CN107422024B - Analysis system and method for oxygen isotope composition in oxygen-free mineral inclusion water - Google Patents
Analysis system and method for oxygen isotope composition in oxygen-free mineral inclusion water Download PDFInfo
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- 238000004458 analytical method Methods 0.000 title claims abstract description 66
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- 239000001301 oxygen Substances 0.000 title claims abstract description 57
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 57
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 239000000203 mixture Substances 0.000 title claims abstract description 32
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- 238000005259 measurement Methods 0.000 claims abstract description 21
- 238000000746 purification Methods 0.000 claims abstract description 17
- 238000000926 separation method Methods 0.000 claims abstract description 14
- 238000009849 vacuum degassing Methods 0.000 claims abstract description 10
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- 239000012084 conversion product Substances 0.000 claims abstract description 5
- 238000001819 mass spectrum Methods 0.000 claims abstract description 3
- 239000002184 metal Substances 0.000 claims description 622
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 140
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- 229910001220 stainless steel Inorganic materials 0.000 claims description 123
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- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 54
- 239000002808 molecular sieve Substances 0.000 claims description 50
- 238000004880 explosion Methods 0.000 claims description 44
- 238000010438 heat treatment Methods 0.000 claims description 39
- 239000007788 liquid Substances 0.000 claims description 34
- 229910052757 nitrogen Inorganic materials 0.000 claims description 32
- 238000007789 sealing Methods 0.000 claims description 24
- 239000003153 chemical reaction reagent Substances 0.000 claims description 18
- TVVNZBSLUREFJN-UHFFFAOYSA-N 2-(4-chlorophenyl)sulfanyl-5-nitrobenzaldehyde Chemical compound O=CC1=CC([N+](=O)[O-])=CC=C1SC1=CC=C(Cl)C=C1 TVVNZBSLUREFJN-UHFFFAOYSA-N 0.000 claims description 16
- 238000012544 monitoring process Methods 0.000 claims description 12
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- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 3
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- 239000003517 fume Substances 0.000 claims description 3
- 239000004571 lime Substances 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 3
- 210000003000 inclusion body Anatomy 0.000 claims description 2
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- 238000012360 testing method Methods 0.000 abstract description 6
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- 238000005474 detonation Methods 0.000 description 4
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- 238000007872 degassing Methods 0.000 description 3
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- RBHJBMIOOPYDBQ-UHFFFAOYSA-N carbon dioxide;propan-2-one Chemical compound O=C=O.CC(C)=O RBHJBMIOOPYDBQ-UHFFFAOYSA-N 0.000 description 2
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- XCAUINMIESBTBL-UHFFFAOYSA-N lead(ii) sulfide Chemical compound [Pb]=S XCAUINMIESBTBL-UHFFFAOYSA-N 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229910052683 pyrite Inorganic materials 0.000 description 2
- 239000011028 pyrite Substances 0.000 description 2
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 229910000619 316 stainless steel Inorganic materials 0.000 description 1
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- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 229910052951 chalcopyrite Inorganic materials 0.000 description 1
- DVRDHUBQLOKMHZ-UHFFFAOYSA-N chalcopyrite Chemical compound [S-2].[S-2].[Fe+2].[Cu+2] DVRDHUBQLOKMHZ-UHFFFAOYSA-N 0.000 description 1
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010442 halite Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
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- 238000005498 polishing Methods 0.000 description 1
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- 235000002639 sodium chloride Nutrition 0.000 description 1
- 229910052950 sphalerite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- WGPCGCOKHWGKJJ-UHFFFAOYSA-N sulfanylidenezinc Chemical compound [Zn]=S WGPCGCOKHWGKJJ-UHFFFAOYSA-N 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Engineering & Computer Science (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Sampling And Sample Adjustment (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention belongs to the field of determination of isotope composition of water in mineral inclusion, and particularly discloses an analysis system and a method for oxygen isotope composition in water without oxygen mineral inclusion, wherein one end of an inclusion burst extraction/purification separation/extract conversion system of the system is connected with a product collection and measurement system, and the other end of the inclusion burst extraction/purification separation/extract conversion system is connected with a waste treatment system; the method comprises the following steps: sampling a mineral sample; baking and vacuum degassing; bursting, extracting and purifying the mineral inclusion; water in the mineral inclusion is converted; collecting and mass spectrum measuring the conversion products; the reaction product is subjected to waste treatment. The invention solves the problems of incomplete water extraction, incomplete impurity component separation, easy oxygen isotope fractionation in the conversion process and the like in the mineral inclusion, and improves the analysis and test precision and the analysis and test efficiency.
Description
Technical Field
The invention belongs to the field of determination of isotope composition of water in mineral inclusion, and particularly relates to an analysis system and an analysis method of oxygen isotope composition in water without oxygen mineral inclusion.
Background
The determination of the oxygen isotope composition in the mineral inclusion water has very important tracing function in revealing the source, migration, evolution and ore forming process of ore deposit ore forming fluid, and provides theoretical basis for clarifying ore deposit ore forming mechanism. The water in the mineral inclusion is fully extracted, purified, fully converted and fully collected, and is a precondition for the analysis of the oxygen isotope composition in the water without the oxygen mineral inclusion.
In the aspect of water extraction in mineral inclusion, single quartz glass tube or nickel tube burst sampling or on-line direct burst extraction is basically adopted in China, and the several modes have respective defects: 1) The burst extraction efficiency of a single quartz glass tube is low; 2) The nickel tube bursting method is difficult to clean and can easily pollute the nickel tube due to complex substance components in minerals; 3) The on-line bursting method is to directly put minerals into an elemental analyzer, burst at high temperature, reduce glass carbon and send the minerals into an isotope mass spectrometer for analysis, the method is easy to pollute the instrument, affects the sensitivity of the instrument and equipment, and meanwhile, water in the minerals cannot be effectively separated from other oxygen-containing components. The method overcomes the problem of mutual interference of burst products, but the components of inclusion in minerals are very complex, so that the actual operation is difficult, and the water in the inclusion in the minerals is difficult to ensure to be completely transferred into an analysis instrument for analysis, thereby causing isotope fractionation and influencing analysis test results.
In the aspect of the test object, the traditional method is to convert oxygen generated by reaction and graphite into CO under the condition of high temperature 2 Mass spectrometry measurements were performed. Due to carbon presence 12 C、 13 C two isotopes participate in calculationThe measurement result needs to be corrected, and meanwhile, the conversion process is easy to cause the fractionation of the O isotope; the conversion system needs to be introduced into a glass pipeline, wherein the glass piston needs to be coated with vacuum grease periodically to ensure the sealing performance and rotation flexibility of the piston, the system is exposed to the atmosphere in the process of coating the vacuum grease, oxygen and water vapor in the air enter the system to cause pollution, and meanwhile, the vacuum sealing grease is easy to cause cross pollution due to oxygen.
In terms of purifying water in extracted mineral inclusions, liquid nitrogen-alcohol or dry ice-acetone refrigerants are mostly used in the existing laboratory to remove impurity gas components. Liquid nitrogen-alcohol is used as a refrigerant, the temperature of the refrigerant is extremely unstable and has a large range of variation, and the impurity gas components are difficult to thoroughly remove; the dry ice-acetone refrigerant is stable in temperature, but acetone is volatile and harmful to human body, and long-time contact should be avoided.
Disclosure of Invention
The invention aims to provide an analysis system and an analysis method for oxygen isotope composition in water without an oxygen-containing mineral inclusion, which solve the problems of incomplete water extraction, incomplete impurity component separation, easy oxygen isotope fractionation in the conversion process and the like of the mineral inclusion, and improve analysis test precision and analysis test efficiency.
The technical scheme for realizing the purpose of the invention comprises the following steps: an analysis system for oxygen isotope composition in water without oxygen-containing mineral inclusion, the system comprising an inclusion burst extraction/purification separation/extract conversion system, a product collection and measurement system, and a waste treatment system; one end of the inclusion burst extraction/purification separation/extract conversion system is connected with the product collection and measurement system, and the other end of the inclusion burst extraction/purification separation/extract conversion system is connected with the waste treatment system.
The inclusion burst extraction/purification separation/extract conversion system comprises a vacuum pressure gauge, a first 1/2inch stainless steel main pipe, a bromine pentafluoride reservoir tank, a second 1/2inch stainless steel main pipe, a first group of burst-extraction units, a second group of burst-extraction units, a third group of burst-extraction units and a fourth group of burst-extraction units, wherein the first 1/2inch stainless steel main pipe is connected with the bottom of the vacuum pressure gauge, and the first 1/2inch stainless steel main pipe is respectively connected with an outlet of the bromine pentafluoride reservoir tank and the second 1/2inch stainless steel main pipe; the second 1/2inch stainless steel main pipeline is 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 third group of burst-extraction units and the fourth group of burst-extraction units are connected in parallel.
A fourth 1/4inch metal valve is arranged between the bottom of the vacuum pressure gauge and the first 1/2inch stainless steel main pipeline.
An eighth 1/4inch metal valve and a ninth 1/4inch metal valve are arranged between the first 1/2inch stainless steel main pipeline and the bromine pentafluoride reservoir tank, and a seventh 1/4inch metal valve is arranged between the eighth 1/4inch metal valve and the ninth 1/4inch metal valve.
The first 1/2inch stainless steel main pipeline and the second 1/2inch stainless steel main pipeline are provided with a first 1/2inch metal valve, and the second 1/2inch stainless steel main pipeline is provided with a second 1/2inch metal valve, a third 1/2inch metal valve and a fourth 1/2inch metal valve.
The first group of burst-extraction units comprise a tenth 1/4inch metal valve, a first quartz sample burst tube assembly, an eleventh 1/4inch metal valve and a first nickel reaction tube, the top of the first quartz sample burst tube assembly is connected 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 and the other end of the eleventh 1/4inch metal valve are connected with one end of a second 1/2inch metal valve on the second 1/2inch stainless steel main pipeline; the second group of burst-extraction units comprises a twelfth 1/4inch metal valve, a second quartz sample burst tube assembly, a thirteenth 1/4inch metal valve and a second nickel reaction tube, the top of the second quartz sample burst tube assembly is connected with one end of the twelfth 1/4inch metal valve, the top of the second nickel reaction tube is connected with one end of the thirteenth 1/4inch metal valve, and the other ends 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 and one end of the third 1/2inch metal valve on the second 1/2inch stainless steel main pipeline; the third group of burst-extraction units comprise a fourteenth 1/4inch metal valve, a third quartz sample burst tube assembly, a fifteenth 1/4inch metal valve and a third nickel reaction tube, the top of the third quartz sample burst tube assembly is connected with one end of the fourteenth 1/4inch metal valve, the top of the third nickel reaction tube is connected with one end of the fifteenth 1/4inch metal valve, the other end of the fourteenth 1/4inch metal valve and the other end of the fifteenth 1/4inch metal valve are connected with the other end of the third 1/2inch metal valve and one end of the fourth 1/2inch metal valve on the second 1/2inch stainless steel main pipeline; the fourth group of burst-extraction units comprises a sixteenth 1/4inch metal valve, a fourth quartz sample burst tube assembly, a seventeenth 1/4inch metal valve and a fourth nickel reaction tube, the top of the fourth quartz sample burst tube assembly is connected with one end of the sixteenth 1/4inch metal valve, the top of the fourth nickel reaction tube is connected with 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 with the other end of the fourth 1/2inch metal valve on the second 1/2inch stainless steel main pipeline.
The conversion product collecting and measuring system comprises a second metal cold trap, a third metal cold trap, a first thermocouple vacuum gauge and a first thermocouple vacuum gaugeMolecular sieve, second->The molecular sieve, the second thermocouple vacuum gauge, the ionization vacuum gauge, the turbo molecular pump and the isotope mass spectrometer are connected, the first 1/2inch stainless steel main pipeline is connected with the inlet of the second metal cold trap, the outlet of the second metal cold trap is connected with the inlet of the third metal cold trap, and the outlet of the third metal cold trap is respectively connected with the first thermocouple vacuum gauge and the first thermocouple vacuum gauge>Molecular sieve inlet, second->The molecular sieve inlet, the ionization vacuum gauge and the air inlet end of the turbomolecular pump are connected, namely the first +.>Molecular sieve outlet, second->The molecular sieve outlets are connected with a second thermocouple vacuum gauge and an isotope mass spectrometer.
An eighteenth 1/4inch metal valve is arranged between the first 1/2inch stainless steel main pipeline and the second metal cold trap inlet, a nineteenth 1/4inch metal valve is arranged between the second metal cold trap outlet and the third metal cold trap inlet, and the third metal cold trap outlet and the first metal cold trap inletA twenty-first 1/4inch metal valve, a twenty-second 1/4inch metal valve, a third metal cold trap outlet and a second +.>A twenty-first 1/4inch metal valve and a twenty-second 1/4inch metal valve are arranged between the molecular sieve inlets, the first +. >A second thirteenth 1/4inch metal valve is arranged between the molecular sieve outlet and the second thermocouple vacuum gauge and the isotope mass spectrometer, and the second thermocouple is arranged between the molecular sieve outlet and the second thermocouple vacuum gauge>A twenty-fifth 1/4inch metal valve is arranged between the molecular sieve outlets, a twenty-first 1/4inch metal valve and a twenty-first 1/4inch metal valve are arranged between the third metal cold trap outlet and the ionization vacuum gauge and between the third metal cold trap outlet and the turbomolecular pump, the first thermocouple vacuum gauge is connected with the twenty-first 1/4inch metal valve, and the third metal cold trap outlet is connected with the first thermocouple vacuum gauge and the first one>Molecular sieve inlet, second->The molecular sieve inlet, the ionization vacuum gauge and the air inlet end of the turbomolecular pump are connected, and a second sixteen 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 comprises a rotary vane mechanical vacuum pump, a first metal cold trap, a fifth 1/4inch metal valve and a sixth 1/4inch metal valve, wherein the first 1/2inch stainless steel main pipeline is respectively connected with an inlet of the first metal cold trap and the sixth 1/4inch metal valve, an outlet of the first metal cold trap is connected with a rotary vane mechanical vacuum pump, and the sixth 1/4inch metal valve is connected with the fifth 1/4inch metal valve.
A third 1/4inch metal valve is arranged between the first 1/2inch stainless steel main pipeline and the first metal cold trap inlet, a second 1/4inch metal valve is arranged between the first metal cold trap outlet and the rotary vane type mechanical vacuum pump, and the first metal cold trap outlet and the second 1/4inch metal valve are connected with the first 1/4inch metal valve.
A quartz sample explodes and splits pipe assembly for analytic system, this quartz sample explodes and splits pipe assembly includes external screw thread stainless steel pipe, quartz explodes and splits pipe, rubber seal, sealed metal sleeve pipe and internal screw thread metal pipe hoop, and quartz explodes and splits the pipe open end and inserts in external screw thread stainless steel pipe bottom, is equipped with rubber seal between external screw thread stainless steel pipe and the quartz explodes and splits the pipe, and rubber seal bottom is equipped with sealed metal sleeve pipe, and sealed metal sleeve pipe bottom is inserted in screw thread metal pipe hoop, and rubber seal, sealed metal sleeve pipe, screw thread metal pipe hoop all overlap outside the quartz explodes the pipe.
The analysis method for the oxygen isotope composition in the oxygen-free mineral inclusion water by adopting the analysis system specifically comprises the following steps:
step 1, mineral sample injection;
step 2, baking and vacuum degassing are carried out on the whole analysis system;
Step 3, after baking and vacuum degassing of the analysis system are completed, bursting mineral inclusion bodies, and extracting and purifying bursting products;
step 4, the water in the mineral inclusion after bursting, extracting and purifying in the step 3 is converted
Step 5, collecting and measuring mass spectrum of the converted product obtained after the mineral inclusion water is converted in the step 4;
and 6, carrying out waste treatment on the residual reagent and the reaction product in the step 3 and the step 4.
The step 1 specifically comprises the following steps: closing a tenth 1/4inch metal valve, an eleventh 1/4inch metal valve, a twelfth 1/4inch metal valve, a thirteenth 1/4inch metal valve, a fourteenth 1/4inch metal valve, a fifteenth 1/4inch metal valve, a sixteenth 1/4inch metal valve and a seventeenth 1/4inch metal valve, removing the first quartz sample explosion tube assembly, the second quartz sample explosion tube assembly, the third quartz sample explosion tube assembly and the fourth quartz sample explosion tube assembly, respectively loading the treated mineral sample particles into the first quartz sample explosion tube assembly, the second quartz sample explosion tube assembly, the third quartz sample explosion tube assembly and the fourth quartz sample explosion tube assembly, and respectively connecting the first quartz sample explosion tube assembly, the second quartz sample explosion tube assembly, the third quartz sample explosion tube assembly and the fourth quartz sample explosion tube assembly with the tenth 1/4inch metal valve, the twelfth 1/4inch metal valve, the sixteenth 1/4inch metal valve and the sixteenth 1/4inch metal valve through a 1/4inch stainless steel wire to finish sample injection operation.
The step 2 specifically comprises the following steps: respectively sleeving the first quartz sample bursting tube assembly, the first nickel reaction tube, the second quartz sample bursting tube assembly, the second nickel reaction tube, the third quartz sample bursting tube assembly, the third nickel reaction tube, the fourth quartz sample bursting tube assembly and the fourth nickel reaction tube outside a digital temperature control heating furnace, and sequentially and slowly opening a tenth 1/4inch metal valve, an eleventh 1/4inch metal valve and a twelfth 1/4inch gold valveThe method comprises the steps of connecting a rotary-vane type mechanical vacuum pump to the analysis system to pump low vacuum, opening an eighteenth 1/4inch metal valve and a nineteenth 1/4inch metal valve, and adjusting the temperature of a digital temperature control heating furnace according to the properties of a mineral sample; after the heating belt power supply is turned on to heat and dehumidify the whole analysis system for 30min, a third 1/4inch metal valve is turned off; sleeving a liquid nitrogen cup on the second metal cold trap and the third metal cold trap, opening a twenty-first 1/4inch metal valve, a twenty-second first 1/4inch metal valve, a twenty-third first 1/4inch metal valve, a twenty-fourth first 1/4inch metal valve, a twenty-third first 1/4inch metal valve and a twenty-fourth first 1/4inch metal valve, connecting a turbo molecular pump to carry out high vacuum pumping on the analysis system, and monitoring that the high vacuum degree of the analysis system reaches 10 through an ionization vacuum meter -5 And continuously pumping for 30min after Pa.
The specific steps of bursting the mineral inclusion in the step 3 are as follows: after the analysis system is subjected to vacuum degassing, the first quartz sample bursting tube assembly, the second quartz sample bursting tube assembly, the third quartz sample bursting tube assembly, the fourth quartz sample bursting tube assembly, and the first nickel reaction tube, the second nickel reaction tube, the third nickel reaction tube and the fourth nickel reaction tube are sleeved with circulating water, a tenth 1/4inch metal valve, a twelfth 1/4inch metal valve, a fourteenth 1/4inch metal valve and a sixteenth 1/4inch metal valve are closed, the bursting temperature of the digital temperature control heating furnace is adjusted according to the properties of mineral samples, the bursting time is 30min, and the bursting of mineral inclusion is completed.
The specific steps of extracting the burst product of the mineral inclusion in the step 3 are as follows: after bursting is finished, the temperature control heating furnaces outside the first nickel reaction tube, the second nickel reaction tube, the third nickel reaction tube and the fourth nickel reaction tube are removed, liquid nitrogen cups are sleeved outside the 4 nickel reaction tubes to fully freeze, the second 1/2inch metal valve, the third 1/2inch metal valve and the fourth 1/2inch metal valve are closed in sequence, 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 opened respectively, and mineral inclusion burst products are automatically transferred and diffused into the first nickel reaction tube, the second nickel reaction tube, the third nickel reaction tube and the fourth nickel reaction tube corresponding to the first nickel reaction tube, the second nickel reaction tube and the third nickel reaction tube; and closing 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 after 20 minutes to finish the extraction of the burst product.
The specific steps of purifying the mineral inclusion burst product in the step 3 are as follows: after removing the liquid nitrogen cups outside the first nickel reaction tube, the second nickel reaction tube, the third nickel reaction tube and the fourth nickel reaction tube, sleeving dry ice-alcohol mixed refrigerant outside the 4 nickel reaction tubes for purifying the burst extract for 20min, sequentially opening a second 1/2inch metal valve, a third 1/2inch metal valve and a fourth 1/2inch metal valve to pump away impurity components in the burst product, and closing an eleventh 1/4inch metal valve, a thirteenth 1/4inch metal valve, a fifteenth 1/4inch metal valve and a seventeenth 1/4inch metal valve to finish the purification of the burst product.
The specific steps of the step 4 are as follows: closing the eighth 1/4inch metal valve and the eighteenth 1/4inch metal valve, opening the ninth 1/4inch metal valve 14, and slowly opening the eighth 1/4inch metal valve to obtain BrF in the bromine pentafluoride reservoir tank 5 The reagent is diffused into the first 1/2inch stainless steel main pipeline and the second 1/2inch stainless steel main pipeline; monitoring of BrF diffusion into first and second 1/2inch stainless steel main pipes by vacuum pressure gauge 6 5 The pressure value of the reagent and the BrF required for the reaction 5 Transferring the reagent into a frozen first nickel reaction tube, a frozen second nickel reaction tube, a frozen third nickel reaction tube and a frozen fourth nickel reaction tube in sequence; removing 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 re-putting the dry ice-alcohol refrigerant in the first nickel reaction tube, the second nickel reaction tube and the first nickel reaction tubeThe outside of the three-nickel reaction tube and the fourth nickel reaction tube are sleeved with a digital temperature control heating furnace, the temperature of the digital temperature control heating furnace is regulated to 300 ℃, and the digital temperature control heating furnace is heated for 20min, and the water and BrF in the first nickel reaction tube, the second nickel reaction tube, the third nickel reaction tube and the fourth nickel reaction tube 5 The reagent completely releases O 2 。
The specific steps of collecting the mineral inclusion conversion products in the step 5 are as follows: and removing the temperature control heating furnaces outside the first nickel reaction tube, the second nickel reaction tube, the third nickel reaction tube and the fourth nickel reaction tube, and sleeving liquid nitrogen cups outside the first nickel reaction tube, the second nickel reaction tube, the third nickel reaction tube and the fourth nickel reaction tube again. Closing an eighth 1/4inch metal valve, a fourth 1/4inch metal valve, an eighteenth 1/4inch metal valve, a nineteenth 1/4inch metal valve, a twenty 1/4inch metal valve twenty-first 1/4inch metal valves, slowly opening an eleventh 1/4inch metal valve on the first nickel reaction tube to enable O generated in the first nickel reaction tube 2 Slowly releasing the first 1/2inch stainless steel main pipeline and the second 1/2inch stainless steel main pipeline; sequentially and slowly opening an eighteenth 1/4inch metal valve, a nineteenth 1/4inch metal valve and a twentieth 1/4inch metal valve, and monitoring the reaction to generate O by a first thermocouple vacuum gauge 2 Is a pressure of (1); opening a twenty-second 1/4inch metal valve to make the firstThe molecular sieve is fully frozen and collected by liquid nitrogen to obtain O in the first nickel reaction tube 2 After that, the twenty-second 1/4inch metal valve is closed and the first +.>Liquid nitrogen outside the molecular sieve.
The specific steps of mass spectrometry of the mineral inclusion transformation product in the step 5 are as follows: opening a thirteenth 1/4inch metal valve, and monitoring the first through a second thermocouple vacuum gaugeRelease of O after thawing of molecular sieves 2 Pressure of O 2 Diffusion into isotope mass spectrometer for isotope measurement, and opening twenty-fourth 1/4inch metal valve to obtain O in second nickel reaction tube 2 Collect in second +.>In the molecular sieve, removing liquid nitrogen to open a twenty-five 1/4inch metal valve, and monitoring the thawing of the molecular sieve by a second thermocouple vacuum gauge to release O 2 Pressure of O 2 The mixture is diffused into an isotope mass spectrometer to carry out isotope measurement, and O in the rest nickel reaction tubes is completed according to the same operation method 2 Collecting and measuring.
The specific steps of the step 6 are as follows: closing an eighteenth 1/4inch metal valve, a fourth 1/4inch metal valve, a first 1/4inch metal valve and a second 1/4inch metal valve, sleeving liquid nitrogen on the outer sleeve of the first metal cold trap, detaching a first quartz sample explosion tube assembly, a second quartz sample explosion tube assembly, a third quartz sample explosion tube assembly and a fourth quartz sample explosion tube assembly, and a cooling water system outside the first nickel reaction tube, the second nickel reaction tube, the third nickel reaction tube and the fourth nickel reaction tube, sleeving a temperature control heating furnace outside the first nickel reaction tube, the second nickel reaction tube, the third nickel reaction tube and the fourth nickel reaction tube again, and adjusting the temperature control heating furnace to 150 ℃ to heat the 4 nickel reaction tubes (29, 31, 33 and 35); opening 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 in sequence after opening the third 1/4inch metal valve, and transferring waste in the 4 nickel reaction pipes (29, 31, 33, 35) to the first metal cold trap; closing the first 1/2inch metal valve, opening the fifth 1/4inch metal valve and the sixth 1/4inch metal valve, removing liquid nitrogen outside the first metal cold trap, opening the first 1/4inch metal valve, carrying waste into a lime bucket in a fume hood communicated with a pipeline on the left side of the first 1/4inch metal valve by Ar gas, and completing waste disposal.
The beneficial technical effects of the invention are as follows: according to the invention, a design that a plurality of quartz glass tubes are respectively loaded with different samples to be analyzed is adopted, each quartz glass tube is connected with one nickel reaction tube to form a set of bursting, extracting and purifying units, each set of units are separated by a metal valve, and the high-temperature bursting, product extracting and purifying operation of minerals can be independently completed, so that the analysis efficiency is greatly improved; the quartz glass tube filled with the sample is hermetically connected with the analysis system by adopting an O-shaped rubber ring and stainless steel spiral clamp combination mode, so that the vacuum degree of the analysis system can be effectively maintained, the quartz sample tube is convenient to clean and replace, and meanwhile, the interference of oxygen-containing components caused by using vacuum sealing grease can be avoided; by usingThe molecular sieve directly collects oxygen generated by reaction under the condition of full freezing of liquid nitrogen for mass spectrometry measurement, so that the problem that a measurement result needs to be corrected due to the introduction of graphite in the traditional method is avoided, the defect that a glass piston is regularly smeared with vacuum lubricating grease to expose an analysis system to the atmosphere is overcome, and meanwhile, cross contamination caused by using oxygen-containing vacuum sealing grease is avoided; the turbo molecular pump with the rotary vane type mechanical pump as the front stage is used as a high vacuum pump group of the analysis system, so that the whole analysis system is ensured to reach higher vacuum degree, and the influence of oxygen-containing gas in the air on the experimental process is further reduced; the digital temperature control heating furnace is adopted as the external heating equipment of the quartz glass tube and the nickel reactor, so that the burst temperature and the reaction temperature can be accurately controlled; experiments show that the dry ice-alcohol mixed solution has the characteristics of stable temperature, strong controllability and no human body hazard, can thoroughly freeze the water separated out by burst of mineral inclusion as a purification refrigerant, can effectively separate and remove impurity components, and avoids the fractionation of oxygen isotopes and the interference of other oxygen-containing impurity gases caused by incomplete extraction of water in the inclusion.
Drawings
FIG. 1 is a schematic diagram of an analysis system for oxygen isotope composition in water without oxygen mineral inclusion provided by the invention;
FIG. 2 is a schematic structural diagram of a quartz sample cracking tube assembly according to the present invention;
in the figure: 1 is a first 1/4inch metal valve, 2 is a second 1/4inch metal valve, 3 is a rotary vane mechanical vacuum pump, 4 is a first metal cold trap, 5 is a third 1/4inch metal valve, 6 is a vacuum pressure gauge, 7 is a fourth 1/4inch metal valve, 8 is a first 1/2inch stainless steel main pipe, 9 is a fifth 1/4inch metal valve, 10 is a sixth 1/4inch metal valve, 11 is a seventh 1/4inch metal valve, 12 is an eighth 1/4inch metal valve, 13 is a first 1/2inch metal valve, 14 is a ninth 1/4inch metal reservoir tank, 15 is a bromine pentafluoride tank, 16 is a second 1/2inch metal valve, 17 is a third 1/2inch metal valve, 18 is a fourth 1/2inch metal valve, 19 is a second 1/2inch stainless steel main pipe, 20 is a tenth 1/4inch metal valve, 21 is an eleventh 1/4inch metal valve, 22 is a twelfth 1/4inch metal valve, 23 is a thirteenth 1/4inch metal valve, 24 is a fourteenth 1/4inch metal valve, 25 is a fifteenth 1/4inch metal valve, 26 is a sixteenth 1/4inch metal valve, 27 is a seventeenth 1/4inch metal valve, 28 is a first quartz sample detonation tube assembly, 29 is a first nickel reaction tube, 30 is a second quartz sample detonation tube assembly, 31 is a second nickel reaction tube, 32 is a third quartz sample detonation tube assembly, 33 is a third nickel reaction tube, 34 is a fourth quartz sample detonation tube assembly, 35 is a fourth nickel reaction tube, 36 is an eighteenth 1/4inch metal valve, 37 is a second metal cold trap, 38 is a nineteenth 1/4inch metal valve, 39 is a third metal cold trap, 40 is a twenty 1/4inch metal valve, 41 is a first thermocouple vacuum gauge, 42 is a twenty-first 1/4inch metal valve, 43 is a twenty-second 1/4inch metal valve, 44 is a first Molecular sieve 45 is twenty-third 1/4inch metal valve, 46 is twenty-fourth 1/4inch metal valve, 47 is second +.>Molecular sieve, 48 is twenty-five 1/4inch metal valve, 49 is twenty-sixteen 1/4inch metal valve,50 is a second thermocouple vacuum gauge, 51 is an ionization vacuum gauge, 52 is a turbomolecular pump, 53 is an isotope mass spectrometer, 54 is an externally threaded stainless steel tube, 55 is a quartz sample bursting tube, 56 is a rubber sealing ring, 57 is a sealing metal sleeve, and 58 is an internally threaded metal pipe hoop.
Detailed Description
The invention is described in further detail below with reference to the drawings and examples.
As shown in fig. 1, an analysis system for oxygen isotope composition in oxygen-free mineral inclusion water includes an inclusion burst extraction/purification separation/extract conversion system, a product collection and measurement system, and a waste treatment system.
As shown in fig. 1, 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, a first 1/2inch metal valve 13, a ninth 1/4inch metal valve 14, a bromine pentafluoride reservoir tank 15, a second 1/2inch metal valve 16, a third 1/2inch metal valve 17, a fourth 1/2inch metal valve 18, a second 1/2inch stainless steel main pipe 19, a first group of burst-extraction units, a second group of burst-extraction units, a third group of burst-extraction units, and a fourth group of burst-extraction units. The bottom of the vacuum pressure gauge 6 is connected with the first 1/2inch stainless steel main pipeline 8 by welding through a 1/4inch stainless steel pipe, a fourth 1/4inch metal valve 7 is arranged between the vacuum pressure gauge 6 and the first 1/2inch stainless steel main pipeline 8, and the opening and closing of the vacuum pressure gauge 6 are controlled through the fourth 1/4inch metal valve 7. The left side of the 1/2inch stainless steel vertical main pipeline 8 is welded with three parallel pipelines on the left side of the 1/2inch stainless steel vertical main pipeline 8, an eighth 1/4inch metal valve 12 is arranged on one side of a transverse pipeline adjacent to the first 1/2inch stainless steel main pipeline 8, a seventh 1/4inch metal valve 11 is arranged on the other side of the transverse pipeline, the seventh 1/4inch metal valve 11 controls an external bromine pentafluoride steel bottle to be connected with the whole analysis system, and the eighth 1/4inch metal valve 12 controls bromine pentafluoride in a bromine pentafluoride reservoir tank 15 to enter the analysis system pipeline; the upper part of the ninth 1/4inch metal valve 14 is connected with a transverse pipeline through a tee joint, the lower part of the ninth 1/4inch metal valve 14 is connected with the top outlet of the bromine pentafluoride reservoir tank 15 through a pipeline, and the ninth 1/4inch metal valve 14 controls the opening and closing of the bromine pentafluoride reservoir tank 15. The bottom of the first 1/2inch stainless steel main pipeline 8 is welded with the middle part of the second 1/2inch stainless steel main pipeline 19, and the two pipelines are mutually perpendicular; the first 1/2inch stainless steel main pipeline 8 is provided with a first 1/2inch metal valve 13 adjacent to the two 1/2inch stainless steel main pipelines 19, and the second 1/2inch stainless steel main pipeline 19 is provided with a second 1/2inch metal valve 16, a third 1/2inch metal valve 17 and a fourth 1/2inch metal valve 18. The first set of burst-extraction units includes a tenth 1/4inch metal valve 20, a first quartz sample burst tube assembly 28, an eleventh 1/4inch metal valve 21, and a first nickel reaction tube 29, the second set of burst-extraction units includes a twelfth 1/4inch metal valve 22, a second quartz sample burst tube assembly 30, a thirteenth 1/4inch metal valve 23, and a second nickel reaction tube 31, the third set of burst-extraction units includes a fourteenth 1/4inch metal valve 24, a third quartz sample burst tube assembly 32, a fifteenth 1/4inch metal valve 25, and a third nickel reaction tube 33, and the fourth set of burst-extraction units includes a sixteenth 1/4inch metal valve 26, a fourth quartz sample burst tube assembly 34, a seventeenth 1/4inch metal valve 27, and a fourth nickel reaction tube 35. The second 1/2inch metal valve 16 controls the first set of burst-extraction units, the third 1/2inch metal valve 17 controls the second set of burst-extraction units, the fourth 1/2inch metal valve 18 controls the third and fourth sets of burst-extraction units, 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 are each welded upwardly to the second 1/2inch stainless steel main pipe 19 by a 1/4inch stainless steel pipeline. The first quartz sample bursting tube 28, the second quartz sample bursting tube 30, the third quartz sample bursting tube 32 and the fourth quartz sample bursting tube 34 are sealed by adopting O-shaped rubber rings (see figure 2), the top outlet of the first quartz sample bursting tube assembly 28 is upwards connected with the tenth 1/4inch metal valve 20 by adopting a metal cutting sleeve through a 1/4inch stainless steel pipeline, the top outlet of the second quartz sample bursting tube assembly 30 is upwards connected with the twelfth 1/4inch metal valve 22 by adopting a metal cutting sleeve through a 1/4inch stainless steel pipeline, the top outlet of the third quartz sample bursting tube assembly 32 is upwards connected with the fourteenth 1/4inch metal valve 24 by adopting a metal cutting sleeve through a 1/4inch stainless steel pipeline, and the top outlet of the fourth quartz sample bursting tube assembly 34 is upwards connected with the sixteenth 1/4inch metal valve 26 by adopting a metal cutting sleeve 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 mode, and outlets at the tops of 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 respectively connected with an eleventh 1/4inch metal valve 21, a thirteenth 1/4inch metal valve 23, a fifteenth 1/4inch metal valve 25 and a seventeenth 1/4inch metal valve 27 by adopting metal cutting sleeves through 1/4inch stainless steel wires.
The product collection and measurement system comprises an eighteenth 1/4inch metal valve 36, a second metal cold trap 37, a nineteenth 1/4inch metal valve 38, a third metal cold trap 39, a twentieth 1/4inch metal valve 40, a first thermocouple vacuum gauge 41, a twenty first 1/4inch metal valve 42, a twenty second 1/4inch metal valve 43, a firstMolecular sieve 44, twenty-third 1/4inch metal valve 45, twenty-fourth 1/4inch metal valve 46, second +.>A molecular sieve 47, a twenty-fifth 1/4inch metal valve 48, a twenty-first 1/4inch metal valve 49, a second thermocouple vacuum gauge 50, an ionization vacuum gauge 51, a turbo molecular pump 52, and an isotope mass spectrometer 53. The right side of the 1/2inch stainless steel vertical main pipeline 8 is connected with one end of an eighteenth 1/4inch metal valve 36 through a pipeline, the other end of the eighteenth 1/4inch metal valve 36 is connected with an inlet of a second metal cold trap 37 through a pipeline, an outlet of the second metal cold trap 37 is connected with one end of a nineteenth 1/4inch metal valve 38 through a pipeline, the other end of the nineteenth 1/4inch metal valve 38 is connected with an inlet of a third metal cold trap 39 through a pipeline, and a thirdThe outlet of the metal cold trap 39 is connected with one end of a twenty-1/4 inch metal valve 40 through a pipeline; the other end of the twenty-first 1/4inch metal valve 40 is respectively connected with one end of the twenty-second 1/4inch metal valve 43 and one end of the twenty-fourth 1/4inch metal valve 46 through a 1/4inch stainless steel pipe line, and the top end of the first thermocouple vacuum gauge 41 and one end of the twenty-first 1/4inch metal valve 42 are respectively connected with the 1/4inch stainless steel pipe line at the other end of the twenty-first 1/4inch metal valve 40 through a tee joint; the first thermocouple vacuum gauge 41 monitors the gas pressure of oxygen generated by the reaction, and the twenty-first 1/4inch metal valve 42 is connected with the ionization vacuum gauge 51 for monitoring the high vacuum degree of the system; the other end of the twenty-second 1/4inch metal valve 43 is connected with one end of a twenty-third 1/4inch metal valve 45 through a 1/4inch stainless steel pipeline for collecting the first +. >The inlet of the molecular sieve 44 is connected with the 1/4inch stainless steel pipeline through a tee joint; the other end of the twenty-fourth 1/4inch metal valve 46 is respectively connected with one end of the twenty-fifth 1/4inch metal valve 48 and the second +.>Inlet connections of molecular sieve 47; 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 connected with a double-way sample injection system of an isotope mass spectrometer 53 through a 1/4inch stainless steel pipeline, a second thermocouple vacuum gauge 50 is connected with the 1/4inch stainless steel pipeline through a tee joint, and the second thermocouple vacuum gauge 50 monitors the pressure of the unfreezing molecular sieve to release oxygen; the other end of the twenty-first 1/4inch metal valve 42 is connected with the air inlet end of the turbomolecular pump 52 through a 1/4inch stainless steel pipeline, the top end of the ionization vacuum gauge 51 is connected with the 1/4inch stainless steel pipeline through a tee joint, the twenty-first 1/4inch metal valve 49 is connected with the 1/4inch stainless steel pipeline upwards through a tee joint, and the twenty-first 1/4inch metal valve 49 is connected with the 1/4inch stainless steel pipeline connected with the isotope mass spectrometer 53 downwards through a tee joint; the turbo molecular pump 52 with the rotary vane mechanical pump as the front stage is the whole analysis systemThe system provides a high vacuum.
The waste treatment system comprises a first 1/4inch metal valve 1, a second 1/4inch metal valve 2, a rotary vane mechanical vacuum pump 3, a first metal cold trap 4, a third 1/4inch metal valve 5, a fifth 1/4inch metal valve 9 and a sixth 1/4inch metal valve 10. One end of a first 1/4inch metal valve 1 is connected with a waste pipeline, the other end of the first 1/4inch metal valve 1 is connected with an outlet of a first metal cold trap 4 through a 1/4inch stainless steel pipeline, one end of a second 1/4inch metal valve 2 is connected with the 1/4inch stainless steel pipeline through a tee joint, and an inlet of the first metal cold trap 4 is connected with one end of a third 1/4inch metal valve 5 through a 1/4inch stainless steel pipeline; the other end of the third 1/4inch metal valve 5 is connected with the first 1/2inch stainless steel main pipeline 8 through a 1/4inch stainless steel pipeline, and the joint of the third 1/4inch metal valve 5 and the first 1/2inch stainless steel main pipeline is positioned 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 with an extraction opening of the mechanical vacuum pump 3 through a 1/4inch stainless steel pipeline, and the rotary-vane mechanical vacuum pump 3 is used for extracting reaction exhaust matters and simultaneously providing low vacuum for the whole analysis system. One end of the fifth 1/4inch metal valve 9 is connected with an Ar gas steel cylinder outside the system through a 1/4inch stainless steel pipeline, the other end of the fifth 1/4inch metal valve 9 is connected with one end of the sixth 1/4inch metal valve 10 through a 1/4inch stainless steel pipeline, the other end of the sixth 1/4inch metal valve 10 is connected with the first 1/2inch stainless steel main pipeline 8 through a 1/4inch stainless steel pipeline, and the sixth 1/4inch metal valve 10 is positioned between the eighteenth 1/4inch 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 together control the flow of Ar gas into the analysis system for purging exhaust.
The stainless steel pipelines are all made of 316 stainless steel materials, the inner walls of the pipelines are subjected to special polishing treatment, and the pipelines except the metal cold trap are all wound with heating belts.
The first mentionedMolecular sieve 44, second->Molecular sieve 47 was packed in a 1/2inch stainless steel tube and oxygen was collected by liquid nitrogen freezing.
An analysis method for oxygen isotope composition in water without oxygen mineral inclusion, which is carried out by adopting an analysis system for oxygen isotope composition in water without oxygen mineral inclusion as shown in figures 1 and 2, specifically comprises the following steps:
step 1, mineral sample injection
Closing 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, removing the first quartz sample explosion tube assembly 28, the second quartz sample explosion tube assembly 30, the third quartz sample explosion tube assembly 32 and the fourth quartz sample explosion tube assembly 34, respectively loading the processed mineral sample particles into the first quartz sample explosion tube assembly 28, the second quartz sample explosion tube assembly 30, the third quartz sample explosion tube assembly 32 and the fourth quartz sample explosion tube assembly 34, and screwing the first quartz sample explosion tube assembly 28, the second quartz sample explosion tube assembly 30, the third quartz sample explosion tube assembly 32 and the fourth quartz sample explosion tube assembly 34 back into the analysis system to complete the mineral sample feeding operation.
The treated mineral sample particles are such as pyrite, galena, sphalerite, fluorite, etc.
Step 2, after the mineral sample injection is completed, baking and vacuum degassing are carried out on the whole analysis system
The first quartz sample bursting tube assembly 28, the first nickel reaction tube 29, the second quartz sample bursting tube assembly 30, the second nickel reaction tube 31, the third quartz sample bursting tube assembly 32, the third nickel reaction tube 33, the fourth quartz sample bursting tube assembly 34 and the fourth nickel reaction tube 35 are respectively sleeved with a digital temperature control heating furnace, and a tenth 1/4inch metal valve 20, an eleventh 1/4inch metal valve 21, a twelfth 1/4inch metal valve 22, a thirteenth 1/4inch metal valve 23 and a fourteenth are slowly opened in sequenceA 1/4inch metal valve 24, a fifteenth 1/4inch metal valve 25, a sixteenth 1/4inch metal valve 26, a seventeenth 1/4inch metal valve 27, a second 1/2inch metal valve 16, a third 1/2inch metal valve 17, a fourth 1/2inch metal valve 18, a first 1/2inch metal valve 13, an eighth 1/4inch metal valve 12, a fourth 1/4inch metal valve 7, and a third 1/4inch metal valve 5. After a liquid nitrogen cup is sleeved outside the first metal cold trap 4, a second 1/4inch metal valve 2 is slowly opened, a rotary-vane mechanical vacuum pump 3 is connected to pump low vacuum for the analysis system, an eighteenth 1/4inch metal valve 36 and a nineteenth 1/4inch metal valve 38 are opened, and the temperature of the digital temperature control heating furnace is regulated according to the properties of mineral samples; and simultaneously, a heating belt power supply is turned on to heat and dehumidify the whole analysis system for 30min, and then the third 1/4inch metal valve 5 is turned off. Sleeving a liquid nitrogen cup on the second metal cold trap 37 and the third metal cold trap 39, opening a twenty-first 1/4inch metal valve 40, a twenty-second 1/4inch metal valve 43, a twenty-third 1/4inch metal valve 45, a twenty-fourth 1/4inch metal valve 46, a twenty-fifth 1/4inch metal valve 48, a twenty-first 1/4inch metal valve 49 and a twenty-first 1/4inch metal valve 42, switching on a turbo molecular pump 52 to apply high vacuum to the analysis system, and monitoring that the high vacuum degree of the analysis system reaches 10 by an ionization vacuum gauge 51 -5 And continuously pumping for 30min after Pa.
For minerals such as pyrite, chalcopyrite, galena, zinc blende, fluorite and the like, the digital temperature control heating furnace can be adjusted to 100-120 ℃ for heating and degassing, while for minerals like halite, heating and degassing are only needed to be adjusted to 40-50 ℃, and if the temperature is too high, inclusion in the minerals bursts in the degassing stage.
The meaning of the letter "LV" on the left side of the rotary-vane mechanical VACUUM pump 3 in FIG. 1 refers to a LOW VACUUM (LOW VACUUM)
Step 3, after baking and vacuum degassing of the analysis system are completed, bursting mineral inclusion, and extracting and purifying products
Step 3.1, bursting of mineral inclusions
After the analysis system is subjected to vacuum degassing, circulating water is sleeved outside the first quartz sample bursting tube assembly 28, the second quartz sample bursting tube assembly 30, the third quartz sample bursting tube assembly 32, the fourth quartz sample bursting tube assembly 34 and 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, a tenth 1/4inch metal valve 20, a twelfth 1/4inch metal valve 22, a fourteenth 1/4inch metal valve 24 and a sixteenth 1/4inch metal valve 26 are closed, the bursting temperature of the digital temperature control heating furnace is adjusted according to the properties of mineral samples, and the bursting time is 30min, so that mineral inclusion bursting is completed.
In step 3.1, the mineral inclusion exists in the mineral sample particles, the size of the inclusion is from a few micrometers to tens micrometers, and the inclusion in the mineral can burst out of the mineral by heating the mineral to a certain temperature. The inclusion component in the mineral is mainly water, sometimes contains a certain amount of carbon dioxide, hydrogen, methane and other gases, and the components of the inclusion component are different according to the types of produced deposits.
The explosion of the mineral inclusion specifically means that the inclusion in the mineral is exploded and separated from the inside of the mineral due to the pressure rise after the mineral is heated to a certain temperature.
Step 3.2, extraction of mineral inclusion burst products
After bursting, 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 removed, a liquid nitrogen cup is sleeved outside the 4 nickel reaction tubes for full freezing, 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, 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 are opened respectively, and mineral inclusion burst products are automatically transferred and diffused into 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 corresponding to the first nickel reaction tube 29, the second nickel reaction tube 31 and the third nickel reaction tube 33; after 20 minutes, 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 were closed to complete the burst product extraction.
Step 3.3 purification of mineral inclusion burst product
After 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 are rapidly removed, dry ice-alcohol mixed refrigerant is rapidly sleeved outside the 4 nickel reaction tubes to purify burst extract for 20min, the second 1/2inch metal valve 16, the third 1/2inch metal valve 17 and the fourth 1/2inch metal valve 18 are sequentially opened to remove impurity components in the burst product, and 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 are closed to finish the purification of the burst product.
The purified popping product is water, which is also the product that is required to be extracted in the analytical method.
Step 4, the water in the mineral inclusion after bursting, extracting and purifying in the step 3 is converted
Closing the eighth 1/4inch metal valve 12, the eighteenth 1/4inch metal valve 36, opening the ninth 1/4inch metal valve 14, and slowly opening the eighth 1/4inch metal valve 12 to allow the BrF in the bromine pentafluoride reservoir tank 15 5 The reagent was diffused into the first 1/2inch stainless steel main pipe 8 and the second 1/2inch stainless steel main pipe 19, and the BrF diffused into the first 1/2inch stainless steel main pipe 8 and the second 1/2inch stainless steel main pipe 19 was monitored by the vacuum pressure gauge 6 5 The pressure value of the reagent and the BrF required for the reaction 5 The reagents are sequentially transferred into 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. Removing dry ice-alcohol cryogen 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, sleeving a digital temperature control 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 again, adjusting the temperature of the digital temperature control heating furnace to 300 ℃ and heating for 20min, and mixing water and BrF 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 5 The reagent completely releases O 2 。
Step 5, converting the mineral inclusion water into O 2 Performing collection and mass spectrometry measurements
Step 5.1, mineral inclusionConversion product-O 2 Collecting
And (3) removing the temperature control heating furnaces 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 sleeving 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 again. Closing 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 first 1/4inch metal valve 40, the twenty first 1/4inch metal valve 42, the twenty second 1/4inch metal valve 43, the twenty third 1/4inch metal valve 45, the twenty fourth 1/4inch metal valve 46, the twenty first fifteenth 1/4inch metal valve 48 and the twenty first 1/4inch metal valve 49, and slowly opening the eleventh 1/4inch metal valve 21 on the first nickel reaction tube 29 to enable O generated in the first nickel reaction tube 29 2 Slowly released into the first 1/2inch stainless steel main pipe 8 and the second 1/2inch stainless steel main pipe 19. The eighteenth 1/4inch metal valve 36, the nineteenth 1/4inch metal valve 38 and the twentieth 1/4inch metal valve 40 are opened slowly in this order, and the reaction is monitored by a first thermocouple vacuum gauge 41 to produce O 2 Is a pressure of (1); opening the twenty-second 1/4inch metal valve 43 to make the firstMolecular sieve 44 is frozen sufficiently with liquid nitrogen to collect O in first nickel reaction tube 29 2 After that, the twenty-second 1/4inch metal valve 43 is closed, and the first +.>Liquid nitrogen outside of molecular sieve 44; closing the eleventh 1/4inch metal valve 21, opening the eleventh 1/4inch metal valve 42, and switching on the turbomolecular pump 52 to apply high vacuum to the first 1/2inch stainless steel main pipeline 8 and the second 1/2inch stainless steel main pipeline 19 to 10 -5 After Pa, all valves are closed.
Step 5.2, mineral inclusion conversion product-O 2 Mass spectrometry measurements
The thirteenth 1/4inch metal valve 45 is opened and the first thermocouple vacuum gauge 50 is used to monitorRelease of O after thawing molecular sieve 44 2 Pressure of O 2 Diffusion into isotope mass spectrometer 53 for isotope measurement, after measurement, twenty-sixth 1/4inch metal valve 49 is opened, turbomolecular pump 52 is turned on for first +. >Molecular sieve 44 is evacuated to a vacuum of 10 -5 Pa, closing the twenty-third 1/4inch metal valve 45 and the twenty-sixth 1/4inch metal valve 49; opening thirteenth 1/4inch metal valve 23 opening twenty-fourth 1/4inch metal valve 46 according to step 5.1 operation can be used to open O in second nickel reaction tube 31 2 Collect in second->In the molecular sieve 47, the twenty-four 1/4inch metal valve 46 is closed, the second +.>Liquid nitrogen outside the molecular sieve 47, a second fifteen 1/4inch metal valve 48 is opened and a second thermocouple vacuum gauge 50 is used to monitor second +.>Release of O after thawing molecular sieve 47 2 Pressure of O 2 Diffusion into an isotope mass spectrometer 53 for isotope measurement; o in the third nickel reaction tube 33 and the fourth nickel reaction tube 35 can be completed according to the operation method in the step 5.1 and the step 5.2 2 Collecting and measuring.
Step 6, waste treatment is carried out on the residual reagent and the reaction product in the step 3 and the step 4
O 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 2 After collection and measurement are completed, the residual reagent and reaction products in the nickel reactor are subjected to innocent treatment, and the specific steps are as follows:
a first nickel reaction tube 29, a second nickel reaction tube 31,The residual reagents in the third nickel reaction tube 33 and the fourth nickel reaction tube 35 are mainly BrF which is not completely reacted 5 Reagents, residual reaction products are BrF 3 HF, HBr, etc.
Closing an eighteenth 1/4inch metal valve 36, a fourth 1/4inch metal valve 7, a first 1/4inch metal valve 1 and a second 1/4inch metal valve 2, sleeving liquid nitrogen on the outer sleeve of the first metal cold trap 4, detaching a first quartz sample bursting tube assembly 28, a second quartz sample bursting tube assembly 30, a third quartz sample bursting tube assembly 32, a fourth quartz sample bursting tube assembly 34 and a 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, sleeving a temperature control 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, adjusting the temperature control heating furnace to 150 ℃, and heating the 4 nickel reaction tubes 29, 31, 33 and 35; after opening the third 1/4inch metal valve 5, the eleventh 1/4inch metal valve 21, thirteenth 1/4inch metal valve 23, fifteenth 1/4inch metal valve 25 and seventeenth 1/4inch metal valve 27 are sequentially opened, and the waste in the 4 nickel reaction tubes 29, 31, 33, 35 is transferred to the first metal cold trap 4. Closing the first 1/2inch metal valve 13, opening the fifth 1/4inch metal valve 9 and the sixth 1/4inch metal valve 10, removing liquid nitrogen outside the first metal cold trap 4, opening the first 1/4inch metal valve 1, carrying waste into a lime bucket in a fume hood communicated with a pipeline on the left side of the first 1/4inch metal valve 1 by Ar gas, and completing waste disposal to avoid environmental pollution.
As shown in fig. 2, the first quartz sample bursting tube assembly 28, the second quartz sample bursting tube assembly 30, the third quartz sample bursting tube assembly 32 and the fourth quartz sample bursting tube assembly 34 have the same structure, the 4 quartz sample bursting tube sets comprise an external thread stainless steel tube 54, a quartz bursting tube 55, an O-shaped rubber seal ring 56, an annular plane sealing metal sleeve 57 and an internal thread metal tube hoop 58, the open end of the quartz bursting tube 55 is inserted into the bottom of the external thread stainless steel tube 54, an O-shaped rubber seal ring 56 is arranged between the external thread stainless steel tube 54 and the quartz bursting tube 55, an annular plane sealing metal sleeve 57 is arranged at the bottom of the O-shaped rubber seal ring 56, the bottom of the annular plane sealing metal sleeve 57 is inserted into the thread metal tube hoop 58, and the O-shaped plane sealing metal sleeve 57 and the thread metal tube hoop 58 are sleeved outside the quartz bursting tube 55.
During assembly, the quartz sample explosion tube 55 extends into the externally threaded stainless steel tube 54, and the annular plane sealing metal sleeve 57 is pushed by rotating the internally threaded metal tube hoop 58 to extrude the O-shaped rubber sealing ring 56, so that the sealing transitional connection between the quartz sample explosion tube 55 and the externally threaded stainless steel tube 54 is realized. The top external threaded rod of the external threaded stainless steel pipe 54 is connected with the metal valve through a 1/4inch stainless steel pipeline.
The inside of the externally threaded stainless steel pipe 54 is polished, and the tail end is designed by adopting a wedge-shaped section. The quartz bursting tube 55 and the external thread stainless steel tube 54 are in sealing transitional connection through elastic deformation of an O-shaped rubber sealing ring 56.
The present invention has been described in detail with reference to the drawings and the embodiments, but the present invention is not limited to the embodiments described above, and various changes can be made within the knowledge of those skilled in the art without departing from the spirit of the present invention. The invention may be practiced otherwise than as specifically described.
Claims (16)
1. An analysis system for oxygen isotope composition in water without oxygen mineral inclusion, which is characterized in that: the system comprises an inclusion burst extraction/purification separation/extract conversion system, a product collection and measurement system, and a waste treatment system; one end of the inclusion burst extraction/purification separation/extract conversion system is connected with the product collection and measurement system, and the other end of the inclusion burst extraction/purification separation/extract conversion system is connected with the waste treatment system; the inclusion burst extraction/purification separation/extract conversion system comprises a vacuum pressure gauge (6), a first 1/2inch stainless steel main pipe (8), a bromine pentafluoride reservoir tank (15), a second 1/2inch stainless steel main pipe (19), a first group of burst-extraction units, a second group of burst-extraction units, a third group of burst-extraction units and a fourth group of burst-extraction units, wherein the first 1/2inch stainless steel main pipe (8), the bottom of the vacuum pressure gauge (6) is connected with the first 1/2inch stainless steel main pipe (8), and the first 1/2inch stainless steel main pipe (8) is respectively connected with an outlet of the bromine pentafluoride reservoir tank (15) and the second 1/2inch stainless steel main pipe (19); the second 1/2inch stainless steel main pipeline (19) is 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 third group of burst-extraction units and the fourth group of burst-extraction units are connected in parallel; the first group of burst-extraction units comprises a tenth 1/4inch metal valve (20), a first quartz sample burst tube assembly (28), an eleventh 1/4inch metal valve (21) and a first nickel reaction tube (29), the top of the first quartz sample burst tube assembly (28) is connected with one end of the tenth 1/4inch metal valve (20), 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) and the other end of the eleventh 1/4inch metal valve (21) are connected with one end of a second 1/2inch metal valve (16) on a second 1/2inch stainless steel main pipeline (19); the second group of burst-extraction units comprises a twelfth 1/4inch metal valve (22), a second quartz sample burst tube assembly (30), a thirteenth 1/4inch metal valve (23) and a second nickel reaction tube (31), the top of the second quartz sample burst tube assembly (30) 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 other ends of the twelfth 1/4inch metal valve (22) and the thirteenth 1/4inch metal valve (23) are connected with the other end of a second 1/2inch metal valve (16) and one end of a third 1/2inch metal valve (17) on a second 1/2inch stainless steel main pipeline (19); the third group of burst-extraction units comprises a fourteenth 1/4inch metal valve (24), a third quartz sample burst tube assembly (32), a fifteenth 1/4inch metal valve (25) and a 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 top of the third nickel reaction tube (33) is connected with one end of the fifteenth 1/4inch metal valve (25), and 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 other end of the third 1/2inch metal valve (17) and one end of the fourth 1/2inch metal valve (18) on the second 1/2inch stainless steel main pipeline (19); the fourth group of burst-extraction units comprises a sixteenth 1/4inch metal valve (26), a fourth quartz sample burst tube assembly (34), a seventeenth 1/4inch metal valve (27) and a fourth nickel reaction tube (35), the top of the fourth quartz sample burst tube assembly (34) is connected with one end of the sixteenth 1/4inch metal valve (26), the top of the fourth nickel reaction tube (35) is connected with one end of the seventeenth 1/4inch metal valve (27), the other end of the sixteenth 1/4inch metal valve (26) and the other end of the seventeenth 1/4inch metal valve (27) are connected with the other end of a fourth 1/2inch metal valve (18) on the second 1/2inch stainless steel main pipeline (19); the first quartz sample bursting tube assembly (28), the second quartz sample bursting tube assembly (30), the third quartz sample bursting tube assembly (32) and the fourth quartz sample bursting tube assembly (34) are identical in structure and comprise an external thread stainless steel tube (54), a quartz bursting tube (55), a rubber sealing ring (56), a sealing metal sleeve (57) and an internal thread metal tube hoop (58), the open end of the quartz bursting tube (55) is inserted into the bottom of the external thread stainless steel tube (54), a rubber sealing ring (56) is arranged between the external thread stainless steel tube (54) and the quartz bursting tube (55), the sealing metal sleeve (57) is arranged at the bottom of the rubber sealing ring (56), the bottom of the sealing metal sleeve (57) is inserted into the thread metal tube hoop (58), and the rubber sealing ring (56), the sealing metal sleeve (57) and the thread metal tube hoop (58) are sleeved outside the quartz bursting tube (55).
2. An analysis system for oxygen isotope composition in oxygen-free mineral inclusion water according to claim 1 wherein: a fourth 1/4inch metal valve (7) is arranged between the bottom of the vacuum pressure gauge (6) and the first 1/2inch stainless steel main pipeline (8).
3. An analysis system for oxygen isotope composition in oxygen-free mineral inclusion water according to claim 2 wherein: an eighth 1/4inch metal valve (12) and a ninth 1/4inch metal valve (14) which are positioned on the same transverse pipeline are arranged between the first 1/2inch stainless steel main pipeline (8) and the bromine pentafluoride storage tank (15), one side, adjacent to the first 1/2inch stainless steel main pipeline (8), of the transverse pipeline is provided with the eighth 1/4inch metal valve (12), and the other side of the transverse pipeline is provided with the seventh 1/4inch metal valve (11).
4. An analysis system for oxygen isotope composition in oxygen-free mineral inclusion water according to claim 3 wherein: a first 1/2inch metal valve (13) is arranged between the first 1/2inch stainless steel main pipeline (8) and the second 1/2inch stainless steel main pipeline (19), and a second 1/2inch metal valve (16), a third 1/2inch metal valve (17) and a fourth 1/2inch metal valve (18) are arranged on the second 1/2inch stainless steel main pipeline (19).
5. The analysis system of oxygen isotope composition in oxygen-free mineral inclusion water of claim 4 wherein: the product collecting and measuring system comprises a second metal cold trap (37), a third metal cold trap (39), a first thermocouple vacuum gauge (41), a first 5A molecular sieve (44), a second 5A molecular sieve (47), a second thermocouple vacuum gauge (50), an ionization vacuum gauge (51), a turbo molecular pump (52) and an isotope mass spectrometer (53), wherein a first 1/2inch stainless steel main pipe (8) is connected with an inlet of the second metal cold trap (37), an outlet of the second metal cold trap (37) is connected with an inlet of the third metal cold trap (39), and an outlet of the third metal cold trap (39) is respectively connected with an inlet of the first thermocouple vacuum gauge (41), an inlet of the first 5A molecular sieve (44), an inlet of the second 5A molecular sieve (47), an ionization vacuum gauge (51) and an inlet of the turbo molecular pump (52), and an outlet of the first 5A molecular sieve (44) and an outlet of the second 5A molecular sieve (47) are respectively connected with the second thermocouple vacuum gauge (50) and the isotope mass spectrometer (53).
6. The analysis system of oxygen isotope composition in oxygen-free mineral inclusion water of claim 5 wherein: an eighteenth 1/4inch metal valve (36) is arranged between the first 1/2inch stainless steel main pipeline (8) and the inlet of the second metal cold trap (37), a nineteenth 1/4inch metal valve (38) is arranged between the outlet of the second metal cold trap (37) and the inlet of the third metal cold trap (39), a twenty-first 1/4inch metal valve (40) is arranged between the outlet of the third metal cold trap (39) and the inlet of the first 5 a molecular sieve (44), a twenty-second 1/4inch metal valve (43) is arranged between the outlet of the third metal cold trap (39) and the inlet of the second 5 a molecular sieve (47), a twenty-first/4 inch metal valve (45) is arranged between the outlet of the first 5 a molecular sieve (44) and the second thermocouple vacuum gauge (50) and the isotope mass spectrometer (53), an ionization valve (52) is arranged between the outlet of the second 5 a molecular sieve (47) and the second thermocouple vacuum gauge (50), a twenty-first metal valve (42) is arranged between the outlet of the third metal cold trap (39) and the inlet of the second 5 a molecular sieve (47), a twenty-second metal valve (52) is arranged between the outlet of the second 5 a vacuum gauge (40) and the second vacuum gauge (53), the first thermocouple vacuum gauge (41) is connected with a twenty-first 1/4inch metal valve (40), and a twenty-first 1/4inch metal valve (49) is arranged between the ionization vacuum gauge (51), the turbomolecular pump (52), the second thermocouple vacuum gauge (50) and the isotope mass spectrometer (53).
7. An analysis system for oxygen isotope composition in oxygen-free mineral inclusion water in accordance with claim 6 wherein: the waste treatment system comprises a rotary vane mechanical vacuum pump (3), a first metal cold trap (4), a fifth 1/4inch metal valve (9) and a sixth 1/4inch metal valve (10), wherein a first 1/2inch stainless steel main pipeline (8) is respectively connected with an inlet of the first metal cold trap (4) and the sixth 1/4inch metal valve (10), an outlet of the first metal cold trap (4) is connected with an extraction opening of the rotary vane mechanical vacuum pump (3), and the sixth 1/4inch metal valve (10) is connected with the fifth 1/4inch metal valve (9).
8. An analysis system for oxygen isotope composition in oxygen-free mineral inclusion water in accordance with claim 7 wherein: a third 1/4inch metal valve (5) is arranged between the first 1/2inch stainless steel main pipeline (8) and the inlet of the first metal cold trap (4), a second 1/4inch metal valve (2) is arranged between the outlet of the first metal cold trap (4) and the rotary vane type mechanical vacuum pump (3), and the outlet of the first metal cold trap (4) and the second 1/4inch metal valve (2) are connected with the first 1/4inch metal valve (1).
9. A method for analysis of the composition of oxygen isotopes in water free of oxygen mineral inclusions using the analysis system according to any of claims 1 to 8, characterized in that it comprises in particular the steps of:
step 1, mineral sample injection; the step 1 specifically comprises the following steps:
closing a tenth 1/4inch metal valve (20), an eleventh 1/4inch metal valve (21), a twelfth 1/4inch metal valve (22), a thirteenth 1/4inch metal valve (23), a fourteenth 1/4inch metal valve (24), a fifteenth 1/4inch metal valve (25), a sixteenth 1/4inch metal valve (26) and a seventeenth 1/4inch metal valve (27), removing the first quartz sample explosion tube assembly (28), the second quartz sample explosion tube assembly (30), the third quartz sample explosion tube assembly (32), the fourth quartz sample explosion tube assembly (34), loading the treated mineral sample particles into the first quartz sample explosion tube assembly (28), the second quartz sample explosion tube assembly (30), the third quartz sample explosion tube assembly (32), the fourth quartz sample explosion tube assembly (34), and connecting the first quartz sample explosion tube assembly (28), the second quartz sample explosion tube assembly (30), the third quartz sample explosion tube assembly (32), the fourth quartz sample explosion tube assembly (24) to the first quartz sample explosion tube assembly (24), the sixteenth 1/4inch metal valve (24) through the sixteenth 1/4inch metal valve (24) respectively, completing mineral sample injection operation;
Step 2, baking and vacuum degassing are carried out on the whole analysis system; the step 2 specifically comprises the following steps:
the first quartz sample bursting tube assembly (28), the first nickel reaction tube (29), the second quartz sample bursting tube assembly (30), the second nickel reaction tube (31), the third quartz sample bursting tube assembly (32), the third nickel reaction tube (33), the fourth quartz sample bursting tube assembly (34) and the fourth nickel reaction tube (35) are respectively sleeved with a digital temperature control heating furnace, a tenth 1/4inch metal valve (20), an eleventh 1/4inch metal valve (21), a twelfth 1/4inch metal valve (22), a thirteenth 1/4inch metal valve (23), a fourteenth 1/4inch metal valve (24), a fifteenth 1/4inch metal valve (25), a sixteenth 1/4inch metal valve (26), a seventeenth 1/4inch metal valve (27), a second 1/2inch metal valve (16), a third 1/2inch metal valve (17), a fourth 1/2inch metal valve (18), a first 1/2inch metal valve (13), a fourteenth 1/4inch metal valve (13) and a fourth 1/4inch metal valve (12) are sequentially opened slowly, the vacuum pump is opened after the vacuum pump is opened on the first vacuum system (3) and the vacuum pump (4 vacuum system, opening an eighteenth 1/4inch metal valve (36) and a nineteenth 1/4inch metal valve (38), and adjusting the temperature of the digital temperature control heating furnace according to the properties of the mineral sample; after the heating belt power supply is turned on to heat and dehumidify the whole analysis system for 30min, a third 1/4inch metal valve (5) is turned off; sleeving a liquid nitrogen cup on the second metal cold trap (37) and the third metal cold trap (39), opening a twenty-first 1/4inch metal valve (40), a twenty-second first 1/4inch metal valve (43), a twenty-third first 1/4inch metal valve (45), a twenty-first 1/4inch metal valve (46), a twenty-first 1/4inch metal valve (48), a twenty-first 1/4inch metal valve (49) and a twenty-first 1/4inch metal valve (42), and connecting the turbine The molecular pump (52) pumps high vacuum to the analysis system, and the ionization vacuum gauge (51) monitors that the high vacuum degree of the analysis system reaches 10 -5 Continuously pumping for 30min after Pa;
step 3, after baking and vacuum degassing of the analysis system are completed, bursting mineral inclusion bodies, and extracting and purifying bursting products;
step 4, the water in the mineral inclusion after bursting, extracting and purifying in the step 3 is converted;
step 5, collecting and measuring mass spectrum of the converted product obtained after the mineral inclusion water is converted in the step 4;
and 6, carrying out waste treatment on the residual reagent and the reaction product in the step 3 and the step 4.
10. The method for analyzing the oxygen isotope composition in water without oxygen-containing mineral inclusion according to claim 9, wherein the specific steps of bursting the mineral inclusion in the step 3 are as follows:
after the analysis system is subjected to vacuum degassing, circulating water is sleeved outside the first quartz sample bursting tube assembly (28), the second quartz sample bursting tube assembly (30), the third quartz sample bursting tube assembly (32), the fourth quartz sample bursting tube assembly (34), 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), a tenth 1/4inch metal valve (20), a twelfth 1/4inch metal valve (22), a fourteenth 1/4inch metal valve (24) and a sixteenth 1/4inch metal valve (26) are closed, the bursting temperature of the digital temperature control heating furnace is adjusted according to the properties of mineral samples, and the bursting time is 30min, so that mineral inclusion bursting is completed.
11. The method for analyzing the oxygen isotope composition in the oxygen-free mineral inclusion water according to claim 10, wherein the specific steps of extracting the mineral inclusion burst product in the step 3 are as follows:
after bursting is finished, 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 removed, a liquid nitrogen cup is sleeved outside the 4 nickel reaction tubes for full freezing, 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, 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) are opened respectively, and mineral inclusion burst products are automatically transferred and diffused into 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) corresponding to the first nickel reaction tube, the second nickel reaction tube and the fourth nickel reaction tube; after 20min, closing a tenth 1/4inch metal valve (20), a twelfth 1/4inch metal valve (22), a fourteenth 1/4inch metal valve (24) and a sixteenth 1/4inch metal valve (26) to finish the burst product extraction.
12. The method for analyzing the oxygen isotope composition in the oxygen-free mineral inclusion water according to claim 11, wherein the specific steps of purifying the mineral inclusion burst product in the step 3 are as follows:
after 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), sleeving dry ice-alcohol mixed refrigerant outside the 4 nickel reaction tubes for purifying burst extract for 20min, sequentially opening a second 1/2inch metal valve (16), a third 1/2inch metal valve (17) and a fourth 1/2inch metal valve (18) to pump out impurity components in the burst product, and closing an eleventh 1/4inch metal valve (21), a thirteenth 1/4inch metal valve (23), a fifteenth 1/4inch metal valve (25) and a seventeenth 1/4inch metal valve (27) to finish the purification of the burst product.
13. The method for analyzing the oxygen isotope composition in water without oxygen-containing mineral inclusion according to claim 12, wherein the specific steps of the step 4 are as follows:
closing the eighth 1/4inch metal valve (12) and the eighteenth 1/4inch metal valve (36), and opening the ninth valve1/4inch metal valve 14, slowly open eighth 1/4inch metal valve (12), brF in bromine pentafluoride reservoir (15) 5 Monitoring and diffusing the reagent into a first 1/2inch stainless steel main pipeline (8) and a second 1/2inch stainless steel main pipeline (19); monitoring BrF diffused into a first 1/2inch stainless steel main pipe (8) and a second 1/2inch stainless steel main pipe (19) by a vacuum pressure gauge 6 5 The pressure value of the reagent and the BrF required for the reaction 5 The reagent is sequentially transferred into a frozen first nickel reaction tube (29), a frozen second nickel reaction tube (31), a frozen third nickel reaction tube (33) and a frozen fourth nickel reaction tube (35); removing 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), sleeving a digital temperature control 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), adjusting the temperature of the digital temperature control heating furnace to 300 ℃, heating for 20min, and mixing water and BrF 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) 5 The reagent completely releases O 2 。
14. The method for analyzing the oxygen isotope composition in the oxygen-free mineral inclusion water according to claim 13, wherein the specific steps of collecting the mineral inclusion conversion products in the step 5 are as follows:
Removing the temperature control heating furnaces 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 sleeving 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); closing 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 first 1/4inch metal valve (40), the twenty first 1/4inch metal valve (42), the twenty second 1/4inch metal valve (43), the twenty first 1/4inch metal valve (45), the twenty first second 1/4inch metal valveTwenty-fourth 1/4inch metal valve (46), twenty-fifth 1/4inch metal valve (48) and twenty-sixth 1/4inch metal valve (49), and slowly opening eleventh 1/4inch metal valve (21) on first nickel reaction tube (29) to make O generated in first nickel reaction tube (29) 2 Slowly releasing the first 1/2inch stainless steel main pipeline (8) and the second 1/2inch stainless steel main pipeline (19); sequentially and slowly opening an eighteenth 1/4inch metal valve (36), a nineteenth 1/4inch metal valve (38) and a twentieth 1/4inch metal valve (40), and monitoring the reaction to generate O by a first thermocouple vacuum gauge (41) 2 Is a pressure of (1); opening a twenty-second 1/4inch metal valve (43), and fully freezing the first 5A molecular sieve (44) with liquid nitrogen to collect O in the first nickel reaction tube (29) 2 Thereafter, the twenty-second 1/4inch metal valve is closed and liquid nitrogen outside of the first 5 a molecular sieve (44) is removed.
15. The method for analyzing the oxygen isotope composition in the oxygen-free mineral inclusion water according to claim 14, wherein the specific steps of mass spectrometry of the mineral inclusion conversion products in the step 5 are as follows:
opening a thirteenth 1/4inch metal valve (45), and monitoring the release of O after thawing the first 5A molecular sieve (44) by a second thermocouple vacuum gauge (50) 2 Pressure of O 2 Diffusion into an isotope mass spectrometer (53) for isotope measurement, and opening a twenty-fourth 1/4inch metal valve to discharge O in a second nickel reaction tube (31) in the above manner 2 Collecting in a second 5A molecular sieve (47) fully frozen by liquid nitrogen, removing the liquid nitrogen, opening a second fifteen 1/4inch metal valve (48), monitoring the molecular sieve to defrost by a second thermocouple vacuum gauge (50), and releasing O 2 Pressure of O 2 Is diffused into an isotope mass spectrometer (53) for isotope measurement, and O in the rest nickel reaction tube is completed according to the same operation method 2 Collecting and measuring.
16. The method for analyzing the oxygen isotope composition in water without oxygen-containing mineral inclusion according to claim 15, wherein the specific steps of the step 6 are as follows:
closing an eighteenth 1/4inch metal valve (36), a fourth 1/4inch metal valve (7), a first 1/4inch metal valve (1) and a second 1/4inch metal valve (2), sleeving liquid nitrogen on the first metal cold trap (4), removing a first quartz sample bursting tube assembly (28), a second quartz sample bursting tube assembly (30), a third quartz sample bursting tube assembly (32) and a fourth quartz sample bursting tube assembly (34), removing 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), sleeving a temperature control 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), and adjusting the temperature control heating furnace to 150 ℃ to heat the 4 nickel reaction tubes (29, 31, 33 and 35); opening 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) after opening the third 1/4inch metal valve (5), and transferring waste in the 4 nickel reaction pipes (29, 31, 33, 35) to the first metal cold trap (4); closing a first 1/2inch metal valve (13), opening a fifth 1/4inch metal valve (9) and a sixth 1/4inch metal valve (10), removing liquid nitrogen outside the first metal cold trap (4), opening the first 1/4inch metal valve (1), carrying waste into a lime bucket in a fume hood communicated with a pipeline on the left side of the first 1/4inch metal valve (1) by Ar gas, and completing waste disposal.
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| CN109060932A (en) * | 2018-09-13 | 2018-12-21 | 中国地质科学院矿产资源研究所 | Carbon and hydrogen isotope analysis system and method for mineral fluid inclusion |
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| CN110530702B (en) * | 2019-07-31 | 2021-11-26 | 中国地质调查局武汉地质调查中心(中南地质科技创新中心) | Water extraction system for oxygen-free mineral inclusion and application method thereof |
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