CN218824131U - Phosphoric acid in-situ treatment and reaction integrated system for carbonate rock isotope analysis - Google Patents
Phosphoric acid in-situ treatment and reaction integrated system for carbonate rock isotope analysis Download PDFInfo
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Abstract
The utility model relates to a device for carbonate isotope analysis, concretely relates to phosphoric acid normal position is handled and reaction integration system for carbonate rock isotope analysis. The device comprises a first liquid storage device, a second liquid storage device, a third liquid storage device, a waste liquid collecting device, a gas storage device, a plurality of valves, a pipeline heating device, a vacuum gauge, a vacuum pump and an acid-proof pump; the acid-proof pump is respectively connected with the liquid storage device I, the liquid storage device II, the gas storage device, the liquid storage device III, the vacuum gauge and the waste liquid collecting device, and pipeline heating devices are arranged on connecting pipelines; the acid-proof pump is connected with the vacuum gauge, and the vacuum gauge is connected with the vacuum pump. The system can remove the water vapor in the detection process, prevent the crystallization of phosphoric acid and realize the constant-temperature and constant-speed transfer of phosphoric acid.
Description
Technical Field
The utility model relates to a device for carbonate rock isotope analysis, concretely relates to phosphoric acid normal position is handled and reaction integration system for carbonate rock isotope analysis.
Background
Carbonate rock carbon-oxygen isotopes have been widely used in lake-phase sediment ancient environment reconstruction studies. In recent years, carbonate carbon isotopes have been produced in ancient lakes, lake-entering water isotope composition and atmospheric CO 2 All made significant progress in the study of the equilibrium process of (a). With the continuous and deep research, the analysis of carbon and oxygen isotopes in carbonate rocks is continuously paid attention, and the research is gradually changed from an early off-line analysis test system to an on-line analysis test system. Particularly, with the intensive research on the lake and ocean environments, the carbon-oxygen isotope analysis of trace carbonate samples is urgently needed.
The carbonate rock isotope analysis is mainly based on the reaction of phosphoric acid and carbonate to generate carbon dioxide gas, and a carbon dioxide signal is detected by a stable mass spectrometer, so that the result of the carbon-oxygen isotope of the carbonate is finally obtained. The article "development of a carbon and oxygen isotope rapid sample preparation device in carbonate" (world nuclear geology science, volume 28, second phase, pages 112-114) system is to detect carbon and oxygen isotopes in carbonate by using the principle. However, when phosphoric acid contains moisture, oxygen atoms in water and oxygen atoms in carbon dioxide undergo a substitution reaction, resulting in deviation of the value of the oxygen isotope. Therefore, it is often necessary to prepare the phosphoric acid solution as a saturated phosphoric acid solution. However, since the saturated phosphoric acid solution is very easy to adsorb moisture, how to ensure that the moisture in the saturated phosphoric acid is effectively removed is one of the key problems of whether the carbon-oxygen isotope of the carbonate can be accurately tested.
The applicant discloses a sample preparation system and a sample preparation method for carbon-oxygen isotopes of carbonate in a patent CN105277401B of the prior invention. The sample preparation system comprises an original sample reaction device, a finished product sample extraction device and a system vacuum degree control device, wherein the original sample reaction device is also connected with an automatic sample introduction device. The sample preparation system adopts the automatic sample injector, so that the automation degree of the sample preparation system is improved, and simultaneously, the saturated phosphoric acid solution is ensured to completely enter the bottom of the reaction tube to participate in the reaction; the touch vacuum valve is adopted to replace the original knob vacuum valve, so that the service life is prolonged, the simplicity of the use of an instrument is improved, and the operation time of the preparation process is shortened; the constant temperature water bath is added, so that the vacuumizing and reaction processes can be simultaneously completed in the instrument, and the transfer step between the vacuumizing and the sample reaction is reduced.
However, the system is an off-line analysis system, and needs to undergo a pretreatment of phosphoric acid dehydration, a phosphoric acid reaction process, a generated carbon dioxide transfer process and the like, so that the whole time consumption is extremely long, carbon dioxide gas leakage is easily caused in a sample transfer analysis process, the reaction precision is influenced, and meanwhile, in the whole phosphoric acid transfer process, due to the lack of a heating and heat preservation step, water vapor in a pipeline is not completely removed, and the system is combined with a saturated phosphoric acid solution to generate crystallization at a low temperature. Whether the problem of pipeline crystallization in a phosphoric acid transfer system can be effectively solved is one of the key problems of accurate test of carbon-oxygen isotopes of carbonate.
Disclosure of Invention
In order to solve the problem that the pipeline is blocked by easy crystallization in the saturated concentrated phosphoric acid transfer among the carbonate carbon oxygen isotope analysis system, the utility model provides a carbonate rock isotope is phosphoric acid normal position for analysis handles and reaction integration system. The system can avoid many times the transfer process, finally realizes effectively getting rid of the steam that appears in the testing process, prevents that phosphoric acid crystallization from blockking up the pipeline, realizes phosphoric acid constant temperature constant speed and shifts.
In order to achieve the above purpose, the utility model adopts the following technical scheme:
the utility model provides a system integrating in-situ treatment and reaction of phosphoric acid for carbonate isotope analysis, which comprises a first liquid storage device, a second liquid storage device, a third liquid storage device, a waste liquid collecting device, a gas storage device, a plurality of valves, a pipeline heating device, a vacuum gauge, a vacuum pump and an acid-proof pump; the acid-proof pump is respectively connected with the first liquid storage device, the second liquid storage device, the gas storage device, the third liquid storage device, the vacuum gauge and the waste liquid collecting device, and pipeline heating devices are arranged on connecting pipelines; the acid-proof pump is connected with the vacuum gauge, and the vacuum gauge is connected with the vacuum pump. Placing saturated phosphoric acid solution in the first liquid storage device, placing distilled water in the second liquid storage device, and placing carbonate sample solution in the third liquid storage device; the gas storage device stores inert gas.
Further, the first liquid storage device is also connected with the second liquid storage device and the gas storage device respectively; the liquid storage device III is also respectively connected with the vacuum gauge and the waste liquid collecting device; the acid-proof pump is connected with the vacuum gauge, and the vacuum gauge is connected with the vacuum pump.
Furthermore, a first valve is arranged on a pipeline of the first liquid storage device connected with the acid-resistant pump, a second valve and a third valve are arranged on a pipeline of the second liquid storage device connected with the acid-resistant pump, and a fourth valve is arranged on a pipeline of the gas storage device connected with the acid-resistant pump.
Furthermore, a fifth valve is arranged on a pipeline connecting the third liquid storage device and the acid-proof pump, a sixth valve is arranged on a pipeline connecting the waste liquid collecting device and the acid-proof pump, and a seventh valve is arranged on a pipeline connecting the vacuum gauge and the acid-proof pump.
Furthermore, the second valve is positioned on a main pipeline of a connecting pipeline of the acid-proof pump and the second liquid storage device and the second gas storage device, and controls the communication of the acid-proof pump and the second liquid storage device and the communication of the second gas storage device.
Further, the pipeline heating device is a spiral heating pipe.
Further, the pipeline is made of quartz.
The use method of the phosphoric acid in-situ treatment and reaction integrated system for carbonate rock isotope analysis comprises the following steps:
1) Water vapor removal:
opening the pipeline heating device and the gas storage device, and removing water in the pipeline through the heating pipeline; or when the pipeline is heated, the gas storage device is opened, inert gas is rapidly filled into the pipeline, and moisture in the pipeline is removed;
2) And (3) vacuum detection:
closing the valve, and carrying out air tightness detection on the whole pipeline; starting the vacuum pump, waiting for the gauge to show schematically 10 -1 When pa, the vacuum system is closed;
3) Reaction of phosphoric acid with carbonate samples
Opening the acid-proof pump, adjusting and controlling the pipeline heating device to reduce the temperature of the pipeline, closing a first valve between the acid-proof pump and the first liquid storage device and a fifth valve between the acid-proof pump and the third liquid storage device to react the saturated phosphoric acid solution with the carbonate sample to generate CO 2 CO produced 2 The carbon-oxygen isotope can enter an isotope mass spectrometer for carbon-oxygen isotope analysis and detection;
4) System cleaning:
after the reaction is finished, opening the second liquid storage device and the pipeline heating device, cleaning the pipeline by using distilled water, and heating the pipeline to prevent the phenomenon of phosphoric acid crystallization caused by contact between the distilled water and a saturated phosphoric acid solution in the cleaning process, so as to effectively remove the residual phosphoric acid solution in the pipeline;
5) Water vapor removal:
the third valve is turned off and the third valve is opened,closing the fourth valve, injecting inert gas into the pipeline, and discharging distilled water; the sixth valve is disconnected, the 7 th valve is closed, the pipeline is heated until the vacuum degree is less than or equal to 10 -1 Pa, finishing the operation.
Compared with the prior art, the utility model has the advantages of it is following:
the phosphoric acid in-situ treatment and reaction integrated system for carbonate isotope analysis can effectively remove water in the pipeline and prevent oxygen in water and oxygen atoms in carbon dioxide gas from being replaced in the reaction process; after the reaction is finished, no residual water vapor exists in the system, so that the crystallization of the phosphoric acid pipeline can be effectively prevented; the constant-temperature constant-speed flow of the saturated concentrated phosphoric acid is realized, and the carbon fractionation effect of carbon dioxide in the reaction process of the saturated phosphoric acid is prevented. The system has realized reaction pretreatment, and phosphoric acid constant temperature constant speed shifts, and phosphoric acid and carbonate reaction and remaining phosphoric acid normal position wash the integration technique, have both guaranteed the accuracy of analysis test result, have also improved analysis efficiency of software testing greatly.
Drawings
Fig. 1 is a schematic structural diagram of a system integrating in-situ treatment and reaction of phosphoric acid for carbonate rock isotope analysis according to embodiment 1 of the present invention.
1. A first liquid storage device; 2. a first valve; 3. a second liquid storage device; 4. a second valve; 5. a third valve; 6. a fourth valve; 7. a gas storage device; 8. an acid-resistant pump; 9. a pipeline; 10. a spiral heating pipe; 11. a third liquid storage device; 12. a fifth valve; 13. a waste liquid collection device; 14. a sixth valve; 15. a seventh valve; 16. a vacuum gauge; 17. a vacuum pump.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the invention. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments in accordance with the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise, and it should also be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of the features, steps, operations and/or combinations thereof.
In order to make the technical solutions of the present invention more clearly understood by those skilled in the art, the technical solutions of the present invention will be described in detail below with reference to specific embodiments.
Example 1
As shown in fig. 1, the integrated system for in-situ treatment and reaction of phosphoric acid for carbonate isotope analysis comprises a first liquid storage device 1, a second liquid storage device 3, a third liquid storage device 11, a waste liquid collecting device 13, a gas storage device 7, a plurality of valves, a spiral heating pipe 10, a vacuum gauge 16, a vacuum pump 17 and an acid-proof pump 8; the acid-proof pump 8 is respectively connected with the liquid storage device I1, the liquid storage device II 3, the gas storage device 7, the liquid storage device III 11 and the waste liquid collecting device 13, and spiral heating pipes 10 are arranged on connecting pipelines; the acid-proof pump 8 is connected to a vacuum gauge 16, and the vacuum gauge 16 is connected to a vacuum pump 17. A saturated phosphoric acid solution is placed in the first liquid storage device 1, distilled water is placed in the second liquid storage device 3, and a carbonate sample solution is placed in the third liquid storage device 11; the gas storage device 7 stores inert gas.
The liquid storage device I1 is also connected with the liquid storage device II 3 and the gas storage device 7 respectively; the third liquid storage device 11 is also connected with a vacuum gauge 16 and a waste liquid collecting device 13 respectively.
A first valve 2 is arranged on a pipeline connecting the first liquid storage device 1 and the acid-proof pump 9, a second valve 4 and a third valve 5 are arranged on a pipeline connecting the second liquid storage device 3 and the acid-proof pump 8, and a fourth valve 6 is arranged on a pipeline connecting the gas storage device 7 and the acid-proof pump 8.
A fifth valve 12 is arranged on a pipeline connecting the third liquid storage device 11 with the acid-proof pump 8, a sixth valve 14 is arranged on a pipeline connecting the waste liquid collecting device 13 with the acid-proof pump 8, and a seventh valve 15 is arranged on a pipeline connecting the vacuum gauge 16 with the acid-proof pump 8. The second valve 4 is positioned on a main pipeline of a connecting pipeline of the acid-proof pump 8, the second liquid storage device 3 and the second gas storage device 7, and controls the communication of the acid-proof pump 8, the second liquid storage device 3 and the second gas storage device 7.
Example 2
The use method of the integrated system for in-situ treatment and reaction of phosphoric acid for carbonate isotope analysis, which is described in example 1, comprises the following steps:
(1) Closing the second valve 4, the fourth valve 6, the fifth valve 12 and the seventh valve 15, starting the vacuum pump 17, starting the spiral heating pipe 10, heating to 70 ℃, vacuumizing the system, and removing water vapor in instruments and saturated concentrated phosphoric acid;
(2) The vacuum degree of the system is observed through the vacuum gauge 16, and when the vacuum gauge 16 displays that the vacuum degree reaches 10 -1 Keeping for 10min when Pa;
(3) Adjusting the spiral heating pipe to the low temperature of 40 ℃, disconnecting the second valve 4, the fourth valve 6 and the seventh valve 15, closing the first valve 2, and adjusting the acid-resistant pump 8 to enable the flow of the saturated phosphoric acid solution to be 1mL/min;
(4) Saturated phosphoric acid is dropped into the carbonate sample in the third liquid storage device 11 to complete the reaction;
(5) Disconnecting the first valve 2 and the fifth valve 12, closing the second valve 4, the third valve 5 and the sixth valve 14, adjusting the flow rate of the acid pump to 10mL/min, adjusting the temperature of 50 ℃ by using the spiral heating pipe 10, enabling distilled water to flow through the pipeline, washing phosphoric acid remained in the pipeline completely, collecting and detecting the washed waste liquid in a waste liquid collecting device 13, and indicating that the phosphoric acid in the pipeline is washed completely when the collected waste water reacts with the carbonate solution and no bubbles are generated;
(6) The third valve 5 is disconnected, the fourth valve 6 is closed, and the inert gas helium is injected into the pipeline to discharge the distilled water until no water drops are discharged from the waste liquid collecting device 13;
(7) The sixth valve 14 is opened, the valve 15 is closed, the spiral heating pipe is adjusted to 70 ℃, the vacuum gauge is observed, and when the vacuum degree reaches 10 -1 And Pa, finishing the operation flow.
The utility model discloses well spare part that does not expand the discussion itself, each spare part connected mode in this application all belong to this technical field's well-known technique, no longer give unnecessary details. Such as welding, threaded connections, etc.
In the present application, the term "plurality" means two or more unless expressly defined otherwise. The terms "mounted," "connected," "fixed," and the like are to be construed broadly, and for example, "connected" may be a fixed connection, a removable connection, or an integral connection; "coupled" may be direct or indirect through an intermediary. The specific meaning of the above terms in the present invention can be understood according to specific situations by those skilled in the art.
In the description of the present invention, it should be understood that the terms "upper", "lower", "left", "right", "front", "back", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplification of description, but do not indicate or imply that the device or unit indicated must have a specific direction, be constructed and operated in a specific orientation, and therefore, should not be construed as limiting the present invention.
Claims (4)
1. The system is characterized by comprising a first liquid storage device, a second liquid storage device, a third liquid storage device, a waste liquid collecting device, a gas storage device, a plurality of valves, a pipeline heating device, a vacuum gauge, a vacuum pump and an acid-resistant pump;
the acid-proof pump is respectively connected with the first liquid storage device, the second liquid storage device, the gas storage device, the third liquid storage device, the vacuum gauge and the waste liquid collecting device, and pipeline heating devices are arranged on connecting pipelines; the vacuum gauge is connected with a vacuum pump;
the first liquid storage device is also connected with the second liquid storage device and the gas storage device respectively; the liquid storage device III is also respectively connected with the vacuum gauge and the waste liquid collecting device; the acid-resistant pump is connected with the vacuum gauge, and the vacuum gauge is connected with the vacuum pump;
a first valve is arranged on a pipeline of the first liquid storage device connected with the acid-resistant pump, a second valve and a third valve are arranged on a pipeline of the second liquid storage device connected with the acid-resistant pump, and a fourth valve is arranged on a pipeline of the gas storage device connected with the acid-resistant pump;
a fifth valve is arranged on a pipeline of the third liquid storage device connected with the acid-resistant pump, a sixth valve is arranged on a pipeline of the waste liquid collecting device connected with the acid-resistant pump, and a seventh valve is arranged on a pipeline of the vacuum gauge connected with the acid-resistant pump;
placing saturated phosphoric acid solution in the first liquid storage device, placing distilled water in the second liquid storage device, and placing carbonate sample solution in the third liquid storage device; the gas storage device stores inert gas.
2. The integrated system for in-situ treatment and reaction of phosphoric acid for isotope analysis of carbonate rock according to claim 1, wherein the second valve is located on a main pipeline of a connecting pipeline between the acid-proof pump and the second liquid storage device and between the acid-proof pump and the second gas storage device, and is used for controlling the communication between the acid-proof pump and the second liquid storage device and between the acid-proof pump and the gas storage device.
3. The integrated system for in-situ treatment and reaction of phosphoric acid for carbonate isotope analysis according to claim 1, wherein the pipeline heating device is a spiral heating pipe.
4. The system of claim 1, wherein the conduit is made of quartz.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202122713095.XU CN218824131U (en) | 2021-11-08 | 2021-11-08 | Phosphoric acid in-situ treatment and reaction integrated system for carbonate rock isotope analysis |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202122713095.XU CN218824131U (en) | 2021-11-08 | 2021-11-08 | Phosphoric acid in-situ treatment and reaction integrated system for carbonate rock isotope analysis |
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| CN202122713095.XU Active CN218824131U (en) | 2021-11-08 | 2021-11-08 | Phosphoric acid in-situ treatment and reaction integrated system for carbonate rock isotope analysis |
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