CN107422024A - The analysis system and method for not oxygen-containing mineral inclusion water oxygen isotopics - Google Patents

Abstract

The invention belongs to the field of determination of isotope composition of water in mineral inclusions, and specifically discloses an analysis system and method for oxygen isotope composition of water in oxygen-free mineral inclusions. The inclusion burst extraction/purification separation/extract conversion system of the system One end is connected to the product collection and measurement system, and the other end of the inclusion burst extraction/purification separation/extract conversion system is connected to the waste treatment system; the method includes: mineral sample injection; baking vacuum degassing; bursting of mineral inclusions , extraction and purification; transformation of water in mineral inclusions; collection and mass spectrometry of transformation products; waste treatment of reaction products. The invention solves the problems of incomplete extraction of water from mineral inclusions, incomplete separation of impurity components, easy oxygen isotope fractionation during the conversion process, etc., and improves the accuracy and efficiency of analysis and testing.

Description

System and method for analyzing oxygen isotopic composition of oxygen-free mineral inclusion water

technical field

The invention belongs to the field of determination of isotope composition of water in mineral inclusions, and in particular relates to an analysis system and method for oxygen isotope composition of oxygen-free mineral inclusion water.

Background technique

The determination of oxygen isotopic composition in mineral inclusion water plays a very important role in revealing the source, migration, evolution and mineralization process of ore-forming fluids, and provides a theoretical basis for elucidating the ore-forming mechanism of ore deposits. Fully extracting the water in mineral inclusions, purifying, converting and collecting them are the prerequisites for the analysis of oxygen isotope composition in oxygen-free mineral inclusion water.

In terms of water extraction from mineral inclusions, domestically, a single quartz glass tube or nickel tube is basically used for burst sampling or online direct burst extraction. These methods have their own disadvantages: 1) The extraction efficiency of a single quartz glass tube burst is low ; 2) The nickel tube bursting method is easy to pollute the nickel tube due to the complex composition of the minerals and is not easy to clean; 3) The online bursting method is to directly put the minerals into the elemental analyzer and send them to the isotope mass spectrometer after high temperature bursting and glassy carbon reduction This method is easy to cause pollution to the instrument and affects the sensitivity of the instrument and equipment. At the same time, it cannot effectively separate the water in the mineral from other oxygen-containing components. A small number of foreign laboratories use carrier gas to send the detonation products to the chromatograph for separation after online detonation. After separation, they are transferred to the elemental analyzer for reduction by high-temperature glassy carbon and then enter the isotope mass spectrometer for analysis. This method overcomes the mutual interference of detonation products. However, the composition of mineral inclusions is very complex, and it is difficult for actual operation. It is difficult to ensure that the water in mineral inclusions is completely transferred to the analytical instrument for analysis, which will cause isotope fractionation and affect the analysis and test results.

In terms of test objects, the traditional method is to convert the oxygen generated by the reaction with graphite into _CO2 under high temperature conditions for mass spectrometry. Because carbon has two isotopes of ¹² C and ¹³ C involved in the calculation, the measurement results need to be corrected, and the conversion process is likely to cause O isotope fractionation; the conversion system needs to introduce glass pipelines, and the glass piston needs to be regularly coated with vacuum grease to ensure the sealing performance of the piston And rotation flexibility, the system is exposed to the atmosphere during the process of applying vacuum grease, oxygen and water vapor in the air enter the system to cause pollution, and the vacuum sealing grease is easy to cause cross-contamination due to oxygen.

In terms of purifying the water in the extracted mineral inclusions, existing laboratories mostly use liquid nitrogen-alcohol or dry ice-acetone refrigerants to remove impurity gas components. Using liquid nitrogen-alcohol as a refrigerant, its temperature is extremely unstable and has a wide range of changes, and it is difficult to ensure the complete removal of impurity gas components; although the temperature of dry ice-acetone refrigerant is relatively stable, acetone is volatile and harmful to the human body, so it should be avoided Prolonged contact.

Contents of the invention

The purpose of the present invention is to provide an analysis system and method for oxygen isotope composition in oxygen-free mineral inclusion water, so as to solve the problems of incomplete water extraction, incomplete separation of impurity components, and oxygen isotope fractionation easily caused by the transformation process, etc. Improve the analysis test accuracy and analysis test efficiency.

The technical solution for realizing the purpose of the present invention: an analysis system for oxygen isotope composition in oxygen-free mineral inclusion water, the system includes inclusion burst extraction/purification separation/extract conversion system, product collection and measurement system, and waste treatment system ; One end of the inclusion burst extraction/purification separation/extract conversion system is connected to the product collection and measurement system, and the other end of the inclusion burst extraction/purification separation/extract conversion system is connected to the waste treatment system.

The inclusion burst extraction/purification separation/extract conversion system includes a vacuum pressure gauge, a first 1/2inch stainless steel main pipeline, a bromine pentafluoride storage tank, a second 1/2inch stainless steel main pipeline, a first set of bursting -extraction unit, the second set of burst-extraction unit, the third set of burst-extraction unit and the fourth set of burst-extraction unit, the first 1/2inch stainless steel main pipe, the bottom of the vacuum pressure gauge and the first 1/2inch stainless steel main pipe Connection, the first 1/2inch stainless steel main pipe is respectively connected to the outlet of the bromine pentafluoride storage tank and the second 1/2inch stainless steel main pipe; the second 1/2inch stainless steel main pipe is respectively connected to the first burst-extraction unit, the second The second group of burst-extraction units, the third group of burst-extraction units, and the fourth group of burst-extraction units are connected, and the first group of burst-extraction units, the second group of burst-extraction units, the third group of burst-extraction units, and the fourth group of burst-extraction units Four burst-extraction units are connected in parallel.

A fourth 1/4inch metal valve is provided between the bottom of the vacuum pressure gauge and the first 1/2inch stainless steel main pipeline.

The eighth 1/4inch metal valve, the ninth 1/4inch metal valve, the eighth 1/4inch metal valve and the ninth 1 There is a seventh 1/4inch metal valve between the /4inch metal valves.

A first 1/2inch metal valve is provided between the first 1/2inch stainless steel main pipeline and the second 1/2inch stainless steel main pipeline, and a second 1/2inch metal valve is provided on the second 1/2inch stainless steel main pipeline. The third 1/2inch metal valve, the fourth 1/2inch metal valve.

The first set of burst-extraction unit includes the tenth 1/4inch metal valve, the first quartz sample burst tube assembly, the eleventh 1/4inch metal valve and the first nickel reaction tube, and the top of the first quartz sample burst tube assembly Connect with one end of the tenth 1/4inch metal valve, the top of the first nickel reaction tube is connected with one end of the eleventh 1/4inch metal valve, the other end of the tenth 1/4inch metal valve, the eleventh 1/4inch metal valve The other end of each is connected with one end of the second 1/2inch metal valve on the second 1/2inch stainless steel main pipe; the second group of burst-extraction unit includes the twelfth 1/4inch metal valve, the second quartz sample burst tube assembly, The thirteenth 1/4inch metal valve and the second nickel reaction tube, the top of the second quartz sample burst tube assembly is connected to one end of the twelfth 1/4inch metal valve, the top of the second nickel reaction tube is connected to the thirteenth 1/4inch One end of the metal valve is connected, the other end of the twelfth 1/4inch metal valve and the thirteenth 1/4inch metal valve are connected with the other end of the second 1/2inch metal valve on the second 1/2inch stainless steel main pipe, the third One end of the 1/2inch metal valve is connected; the third group of burst-extraction unit includes the fourteenth 1/4inch metal valve, the third quartz sample burst tube assembly, the fifteenth 1/4inch metal valve and the third nickel reaction tube, the first The top of the three-quartz sample burst tube assembly is connected to one end of the fourteenth 1/4inch metal valve, the top of the third nickel reaction tube is connected to one end of the fifteenth 1/4inch metal valve, and the other end of the fourteenth 1/4inch metal valve , The other end of the fifteenth 1/4inch metal valve is connected to the other end of the third 1/2inch metal valve on the second 1/2inch stainless steel main pipe, and one end of the fourth 1/2inch metal valve; the fourth group burst- The extraction unit includes the sixteenth 1/4inch metal valve, the fourth quartz sample burst tube assembly, the seventeenth 1/4inch metal valve and the fourth nickel reaction tube, the top of the fourth quartz sample burst tube assembly and the sixteenth 1/4inch One end of the metal valve is connected, the top of the fourth nickel reaction tube is connected to one end of the seventeenth 1/4inch metal valve, the other end of the sixteenth 1/4inch metal valve, and the other end of the seventeenth 1/4inch metal valve are connected to Connect the other end of the fourth 1/2inch metal valve on the second 1/2inch stainless steel main pipe.

The conversion product collection and measurement system includes a second metal cold trap, a third metal cold trap, a first thermocouple vacuum gauge, a first Molecular sieve, the second Molecular sieve, second thermocouple vacuum gauge, ionization vacuum gauge, turbomolecular pump and isotope mass spectrometer, the first 1/2inch stainless steel main pipe is connected to the inlet of the second metal cold trap, and the outlet of the second metal cold trap is connected to the third metal cold trap The inlet is connected, and the outlet of the third metal cold trap is respectively connected with the first thermocouple vacuum gauge, the first Molecular sieve inlet, the second Molecular sieve inlet, ionization vacuum gauge, inlet connection of turbomolecular pump, first Molecular sieve outlet, the second The molecular sieve outlets are all connected to the second thermocouple vacuum gauge and isotope mass spectrometer.

The eighteenth 1/4inch metal valve is arranged between the first 1/2inch stainless steel main pipe and the second metal cold trap inlet, and the tenth metal valve is arranged between the second metal cold trap outlet and the third metal cold trap inlet. Nine 1/4inch metal valves, the third metal cold trap outlet and the first There is a 20th 1/4inch metal valve and a 22nd 1/4inch metal valve between the inlets of the molecular sieve, and the outlet of the third metal cold trap is connected to the second There are 20th 1/4inch metal valves and 24th 1/4inch metal valves between the molecular sieve inlets, the first There is a 23rd 1/4inch metal valve between the molecular sieve outlet and the second thermocouple vacuum gauge and isotope mass spectrometer. There is a twenty-fifth 1/4inch metal valve between the outlet of the molecular sieve, a twenty-first 1/4inch metal valve and a twenty-first 1/4inch metal valve between the outlet of the third metal cold trap and the ionization vacuum gauge and turbomolecular pump. Metal valve, the first thermocouple vacuum gauge is connected to the twentieth 1/4inch metal valve, the outlet of the third metal cold trap is connected to the first thermocouple vacuum gauge, the first Molecular sieve inlet, the second The inlet of the molecular sieve, the ionization vacuum gauge, and the intake end of the turbomolecular pump are connected, and a twenty-sixth 1/4inch metal valve is arranged between the ionization vacuum gauge, the turbomolecular pump, the second thermocouple vacuum gauge, and the isotope mass spectrometer.

The waste treatment system includes a rotary vane mechanical vacuum pump, the first metal cold trap, the fifth 1/4inch metal valve and the sixth 1/4inch metal valve, the first 1/2inch stainless steel main pipe is connected with the first metal cold trap respectively The inlet and the sixth 1/4inch metal valve are connected, the outlet of the first metal cold trap is connected to the suction port of the rotary vane mechanical vacuum pump, and the sixth 1/4inch metal valve is connected to the fifth 1/4inch metal valve.

A third 1/4inch metal valve is provided between the first 1/2inch stainless steel main pipe and the inlet of the first metal cold trap, and a second 1/4inch metal valve is provided between the outlet of the first metal cold trap and the rotary vane mechanical vacuum pump. 4inch metal valve, the outlet of the first metal cold trap, and the second 1/4inch metal valve are all connected to the first 1/4inch metal valve.

A quartz sample burst tube assembly for the analysis system, the quartz sample burst tube assembly includes an external threaded stainless steel tube, a quartz burst tube, a rubber sealing ring, a sealed metal sleeve and an internal threaded metal pipe ferrule, the quartz burst tube is open The mouth end is inserted into the bottom of the externally threaded stainless steel pipe, and there is a rubber sealing ring between the externally threaded stainless steel pipe and the quartz bursting pipe. The bottom of the rubber sealing ring is provided with a sealing metal sleeve, and the bottom of the sealing metal sleeve is inserted into the threaded metal pipe ferrule. The rubber sealing ring, sealing metal casing and threaded metal pipe hoop are all set on the outside of the quartz bursting tube.

A method for analyzing oxygen isotope composition in oxygen-free mineral inclusion water by using the analysis system, the method specifically includes the following steps:

Step 1, mineral sample injection;

Step 2. Baking and vacuum degassing the entire analysis system;

Step 3. After the vacuum degassing of the analysis system is completed, the mineral inclusions are burst and the burst products are extracted and purified;

Step 4. Transform the water in the mineral inclusions that have been exploded, extracted and purified in Step 3 above

Step 5, collecting and mass spectrometrically measuring the transformation product obtained in the above step 4 after water transformation of the mineral inclusions;

Step 6. Perform waste treatment on the residual reagents and reaction products in the above steps 3 and 4.

The step 1 specifically includes the following steps: closing the tenth 1/4inch metal valve, the eleventh 1/4inch metal valve, the twelfth 1/4inch metal valve, the thirteenth 1/4inch metal valve, the fourteenth 1 /4inch metal valve, fifteenth 1/4inch metal valve, sixteenth 1/4inch metal valve and seventeenth 1/4inch metal valve, remove the first quartz sample burst tube assembly, the second quartz sample burst tube assembly, The third quartz sample burst tube assembly, the fourth quartz sample burst tube assembly, the processed mineral sample particles are respectively loaded into the first quartz sample burst tube assembly, the second quartz sample burst tube assembly, the third quartz sample burst tube assembly, The fourth quartz sample burst tube assembly, and the first quartz sample burst tube assembly, the second quartz sample burst tube assembly, the third quartz sample burst tube assembly, and the fourth quartz sample burst tube assembly are respectively upwardly connected with the 1/4inch stainless steel pipeline The tenth 1/4inch metal valve, the twelfth 1/4inch metal valve, the fourteenth 1/4inch metal valve, and the sixteenth 1/4inch metal valve are connected to complete the mineral sample injection operation.

The step 2 specifically includes the following steps: the first quartz sample burst tube assembly, the first nickel reaction tube, the second quartz sample burst tube assembly, the second nickel reaction tube, the third quartz sample burst tube assembly, the third nickel The reaction tube, the fourth quartz sample burst tube assembly and the fourth nickel reaction tube are respectively fitted with a digital temperature-controlled heating furnace, and the tenth 1/4inch metal valve, the eleventh 1/4inch metal valve, the twelfth 1 /4inch metal valve, thirteenth 1/4inch metal valve, fourteenth 1/4inch metal valve, fifteenth 1/4inch metal valve, sixteenth 1/4inch metal valve, seventeenth 1/4inch metal valve, The second 1/2inch metal valve, the third 1/2inch metal valve, the fourth 1/2inch metal valve, the first 1/2inch metal valve, the eighth 1/4inch metal valve, the fourth 1/4inch metal valve, the third 1/4inch metal valve, put the liquid nitrogen cup on the outside of the first metal cold trap and slowly open the second 1/4inch metal valve to connect the rotary vane mechanical vacuum pump to draw a low vacuum for the analysis system, open the eighteenth 1/4inch The metal valve and the nineteenth 1/4inch metal valve adjust the temperature of the digital temperature-controlled heating furnace according to the properties of the mineral sample; turn on the power supply of the heating belt to heat and degas the entire analysis system for 30 minutes, then close the third 1/4inch metal valve; Put the liquid nitrogen cup on the second metal cold trap and the third metal cold trap, open the twenty-second 1/4inch metal valve, the twenty-second 1/4inch metal valve, the twenty-third 1/4inch metal valve, the twenty-fourth The 1/4inch metal valve, the twenty-fifth 1/4inch metal valve, the twenty-sixth 1/4inch metal valve and the twenty-first 1/4inch metal valve are connected to the turbomolecular pump to pump the analysis system to high vacuum, After the high vacuum degree of the analysis system reaches 10 ^-5 Pa, continue to pump for 30 min by monitoring the ionization vacuum gauge.

The specific steps for the bursting of mineral inclusions in step 3 are as follows: after the vacuum degassing of the analysis system is completed, the first quartz sample bursting tube assembly, the second quartz sample bursting tube assembly, the third quartz sample bursting tube assembly, the second quartz sample bursting tube assembly, Four quartz sample burst tube assemblies, and the first nickel reaction tube, the second nickel reaction tube, the third nickel reaction tube, and the fourth nickel reaction tube are covered with circulating water, close the tenth 1/4inch metal valve, the twelfth 1 /4inch metal valve, the fourteenth 1/4inch metal valve and the sixteenth 1/4inch metal valve, adjust the burst temperature of the digital temperature-controlled heating furnace according to the properties of the mineral sample, and the burst time is 30 minutes to complete the burst of mineral inclusions.

The specific steps for extracting mineral inclusion explosion products in step 3 are as follows: remove the first nickel reaction tube, the second nickel reaction tube, the third nickel reaction tube and the temperature-controlled heating outside the fourth nickel reaction tube after the explosion is completed. furnace, and put liquid nitrogen cups on the outside of the four nickel reaction tubes for full freezing, after closing the second 1/2inch metal valve, the third 1/2inch metal valve and the fourth 1/2inch metal valve in turn, open the tenth 1/4inch metal valve, 12th 1/4inch metal valve, 14th 1/4inch metal valve and 16th 1/4inch metal valve, mineral inclusion explosion products are automatically transferred and diffused to the corresponding first nickel reaction tube, the second nickel reaction tube, the third nickel reaction tube, and the fourth nickel reaction tube; after 20 minutes, close the tenth 1/4inch metal valve, the twelfth 1/4inch metal valve, the fourteenth 1/4inch metal valve and the first Sixteen 1/4inch metal valves complete extraction of popping products.

The specific steps for the purification of mineral inclusion detonation products in step 3 are as follows: After removing the first nickel reaction tube, the second nickel reaction tube, the third nickel reaction tube and the liquid nitrogen cup outside the fourth nickel reaction tube, The four nickel reaction tubes are covered with dry ice-alcohol mixed refrigerant to purify the burst extract for 20 minutes, and then open the second 1/2inch metal valve, the third 1/2inch metal valve and the fourth 1/2inch metal valve to pump out the burst For impurity components in the product, close the eleventh 1/4inch metal valve, the thirteenth 1/4inch metal valve, the fifteenth 1/4inch metal valve and the seventeenth 1/4inch metal valve to complete the purification of the explosion product.

The specific steps of step 4 are as follows: close the eighth 1/4inch metal valve, the eighteenth 1/4inch metal valve, open the ninth 1/4inch metal valve 14, slowly open the eighth 1/4inch metal valve, pentafluoro The BrF ₅ reagent in the bromine storage tank diffuses into the first 1/2inch stainless steel main pipe and the second 1/2inch stainless steel main pipe; monitor the diffusion into the first 1/2inch stainless steel main pipe and the second 1/2inch stainless steel main pipe through vacuum pressure gauge 6 /2inch the pressure value of the BrF ₅ reagent in the stainless steel main pipe, and transfer the BrF ₅ reagent needed for the reaction into the frozen first nickel reaction tube, the second nickel reaction tube, the third nickel reaction tube, and the fourth nickel reaction tube Remove the dry ice-alcohol refrigerant outside the first nickel reaction tube, the second nickel reaction tube, the third nickel reaction tube, and the fourth nickel reaction tube, and reapply the first nickel reaction tube, the second nickel reaction tube, the third nickel reaction tube The nickel reaction tube and the fourth nickel reaction tube are equipped with a digital temperature-controlled heating furnace. The temperature of the digital temperature-controlled heating furnace is adjusted to 300°C and heated for 20 minutes. The first nickel reaction tube, the second nickel reaction tube, and the third nickel reaction tube , The water in the fourth nickel reaction tube reacts with the BrF ₅ reagent to completely release O ₂ .

The specific steps for collecting the mineral inclusion transformation product in the step 5 are as follows: remove the temperature-controlled heating furnace outside the first nickel reaction tube, the second nickel reaction tube, the third nickel reaction tube, and the fourth nickel reaction tube, and re- Put a liquid nitrogen cup on the outside of the first nickel reaction tube, the second nickel reaction tube, the third nickel reaction tube and the fourth nickel reaction tube. Close the eighth 1/4inch metal valve, the fourth 1/4inch metal valve, the eighteenth 1/4inch metal valve, the nineteenth 1/4inch metal valve, the twentieth 1/4inch metal valve, the twenty-first 1/ 4inch metal valve, twenty-second 1/4inch metal valve, twenty-third 1/4inch metal valve, twenty-fourth 1/4inch metal valve, twenty-fifth 1/4inch metal valve and twenty-sixth 1/ 4inch metal valve, slowly open the eleventh 1/4inch metal valve on the first nickel reaction tube, so that the _O2 generated in the first nickel reaction tube is slowly released to the first 1/2inch stainless steel main pipe and the second 1/2 inch In the 2inch stainless steel main pipeline; slowly open the eighteenth 1/4inch metal valve, the nineteenth 1/4inch metal valve and the twentieth 1/4inch metal valve in sequence, and monitor the pressure of _O2 generated by the reaction through the first thermocouple vacuum gauge ; Open the twenty-second 1/4inch metal valve, and turn the first Molecular sieves are fully frozen with liquid nitrogen to collect _O2 in the first nickel reaction tube, close the twenty-second 1/4inch metal valve, and remove the first Liquid nitrogen over molecular sieves.

The specific steps of the mass spectrometry measurement of mineral inclusion transformation products in the step 5 are as follows: open the twenty-third 1/4inch metal valve, and monitor the first thermocouple vacuum gauge through the second thermocouple vacuum gauge. After the molecular sieve is thawed, the pressure of O ₂ is released, and O ₂ diffuses into the isotope mass spectrometer for isotope measurement. According to the above operation, open the twenty-fourth 1/4inch metal valve to collect the O ₂ in the second nickel reaction tube and fully freeze it with liquid nitrogen the second In the molecular sieve, remove the liquid nitrogen and open the twenty-fifth 1/4inch metal valve, monitor the pressure of _O2 released after the molecular sieve is thawed through the second thermocouple vacuum gauge, _O2 diffuses into the isotope mass spectrometer for isotope measurement, and follow the same operation method Complete the collection and measurement of _O2 in the remaining nickel reaction tubes.

The specific steps of the step 6 are as follows: close the eighteenth 1/4inch metal valve, the fourth 1/4inch metal valve, the first 1/4inch metal valve and the second 1/4inch metal valve, in the first metal cold trap Put liquid nitrogen on the jacket, remove the first quartz sample burst tube assembly, the second quartz sample burst tube assembly, the third quartz sample burst tube assembly, the fourth quartz sample burst tube assembly, and the first nickel reaction tube, the second nickel reaction tube tube, the third nickel reaction tube, and the cooling water system outside the fourth nickel reaction tube, re-cover the temperature-controlled heating tube outside the first nickel reaction tube, the second nickel reaction tube, the third nickel reaction tube, and the fourth nickel reaction tube furnace, the temperature-controlled heating furnace is adjusted to 150°C, and the four nickel reaction tubes (29, 31, 33, 35) are heated; after opening the third 1/4inch metal valve, open the eleventh 1/4inch metal valve, the first The thirteenth 1/4inch metal valve, the fifteenth 1/4inch metal valve and the seventeenth 1/4inch metal valve transfer the waste in the four nickel reaction tubes (29, 31, 33, 35) to the first metal cold In the well; close the first 1/2inch metal valve, open the fifth 1/4inch metal valve and the sixth 1/4inch metal valve, remove the liquid nitrogen outside the first metal cold trap, open the first 1/4inch metal valve, The waste is carried by Ar gas to the lime bucket in the fume hood connected to the pipeline on the left side of the first 1/4inch metal valve to complete the waste disposal.

The beneficial technical effect of the present invention is: the present invention adopts the design that a plurality of quartz glass tubes are respectively loaded with different samples to be analyzed, and each quartz glass tube is connected with a nickel reaction tube to form a set of bursting, extraction and purification units, each set of units Separated by a metal valve, it can independently complete the high-temperature explosion, product extraction and purification of minerals, which greatly improves the analysis efficiency; the design adopts the combination of "O" type rubber ring and stainless steel spiral clamp to clean the quartz glass with samples. The tube is sealed with the analysis system, which can not only effectively maintain the vacuum of the analysis system, but also facilitate the cleaning and replacement of the quartz sample tube, and at the same time avoid the interference of oxygen-containing components caused by the use of vacuum sealing grease; The molecular sieve directly collects the oxygen generated by the reaction under the sufficient freezing of liquid nitrogen for mass spectrometry measurement, avoiding the problem of correcting the measurement results due to the introduction of graphite in the traditional method, and overcoming the regular application of vacuum lubricating grease on the glass piston to expose the analysis system to the atmosphere At the same time, it avoids cross-contamination caused by the use of oxygen-containing vacuum sealing grease; the rotary vane mechanical pump is used as the front-stage turbomolecular pump as the high-vacuum pump unit of the analysis system to ensure that the entire analysis system achieves a high degree of vacuum and further reduces The influence of oxygen-containing gas in the air on the experimental process; the digital temperature-controlled heating furnace is used as the quartz glass tube and the external heating equipment of the nickel reactor, which can accurately control the burst temperature and reaction temperature; the experiment found that the dry ice-alcohol mixture has temperature stability, With the characteristics of strong controllability and no harm to the human body, as a purification refrigerant, it can completely freeze the water precipitated by the bursting of mineral inclusions, and at the same time, it can effectively separate and remove impurity components, and avoid the occurrence of oxygen isotopes caused by incomplete extraction of water in inclusions. Fractionation and interference with other oxygen-containing impurity gases.

Description of drawings

Fig. 1 is a schematic diagram of an analysis system for the composition of oxygen isotopes in water of oxygen-free mineral inclusions provided by the present invention;

Fig. 2 is a schematic structural view of a quartz sample burst tube assembly provided by the present invention;

In the figure: 1 is the first 1/4inch metal valve, 2 is the second 1/4inch metal valve, 3 is the rotary vane mechanical vacuum pump, 4 is the first metal cold trap, 5 is the third 1/4inch metal valve, 6 7 is the fourth 1/4inch metal valve, 8 is the first 1/2inch stainless steel main pipe, 9 is the fifth 1/4inch metal valve, 10 is the sixth 1/4inch metal valve, 11 is the seventh 1/4inch metal valve, 12 is the eighth 1/4inch metal valve, 13 is the first 1/2inch metal valve, 14 is the ninth 1/4inch metal valve, 15 is the bromine pentafluoride storage tank, 16 is the second 1/2inch metal valve, 17 is the third 1/2inch metal valve, 18 is the fourth 1/2inch metal valve, 19 is the second 1/2inch stainless steel main pipe, 20 is the tenth 1/4inch metal valve, 21 is the first Eleven 1/4inch metal valves, 22 for the twelfth 1/4inch metal valves, 23 for the thirteenth 1/4inch metal valves, 24 for the fourteenth 1/4inch metal valves, 25 for the fifteenth 1/4inch metal valves Valve, 26 is the sixteenth 1/4inch metal valve, 27 is the seventeenth 1/4inch metal valve, 28 is the first quartz sample burst tube assembly, 29 is the first nickel reaction tube, 30 is the second quartz sample burst tube Components, 31 is the second nickel reaction tube, 32 is the third quartz sample burst tube assembly, 33 is the third nickel reaction tube, 34 is the fourth quartz sample burst tube assembly, 35 is the fourth nickel reaction tube, 36 is the tenth Eight 1/4inch metal valves, 37 is the second metal cold trap, 38 is the nineteenth 1/4inch metal valve, 39 is the third metal cold trap, 40 is the twentieth 1/4inch metal valve, 41 is the first heat Even vacuum gauge, 42 is the twenty-first 1/4inch metal valve, 43 is the twenty-second 1/4inch metal valve, 44 is the first Molecular sieve, 45 is the twenty-third 1/4inch metal valve, 46 is the twenty-fourth 1/4inch metal valve, 47 is the second Molecular sieve, 48 is the twenty-fifth 1/4inch metal valve, 49 is the twenty-sixth 1/4inch metal valve, 50 is the second thermocouple vacuum gauge, 51 is the ionization vacuum gauge, 52 is the turbomolecular pump, 53 is the isotope Mass spectrometer, 54 is an external thread stainless steel tube, 55 is a quartz sample burst tube, 56 is a rubber sealing ring, 57 is a sealing metal sleeve, and 58 is an internal thread metal pipe collar.

detailed description

The present invention will be described in further detail below in conjunction with the accompanying drawings and embodiments.

As shown in Figure 1, an analysis system for oxygen isotope composition in oxygen-free mineral inclusion water, the system includes inclusion burst extraction/purification separation/extract conversion system, product collection and measurement system, and waste treatment system .

As shown in Figures 1 and 2, the inclusion burst extraction/purification separation/extract conversion system includes a vacuum pressure gauge 6, a fourth 1/4inch metal valve 7, a first 1/2inch stainless steel main pipe 8, a seventh 1/4inch Metal valve 11, the first 1/2inch metal valve 13, the ninth 1/4inch metal valve 14, bromine pentafluoride storage tank 15, the second 1/2inch metal valve 16, the third 1/2inch metal valve 17, the Four 1/2inch metal valves 18, the second 1/2inch stainless steel main pipe 19, the first burst-extraction unit, the second burst-extraction unit, the third burst-extraction unit and the fourth burst-extraction unit. The bottom of the vacuum pressure gauge 6 is welded to the first 1/2inch stainless steel main pipe 8 through a 1/4inch stainless steel pipe, and a fourth 1/4inch metal valve is arranged between the vacuum pressure gauge 6 and the first 1/2inch stainless steel main pipe 8 7. Control the opening and closing of the vacuum pressure gauge 6 through the fourth 1/4inch metal valve 7. The left side of the 1/2inch stainless steel vertical main pipe 8 is welded and connected with three pipelines parallel to the left side of the 1/2inch stainless steel vertical main pipe 8, and the horizontal pipeline is provided with the first 1/2inch stainless steel main pipe 8 on one side Eight 1/4inch metal valves 12, the seventh 1/4inch metal valve 11 is provided on the other side of the horizontal pipeline, the seventh 1/4inch metal valve 11 controls the connection of the external bromine pentafluoride steel cylinder with the entire analysis system, and the eighth 1/4inch metal valve 11 is connected to the entire analysis system. The 4inch metal valve 12 controls the bromine pentafluoride in the bromine pentafluoride storage tank 15 to enter the analysis system pipeline; the upper part of the ninth 1/4inch metal valve 14 is connected to the horizontal pipeline through a tee, and the lower part of the ninth 1/4inch metal valve 14 The ninth 1/4 inch metal valve 14 controls the opening and closing of the bromine pentafluoride storage tank 15 through a pipeline connected to the top outlet of the bromine pentafluoride storage tank 15 . The bottom of the first 1/2inch stainless steel main pipe 8 is welded to the middle of the second 1/2inch stainless steel main pipe 19, and the two are perpendicular to each other; the first 1/2inch stainless steel main pipe 8 is adjacent to the second 1/2inch stainless steel main pipe There is a first 1/2inch metal valve 13 at 19, a second 1/2inch metal valve 16, a third 1/2inch metal valve 17, and a fourth 1/2inch metal valve on the second 1/2inch stainless steel main pipe 19 18. The first group of burst-extraction unit includes the tenth 1/4inch metal valve 20, the first quartz sample burst tube assembly 28, the eleventh 1/4inch metal valve 21 and the first nickel reaction tube 29, the second group of burst-extraction unit Including the twelfth 1/4inch metal valve 22, the second quartz sample burst tube assembly 30, the thirteenth 1/4inch metal valve 23 and the second nickel reaction tube 31, the third group of burst-extraction unit includes the fourteenth 1/4inch 4inch metal valve 24, the third quartz sample burst tube assembly 32, the fifteenth 1/4inch metal valve 25 and the third nickel reaction tube 33, the fourth group of burst-extraction unit includes the sixteenth 1/4inch metal valve 26, the Four quartz sample burst tube assembly 34 , seventeenth 1/4 inch metal valve 27 and fourth nickel reaction tube 35 . The second 1/2inch metal valve 16 controls the first burst-extraction unit, the third 1/2inch metal valve 17 controls the second burst-extraction unit, and the fourth 1/2inch metal valve 18 controls the third and fourth groups Burst-extraction unit, tenth 1/4inch metal valve 20, eleventh 1/4inch metal valve 21, twelfth 1/4inch metal valve 22, thirteenth 1/4inch metal valve 23, fourteenth 1/4inch The metal valve 24, the fifteenth 1/4inch metal valve 25, the sixteenth 1/4inch metal valve 26 and the seventeenth 1/4inch metal valve 27 respectively pass through the 1/4inch stainless steel pipeline and the second 1/2inch stainless steel main Pipeline 19 is connected by welding. The first quartz sample burst tube 28, the second quartz sample burst tube 30, the third quartz sample burst tube 32 and the fourth quartz sample burst tube 34 adopt "O" type rubber ring seal (see Figure 2), and the first quartz sample bursts The top outlet of the tube assembly 28 is connected upwards with the tenth 1/4inch metal valve 20 through a 1/4inch stainless steel pipeline with a metal ferrule, and the top outlet of the second quartz sample burst tube assembly 30 is connected upwards with the twelfth 1/4inch stainless steel pipeline through a 1/4inch stainless steel pipeline. The 4inch metal valve 22 is connected with a metal ferrule, the top outlet of the third quartz sample burst tube assembly 32 is connected upwardly with the fourteenth 1/4inch metal valve 24 through a 1/4inch stainless steel pipeline, and the fourth quartz sample burst tube assembly The top outlet of 34 is connected upwardly with the sixteenth 1/4inch metal valve 26 through a metal ferrule through a 1/4inch stainless steel pipeline. The first nickel reaction tube 29, the second nickel reaction tube 31, the third nickel reaction tube 33 and the fourth nickel reaction tube 35 adopt a metal screw buckle and gasket sealing method, the first nickel reaction tube 29, the second nickel reaction tube 31, The top outlets of the third nickel reaction tube 33 and the fourth nickel reaction tube 35 respectively pass through 1/4 inch stainless steel pipelines to connect with the eleventh 1/4 inch metal valve 21, the thirteenth 1/4 inch metal valve 23, and the fifteenth 1/4 inch metal valve respectively. The 4inch metal valve 25 and the seventeenth 1/4inch metal valve 27 are connected by metal ferrules.

The product collection and measurement system includes the eighteenth 1/4inch metal valve 36, the second metal cold trap 37, the nineteenth 1/4inch metal valve 38, the third metal cold trap 39, the twentieth 1/4inch metal valve 40, The first thermocouple vacuum gauge 41, the twenty-first 1/4inch metal valve 42, the twenty-second 1/4inch metal valve 43, the first Molecular sieve 44, twenty-third 1/4inch metal valve 45, twenty-fourth 1/4inch metal valve 46, second Molecular sieve 47, twenty-fifth 1/4inch metal valve 48, twenty-sixth 1/4inch metal valve 49, second thermocouple vacuum gauge 50, ionization vacuum gauge 51, turbomolecular pump 52 and isotope mass spectrometer 53. 1/ The right side of the 2inch stainless steel vertical main pipeline 8 is connected with one end of the eighteenth 1/4inch metal valve 36 through a pipeline, and the other end of the eighteenth 1/4inch metal valve 36 is connected with the second metal cold trap 37 inlet through a pipeline, The outlet of the second metal cold trap 37 is connected with one end of the nineteenth 1/4inch metal valve 38 through a pipeline, and the other end of the nineteenth 1/4inch metal valve 38 is connected with the inlet of the third metal cold trap 39 through a pipeline, and the third metal The outlet of the cold trap 39 is connected to one end of the twentieth 1/4inch metal valve 40 through a pipeline; One end of the twenty-fourth 1/4inch metal valve 46 is connected, and the top of the first thermocouple vacuum gauge 41 and one end of the twenty-first 1/4inch metal valve 42 are respectively connected to the twenty-first through a tee The 1/4inch stainless steel pipeline at the other end of the /4inch metal valve 40 is connected; the first thermocouple vacuum gauge 41 monitors the gas pressure of the reaction to generate oxygen, and the twenty-first 1/4inch metal valve 42 is connected to the ionization of the high vacuum degree of the monitoring system The vacuum gauge 51 is connected; the other end of the twenty-second 1/4inch metal valve 43 is connected with one end of the twenty-third 1/4inch metal valve 45 through a 1/4inch stainless steel pipeline, which is used to collect the first oxygen generated by the reaction. The inlet of the molecular sieve 44 is connected to the 1/4inch stainless steel pipeline through a tee; the other end of the twenty-fourth 1/4inch metal valve 46 is respectively connected to one end of the twenty-fifth 1/4inch metal valve 48 through a 1/4inch stainless steel pipeline and second The inlet of the molecular sieve 47 is connected; the other end of the twenty-third 1/4inch metal valve 45 and the other end of the twenty-fifth 1/4inch metal valve 48 are all through the double-way sampling of the 1/4inch stainless steel pipeline and the isotope mass spectrometer 53 System connection, the second thermocouple vacuum gauge 50 is connected with the 1/4inch stainless steel pipeline through a tee, and the second thermocouple vacuum gauge 50 monitors the pressure of the molecular sieve thawing to release oxygen; the other end of the twenty-first 1/4inch metal valve 42 The 1/4inch stainless steel pipeline is connected to the intake end of the turbomolecular pump 52, the top of the ionization vacuum gauge 51 is connected to the 1/4inch stainless steel pipeline through a tee, and the twenty-sixth 1/4inch metal valve 49 is connected upwardly through the tee. The 1/4inch stainless steel pipeline is connected, and the twenty-sixth 1/4inch metal valve 49 is connected downward with the 1/4inch stainless steel pipeline connected to the isotope mass spectrometer 53 through a tee; the turbomolecular pump with the rotary vane mechanical pump as the front stage 52 provides high vacuum for the entire analysis system.

The waste treatment system includes the first 1/4inch metal valve 1, the second 1/4inch metal valve 2, the rotary vane mechanical vacuum pump 3, the first metal cold trap 4, the third 1/4inch metal valve 5, the fifth 1/4inch Metal valve 9 and sixth 1/4inch metal valve 10. One end of the first 1/4inch metal valve 1 is connected to the waste pipeline, the other end of the first 1/4inch metal valve 1 is connected to the outlet of the first metal cold trap 4 through a 1/4inch stainless steel pipeline, and the second 1/4inch metal valve One end of 2 is connected to the 1/4inch stainless steel pipeline through a tee, and the inlet of the first metal cold trap 4 is connected to one end of the third 1/4inch metal valve 5 through a 1/4inch stainless steel pipeline; the third 1/4inch metal valve 5 The other end is connected to the first 1/2inch stainless steel main pipe 8 through a 1/4inch stainless steel pipeline, and the connection between the two is located between the fourth 1/4inch metal valve 7 and the eighteenth 1/4inch metal valve 36 . The other end of the second 1/4inch metal valve 2 is connected to the exhaust port of the mechanical vacuum pump 3 through a 1/4inch stainless steel pipeline. The rotary vane mechanical vacuum pump 3 is used to extract reaction waste gas and provide a low vacuum for the entire analysis system. One end of the fifth 1/4inch metal valve 9 is connected to the Ar gas cylinder outside the system through a 1/4inch stainless steel pipeline, and the other end of the fifth 1/4inch metal valve 9 is connected to the sixth 1/4inch metal valve through a 1/4inch stainless steel pipeline One end of 10 is connected, the other end of the sixth 1/4inch metal valve 10 is connected to the first 1/2inch stainless steel main pipe 8 through a 1/4inch stainless steel pipeline, and the sixth 1/4inch metal valve 10 is located at the eighteenth 1/4inch Between the metal valve 36 and the eighth 1/4inch metal valve 12 . The fifth 1/4inch metal valve 9 and the sixth 1/4inch metal valve 10 jointly control the flow of Ar gas entering the analysis system for purging waste gas.

The stainless steel pipelines are all made of 316 stainless steel, the inner wall of the pipeline is specially polished, and the pipelines except the metal cold trap are all wound with heating tape.

the first Molecular sieve 44, the second Molecular sieve 47 is filled in a stainless steel tube with an outer diameter of 1/2 inch, and oxygen is collected by freezing with liquid nitrogen.

An analysis system for oxygen isotope composition in oxygen-free mineral inclusion water as shown in Figures 1 and 2 is used to analyze the oxygen isotope composition in oxygen-free mineral inclusion water. The method specifically includes the following steps:

Step 1. Mineral sample injection

Close the tenth 1/4inch metal valve 20, the eleventh 1/4inch metal valve 21, the twelfth 1/4inch metal valve 22, the thirteenth 1/4inch metal valve 23, the fourteenth 1/4inch metal valve 24, The fifteenth 1/4inch metal valve 25, the sixteenth 1/4inch metal valve 26 and the seventeenth 1/4inch metal valve 27, remove the first quartz sample burst tube assembly 28, the second quartz sample burst tube assembly 30, The third quartz sample burst tube assembly 32, the fourth quartz sample burst tube assembly 34, the processed mineral sample particles are respectively loaded into the first quartz sample burst tube assembly 28, the second quartz sample burst tube assembly 30, the third quartz sample Burst tube assembly 32, the fourth quartz sample burst tube assembly 34, and the first quartz sample burst tube assembly 28, the second quartz sample burst tube assembly 30, the third quartz sample burst tube assembly 32, the fourth quartz sample burst tube assembly 34 Retighten and put back into the analysis system to complete the mineral sample injection operation.

Processed mineral sample particles such as pyrite, galena, sphalerite, fluorspar, etc.

Step 2. After the mineral sample injection is completed, the entire analysis system is baked and vacuum degassed

The first quartz sample burst tube assembly 28, the first nickel reaction tube 29, the second quartz sample burst tube assembly 30, the second nickel reaction tube 31, the third quartz sample burst tube assembly 32, the third nickel reaction tube 33, the second The four-quartz sample burst tube assembly 34 and the fourth nickel reaction tube 35 are respectively fitted with a digital temperature-controlled heating furnace, and the tenth 1/4inch metal valve 20, the eleventh 1/4inch metal valve 21, and the twelfth one are slowly opened in sequence. /4inch metal valve 22, thirteenth 1/4inch metal valve 23, fourteenth 1/4inch metal valve 24, fifteenth 1/4inch metal valve 25, sixteenth 1/4inch metal valve 26, seventeenth 1 /4inch metal valve 27, second 1/2inch metal valve 16, third 1/2inch metal valve 17, fourth 1/2inch metal valve 18, first 1/2inch metal valve 13, eighth 1/4inch metal valve 12 , The fourth 1/4inch metal valve 7, the third 1/4inch metal valve 5. Put a liquid nitrogen cup on the outside of the first metal cold trap 4 and slowly open the second 1/4inch metal valve 2 to connect the rotary vane mechanical vacuum pump 3 to draw a low vacuum for the analysis system, and open the eighteenth 1/4inch metal valve 36 And the nineteenth 1/4inch metal valve 38, adjust the temperature of the digital temperature-controlled heating furnace according to the properties of the mineral sample; at the same time, turn on the power supply of the heating belt to heat and degas the entire analysis system for 30 minutes, and then close the third 1/4inch metal valve 5. Put the second metal cold trap 37 and the third metal cold trap 39 on the liquid nitrogen cup, open the 20th 1/4inch metal valve 40, the 22nd 1/4inch metal valve 43, the 23rd 1/4inch metal valve Valve 45, twenty-fourth 1/4inch metal valve 46, twenty-fifth 1/4inch metal valve 48, twenty-sixth 1/4inch metal valve 49 and twenty-first 1/4inch metal valve 42, turn on the turbine Molecular pump 52 draws a high vacuum to the analysis system, and continues pumping for 30 minutes after the high vacuum degree of the analysis system reaches 10 ⁻⁵ Pa as monitored by ionization vacuum gauge 51 .

For pyrite, chalcopyrite, galena, sphalerite, fluorite and other minerals, the digital temperature-controlled heating furnace can be adjusted to 100-120 ℃ for heating and degassing, while minerals such as halite only need to be adjusted to 40- Heating at 50°C for degassing, if the temperature is too high, the inclusions in the mineral will burst out during the degassing stage.

The meaning of the letter "LV" on the left side of the rotary vane mechanical vacuum pump 3 in Figure 1 refers to low vacuum (LOW VACUUM)

Step 3. After the analysis system is baked and vacuum degassed, the mineral inclusions are exploded, and the product is extracted and purified.

Step 3.1, Mineral inclusions burst

After the vacuum degassing of the analysis system is completed, the first quartz sample burst tube assembly 28, the second quartz sample burst tube assembly 30, the third quartz sample burst tube assembly 32, the fourth quartz sample burst tube assembly 34, and the first The nickel reaction tube 29, the second nickel reaction tube 31, the third nickel reaction tube 33, and the fourth nickel reaction tube 35 are covered with circulating water, and the tenth 1/4inch metal valve 20 and the twelfth 1/4inch metal valve 22 are closed 1. The fourteenth 1/4inch metal valve 24 and the sixteenth 1/4inch metal valve 26 adjust the bursting temperature of the digital temperature-controlled heating furnace according to the properties of the mineral sample, and the bursting time is 30 minutes to complete the bursting of mineral inclusions.

In step 3.1, mineral inclusions exist in the mineral sample particles, and the size of the inclusions ranges from a few microns to tens of microns. By heating the minerals to a certain temperature, the internal inclusions will burst out of the minerals. The mineral inclusions are mainly composed of water, and sometimes contain a certain amount of carbon dioxide, hydrogen, methane and other gases, and their composition varies with the type of deposits produced.

Mineral inclusion bursting specifically means that after the mineral is heated to a certain temperature, the inclusion in the mineral will burst due to the increase in pressure and be separated from the inside of the mineral.

Step 3.2, Extraction of Mineral Inclusion Explosion Products

Remove the temperature-controlled heating furnace outside the first nickel reaction tube 29, the second nickel reaction tube 31, the third nickel reaction tube 33 and the fourth nickel reaction tube 35 after the bursting is completed, and cover the outside of these 4 nickel reaction tubes After the liquid nitrogen cup is fully frozen, the second 1/2inch metal valve 16, the third 1/2inch metal valve 17 and the fourth 1/2inch metal valve 18 are closed in sequence, and the tenth 1/4inch metal valve 20 and the tenth The second 1/4inch metal valve 22, the fourteenth 1/4inch metal valve 24 and the sixteenth 1/4inch metal valve 26, the mineral inclusion explosion product is automatically transferred and diffused to the corresponding first nickel reaction tube 29, the second Inside the nickel reaction tube 31, the third nickel reaction tube 33, and the fourth nickel reaction tube 35; after 20 minutes, close the tenth 1/4inch metal valve 20, the twelfth 1/4inch metal valve 22, and the fourteenth 1/4inch metal valve 24 and the sixteenth 1/4inch metal valve 26 complete the extraction of detonation products.

Step 3.3, Purification of Mineral Inclusion Explosion Products

After quickly removing the liquid nitrogen cups outside the first nickel reaction tube 29, the second nickel reaction tube 31, the third nickel reaction tube 33 and the fourth nickel reaction tube 35, quickly put dry ice on the outside of the 4 nickel reaction tubes- Purify the popping extract with alcohol mixed refrigerant for 20 minutes, open the second 1/2inch metal valve 16, the third 1/2inch metal valve 17 and the fourth 1/2inch metal valve 18 to remove the impurity components in the popping product, close the second The eleventh 1/4inch metal valve 21, the thirteenth 1/4inch metal valve 23, the fifteenth 1/4inch metal valve 25 and the seventeenth 1/4inch metal valve 27 complete the purification of detonation products.

The purified detonation product is water, which is also the product that needs to be extracted in the analytical method.

Step 4. Transform the water in the mineral inclusions that have been exploded, extracted and purified in Step 3 above

Close the eighth 1/4inch metal valve 12 and the eighteenth 1/4inch metal valve 36, open the ninth 1/4inch metal valve 14, slowly open the eighth 1/4inch metal valve 12, and make the bromine pentafluoride storage tank 15 The BrF ₅ reagent in the medium diffuses into the first 1/2inch stainless steel main pipe 8 and the second 1/2inch stainless steel main pipe 19, and monitors the diffusion into the first 1/2inch stainless steel main pipe 8 and the second 1 through the vacuum pressure gauge 6 _The pressure value of the BrF5 reagent in the /2inch stainless steel main pipeline 19, and the _BrF5 reagent needed for the reaction is transferred to the first nickel reaction tube 29, the second nickel reaction tube 31, the third nickel reaction tube 33, the fourth nickel reaction tube successively. Inside the nickel reaction tube 35. Remove the dry ice-alcohol refrigerant outside the first nickel reaction tube 29, the second nickel reaction tube 31, the third nickel reaction tube 33, and the fourth nickel reaction tube 35, and react again in the first nickel reaction tube 29, the second nickel reaction tube Tube 31, the third nickel reaction tube 33, and the fourth nickel reaction tube 35 are equipped with a digital temperature-controlled heating furnace. The temperature of the digital temperature-controlled heating furnace is adjusted to 300°C and heated for 20 minutes. The first nickel reaction tube 29 and the second nickel The water in the reaction tube 31 , the third nickel reaction tube 33 , and the fourth nickel reaction tube 35 reacts with the BrF ₅ reagent to completely release O ₂ .

Step 5. Collect and mass spectrometer the mineral inclusion water conversion product— _O2 obtained in the above step 4

Step 5.1, Mineral inclusion transformation product— _O2 collection

Remove the temperature control heating furnace outside the first nickel reaction tube 29, the second nickel reaction tube 31, the 3rd nickel reaction tube 33, the 4th nickel reaction tube 35, re-in the first nickel reaction tube 29, the second nickel reaction tube 31. A liquid nitrogen cup is placed on the outside of the third nickel reaction tube 33 and the fourth nickel reaction tube 35 . Close the eighth 1/4inch metal valve 12, the fourth 1/4inch metal valve 7, the eighteenth 1/4inch metal valve 36, the nineteenth 1/4inch metal valve 38, the twentieth 1/4inch metal valve 40, the eighth Twenty-one 1/4inch metal valve 42, twenty-second 1/4inch metal valve 43, twenty-third 1/4inch metal valve 45, twenty-fourth 1/4inch metal valve 46, twenty-fifth 1/4inch The metal valve 48 and the twenty-sixth 1/4inch metal valve 49 slowly open the eleventh 1/4inch metal valve ₂₁ on the first nickel reaction tube 29, so that the O generated in the first nickel reaction tube 29 Slowly Discharge into the first 1/2inch stainless steel main pipe 8 and the second 1/2inch stainless steel main pipe 19. Slowly open the eighteenth 1/4inch metal valve 36, the nineteenth 1/4inch metal valve 38 and the twentieth ₁ /4inch metal valve 40 in sequence, and monitor the reaction to generate O by the first thermocouple vacuum gauge 41 Pressure; Open the twenty-second 1/4inch metal valve 43, turn the first Molecular sieve 44 is fully frozen with liquid nitrogen to collect the O in the first nickel reaction tube 29 After that, close the twenty- _second 1/4inch metal valve 43, remove the first Liquid nitrogen outside the molecular sieve 44; close the eleventh 1/4inch metal valve 21, open the twenty-first 1/4inch metal valve 42 to connect the turbomolecular pump 52 to the first 1/2inch stainless steel main pipe 8 and the second 1/2inch Close all valves after the 2inch stainless steel main pipeline 19 is evacuated to 10 ⁻⁵ Pa.

Step 5.2, mineral inclusion transformation product— _O2 mass spectrometry measurement

Open the twenty-third 1/4inch metal valve 45, and monitor the first thermocouple vacuum gauge 50 through the second Molecular sieve 44 releases the pressure of _O2 after thawing, and _O2 diffuses into isotope mass spectrometer 53 to carry out isotope measurement. Molecular sieve 44 is evacuated to 10 ^-5 Pa, close the twenty-third 1/4inch metal valve 45 and the twenty-sixth 1/4inch metal valve 49; open the thirteenth 1/4inch metal valve 23 and open the first step 5.1 Twenty-four 1/4inch metal valves 46 can collect the O in the _second nickel reaction tube 31 in the second In the molecular sieve 47, close the twenty-fourth 1/4inch metal valve 46, remove the second Liquid nitrogen outside the molecular sieve 47, open the twenty-fifth 1/4inch metal valve 48, monitor the second by the second thermocouple vacuum gauge 50 After the molecular sieve 47 is thawed, release O ₂ pressure, O ₂ diffuses into the isotope mass spectrometer 53 and carries out isotope measurement; According to the operation method in step 5.1 and step 5.2, the O in the third nickel reaction tube 33 and the fourth nickel reaction tube 35 can be completed. ₂ Collect and measure.

Step 6, carrying out waste treatment to the residual reagents and reaction products in the above steps 3 and 4

After the O in the first nickel reaction tube 29, the _second nickel reaction tube 31, the 3rd nickel reaction tube 33, and the fourth nickel reaction tube 35 completed collection and measurement, the remaining reagent and reaction product in the nickel reactor need For harmless treatment, the specific steps are as follows:

The reagents remaining in the first nickel reaction tube 29, the second nickel reaction tube 31, the third nickel reaction tube 33, and the fourth nickel reaction tube 35 are mainly unreacted BrF ₅ reagents, and the remaining reaction products include BrF ₃ , HF , HBr, etc.

Close the eighteenth 1/4inch metal valve 36, the fourth 1/4inch metal valve 7, the first 1/4inch metal valve 1 and the second 1/4inch metal valve 2, and put liquid nitrogen on the first metal cold trap 4 coat, Remove the first quartz sample burst tube assembly 28, the second quartz sample burst tube assembly 30, the third quartz sample burst tube assembly 32, the fourth quartz sample burst tube assembly 34 and the first nickel reaction tube 29, the second nickel reaction tube 31. The cooling water system outside the third nickel reaction tube 33 and the fourth nickel reaction tube 35, outside the first nickel reaction tube 29, the second nickel reaction tube 31, the third nickel reaction tube 33, and the fourth nickel reaction tube 35 Re-install the temperature-controlled heating furnace, adjust the temperature-controlled heating furnace to 150°C, and heat the four nickel reaction tubes 29, 31, 33, and 35; open the third 1/4inch metal valve 5 and then open the eleventh 1/4 inch 4inch metal valve 21, the thirteenth 1/4inch metal valve 23, the fifteenth 1/4inch metal valve 25 and the seventeenth 1/4inch metal valve 27, the four nickel reaction tubes 29, 31, 33, 35 The waste is transferred to the first metal cold trap 4. Close the first 1/2inch metal valve 13, open the fifth 1/4inch metal valve 9 and the sixth 1/4inch metal valve 10, remove the liquid nitrogen outside the first metal cold trap 4, and open the first 1/4inch metal valve 1 , Carry the waste with Ar gas to the lime bucket in the fume hood connected to the pipeline on the left side of the first 1/4inch metal valve 1 to complete waste disposal and avoid environmental pollution.

As shown in Figure 2, the structures of the first quartz sample burst tube assembly 28, the second quartz sample burst tube assembly 30, the third quartz sample burst tube assembly 32, and the fourth quartz sample burst tube assembly 34 are exactly the same, and the four quartz sample burst tube assemblies The bursting tube group includes external thread stainless steel tube 54, quartz bursting tube 55, "O" type rubber sealing ring 56, annular flat sealing metal sleeve 57 and internal threaded metal pipe collar 58, and the open end of quartz bursting tube 55 is inserted into the external thread Inside the bottom of the stainless steel pipe 54, an "O" rubber sealing ring 56 is provided between the externally threaded stainless steel pipe 54 and the quartz burst pipe 55. The bottom of the "O" rubber sealing ring 56 is provided with an annular plane sealing metal sleeve 57, and the annular plane The bottom of the sealing metal casing 57 is inserted in the threaded metal pipe ferrule 58, and the "O" type rubber sealing ring 56, the annular plane sealing metal casing 57 and the threaded metal pipe ferrule 58 are all set on the outside of the quartz burst pipe 55.

When assembling, insert the quartz sample burst tube 55 into the externally threaded stainless steel tube 54, and push the ring-shaped flat sealing metal sleeve 57 by rotating the internally threaded metal pipe ferrule 58 to squeeze the "O"-shaped rubber sealing ring 56 to realize the bursting of the quartz sample Tube 55 is a sealed transition connection with externally threaded stainless steel tube 54 . The externally threaded stainless steel pipe 54 top externally threaded rod is connected with the metal valve through a 1/4inch stainless steel pipeline.

The externally threaded stainless steel tube 54 is internally polished, and the end is designed with a wedge-shaped facet. The quartz burst tube 55 and the externally threaded stainless steel tube 54 are elastically deformed by an "O"-shaped rubber sealing ring 56 to realize a sealed transition connection.

The present invention has been described in detail above in conjunction with the accompanying drawings and embodiments, but the present invention is not limited to the above-mentioned embodiments, and can also be made without departing from the gist of the present invention within the scope of knowledge possessed by those of ordinary skill in the art. kind of change. The content that is not described in detail in the present invention can adopt the prior art.

Claims (21)

1. An analysis system for oxygen isotope composition in oxygen-free mineral inclusion water, characterized in that: the system includes inclusion burst extraction/purification separation/extract conversion system, product collection and measurement system, and waste treatment system; One end of the body burst extraction/purification separation/extract conversion system is connected to the product collection and measurement system, and the other end of the inclusion burst extraction/purification separation/extract conversion system is connected to the waste treatment system. 2. the analysis system of oxygen isotope composition in a kind of oxygen-free mineral inclusion water according to claim 1, it is characterized in that: described inclusion burst extraction/purification separation/extract transformation system comprises vacuum pressure gauge (6 ), the first 1/2inch stainless steel main pipe (8), bromine pentafluoride storage tank (15), the second 1/2inch stainless steel main pipe (19), the first burst-extraction unit, the second burst- Extraction unit, the third set of burst-extraction unit and the fourth set of burst-extraction unit, the first 1/2inch stainless steel main pipe (8), the bottom of the vacuum pressure gauge (6) and the first 1/2inch stainless steel main pipe (8) Connection, the first 1/2inch stainless steel main pipe (8) is connected with the outlet of bromine pentafluoride storage tank (15) and the second 1/2inch stainless steel main pipe (19) respectively; the second 1/2inch stainless steel main pipe (19 ) are respectively connected with the first group of burst-extraction units, the second group of burst-extraction units, the third group of burst-extraction units, and the fourth group of burst-extraction units, and the first group of burst-extraction units, the second group of burst-extraction units The extraction unit, the third group of burst-extraction units, and the fourth group of burst-extraction units are connected in parallel. 3. the analysis system of oxygen isotope composition in a kind of oxygen-free mineral inclusion water according to claim 2, it is characterized in that: the bottom of described vacuum pressure gauge (6) and the first 1/2inch stainless steel main pipe (8 ) is provided with a fourth 1/4inch metal valve (7). 4. the analysis system of oxygen isotope composition in a kind of oxygen-free mineral inclusion water according to claim 3, it is characterized in that: described first 1/2inch stainless steel main pipe (8) and bromine pentafluoride storage The eighth 1/4inch metal valve (12), the ninth 1/4inch metal valve (14), the eighth 1/4inch metal valve (12) and the ninth 1/4inch metal valve (14) are arranged between the tanks (15). ) is provided with a seventh 1/4inch metal valve (11). 5. The analysis system for oxygen isotope composition in a kind of oxygen-free mineral inclusion water according to claim 4, characterized in that: the first 1/2inch stainless steel main pipe (8) and the second 1/2inch stainless steel A first 1/2inch metal valve (13) is provided between the main pipes (19), a second 1/2inch metal valve (16) and a third 1/2inch metal valve (16) are provided on the second 1/2inch stainless steel main pipe (19). Metal valve (17), fourth 1/2inch metal valve (18). 6. The analysis system of oxygen isotope composition in a kind of oxygen-free mineral inclusion water according to claim 5, it is characterized in that: described first group burst-extraction unit comprises the tenth 1/4inch metal valve (20) , the first quartz sample burst tube assembly (28), the eleventh 1/4inch metal valve (21) and the first nickel reaction tube (29), the top of the first quartz sample burst tube assembly (28) and the tenth 1/4inch One end of the metal valve (20) is connected, the top of the first nickel reaction tube (29) is connected with one end of the eleventh 1/4inch metal valve (21), the other end of the tenth 1/4inch metal valve (20), the tenth The other end of a 1/4inch metal valve (21) is all connected with an end of the second 1/2inch metal valve (16) on the second 1/2inch stainless steel main pipe (19); the second group of explosion-extraction unit includes the first Twelve 1/4inch metal valves (22), the second quartz sample burst tube assembly (30), the thirteenth 1/4inch metal valve (23) and the second nickel reaction tube (31), the second quartz sample burst tube assembly (30) the top is connected with one end of the twelfth 1/4inch metal valve (22), the top of the second nickel reaction tube (31) is connected with one end of the thirteenth 1/4inch metal valve (23), and the twelfth 1/4inch metal valve (23) is connected with one end. The other end of the 4inch metal valve (22), the thirteenth 1/4inch metal valve (23) is all connected with the other end of the second 1/2inch metal valve (16) on the second 1/2inch stainless steel main pipe (19), One end of the third 1/2inch metal valve (17) is connected; the third group of burst-extraction unit includes the fourteenth 1/4inch metal valve (24), the third quartz sample burst tube assembly (32), the fifteenth 1/4 inch 4inch metal valve (25) and the third nickel reaction tube (33), the top of the third quartz sample burst tube assembly (32) is connected with one end of the fourteenth 1/4inch metal valve (24), the third nickel reaction tube (33 ) top is connected with one end of the fifteenth 1/4inch metal valve (25), the other end of the fourteenth 1/4inch metal valve (24) and the other end of the fifteenth 1/4inch metal valve (25) are connected with the first The other end of the third 1/2inch metal valve (17) on the two 1/2inch stainless steel main pipes (19), one end of the fourth 1/2inch metal valve (18) are connected; the fourth group of burst-extraction unit includes the tenth Six 1/4inch metal valves (26), the fourth quartz sample burst tube assembly (34), the seventeenth 1/4inch metal valve (27) and the fourth nickel reaction tube (35), the fourth quartz sample burst tube assembly ( 34) The top is connected to one end of the sixteenth 1/4inch metal valve (26), the top of the fourth nickel reaction tube (35) is connected to one end of the seventeenth 1/4inch metal valve (27), and the sixteenth 1/4inch Another metal valve (26) The other end of end, the seventeenth 1/4inch metal valve (27) is all connected with the other end of the 4th 1/2inch metal valve (18) on the second 1/2inch stainless steel main pipe (19). 7. The analysis system of oxygen isotope composition in a kind of oxygen-free mineral inclusion water according to claim 6, it is characterized in that: described transformation product collection and measurement system comprises the second metal cold trap (37), the third Metal cold trap (39), the first thermocouple vacuum gauge (41), the first Molecular sieve (44), the second Molecular sieve (47), second thermocouple vacuum gauge (50), ionization vacuum gauge (51), turbomolecular pump (52) and isotope mass spectrometer (53), the first 1/2inch stainless steel main pipe (8) and the second The metal cold trap (37) inlet is connected, the second metal cold trap (37) outlet is connected with the third metal cold trap (39) inlet, and the third metal cold trap (39) outlet is respectively connected with the first thermocouple vacuum gauge (41) ,First Molecular sieve (44) inlet, the second Molecular sieve (47) inlet, ionization vacuum gauge (51), output end of turbomolecular pump (52) are connected, the first Molecular sieve (44) outlet, the second The outlets of the molecular sieves (47) are all connected to the second thermocouple vacuum gauge (50) and the isotope mass spectrometer (53). 8. the analysis system of oxygen isotope composition in a kind of oxygen-free mineral inclusion water according to claim 7, it is characterized in that: described first 1/2inch stainless steel main pipeline (8) and the second metal cold trap ( 37) An eighteenth 1/4inch metal valve (36) is provided between the inlets, and a nineteenth 1/4inch metal valve is provided between the outlet of the second metal cold trap (37) and the inlet of the third metal cold trap (39) (38), the third metal cold trap (39) outlet and the first The twentieth 1/4inch metal valve (40) and the twenty-second 1/4inch metal valve (43) are arranged between the molecular sieve (44) inlets, and the third metal cold trap (39) outlet and the second The twentieth 1/4inch metal valve (40) and the twenty-fourth 1/4inch metal valve (46) are arranged between the inlets of the molecular sieve (47), and the first A twenty-third 1/4inch metal valve (45) is arranged between the molecular sieve (44) outlet and the second thermocouple vacuum gauge (50) and the isotope mass spectrometer (53). A twenty-fifth 1/4inch metal valve (48) is provided between the outlet of the molecular sieve (47), and a third metal valve (48) is provided between the outlet of the third metal cold trap (39) and the ionization vacuum gauge (51) and the turbomolecular pump (52). Twenty 1/4inch metal valve (40), twenty-first 1/4inch metal valve (42), the first thermocouple vacuum gauge (41) is connected with the twenty-second 1/4inch metal valve (40), the third metal Cold trap (39) outlet and the first thermocouple vacuum gauge (41), the first Molecular sieve (44) inlet, the second Molecular sieve (47) inlet, ionization vacuum gauge (51), the intake end of turbomolecular pump (52) are connected, ionization vacuum gauge (51), turbomolecular pump (52) and the second thermocouple vacuum gauge (50), isotope A twenty-sixth 1/4inch metal valve (49) is provided between the mass spectrometers (53). 9. The analysis system of oxygen isotope composition in a kind of oxygen-free mineral inclusion water according to claim 10, it is characterized in that: described waste treatment system comprises rotary vane mechanical vacuum pump (3), the first metal cold trap (4), the fifth 1/4inch metal valve (9) and the sixth 1/4inch metal valve (10), the first 1/2inch stainless steel main pipe (8) and the inlet of the first metal cold trap (4), respectively The sixth 1/4inch metal valve (10) is connected, the outlet of the first metal cold trap (4) is connected to the suction port of the rotary vane mechanical vacuum pump (3), the sixth 1/4inch metal valve (10) is connected to the fifth 1/ 4inch metal valve (9) connection. 10. the analysis system of oxygen isotope composition in a kind of oxygen-free mineral inclusion water according to claim 9, it is characterized in that: described first 1/2inch stainless steel main pipeline (8) and first metal cold trap ( 4) A third 1/4inch metal valve (5) is provided between the inlet, and a second 1/4inch metal valve (2) is provided between the outlet of the first metal cold trap (4) and the rotary vane mechanical vacuum pump (3) , the outlet of the first metal cold trap (4) and the second 1/4inch metal valve (2) are all connected to the first 1/4inch metal valve (1). 11. A quartz sample burst tube assembly for the analysis system described in claims 6 to 10, characterized in that: the quartz sample burst tube assembly comprises an externally threaded stainless steel tube (54), a quartz burst tube (55), a rubber seal Ring (56), sealing metal sleeve (57) and internal thread metal pipe collar (58), the open end of quartz burst pipe (55) is inserted in the bottom of external thread stainless steel pipe (54), external thread stainless steel pipe (54) and A rubber sealing ring (56) is arranged between the quartz bursting pipes (55), and a sealing metal casing (57) is arranged at the bottom of the rubber sealing ring (56), and the bottom of the sealing metal casing (57) is inserted into the threaded metal pipe collar (58 ), rubber sealing ring (56), sealing metal casing (57), threaded metal pipe collar (58) are all enclosed within the quartz burst pipe (55) outside. 12. A method for analyzing the composition of oxygen isotopes in oxygen-free mineral inclusion water using the analysis system described in claims 1 to 10, characterized in that the method specifically comprises the following steps: Step 1, mineral sample injection; Step 2. Baking and vacuum degassing the entire analysis system; Step 3. After the vacuum degassing of the analysis system is completed, the mineral inclusions are burst and the burst products are extracted and purified; Step 4, transforming the water in the mineral inclusions that have been exploded, extracted and purified in the above step 3; Step 5, collecting and mass spectrometrically measuring the transformation product obtained in the above step 4 after water transformation of the mineral inclusions; Step 6. Perform waste treatment on the residual reagents and reaction products in the above steps 3 and 4. 13. the analytical method of oxygen isotope composition in oxygen-free mineral inclusion water according to claim 12, is characterized in that, described step 1 specifically comprises the following steps: Close the tenth 1/4inch metal valve (20), the eleventh 1/4inch metal valve (21), the twelfth 1/4inch metal valve (22), the thirteenth 1/4inch metal valve (23), the tenth Four 1/4inch metal valves (24), fifteenth 1/4inch metal valves (25), sixteenth 1/4inch metal valves (26) and seventeenth 1/4inch metal valves (27), remove the first Quartz sample burst tube assembly (28), the second quartz sample burst tube assembly (30), the third quartz sample burst tube assembly (32), the fourth quartz sample burst tube assembly (34), the processed mineral sample particles are respectively Load the first quartz sample burst tube assembly (28), the second quartz sample burst tube assembly (30), the third quartz sample burst tube assembly (32), the fourth quartz sample burst tube assembly (34), and place the first The quartz sample burst tube assembly (28), the second quartz sample burst tube assembly (30), the third quartz sample burst tube assembly (32), and the fourth quartz sample burst tube assembly (34) are respectively connected upwardly with the 1/4inch stainless steel pipeline. The tenth 1/4inch metal valve (20), the twelfth 1/4inch metal valve (22), the fourteenth 1/4inch metal valve (24), the sixteenth 1/4inch metal valve (26) are connected to complete the mineral Sample injection operation. 14. the analytical method of oxygen isotope composition in oxygen-free mineral inclusion water according to claim 13, is characterized in that, described step 2 specifically comprises the following steps: The first quartz sample burst tube assembly (28), the first nickel reaction tube (29), the second quartz sample burst tube assembly (30), the second nickel reaction tube (31), the third quartz sample burst tube assembly (32 ), the third nickel reaction tube (33), the fourth quartz sample burst tube assembly (34) and the fourth nickel reaction tube (35) are respectively put on a digital temperature-controlled heating furnace, and slowly open the tenth 1/4inch metal valve in sequence (20), the eleventh 1/4inch metal valve (21), the twelfth 1/4inch metal valve (22), the thirteenth 1/4inch metal valve (23), the fourteenth 1/4inch metal valve (24 ), the fifteenth 1/4inch metal valve (25), the sixteenth 1/4inch metal valve (26), the seventeenth 1/4inch metal valve (27), the second 1/2inch metal valve (16), the first Three 1/2inch metal valves (17), fourth 1/2inch metal valves (18), first 1/2inch metal valves (13), eighth 1/4inch metal valves (12), fourth 1/4inch metal valves (7), the third 1/4inch metal valve (5), put the liquid nitrogen cup on the outside of the first metal cold trap (4), and then slowly open the second 1/4inch metal valve (2) to connect the rotary vane mechanical vacuum pump (3) For this analysis system, draw a low vacuum, open the eighteenth 1/4inch metal valve (36) and the nineteenth 1/4inch metal valve (38), and adjust the temperature of the digital temperature-controlled heating furnace according to the properties of the mineral sample; open After heating and degassing the entire analysis system for 30 minutes with the power supply of the heating belt, close the third 1/4inch metal valve (5); put the second metal cold trap (37) and the third metal cold trap (39) on the liquid nitrogen cup, and open The 20th 1/4inch metal valve (40), the 22nd 1/4inch metal valve (43), the 23rd 1/4inch metal valve (45), the 24th 1/4inch metal valve (46) , the twenty-fifth 1/4inch metal valve (48), the twenty-sixth 1/4inch metal valve (49) and the twenty-first 1/4inch metal valve (42), connect the turbomolecular pump (52) to the The analysis system is subjected to high vacuum pumping, and the high vacuum degree of the analysis system is monitored by an ionization vacuum gauge (51) to reach 10 ⁻⁵ Pa, and the pumping is continued for 30 min. 15. the method for analyzing the composition of oxygen isotopes in oxygen-free mineral inclusion water according to claim 14, characterized in that, the concrete steps of mineral inclusion bursting in the described step 3 are as follows: After the vacuum degassing of the analysis system is completed, the first quartz sample burst tube assembly (28), the second quartz sample burst tube assembly (30), the third quartz sample burst tube assembly (32), the fourth quartz sample burst tube assembly (34), and the first nickel reaction tube (29), the second nickel reaction tube (31), the third nickel reaction tube (33), the outside of the fourth nickel reaction tube (35) put circulating water, close the tenth 1st /4inch metal valve (20), twelfth 1/4inch metal valve (22), fourteenth 1/4inch metal valve (24) and sixteenth 1/4inch metal valve (26), adjust the number according to the properties of mineral samples The bursting temperature of the heating furnace is controlled by temperature, and the bursting time is 30 minutes to complete the bursting of mineral inclusions. 16. The method for analyzing the composition of oxygen isotopes in oxygen-free mineral inclusion water according to claim 15, characterized in that, the specific steps of extracting mineral inclusion detonation products in the step 3 are as follows: Remove the first nickel reaction tube (29), the second nickel reaction tube (31), the third nickel reaction tube (33) and the temperature control heating furnace outside the 4th nickel reaction tube (35) after bursting is completed, and in 4 Put a liquid nitrogen cup on the outside of the first nickel reaction tube to fully freeze, close the second 1/2inch metal valve (16), the third 1/2inch metal valve (17) and the fourth 1/2inch metal valve (18) in sequence, Open the tenth 1/4inch metal valve (20), the twelfth 1/4inch metal valve (22), the fourteenth 1/4inch metal valve (24) and the sixteenth 1/4inch metal valve (26), mineral The inclusion explosion product is automatically transferred and diffused into the corresponding first nickel reaction tube (29), second nickel reaction tube (31), third nickel reaction tube (33), and fourth nickel reaction tube (35); 20min After closing the tenth 1/4inch metal valve (20), the twelfth 1/4inch metal valve (22), the fourteenth 1/4inch metal valve (24) and the sixteenth 1/4inch metal valve (26) to complete the burst Product extraction. 17. The method for analyzing the composition of oxygen isotopes in oxygen-free mineral inclusion water according to claim 16, characterized in that, in the step 3, the specific steps for the purification of mineral inclusion detonation products are as follows: After removing the liquid nitrogen cup outside the first nickel reaction tube (29), the second nickel reaction tube (31), the third nickel reaction tube (33) and the fourth nickel reaction tube (35), in the 4 nickel reaction tubes Put a dry ice-alcohol mixed refrigerant on the outside of the tube to purify the burst extract for 20 minutes, and open the second 1/2inch metal valve (16), the third 1/2inch metal valve (17) and the fourth 1/2inch metal valve (18 ) to remove the impurity components in the explosion product, close the eleventh 1/4inch metal valve (21), the thirteenth 1/4inch metal valve (23), the fifteenth 1/4inch metal valve (25) and the seventeenth The 1/4inch metal valve (27) completes the detonation product purification. 18. The analytical method of oxygen isotope composition in oxygen-free mineral inclusion water according to claim 16, is characterized in that, the specific steps of described step 4 are as follows: Close the eighth 1/4inch metal valve (12), the eighteenth 1/4inch metal valve (36), open the ninth 1/4inch metal valve 14, slowly open the eighth 1/4inch metal valve (12), pentafluoride The BrF ₅ reagent monitoring in the bromine storage tank (15) diffuses into the first 1/2inch stainless steel main pipeline (8) and the second 1/2inch stainless steel main pipeline (19); 1/2inch stainless steel main pipeline (8) and the pressure value of the BrF5 reagent in the second ₁ /2inch stainless steel main pipeline (19), and the _BrF5 reagent needed for reaction is transferred to the first nickel reaction tube of freezing successively ( 29), the second nickel reaction tube (31), the third nickel reaction tube (33), the fourth nickel reaction tube (35); remove the first nickel reaction tube (29), the second nickel reaction tube (31) , the dry ice-alcohol refrigerant outside the 3rd nickel reaction tube (33), the 4th nickel reaction tube (35), again in the first nickel reaction tube (29), the second nickel reaction tube (31), the 3rd nickel reaction Tube (33) and the fourth nickel reaction tube (35) are equipped with a digital temperature-controlled heating furnace. The temperature of the digital temperature-controlled heating furnace is adjusted to 300° C. and heated for 20 minutes. The first nickel reaction tube (29) and the second nickel reaction The water in the tube (31), the third nickel reaction tube (33), and the fourth nickel reaction tube (35) reacts with the BrF ₅ reagent to completely release O ₂ . 19. The method for analyzing the composition of oxygen isotopes in oxygen-free mineral inclusion water according to claim 18, characterized in that, the specific steps for collecting the transformation product of mineral inclusions in the step 5 are as follows: Remove the temperature control heating furnace outside the first nickel reaction tube (29), the second nickel reaction tube (31), the third nickel reaction tube (33), the 4th nickel reaction tube (35), and react in the first nickel reaction tube again Pipe (29), the second nickel reaction tube (31), the third nickel reaction tube (33), and the fourth nickel reaction tube (35) are covered with liquid nitrogen cups. Close the eighth 1/4inch metal valve (12), the fourth 1/4inch metal valve (7), the eighteenth 1/4inch metal valve (36), the nineteenth 1/4inch metal valve (38), the twenty 1/4inch metal valve (40), twenty-first 1/4inch metal valve (42), twenty-second 1/4inch metal valve (43), twenty-third 1/4inch metal valve (45), second Fourteen 1/4inch metal valves (46), twenty-fifth 1/4inch metal valves (48) and twenty-sixth 1/4inch metal valves (49), slowly open the first nickel reaction tube (29) Eleven 1/4inch metal valves (21), so that the _O2 generated in the first nickel reaction tube (29) is slowly released to the first 1/2inch stainless steel main pipeline (8) and the second 1/2inch stainless steel main pipeline (19); slowly open the eighteenth 1/4inch metal valve (36), the nineteenth 1/4inch metal valve (38) and the twentieth 1/4inch metal valve (40) in turn, and pass the first thermocouple Vacuum gauge (41) monitoring reaction generates O ₂ pressure; Open the twenty-second 1/4inch metal valve (43), the first Molecular sieve (44) fully freezes and collects the O in the first nickel reaction tube (29) with liquid nitrogen After , close the twenty- _second 1/4inch metal valve, remove the first Liquid nitrogen over molecular sieve (44). 20. The method for analyzing the composition of oxygen isotopes in oxygen-free mineral inclusion water according to claim 19, characterized in that, the specific steps of mass spectrometry measurement of mineral inclusion conversion products in the step 5 are as follows: Open the twenty-third 1/4inch metal valve (45), and monitor the first thermocouple vacuum gauge (50) through the second Molecular sieve (44) releases the pressure of _O2 after thawing, and _O2 diffuses into the isotope mass spectrometer (53) to carry out isotope measurement, and opens the twenty-fourth 1/4inch metal valve according to the above operation to put the second nickel reaction tube (31) The O ₂ was collected in a second well frozen with liquid nitrogen In the molecular sieve (47), remove the liquid nitrogen and open the twenty-fifth 1/4inch metal valve (48), and monitor the pressure of _O2 released after the molecular sieve is thawed through the second thermocouple vacuum gauge (50), and _O2 diffuses into the isotope mass spectrometer Carry out isotope measurement in (53 ₎ , finish O in all the other nickel reaction tubes by the same operation method Collection, measurement. 21. The analytical method of oxygen isotope composition in oxygen-free mineral inclusion water according to claim 20, is characterized in that, the specific steps of described step 6 are as follows: Close the eighteenth 1/4inch metal valve (36), the fourth 1/4inch metal valve (7), the first 1/4inch metal valve (1) and the second 1/4inch metal valve (2), on the first metal Liquid nitrogen is put on the cold trap (4), and the first quartz sample burst tube assembly (28), the second quartz sample burst tube assembly (30), the third quartz sample burst tube assembly (32), and the fourth quartz sample burst tube assembly are removed. Tube assembly (34), and the cooling water system outside the first nickel reaction tube (29), the second nickel reaction tube (31), the third nickel reaction tube (33), and the fourth nickel reaction tube (35), in A nickel reaction tube (29), the second nickel reaction tube (31), the third nickel reaction tube (33), and the fourth nickel reaction tube (35) are put on the temperature-controlled heating furnace again, and the temperature-controlled heating furnace is adjusted to 150 ℃, 4 nickel reaction tubes (29, 31, 33, 35) are heated; after opening the third 1/4inch metal valve (5), open the eleventh 1/4inch metal valve (21), the thirteenth 1 /4inch metal valve (23), the fifteenth 1/4inch metal valve (25) and the seventeenth 1/4inch metal valve (27), the waste in 4 nickel reaction tubes (29,31,33,35) Transfer to the first metal cold trap (4); close the first 1/2inch metal valve (13), open the fifth 1/4inch metal valve (9) and the sixth 1/4inch metal valve (10), remove the first Liquid nitrogen outside the metal cold trap (4), open the first 1/4inch metal valve (1), and carry the waste with Ar gas to the fume hood connected to the pipeline on the left side of the first 1/4inch metal valve (1) Lime bucket to complete waste disposal.