149   26928 26928   553.5 553.5   588.4 588.4   700.5 700.5   60 60   18759 18759   17584 17584   27281 27281   554.6 554.6   595.6 595.6   709.7 709.7   70 70   19057 19057   17650 17650   27683 27683   555.6 555.6   620.6 620.6   711.2 711.2   80 80   19236 19236   17775 17775   27997 27997   560.6 560.6   623.7 623.7   721.4 721.4   90 90   19591 19591   17862 17862   28405 28405   560.3 560.3   625.2 625.2   721.7 721.7   100 100   19824 19824   18210 18210   28404 28404   566.7 566.7   632.7 632.7   721.0 721.0

  180 180   20576 20576   18517 18517   29215 29215   575.4 575.4   631.6 631.6   733.9 733.9   220 220   20581 20581   18676 18676   29638 29638   574.3 574.3   635.5 635.5   742.0 742.0   250 250   20595 20595   18900 18900   29720 29720   575.1 575.1   637.0 637.0   737.1 737.1   280 280   20600 20600   18914 18914   29896 29896   575.5 575.5   630.5 630.5   736.8 736.8   310 310   20605 20605   18958 18958   30048 30048   576.1 576.1   636.1 636.1   742.8 742.8   340 340   20868 20868   18973 18973   30169 30169   580.0 580.0   636.7 636.7   745.0 745.0   370 370   20900 20900   19023 19023   30345 30345   579.4 579.4   639.1 639.1   748.6 748.6   400 400   21043 21043   19161 19161   30381 30381   581.1 581.1   643.1 643.1   756.4 756.4   500 500   21276 21276   19645 19645   30727 30727   585.5 585.5   651.3 651.3   762.5 762.5   560 560   21211 21211   19692 19692   30800 30800   585.3 585.3   653.5 653.5   764.3 764.3   620 620   21292 21292   19853 19853   30885 30885   588.1 588.1   660.9 660.9   765.9 765.9   740 740   21350 21350   19909 19909   30960 30960   589.1 589.1   662.1 662.1   767.3 767.3   860 860   21456 21456   19950 19950   30969 30969   590.1 590.1   662.5 662.5   766.0 766.0   980 980   21618 21618   20204 20204   31000 31000   592.0 592.0   662.4 662.4   766.2 766.2   1000 1000   21690 21690   20191 20191   31050 31050   592.0 592.0   662.7 662.7   766.3 766.3   1120 1120   21707 21707   20213 20213   31101 31101   592.0 592.0   662.5 662.5   766.5 766.5   1240 1240   21754 21754   20250 20250   31105 31105   592.1 592.1   663.0 663.0   766.8 766.8   1360 1360   21772 21772   20253 20253   31144 31144   592.3 592.3   662.4 662.4   765.9 765.9

表2.测量的煤粒试样的三方向的形状系数和溶胀率及其平均值的变化(图7使用的数据,0.6~0.9mm大同烟煤,28℃砒啶溶液)Table 2. The three-direction shape coefficient and swelling rate of the measured coal particle samples and their average changes (data used in Figure 7, 0.6-0.9mm Datong bituminous coal, 28 ℃ pyridine solution)

  时间(分) Time (minutes)   F1(-)F 1 (-)   F2(-)F 2 (-)   F3(-)F 3 (-)   Qvt,1(-)Qvt , 1 (-)   Qvt,2(-)Q vt, 2 (-)   Qvt,3(-)Q vt, 3 (-)   Qvt(-)Q vt (-)   0 0   0.78 0.78   0.67 0.67   0.74 0.74   1 1   1 1   1 1   1 1   10 10   0.76 0.76   0.67 0.67   0.73 0.73   1.56 1.56   1.56 1.56   1.77 1.77   1.64 1.64   20 20   0.77 0.77   0.67 0.67   0.74 0.74   1.89 1.89   1.64 1.64   2.17 2.17   1.91 1.91   30 30   0.78 0.78   0.63 0.63   0.72 0.72   2.14 2.14   1.78 1.78   2.31 2.31   2.10 2.10   40 40   0.77 0.77   0.63 0.63   0.68 0.68   2.27 2.27   1.91 1.91   2.38 2.38   2.20 2.20   50 50   0.76 0.76   0.62 0.62   0.69 0.69   2.31 2.31   2.01 2.01   2.51 2.51   2.29 2.29   60 60   0.77 0.77   0.62 0.62   0.68 0.68   2.36 2.36   2.09 2.09   2.53 2.53   2.34 2.34   70 70   0.78 0.78   0.58 0.58   0.69 0.69   2.44 2.44   1.94 1.94   2.61 2.61   2.35 2.35   80 80   0.77 0.77   0.57 0.57   0.68 0.68   2.46 2.46   1.95 1.95   2.61 2.61   2.36 2.36   90 90   0.78 0.78   0.57 0.57   0.69 0.69   2.57 2.57   1.97 1.97   2.70 2.70   2.44 2.44   100 100   0.78 0.78   0.57 0.57   0.69 0.69   2.59 2.59   2.02 2.02   2.71 2.71   2.46 2.46   180 180   0.78 0.78   0.58 0.58   0.68 0.68   2.76 2.76   2.11 2.11   2.80 2.80   2.58 2.58   220 220   0.78 0.78   0.58 0.58   0.68 0.68   2.77 2.77   2.13 2.13   2.84 2.84   2.61 2.61   250 250   0.78 0.78   0.59 0.59   0.69 0.69   2.77 2.77   2.18 2.18   2.90 2.90   2.64 2.64   280 280   0.78 0.78   0.60 0.60   0.69 0.69   2.77 2.77   2.23 2.23   2.95 2.95   2.67 2.67   310 310   0.78 0.78   0.59 0.59   0.68 0.68   2.76 2.76   2.21 2.21   2.94 2.94   2.66 2.66   340 340   0.78 0.78   0.59 0.59   0.68 0.68   2.81 2.81   2.21 2.21   2.95 2.95   2.68 2.68   370 370   0.78 0.78   0.59 0.59   0.68 0.68   2.83 2.83   2.20 2.20   2.96 2.96   2.69 2.69

  400 400   0.78 0.78   0.58 0.58   0.67 0.67   2.86 2.86   2.22 2.22   2.91 2.91   2.69 2.69   500 500   0.78 0.78   0.58 0.58   0.66 0.66   2.90 2.90   2.30 2.30   2.95 2.95   2.74 2.74   560 560   0.78 0.78   0.58 0.58   0.66 0.66   2.88 2.88   2.30 2.30   2.95 2.95   2.74 2.74   620 620   0.77 0.77   0.57 0.57   0.66 0.66   2.88 2.88   2.29 2.29   2.96 2.96   2.74 2.74   740 740   0.77 0.77   0.57 0.57   0.66 0.66   2.89 2.89   2.30 2.30   2.96 2.96   2.74 2.74   860 860   0.77 0.77   0.57 0.57   0.66 0.66   2.91 2.91   2.31 2.31   2.98 2.98   2.76 2.76   980 980   0.78 0.78   0.58 0.58   0.66 0.66   2.95 2.95   2.39 2.39   2.98 2.98   2.80 2.80   1000 1000   0.78 0.78   0.58 0.58   0.66 0.66   2.97 2.97   2.38 2.38   2.99 2.99   2.81 2.81   1120 1120   0.78 0.78   0.58 0.58   0.67 0.67   2.98 2.98   2.39 2.39   3.01 3.01   2.82 2.82   1240 1240   0.78 0.78   0.58 0.58   0.66 0.66   2.99 2.99   2.40 2.40   3.00 3.00   2.83 2.83   1360 1360   0.78 0.78   0.58 0.58   0.67 0.67   3.00 3.00   2.40 2.40   3.02 3.02   2.83 2.83

表3.测量的黄豆试样的三方向投影面积和周长随时间的变化(图9使用的数据,5.5×5.5×6.5mm黄豆,27℃纯净水)Table 3. The three-direction projected area and perimeter of the measured soybean sample change with time (data used in Figure 9, 5.5×5.5×6.5mm soybeans, 27°C purified water)

  时间(分) Time (minutes)   P1(μm2)P 1 (μm 2 )   P2(μm2)P 2 (μm 2 )   P3(μm2)P 3 (μm 2 )   周长1(μm) Circumference 1(μm)   周长2(μm) Circumference 2 (μm)   周长3(μm) Circumference3(μm)   0 0   80072 80072   74916 74916   61184 61184   1088.6 1088.6   1063.1 1063.1   964 964   5.33 5.33   80805 80805   76143 76143   63832 63832   1101.1 1101.1   1074.6 1074.6   987 987   10.67 10.67   82746 82746   77397 77397   66748 66748   1124.1 1124.1   1081 1081   1002.4 1002.4   16 16   84034 84034   77972 77972   68533 68533   1128.5 1128.5   1081.2 1081.2   1013.9 1013.9   21.33 21.33   85513 85513   78176 78176   70095 70095   1132.1 1132.1   1088.5 1088.5   1025.8 1025.8   26.67 26.67   86612 86612   78281 78281   70719 70719   1140.8 1140.8   1095.4 1095.4   1028.3 1028.3   32 32   88492 88492   78853 78853   70832 70832   1145.7 1145.7   1095.3 1095.3   1028.3 1028.3   37.33 37.33   88755 88755   80294 80294   71137 71137   1151.2 1151.2   1096.7 1096.7   1032.4 1032.4   42.67 42.67   89904 89904   81312 81312   71989 71989   1165.8 1165.8   1108.9 1108.9   1032.0 1032.0   48 48   92456 92456   81623 81623   72841 72841   1187.2 1187.2   1133.1 1133.1   1039.3 1039.3   53.33 53.33   94559 94559   83442 83442   73217 73217   1194.6 1194.6   1143.0 1143.0   1043.3 1043.3   58.67 58.67   96874 96874   85007 85007   74181 74181   1228.8 1228.8   1152.9 1152.9   1054.3 1054.3   64 64   98826 98826   89424 89424   75764 75764   1250.9 1250.9   1180.3 1180.3   1069.1 1069.1   69.33 69.33   100654 100654   89938 89938   77162 77162   1256.1 1256.1   1186.3 1186.3   1093.2 1093.2   74.67 74.67   104385 104385   95982 95982   77656 77656   1288.1 1288.1   1209.2 1209.2   1093.5 1093.5   80 80   105441 105441   98376 98376   79045 79045   1290.9 1290.9   1230.5 1230.5   1109.4 1109.4   85.33 85.33   106921 106921   101029 101029   81077 81077   1291.8 1291.8   1246.6 1246.6   1113.6 1113.6   90.67 90.67   110415 110415   101935 101935   82093 82093   1298.7 1298.7   1252.6 1252.6   1116.9 1116.9   96 96   111956 111956   105185 105185   83779 83779   1322 1322   1285.8 1285.8   1138.3 1138.3   101.33 101.33   111210 111210   107132 107132   84994 84994   1325 1325   1307.5 1307.5   1152.5 1152.5   106.67 106.67   115487 115487   107248 107248   86248 86248   1345.1 1345.1   1308.2 1308.2   1160.3 1160.3   112 112   119399 119399   107817 107817   87069 87069   1352.9 1352.9   1308.6 1308.6   1164.3 1164.3   117.33 117.33   120374 120374   108039 108039   89119 89119   1354.9 1354.9   1308.7 1308.7   1175.4 1175.4   122.67 122.67   124029 124029   108465 108465   90403 90403   1381.5 1381.5   1316.5 1316.5   1177.5 1177.5   128 128   124425 124425   111400 111400   91900 91900   1386.8 1386.8   1320.3 1320.3   1189.4 1189.4   133.33 133.33   126027 126027   113053 113053   92020 92020   1389.6 1389.6   1323.7 1323.7   1190.2 1190.2

  138.67 138.67   127263 127263   115154 115154   93206 93206   1392.7 1392.7   1333.8 1333.8   1195.4 1195.4   144 144   128146 128146   117863 117863   93650 93650   1404.4 1404.4   1363.5 1363.5   1199.6 1199.6   149.33 149.33   130129 130129   120108 120108   94049 94049   1412.7 1412.7   1376.5 1376.5   1206.9 1206.9   154.67 154.67   131395 131395   120498 120498   94483 94483   1428.5 1428.5   1383.6 1383.6   1217.2 1217.2   160 160   132041 132041   124174 124174   96494 96494   1438.4 1438.4   1402.9 1402.9   1226.4 1226.4   165.33 165.33   135607 135607   126129 126129   97388 97388   1457.2 1457.2   1426.8 1426.8   1244.9 1244.9   170.67 170.67   137305 137305   128201 128201   98639 98639   1463.4 1463.4   1429.2 1429.2   1246.5 1246.5   176 176   140256 140256   130866 130866   99074 99074   1494.3 1494.3   1464.6 1464.6   1259.6 1259.6   181.33 181.33   141213 141213   132459 132459   101146 101146   1522.3 1522.3   1479.1 1479.1   1269.1 1269.1   186.67 186.67   142830 142830   133972 133972   101844 101844   1526.3 1526.3   1490.1 1490.1   1289.1 1289.1   192 192   145851 145851   135383 135383   101892 101892   1531.9 1531.9   1500.1 1500.1   1278.9 1278.9   197.33 197.33   147295 147295   137376 137376   102755 102755   1545.1 1545.1   1511.9 1511.9   1276.4 1276.4   202.67 202.67   148025 148025   138175 138175   105715 105715   1545.1 1545.1   1514 1514   1287.6 1287.6   208 208   149355 149355   139446 139446   106403 106403   1553.8 1553.8   1521 1521   1295.1 1295.1   213.33 213.33   150686 150686   139989 139989   109657 109657   1557.6 1557.6   1525.9 1525.9   1314.7 1314.7   277.33 277.33   156867 156867   143403 143403   113532 113532   1595.2 1595.2   1546.5 1546.5   1343.4 1343.4   341.33 341.33   158129 158129   145834 145834   114142 114142   1599.6 1599.6   1561.6 1561.6   1347.3 1347.3   469.33 469.33   159375 159375   149397 149397   114991 114991   1618.7 1618.7   1581.6 1581.6   1365.6 1365.6   597.33 597.33   159919 159919   151306 151306   115270 115270   1623.7 1623.7   1590.8 1590.8   1367.0 1367.0   853.33 853.33   160000 160000   152929 152929   115313 115313   1624.2 1624.2   1594.8 1594.8   1374.9 1374.9   1109.33 1109.33   160082 160082   153777 153777   115643 115643   1625 1625   1600.8 1600.8   1380.3 1380.3   1388.8 1388.8   160360 160360   154470 154470   115924 115924   1626.6 1626.6   1601.7 1601.7   1386.9 1386.9

表4.测量的黄豆试样的形状系数和溶胀体积及其平均值的变化(图9使用的数据,5.5×5.5×6.5mm黄豆,27℃纯净水)Table 4. The measured shape coefficient and swollen volume of soybean samples and their average changes (data used in Figure 9, 5.5 × 5.5 × 6.5 mm soybeans, 27 ° C purified water)

  时间(分) Time (minutes)   F1(-)F 1 (-)   F2(-)F 2 (-)   F3(-)F 3 (-)   Qvt,1(-)Qvt , 1 (-)   Qvt,2(-)Q vt, 2 (-)   Qvt,3(-)Q vt, 3 (-)   Qvt(-)Q vt (-)   0 0   0.849 0.849   0.833 0.833   0.827 0.827   1 1   1 1   1 1   1.000 1.000   5.33 5.33   0.838 0.838   0.829 0.829   0.823 0.823   1.000 1.000   1.019 1.019   1.061 1.061   1.027 1.027   10.67 10.67   0.823 0.823   0.832 0.832   0.835 0.835   1.018 1.018   1.049 1.049   1.150 1.150   1.072 1.072   16 16   0.829 0.829   0.838 0.838   0.838 0.838   1.050 1.050   1.068 1.068   1.200 1.200   1.106 1.106   21.33 21.33   0.838 0.838   0.829 0.829   0.837 0.837   1.090 1.090   1.061 1.061   1.241 1.241   1.131 1.131   26.67 26.67   0.836 0.836   0.820 0.820   0.840 0.840   1.108 1.108   1.051 1.051   1.262 1.262   1.141 1.141   32 32   0.847 0.847   0.826 0.826   0.842 0.842   1.159 1.159   1.071 1.071   1.267 1.267   1.166 1.166   37.33 37.33   0.842 0.842   0.839 0.839   0.839 0.839   1.157 1.157   1.117 1.117   1.271 1.271   1.182 1.182   42.67 42.67   0.831 0.831   0.831 0.831   0.849 0.849   1.165 1.165   1.128 1.128   1.310 1.310   1.201 1.201   48 48   0.824 0.824   0.799 0.799   0.847 0.847   1.205 1.205   1.091 1.091   1.331 1.331   1.209 1.209   53.33 53.33   0.833 0.833   0.803 0.803   0.845 0.845   1.258 1.258   1.133 1.133   1.337 1.337   1.243 1.243   58.67 58.67   0.806 0.806   0.804 0.804   0.839 0.839   1.264 1.264   1.166 1.166   1.353 1.353   1.261 1.261   64 64   0.794 0.794   0.807 0.807   0.833 0.833   1.282 1.282   1.263 1.263   1.387 1.387   1.311 1.311   69.33 69.33   0.802 0.802   0.803 0.803   0.811 0.811   1.331 1.331   1.268 1.268   1.389 1.389   1.329 1.329

  74.67 74.67   0.791 0.791   0.825 0.825   0.816 0.816   1.386 1.386   1.436 1.436   1.410 1.410   1.411 1.411   80 80   0.795 0.795   0.816 0.816   0.807 0.807   1.415 1.415   1.475 1.475   1.432 1.432   1.441 1.441   85.33 85.33   0.805 0.805   0.817 0.817   0.822 0.822   1.463 1.463   1.536 1.536   1.515 1.515   1.505 1.505   90.67 90.67   0.823 0.823   0.816 0.816   0.827 0.827   1.569 1.569   1.556 1.556   1.553 1.553   1.559 1.559   96 96   0.805 0.805   0.799 0.799   0.813 0.813   1.567 1.567   1.597 1.597   1.574 1.574   1.579 1.579   101.33 101.33   0.796 0.796   0.787 0.787   0.804 0.804   1.534 1.534   1.617 1.617   1.591 1.591   1.581 1.581   106.67 106.67   0.802 0.802   0.788 0.788   0.805 0.805   1.636 1.636   1.619 1.619   1.629 1.629   1.628 1.628   112 112   0.820 0.820   0.791 0.791   0.807 0.807   1.758 1.758   1.640 1.640   1.656 1.656   1.685 1.685   117.33 117.33   0.824 0.824   0.793 0.793   0.811 0.811   1.789 1.789   1.648 1.648   1.722 1.722   1.720 1.720   122.67 122.67   0.817 0.817   0.786 0.786   0.819 0.819   1.854 1.854   1.645 1.645   1.779 1.779   1.759 1.759   128 128   0.813 0.813   0.803 0.803   0.816 0.816   1.855 1.855   1.748 1.748   1.816 1.816   1.806 1.806   133.33 133.33   0.820 0.820   0.811 0.811   0.816 0.816   1.907 1.907   1.804 1.804   1.820 1.820   1.844 1.844   138.67 138.67   0.825 0.825   0.813 0.813   0.820 0.820   1.946 1.946   1.861 1.861   1.863 1.863   1.890 1.890   144 144   0.816 0.816   0.797 0.797   0.818 0.818   1.947 1.947   1.887 1.887   1.872 1.872   1.902 1.902   149.33 149.33   0.819 0.819   0.797 0.797   0.811 0.811   1.999 1.999   1.941 1.941   1.869 1.869   1.937 1.937   154.67 154.67   0.809 0.809   0.791 0.791   0.801 0.801   2.003 2.003   1.937 1.937   1.859 1.859   1.933 1.933   160 160   0.802 0.802   0.793 0.793   0.806 0.806   2.000 2.000   2.031 2.031   1.930 1.930   1.987 1.987   165.33 165.33   0.803 0.803   0.779 0.779   0.790 0.790   2.083 2.083   2.042 2.042   1.917 1.917   2.014 2.014   170.67 170.67   0.806 0.806   0.789 0.789   0.798 0.798   2.131 2.131   2.120 2.120   1.974 1.974   2.075 2.075   176 176   0.789 0.789   0.767 0.767   0.785 0.785   2.155 2.155   2.125 2.125   1.954 1.954   2.078 2.078   181.33 181.33   0.766 0.766   0.761 0.761   0.789 0.789   2.112 2.112   2.147 2.147   2.027 2.027   2.096 2.096   186.67 186.67   0.770 0.770   0.758 0.758   0.770 0.770   2.162 2.162   2.177 2.177   1.999 1.999   2.113 2.113   192 192   0.781 0.781   0.756 0.756   0.783 0.783   2.261 2.261   2.205 2.205   2.033 2.033   2.167 2.167   197.33 197.33   0.775 0.775   0.755 0.755   0.793 0.793   2.278 2.278   2.251 2.251   2.085 2.085   2.205 2.205   202.67 202.67   0.779 0.779   0.758 0.758   0.801 0.801   2.307 2.307   2.278 2.278   2.200 2.200   2.261 2.261   208 208   0.777 0.777   0.757 0.757   0.797 0.797   2.332 2.332   2.309 2.309   2.210 2.210   2.284 2.284   213.33 213.33   0.780 0.780   0.756 0.756   0.797 0.797   2.373 2.373   2.317 2.317   2.312 2.312   2.334 2.334   277.33 277.33   0.775 0.775   0.753 0.753   0.791 0.791   2.502 2.502   2.396 2.396   2.415 2.415   2.437 2.437   341.33 341.33   0.777 0.777   0.752 0.752   0.790 0.790   2.538 2.538   2.450 2.450   2.434 2.434   2.474 2.474   469.33 469.33   0.764 0.764   0.751 0.751   0.775 0.775   2.528 2.528   2.537 2.537   2.413 2.413   2.493 2.493   597.33 597.33   0.762 0.762   0.751 0.751   0.775 0.775   2.534 2.534   2.589 2.589   2.423 2.423   2.515 2.515   853.33 853.33   0.762 0.762   0.756 0.756   0.767 0.767   2.535 2.535   2.646 2.646   2.397 2.397   2.526 2.526   1109.33 1109.33   0.762 0.762   0.754 0.754   0.763 0.763   2.536 2.536   2.662 2.662   2.396 2.396   2.531 2.531   1388.8 1388.8   0.762 0.762   0.757 0.757   0.757 0.757   2.542 2.542   2.689 2.689   2.387 2.387   2.540 2.540

Claims (4)

1.一种三维正交显微镜摄像观测装置,包括三台显微镜(1、2、3)、三台CCD摄像机(4、5、6)、三条数据线(7、8、9)和计算机(10),其特征是:所述装置使用三台万能台架(11、12、13)三维正交固定三台显微镜(1、2、3),三台显微镜(1、2、3)分别与三台CCD摄像机(4、5、6)相连,三台CCD摄像机(4、5、6)的三条数据线(7、8、9)分别与计算机(10)相连接;反应器台架(14)三维位置可调,反应器台架(14)上放置石英玻璃反应器(16),石英玻璃反应器(16)内放置试样(17)和溶液;多点光纤冷光源(15)的两个灯头设置在试样(17)的上方和下方;在石英玻璃透明反应器(16)的水平方向后方放置两个帮助获得清晰图像的背景色板。1. A three-dimensional orthogonal microscope imaging observation device, comprising three microscopes (1,2,3), three CCD cameras (4,5,6), three data lines (7,8,9) and computer (10 ), which is characterized in that: the device uses three universal stands (11, 12, 13) to fix three microscopes (1, 2, 3) three-dimensionally and orthogonally, and the three microscopes (1, 2, 3) are respectively connected with the three The CCD cameras (4, 5, 6) are connected, and the three data lines (7, 8, 9) of the three CCD cameras (4, 5, 6) are respectively connected with the computer (10); the reactor bench (14) The three-dimensional position is adjustable, and the quartz glass reactor (16) is placed on the reactor stand (14), and the sample (17) and solution are placed in the quartz glass reactor (16); two of the multi-point optical fiber cold light source (15) The lamp head is arranged above and below the sample (17); two background color plates to help obtain a clear image are placed behind the horizontal direction of the quartz glass transparent reactor (16). 2.根据权利要求1所述的三维正交显微镜摄像观测装置,其特征是:三台显微镜(1、2、3)的聚焦距离di(i=1,2,3)=40~110mm,三台显微镜(1、2、3)目镜放大倍率fi(i=1,2,3)=0.68~4.5。2. three-dimensional orthogonal microscope imaging observation device according to claim 1, characterized in that: the focal distance di (i=1,2,3)=40~110mm of three microscopes (1,2,3), The eyepiece magnification f i (i=1, 2, 3) of the three microscopes (1, 2, 3) = 0.68-4.5. 3.根据权利要求1所述的三维正交显微镜摄像观测装置,其特征是:所述反应器台架(14)有透明窗。3. The three-dimensional orthogonal microscope imaging observation device according to claim 1, characterized in that: the reactor stand (14) has a transparent window. 4.一种根据权利要求1所述的三维正交显微镜摄像观测装置的图像定量方法,其特征是:所述方法包括以下步骤:4. a kind of image quantification method of three-dimensional orthogonal microscope imaging observation device according to claim 1, is characterized in that: described method comprises the following steps: a.利用密度剃度离心分离等方法获得粒度、密度和成分相对均匀,储存状态一致的2~6组观测用试样(17);a. Obtain 2 to 6 groups of observation samples (17) with relatively uniform particle size, density and composition, and consistent storage state by using methods such as density ratio centrifugation; b.观测采用无溶液和有溶液两种方式,有溶液观测使用有机溶液或水;观测可在室温和环境压力下进行,也可在控制温度和控制压力条件下进行;b. Observation adopts two methods without solution and with solution, and with solution, organic solution or water is used for observation; observation can be carried out at room temperature and ambient pressure, or under controlled temperature and controlled pressure conditions; c.有溶液观测时,在观测温度和压力下,首先将3~5ml溶液注射进透明石英玻璃反应器(16),然后将试样(17)放入石英玻璃反应器(16)的溶液中后开始按设定时间三维正交显微镜摄像观测装置(三通道)自动定时摄像取样;c. When there is solution observation, under observation temperature and pressure, at first inject 3~5ml solution into transparent quartz glass reactor (16), then put sample (17) into the solution of quartz glass reactor (16) Afterwards, the three-dimensional orthogonal microscope camera observation device (three channels) will start automatically timing camera sampling according to the set time; d.对无溶液试样(17)三维方向的投影面积、投影面积周长进行测量;然后计算同一试样(17)三个方向的形状系数和体积;最后通过平均处理三维图像数据获得试样(17)的形状系数和体积;d. Measure the projected area and the perimeter of the projected area of the three-dimensional direction of the solution-free sample (17); then calculate the shape factor and volume of the same sample (17) in three directions; finally obtain the sample by averaging the three-dimensional image data (17) shape factor and volume; 试样(17)的体积V按式(1)计算:The volume V of the sample (17) is calculated according to formula (1): VV == 44 33 ππ (( Ff 11 PP 11 ++ Ff 22 PP 22 ++ Ff 33 PP 33 )) 33 22 33 -- -- -- (( 11 )) 式(1)中,P1、P2、P3分别为三维直交显微镜观测得到的同一试样(17)三个方向的投影面积;F1、F2、F3分别为三维直交显微镜观测得到的同一试样(17)三个方向的形状系数,由式(2)计算:In formula (1), P 1 , P 2 , and P 3 are the projected areas of the same sample ( 17 ) in three directions observed by a three-dimensional orthogonal microscope; The shape factor of the same sample (17) in three directions is calculated by formula (2):
Figure A2009101438780003C2
Figure A2009101438780003C2
e.对溶液中试样(17)三维方向图象的投影面积、投影面积周长进行测量;然后计算同一试样(17)三个方向的形状系数、体积变化率;最后通过平均处理三维图像数据获得试样(17)形状系数和体积变化率;e. Measure the projected area and the perimeter of the projected area of the three-dimensional image of the sample (17) in the solution; then calculate the shape factor and volume change rate of the same sample (17) in three directions; finally process the three-dimensional image by averaging Data acquisition sample (17) shape factor and volume change rate; 试样(17)在t时刻的体积变化率(Qv,t)定义为t时刻的试样(17)体积(Vt)与时刻的试样(17)体积(V0)之比,式(3):The volume change rate (Q v, t ) of sample (17) at time t is defined as the ratio of the volume of sample (17) at time t (V t ) to the volume of sample (17) at time (V 0 ), the formula (3): QQ vv ,, tt == VV tt VV 00 -- -- -- (( 33 )) 考虑到试样(17)本身形状的不规则性和试样(17)体积变化的异方性特点,将三个显微镜各自测得的t时刻试样(17)体积变化率的算术平均作为试样(17)在t时刻的体积变化率,式(4);Considering the irregularity of the shape of the sample (17) itself and the anisotropic characteristics of the volume change of the sample (17), the arithmetic mean of the volume change rate of the sample (17) measured by the three microscopes at time t is taken as The volume change rate of sample (17) at time t, formula (4); QQ vv ,, tt == 11 33 {{ [[ Ff 11 ,, tt PP 11 ,, tt 33 // 22 Ff 1,01,0 PP 1,01,0 33 // 22 ]] ++ [[ Ff 2,02,0 PP 22 ,, tt 33 // 22 Ff 2,02,0 PP 2,02,0 33 // 22 ]] ++ [[ Ff 33 ,, tt PP 33 ,, tt 33 // 22 Ff 3,03,0 PP 3,03,0 33 // 22 ]] }} -- -- -- (( 44 )) 式(4)中,Fi,t(i=1,2,3)是t时刻试样(17)在x,y,z三个方向的形状系数;Fi,0(i=1,2,3)是零时刻试样(17)在x,y,z三个方向的形状系数;Pi,t(i=1,2,3)是t时刻试样(17)在x,y,z三个方向的投影面积;Pi,0(i=1,2,3)是零时刻试样(17)在x,y,z三个方向的投影面积;式(4)可简写为式(5);In formula (4), F i , t (i=1, 2, 3) is the shape coefficient of the sample (17) in the three directions of x, y, and z at time t; F i, 0 (i=1, 2 , 3) is the shape factor of the sample (17) at the time of zero in x, y, and z directions; The projected area in the three directions of z; Pi ,0 (i=1, 2, 3) is the projected area of the sample (17) at zero time in the three directions of x, y, and z; formula (4) can be abbreviated as formula (5); QQ vv ,, tt == 11 33 (( QQ 11 vv ,, tt ++ QQ 22 vv ,, tt ++ QQ 33 vv ,, tt )) -- -- -- (( 55 )) 式(5)中,Qiv,t(i=1,2,3)是t时刻试样(17)在x,y,z三个方向的体积变化率;In formula (5), Q iv, t (i=1,2,3) is the volume change rate of sample (17) at time t in x, y, three directions of z; 由于试样中含有的体积不变物质,如矿物杂质等的体积应当从试样(17)体积中扣除;采用式(6)修正式(4)和式(5);Due to the volume-invariant substances contained in the sample, such as the volume of mineral impurities, etc. should be deducted from the volume of the sample (17); use formula (6) to correct formula (4) and formula (5); QQ dmmfdmmf == (( QQ measuredmeasured -- ythe y )) (( 11 -- ythe y )) -- -- -- (( 66 )) 式(6)中,Qdmmf为干燥基无体积变化物质试样(17)的体积变化率,Qmeasured为观测试样(17)的体积变化率;In the formula (6), Qdmmf is the volume change rate of the dry base non-volume change material sample (17), and Q measured is the volume change rate of the observed sample (17);
Figure A2009101438780004C2
Figure A2009101438780004C2
修正后的式(4)和式(5)成为式(8)和式(9);The revised formula (4) and formula (5) become formula (8) and formula (9); QQ vv ,, tt == {{ 11 33 [[ (( Ff 11 ,, tt PP 11 ,, tt 33 // 22 Ff 1,01,0 PP 1,01,0 33 // 22 )) ++ (( Ff 22 ,, tt PP 22 ,, tt 33 // 22 Ff 2,02,0 PP 2,02,0 33 // 22 )) ++ (( Ff 33 ,, tt PP 33 ,, tt 33 // 22 Ff 3,03,0 PP 3,03,0 33 // 22 )) ]] -- ythe y }} (( 11 -- ythe y )) -- -- -- (( 88 )) QQ vv ,, tt == {{ 11 33 (( QQ 11 vv ,, tt ++ QQ 22 vv ,, tt ++ QQ 33 vv ,, tt )) -- ythe y }} (( 11 -- ythe y )) -- -- -- (( 99 )) 式(8)和式(9)是本发明中试样体(17)积变化率的通用计算式;当y=0时,即试样(17)不含体积不变物质时,式(8)和式(9)成为式(4)和式(5)。Formula (8) and formula (9) are the general calculation formulas of sample body (17) volume change rate among the present invention; ) and formula (9) become formula (4) and formula (5).
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Open date: 20091021