CN208766030U - Fluid inclusion carbon and hydrogen isotope analysis system for minerals difficult to thermally decompose - Google Patents
Fluid inclusion carbon and hydrogen isotope analysis system for minerals difficult to thermally decompose Download PDFInfo
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- CN208766030U CN208766030U CN201821502242.0U CN201821502242U CN208766030U CN 208766030 U CN208766030 U CN 208766030U CN 201821502242 U CN201821502242 U CN 201821502242U CN 208766030 U CN208766030 U CN 208766030U
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 107
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 107
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 229910052500 inorganic mineral Inorganic materials 0.000 title claims abstract description 56
- 239000011707 mineral Substances 0.000 title claims abstract description 56
- 238000004458 analytical method Methods 0.000 title claims abstract description 26
- 239000012530 fluid Substances 0.000 title claims abstract description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims description 15
- 229910052799 carbon Inorganic materials 0.000 title claims description 15
- 238000004880 explosion Methods 0.000 claims abstract description 60
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 55
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000005751 Copper oxide Substances 0.000 claims abstract description 30
- 229910000431 copper oxide Inorganic materials 0.000 claims abstract description 30
- 238000004519 manufacturing process Methods 0.000 claims abstract description 29
- 230000009467 reduction Effects 0.000 claims abstract description 24
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 59
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 43
- 238000005086 pumping Methods 0.000 claims description 39
- 238000005422 blasting Methods 0.000 claims description 38
- 239000001569 carbon dioxide Substances 0.000 claims description 25
- 238000000746 purification Methods 0.000 claims description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 7
- 239000007789 gas Substances 0.000 abstract description 66
- 238000012360 testing method Methods 0.000 abstract description 34
- 238000006243 chemical reaction Methods 0.000 abstract description 29
- 239000004215 Carbon black (E152) Substances 0.000 abstract description 5
- 229930195733 hydrocarbon Natural products 0.000 abstract description 5
- 150000002430 hydrocarbons Chemical class 0.000 abstract description 4
- 238000002474 experimental method Methods 0.000 abstract description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052725 zinc Inorganic materials 0.000 abstract description 2
- 239000011701 zinc Substances 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract 1
- 238000005979 thermal decomposition reaction Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 50
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 42
- 238000006722 reduction reaction Methods 0.000 description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 27
- 229960004424 carbon dioxide Drugs 0.000 description 23
- 239000007788 liquid Substances 0.000 description 22
- 229910052757 nitrogen Inorganic materials 0.000 description 21
- 238000010438 heat treatment Methods 0.000 description 19
- 239000010453 quartz Substances 0.000 description 16
- 230000008569 process Effects 0.000 description 14
- 239000000203 mixture Substances 0.000 description 11
- 150000002431 hydrogen Chemical class 0.000 description 9
- 238000001819 mass spectrum Methods 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 238000011068 loading method Methods 0.000 description 8
- 238000010926 purge Methods 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 235000011089 carbon dioxide Nutrition 0.000 description 5
- 238000007710 freezing Methods 0.000 description 5
- 230000008014 freezing Effects 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 239000011651 chromium Substances 0.000 description 4
- COUNCWOLUGAQQG-UHFFFAOYSA-N copper;hydrogen peroxide Chemical compound [Cu].OO COUNCWOLUGAQQG-UHFFFAOYSA-N 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000010998 test method Methods 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000006479 redox reaction Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 241000190070 Sarracenia purpurea Species 0.000 description 2
- GCNLQHANGFOQKY-UHFFFAOYSA-N [C+4].[O-2].[O-2].[Ti+4] Chemical compound [C+4].[O-2].[O-2].[Ti+4] GCNLQHANGFOQKY-UHFFFAOYSA-N 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 230000009172 bursting Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002223 garnet Substances 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000002307 isotope ratio mass spectrometry Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 241000894007 species Species 0.000 description 2
- 238000012956 testing procedure Methods 0.000 description 2
- 229910001428 transition metal ion Inorganic materials 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 210000000476 body water Anatomy 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 239000008246 gaseous mixture Substances 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 125000001183 hydrocarbyl group Chemical group 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000000155 isotopic effect Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004901 spalling Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 210000003462 vein Anatomy 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Landscapes
- Sampling And Sample Adjustment (AREA)
Abstract
The utility model provides a hydrocarbon isotope analytic system of fluid inclusion of difficult thermal decomposition mineral. The system provided by the utility model uses the fixed chromium powder furnace to replace the movable chromium powder reaction tube or the traditional zinc particle furnace, so that the hydrogen production reaction is rapid and complete; the copper oxide furnace is integrated into the system, the function of collecting hydrocarbon by the copper oxide furnace can be utilized, and meanwhile, the test step without passing through the copper oxide furnace is simplified; the thermal explosion gas taking and the chromium powder reduction hydrogen production are designed into two units which are relatively independent and are connected, so that the experiment is conveniently arranged, the time is saved, and the thermal explosion gas taking of the current sample and the reduction hydrogen production of the previous sample are carried out simultaneously. The system is used for analyzing the hydrocarbon isotope of the mineral fluid inclusion, and has high analysis precision, good repeatability and simple operation.
Description
Technical field
The utility model relates to the technical field of analysis detection, in particular to a kind of Fluid inclusions for being not easy to thermally decompose mineral
Body carbon, hydrogen isotope analysis system.
Background technique
Mineral fluid inclusions are the mineral crystal diagenesis of trap or BIFhosted gold deposits by crystal defect during the growth process.
The original fluid in its host forming process is represented just because of fluid inclusion, contains the initial shape of the mineral abundant
At when physical chemistry information, its ingredient (including Element and isotope composition) and phase research is always geoscience, ring
The very important research contents of the subjects such as border science.
Mineral fluid inclusions Stable Isotopic Analysis has two class methods at present: one is the offline of traditional two-way sample introduction
That is, under vacuum conditions analytic approach discharges the gas and liquid in inclusion enclave using various methods (burst, crush and grind)
Body, then by separation, purification and redox reaction, gas can be tested (for example, H by finally collecting2And CO2Gas), using double
The mode of road sample introduction (duel inlet) enters gas isotope than mass spectrograph (IRMS, Isotope Ratio Mass
Spectrometry it) is detected；Another kind is the on-line analysis method of the continuous flow sample introduction to grow up in recent years, this method
Exactly using in elemental analyser (instrument model: Flash 2000HT) high temperature (temperature is at 2100 DEG C or so) cracking inclusion enclave
Water generates hydrogen, is then directly entered matter by chromatography post separation and with the sample introduction mode of continuous flow (continuous flow)
Spectrum is tested.The latter, instead of the former cumbersome sample making course, takes continuous flow directly to carry out mass spectrum using elemental analyser
Sample introduction, so that this method is simple, quick, few with sample amount.But the disadvantages of the method are as follows hydrogen isotope can only be analyzed, because with
The few and representative difference of sample amount, and its analysis precision is not so good as traditional two-way sampling system.In addition, continuous flow sample introduction on-line analysis method
The shortcomings that there are one cannot ignore is to need constantly to clear up in elemental analyser to react remaining mineral residue (general one
It is secondary to test 20 or so samples, not as water sample can be several hundred with follow-on test), not so influence the test of subsequent sample.
In order to solve the problems, such as the mineral residue cleaning of continuous flow sample introduction on-line testing method, Chinese Academy of Sciences's geology and the earth
Hydrogen isotope analysis system (the patent No.: CN 104222728 in a kind of fluid inclusion water of a system-is invented by physics Institute
A).The basic fundamental of the patent is exactly that both the above method is combined, and is worked first with two-way sample introduction pre-treatment mineral
Water in inclusion enclave bursts out, then by sealing up for safekeeping in capillary after purification processes, enters finally by solid sampler
Elemental analyser carries out the test of hydrogen isotope using continuous flow mode.The system being reduced to 0.3g from 3g with sample amount,
But since the technology is the split of two methods, so having the shortcomings that two methods simultaneously: both not reaching two-way sample introduction
The measuring accuracy of mode, entire test process are again complicated cumbersome, time-consuming more；There is no the reduction of matter with sample amount, and is only capable of testing
Hydrogen isotope.
In November, 2017, Inst of Geology and Geophysics, Chinese Academy of Sciences has applied for a new continuous flow sample introduction again
The method (patent No.: 108072713 A of CN) of hydrogen isotope in on-line analysis-on-line analysis fluid inclusion water.The skill
Art is to discharge the water in mineral fluid inclusions using flash burn method (being substantially thermal explosion method), and generate oxygen at high temperature with chromium powder
Change reduction reaction generate the gaseous mixture containing hydrogen, then using chromatographic column and cold-trap separation, enrichment and purifying hydrogen of hydrogen, finally with
The mode of continuous flow is brought mass spectrum into carrier gas and is tested.The patent is contained unlike a patent thereon with what is quickly heated
Chromium powder reaction tube replaces the pyroreaction pyrolysis furnace of the carbon granule containing glass of elemental analyser, the mineral residue after reaction may be not present
Cleaning problem.But due to there is the presence of chromium powder reaction tube, vacuumize system very time-consuming, and chromium powder is easy to extract out
Reaction tube pollutes the entirety of system.
At the beginning of 2017, Inst of Geology and Geophysics, Chinese Academy of Sciences has applied for a two-way off-line test method
The method (patent No.: 106769346 A of CN) of hydrogen isotope in patent-analysis water.The basic thought of the patent is using chromium powder
Hydrogen making is reacted with water at high temperature, hydrogen is then regathered and carries out the offline mass spectrometric measurement of two-way.The advantages of technology be with
Chromium powder replaces zinc granule to keep hydrogen production reaction complete, time saving；And the reaction is carried out in the Muffle furnace being detached under vacuum condition,
It is easy to operate easily controllable.The shortcomings that patented technology, is: 1) method that the patent is fetched water without reference to mineral fluid inclusions；
2) it before the first collecting pipe equipped with water sample being put into the second collecting pipe containing chromium powder and sealed, needs to vacuumize, but to containing
When having the test tube of chromium powder to vacuumize or vacuum does not reach requirement or chromium powder is taken away, is difficult to realize experiment purpose；3) chromium
Powder is reacted with water at high temperature generally also generates other gases, which just directly surveys into mass spectrum without purification processes
Examination, this not only influences measuring accuracy, and impact analysis system vacuum and reduction mass spectrum burn-out life；4) chromium powder high temperature and water are anti-
It is disposable for answering the collecting pipe of hydrogen manufacturing, and to make fully reacting, provides excessive chromium powder every time, this leads to the wave of experimental material
Take；5) technology repeatedly uses sealing, this requires laboratory technician relatively high, it is necessary to grasp high temperature welding gun using technology, and make
The cumbersome time-consuming of whole experiment process.
Utility model content
In view of this, the utility model aim is to provide a kind of hydrocarbon same position of fluid inclusion for being not easy to thermally decompose mineral
Plain analysis system, system operatio provided by the utility model is simple, can take gas and hydrogen manufacturing by the independent thermal explosion that is respectively completed simultaneously
Two processes, and precision is high, high-efficient.
In order to realize above-mentioned purpose of utility model, the utility model the following technical schemes are provided:
It is a kind of to be not easy to thermally decompose the fluid inclusion carbon of mineral, hydrogen isotope analysis system, including thermal explosion-collection and purifying
System, reduction hydrogen manufacturing and collection system and vacuum-control(led) system；
Thermal explosion-the collection and purification system include the blasting cartridge being sequentially connected in series on pipeline, the first cold-trap and titanium dioxide
Carbon collecting pipe is disposed with the 13rd valve, the 12nd valve and the 11st valve between the blasting cartridge and the first cold-trap,
Copper oxide furnace is also parallel between 12nd valve and the 11st valve；First cold-trap and carbon dioxide collection pipe it
Between be provided with the tenth valve；
It further includes that explosion furnace is bursting the explosion boiler clothing when carrying out thermal explosion that the thermal explosion, which is collected with purification system,
Guan Shang；
The reduction hydrogen manufacturing and collection system include the cold finger being sequentially connected in series on pipeline, chromium powder furnace, the second cold-trap and hydrogen
Gas collecting pipe；The cold finger is connected on pipeline by the 7th valve；The 6th valve is provided between the cold finger and chromium powder furnace；
The 5th valve and third valve are disposed among second cold-trap and Hydrogen collection pipe；
Thermal explosion-the collection is connected to purification system and reduction hydrogen manufacturing with collection system by the 9th valve, the 9th valve
It is arranged between carbon dioxide collection pipe and cold finger；
The vacuum-control(led) system includes low vacuum extract system, fine pumping system, the first low vacuum table and second
Low vacuum table；The low vacuum extract system and fine pumping system pass through the 4th valve access pipeline；The high vacuum is taken out
The first valve is additionally provided between gas system and the 4th valve；Is provided between the low vacuum extract system and the 4th valve
Two valves；
4th valve and the 13rd valve are connected to form main vacuum-pumping pipeline；
9th valve is connected to main vacuum-pumping pipeline, and the 8th valve is provided on connecting pipeline；Described first is low
Vacuum meter is arranged between the 9th valve and the 8th valve；
The second low vacuum table is arranged between the 5th valve and third valve；5th valve and main vacuum-pumping tube
Road connection；
First valve, the second valve, third valve, the 8th valve and the tenth valve are two two-way valves；4th valve
Door, the 11st valve and the 12nd valve are three two-way valves；5th valve, the 6th valve, the 7th valve, the 9th valve and
13 valves are three triple valves.
Preferably, standard sample injector is additionally provided on the 6th valve.
Preferably, the material of the copper oxide furnace, chromium powder furnace and blasting cartridge is quartz glass.
The utility model provides a kind of fluid inclusion carbon-hydrogen isotopes analysis system for being not easy to thermally decompose mineral, including
Thermal explosion-collection and purification system, reduction hydrogen manufacturing and collection system and vacuum-control(led) system.System provided by the utility model is with admittedly
Fixed chromium powder furnace replaces movable chromium powder reaction tube to keep hydrogen production reaction quick and complete；Copper oxide furnace is incorporated to system, it can the same time-division
The composition of hydrocarbon two kinds of isotopes is analysed, while simplifying and being not required to the testing procedure by copper oxide furnace (as only tested quartz specimen packet
Body water phase hydrogen isotope is wrapped up in, can control by valve makes the vapor of purifying be directly entered subsequent chromium powder furnace)；Thermal explosion is taken gas
Relatively independent and connection two units are designed to chromium powder reduction hydrogen manufacturing, are tested convenient for overall arrangement, are saved the time, make current
The thermal explosion of sample takes the reduction hydrogen manufacturing of gas and a upper sample while carrying out；And system provided by the utility model only includes two
Cold-trap, process is simple, easy to operate.
Detailed description of the invention
Fig. 1 is the structure of the fluid inclusion carbon for being not easy to thermally decompose mineral of the utility model, hydrogen isotope analysis system
Schematic diagram；
In Fig. 1,2-1 blasting cartridge, the first cold-trap of 2-2,2-3 carbon dioxide collection pipe, 2-4 copper oxide furnace, 2-5 explosion furnace,
2-6 cold finger, 2-7 chromium powder furnace, the second cold-trap of 2-8,2-9 Hydrogen collection pipe, 2-10 low vacuum extract system, 2-11 fine pumping
System, 2-12 the first low vacuum table, 2-13 the second low vacuum table, 2-14 standard sample injector；
The first valve of 1-, the second valve of 2-, 3- third valve, the 4th valve of 4-, the 5th valve of 5-, the 6th valve of 6-, 7-
7th valve, the 8th valve of 8-, the 9th valve of 9-, the tenth valve of 10-, the 11st valve of 11-, the 12nd valve of 12-, 13-
13 valves.
Specific embodiment
The utility model provide it is a kind of be not easy to thermally decompose the fluid inclusion carbon of mineral, hydrogen isotope analysis system, tie
Structure is as shown in Figure 1, in Fig. 1,2-1 blasting cartridge, the first cold-trap of 2-2,2-3 carbon dioxide collection pipe, 2-4 copper oxide furnace, 2-5 explosion
Furnace, 2-6 cold finger, 2-7 chromium powder furnace, the second cold-trap of 2-8,2-9 Hydrogen collection pipe, 2-10 low vacuum extract system, 2-11 high vacuum
Extract system, 2-12 the first low vacuum table, 2-13 the second low vacuum table, 2-14 standard sample injector；
The first valve of 1-, the second valve of 2-, 3- third valve, the 4th valve of 4-, the 5th valve of 5-, the 6th valve of 6-, 7-
7th valve, the 8th valve of 8-, the 9th valve of 9-, the tenth valve of 10-, the 11st valve of 11-, the 12nd valve of 12-, 13-
13 valves.
It is provided by the utility model to be not easy to thermally decompose the fluid inclusion carbon of mineral, hydrogen isotope analysis system, including heat
It is quick-fried-to collect and purification system, reduction hydrogen manufacturing and collection system and vacuum-control(led) system；
Thermal explosion-the collection and purification system include the blasting cartridge being sequentially connected in series on pipeline, the first cold-trap and titanium dioxide
Carbon collecting pipe is disposed with the 13rd valve, the 12nd valve and the 11st valve between the blasting cartridge and the first cold-trap,
Copper oxide furnace is also parallel between 12nd valve and the 11st valve；First cold-trap and carbon dioxide collection pipe it
Between be provided with the tenth valve；
It further includes that explosion furnace is bursting the explosion boiler clothing when carrying out thermal explosion that the thermal explosion, which is collected with purification system,
Guan Shang；
The reduction hydrogen manufacturing and collection system include the cold finger being sequentially connected in series on pipeline, chromium powder furnace, the second cold-trap and hydrogen
Gas collecting pipe；The cold finger is connected on pipeline by the 7th valve；The 6th valve is provided between the cold finger and chromium powder furnace；
The 5th valve and third valve are disposed among second cold-trap and Hydrogen collection pipe；
Thermal explosion-the collection is connected to purification system and reduction hydrogen manufacturing with collection system by the 9th valve, the 9th valve
It is arranged between carbon dioxide collection pipe and cold finger；
The vacuum-control(led) system includes low vacuum extract system, fine pumping system, the first low vacuum table and second
Low vacuum table；The low vacuum extract system and fine pumping system pass through the 4th valve access pipeline；The high vacuum is taken out
The first valve is additionally provided between gas system and the 4th valve；Is provided between the low vacuum extract system and the 4th valve
Two valves；
4th valve and the 13rd valve are connected to form main vacuum-pumping pipeline；
9th valve is connected to main vacuum-pumping pipeline, and the 8th valve is provided on connecting pipeline；Described first is low
Vacuum meter is arranged between the 9th valve and the 8th valve；
The second low vacuum table is arranged between the 5th valve and third valve；5th valve and main vacuum-pumping tube
Road connection.
Thermal explosion-collection described in the utility model and purification system include blasting cartridge, in the present invention, the blasting cartridge
Material be preferably quartz glass；The utility model does not have particular/special requirement to the size of the blasting cartridge, uses art technology
The blasting cartridge of the known size of personnel.
Thermal explosion-collection described in the utility model and purification system include and concatenated first cold-trap of blasting cartridge.In this reality
In novel, the utility model does not have particular/special requirement to the shape design of first cold-trap, ripe using those skilled in the art
The cold-trap known.In the present invention, the 13rd valve, the tenth are disposed between the blasting cartridge and the first cold-trap
Two valves and the 11st valve.
In the present invention, it is also parallel with copper oxide furnace between the 11st valve and the 12nd valve, in this reality
In novel, the material of the copper oxide furnace is preferably quartz glass；In specific embodiment of the utility model, the oxidation
Copper furnace preferably includes air inlet pipe and an air outlet pipe, and the air inlet pipe protrudes into copper oxide furnace bottom, and escape pipe is located at copper oxide furnace roof portion,
To ensure going on smoothly for reaction in furnace.In the present invention, copper oxide is filled in the copper oxide furnace；The utility model
There is no particular/special requirement to the specific loadings of the copper oxide, it can be according to the access times of system and the amount of mineral samplers come really
Determine the loadings of copper oxide.When the only hydrogen isotope of test mineral package fluid, then pass through control the 11st valve and the tenth
Two valves make thermal explosion gas without copper dioxide furnace, to simplify testing procedure.In the present invention, the blasting cartridge passes through
13rd valve is connected on pipeline, and blasting cartridge can be dismantled when loading sample.
Thermal explosion-collection described in the utility model and purification system include that the carbon dioxide after being connected on the first cold-trap is received
Collector.In the present invention, the tenth valve is provided between first cold-trap and carbon dioxide collection pipe.It is practical new at this
In type, the carbon dioxide collection pipe is connected on pipeline by the tenth valve, collects CO2Afterwards, carbon dioxide collection pipe is removable
It unloads down.The utility model does not have particular/special requirement to the carbon dioxide collection pipe, uses well known to those skilled in the art two
Carbonoxide collecting pipe.
In the present invention, it further includes explosion furnace that the thermal explosion, which is collected with purification system,, will be described when carrying out thermal explosion
Boiler clothing burst on blasting cartridge；The utility model heats blasting cartridge using explosion furnace, and the temperature for the furnace that bursts is preferably by can
Become the control of silicon transformer.
In the present invention, it is mineral inclusion to be carried out thermal explosion and incited somebody to action that the thermal explosion, which collects the effect with purification system,
The gas produced is purified and is collected.
Reduction hydrogen manufacturing described in the utility model and collection system include cold finger.Structure of the utility model to the cold finger
There is no particular/special requirement, uses cold finger well known to those skilled in the art；The cold finger is connected to pipeline by the 7th valve
On；By the 7th valve may be implemented cold finger and pipeline be connected to or closing.
Reduction hydrogen manufacturing described in the utility model and collection system include the chromium powder furnace after being connected on cold finger.It is practical at this
In novel, the material of the chromium powder furnace is preferably quartz glass；The structure of the chromium powder furnace is preferably consistent with copper oxide furnace, herein
It repeats no more；Chromium powder is filled in the chromium powder furnace；It, can when chromium powder loadings are 120g in the embodiments of the present invention
With mineral sample 2000 or more for testing 2g.In the present invention, the 6th valve is provided between the cold finger and chromium powder furnace
Door realizes the connection or closing between cold finger and chromium powder furnace by the 6th valve.
In the present invention, it is preferably additionally provided with standard sample injector on the 6th valve, the standard sample injector is
Rotary L-type test tube, the L-type test tube has the hollow screw lid of rubber gasket, when preparing standard hydrogen, uses
Standard sample injector injects standard water into system.
Reduction hydrogen manufacturing described in the utility model and collection system include the second cold-trap after being connected on chromium powder furnace.At this
In utility model, the structure of second cold-trap is preferably consistent with the first cold-trap, and details are not described herein.
Reduction hydrogen manufacturing described in the utility model and collection system include the Hydrogen collection pipe after being connected on the second cold-trap.
In the present invention, it is preferably filled with active carbon in the Hydrogen collection pipe, to realize the collection to hydrogen.Described second is cold
The 5th valve and third valve are disposed in trap and Hydrogen collection pipe；Wherein third valve can control Hydrogen collection pipe and pipe
The connection or closing on road, the 5th valve are connected to main vacuum-pumping pipeline.
In the present invention, the reduction hydrogen manufacturing and the effect of collection system are to from thermal explosion collection and purification system
H2O is restored, and collects hydrogen.
In the present invention, the thermal explosion-collection and purification system and reduction hydrogen manufacturing and collection system pass through the 9th valve
Door connection, the 9th valve are arranged between carbon dioxide collection pipe and cold finger, and the 9th valve can control between two systems
Connection is closed.
Vacuum-control(led) system described in the utility model includes low vacuum extract system.In the present invention, described low
Vacuum-pumping system is preferably low vacuum mechanical pump；The operating pressure range of the low vacuum mechanical system is 105~10-2Pa。
Vacuum-control(led) system described in the utility model includes fine pumping system.In the present invention, the height
Vacuum-pumping system preferably includes concatenated fore pump and high vacuum metal diffusion pump；The work pressure of the high vacuum mechanical system
Strong range is 10-2~10-6Pa。
In the present invention, the low vacuum extract system and fine pumping system pass through the 4th valve access tube
Road；It is additionally provided with the first valve between the fine pumping system and the 4th valve, for controlling fine pumping system；Institute
It states and is provided with the second valve between low vacuum extract system and the 4th valve, for controlling low vacuum extract system.
In the present invention, the 4th valve and the 13rd valve are connected to form main vacuum-pumping pipeline.
In the present invention, the 9th valve is connected to main vacuum-pumping pipeline, and the 8th is provided on connecting pipeline
Valve；The first low vacuum table is provided between 9th valve and the 8th valve；Between 5th valve and third valve
It is provided with the second low vacuum table.In the present invention, two low vacuum tables are used for the low vacuum state of detection system.
In the present invention, the vacuum-control(led) system provides vacuum condition for reaction and detects physico in reaction
Learn change procedure.
In the present invention, first valve, the second valve, third valve, the 8th valve and the tenth valve are two
Branch two-way valve；The 11st valve of 4th valve and the 12nd valve are preferably three two-way valves；5th valve, the 6th valve,
Seven valves, the 9th valve and the 13rd valve are preferably three triple valves；The utility model by valve control thermal explosion-collection with
The circulation feelings of connection and gas in system between purification system, reduction hydrogen manufacturing and collection system and vacuum-control(led) system
Condition.
In the present invention, in addition to copper oxide furnace, chromium powder furnace and blasting cartridge, the material of all valves and pipe-line system
Preferably simple glass.
System provided by the utility model, which is directed to, is not easy the mineral that thermally decompose, to being not easy to thermally decompose the fluid inclusion of mineral
Carry out the collection of carbon, hydrogen, the test of further progress isotope.
When to being not easy to thermally decompose the fluid inclusion progress carbon, hydrogen isotope analysis of mineral, the utility model body is provided
System applied by the following method:
(1) vacuumize process is carried out to system；
(2) mineral samplers are fitted into blasting cartridge and carry out preheating purging, then carry out thermal expousure under vacuum conditions, produced
For raw thermal explosion gas by copper oxide furnace, generating includes CO2And H2The mixed gas of O, mixed gas carry out cold in the first cold-trap
Freeze and collects；
(3) carrying out the first heating to the first cold-trap makes the CO in the mixed gas2It discharges and is collected into carbon dioxide receipts
In collector；
H in the mixed gas is made to the second heating of the first cold-trap progress2O is transferred in cold finger；
(4) carrying out heating to cold finger makes H2O, which enters, carries out reduction reaction in chromium powder furnace, by obtained Hydrogen collection in hydrogen
In collecting pipe；
(5) carbon dioxide being collected into and hydrogen are subjected to mass spectrum two-way off-line test.
The utility model carries out vacuumize process to system.In the present invention, the vacuumize process preferably includes
The pumping low vacuum and pumping high vacuum successively carried out, specifically includes the following steps: the 4th valve of control make whole system only with it is low true
Empty pump gas system connectivity carries out pumping low vacuum；During taking out low vacuum, the 5th valve and the 6th valve are controlled, opens chromium powder
Furnace, so that gas miscellaneous in furnace be taken away；When the reading of the first low vacuum table and the second low vacuum table is 10Pa, the 4th valve is controlled
Whole system and fine pumping system connectivity is set to carry out pumping high vacuum.The utility model removes system pipeline by taking out low vacuum
In miscellaneous gas；Good vacuum condition is provided by pumping high vacuum for reaction.
After the completion of vacuumize process, mineral samplers are fitted into blasting cartridge and carry out preheating purging by the utility model, then exist
Thermal expousure is carried out under vacuum condition, for the thermal explosion gas of generation by copper oxide furnace, generating includes CO2And H2The mixed gas of O,
Mixed gas carries out condensation collection in the first cold-trap.In the present invention, the mineral are preferably the mine for being not easy to thermally decompose
Object；The temperature of the preheating purging is preferably 100~105 DEG C, and the time is preferably 20min；The utility model is preferably by blasting cartridge
It is dismantled from system, mineral samplers is fitted into blasting cartridge, then the blasting cartridge equipped with mineral samplers is put into vacuum system
Carry out preheating purging；The granularity of the mineral samplers is preferably 40~60 mesh, more preferably 50 mesh, the filling of the mineral samplers
Amount is preferably 3~5g, more preferably 4g；In specific embodiment of the utility model, mineral preferably are determined according to mineral species
The loadings of sample, e.g., for the mineral that magmatic hydrotherm is formed, mineral samplers loadings are preferably 3g, for epithermal and
Sedimentogenic mineral, mineral samplers loadings are preferably 5g；When only needing to test the hydrogen isotope of mineral, then mine
Object sample loadings halve on the basis of the above.
In the present invention, the temperature of the thermal expousure is preferably 500~650 DEG C, and the time is preferably 20min.This
Utility model preferably determines the actual temp of thermal expousure according to mineral species, such as high temperature mineral (garnet and magnetic iron ore
Deng), the temperature of thermal expousure is preferably 650 DEG C.During thermal expousure, mineral samplers burst, and release organic gas
Body, as thermal explosion gas.
For the thermal explosion gas of generation through copper dioxide furnace, generating includes CO2And H2The mixed gas of O.In the present invention,
The set temperature of the copper oxide furnace is preferably 600 DEG C；It include CH in thermal explosion gas4With the gases such as CO, the quilt in aoxidizing logical furnace
It is reduced to CO2And H2O, reaction equation are shown below:
CH4+ 4CuO=CO2+2H2O+4Cu；
CO+CuO=CO2+Cu。
In addition, for the mineral containing transition-metal ions, such as magnetic iron ore, garnet, Fe therein2+And/or Mn2+In height
Lower react with the water in inclusion enclave of temperature generates hydrogen, and hydrogen reacts in oxidation furnace and generates H2O, to prevent these hydrogen from escaping
It loses and causes isotope fractionation.Specific reaction equation are as follows: H2+ CuO=H2O+Cu。
In the present invention, freezing collection is carried out in the first cold-trap from the mixed gas come out in copper oxide furnace.?
In the utility model, the temperature that the freezing is collected is preferably -196 DEG C；The freezing collects temperature and passes through liquid nitrogen cooling first
Cold-trap reaches；, it is preferable to use liquid nitrogen glass holder lives the first cold-trap in specific embodiment of the utility model.At low temperature, H2O and
CO2It is frozen, collects in the first cold-trap, the gas not being frozen is preferably taken away by pumped vacuum systems, and impact analysis is avoided
As a result.
After carrying out vacuumize process to system, mineral samplers are fitted into blasting cartridge and carry out preheating purging by the utility model,
Then thermal expousure is carried out under vacuum conditions, and for the thermal explosion gas of generation by copper oxide furnace, generating includes CO2And H2The mixing of O
Gas, mixed gas carry out freezing collection in the first cold-trap.
In the present invention, above-mentioned steps are preferred specifically: when the reading of the first low vacuum table and the second low vacuum table
For 0Pa, and copper oxide furnace temperature reaches set temperature and loads onto explosion on the 13rd valve when explosion furnace reaches burst temperature
Pipe；Mineral samplers are filled in the blasting cartridge；
The 4th valve is controlled, connect whole system with low vacuum extract system, when two low vacuum meter readings are less than
When 10Pa, then controls the 4th valve and entire reaction system is connect with fine pumping system；When two low vacuum meter readings are
When 0Pa, the 8th valve of control, the 9th valve, the 11st valve, the 12nd valve and the 13rd valve, make the first low vacuum table,
First cold-trap, copper oxide furnace are connected to blasting cartridge, to carrying out preheating purging on blasting cartridge；Preheating terminates, and two vacuum meter readings
When for 0Pa, explosion boiler clothing on blasting cartridge, on liquid nitrogen glass holder to the first cold-trap, starts thermal expousure and simultaneously collect gas.
In the present invention, the preheating purging specifically: by preheating boiler clothing on blasting cartridge, preheating temperature pair is set
Mineral samplers are preheated in blasting cartridge, and the utility model does not have particular/special requirement to the type of preheating furnace, blasting cartridge can be made to reach
To the common heating furnace of preheating temperature.
After the completion of freezing is collected, the utility model, which carries out the first heating to the first cold-trap, makes the CO in mixed gas2Release
And it is collected into carbon dioxide collection pipe.In the present invention, the temperature of the first heating is preferably -70~-80 DEG C；Institute
The temperature for stating the first heating is preferably impregnated the first cold-trap by using dry ice-crude alcohol mixture and is reached；In the tool of the utility model
In body embodiment, the liquid nitrogen cup for entangling the first cold-trap is preferably replaced with into dry ice-crude alcohol mixture cup.In the present invention,
The temperature of the dry ice-crude alcohol mixture is about -70~-80 DEG C, and the first cold-trap is gradually warmed up, CO2It is changed into gas to be released
Out, H2O is then remained in the first cold-trap.The utility model makes the CO released by the tenth valve of control2It is collected into
CO2In collecting pipe, CO is collected2Time be preferably 5min.
CO2After collection, the utility model makes the H in mixed gas to the second heating of the first cold-trap progress2O is transferred to
In cold finger.In the present invention, the temperature of second heating is preferably room temperature；The temperature of second heating preferably passes through
The dry ice for impregnating the first cold-trap-crude alcohol mixture removal is reached；In specific embodiment of the utility model, by dry ice-wine
Smart mixture cup is removed.In the present invention, the initial temperature of the cold finger is preferably -196 DEG C；At the beginning of the cold finger
Beginning temperature is preferably reached by liquid nitrogen cooling, H2O is frozen in cold finger after releasing in the first cold-trap, to realize
H2The transfer of O；The H2The transfer time of O is preferably 5min；The H of the utility model2O transfer time mixes from by dry ice-alcohol
Object cup starts to calculate when removing.
The utility model, which carries out the first heating to the first cold-trap, makes the CO in thermal explosion gas2It discharges and is collected into carbon dioxide
In collecting pipe；H in thermal explosion gas is made to the second heating of the first cold-trap progress2O is transferred in cold finger.
In the present invention, preferably specifically: after thermal expousure, closing the 9th valve and the 11st valve makes to mix
Gas is closed to be defined in the first cold-trap；The 8th valve and the 9th valve are opened, the gas not freezed by liquid nitrogen in the first cold-trap
Body is taken away；The 9th valve is turned off, the liquid nitrogen cup outside the first cold-trap is changed into dry ice crude alcohol mixture cup, is made in the first cold-trap
CO2It releases, and is collected into the CO below the tenth valve2In sample collection tube；Collect CO2After, then open the 9th valve
Door, pumps the gas not freezed again；Controlling the 9th valve and the 7th valve is connected to the first cold-trap only with cold finger, removes
Cold finger, is put on liquid nitrogen cup by the dry ice crude alcohol mixture cup outside one cold-trap, by the H in the first cold-trap2O is transferred in cold finger.
H2After O is shifted, the utility model, which carries out heating to cold finger, makes H2O, which enters, carries out reduction reaction in chromium powder furnace, will
Obtained Hydrogen collection is in Hydrogen collection pipe.In the present invention, the heating final temperature of the cold finger is preferably 40~60 DEG C,
More preferably 50 DEG C；The heating of the cold finger is reached by using hot-water soak cold finger, in specific embodiment of the utility model
In, it is preferable to use temperature is that 40~60 DEG C of hot water cup entangles cold finger.
After cold finger heating, H2O, which is released and enters, carries out reduction reaction in chromium powder furnace.In the present invention, institute
The temperature for stating reduction reaction is preferably 830~860 DEG C, and more preferably 850 DEG C, the time is preferably 6min；In the utility model, institute
The reduction reaction time is stated from calculating when starting to warm up to cold finger.In the present invention, the H2O is reduced in chromium powder furnace
Hydrogen, specific reaction equation are as follows:
2Cr+3H2O=Cr2O3+3H2↑。
The utility model, which carries out heating to cold finger, makes H2O, which enters, carries out reduction reaction in chromium powder furnace, obtained hydrogen is received
It combines in Hydrogen collection pipe.In the present invention, the reduction reaction is preferred specifically: control the 5th valve, the 6th valve
With the 7th valve, cold finger is made only to be connected with chromium powder furnace, the liquid nitrogen for being used to cool down cold finger is removed, using hot-water soak cold finger, made
H2O enters in a gaseous form carries out reduction reaction in chromium powder furnace.
After the completion of reduction reaction, the Hydrogen collection that reaction is generated preferably specifically includes following step in Hydrogen collection pipe
It is rapid:
Upper liquid nitrogen cup is covered in the second cold-trap, the 5th valve of control is connected to the second low vacuum table and cuts off and fine pumping system
The connection of system；Then third valve is opened, in the Hydrogen collection pipe after Hydrogen collection to third valve.Hydrogen collection when collection
Liquid nitrogen cup on pipe sleeve, acquisition time are preferably 3 minutes.
After collection obtains carbon dioxide and hydrogen, the carbon dioxide being collected into and hydrogen are subjected to mass spectrum two-way and surveyed offline
Examination.The utility model does not have particular/special requirement to the specific method of the mass spectrum two-way off-line test, uses those skilled in the art
Well known method.
In the present invention, the hydrogen isotope test result of the mineral samplers inclusion enclave is according to the test of standard hydrogen
As a result conversion obtains.It is preferable to use above systems to produce standard hydrogen for the utility model, then uses mass spectrum two-way off-line test
Standard hydrogen is tested.
In the present invention, producing for the standard hydrogen preferably injects standard water in chromium powder furnace, collects reaction
Obtained hydrogen, as standard hydrogen.In the present invention, the standard water is preferably national standard water, specific such as QYTB1
(seawater) and QYTB2 (Xi Zangshui).
In the present invention, the producing for standard hydrogen preferably includes following steps:
(a) vacuumize process is carried out to system；
(b) standard water injected system is entered standard water in chromium powder furnace with gaseous state and is restored by standard sample injector
Reaction；
(c) after the completion of reduction reaction, by the standard Hydrogen collection of generation in Hydrogen collection pipe.
In the present invention, the mode of the vacuumize process of the step (a) is preferably consistent with above scheme, herein not
It repeats again；
In the present invention, the reduction reaction temperature in the step (b) is preferably consistent with above scheme with the time,
This is repeated no more；The injection rate of the standard water is preferably 2 μ L.
In the present invention, the step (b) specifically: when the first low vacuum table and the second low vacuum meter reading are
0Pa, and when chromium powder furnace reaches reduction reaction temperature, controlling the 5th valve is isolated chromium powder furnace with other with the 6th valve, and with
Standard sample injector connection；Then use standard syringe, take 2 μ l of standard water, inject reduction reaction system, standard water in heating tape or
In the case where external heat source, enter Cr powder furnace in a gaseous form, redox reaction occurs.
In the present invention, the mode that hydrogen is collected in the step (c) is preferably consistent with above scheme, herein no longer
It repeats.
In the present invention, the mineral samplers inclusion enclave carbon isotope test result is tested according to standard carbon dioxide
As a result conversion obtains.Standard carbon dioxide gas be by standard GB/T W04405 and GBW04406 with anhydrous phosphoric acid the system of reacting
, then its result is measured using mass spectrum two-way off-line test.
In the present invention, when only testing the hydrogen isotope in the mineral without transition-metal ions, control the
11 valves and the 12nd valve, make thermal explosion gas around copper dioxide furnace, other steps and operations methods are consistent with above scheme.
The thermal explosion of system provided by the utility model takes gas and chromium powder reduction process is relatively independent and connection two lists
Member, the thermal explosion of current sample takes gas and the reduction hydrogen manufacturing of a upper sample that can carry out simultaneously, and copper oxide furnace is connected in parallel on pipeline
On, when not needing to restore organic gas, then around copper dioxide furnace, further simplify analysis process.
It is same to a kind of fluid inclusion carbon, hydrogen for being not easy to thermally decompose mineral provided by the utility model below with reference to embodiment
The plain analysis system in position is described in detail, but they cannot be interpreted as the restriction to scope of protection of the utility model.
Embodiment 1
5 test comparisons, mineral sample are carried out to quartz in a magma hydrothermal Deposits ore using the system of the utility model
Product be labeled as 15ND01, each test condition and operating method are consistent, test method the following steps are included:
(1) standard hydrogen is prepared
1) preparation.The prime mechanical pump and metal diffusion pump opened low vacuum mechanical pump, successively open high vacuum, and
Open the first valve and the second valve；Open CuO furnace, explosion furnace and chromium powder furnace power supply；Controlling the 4th valve makes entirely to react dress
Low vacuum extract system after being connected to the second valve is set, and opens remaining valve of system；When low vacuum meter reading is less than 10Pa,
The fine pumping system that the 4th valve is connected to after the first valve is controlled again, and cuts off entire reaction unit and low vacuum pumping simultaneously
The connection of gas system.
2) hydrogen manufacturing is restored.When the first low vacuum table and the second low vacuum meter reading are 0Pa, and when chromium powder furnace is up to 850 DEG C, control
Making the 5th valve is isolated Cr powder furnace with other with the 6th valve, and is connected to standard sample injector；Then it is infused with special standard
Emitter takes 2 μ l of standard water, injects reduction reaction system.Standard water is in the case where heating tape or external heat source, in a gaseous form
Into Cr powder furnace, redox reaction occurs.Controlling the reaction time is 6 minutes.
3) hydrogen is collected.At the end of step 2) reaction, upper liquid nitrogen cup is covered in the second cold-trap, the 5th valve of control connection the
The connection of two low vacuum tables and cutting and fine pumping system；The reading of vacuum meter is write down, third valve is then opened, hydrogen
Gas is collected into the sample collection tube after third valve.Sample collection tube is provided with active carbon, collection pipe sleeve when collecting gas
Upper liquid nitrogen cup, acquisition time are 3 minutes.
(2) standard carbon dioxide gas is prepared
It is reacted and is made with anhydrous phosphoric acid by standard GB/T W04405 and GBW04406.
(3) sample gas produces (including hydrogen and carbon dioxide)
1) preparation.Controlling the 4th valve connect entire reaction unit only with low vacuum extract system, control the 5th
Valve and the 6th valve open chromium powder furnace, extract miscellaneous gas in furnace；When the first low vacuum table and the second low vacuum meter reading are 10Pa
When, then control the 4th valve and connect entire reaction unit and connect that (while cutting is evacuated system with low vacuum with fine pumping system
The connection of system).
2) thermal explosion takes gas.When the first low vacuum table and the second low vacuum meter reading are 0Pa, and CuO furnace reaches 600 DEG C,
Explosive spalling furnace is 500 DEG C, controls the 13rd valve, the blasting cartridge for being already equipped with sample is loaded on the 13rd valve left side；Control
The 4th valve is made, connect entire reaction system with low vacuum extract system, when the first low vacuum table and the second low vacuum table are read
When number is less than 10Pa, then controls the 4th valve and entire reaction system is connect with fine pumping system；When two low vacuum tables
When reading is 0Pa, the eight, the nine, 11,12,13 valves are controlled, make the first low vacuum table, the first cold-trap, CuO furnace, explosion
Pipe connection, preheating boiler clothing, (furnace temperature is 100-105 DEG C) is preheated purging 20 minutes on blasting cartridge；Preheating time terminates, and two
When vacuum meter reading is 0Pa, explosion boiler clothing on blasting cartridge, on liquid nitrogen glass holder to the first cold-trap, starts thermal explosion and take gas, control
Time is 20 minutes.
3) purification for gas and CO2Collection.At the end of explosion 20 minutes, close the 9th valve and the 11st valve make it is quick-fried
Gas that is out and reacting generation with CuO is split to be defined in the first cold-trap for being cased with liquid nitrogen cup；The liquid for being cased with the first cold-trap
Nitrogen cup fills it up with liquid nitrogen, then opens the 8th valve and the 9th valve, the gas not freezed by liquid nitrogen in the first cold-trap is taken away；Again
The 9th valve is closed, the liquid nitrogen cup outside the first cold-trap is changed into dry ice crude alcohol mixture cup, allows the CO of the first cold-trap2It releases
Come, and is collected into the CO below the tenth valve2In sample collection tube, CO is collected2Timing is 5 minutes；Collect CO2After, then beat
The 9th valve is opened, pumps the gas not freezed again；The 9th valve and the 7th valve are controlled, connects the first cold-trap only with cold finger
It is logical, remove the dry ice crude alcohol mixture cup outside the first cold-trap, cold finger is put on liquid nitrogen cup, in this way the H in the first cold-trap2O turns
It moves on in cold finger, transfer time is 5 minutes.
4) hydrogen manufacturing is restored.At the end of previous step 5 minutes, the 5th valve of control, the 6th valve and the 7th valve make cold finger
Only it is connected to Cr powder furnace；Then remove the liquid nitrogen cup outside cold finger, change hot water cup (40~60 DEG C of hot water temperature), when record reacts
Between 6 minutes.
5) Hydrogen collection.It is consistent with the step of collecting standard hydrogen above.
The standard hydrogen come, standard CO are collected to above2, sample hydrogen and backpack body CO2, carry out mass spectrometric measurement.Test
Method is the off-line test mode of the two-way sample introduction used.The result of test is the isotope ratio of sample or standard to reference gas
Then value calculates separately out value (the opposite international standard of mineral inclusion carbon-hydrogen isotopes according still further to following formula (1) and (2)
Value).
In formula (1):
δ13CSA-RE--- δ of the sample with respect to reference gas13C value；
δ13CST-RE--- δ of the working stamndard with respect to reference gas13C value；
δ13CST-V-PDB--- δ of the working stamndard with respect to international standard V-PDB13C value.
In formula (2):
δDSA-RE--- δ D value of the sample with respect to reference gas；
δDST-RE--- δ D value of the working stamndard with respect to reference gas；
δDST-VSMOW--- δ D value of the working stamndard with respect to international standard V-SMOW.
Gained test result is listed in Table 1 below.
Table 1: five thermal explosion method Measurement results tables of same sample
| Sample number | Sample type | Sample size/g | Test result/‰ | Using method |
| 15ND01 | Quartz | 2.5 | -76 | Thermal explosion method |
| 15ND01 | Quartz | 2.5 | -73 | Thermal explosion method |
| 15ND01 | Quartz | 2.5 | -78 | Thermal explosion method |
| 15ND01 | Quartz | 2.5 | -74 | Thermal explosion method |
| 15ND01 | Quartz | 2.5 | -75 | Thermal explosion method |
According to table 1 as can be seen that the average value of five test results of same sample is -75.2 ‰, standard deviation is
1.92‰(<2.0‰).Due to the content of inclusion enclave in sample and it is unevenly distributed, even same sample, inclusion enclave
It is also inhomogenous.As shown in the results summarized in table 1, standard deviation < 2.0 ‰ have been very good to Natural Samples as a result, this is also demonstrate,proved
The feasibility of bright this method.
Embodiment 2
Thermal explosion method test analysis has been carried out respectively to the quartz in five ores of a quartz vein gold ore.Quartz specimen difference
Labeled as 15YE21,15YE22,15YE23,15YE24,15YE25.
Method for testing and analyzing is consistent with embodiment 1, and test result is listed in Table 2 below.
Table 2: different sample thermal explosion method Measurement results tables
| Sample number | Sample type | Sample size/g | Test result/‰ | Using method |
| 15YE21 | Quartz | 2.5 | -84 | Thermal explosion method |
| 15YE22 | Quartz | 2.5 | -81 | Thermal explosion method |
| 15YE23 | Quartz | 2.5 | -87 | Thermal explosion method |
| 15YE24 | Quartz | 2.5 | -92 | Thermal explosion method |
| 15YE25 | Quartz | 2.5 | -91 | Thermal explosion method |
It can be seen that according to the data in table 2 to different quartz specimens, the analysis test method of the utility model is steady
Fixed.
The above is only the preferred embodiment of the utility model, it is noted that for the common skill of the art
For art personnel, without departing from the principle of this utility model, several improvements and modifications can also be made, these improve and
Retouching also should be regarded as the protection scope of the utility model.
Claims (3)
1. a kind of be not easy to thermally decompose the fluid inclusion carbon of mineral, hydrogen isotope analysis system, including thermal explosion-collection and purifying are
System, reduction hydrogen manufacturing and collection system and vacuum-control(led) system；
Thermal explosion-the collection and purification system include that the blasting cartridge being sequentially connected in series on pipeline, the first cold-trap and carbon dioxide are received
Collector is disposed with the 13rd valve, the 12nd valve and the 11st valve between the blasting cartridge and the first cold-trap, described
Copper oxide furnace is also parallel between 12nd valve and the 11st valve；It is set between first cold-trap and carbon dioxide collection pipe
It is equipped with the tenth valve；
Thermal explosion-the collection and purification system further include explosion furnace, when carrying out thermal explosion, by the explosion boiler clothing in blasting cartridge
On；
The reduction hydrogen manufacturing and collection system include that the cold finger being sequentially connected in series on pipeline, chromium powder furnace, the second cold-trap and hydrogen are received
Collector；The cold finger is connected on pipeline by the 7th valve；The 6th valve is provided between the cold finger and chromium powder furnace；It is described
The 5th valve and third valve are disposed among second cold-trap and Hydrogen collection pipe；
Thermal explosion-the collection is connected to purification system and reduction hydrogen manufacturing with collection system by the 9th valve, the setting of the 9th valve
Between carbon dioxide collection pipe and cold finger；
The vacuum-control(led) system includes that low vacuum extract system, fine pumping system, the first low vacuum table and second are low true
Empty table；The low vacuum extract system and fine pumping system pass through the 4th valve access pipeline；The fine pumping system
The first valve is additionally provided between system and the 4th valve；The second valve is provided between the low vacuum extract system and the 4th valve
Door；
4th valve and the 13rd valve are connected to form main vacuum-pumping pipeline；
9th valve is connected to main vacuum-pumping pipeline, and the 8th valve is provided on connecting pipeline；First low vacuum
Table is arranged between the 9th valve and the 8th valve；
The second low vacuum table is arranged between the 5th valve and third valve；5th valve and main vacuum-pumping pipeline connect
It is logical；
First valve, the second valve, third valve, the 8th valve and the tenth valve are two two-way valves；4th valve,
11 valves and the 12nd valve are three two-way valves；5th valve, the 6th valve, the 7th valve, the 9th valve and the 13rd
Valve is three triple valves.
2. system according to claim 1, which is characterized in that be additionally provided with standard sample injector on the 6th valve.
3. system according to claim 1, which is characterized in that the material of the copper oxide furnace, chromium powder furnace and blasting cartridge is
Quartz glass.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108844801A (en) * | 2018-09-13 | 2018-11-20 | 中国地质科学院矿产资源研究所 | Fluid inclusion carbon and hydrogen isotope analysis system and method for minerals difficult to thermally decompose |
| CN110530702A (en) * | 2019-07-31 | 2019-12-03 | 中国地质调查局武汉地质调查中心(中南地质科技创新中心) | Not oxygen-containing mineral inclusion water extraction system and its apply and methods for using them |
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2018
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108844801A (en) * | 2018-09-13 | 2018-11-20 | 中国地质科学院矿产资源研究所 | Fluid inclusion carbon and hydrogen isotope analysis system and method for minerals difficult to thermally decompose |
| CN110530702A (en) * | 2019-07-31 | 2019-12-03 | 中国地质调查局武汉地质调查中心(中南地质科技创新中心) | Not oxygen-containing mineral inclusion water extraction system and its apply and methods for using them |
| CN110530702B (en) * | 2019-07-31 | 2021-11-26 | 中国地质调查局武汉地质调查中心(中南地质科技创新中心) | Water extraction system for oxygen-free mineral inclusion and application method thereof |
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