CN110031536B - Device and method for analyzing and extracting oxygen isotope composition in rock and mineral - Google Patents
Device and method for analyzing and extracting oxygen isotope composition in rock and mineral Download PDFInfo
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- CN110031536B CN110031536B CN201910359063.9A CN201910359063A CN110031536B CN 110031536 B CN110031536 B CN 110031536B CN 201910359063 A CN201910359063 A CN 201910359063A CN 110031536 B CN110031536 B CN 110031536B
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000001301 oxygen Substances 0.000 title claims abstract description 58
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 58
- 239000011435 rock Substances 0.000 title claims abstract description 28
- 229910052500 inorganic mineral Inorganic materials 0.000 title claims abstract description 27
- 239000011707 mineral Substances 0.000 title claims abstract description 27
- 239000000203 mixture Substances 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 19
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 69
- 239000010935 stainless steel Substances 0.000 claims abstract description 69
- 238000000605 extraction Methods 0.000 claims abstract description 31
- 238000004458 analytical method Methods 0.000 claims abstract description 29
- 239000002699 waste material Substances 0.000 claims abstract description 23
- 238000000746 purification Methods 0.000 claims abstract description 20
- 238000000926 separation method Methods 0.000 claims abstract 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 abstract description 13
- 238000002347 injection Methods 0.000 claims abstract description 8
- 239000007924 injection Substances 0.000 claims abstract description 8
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 7
- 238000003682 fluorination reaction Methods 0.000 claims abstract description 7
- 238000009849 vacuum degassing Methods 0.000 claims abstract description 5
- 239000002184 metal Substances 0.000 claims description 360
- 229910052751 metal Inorganic materials 0.000 claims description 360
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 86
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 62
- 238000006243 chemical reaction Methods 0.000 claims description 45
- 229910052759 nickel Inorganic materials 0.000 claims description 43
- 239000007788 liquid Substances 0.000 claims description 31
- 229910052757 nitrogen Inorganic materials 0.000 claims description 31
- 238000010438 heat treatment Methods 0.000 claims description 27
- 239000002808 molecular sieve Substances 0.000 claims description 15
- 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 14
- 238000003466 welding Methods 0.000 claims description 12
- 238000007789 sealing Methods 0.000 claims description 11
- 238000007710 freezing Methods 0.000 claims description 10
- 230000008014 freezing Effects 0.000 claims description 10
- 238000005086 pumping Methods 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 6
- 239000002912 waste gas Substances 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 5
- 239000007795 chemical reaction product Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 229910000619 316 stainless steel Inorganic materials 0.000 claims description 3
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- 239000006227 byproduct Substances 0.000 claims description 3
- 239000000498 cooling water Substances 0.000 claims description 3
- 238000003912 environmental pollution Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- 238000010408 sweeping Methods 0.000 claims description 3
- 238000010257 thawing Methods 0.000 claims description 3
- 238000009423 ventilation Methods 0.000 claims description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims 1
- 235000011941 Tilia x europaea Nutrition 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 claims 1
- 238000010168 coupling process Methods 0.000 claims 1
- 238000005859 coupling reaction Methods 0.000 claims 1
- 238000007872 degassing Methods 0.000 claims 1
- 210000002478 hand joint Anatomy 0.000 claims 1
- 239000004571 lime Substances 0.000 claims 1
- 238000005259 measurement Methods 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 5
- 238000012360 testing method Methods 0.000 abstract description 5
- 238000005194 fractionation Methods 0.000 abstract description 3
- 239000004519 grease Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000001819 mass spectrum Methods 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 150000002500 ions Chemical group 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- -1 bromine pentafluoride oxygen Chemical compound 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000012864 cross contamination Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000012025 fluorinating agent Substances 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001004 secondary ion mass spectrometry Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000006276 transfer reaction Methods 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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- General Health & Medical Sciences (AREA)
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Abstract
The invention belongs to the technical field of rock and mineral isotope composition measurement, and particularly relates to an analysis and extraction device and method for oxygen isotope composition in rock and minerals. The device comprises a waste treatment system, a first 1/2inch stainless steel vertical main pipeline and 12 sets of identical oxygen isotope sample extraction, separation, purification and collection systems; the method comprises the following steps: step 1, sample injection; step 2, baking and vacuum degassing the whole system; step 3, transferring bromine pentafluoride reagent and carrying out fluorination reaction; step 4, separating, purifying and collecting oxygen; and 5, waste treatment. The invention can solve the problem that oxygen isotope fractionation is easy to cause in the isotope sample preparation process, and improves the analysis and test precision and the analysis and test efficiency.
Description
Technical Field
The invention belongs to the technical field of rock and mineral isotope composition measurement, and particularly relates to an analysis and extraction device and method for oxygen isotope composition in rock and minerals.
Background
Determination of rock and oxygen isotope composition in minerals formation conditions and mechanisms, sources, evolution, interactions with surrounding rock, etc. can be studied. Oxygen isotope analysis has become a powerful tool for petrology and mineralogy research, 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 elucidating ore deposit ore forming mechanism. The oxygen in the rock and the mineral is fully extracted, purified and fully collected, and is a precondition for the analysis of the oxygen isotope composition in the rock and the mineral.
In the analysis of oxygen isotope composition in rock and minerals, a laser method, a secondary ion mass spectrometry and a traditional bromine pentafluoride method are basically adopted at home and abroad. These several methods of oxygen isotope composition analysis have respective drawbacks: 1) In the analysis of oxygen isotope composition by a laser method, factors such as particle size effect, system memory effect, edge effect, powder splashing and the like of a sample are easy to cause oxygen isotope fractionation, so that the analysis precision and accuracy are reduced; 2) The secondary ion mass spectrum oxygen isotope composition analysis technology has unique superiority for researching celestial body samples with large isotope composition difference, but has serious matrix effect, namely mutual interference among various scattered ions, when analyzing common rock and mineral samples, so that the analysis precision is greatly reduced; 3) In the traditional bromine pentafluoride oxygen isotope composition analysis, as the reaction products in each reactor adopt a shared analysis pipeline system, purification, conversion and collection are required one by one, so that the analysis efficiency is low. Meanwhile, in the aspect of a test object, in the traditional bromine pentafluoride method, oxygen generated by reaction and graphite are converted into CO 2 under the high-temperature condition for mass spectrum measurement, and as the carbon has 12C、13 C two isotopes to participate in calculation, the measurement result needs to be corrected, and the O isotope fractionation is easy to cause in the conversion process. In addition, 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.
Disclosure of Invention
The invention solves the technical problems that:
Aiming at the defects of the prior art, the invention provides a device and a method for analyzing and extracting oxygen isotopes in rocks and minerals, which can solve the problem that oxygen isotopes are easy to fractionate in the preparation process of isotope samples, and improve the analysis and test precision and the analysis and test efficiency.
The invention adopts the technical scheme that:
The analysis and extraction device for oxygen isotope composition in rock and minerals comprises a waste treatment system, a first 1/2inch stainless steel vertical main pipeline and 12 sets of identical oxygen isotope sample extraction, separation, purification and collection systems;
The vacuum pressure gauge is connected with a fourth 1/4inch metal valve downwards through a 1/4inch stainless steel pipe by a cutting sleeve, the lower end of the fourth 1/4inch metal valve is connected with a first 1/2inch stainless steel vertical main pipe through welding by a 1/4inch stainless steel pipe, the vertical main pipe is vertically connected with a second 1/2inch metal pipeline through welding, and the on-off of the two pipelines is controlled through the first 1/2inch metal valve;
The bromine pentafluoride steel bottle is connected with the vertical main pipeline through a 1/4inch metal pipeline through welding, a seventh 1/4inch metal valve and a ninth 1/4inch metal valve are arranged on the 1/4inch metal pipeline, a tee joint is arranged on the 1/4inch metal pipeline between the seventh 1/4inch metal valve and the ninth 1/4inch metal valve, and the tee joint is downwards connected with an eighth 1/4inch metal valve and a bromine pentafluoride reservoir tank in sequence;
The turbo molecular pump is welded and connected with a first 1/2inch stainless steel pipe through a 1/4inch stainless steel pipe, a twenty-eighth 1/4inch metal valve, an eighth metal cold trap, a twenty-ninth 1/4inch metal valve and a thirty-first 1/4inch metal valve are sequentially arranged between the first 1/2inch stainless steel pipe and the turbo molecular pump, a tee joint is arranged between the twenty-eighth 1/4inch metal valve and the eighth metal cold trap, a third tee joint is connected with a thirty-first 1/4inch metal valve through a 1/4inch metal pipe, a tee joint is arranged between the twenty-ninth 1/4inch metal valve and the thirty-first 1/4inch metal valve, and the tee joint is downwards connected with a first compound vacuum gauge.
The oxygen isotope sample extraction, separation, purification and collection system comprises a tenth 1/4inch metal valve and an eleventh 1/4inch metal valve which are welded with a second 1/2inch metal pipeline through a 1/4inch stainless steel pipeline; the first nickel reaction tube is connected with a tenth 1/4inch metal valve in a cutting sleeve sealing mode by adopting a metal thread and gasket sealing mode and a 1/4inch stainless steel pipeline upwards; the eleventh 1/4inch metal valve is connected with the second metal cold trap through a 1/4inch stainless steel pipeline, the second metal cold trap is connected with the third metal cold trap through a twelfth 1/4inch metal valve and a 1/4inch stainless steel pipeline, the two ends of the thirteenth 1/4inch metal valve are respectively connected with the third metal cold trap and the first metal hot trap through a 1/4inch stainless steel pipeline, the first metal hot trap is connected with the fourth metal cold trap through a fourteenth 1/4inch metal valve and a 1/4inch stainless steel pipeline, one end of the fifteenth 1/4inch metal valve is connected with the fourth metal cold trap, the other end of the fifteenth 1/4inch metal valve is connected with a 1/4inch tee joint, the tee joint is connected with the sixteenth 1/4inch metal valve upwards, the right hand is connected with the other 1/4inch tee joint through a 1/4inch stainless steel pipeline, the other 1/4inch tee joint is connected with one end of the seventeenth 1/4inch metal valve downwards, the right hand is connected with one end of the first VCO quick joint, the first quick joint is connected with the other end of the VCO quick joint, and the first quick joint is connected with the eighteenth quick joint through the eighteenth 1/4inch metal valveThe molecular sieve collecting pipe is connected with a 1/4inch stainless steel pipe, the other end of a seventeenth 1/4inch metal valve is downwards connected with a first capacitance vacuum gauge through a 1/4inch stainless steel pipe in a welding way, a sixteenth 1/4inch metal valve is connected with a thirty-first 1/4inch metal valve through a 1/4inch metal pipe, and the three-way pipe is connected with another two sets of extraction, separation, purification and collection systems through a twenty-first 1/4inch metal pipe to the right through a 1/4inch metal pipe and a twenty-fifth 1/4inch metal valve; the parts and connection modes of the other two sets of oxygen isotope sample extraction, separation, purification and collection systems are the same as those of the first set.
The extraction, separation, purification, collection system is controlled by a second 1/2inch metal valve.
The waste treatment system comprises a second 1/4inch metal valve which is connected with a waste pipeline leftwards, the first 1/4inch metal valve is upwards connected with an air inlet of a rotary vane type mechanical vacuum pump which is used for pumping reaction waste gas and simultaneously providing low vacuum for the whole system, a first metal cold trap is connected with a third 1/4inch metal valve rightwards, and a fifth 1/4inch metal valve and a sixth 1/4inch metal valve jointly control Ar air flow which enters the system and is used for sweeping the waste gas.
The whole set of system metal pipelines are all made of 316 stainless steel materials, the inner walls of the pipelines are subjected to special polishing treatment, and all pipelines except the metal cold trap are wound with heating belts.
The saidMolecular sieve is filled in a stainless steel tube with the outer diameter of 3/8inch, and oxygen is collected by liquid nitrogen freezing.
An extraction method for analysis of oxygen isotope composition in rock and minerals, comprising the steps of: step 1, sample injection; step 2, baking and vacuum degassing the whole system; step 3, transferring bromine pentafluoride reagent and carrying out fluorination reaction; step 4, separating, purifying and collecting oxygen; and 5, waste treatment.
The step 1 specifically comprises the following steps: closing a tenth 1/4inch metal valve, loading the pretreated oxygen-containing rock or mineral sample into the bottom of the first nickel reaction tube, and accessing the system to complete the sample injection operation.
The step 2 specifically comprises the following steps: and slowly opening a tenth 1/4inch metal valve, a second 1/2inch metal valve, a first 1/2inch metal valve and a fourth 1/4inch metal valve on a first nickel reaction tube, slowly connecting a third 1/4inch metal valve and the first 1/4inch metal valve with a rotary vane type mechanical vacuum pump to pump low vacuum for the system after the first metal cold trap is sleeved with a liquid nitrogen cup, opening a ninth 1/4inch metal valve, setting the temperature of the digital temperature control heating furnace to 120 ℃, opening a heating belt power supply to heat and remove air for 30min for the whole system, closing the third 1/4inch metal valve, connecting a liquid nitrogen cup on an eighth metal cold trap, opening a second nineteenth 1/4inch metal valve and a thirty-first 1/4inch metal valve, and continuously pumping the high vacuum of the pumping system for 30min after the high vacuum of the system reaches -5 Pa through a composite vacuum gauge monitoring system.
The step 3 specifically comprises the following steps: after the system is completely degassed by vacuum, removing a temperature control heating furnace, sleeving circulating water on a nickel reaction tube, fully freezing by a liquid nitrogen cup, closing a tenth 1/4inch metal valve, an eleventh 1/4inch metal valve, a ninth 1/4inch metal valve and a twenty-eighth 1/4inch metal valve, opening the eighth 1/4inch metal valve, half-opening the ninth 1/4inch metal valve, monitoring the pressure values of BrF 5 diffused into a first 1/2inch stainless steel main tube and a second 1/2inch stainless steel main tube by a vacuum pressure gauge, closing the ninth 1/4inch metal valve after the consumption of BrF 5 required by the reaction is reached, opening the tenth 1/4inch metal valve, transferring BrF 5 in the tube into the frozen first nickel reaction tube, repeating the operation to finish the transfer of BrF 5 in other nickel reaction tubes, pumping the system again with low vacuum and high vacuum, and closing the metal valves above the nickel reaction tubes after the high vacuum degree reaches 10 Pa; and (3) removing a liquid nitrogen cup outside the nickel reaction tube, after thawing, sleeving a digital temperature control heating furnace again, and performing a fluorination reaction for 12 hours according to the set heating temperature of the sample type to generate oxygen and other byproducts.
The step 4 specifically comprises the following steps: the temperature control heating furnace outside the nickel reactor is removed, a liquid nitrogen cup is sleeved again for full freezing, each cold trap is sleeved with the liquid nitrogen cup, the system is maintained in a high vacuum state, and all metal valves are closed; sequentially opening a tenth 1/4inch metal valve, an eleventh 1/4inch metal valve, opening a twelfth 1/4inch metal valve after 2min, opening a thirteenth 1/4inch metal valve after 2min, opening a fourteenth 1/4inch metal valve after 5min, opening a fifteenth 1/4inch metal valve and a seventeenth 1/4inch metal valve after 2min, observing the unit to generate O 2 by a first capacitance vacuum gauge, opening an eighteenth 1/4inch metal valve, and fully freezing O 2 by liquid nitrogen to obtain the first stainless steelAnd (3) adsorbing and collecting the molecular sieve collecting pipe, observing the adsorption and collection state through a first capacitance vacuum gauge, closing a fifteenth 1/4inch metal valve, a seventeenth 1/4inch metal valve and an eighteenth 1/4inch metal valve after the reading of the capacitance vacuum gauge is not lowered any more, removing a liquid nitrogen cup outside the collecting pipe, taking the collecting pipe and the eighteenth 1/4inch metal valve off at a first VCO quick joint to be subjected to isotope composition analysis, and thus completing the preparation of an oxygen isotope sample.
The step 4 specifically comprises the following steps: after O 2 in the nickel reactor is separated and collected, the residual reagent and reaction products in the reactor need to be subjected to innocent treatment, an eleventh 1/4inch metal valve is closed, a second 1/2inch metal valve is opened, a cooling water system outside a nickel reaction tube is removed, a temperature control heating furnace is sleeved again, the temperature is adjusted to be 150 ℃, the metal valve above the nickel reaction tube is opened, waste in the nickel reactor is transferred into a first metal cold trap, the first 1/2inch metal valve is closed, a fifth 1/4inch metal valve is opened, liquid nitrogen outside the first metal cold trap is removed, a second 1/4inch metal valve is opened, the waste is carried into a lime water barrel in a ventilation kitchen by Ar gas, and the waste treatment is completed to avoid environmental pollution.
The invention has the beneficial effects that:
(1) According to the invention, the design that different samples to be analyzed are respectively loaded by adopting independent nickel reactors is adopted, each nickel reaction tube, a metal cold trap, a metal hot trap and a molecular sieve form a set of extraction, purification and collection units, each set of units are separated by metal valves, and the operations of extracting, purifying and collecting oxygen in rocks and minerals can be independently completed, so that the analysis efficiency is greatly improved;
(2) The design of three metal cold traps and one metal hot trap filled with NaCl crystal particles is adopted, so that impurity gas and residual fluorinating agent generated by the reaction can be thoroughly removed, and generated O 2 can be fully purified;
(3) The molecular sieve is adopted to directly collect O 2 generated by reaction under the condition of full freezing of liquid nitrogen for mass spectrum 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, and the defect that a system is exposed to the atmosphere due to the fact that a glass piston is coated with vacuum lubricating grease regularly is overcome;
(4) Using filling The stainless steel tube of the molecular sieve is used as a collecting tube of O 2, so that the molecular sieve is activated conveniently; filling/>The stainless steel collecting pipe of the molecular sieve is connected with the metal valve in a sealing mode of a VCR, so that the molecular sieve is convenient to detach, and meanwhile, cross contamination caused by using oxygen-containing vacuum sealing grease is avoided;
(5) The collecting pipe with the metal valve is connected with a metal pipeline of the sample preparation device in a sealing mode by adopting a VCO quick connector, so that the collecting pipe after collecting samples is convenient to replace and is matched with a dual-path sample injection system of the isotope mass spectrometer;
(6) The turbo molecular pump with the rotary vane type mechanical pump as the front stage is used as a high-vacuum pump set of the system, so that the whole 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.
Drawings
FIG. 1 is a schematic diagram of a structure of an analysis and extraction device for oxygen isotope composition in rocks and minerals;
In the figure: 1 is a rotary vane type mechanical vacuum pump, 2 is a first 1/4inch metal valve, 3 is a second 1/4inch metal valve, 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 fifth 1/4inch metal valve, 9 is a sixth 1/4inch metal valve, 10 is a seventh 1/4inch metal valve, 11 is an eighth 1/4inch metal valve, 12 is a bromine pentafluoride reservoir tank, 13 is a ninth 1/4inch metal valve, 14 is a first 1/2inch metal valve, 15 is a tenth 1/4inch metal valve, 16 is a first nickel reaction tube, 17 is an eleventh 1/4inch metal valve, 18 is a second metal cold trap, 19 is a twelfth 1/4inch metal valve, 20 is a third metal cold trap, 21 is a thirteenth 1/4inch metal valve, 22 is a first metal hot trap, 23 is a fourteenth 1/4inch metal valve, 24 is a fourth metal cold trap, 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 capacitance vacuum gauge, 29 is a first "VCO" quick connector, 30 is an eighteenth 1/4inch metal valve, 31 is a first stainless steel The molecular sieve collecting pipe 32 is a second 1/2inch metal valve, 33 is a third 1/2inch metal valve, 34 is a nineteenth 1/4inch metal valve, 35 is a second nickel reaction pipe, 36 is a twenty-first/4 inch metal valve, 37 is a fifth metal cold trap, 38 is a twenty-first 1/4inch metal valve, 39 is a sixth metal cold trap, 40 is a twenty-second 1/4inch metal valve, 41 is a second metal hot trap, 42 is a twenty-first/4 inch metal valve, 43 is a seventh metal cold trap, 44 is a twenty-first/4 inch metal valve, 45 is a twenty-first/4 inch metal valve, 46 is a twenty-first/4 inch metal valve, 47 is a second capacitance vacuum gauge, 48 is a second 'VCO' quick connector, 49 is a twenty-first/4 inch metal valve, 50 is a second stainless steel/>The molecular sieve collecting pipe, 51 is a twenty-eighth 1/4inch metal valve, 52 is an eighth metal cold trap, 53 is a twenty-ninth 1/4inch metal valve, 54 is a first composite vacuum gauge, 55 is a thirty-first 1/4inch metal valve, 56 is a turbomolecular pump, 57 is a thirty-first 1/4inch metal valve, 58 is a first 1/2inch stainless steel pipeline, and 59 is a second 1/2inch stainless steel pipeline.
Detailed Description
The invention provides a rock and mineral oxygen isotope composition analysis and extraction device and a method thereof, which are further described in detail below with reference to the accompanying drawings and specific examples.
As shown in fig. 1, the invention provides an analysis and extraction device for oxygen isotope composition in rock and minerals, which comprises a waste treatment system, a first 1/2inch stainless steel vertical main pipeline 58 and 12 sets of identical oxygen isotope sample extraction, separation, purification and collection systems;
The vacuum pressure gauge 6 is connected with a fourth 1/4inch metal valve 7 downwards through a 1/4inch stainless steel pipe by a cutting sleeve, the lower end of the fourth 1/4inch metal valve 7 is connected with a first 1/2inch stainless steel vertical main pipe 58 through a 1/4inch stainless steel pipe by welding, the vertical main pipe 58 is vertically connected with a second 1/2inch metal pipeline 59 through welding, and the on-off state of the two pipelines is controlled through a first 1/2inch metal valve 14;
The bromine pentafluoride steel bottle is connected with the vertical main pipeline 58 through a 1/4inch metal pipeline by welding, a seventh 1/4inch metal valve 10 and a ninth 1/4inch metal valve 13 are arranged on the 1/4inch metal pipeline, a tee joint is arranged on the 1/4inch metal pipeline between the seventh 1/4inch metal valve 10 and the ninth 1/4inch metal valve 13, and the tee joint is downwards connected with an eighth 1/4inch metal valve 11 and a bromine pentafluoride reservoir tank 12 in sequence;
The turbo molecular pump 56 is welded with a first 1/2inch stainless steel pipe 58 through a 1/4inch stainless steel pipe, a twenty-eighth 1/4inch metal valve 51, an eighth metal cold trap 52, a twenty-eighth 1/4inch metal valve 53 and a thirty-first 1/4inch metal valve 55 are sequentially arranged between the first 1/2inch stainless steel pipe 58 and the turbo molecular pump 56, a tee joint is arranged between the twenty-eighth 1/4inch metal valve 51 and the eighth metal cold trap 52, the third tee joint is connected with a thirty-first 1/4inch metal valve 57 through a 1/4inch metal pipe, a tee joint is arranged between the twenty-eighth 1/4inch metal valve 53 and the thirty-first 1/4inch metal valve 55, and the tee joint is downwards connected with a first compound vacuum gauge 54;
Taking two sets of oxygen isotope sample extraction, separation, purification and collection systems as an example,
The second 1/2inch metal valve 32 controls the first set of extraction, separation, purification, collection systems, and the third 1/2inch metal valve 33 controls the second set of extraction, separation, purification, collection systems;
In the first set of extraction, separation, purification and collection systems, a tenth 1/4inch metal valve 15 and an eleventh 1/4inch metal valve 17 are welded and connected with a second 1/2inch metal pipeline 59 through a 1/4inch stainless steel pipeline; the first nickel reaction tube 16 is connected with the tenth 1/4inch metal valve 15 in a cutting sleeve sealing mode by adopting a metal thread and gasket sealing mode through a 1/4inch stainless steel pipeline upwards; the eleventh 1/4inch metal valve 17 is connected with the second metal cold trap 18 through a 1/4inch stainless steel pipeline, the second metal cold trap 18 is connected with the third metal cold trap 20 through a twelfth 1/4inch stainless steel pipeline through a twelfth 1/4inch metal valve 19, both ends of the thirteenth 1/4inch metal valve 21 are respectively connected with the third metal cold trap 20 and the first metal hot trap 22 through a 1/4inch stainless steel pipeline, the first metal hot trap 22 is connected with the fourth metal cold trap 24 through a fourteenth 1/4inch metal valve 23 through a 1/4inch stainless steel pipeline, one end of the fifteenth 1/4inch metal valve 25 is connected with the fourth metal cold trap 24, the other end of the fifteenth 1/4inch metal valve 25 is connected with a 1/4inch tee joint, the tee joint is connected with the sixteenth 1/4inch metal valve 26 upwards, the right is connected with another 1/4inch tee joint through a 1/4inch stainless steel pipeline, the other 1/4inch metal valve 27 is connected with one end of the seventeenth 1/4inch metal valve downwards, the other end of the first metal hot trap 22 is connected with the VCO joint 29 to the right through a first/4 inch stainless steel pipeline, the other end of the VCO joint 29 is connected with the first quick coupler 30 through a first quick coupler 30, the quick coupler is connected with the first quick coupler 29 The molecular sieve collecting pipe 31 is connected with a 1/4inch stainless steel pipe line, the other end of a seventeenth 1/4inch metal valve 27 is connected with a first capacitance vacuum gauge 28 through a 1/4inch stainless steel pipe line in a welding mode, a sixteenth 1/4inch metal valve 26 is connected with a thirty-first 1/4inch metal valve 57 through a 1/4inch metal pipe line, the three-way pipe is connected with a second set of extraction, separation, purification and collection system through a fifteenth 1/4inch metal valve 45 from right through a 1/4inch metal pipe line; the parts and connection modes of the second set of oxygen isotope sample extraction, separation, purification and collection system are the same as those of the first set;
The waste treatment system comprises a second 1/4inch metal valve 3 which is connected with a waste pipeline leftwards, a first 1/4inch metal valve 2 which is connected with an air inlet of a rotary-vane mechanical vacuum pump 1 for pumping out reaction waste gas and simultaneously providing low vacuum for the whole system, a first metal cold trap 4 which is connected with a third 1/4inch metal valve 5 rightwards, and a fifth 1/4inch metal valve 8 and a sixth 1/4inch metal valve 9 which jointly control Ar air flow entering the system for sweeping the waste gas.
The whole set of system metal pipelines are all made of 316 stainless steel materials, the inner walls of the pipelines are subjected to special polishing treatment, and all pipelines except the metal cold trap are wound with heating belts.
The saidMolecular sieve is filled in a stainless steel tube with the outer diameter of 3/8inch, and oxygen is collected by liquid nitrogen freezing.
An extraction method for analysis of oxygen isotope composition in rock and minerals, which comprises the following steps:
Step 1, sample injection
Closing a tenth 1/4inch metal valve 15, loading the pretreated oxygen-containing rock or mineral sample into the bottom of the first nickel reaction tube, and accessing the system to finish the sample injection operation;
Step 2, baking the whole system, and vacuum degassing
The method comprises the steps of sleeving a first nickel reaction tube 16 with a digital temperature control heating furnace, slowly opening a tenth 1/4inch metal valve 15, a second 1/2inch metal valve 32, a first 1/2inch metal valve 14 and a fourth 1/4inch metal valve 7, sleeving a liquid nitrogen cup on a first metal cold trap 4, slowly switching on a third 1/4inch metal valve 5 and a first 1/4inch metal valve 2, switching on a rotary-vane mechanical vacuum pump 1 to pump a low vacuum for the system, opening a ninth 1/4inch metal valve 13, setting the temperature of the digital temperature control heating furnace to 120 ℃, switching on a heating belt power supply to heat and remove gas for 30min for the whole system, closing the third 1/4inch metal valve 5, sleeving a liquid nitrogen cup on an eighth metal cold trap 52, switching on a turbo molecular pump 56 by opening a second nineteenth 1/4inch metal valve 53 and a thirty-1/4 inch metal valve 55, and continuously pumping 30min after the high vacuum of the pumping system is monitored to reach 10 -5 Pa by a compound vacuum gauge 54;
Step 3, bromine pentafluoride reagent transfer and fluorination reaction
After the system is completely evacuated, the temperature control heating furnace is removed, circulating water is sleeved on the nickel reaction tube and fully frozen by a liquid nitrogen cup, the tenth 1/4inch metal valve 15, the eleventh 1/4inch metal valve 17, the ninth 1/4inch metal valve 13 and the twenty-eighth 1/4inch metal valve 51 are closed, the eighth 1/4inch metal valve 11 is opened, the ninth 1/4inch metal valve 13 is half opened, the pressure value of BrF 5 diffused into the first 1/2inch stainless steel main pipeline 58 and the second 1/2inch stainless steel main pipeline 59 is monitored by a vacuum pressure gauge 6, after the consumption of BrF 5 required by the reaction is reached, the ninth 1/4inch metal valve 13 is closed, the tenth 1/4inch metal valve 15 is opened, the BrF 5 in the pipeline is transferred into the frozen first nickel reaction tube 16, the transfer of BrF 5 in other nickel reaction tubes can be completed by repeating the operation, the system low vacuum and high vacuum is pumped again, and the pressure value of BrF 5 in the nickel reaction tube is closed after the nickel reaction tube is subjected to the vacuum of -5 Pa. Removing a liquid nitrogen cup outside the nickel reaction tube, after thawing, sleeving a digital temperature control heating furnace again, and performing a fluorination reaction for 12 hours according to the set heating temperature of the sample type to generate oxygen and other byproducts;
step 4, separating, purifying and collecting oxygen
And (3) removing the temperature control heating furnace outside the nickel reactor, sleeving a liquid nitrogen cup again for full freezing, sleeving liquid nitrogen cups on all cold traps, maintaining the system in a high vacuum state, and closing all metal valves. Sequentially opening a tenth 1/4inch metal valve 15, an eleventh 1/4inch metal valve 17, a twelfth 1/4inch metal valve 19 after 2min, a thirteenth 1/4inch metal valve 21 after 2min, a fourteenth 1/4inch metal valve 23 after 5min, a fifteenth 1/4inch metal valve 25 and a seventeenth 1/4inch metal valve 27 after 2min, observing the unit to generate O 2 through a first capacitance vacuum gauge 28, opening an eighteenth 1/4inch metal valve 30, and fully freezing the O 2 by liquid nitrogen to obtain a first stainless steelThe molecular sieve collecting pipe is adsorbed and collected, the adsorption and collection state is observed through the first capacitance vacuum gauge 28, the fifteenth 1/4inch metal valve 25, the seventeenth 1/4inch metal valve 27 and the eighteenth 1/4inch metal valve 30 are closed after the capacitance vacuum gauge reading is not lowered any more, a liquid nitrogen cup outside the collecting pipe is removed, the collecting pipe and the eighteenth 1/4inch metal valve 30 are taken down at the first VCO quick connector 29 to be subjected to isotope composition analysis, and the preparation of the oxygen isotope sample is completed;
Step 5, waste treatment
After O 2 in the nickel reactor is separated and collected, the residual reagent and reaction products in the reactor need to be subjected to innocent treatment, an eleventh 1/4inch metal valve 17 is closed, a second 1/2inch metal valve 32 is opened, a cooling water system outside the nickel reaction tube is removed, a temperature control heating furnace is sleeved again, the temperature is adjusted to be 150 ℃, the metal valve above the nickel reaction tube is opened, waste in the nickel reactor is transferred to a first metal cold trap 4, the first 1/2inch metal valve 14 is closed, a fifth 1/4inch metal valve 8 is opened, a sixth 1/4inch metal valve 9 is opened, liquid nitrogen outside the first metal cold trap 4 is removed, a second 1/4inch metal valve 3 is opened, the waste is carried into a lime water barrel in a ventilation kitchen by Ar gas, and waste disposal is completed to avoid environmental pollution.
Claims (5)
1. An analysis and extraction device for oxygen isotope composition in rock and minerals is characterized in that: comprises a waste treatment system, a first 1/2inch stainless steel vertical main pipeline (58) and 2 sets of identical oxygen isotope sample extraction, separation, purification and collection systems;
the vacuum pressure gauge (6) is connected with a fourth 1/4inch metal valve (7) downwards through a 1/4inch stainless steel pipe by a clamping sleeve, the lower end of the fourth 1/4inch metal valve (7) is connected with a first 1/2inch stainless steel vertical main pipe (58) through welding by a 1/4inch stainless steel pipe, the vertical main pipe (58) is vertically connected with a second 1/2inch metal pipeline (59) through welding, and the on-off of the two pipelines is controlled through a first 1/2inch metal valve (14);
The bromine pentafluoride steel cylinder is connected with a vertical main pipeline (58) through a 1/4inch metal pipeline by welding, a seventh 1/4inch metal valve (10) and a ninth 1/4inch metal valve (13) are arranged on the 1/4inch metal pipeline, a tee joint is arranged on the 1/4inch metal pipeline between the seventh 1/4inch metal valve (10) and the ninth 1/4inch metal valve (13), and the tee joint is downwards connected with an eighth 1/4inch metal valve (11) and a bromine pentafluoride reservoir tank (12) in sequence;
The turbo molecular pump (56) is welded with the first 1/2inch stainless steel pipe line (58) through a 1/4inch stainless steel pipe line, a twenty-eighth 1/4inch metal valve (51), an eighth metal cold trap (52), a twenty-eighth 1/4inch metal valve (53) and a thirty-eighth 1/4inch metal valve (55) are sequentially arranged between the first 1/2inch stainless steel pipe line (58) and the turbo molecular pump (56), a tee joint is arranged between the twenty-eighth 1/4inch metal valve (51) and the eighth metal cold trap (52), the third tee joint is connected with the thirty-first 1/4inch metal valve (57) through the 1/4inch metal pipe line, a tee joint is arranged between the twenty-eighth 1/4inch metal valve (53) and the thirty-eighth 1/4inch metal valve (55), and the tee joint is connected with the first compound vacuum gauge (54) downwards;
The oxygen isotope sample extraction, separation, purification and collection system comprises a tenth 1/4inch metal valve (15) and an eleventh 1/4inch metal valve (17) which are welded with a second 1/2inch metal pipeline (59) through a 1/4inch stainless steel pipeline; the first nickel reaction tube (16) is connected with the tenth 1/4inch metal valve (15) in a cutting sleeve sealing mode by adopting a metal thread and gasket sealing mode and a 1/4inch stainless steel pipeline upwards; the eleventh 1/4inch metal valve (17) is connected with the second metal cold trap (18) through a 1/4inch stainless steel pipeline, the second metal cold trap (18) is connected with the third metal cold trap (20) through a twelfth 1/4inch stainless steel pipeline through a twelfth 1/4inch metal valve (19), two ends of the thirteenth 1/4inch metal valve (21) are respectively connected with the third metal cold trap (20) and the first metal hot trap (22) through a 1/4inch stainless steel pipeline, the first metal hot trap (22) is connected with the fourth metal cold trap (24) through a fourteenth 1/4inch metal valve (23), one end of the fifteenth 1/4inch metal valve (25) is connected with the other end of the fourth metal cold trap (24) through a 1/4inch stainless steel pipeline, a tee joint is connected with the other end of the thirteenth 1/4inch cold trap (26) upwards, the right hand joint is connected with the other end of the first metal cold trap (20) through a 1/4inch stainless steel pipeline, the other end of the first cold trap is connected with the first end of a first VCO (29) through a fourteenth 1/4inch stainless steel pipeline, the other end of the first metal cold trap (29) is connected with the first end of the first VCO (29) through a seventeenth 1/4inch stainless steel pipeline, the other end of the seventeenth 1/4inch metal valve (27) is downwards connected with the first capacitance vacuum gauge (28) through a 1/4inch stainless steel pipe line in a welding mode, the sixteenth 1/4inch metal valve (26) is connected with the thirty first 1/4inch metal valve (57) through a 1/4inch metal pipe line, and the three-way pipe is connected with the second set of extraction, separation, purification and collection system through a fifteenth 1/4inch metal valve (45) to the right through a 1/4inch metal pipe line; the parts and connection modes of the second set of oxygen isotope sample extraction, separation, purification and collection system are the same as those of the first set;
The waste treatment system comprises a second 1/4inch metal valve (3) which is connected with a waste pipeline leftwards, a first 1/4inch metal valve (2) is upwards connected with an air inlet of a rotary vane type mechanical vacuum pump (1) which is used for pumping reaction waste gas and simultaneously providing low vacuum for the whole system, a first metal cold trap (4) is connected with a third 1/4inch metal valve (5) rightwards, and a fifth 1/4inch metal valve (8) and a sixth 1/4inch metal valve (9) jointly control Ar air flow which enters the system and is used for sweeping waste gas.
2. The device for analyzing and extracting oxygen isotopes in rock and minerals according to claim 1, wherein: the extraction, separation, purification, collection system is controlled by a second 1/2inch metal valve (32).
3. The device for analyzing and extracting oxygen isotopes in rock and minerals according to claim 2, wherein: the metal 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.
4. A rock and mineral oxygen isotope composition analysis and extraction apparatus in accordance with claim 3 wherein: the 5A molecular sieve is filled in a stainless steel tube with the outer diameter of 3/8inch, and oxygen is collected by liquid nitrogen freezing.
5. An extraction method based on the analysis and extraction device of oxygen isotope composition in rock and minerals, which is characterized in that: the method comprises the following steps: step (1), sample injection is carried out; step (2), baking the whole system and vacuum degassing; step (3), transferring bromine pentafluoride reagent and carrying out fluorination reaction; step (4), separating, purifying and collecting oxygen; step (5), waste treatment;
The step (1) specifically comprises the following steps: closing a tenth 1/4inch metal valve (15) to load the pretreated oxygen-containing rock or mineral sample into the bottom of the first nickel reaction tube and accessing the system to finish the sample injection operation;
The step (2) specifically comprises the following steps: a first nickel reaction tube (16) is sleeved with a digital temperature control heating furnace, a tenth 1/4inch metal valve (15), a second 1/2inch metal valve (32), a first 1/2inch metal valve (14) and a fourth 1/4inch metal valve (7) are slowly opened, after the first metal cold trap (4) is sleeved with a liquid nitrogen cup, a third 1/4inch metal valve (5) and the first 1/4inch metal valve (2) are slowly connected with a rotary-vane mechanical vacuum pump (1) to pump low vacuum for the system, a ninth 1/4inch metal valve (13) is opened, the temperature of the digital temperature control heating furnace is set to 120 ℃, after a heating belt power supply is opened for heating and degassing of the whole system for 30min, the third 1/4inch metal valve (5) is closed, an eighth metal cold trap (52) is sleeved with the liquid nitrogen cup, a second nineteenth 1/4inch metal valve (53) and a thirty-first/4 inch metal valve (55) are opened, a turbomolecular pump (56) is connected with the high vacuum pump (54) is connected with a vacuum pump, and the high vacuum pump system is continuously pumped through a compound vacuum gauge (54) to pump high vacuum for -5 Pa for 10 min;
The step (3) specifically comprises the following steps: after the system vacuum degassing is completed, the temperature control heating furnace is removed, circulating water is sleeved on a nickel reaction tube and fully frozen by a liquid nitrogen cup, a tenth 1/4inch metal valve (15) and an eleventh 1/4inch metal valve (17) are closed, a ninth 1/4inch metal valve (13) and a twenty-eighth 1/4inch metal valve (51) are opened, an eighth 1/4inch metal valve (11) is opened, the ninth 1/4inch metal valve (13) is half-opened, the pressure value of BrF 5 diffused into a first 1/2inch stainless steel main tube (58) and a second 1/2inch stainless steel main tube (59) is monitored by a vacuum pressure gauge (6), after the consumption of BrF 5 required by the reaction is reached, the ninth 1/4inch metal valve (13) is closed, the tenth 1/4inch metal valve (15) is opened, the BrF 5 in the tube is transferred into a frozen first nickel reaction tube (16), the other BrF 5 in the nickel reaction tube can be completed by repeating the operations, and the vacuum system is closed again until the vacuum degree reaches the vacuum degree of -5 Pa; removing a liquid nitrogen cup outside the nickel reaction tube, after thawing, sleeving a digital temperature control heating furnace again, and performing a fluorination reaction for 12 hours according to the set heating temperature of the sample type to generate oxygen and other byproducts;
the step (4) specifically comprises the following steps: the temperature control heating furnace outside the nickel reactor is removed, a liquid nitrogen cup is sleeved again for full freezing, each cold trap is sleeved with the liquid nitrogen cup, the system is maintained in a high vacuum state, and all metal valves are closed; sequentially opening a tenth 1/4inch metal valve (15), an eleventh 1/4inch metal valve (17), opening a twelfth 1/4inch metal valve (19) after 2min, opening a thirteenth 1/4inch metal valve (21) after 2min, opening a fourteenth 1/4inch metal valve (23) after 5min, opening a fifteenth 1/4inch metal valve (25) and a seventeenth 1/4inch metal valve (27) after 2min, observing the generated O 2 quantity through a first capacitance vacuum gauge (28), opening an eighteenth 1/4inch metal valve (30), absorbing and collecting O 2 by a first stainless steel 5A molecular sieve collecting pipe which is fully frozen through liquid nitrogen, observing the absorption and collection state through a first capacitance vacuum gauge (28), closing a fifteenth 1/4inch metal valve (25), a seventeenth 1/4inch VCO metal valve (27) and an eighteenth 1/4inch metal valve (30) after the capacitance vacuum gauge reading is not lowered any more, withdrawing a liquid nitrogen cup outside the collecting pipe and taking out the collecting pipe and the eighteenth 1/4inch metal valve (30) along with the eighteenth 1/4inch metal valve to form a quick-to-coupling (29) to be analyzed at a quick-joint for preparing isotope sample to be analyzed;
The step (5) specifically comprises the following steps: after O 2 in the nickel reactor is separated and collected, the residual reagent and reaction products in the reactor need to be subjected to innocent treatment, an eleventh 1/4inch metal valve (17) is closed, a second 1/2inch metal valve (32) is opened, a cooling water system outside the nickel reaction tube is removed and is sleeved with a temperature control heating furnace again, the temperature is adjusted to be 150 ℃, the metal valve above the nickel reaction tube is opened, waste in the nickel reactor is transferred to a first metal cold trap (4), the first 1/2inch metal valve (14) is closed, a fifth 1/4inch metal valve (8) is opened, a sixth 1/4inch metal valve (9) is opened, liquid nitrogen outside the first metal cold trap (4) is removed, the second 1/4inch metal valve (3) is opened, the waste is carried into a lime bucket in a ventilation kitchen by Ar gas, and waste disposal is completed, and environmental pollution is avoided.
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