CN113075015A - Secondary distillation system and method of use - Google Patents
Secondary distillation system and method of use Download PDFInfo
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- CN113075015A CN113075015A CN202110174840.XA CN202110174840A CN113075015A CN 113075015 A CN113075015 A CN 113075015A CN 202110174840 A CN202110174840 A CN 202110174840A CN 113075015 A CN113075015 A CN 113075015A
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- electrolytic cell
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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
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
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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
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
- G01N2001/4033—Concentrating samples by thermal techniques; Phase changes sample concentrated on a cold spot, e.g. condensation or distillation
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- General Health & Medical Sciences (AREA)
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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention belongs to the technical field of distillation equipment, and particularly relates to a secondary distillation system and a using method thereof, wherein the secondary distillation system comprises a constant-temperature heating box, an electrolytic cell, a first stainless steel joint, a capillary exhaust pipe, a second stainless steel joint, a collecting bottle, a vacuum valve, a cold trap and a vacuum pump, wherein the electrolytic cell is arranged in the constant-temperature heating box, the outlet at the top end of the electrolytic cell is hermetically connected with the capillary exhaust pipe by virtue of the first stainless steel joint, and the outlet end of the capillary exhaust pipe is connected with the collecting bottle by virtue of the second stainless steel joint; the capillary exhaust pipe is also communicated with a branch pipe, a vacuum valve is arranged between the capillary exhaust pipe and the branch pipe, the branch pipe is communicated with the cold trap in a sealing way, and the vacuum pump is communicated with the cold trap in a sealing way; the in-situ vacuum low-temperature distillation can be simultaneously completed by 24 electrolytic cells, the cell water is completely transferred to the receiving bottle under the condition of not transferring the cell water, the obtained distilled water sample has low conductivity, and the scintillation liquid can be directly added to prepare a test sample.
Description
Technical Field
The invention belongs to the technical field of distillation equipment, and particularly relates to a secondary distillation system and a using method thereof.
Background
The operation of transferring the concentrated pond water for finishing the secondary distillation is not only complicated, but also easy to absorb the environmental moisture to cause pollution.
The residual loss in the pond water transfer process also causes the necessity of increasing the quality of the water sample after the electrolysis termination, which results in the concentration ratio mI/mFDecrease, and thus, the uncertainty and detection of the analysisThe improvement in out-limits causes adverse effects.
Disclosure of Invention
In response to the deficiencies of the prior art, the present invention provides a secondary distillation system that can completely transfer pond water to a receiving bottle within 1 hour without transferring the pond water.
In order to solve the problems, the invention adopts the following technical scheme: the secondary distillation system has the key points that: the device comprises a constant-temperature heating box, an electrolytic cell, a first stainless steel joint, a capillary exhaust pipe, a second stainless steel joint, a collecting bottle, a vacuum valve, a cold trap and a vacuum pump, wherein the electrolytic cell is arranged in the constant-temperature heating box, the outlet at the top end of the electrolytic cell is hermetically connected with the capillary exhaust pipe through the first stainless steel joint, and the outlet end of the capillary exhaust pipe is connected with the collecting bottle through the second stainless steel joint;
the capillary exhaust pipe is also communicated with a branch pipe, a vacuum valve is arranged between the capillary exhaust pipe and the branch pipe, the branch pipe is communicated with the cold trap in a sealing manner, an air suction pipe of the vacuum pump extends into the bottom end inside the cold trap, and the vacuum pump is communicated with the cold trap in a sealing manner.
Preferably, 1-24 electrolytic cells are arranged in the constant-temperature heating box, each electrolytic cell is hermetically connected with a capillary exhaust pipe by virtue of a first stainless steel joint, and the capillary exhaust pipes connected with each electrolytic cell are communicated with each other.
Preferably, the outer surface of the capillary exhaust pipe is wound with a heating belt.
Preferably, the branch pipe is provided with a vacuum gauge, and the temperature measuring end of the vacuum gauge extends into the branch pipe.
The use method of the secondary distillation system comprises the following steps:
A. inserting the electrolytic cell into a constant-temperature heating box, and connecting the electrolytic cell to an inlet of a capillary exhaust pipe through a first stainless steel joint;
B. a glass collection bottle is arranged on the outlet of the capillary exhaust pipe, and a liquid nitrogen cup is sleeved on the cold trap; the modem adjusts the temperature of the heating zone to about-deg.C;
C. starting a vacuum pump, opening a vacuum valve, starting vacuumizing, and pumping air in a vacuum system, an electrolytic cell and a glass collecting bottle;
D. when the vacuum degree is less than Pa, the collection bottle is sleeved with a liquid nitrogen cup;
E. continuously vacuumizing until the vacuum degree is less than Pa, and closing a unit vacuum valve formed by the electrolytic cell and the sample collecting bottle to keep a unit formed by the electrolytic cell and the sample collecting bottle in a vacuum state;
F. closing a vacuum valve of the vacuum system to keep the vacuum system in a vacuum state;
G. closing the vacuum pump; presetting a temperature control temperature of-DEG C on a digital temperature controller of an electric heating system of a constant temperature heating box; presetting distillation time-minute on a time timer;
H. starting an electric heating system of the constant-temperature heating box;
I. when the working time preset by the time timer is up, the electric heating system of the constant-temperature heating box automatically closes the main power switch;
J. taking down the liquid nitrogen cup sleeved on the collecting bottle, and taking down the collecting bottle after a water sample distilled from the electrolytic cell in the collecting bottle is melted to prepare a measuring sample;
K. the cell was separated from the first stainless steel joint and the cell was removed from the heated incubator.
The invention has the beneficial effects that: the secondary distillation system can realize that 24 electrolytic cells can complete in-situ vacuum low-temperature distillation at the same time, the cell water can be completely transferred into a receiving bottle within 1 hour without transferring the cell water, the distillation temperature is less than 100 ℃, the vacuum degree is less than 30Pa, the obtained distilled water sample has low conductivity, and scintillation liquid can be directly added to prepare a test sample.
Drawings
FIG. 1 is a schematic structural view of the present invention;
1. constant temperature heating cabinet, 2, electrolytic cell, 3, first stainless steel connects, 4, capillary blast pipe, 41, branch pipe, 5, second stainless steel connects, 6, receiving flask, 7, vacuum valve, 8 cold traps, 9, vacuum pump, 10, heating tape, 11, vacuum gauge pipe.
Detailed Description
The following detailed description is further described in conjunction with the accompanying drawings and the detailed description.
In order to solve the problems, the invention adopts the following technical scheme: the secondary distillation system comprises a constant-temperature heating box 1, an electrolytic cell 2, a first stainless steel joint 3, a capillary exhaust pipe 4, a second stainless steel joint 5, a collecting bottle 6, a vacuum valve 7, a cold trap 8 and a vacuum pump 9, wherein the electrolytic cell 2 is arranged in the constant-temperature heating box 1, the outlet at the top end of the electrolytic cell 2 is hermetically connected with the capillary exhaust pipe 4 through the first stainless steel joint 3, and the outlet end of the capillary exhaust pipe 4 is connected with the collecting bottle 6 through the second stainless steel joint 5;
the capillary exhaust pipe 4 is further communicated with a branch pipe 41, a vacuum valve 7 is arranged between the capillary exhaust pipe 4 and the branch pipe 41, the branch pipe 41 is communicated with the cold trap 8 in a sealing mode, an air suction pipe of the vacuum pump 9 extends into the bottom end of the interior of the cold trap 8, and the vacuum pump 9 is communicated with the cold trap 8 in a sealing mode.
A. Inserting an electrolytic cell 2 into a constant temperature heating box 1, and connecting the electrolytic cell 2 to an inlet of a capillary exhaust pipe 4 through a first stainless steel joint 3;
B. a glass collection bottle 6 is arranged on the outlet of the capillary exhaust pipe 4, and a liquid nitrogen cup is sleeved on the cold trap 8; the modem adjusts the temperature of the heating belt 10 to about 60-80 deg.c;
C. starting a vacuum pump 9, opening a vacuum valve 7, starting vacuumizing, and pumping air in a vacuum system, an electrolytic cell and a glass collecting bottle;
D. when the vacuum degree is less than 300Pa, the collection bottle 6 is sleeved with a liquid nitrogen cup;
E. continuously vacuumizing until the vacuum degree is less than 30Pa, and closing a vacuum valve 7 of the unit consisting of the electrolytic cell and the sample collecting bottle to keep the unit consisting of the electrolytic cell 2 and the collecting bottle 6 in a vacuum state;
F. closing a vacuum valve 7 of the vacuum system to keep the vacuum system in a vacuum state;
G. the vacuum pump 9 is turned off; presetting a temperature control temperature of 80-100 ℃ on a digital temperature controller of an electric heating system of a constant temperature heating box 1; presetting distillation time on a time timer for 50-60 minutes;
H. starting an electric heating system of the constant temperature heating box 1;
I. when the working time preset by the time timer is up, the electric heating system of the constant temperature heating box 1 automatically closes the main power switch;
J. taking down the liquid nitrogen cup sleeved on the collecting bottle 6, and taking down the collecting bottle 6 after the water sample distilled from the electrolytic cell 2 in the collecting bottle 6 is melted to prepare a measuring sample;
K. the electrolytic cell 2 is separated from the first stainless steel joint 3, and the electrolytic cell 2 is taken out of the heating thermostat.
As shown in figure 1, the arrangement can realize that 24 electrolytic cells can simultaneously complete in-situ vacuum low-temperature distillation, the water in the electrolytic cells can be completely transferred into a receiving bottle within 1 hour without transferring the water in the electrolytic cells, the conductivity of the obtained distilled water sample is very low, and a scintillation liquid can be directly added to prepare a test sample; the phenomenon of pollution caused by absorbing environmental moisture in the transfer process of the pool water is avoided, and the improvement of analysis uncertainty and detection limit is not adversely affected;
as shown in fig. 1, 1-24 electrolytic cells 2 are arranged in the constant temperature heating box 1, each electrolytic cell 2 is hermetically connected with a capillary exhaust pipe 4 by a first stainless steel joint 3, and the capillary exhaust pipes 4 connected with each electrolytic cell 2 are communicated with each other.
The electrolytic cell 2 can be simultaneously provided with 24 electrolytic cells, and the capillary exhaust pipes 4 are mutually communicated, so that the efficiency is high.
And a heating belt 10 is wound on the outer surface of the capillary exhaust pipe 4.
As shown in figure 1, the heating belt 10 is wound on the outer surface of the capillary exhaust pipe 4, so that the high temperature in the capillary exhaust pipe 4 can be kept, moisture cannot be condensed on the glass pipe, and a water sample can be rapidly transferred into the collecting bottle.
As shown in FIG. 1, the branch pipe 41 is provided with a vacuum gauge 11, and the temperature measuring end of the vacuum gauge 11 extends into the branch pipe 41.
The vacuum gauge 11 can detect the vacuum degree, so that the worker can accurately control the vacuum degree in the device.
Claims (5)
1. The secondary distillation system is characterized in that: the device comprises a constant-temperature heating box (1), an electrolytic cell (2), a first stainless steel joint (3), a capillary exhaust pipe (4), a second stainless steel joint (5), a collecting bottle (6), a vacuum valve (7), a cold trap (8) and a vacuum pump (9), wherein the electrolytic cell (2) is arranged in the constant-temperature heating box (1), the outlet at the top end of the electrolytic cell (2) is hermetically connected with the capillary exhaust pipe (4) by virtue of the first stainless steel joint (3), and the outlet end of the capillary exhaust pipe (4) is connected with the collecting bottle (6) by virtue of the second stainless steel joint (5);
capillary blast pipe (4) still communicate with branch pipe (41), capillary blast pipe (4) and branch pipe (41) between be provided with vacuum valve (7), branch pipe (41) and cold-trap (8) sealed intercommunication, vacuum pump (9) the breathing pipe stretch into the inside bottom of cold-trap (8), vacuum pump (9) and cold-trap (8) sealed intercommunication.
2. The secondary distillation system of claim 1, wherein: the constant temperature heating box (1) in be provided with 1-24 electrolytic cell (2), every electrolytic cell (2) all have capillary blast pipe (4) with the help of first stainless steel joint (3) sealing connection, and capillary blast pipe (4) that every electrolytic cell (2) are connected all communicate each other.
3. The secondary distillation system of claim 2, wherein: and a heating belt (10) is wound on the outer surface of the capillary exhaust pipe (4).
4. The secondary distillation system as claimed in claim 2 or 3, wherein: the branch pipe (41) is provided with a vacuum gauge pipe (11), and the temperature measuring end of the vacuum gauge pipe (11) extends into the branch pipe (41).
5. The method of using a secondary distillation system as claimed in claim 1, comprising the steps of:
A. inserting an electrolytic cell (2) into a constant-temperature heating box (1), and connecting the electrolytic cell (2) to an inlet of a capillary exhaust pipe (4) through a first stainless steel joint (3);
B. a glass collection bottle (6) is arranged on the outlet of the capillary exhaust pipe (4), and a liquid nitrogen cup is sleeved on the cold trap (8); the modem adjusts the temperature of the heating belt (10) to about 60-80 ℃;
C. starting a vacuum pump (9), opening a vacuum valve (7), starting vacuumizing, and pumping air in a vacuum system, an electrolytic cell and a glass collecting bottle;
D. when the vacuum degree is less than 300Pa, the collection bottle (6) is sleeved on a liquid nitrogen cup;
E. continuously vacuumizing until the vacuum degree is less than 30Pa, closing a vacuum valve (7) of the unit consisting of the electrolytic cell and the sample collecting bottle, and keeping the unit consisting of the electrolytic cell (2) and the sample collecting bottle (6) in a vacuum state;
F. closing a vacuum valve (7) of the vacuum system to keep the vacuum system in a vacuum state;
G. turning off the vacuum pump (9); presetting a temperature control temperature of 80-100 ℃ on a digital temperature controller of an electric heating system of a constant temperature heating box (1); presetting distillation time on a time timer for 50-60 minutes;
H. starting an electric heating system of the constant-temperature heating box (1);
I. when the working time preset by the time timer is up, the electric heating system of the constant-temperature heating box (1) automatically closes the main power switch;
J. taking down the liquid nitrogen cup sleeved on the collecting bottle (6), and taking down the collecting bottle (6) after the water sample distilled from the electrolytic cell (2) in the collecting bottle (6) is melted to prepare a measuring sample;
K. the electrolytic cell (2) is separated from the first stainless steel joint (3) and the electrolytic cell (2) is taken out of the heating thermostat.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110174840.XA CN113075015A (en) | 2021-02-07 | 2021-02-07 | Secondary distillation system and method of use |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110174840.XA CN113075015A (en) | 2021-02-07 | 2021-02-07 | Secondary distillation system and method of use |
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| CN113075015A true CN113075015A (en) | 2021-07-06 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202110174840.XA Pending CN113075015A (en) | 2021-02-07 | 2021-02-07 | Secondary distillation system and method of use |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4600559A (en) * | 1982-03-26 | 1986-07-15 | The United States Of America As Represented By The Administrator Environmental Protection Agency | Vacuum extractor with cryogenic concentration and capillary interface |
| US20040069014A1 (en) * | 2002-10-15 | 2004-04-15 | Cheng-Ming Chou | Multi-stage vacuum distilling, cooling and freezing processes and apparatuses for solution separation and seawater desalination |
| CN101231249A (en) * | 2008-02-26 | 2008-07-30 | 东北大学 | Vacuum low temperature microscopic visualizer |
| CN202853951U (en) * | 2012-08-31 | 2013-04-03 | 中国科学院地理科学与资源研究所 | Low-temperature vacuum distillation device |
| US20130192277A1 (en) * | 2012-01-31 | 2013-08-01 | Sumitomo Heavy Industries, Ltd. | Cold trap and method of controlling cold trap |
| CN113075014A (en) * | 2021-02-07 | 2021-07-06 | 中国地质科学院水文地质环境地质研究所 | Tritium analysis sample preparation system |
| US20220010800A1 (en) * | 2019-05-08 | 2022-01-13 | University Of Science And Technology Of China | Enrichment and purification device for single gas in mixed gas |
-
2021
- 2021-02-07 CN CN202110174840.XA patent/CN113075015A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4600559A (en) * | 1982-03-26 | 1986-07-15 | The United States Of America As Represented By The Administrator Environmental Protection Agency | Vacuum extractor with cryogenic concentration and capillary interface |
| US20040069014A1 (en) * | 2002-10-15 | 2004-04-15 | Cheng-Ming Chou | Multi-stage vacuum distilling, cooling and freezing processes and apparatuses for solution separation and seawater desalination |
| CN101231249A (en) * | 2008-02-26 | 2008-07-30 | 东北大学 | Vacuum low temperature microscopic visualizer |
| US20130192277A1 (en) * | 2012-01-31 | 2013-08-01 | Sumitomo Heavy Industries, Ltd. | Cold trap and method of controlling cold trap |
| CN202853951U (en) * | 2012-08-31 | 2013-04-03 | 中国科学院地理科学与资源研究所 | Low-temperature vacuum distillation device |
| US20220010800A1 (en) * | 2019-05-08 | 2022-01-13 | University Of Science And Technology Of China | Enrichment and purification device for single gas in mixed gas |
| CN113075014A (en) * | 2021-02-07 | 2021-07-06 | 中国地质科学院水文地质环境地质研究所 | Tritium analysis sample preparation system |
Non-Patent Citations (1)
| Title |
|---|
| 孔繁信等: "用电解浓集法测定水中氚", 《辐射防护》 * |
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Application publication date: 20210706 |
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