CN110031536A - Oxygen isotope composition analysis extraction element and method in a kind of rock and mineral - Google Patents
Oxygen isotope composition analysis extraction element and method in a kind of rock and mineral Download PDFInfo
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- CN110031536A CN110031536A CN201910359063.9A CN201910359063A CN110031536A CN 110031536 A CN110031536 A CN 110031536A CN 201910359063 A CN201910359063 A CN 201910359063A CN 110031536 A CN110031536 A CN 110031536A
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 239000001301 oxygen Substances 0.000 title claims abstract description 67
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 67
- 238000004458 analytical method Methods 0.000 title claims abstract description 41
- 239000011435 rock Substances 0.000 title claims abstract description 36
- 229910052500 inorganic mineral Inorganic materials 0.000 title claims abstract description 34
- 239000011707 mineral Substances 0.000 title claims abstract description 34
- 239000000203 mixture Substances 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000000605 extraction Methods 0.000 title claims abstract description 18
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 68
- 239000010935 stainless steel Substances 0.000 claims abstract description 68
- 239000002699 waste material Substances 0.000 claims abstract description 23
- 150000001649 bromium compounds Chemical class 0.000 claims abstract description 14
- 238000003682 fluorination reaction Methods 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 8
- 238000009849 vacuum degassing Methods 0.000 claims abstract description 7
- 238000002360 preparation method Methods 0.000 claims abstract description 6
- 230000000155 isotopic effect Effects 0.000 claims abstract description 5
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 4
- 239000002184 metal Substances 0.000 claims description 349
- 229910052751 metal Inorganic materials 0.000 claims description 349
- 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 60
- 229910052759 nickel Inorganic materials 0.000 claims description 43
- 239000000376 reactant Substances 0.000 claims description 42
- 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 28
- 239000002808 molecular sieve Substances 0.000 claims description 16
- 239000003990 capacitor Substances 0.000 claims description 13
- 230000008878 coupling Effects 0.000 claims description 12
- 238000010168 coupling process Methods 0.000 claims description 12
- 238000005859 coupling reaction Methods 0.000 claims description 12
- 238000007789 sealing Methods 0.000 claims description 10
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 9
- 239000010931 gold Substances 0.000 claims description 9
- 229910052737 gold Inorganic materials 0.000 claims description 9
- 229910000831 Steel Inorganic materials 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000010959 steel Substances 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 7
- 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 7
- 238000003466 welding Methods 0.000 claims description 7
- 238000005520 cutting process Methods 0.000 claims description 6
- 238000007710 freezing Methods 0.000 claims description 6
- 230000008014 freezing Effects 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 238000012544 monitoring process Methods 0.000 claims description 5
- 229910014271 BrF5 Inorganic materials 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 4
- 238000003860 storage Methods 0.000 claims description 4
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 3
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 3
- 239000006227 byproduct Substances 0.000 claims description 3
- 239000007795 chemical reaction product Substances 0.000 claims description 3
- 239000000498 cooling water Substances 0.000 claims description 3
- 238000007872 degassing Methods 0.000 claims description 3
- 239000004571 lime Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- 238000002203 pretreatment Methods 0.000 claims description 3
- 238000010926 purge Methods 0.000 claims description 3
- 238000010257 thawing Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 241000416536 Euproctis pseudoconspersa Species 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 claims 1
- 230000005611 electricity Effects 0.000 claims 1
- 238000005194 fractionation Methods 0.000 abstract description 4
- 238000012360 testing method Methods 0.000 abstract description 3
- 238000006276 transfer reaction Methods 0.000 abstract description 3
- 238000005259 measurement Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000004519 grease Substances 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000012864 cross contamination Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen(.) Chemical compound [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000001004 secondary ion mass spectrometry Methods 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000010687 lubricating oil Substances 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
- 230000001089 mineralizing effect Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000700 radioactive tracer Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
Classifications
-
- 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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention belongs to rocks and mineral isotopics determination techniques field, and in particular to oxygen isotope composition analysis extraction element and method in a kind of rock and mineral.Apparatus of the present invention include waste treatment system, the vertical main pipeline of the first 1/2inch stainless steel and 12 sets of identical oxygen isotope sample extracting and developings, purifying, collection system；The method of the present invention includes the following steps: step 1, sample introduction；Step 2, vacuum degassing is toasted to whole system；Step 3, brominated bromide agent transfer and fluorination reaction；Step 4, oxygen separation, purifying and collection；Step 5, waste is handled.The present invention is able to solve in isotope sample preparation the problem of easily causing OXYGEN ISOTOPE FRACTIONATION, improves analysis measuring accuracy and analysis testing efficiency.
Description
Technical field
The invention belongs to rocks and mineral isotopics determination techniques field, and in particular to oxygen in a kind of rock and mineral
Extraction element and method are analyzed in isotopics.
Background technique
The measurement that oxygen isotope forms in rock and mineral can formation condition to mineral and rock and mechanism, source,
Develop and is studied with the interaction of country rock etc..Oxygen isotope analysis has become petrology, one of mineralogical study
Strong tool is made disclosing ore deposit fluid origin, migration, evolution and mineralizing process with very important tracer
With, and theoretical foundation is provided to illustrate ore deposit mechanism.It sufficiently extracts rock and oxygen in mineral and it is purified, is complete
Complete collect is the premise for carrying out oxygen isotope composition analysis in rock and mineral.
In rock and mineral in oxygen isotope composition analysis, home and abroad uses laser method, secondary ion mass spectrometry substantially
And traditional brominated bromide method.These types of oxygen isotope composition analysis method has respective drawback: 1) laser method oxygen isotope group
At in analysis, the factors such as Particle size, systematic memory effect, edge effect and powder splashing of sample easily cause oxygen isotope
Fractionation, causes analytical precision and accuracy；2) Secondary Ion Mass Spectrometry oxygen isotope composition analysis technology is same for studying
The position celestial body sample that differs greatly of element composition has unique superiority, but when for analysis common rocks, mineral samplers, seriously
Matrix effect, that is, various scatterings ion between interfere with each other so that analysis precision substantially reduces；3) traditional brominated bromide method
Oxygen isotope composition analysis, since the reaction product in each reactor is using shared analysis conduit system, need one by one into
Row purifying, conversion and collection, so that analysis efficiency is low.Meanwhile in terms of test object, traditional brominated bromide method is will be anti-
The oxygen and graphite that should be generated are converted into CO under the high temperature conditions2Mass-spectrometer measurement is carried out, since carbon has12C、13Two kinds of isotope ginsengs of C
It with calculating, needs to be corrected measurement result, conversion process easily causes O isotope fractionation.In addition, conversion system needs to introduce
Glass pipeline, wherein glass piston need to smear vacuum grease periodically to guarantee piston seal performance and rotation flexibility, smear true
System is set to be exposed to atmosphere during empty grease, the oxygen, steam in air enter system and pollutes, while vacuum sealing oil
Rouge easily causes cross contamination because oxygen-containing.
Summary of the invention
Present invention solves the technical problem that:
In view of the deficiencies of the prior art, the present invention provides oxygen isotope composition analysis extraction element in a kind of rock and mineral
And method, it is able to solve in isotope sample preparation the problem of easily causing OXYGEN ISOTOPE FRACTIONATION, improves analysis measuring accuracy
And analysis testing efficiency.
The technical solution adopted by the present invention:
Oxygen isotope composition analysis extraction element in a kind of rock and mineral, including waste treatment system, the first 1/2inch
The vertical main pipeline of stainless steel and 12 sets of identical oxygen isotope sample extracting and developings, purifying, collection system；
Pressure vacuum gauge is connect with the 4th 1/4inch metal valve by cutting ferrule downwards with 1/4inch stainless steel tube, and the 4th
1/4inch metal valve lower end passes through welding phase with 1/4inch stainless steel tube and the first vertical main pipeline of 1/2inch stainless steel
Even, vertical main pipeline is vertically connected with the 2nd 1/2inch metal pipe line by welding, passes through the first 1/2inch between two pipelines
Metal valve controls on-off；
Brominated bromide steel cylinder is connected by welding by 1/4inch metal pipe line and vertical main pipeline, 1/4inch metal tube
Line is equipped with the 7th 1/4inch metal valve and the 9th 1/4inch metal valve, the 7th 1/4inch metal valve and the 9th 1/
1/4inch metal pipe line between 4inch metal valve is equipped with threeway, and threeway is connected with downwards the 8th 1/4inch gold in turn
Belong to valve and brominated bromide storage cylinder；
Turbomolecular pump is weldingly connected by 1/4inch stainless steel tubing and the first 1/2inch stainless steel tubing, and the one 1/
2inch stainless steel tubing is cold to the 28th 1/4inch metal valve, the 8th metal between turbomolecular pump, is disposed with
Trap, the 29th 1/4inch metal valve, the 30th 1/4inch metal valve, the 28th 1/4inch metal valve and
Threeway is equipped between eight metal cold-traps, third crosses 1/4inch metal pipe line all and the 31st 1/4inch metal valve connects
It connects, threeway is equipped between the 29th 1/4inch metal valve, the 30th 1/4inch metal valve, threeway is connected with downwards the
One compound vacuum gauge.
The oxygen isotope sample extracting and developing, purifying, collection system include the tenth 1/4inch metal valve, the tenth
One 1/4inch metal valve is weldingly connected by 1/4inch stainless steel tubing and the 2nd 1/2inch metal pipe line；First nickel is anti-
Should pipe using metal threaded cushioning circle sealing means by 1/4inch stainless steel tubing upwards with the tenth 1/4inch metal valve
It is connected using cutting ferrule sealing means；11st 1/4inch metal valve passes through 1/4inch stainless steel tubing and the second metal cold-trap
It is connected, the second metal cold-trap passes through 1/4inch stainless steel tubing by the 12nd 1/4inch metal valve and third metal cold-trap
Be connected, the 13rd 1/4inch metal valve both ends by 1/4inch stainless steel tubing respectively with third metal cold-trap and the first gold medal
Belong to hot trap to be connected, the first metal hot trap is stainless by 1/4inch with the 4th metal cold-trap by the 14th 1/4inch metal valve
Steel pipeline is connected, and the 15th 1/4inch metal valve one end is connected the other end and 1/4inch threeway phase with the 4th metal cold-trap
Even, threeway is connected with the 16th 1/4inch metal valve upwards, passes through 1/4inch stainless steel tubing and another 1/4inch to the right
Threeway is connected, and another 1/4inch threeway is connected with the 17th 1/4inch metal valve one end downwards, fast with first " VCO " to the right
Quick coupling one end is connected, and first " VCO " quick coupling other end passes through the 18th 1/4inch metal valve and the first stainless steelMolecular sieve collecting pipe is connected by 1/4inch stainless steel tubing, and the 17th 1/4inch metal valve other end is downwards with the
One capacitor vacuum gauge is weldingly connected by 1/4inch stainless steel tubing, the 16th 1/4inch metal valve and the 31st
4inch metal valve is connected by 1/4inch metal pipe line with threeway, and threeway passes through to the right 1/4inch metal pipe line and passes through the
25 1/4inch metal valves are connected with a separate set of extracting and developing, purifying, collection system；A separate set of oxygen isotope sample mentions
Take, separate, purifying, the component of collection system and connection type it is identical as first set.
Extracting and developing, purifying, collection system are controlled by the 2nd 1/2inch metal valve.
The waste treatment system includes that the 2nd 1/4inch metal valve is connected with waste line to the left, the first 1/4inch
Metal valve provides the air inlet of the rotary-vane pump of whole system low vacuum simultaneously with abstraction reactor off-gas object upwards
It is connected, the first metal cold-trap is connected with the 3rd 1/4inch metal valve to the right, the 5th 1/4inch metal valve and the 6th 1/
4inch metal valve co- controlling enters system for purging the Ar throughput of Litter.
The whole system metal pipe line all uses 316 type stainless steel materials, and pipeline inner wall passes through special polishing treatment,
Pipeline in addition to metal cold-trap all winds heating tape.
It is describedIt is to collect oxygen by liquid nitrogen frozen in 3/8inch stainless steel tube that molecular sieve, which is filled in outer diameter,.
A kind of extracting method for oxygen isotope composition analysis in rock and mineral, includes the following steps: step 1, into
Sample；Step 2, vacuum degassing is toasted to whole system；Step 3, brominated bromide agent transfer and fluorination reaction；Step 4, oxygen point
From, purifying and collect；Step 5, waste is handled.
The step 1 specifically: close the tenth 1/4inch metal valve oxygen-containing rock or mineral samplers that pre-treatment is good
It is packed into the first nickel reactant bottom of the tube and access system, completes sample introduction operation.
The step 2 specifically: by digital temperature control heating furnace on the first nickel reactant pipe sleeve, slowly open the tenth 1/4inch
Metal valve, the 2nd 1/2inch metal valve, the first 1/2inch metal valve, the 4th 1/4inch metal valve, in the first gold medal
It is mechanical true to belong to that cold-trap puts on slow 3rd 1/4inch metal valve after liquid nitrogen cup, the first 1/4inch metal valve connects rotary vane type
Sky pump is that system takes out low vacuum, opens the 9th 1/4inch metal valve, sets the temperature of digital temperature control heating furnace as 120 DEG C, beat
Opening heating charged is after whole system heats degassing 30min, the 3rd 1/4inch metal valve to be closed, by the 8th metal cold-trap
Liquid nitrogen cup is put on, the 29th 1/4inch metal valve is opened and the 30th 1/4inch metal valve connects turbomolecular pump,
Pumping system high vacuum monitors system condition of high vacuum degree by compound vacuum gauge and reaches 10-5Continue to take out 30min after Pa.
The step 3 specifically: after the completion of system vacuum degassing, remove temperature control heating furnace, recycled on nickel reactant pipe sleeve
Water is simultaneously sufficiently freezed with liquid nitrogen cup, closing the tenth 1/4inch metal valve, the 11st 1/4inch metal valve, and the 9th 1/
4inch metal valve, the 28th 1/4inch metal valve, the 8th 1/4inch metal valve of opening, the semi-open 9th 1/
4inch metal valve is simultaneously diffused into the first 1/2inch stainless steel main pipeline and the 2nd 1/2inch not by pressure vacuum gauge monitoring
BrF in rust steel main pipeline5Pressure values, reach reaction required for BrF5After dosage, the 9th 1/4inch metal valve is closed,
The tenth 1/4inch metal valve is opened, by the BrF in pipeline5It is transferred in the first nickel reactant pipe of freezing, repeating aforesaid operations can
Complete BrF in other nickel reactant pipes5Be transferred to, and take out system low vacuum and high vacuum again, condition of high vacuum degree is up to 10-5After Pa, close
Close the metal valve above each nickel reactant device；The liquid nitrogen cup outside nickel reactant pipe is removed, puts on digital temperature control heating after defrosting again
Furnace sets heating temperature according to sample type and carries out 12h fluorination reaction generation oxygen and other by-products.
The step 4 specifically: remove the temperature control heating furnace outside nickel reactant device, it is sufficiently cold to put on the progress of liquid nitrogen cup again
Freeze, each cold-trap is sleeved on liquid nitrogen cup, and system is maintained to be in high vacuum state, closes all metal valves；Successively open the tenth
1/4inch metal valve, the 11st 1/4inch metal valve open the 12nd 1/4inch metal valve after 2min, after 2min
The 13rd 1/4inch metal valve is opened, the 14th 1/4inch metal valve is opened after 5min, opens the 15th after 2min
4inch metal valve, the 17th 1/4inch metal valve observe the unit by first capacitor vacuum gauge and generate O2Amount is opened
18th 1/4inch metal valve, O2Passed through sufficiently chilled first stainless steel of liquid nitrogenMolecular sieve collecting pipe adsorbs receipts
Collection, and absorptive collection state is observed by first capacitor vacuum gauge, capacitor vacuum gauge reading closes the 15th after no longer declining
4inch metal valve, the 17th 1/4inch metal valve and the 18th 1/4inch metal valve, remove the liquid nitrogen outside collecting pipe
Collecting pipe is simultaneously removed pending isotope groups at first " VCO " quick coupling together with the 18th 1/4inch metal valve by cup
At analysis, the preparation of oxygen isotope sample is completed.
The step 4 specifically: the O in nickel reactant device2After completing separation and collecting, remaining reagent and anti-in reactor
It answers product to need to carry out harmless treatment, closes the 11st 1/4inch metal valve, open the 2nd 1/2inch metal valve, unload
Cooling water system outside lower nickel reactant pipe puts on temperature control heating furnace again, adjusts 150 DEG C and heats to it, opens nickel reactant pipe
Waste in nickel reactant device is transferred in the first metal cold-trap by the metal valve of top, closes the first 1/2inch metal valve
Door opens the 5th 1/4inch metal valve, and the 6th 1/4inch metal valve removes the liquid nitrogen outside the first metal cold-trap, opens
Waste is downloaded in the lime bucket in ventilating kitchen by the 2nd 1/4inch metal valve with Ar fate, is completed Waste disposal and is avoided dirt
Contaminate environment.
Beneficial effects of the present invention:
(1) present invention loads the design of different sample to be analysed, every nickel reactant pipe using independent nickel reactant device respectively
A set of extraction, purifying and collector unit are formed with metal cold-trap, metal hot trap and molecular sieve, uses metal valve between every set unit
Door separates, can complete independently the extraction, purifying of oxygen in rock and mineral and collecting is operated, analysis efficiency is greatly improved；
(2) it is designed, reaction can be given birth to using three metal cold-traps and a metal hot trap equipped with NaCl crystal grain
At foreign gas and remaining fluorination reagent thoroughly remove, to the O of generation2Sufficiently purifying；
(3) O that reaction is generated in the case where liquid nitrogen sufficiently freezes using molecular sieve2It directly collects and carries out mass-spectrometer measurement, avoid
The problem of need to being corrected to measurement result in conventional method because of the introducing of graphite, overcomes glass piston periodically to smear vacuum profit
Lubricating oil rouge and make system exposure atmosphere defect；
(4) using fillingThe stainless steel tube of molecular sieve is as O2Collecting pipe, convenient for being activated to molecular sieve；Dress
It fills outIt is connected between the stainless steel collecting pipe and metal valve of molecular sieve using " VCR " sealing means, it is easy to disassemble, it keeps away simultaneously
Exempt from because of the cross contamination caused by using oxygen-containing vacuum sealing grease；
(5) collecting pipe with metal valve and sample preparation device metal pipe line use the sealing means of " VCO " quick coupling
Connection convenient for replacing to the collecting pipe for having collected sample, and matches with isotope mass spectrometer two-way sampling system；
(6) using rotary vane mechanical pump is the turbomolecular pump of prime as system high vacuum pump group, it is ensured that total system reaches
To higher vacuum, oxygen-containing gas influence caused by experimentation in air is further decreased.
Detailed description of the invention
Fig. 1 is oxygen isotope composition analysis extraction element structural schematic diagram in rock and mineral；
In figure: 1 is rotary-vane pump, and 2 be the first 1/4inch metal valve, and 3 be the 2nd 1/4inch metal valve
Door, 4 be the first metal cold-trap, and 5 be the 3rd 1/4inch metal valve, and 6 be pressure vacuum gauge, and 7 be the 4th 1/4inch metal valve
Door, 8 be the 5th 1/4inch metal valve, and 9 be the 6th 1/4inch metal valve, and 10 be the 7th 1/4inch metal valve, and 11 are
8th 1/4inch metal valve, 12 be brominated bromide storage cylinder, and 13 be the 9th 1/4inch metal valve, and 14 be the 1st
2inch metal valve, 15 be the tenth 1/4inch metal valve, and 16 be the first nickel reactant pipe, and 17 be the 11st 1/4inch metal
Valve, 18 be the second metal cold-trap, and 19 for the 12nd be 1/4inch metal valve, and 20 be third metal cold-trap, and 21 be the 13rd
1/4inch metal valve, 22 be the first metal hot trap, and 23 be the 14th 1/4inch metal valve, and 24 be the 4th metal cold-trap,
25 be the 15th 1/4inch metal valve, and 26 be the 16th 1/4inch metal valve, and 27 be the 17th 1/4inch metal valve
Door, 28 be first capacitor vacuum gauge, and 29 be first " VCO " quick coupling, and 30 be the 18th 1/4inch metal valve, and 31 be the
One stainless steelMolecular sieve collecting pipe, 32 be the 2nd 1/2inch metal valve, and 33 be the 3rd 1/2inch metal valve, and 34 are
19th 1/4inch metal valve, 35 be the second nickel reactant pipe, and 36 be the 20th 1/4inch metal valve, and 37 be fifth metal
Cold-trap, 38 be the 21st 1/4inch metal valve, and 39 be the 6th metal cold-trap, and 40 be the 22nd 1/4inch metal valve
Door, 41 be the second metal hot trap, and 42 be the 23rd 1/4inch metal valve, and 43 be the 7th metal cold-trap, and 44 be the 24th
1/4inch metal valve, 45 be the 25th 1/4inch metal valve, and 46 be the 26th 1/4inch metal valve, and 47 are
Second capacitor vacuum gauge, 48 be second " VCO " quick coupling, and 49 be the 27th 1/4inch metal valve, and 50 is stainless for second
SteelMolecular sieve collecting pipe, 51 be the 28th 1/4inch metal valve, and 52 be the 8th metal cold-trap, and 53 be the 29th
4inch metal valve, 54 be the first compound vacuum gauge, and 55 be the 30th 1/4inch metal valve, and 56 be turbomolecular pump, 57
It is the first 1/2inch stainless steel tubing for the 31st 1/4inch metal valve, 58,59 be the 2nd 1/2inch stainless steel tube
Line.
Specific embodiment
In the following with reference to the drawings and specific embodiments to oxygen isotope group ingredient in a kind of rock provided by the invention and mineral
Analysis extraction element and method are described in further detail.
As shown in Figure 1, oxygen isotope composition analysis extraction element, the device in a kind of rock provided by the invention and mineral
Extracted including waste treatment system, the vertical main pipeline 58 of the first 1/2inch stainless steel and 12 sets of identical oxygen isotope samples,
Separation, purifying, collection system；
The 1/4inch stainless steel tube of pressure vacuum gauge 6 is connect with the 4th 1/4inch metal valve 7 by cutting ferrule downwards, the
Four 1/4inch metal valves, 7 lower end 1/4inch stainless steel tube and the vertical main pipeline 58 of the first 1/2inch stainless steel pass through weldering
Connect connected, vertical main pipeline 58 and the 2nd 1/2inch metal pipe line 59 are vertically connected by welding, pass through first between two pipelines
1/2inch metal valve 14 controls on-off；
Brominated bromide steel cylinder is connected by welding by 1/4inch metal pipe line with vertical main pipeline 58,1/4inch metal
Pipeline is equipped with the 7th 1/4inch metal valve 10 and the 9th 1/4inch metal valve 13, the 7th 1/4inch metal valve 10
And the 9th 1/4inch metal pipe line between 1/4inch metal valve 13 is equipped with threeway, threeway is connected with downwards the 8th in turn
1/4inch metal valve 11 and brominated bromide storage cylinder 12；
Turbomolecular pump 56 is weldingly connected by 1/4inch stainless steel tubing with the first 1/2inch stainless steel tubing 58, the
One 1/2inch stainless steel tubing 58 between turbomolecular pump 56, be disposed with the 28th 1/4inch metal valve 51,
8th metal cold-trap 52, the 29th 1/4inch metal valve 53, the 30th 1/4inch metal valve 55, the 28th
Threeway is equipped between 4inch metal valve 51 and the 8th metal cold-trap 52, third crosses 1/4inch metal pipe line and the 30th all
One 1/4inch metal valve 57 connection, between the 29th 1/4inch metal valve 53, the 30th 1/4inch metal valve 55
Equipped with threeway, threeway is connected with downwards the first compound vacuum gauge 54；
By taking wherein two sets of oxygen isotope sample extracting and developings, purifying, collection systems as an example,
2nd 1/2inch metal valve 32 controls first set extracting and developing, purifying, collection system, the 3rd 1/2inch gold
Belong to valve 33 and controls second set of extracting and developing, purifying, collection system；
First set extracting and developing, purifying, in collection system, the tenth 1/4inch metal valve 15, the 11st 1/4inch gold
Belong to valve 17 to be weldingly connected by 1/4inch stainless steel tubing with the 2nd 1/2inch metal pipe line 59；First nickel reactant pipe 16 is adopted
It is used upwards with the tenth 1/4inch metal valve 15 with metal threaded cushioning circle sealing means by 1/4inch stainless steel tubing
The connection of cutting ferrule sealing means；11st 1/4inch metal valve 17 passes through 1/4inch stainless steel tubing and the second metal cold-trap 18
It is connected, the second metal cold-trap 18 is stainless by 1/4inch with third metal cold-trap 20 by the 12nd 1/4inch metal valve 19
Steel pipeline be connected, 21 both ends of the 13rd 1/4inch metal valve by 1/4inch stainless steel tubing respectively with third metal cold-trap
20 are connected with the first metal hot trap 22, and the first metal hot trap 22 is cold by the 14th 1/4inch metal valve 23 and the 4th metal
Trap 24 is connected by 1/4inch stainless steel tubing, and 25 one end of the 15th 1/4inch metal valve is connected with the 4th metal cold-trap 24
The other end is connected with 1/4inch threeway, and threeway is connected with the 16th 1/4inch metal valve 26 upwards, passes through 1/4inch to the right
Stainless steel tubing is connected with another 1/4inch threeway, another 1/4inch threeway downwards with the 17th 1/4inch metal valve 27
One end is connected, and is connected with first " VCO " quick coupling, 29 one end to the right, and first " VCO " quick coupling, 29 other end passes through the tenth
Eight 1/4inch metal valves 30 and the first stainless steelMolecular sieve collecting pipe 31 is connected by 1/4inch stainless steel tubing, the
17 1/4inch metal valve, 27 other end passes through 1/4inch stainless steel tube wire bonding phase with first capacitor vacuum gauge 28 downwards
Even, the 16th 1/4inch metal valve 26 and the 31st 1/4inch metal valve 57 pass through 1/4inch metal pipe line and three
It is logical to be connected, threeway pass through to the right 1/4inch metal pipe line by the 25th 1/4inch metal valve 45 and second set of extraction,
Separation, purifying, collection system are connected；Second set of oxygen isotope sample extracting and developing, purifying, the component of collection system and connection
Mode is identical as first set；
Waste treatment system includes that the 2nd 1/4inch metal valve 3 is connected with waste line to the left, the first 1/4inch gold
Belong to the air inlet that valve 2 provides the rotary-vane pump 1 of whole system low vacuum simultaneously with abstraction reactor off-gas object upwards
It is connected, the first metal cold-trap 4 is connected with the 3rd 1/4inch metal valve 5 to the right, the 5th 1/4inch metal valve 8 and the 6th 1/
9 co- controlling of 4inch metal valve enters system for purging the Ar throughput of Litter.
The whole system metal pipe line all uses 316 type stainless steel materials, and pipeline inner wall passes through special polishing treatment,
Pipeline in addition to metal cold-trap all winds heating tape.
It is describedIt is to collect oxygen by liquid nitrogen frozen in 3/8inch stainless steel tube that molecular sieve, which is filled in outer diameter,.
A kind of extracting method for oxygen isotope composition analysis in rock and mineral, this method specifically include following step
It is rapid:
Step 1, sample introduction
It closes the tenth 1/4inch metal valve 15 and the good oxygen-containing rock of pre-treatment or mineral samplers is packed into the first nickel reactant
Bottom of the tube and access system complete sample introduction operation；
Step 2, vacuum degassing is toasted to whole system
First nickel reactant pipe 16 is put on into digital temperature control heating furnace, slowly opens the tenth 1/4inch metal valve 15, second
1/2inch metal valve 32, the first 1/2inch metal valve 14, the 4th 1/4inch metal valve 7, in the first metal cold-trap 4
Put on slow 3rd 1/4inch metal valve 5 after liquid nitrogen cup, the first 1/4inch metal valve 2 connects rotary-vane pump
1 takes out low vacuum for system, opens the 9th 1/4inch metal valve 13, sets the temperature of digital temperature control heating furnace as 120 DEG C, beat
Opening heating charged is after whole system heats degassing 30min, the 3rd 1/4inch metal valve 5 to be closed, by the 8th metal cold-trap
52 put on liquid nitrogen cup, open the 29th 1/4inch metal valve 53 and connect turbine point with the 30th 1/4inch metal valve 55
Son pump 56 takes out system high vacuum by the monitoring system condition of high vacuum degree of compound vacuum gauge 54 and reaches 10-5Continue to take out 30min after Pa；
Step 3, brominated bromide agent transfer and fluorination reaction
After the completion of system vacuum degassing, remove temperature control heating furnace, nickel reactant pipe sleeve upper circulation water and with liquid nitrogen cup it is abundant
Freezing, closing the tenth 1/4inch metal valve 15, the 11st 1/4inch metal valve 17, the 9th 1/4inch metal valve 13,
28th 1/4inch metal valve 51 opens the 8th 1/4inch metal valve 11, semi-open 9th 1/4inch metal valve
13 and by pressure vacuum gauge 6 monitoring be diffused into the first 1/2inch stainless steel main pipeline 58 and the 2nd 1/2inch stainless steel supervisor
BrF in road 595Pressure values, reach reaction required for BrF5After dosage, the 9th 1/4inch metal valve 13 is closed, is opened
Tenth 1/4inch metal valve 15, by the BrF in pipeline5It is transferred in the first nickel reactant pipe 16 of freezing, repeating aforesaid operations can
Complete BrF in other nickel reactant pipes5Be transferred to, and take out system low vacuum and high vacuum again, condition of high vacuum degree is up to 10-5After Pa, close
Close the metal valve above each nickel reactant device.The liquid nitrogen cup outside nickel reactant pipe is removed, puts on digital temperature control heating after defrosting again
Furnace sets heating temperature according to sample type and carries out 12h fluorination reaction generation oxygen and other by-products；
Step 4, oxygen separation, purifying and collection
The temperature control heating furnace outside nickel reactant device is removed, liquid nitrogen cup is put on again and is sufficiently freezed, each cold-trap is sleeved on liquid
Nitrogen cup, and system is maintained to be in high vacuum state, close all metal valves.The tenth 1/4inch metal valve 15 is successively opened,
11st 1/4inch metal valve 17 opens the 12nd 1/4inch metal valve 19 after 2min, opens the 13rd after 2min
4inch metal valve 21 opens the 14th 1/4inch metal valve 23 after 5min, opens the 15th 1/4inch metal after 2min
Valve 25, the 17th 1/4inch metal valve 27 observe the unit by first capacitor vacuum gauge 28 and generate O2Amount opens the
18 1/4inch metal valves 30, O2Passed through sufficiently chilled first stainless steel of liquid nitrogenMolecular sieve collecting pipe adsorbs receipts
Collection, and absorptive collection state is observed by first capacitor vacuum gauge 28, capacitor vacuum gauge reading closes the 15th after no longer declining
1/4inch metal valve 25, the 17th 1/4inch metal valve 27 and the 18th 1/4inch metal valve 30, remove collecting pipe
Outer liquid nitrogen cup and collecting pipe is removed at first " VCO " quick coupling 29 together with the 18th 1/4inch metal valve 30 to
Isotopics analysis is carried out, the preparation of oxygen isotope sample is completed；
Step 5, waste is handled
O in nickel reactant device2After completing separation and collecting, remaining reagent and reaction product need to carry out nothing in reactor
Evilization processing, closes the 11st 1/4inch metal valve 17, opens the 2nd 1/2inch metal valve 32, unloads outside nickel reactant pipe
Cooling water system put on temperature control heating furnace again, adjust 150 DEG C and it heated, open the metal valve above nickel reactant pipe
Door, the waste in nickel reactant device is transferred in the first metal cold-trap 4, closes the first 1/2inch metal valve 14, opens the 5th
1/4inch metal valve 8, the 6th 1/4inch metal valve 9 remove the liquid nitrogen outside the first metal cold-trap 4, open the 2nd 1/
Waste is downloaded in the lime bucket in ventilating kitchen by 4inch metal valve 3 with Ar fate, is completed Waste disposal and is avoided pollution ring
Border.
Claims (12)
1. oxygen isotope composition analysis extraction element in a kind of rock and mineral, it is characterised in that: including waste treatment system,
The one vertical main pipeline of 1/2inch stainless steel (58) and 12 sets of identical oxygen isotope sample extracting and developings, collect system at purifying
System；
Pressure vacuum gauge (6) 1/4inch stainless steel tube is connect with the 4th 1/4inch metal valve (7) by cutting ferrule downwards, the
Four 1/4inch metal valve (7) lower end 1/4inch stainless steel tubes and the first vertical main pipeline of 1/2inch stainless steel (58) are logical
It crosses and is weldingly connected, vertical main pipeline (58) is vertically connected with the 2nd 1/2inch metal pipe line (59) by welding, between two pipelines
On-off is controlled by the first 1/2inch metal valve (14)；
Brominated bromide steel cylinder is connected by welding by 1/4inch metal pipe line with vertical main pipeline (58), 1/4inch metal tube
Line is equipped with the 7th 1/4inch metal valve (10) and the 9th 1/4inch metal valve (13), the 7th 1/4inch metal valve
(10) the 1/4inch metal pipe line between the 9th 1/4inch metal valve (13) is equipped with threeway, and threeway is sequentially connected downwards
There are the 8th 1/4inch metal valve (11) and brominated bromide storage cylinder (12)；
Turbomolecular pump (56) is weldingly connected by 1/4inch stainless steel tubing with the first 1/2inch stainless steel tubing (58), the
One 1/2inch stainless steel tubing (58) is disposed with the 28th 1/4inch metal valve between turbomolecular pump (56)
(51), the 8th metal cold-trap (52), the 29th 1/4inch metal valve (53), the 30th 1/4inch metal valve (55),
Threeway is equipped between 28th 1/4inch metal valve (51) and the 8th metal cold-trap (52), third crosses 1/4inch gold all
Belong to pipeline to connect with the 31st 1/4inch metal valve (57), the 29th 1/4inch metal valve (53), the 30th
Threeway is equipped between 4inch metal valve (55), threeway is connected with downwards the first compound vacuum gauge (54).
2. oxygen isotope composition analysis extraction element in a kind of rock according to claim 1 and mineral, it is characterised in that:
The oxygen isotope sample extracting and developing, purifying, collection system include the tenth 1/4inch metal valve (15), the 11st
4inch metal valve (17) is weldingly connected by 1/4inch stainless steel tubing with the 2nd 1/2inch metal pipe line (59)；First
Nickel reactant pipe (16) using metal threaded cushioning circle sealing means by 1/4inch stainless steel tubing upwards with the tenth 1/4inch
Metal valve (15) is connected using cutting ferrule sealing means；11st 1/4inch metal valve (17) passes through 1/4inch stainless steel tube
Line is connected with the second metal cold-trap (18), and the second metal cold-trap (18) passes through the 12nd 1/4inch metal valve (19) and third
Metal cold-trap (20) is connected by 1/4inch stainless steel tubing, and the 13rd 1/4inch metal valve (21) both ends pass through 1/
4inch stainless steel tubing is connected with third metal cold-trap (20) and the first metal hot trap (22) respectively, the first metal hot trap (22)
It is connected with the 4th metal cold-trap (24) by 1/4inch stainless steel tubing by the 14th 1/4inch metal valve (23), the tenth
Five 1/4inch metal valve (25) one end other end that is connected with the 4th metal cold-trap (24) is connected with 1/4inch threeway, and three lead to
It is upper to be connected with the 16th 1/4inch metal valve (26), pass through 1/4inch stainless steel tubing and another 1/4inch threeway to the right
It is connected, another 1/4inch threeway is connected with the 17th 1/4inch metal valve (27) one end downwards, fast with first " VCO " to the right
Quick coupling (29) one end be connected, first " VCO " quick coupling (29) other end by the 18th 1/4inch metal valve (30) with
First stainless steelMolecular sieve collecting pipe (31) is connected by 1/4inch stainless steel tubing, the 17th 1/4inch metal valve
(27) other end is weldingly connected with first capacitor vacuum gauge (28) by 1/4inch stainless steel tubing downwards, the 16th 1/4inch
Metal valve (26) is connected by 1/4inch metal pipe line with threeway with the 31st 1/4inch metal valve (57), and three lead to
The right side is by 1/4inch metal pipe line by the 25th 1/4inch metal valve (45) and a separate set of extracting and developing, purifying, receipts
Collecting system is connected；A separate set of oxygen isotope sample extracting and developing, purifying, the component of collection system and connection type and first set
It is identical.
3. oxygen isotope composition analysis extraction element in a kind of rock according to claim 2 and mineral, it is characterised in that:
Extracting and developing, purifying, collection system are controlled by the 2nd 1/2inch metal valve (32).
4. oxygen isotope composition analysis extraction element in a kind of rock according to claim 3 and mineral, it is characterised in that:
The waste treatment system includes that the 2nd 1/4inch metal valve (3) is connected with waste line to the left, the first 1/4inch metal
Valve (2) provides the air inlet of the rotary-vane pump (1) of whole system low vacuum simultaneously with abstraction reactor off-gas object upwards
Mouth is connected, and the first metal cold-trap (4) is connected with the 3rd 1/4inch metal valve (5) to the right, the 5th 1/4inch metal valve (8)
Enter system for purging the Ar throughput of Litter with the 6th 1/4inch metal valve (9) co- controlling.
5. oxygen isotope composition analysis extraction element in a kind of rock according to claim 4 and mineral, it is characterised in that:
The whole system metal pipe line all uses 316 type stainless steel materials, and pipeline inner wall passes through special polishing treatment, except metal is cold
Pipeline outside trap all winds heating tape.
6. oxygen isotope composition analysis extraction element in a kind of rock according to claim 5 and mineral, it is characterised in that:
It is describedIt is to collect oxygen by liquid nitrogen frozen in 3/8inch stainless steel tube that molecular sieve, which is filled in outer diameter,.
7. a kind of extracting method for oxygen isotope composition analysis in rock and mineral, characterized by the following steps:
Step (1), sample introduction；Step (2) toasts vacuum degassing to whole system；Step (3), brominated bromide agent transfer and fluorination are anti-
It answers；Step (4), oxygen separation, purifying and collection；Step (5), waste processing.
8. a kind of extracting method for oxygen isotope composition analysis in rock and mineral according to claim 7, special
Sign is: the step (1) specifically: closes the tenth 1/4inch metal valve (15) for the good oxygen-containing rock of pre-treatment or mine
Object sample is packed into the first nickel reactant bottom of the tube and access system, completes sample introduction operation.
9. a kind of extracting method for oxygen isotope composition analysis in rock and mineral according to claim 8, special
Sign is: the step (2) specifically: the first nickel reactant pipe (16) is put on digital temperature control heating furnace, slowly opens the 10th
4inch metal valve (15), the 2nd 1/2inch metal valve (32), the first 1/2inch metal valve (14), the 4th 1/4inch
Metal valve (7), slow 3rd 1/4inch metal valve (5), the 1st after the first metal cold-trap (4) puts on liquid nitrogen cup
It is that system takes out low vacuum that 4inch metal valve (2), which connects rotary-vane pump (1), opens the 9th 1/4inch metal valve
(13), the temperature of digital temperature control heating furnace is set as 120 DEG C, after opening heating charged as whole system heating degassing 30min,
The 3rd 1/4inch metal valve (5) is closed, the 8th metal cold-trap (52) is put on into liquid nitrogen cup, opens the 29th 1/4inch gold
Belong to valve (53) to connect turbomolecular pump (56) with the 30th 1/4inch metal valve (55), pumping system high vacuum passes through compound
Vacuum meter (54) monitoring system condition of high vacuum degree reaches 10-5Continue to take out 30min after Pa.
10. a kind of extracting method for oxygen isotope composition analysis in rock and mineral according to claim 9, special
Sign is: the step (3) specifically: after the completion of system vacuum degassing, remove temperature control heating furnace, recycle on nickel reactant pipe sleeve
Water is simultaneously sufficiently freezed with liquid nitrogen cup, closes the tenth 1/4inch metal valve (15), the 11st 1/4inch metal valve (17), the
Nine 1/4inch metal valves (13), the 28th 1/4inch metal valve (51) open the 8th 1/4inch metal valve
(11), semi-open 9th 1/4inch metal valve (13) and by pressure vacuum gauge (6) monitoring be diffused into the first 1/2inch not
BrF in rust steel main pipeline (58) and the 2nd 1/2inch stainless steel main pipeline (59)5Pressure values, reach required for reaction
BrF5After dosage, the 9th 1/4inch metal valve (13) is closed, opens the tenth 1/4inch metal valve (15), it will be in pipeline
BrF5It is transferred in the first nickel reactant pipe (16) of freezing, repeats BrF in other achievable nickel reactant pipes of aforesaid operations5Be transferred to, and
Take out system low vacuum and high vacuum again, condition of high vacuum degree is up to 10-5After Pa, the metal valve above each nickel reactant device is closed；It removes
Liquid nitrogen cup outside nickel reactant pipe puts on digital temperature control heating furnace according to sample type again and sets heating temperature progress after defrosting
12h fluorination reaction generates oxygen and other by-products.
11. a kind of extracting method for oxygen isotope composition analysis in rock and mineral according to claim 10,
It is characterized in that: the step (4) specifically: remove the temperature control heating furnace outside nickel reactant device, put on liquid nitrogen cup again and carry out sufficiently
Freezing, each cold-trap is sleeved on liquid nitrogen cup, and system is maintained to be in high vacuum state, closes all metal valves；Successively open
Ten 1/4inch metal valves (15), the 11st 1/4inch metal valve (17) open the 12nd 1/4inch metal valve after 2min
Door (19) opens the 13rd 1/4inch metal valve (21) after 2min, opens the 14th 1/4inch metal valve after 5min
(23), the 15th 1/4inch metal valve (25), the 17th 1/4inch metal valve (27) are opened after 2min, pass through the first electricity
Hold vacuum gauge (28) and observes unit generation O2Amount opens the 18th 1/4inch metal valve (30), O2By abundant by liquid nitrogen
First stainless steel of freezingMolecular sieve collecting pipe institute absorptive collection, and received by first capacitor vacuum gauge (28) observation absorption
Collection state, capacitor vacuum gauge reading close the 15th 1/4inch metal valve (25), the 17th 1/4inch gold after no longer declining
Belong to valve (27) and the 18th 1/4inch metal valve (30), removes the liquid nitrogen cup outside collecting pipe and by collecting pipe together with the tenth
Eight 1/4inch metal valves (30) remove pending isotopics analysis at first " VCO " quick coupling (29), complete oxygen
The preparation of isotope sample.
12. a kind of extracting method for oxygen isotope composition analysis in rock and mineral according to claim 11,
It is characterized in that: the step (5) specifically: the O in nickel reactant device2After completing separation and collecting, remaining reagent in reactor
And reaction product needs to carry out harmless treatment, closes the 11st 1/4inch metal valve (17), opens the 2nd 1/2inch gold
Belong to valve (32), unloads the cooling water system outside nickel reactant pipe and put on temperature control heating furnace again, adjust 150 DEG C and it is added
Heat opens the metal valve above nickel reactant pipe, the waste in nickel reactant device is transferred in the first metal cold-trap (4), closes
First 1/2inch metal valve (14), opens the 5th 1/4inch metal valve (8), and the 6th 1/4inch metal valve (9) is removed
The liquid nitrogen of the first metal cold-trap (4) outside is removed, the 2nd 1/4inch metal valve (3) is opened, waste is downloaded to ventilating kitchen with Ar fate
In interior lime bucket, completes Waste disposal and avoid pollution environment.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115060783A (en) * | 2022-08-16 | 2022-09-16 | 中国科学院地质与地球物理研究所 | Carbonate total oxygen isotope measuring system and measuring method thereof |
Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3953568A (en) * | 1971-07-22 | 1976-04-27 | Maomi Seko | Method of simultaneous concentration and dilution of isotopes |
| IL106066A0 (en) * | 1993-06-18 | 1993-10-20 | Univ Ramot | Method of measuring the 17o content and distribution in a body |
| US20040235186A1 (en) * | 2002-07-16 | 2004-11-25 | President And Fellows Of Harvard College | Non-affinity based isotope tagged peptides and methods for using the same |
| CN103675087A (en) * | 2013-12-20 | 2014-03-26 | 中国科学院地质与地球物理研究所 | Analytic method of oxygen isotopes in sulfate radicals |
| CN107063784A (en) * | 2016-10-31 | 2017-08-18 | 核工业北京地质研究院 | It is a kind of to be used for the extraction purification system and its method for extraction and purification of dissolving xenon in water |
| CN107144624A (en) * | 2017-05-15 | 2017-09-08 | 中国科学院生态环境研究中心 | The method for screening silica dioxide granule source |
| CN107422024A (en) * | 2017-08-03 | 2017-12-01 | 核工业北京地质研究院 | The analysis system and method for not oxygen-containing mineral inclusion water oxygen isotopics |
| CN207379974U (en) * | 2017-08-03 | 2018-05-18 | 核工业北京地质研究院 | The analysis system of not oxygen-containing mineral inclusion water oxygen isotopics |
| CN207457129U (en) * | 2017-08-03 | 2018-06-05 | 核工业北京地质研究院 | High temperature refractory mineral laser-BrF5Method oxygen isotope composition analysis system |
| 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 |
| JP2019059650A (en) * | 2017-09-27 | 2019-04-18 | 大陽日酸株式会社 | Oxygen isotope substitution method and oxygen isotope substitution device |
| CN211318298U (en) * | 2019-04-30 | 2020-08-21 | 核工业北京地质研究院 | Oxygen isotope composition analysis extraction element in rock and mineral |
-
2019
- 2019-04-30 CN CN201910359063.9A patent/CN110031536B/en active Active
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3953568A (en) * | 1971-07-22 | 1976-04-27 | Maomi Seko | Method of simultaneous concentration and dilution of isotopes |
| IL106066A0 (en) * | 1993-06-18 | 1993-10-20 | Univ Ramot | Method of measuring the 17o content and distribution in a body |
| US20040235186A1 (en) * | 2002-07-16 | 2004-11-25 | President And Fellows Of Harvard College | Non-affinity based isotope tagged peptides and methods for using the same |
| CN103675087A (en) * | 2013-12-20 | 2014-03-26 | 中国科学院地质与地球物理研究所 | Analytic method of oxygen isotopes in sulfate radicals |
| CN107063784A (en) * | 2016-10-31 | 2017-08-18 | 核工业北京地质研究院 | It is a kind of to be used for the extraction purification system and its method for extraction and purification of dissolving xenon in water |
| CN107144624A (en) * | 2017-05-15 | 2017-09-08 | 中国科学院生态环境研究中心 | The method for screening silica dioxide granule source |
| CN107422024A (en) * | 2017-08-03 | 2017-12-01 | 核工业北京地质研究院 | The analysis system and method for not oxygen-containing mineral inclusion water oxygen isotopics |
| CN207379974U (en) * | 2017-08-03 | 2018-05-18 | 核工业北京地质研究院 | The analysis system of not oxygen-containing mineral inclusion water oxygen isotopics |
| CN207457129U (en) * | 2017-08-03 | 2018-06-05 | 核工业北京地质研究院 | High temperature refractory mineral laser-BrF5Method oxygen isotope composition analysis system |
| JP2019059650A (en) * | 2017-09-27 | 2019-04-18 | 大陽日酸株式会社 | Oxygen isotope substitution method and oxygen isotope substitution device |
| 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 |
| CN211318298U (en) * | 2019-04-30 | 2020-08-21 | 核工业北京地质研究院 | Oxygen isotope composition analysis extraction element in rock and mineral |
Non-Patent Citations (5)
| Title |
|---|
| BI QF 等: "The microbial cycling of phosphorus on long-term fertilized soil:Insights from phosphate oxygen isotope ratios", 《CHEMICAL GEOLOGY》, vol. 483, pages 56 - 64 * |
| CHAPLIGIN B 等: "A high-performance, safer and semi-automated approach for the δ18O analysis of diatom silica and new methods for removing exchangeable oxygen", 《RAPID COMMUNICATIONS IN MASS SPECTROMETRY》, vol. 24, no. 17, pages 2655 - 2664 * |
| 刘熙 等: "利用激光氟化系统分析硅酸盐矿物的三氧同位素组成", 《矿物岩石地球化学通报》, vol. 35, no. 03, pages 448 - 453 * |
| 张建锋 等: "铀矿物中的氧同位素分析装置及方法", 《中国核科学技术进展报告》, vol. 6, pages 35 - 43 * |
| 李铁军 等: "氧同位素在岩石成因研究的新进展", 《岩矿测试》, vol. 32, no. 06, pages 13 - 26 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115060783A (en) * | 2022-08-16 | 2022-09-16 | 中国科学院地质与地球物理研究所 | Carbonate total oxygen isotope measuring system and measuring method thereof |
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