CN114184518A - Device and method for high-precision determination of solubility of hydrophobic organic matter in subcritical water - Google Patents
Device and method for high-precision determination of solubility of hydrophobic organic matter in subcritical water Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 73
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000005416 organic matter Substances 0.000 title claims description 22
- 239000010453 quartz Substances 0.000 claims abstract description 158
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 158
- 239000002904 solvent Substances 0.000 claims abstract description 13
- 238000005259 measurement Methods 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 8
- 230000000007 visual effect Effects 0.000 claims description 8
- 238000001514 detection method Methods 0.000 claims description 7
- 230000008859 change Effects 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 4
- 239000007924 injection Substances 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- 238000003466 welding Methods 0.000 claims description 3
- 230000033228 biological regulation Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000012071 phase Substances 0.000 description 11
- 238000001308 synthesis method Methods 0.000 description 7
- 238000004364 calculation method Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
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- 238000005070 sampling Methods 0.000 description 3
- 229910052594 sapphire Inorganic materials 0.000 description 3
- 239000010980 sapphire Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
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- 230000001276 controlling effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011197 physicochemical method Methods 0.000 description 1
- 150000003071 polychlorinated biphenyls Chemical group 0.000 description 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
- G01N7/02—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder
- G01N7/04—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder by absorption or adsorption alone
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Abstract
The invention discloses a device and a method for measuring the solubility of hydrophobic organic matters in subcritical water with high precision, wherein the device comprises a quartz capillary balance kettle, a temperature controller, a circulating water system, a cold-hot table, a camera, a microscope and a computer, wherein a quartz capillary with the outer diameter smaller than the inner diameter of the capillary balance kettle is loaded in the quartz capillary balance kettle; the device comprises a quartz capillary tube, a microscope, a camera and a computer, wherein hydrophobic organic matters are sucked in the quartz capillary tube, two ends of the quartz capillary tube are opened, solvent water is injected into a quartz capillary tube balance kettle, the microscope is used for observing images of the water in the quartz capillary tube balance kettle and the hydrophobic organic matters in the quartz capillary tube, the camera is used for collecting the images of the water and the hydrophobic organic matters observed by the microscope, and image data are transmitted to the computer. The method can accurately measure the solubility of different hydrophobic organic matters in subcritical water, and the device is simple, high in measurement precision, safe and efficient.
Description
Technical Field
The invention belongs to the technical field of chemistry, chemical industry and environment, and particularly relates to a device and a method for high-precision determination of solubility of hydrophobic organic matters in subcritical water.
Background
The subcritical water technology has the advantages of no toxicity, low cost, easy acquisition and the like, is gradually applied to the degradation and reclamation of wastes, the extraction of compounds such as polycyclic aromatic hydrocarbon, polychlorinated biphenyl and the like from soil, and the preparation of particles of hydrophobic drugs and hydrophobic materials and the like. Despite the great advantages of subcritical water treatment technology, many potential applications have not yet been developed due to the lack of basic data. Solubility studies of hydrophobic organics in subcritical water are essential to separation and extraction process design, as they quantify the ability of subcritical water to act as a solvent, thereby determining the feasibility and economic benefits of a particular process.
Because the equilibrium measurement under the conditions of high temperature and high pressure is complex and difficult, the solubility data of the hydrophobic organic matters in the range of 100-374 ℃ is less. At present, many methods and techniques are available for experimental studies of high-temperature and high-pressure phase equilibrium, and can be divided into two main categories: analytical methods and synthetic methods. The analytical method involves analytical determination of the phase composition in coexistence, at the start of the experiment, when the autoclave is filled with various components, the mixture is separated into two or more phases under a certain temperature and pressure condition, and the phase composition in the equilibrium chamber is analyzed by sampling from each phase and analyzing these samples under the ambient pressure outside the equilibrium chamber or applying a physicochemical method. The synthesis method is to add a mixture of precisely known ingredients to an equilibrium still, then observe the phase behavior in the equilibrium still, and measure the properties (e.g., pressure and temperature) at equilibrium, without sampling. The synthesis method can be classified into a visible synthesis method and a non-visible synthesis method, and among the methods for measuring the solubility of a high-temperature high-pressure system, the visible synthesis method is the most commonly used method type. Researchers have built various visual synthesis research devices, mainly using sapphire, quartz or glass balance kettles or observation windows, and different methods for analyzing phase balance data. For example, Fonseca et al (Jose M.S. Fonseca, R Dohrn, S Peper. journal of Supercritical Fluids,2014,86:49-56) have established a set of stainless steel equilibrium still experimental apparatus with sapphire windows using visual synthesis for measuring the solubility data of methane and carbon dioxide in water at a temperature of 243-353K and a pressure of 20 MPa. The sapphire windows are scaled and after calibration, the volume occupied by each phase can be determined. The cylinder was separated from the autoclave and weighed to determine the amount of gas added to the balance kettle. From the volume and density of the gas phase at equilibrium, the solubility of the gas in the liquid phase can be calculated. The method has the problems of large volume of the balance kettle, long balance time and the like.
Disclosure of Invention
Aiming at the problems of complexity and low efficiency of the prior determination technology device, the invention provides a device and a method for high-precision determination of the solubility of hydrophobic organic matters in subcritical water on the basis of the prior patent application CN202110247139.6 through improvement, wherein the determination temperature range is increased from 0-100 ℃ to 100-374 ℃, and the device can resist 120MPa high pressure at most. Compared with the prior art for measuring the solubility of the hydrophobic inorganic substance in a high-temperature and high-pressure subcritical water system, the device is simple, high in measurement precision, safe and efficient.
The device for high-precision determination of the solubility of the hydrophobic organic matters in subcritical water comprises a quartz capillary balance kettle, a temperature controller, a circulating water system, a cold and hot table, a camera, a microscope and a computer; wherein the quartz capillary balance kettle is loaded with a quartz capillary with an outer diameter smaller than the inner diameter of the quartz capillary balance kettle; absorb in the quartz capillary and have hydrophobic organic matter and both ends opening, the injection has solvent water and both ends all to seal in the quartz capillary balance kettle, temperature control appearance, circulating water system and cold and hot platform are used for carrying out the temperature regulation and control to the quartz capillary balance kettle, the microscope is used for observing the image of hydrophobic organic matter in the water and the quartz capillary in the quartz capillary balance kettle, camera and computer are by circuit connection, and the camera is used for gathering the water and the hydrophobic organic matter image that the microscope was surveyd to image data transmission in the computer.
The method for high-precision determination of the solubility of the hydrophobic organic matter in subcritical water is characterized by comprising the following steps:
s1: one end of the quartz capillary tube balance kettle is opened, the other end of the quartz capillary tube balance kettle is sealed, water is injected into the quartz capillary tube balance kettle by a miniature injector, the water is centrifuged to the bottom end sealing position of the quartz capillary tube balance kettle by a capillary centrifuge, then a microscope is adopted to observe the water image in the quartz capillary tube balance kettle, and an online image acquisition and detection device and a computer are utilized to record and calculate the volume of the injected water;
s2: placing the quartz capillary tube with the hydrophobic organic matters absorbed inside into the quartz capillary tube balance kettle treated in the step S1, sealing an opening at one end of the quartz capillary tube balance kettle by oxyhydrogen flame welding, and cooling; horizontally placing a quartz capillary tube balance kettle, wherein water in the quartz capillary tube balance kettle just overflows two end openings of the quartz capillary tube, observing a length image of hydrophobic organic matters in the quartz capillary tube by using a microscope, measuring the length of the hydrophobic organic matters in the quartz capillary tube by using an online image acquisition and detection device and a computer, and calculating to obtain the initial volume of solute hydrophobic organic matters;
s3: and finally, placing the quartz capillary tube balance kettle filled with the quartz capillary tube in a cold and hot table of a temperature control device, heating the quartz capillary tube balance kettle, carrying out phase behavior observation on hydrophobic organic matters in the quartz capillary tube during the heating, recording the change condition of the residual quantity of the hydrophobic organic matters in the quartz capillary tube, recording the temperature T when the quartz capillary tube is just completely dissolved and the system reaches a uniform state, and calculating to obtain the solubility of the hydrophobic organic matters at the temperature.
The manufacturing method of the quartz capillary tube with the hydrophobic organic matters absorbed inside comprises the following steps: intercepting a certain length of quartz capillary tube, burning off an organic coating on the outer surface of the quartz capillary tube by oxyhydrogen flame to form a transparent visual tube body, then absorbing a certain amount of hydrophobic organic matters by the transparent visual quartz capillary tube, and absorbing a small amount of solvent water at two ends of the quartz capillary tube after absorbing the organic matters for plugging the organic matters in the quartz capillary tube.
Further, the solubility of hydrophobic organic substances in water generally increases gradually with increasing temperature. Therefore, it is possible to fabricate quartz capillaries loaded with different contents of hydrophobic organic substances, load the quartz capillaries in quartz capillary equilibrium vessels, and repeat the above-mentioned operations from S1 to S3 to test temperature data corresponding to solubility data of hydrophobic organic substances in water of different volumes.
The method for high-precision determination of the solubility of the hydrophobic organic matter in subcritical water is characterized in that the inner diameter of the quartz capillary equilibrium kettle is 0.250-0.350 mm, and the outer diameter of the quartz capillary equilibrium kettle is 0.375-0.665 mm; the inner diameter of the quartz capillary tube is 0.020-0.080 mm, and the outer diameter of the quartz capillary tube is 0.100-0.200 mm; the length of the quartz capillary is less than that of the quartz capillary balance kettle.
The method for high-precision determination of the solubility of the hydrophobic organic matter in subcritical water is characterized in that in step S3, the temperature range of the quartz capillary equilibrium kettle for temperature rise determination is 100-374 ℃, and the pressure in the quartz capillary equilibrium kettle is the saturated vapor pressure of a hydrophobic organic matter-water system.
The method for high-precision determination of the solubility of the hydrophobic organic matter in subcritical water is characterized in that in step S3, the total time for determination when the dissolution equilibrium is reached is 0.5-2 days.
Compared with the prior art, the invention has the beneficial effects that:
1. compared with the CN202110247139.6, the method for measuring the solubility of the organic matters in water can measure the solubility data of a plurality of temperature points by using one reactor, namely, in order to solve the problem that the organic matters can obviously change in volume (absorb water and thermally expand) under the subcritical water temperature and pressure condition, namely, in order to avoid the influence of the volume change of the organic matters under the subcritical water temperature and pressure condition, a test method of 'enabling the organic matters to be just completely dissolved to obtain the solubility of the temperature and pressure condition at the moment' is adopted, so that the detection precision can be obviously improved, and the error is reduced.
2. According to the basic principle of a visual synthesis method, a quartz capillary tube is used as a balance kettle, so that a high-temperature high-pressure system of subcritical water can be measured; the solute (namely the hydrophobic organic matter) is absorbed by the quartz capillary with smaller size, and the solubility data is obtained by calculation, so that the solubility measurement precision is improved.
3. The measuring process does not need sampling, the balance kettle is small in size and simple and convenient to operate, the measuring efficiency of the visual synthesis method is improved, and the experiment cost is further reduced.
Drawings
FIG. 1 is a schematic diagram of the structure of a quartz capillary and a quartz capillary equilibrium vessel according to the present invention;
FIG. 2 is a schematic configuration diagram of an apparatus for measuring solubility of a hydrophobic organic substance in subcritical water according to the present invention.
Detailed Description
The present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the invention.
Example (b): compare FIGS. 1-2
The present invention provides an apparatus for measuring solubility of a hydrophobic organic substance in subcritical water with high accuracy, comprising: the device comprises a quartz capillary tube balance kettle 1, a temperature controller 3, a circulating water system 4, a cold and hot platform 5, a camera 6, a microscope 7 and a computer 8, wherein the quartz capillary tube 2 with the outer diameter smaller than the inner diameter of the quartz capillary tube balance kettle is loaded in the quartz capillary tube balance kettle 1, hydrophobic organic matters are sucked in the quartz capillary tube 2, two ends of the quartz capillary tube 2 are opened, solvent water is injected in the quartz capillary tube balance kettle 1, and two ends of the quartz capillary tube balance kettle 1 are sealed; the temperature controller 3, the circulating water system 4 and the cold and hot table 5 are used for regulating and controlling the temperature of the quartz capillary balance kettle; the microscope 7 is used for observing images of water in the quartz capillary balance kettle 1 and hydrophobic organic matters in the quartz capillary 2; the camera 6 is connected with the computer 8 through a circuit, and the camera 6 is used for collecting the water and hydrophobic organic matter images observed by the microscope 7 and transmitting the image data to the computer 7; the solvent water in the quartz capillary balance kettle 1 just can immerse the two end openings of the quartz capillary 2.
The temperature control device adopts a cold-hot table, and the temperature can be accurately regulated and controlled. Further, the device of the application also comprises a micro sample injection needle so as to inject solvent water into the quartz capillary balance kettle through the micro sample injection needle.
In the comparison of fig. 2, the device of the present application further includes a cold-hot table 5, the quartz capillary equilibrium still 1 is placed in the cold-hot table 5, and the temperature of the cold-hot table 5 is adjusted through the temperature controller 3 and the circulating water system 4, so that the quartz capillary equilibrium still 1 is at the required temperature. The cold and hot table 5 is placed under a microscope 7, and the quartz capillary balance kettle 1 can be directly observed through the microscope 7.
The specific process flow for determining the solubility of the hydrophobic organic matter in the subcritical water comprises the following steps:
s1: intercepting a certain length of quartz capillary tube 2, burning off an organic coating on the outer surface of the quartz capillary tube by oxyhydrogen flame to form a transparent visible tube body, absorbing a certain amount of hydrophobic organic matters by the transparent visible quartz capillary tube 2, and absorbing a small amount of solvent water at two ends of the quartz capillary tube after absorbing the organic matters for plugging so as to prevent the organic matters in the quartz capillary tube 2 from being extruded out due to capillary action;
s2: in addition, a quartz capillary tube with a certain length and a relatively large size is cut, one end of the quartz capillary tube is welded and sealed by oxyhydrogen flame, and the other end of the quartz capillary tube is provided with an opening and is used as a quartz capillary tube balance kettle. Injecting water into a quartz capillary balance kettle by using a micro injector, centrifuging the water to the bottom end of a seal of the quartz capillary balance kettle by using a capillary centrifuge, observing an image of the water in the quartz capillary balance kettle by using a microscope, and recording and calculating the volume of the injected water by using an online image acquisition and detection device and a computer;
and (4) placing the quartz capillary tube with the hydrophobic organic matters absorbed inside obtained in the step (S1) into the quartz capillary tube balance kettle after the treatment, sealing an opening at one end of the quartz capillary tube balance kettle by oxyhydrogen flame welding, and cooling to obtain the quartz capillary tube balance kettle 1 filled with the solvent, the solute and the quartz capillary tube 2. The quartz capillary tube balance kettle is horizontally arranged, and water in the quartz capillary tube balance kettle just submerges openings at two ends of the quartz capillary tube.
S3: observing the length image of the hydrophobic organic matter in the quartz capillary tube by using a microscope, measuring the length of the hydrophobic organic matter in the quartz capillary tube by using an online image acquisition and detection device and a computer, and calculating to obtain the initial volume of the solute hydrophobic organic matter;
s4: and finally, placing the quartz capillary tube balance kettle filled with the quartz capillary tube in a cold and hot table of a temperature control device, heating the quartz capillary tube balance kettle, carrying out phase behavior observation on hydrophobic organic matters in the quartz capillary tube during the heating, recording the change condition of the residual quantity of the hydrophobic organic matters in the quartz capillary tube, recording the temperature T when the quartz capillary tube is just completely dissolved and the system reaches a uniform state, and calculating to obtain the solubility of the hydrophobic organic matters at the temperature.
Furthermore, the inner diameter of the quartz capillary tube balance kettle is 0.250-0.350 mm, and the outer diameter is 0.375-0.665 mm; the inner diameter of the quartz capillary tube is 0.020-0.080 mm, and the outer diameter of the quartz capillary tube is 0.100-0.200 mm; the length of the quartz capillary is less than that of the quartz capillary balance kettle.
In the step S2, the volume of the water injected into the quartz capillary balance kettle is calculated, and the calculation method can refer to the doctor academic thesis (micro capillary balance kettle and in-situ raman spectroscopy combined study for simulating CO under geological conditions)2Oil model compound swelling law, authors beck et al, university of industry, zhejiang). The specific calculation method comprises the following steps: recording images of water in the quartz capillary by using a camera and a computer, approximately dividing the images into regular pattern cones, round tables, cylinders and segments, and respectively measuring the volume of each image:
radius of conical bottom surface r1And height h1(ii) a Radius R of bottom surface of circular truncated cone2Radius of the top surface r2And height h2(ii) a Length of cylinder3And a bottom surface radius r3(ii) a And the height h of the segment4And radius r of the corresponding sphere4Then according to the liquid density calculating the volume and mass of injected water to obtain initial solvent water volume VWater (W). The calculation formula is as follows:
Vcylinder＝πr3 2l3...........................(3)
VWater (W)＝VCone with conical surface+VRound table+VCylinder-VSegment of ball.................(5)
The formulas (1) to (5) are respectively the volume of a cone graph, the volume of a circular truncated cone graph, the volume of a cylindrical graph, the volume of a spherical segment graph and the volume of water.
In step S4, the temperature range of the quartz capillary equilibrium still for temperature rise measurement is 100-374 ℃, and the pressure in the quartz capillary equilibrium still is the saturated vapor pressure of the hydrophobic organic matter-water system. In step S4, the total time measured to reach the dissolution equilibrium is 0.5 to 2 days.
In step S4, when the temperature of the quartz capillary equilibrium still is raised, the temperature raising rate may be decreased as the remaining amount of the hydrophobic organic substance in the quartz capillary gradually decreases. For example, when the remaining amount of undissolved hydrophobic organic matter in the quartz capillary is less than 5%, the heating rate is adjusted to 0.5-2 ℃/h, and the temperature is kept at 0.5-2 ℃ per liter for dissolving for 1-3 hours.
When the hydrophobic organic matter in the quartz capillary tube is dissolved in the solvent water and reaches the end point (for example, the residual quantity of the undissolved hydrophobic organic matter is less than 5%), the heating rate is correspondingly reduced, and the temperature is raised at certain intervals, and the temperature is kept for dissolving for certain time. By the method, the temperature of the completely dissolved hydrophobic organic matter can be accurately monitored, and the error is small.
The statements in this specification merely set forth a list of implementations of the inventive concept and the scope of the present invention should not be construed as limited to the particular forms set forth in the examples.
Claims (6)
1. A method for high-precision determination of solubility of hydrophobic organic matters in subcritical water is characterized by comprising the following steps:
s1: one end of the quartz capillary tube balance kettle is opened, the other end of the quartz capillary tube balance kettle is sealed, water is injected into the quartz capillary tube balance kettle by a miniature injector, the water is centrifuged to the bottom end sealing position of the quartz capillary tube balance kettle by a capillary centrifuge, then a microscope is adopted to observe the water image in the quartz capillary tube balance kettle, and an online image acquisition and detection device and a computer are utilized to record and calculate the volume of the injected water;
s2: placing the quartz capillary tube with the hydrophobic organic matters absorbed inside into the quartz capillary tube balance kettle treated in the step S1, sealing an opening at one end of the quartz capillary tube balance kettle by oxyhydrogen flame welding, and cooling; horizontally placing a quartz capillary tube balance kettle, wherein water in the quartz capillary tube balance kettle just overflows two end openings of the quartz capillary tube, observing a length image of hydrophobic organic matters in the quartz capillary tube by using a microscope, measuring the length of the hydrophobic organic matters in the quartz capillary tube by using an online image acquisition and detection device and a computer, and calculating to obtain the initial volume of solute hydrophobic organic matters;
s3: and finally, placing the quartz capillary tube balance kettle filled with the quartz capillary tube in a cold and hot table of a temperature control device, heating the quartz capillary tube balance kettle, carrying out phase behavior observation on hydrophobic organic matters in the quartz capillary tube during the heating, recording the change condition of the residual quantity of the hydrophobic organic matters in the quartz capillary tube, recording the temperature T when the quartz capillary tube is just completely dissolved and the system reaches a uniform state, and calculating to obtain the solubility of the hydrophobic organic matters at the temperature.
2. The method for highly accurately measuring the solubility of a hydrophobic organic substance in subcritical water according to claim 1, wherein in step S2, the method for manufacturing the quartz capillary tube having the hydrophobic organic substance sucked therein comprises: intercepting a certain length of quartz capillary tube, burning off an organic coating on the outer surface of the quartz capillary tube by oxyhydrogen flame to form a transparent visual tube body, then absorbing a certain amount of hydrophobic organic matters by the transparent visual quartz capillary tube, and absorbing a small amount of solvent water at two ends of the quartz capillary tube after absorbing the organic matters for plugging the organic matters in the quartz capillary tube.
3. The method for high-precision determination of the solubility of hydrophobic organic substances in subcritical water according to claim 1, wherein the quartz capillary equilibrium still has an inner diameter of 0.250-0.350 mm and an outer diameter of 0.375-0.665 mm; the inner diameter of the quartz capillary tube is 0.020-0.080 mm, and the outer diameter of the quartz capillary tube is 0.100-0.200 mm; the length of the quartz capillary is less than that of the quartz capillary balance kettle.
4. The method according to claim 1, wherein in step S3, the temperature range for temperature rise measurement of the quartz capillary equilibrium still is 100-374 ℃, and the pressure in the quartz capillary equilibrium still is the saturated vapor pressure of the hydrophobic organic-water system.
5. The method according to claim 1, wherein in step S3, the total time measured for reaching the dissolution equilibrium is 0.5-2 days.
6. The apparatus for measuring the solubility of hydrophobic organic substances in subcritical water with high accuracy according to claim 1, comprising a quartz capillary equilibrium still (1), a temperature controller (3), a circulating water system (4), a cold and hot stage (5), a video camera (6), a microscope (7) and a computer (8); wherein a quartz capillary tube (2) with the outer diameter smaller than the inner diameter of the quartz capillary tube is loaded in the quartz capillary tube balance kettle (1); absorb in quartz capillary (2) and have hydrophobic organic matter and both ends opening, the injection has solvent water and both ends all to seal in quartz capillary balance kettle (1), temperature control appearance, circulating water system and cold and hot platform are used for carrying out the temperature regulation and control to quartz capillary balance kettle (1), the microscope is used for observing the water in quartz capillary balance kettle (1) and the image of hydrophobic organic matter in quartz capillary (2), camera and computer are by circuit connection, and the camera is used for gathering the water and the hydrophobic organic matter image that the microscope was surveyed to transmit image data in the computer.
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