CN102928276A - Manufacturing method of inclusion standard sample synthesized by fused silica capillary - Google Patents
Manufacturing method of inclusion standard sample synthesized by fused silica capillary Download PDFInfo
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- CN102928276A CN102928276A CN2012104397783A CN201210439778A CN102928276A CN 102928276 A CN102928276 A CN 102928276A CN 2012104397783 A CN2012104397783 A CN 2012104397783A CN 201210439778 A CN201210439778 A CN 201210439778A CN 102928276 A CN102928276 A CN 102928276A
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Abstract
The invention discloses a manufacturing method of an inclusion standard sample synthesized by a fused silica capillary. The manufacturing method includes the following steps: a fused silica capillary with the length of 45-60mm is intercepted; one end of the fused silica capillary is sealed; moderate liquid is sucked in the capillary through the other end of the fused silica capillary by using the siphon principle; high-speed centrifugal processing is performed on the fused silica capillary filled with the liquid by using a high-speed centrifugal machine so as to enable the liquid to sink at the bottom of the sealed end of the capillary; refrigeration is performed, and the liquid has phase transition to be condensed into a solid state; air in the capillary is exhausted by controlling a vacuum system; and pipe sealing is performed on the open end of the fused silica capillary under the vacuum state. The manufacturing method is simple to operate, small in equipment investment, high in production efficiency and finished product rate and regular in products.
Description
Technical field
The present invention relates to a kind of preparation method of fluid inclusion standard specimen.
Background technology
The analysis of fluid inclusion is important method means of present geological research.Fluid inclusion is applied to the demarcation of the pertinent instruments such as cold and hot thermometric demarcation, Raman spectrometer, and fluid (fields such as mineral products, oil gas, environment, geography) balances each other and the fluid reaction simulation, chemical reaction observation simulation." synthetic method of fluid inclusion and to the meaning of research on mineral deposits " (" mineral products and geology " the 2nd phase in 2003, Zhang Zhen is bright, Lv Xinbiao, Rao Bing) put down in writing the artificial synthesis of present fluid inclusion standard specimen, a kind of method is: manually make in advance the crack on quartz, the method in generation crack is included in without the horizontal junction crystallographic axis boring of the artificial quartz column of rectangle of the optics cleaning of inclusion and then exerts pressure, breaks along main shaft, another kind is to quench in cold water after the quartz column of well cutting or the rod heating, to make it to crack and don't break.Put into again moisture high temperature and high pressure kettle with fissare quartz column and keep the long enough time so that fluid-water enters the crack, and make the crack by involution, form fluid inclusion.Another kind of method is to utilize without the crack quartz ampoule, namely in an outer tube (Pt or Au), enclose one and contain the quartz ampoule of crystallized sample material and the Pt pipe of a hydrogen buffering agent, and around two inner tubes, closely fill silica flour, under 900 ℃, 1GPa condition, continue 72h, so that fluid is wrapped up by quartz, form fluid inclusion.The synthetic method of this fluid inclusion standard specimen, technical difficulty are very large, and equipment requirement is very high, all need under high pressure and high temperature, to carry out in the autoclave, and the inclusion shape that forms is wayward, and the parcel fluid phase state is unstable, thereby has affected clear view and application.In addition, no matter be means or filling and the occlude crack that forms the crack, operate waywardly, cause yield rate very low.
Summary of the invention
Fluid inclusion standard specimen synthetic method above shortcomings for present the invention provides a kind of new synthetic method, to reduce production difficulty and to improve controllability.
The preparation method of fused quartz kapillary synthetic inclusion standard specimen of the present invention comprises the steps:
(1) the long quartz capillary of intercepting 45-60mm; The long fused quartz kapillary of intercepting 45-60mm;
(2) with oxyhydrogen flame burn off fused quartz kapillary one end surfaces coating, keep the other end from the coating of port one 0-15mm, and with burn off surface coating fused quartz kapillary one end closure;
(3) utilize siphon principle to pass through fused quartz capillary coating end and in kapillary, suck appropriate amount of fluid;
(4) with hydro-extractor the fused quartz kapillary that is filled with liquid is carried out centrifugal treating, make liquid fully be sunken to fused quartz kapillary sealing end bottom;
(5) carry out freezingly with being contained in liquid nitrogen in the Platinum crucible, liquid is undergone phase transition condense into solid-state;
(6) with vacuum equipment the air in the fused quartz kapillary is taken out to the greatest extent, made in the fused quartz kapillary to keep vacuum state;
(7) under vacuum state and freezing state fused quartz kapillary openend being carried out tube sealing processes.
Said method can be realized the preparation of neat liquid inclusion.In addition, can also be by said process be suitably adjusted, realize the preparation of liquid-gas two-phase fluid fused quartz kapillary inclusion, namely at described step (6) liquid freezing and through after vacuumizing, in the fused quartz kapillary, be filled with desired gas, and then the freezing so that gas that is filled with sublimates into solid-stately, vacuumizes and at the vacuum condition lower sealing again.The more important thing is, need under vacuum state first with in the fused quartz kapillary freezing fluid media (medium) thaw, be filled with again desired gas, and then carry out freezing to freeze liquid and gas is sublimated, find through lot of experiments, thaw first to inflate with the directly inflation of not thawing again and compare, the finished product rate has improved several times during sealing.
Kapillary can adopt the pure quartz ampoule of optics cleaning, and the quartz capillary that also can select gas chromatographic column to use, this capillary surface have coating can affect light transmission, can be with the flame calcination to remove this coating.Destroy quartz capillary, the flame envelope calcination of the most handy hydrogen flame gun when avoiding calcination.
Can rotate kapillary and with the internal flame heating of hydrogen flame gun, can guarantee that sealing end is tight attractive in appearance in when sealing.
Behind the calcination kapillary, also the kapillary top layer is cleaned and is made its dry tack free.Described cleaning can be to use the wet tissue wiped clean, and described drying can be to dry with dust-free paper.
Can adopt such method during filling liquid: gently bake the kapillary sealing end to discharge inner air tube with flame, then rapidly the kapillary openend is stretched in the liquid, utilize pressure official post liquid to be inhaled into, can realize sucking fast appropriate amount of fluid, described be in right amount the liquid that sucks should not surpass product length 1/3 for well.
After step (4) is centrifugal, before step (5) is freezing also with body formula microscopy survey the tightness of sealing end and liquid whether all by centrifugal in manage the end, the liquid of the inserting situation such as an amount of whether, if sealing is not tight or liquid is all not centrifugal to managing the end, then do over again or discarded this kapillary, to guarantee the following process yield rate.
Used liquids and gases are selected according to actual needs.
The preparation method of fused quartz kapillary synthetic inclusion standard specimen of the present invention, compare with present technology and to have following beneficial effect:
(1) do not need to utilize pressure or cold quenching to form the crack, also do not need autoclave and high temperature, high pressure and keep for a long time, operation easier and equipment cost can reduce greatly, and production efficiency can significantly improve simultaneously.
(2) because simple to operate, operating process and precision are easily controlled, so yield rate significantly improves.
(3) as standard specimen, adopt quartz capillary, the shape of the shape of quartz ampoule and the liquids and gases that are closed and final inclusion standard specimen is fixed, fluid (comprising liquids and gases) forms, phase is easily controlled, product is regular, can produce required fluid inclusion according to different needs, dirigibility is high.
Description of drawings
Fig. 1 is the preparation flow figure of neat liquid fused quartz kapillary inclusion standard specimen;
Fig. 2 is the preparation flow figure of liquid-gas fused quartz kapillary inclusion standard specimen.
Embodiment
Below by specific embodiment the present invention is described in further detail, to help understanding content of the present invention.
Embodiment 1: the preparation method of neat liquid fused quartz kapillary inclusion
In conjunction with shown in Figure 1, be a kind of method for making of neat liquid fused quartz kapillary inclusion standard specimen, namely form the fluid inclusion standard specimen with quartz parcel neat liquid, take water as fluid as example, illustrate that its step is as follows:
(1) intercepting kapillary: intercept every segment length and be the quartz capillary about 50mm, the fused quartz kapillary of selecting gas chromatographic column to use; The kapillary of intercepting is take to as unit, and every pair of two length capillaceous will equate; So that hydro-extractor beat not during centrifugally operated;
(2) calcination coating: apart from the coating on the extracapillary surface about fused quartz kapillary one end 35mm, with the flame envelope calcination coating of hydrogen flame gun, to remove this coating, increase the kapillary transparency;
(3) sealing: will by calcination remove after the coating without the coated ends sealing, destroyed change is curved near the sealing of fused quartz kapillary when avoiding sealing, and rotates kapillary during sealing and with the internal flame heating of hydrogen flame gun, guarantees that sealing end is tight attractive in appearance;
(4) clean the kapillary top layer: with extracapillary surface liquid contact jaw wet tissue wiped clean particularly, and dry with dust-free paper, sneak into target liq and change target liq purity to avoid the surface to attach impurity, and affect transparency;
(5) insert fluid media (medium): clamp kapillary apart from 1/3 place of openend with tweezers, gently bake sealing end with flammule, to discharge air, then rapidly coated ends is stretched in the liquid, the appropriate amount of fluid siphon is entered in the microcapillary tube;
(6) centrifugal: with every pair of fused quartz kapillary as in the glass capillary sleeve pipe, to be equipped with fused quartz glass capillary symmetry capillaceous be positioned over carry out on the hydro-extractor centrifugal, because of centrifuge speed larger, must build loam cake, the turn time switch, centrifugal 3 minutes, water is fully fallen at the bottom of the kapillary sealing end pipe;
(7) body formula microscopy is surveyed: survey with body formula microscopy, detect and mainly comprise the sealing end reality of whether having obturaged, whether whether water all an amount of etc. by centrifugal water in the pipe end, suction; If sealing is not tight or liquid is all centrifugal not too much to managing the end or sucking liquid, then need do over again, or discarded this kapillary;
(8) extracting vacuum: the fused quartz capillary coating end after centrifugal is inserted the capillary column packing washer, and be fixed on the port of vacuum pipeline system by reducing reducer coupling head, by vacuum pump whole pipeline system and fused quartz kapillary are evacuated, satisfy target inclusion synthetic environment;
(9) frozen liquid medium: be that water cools off to the capillary liquid in pipe, make it to condense into solid-state;
(10) extracting vacuum again: the control vacuum valve vacuumizes processing again, and it is retained to tube sealing finishes;
(11) tube sealing: under fused quartz kapillary destination end immerses the liquid level of liquid nitrogen in the Platinum crucible fill liquid nitrogen, with flame to approximately carrying out the calcination tube sealing in the 10mm place from fused quartz kapillary sealing end; If the quantity not sufficient of liquid nitrogen in the Platinum crucible should be filled it up with then tube sealing of liquid nitrogen;
(12) detect: whether tightly under stereoscope, detect sealing, at cold and hot---the parameter qualification of microscopically testing product.
By step (5) gently roasting sealing end can be easily, be drawn onto liquid as far as possible near sealing end rapidly, again in conjunction with centrifugal, can guarantee to be filled into fused quartz kapillary bottom, further vacuumize again the discharge air after freezing and make fluid non-volatile, at the vacuum lower sealing, realized the preparation of neat liquid fused quartz kapillary inclusion standard specimen with fairly simple technology and equipment.
Embodiment 2
As shown in Figure 2, be the preparation method of the liquid that is packaged with the solution-air two-phase fluid in a kind of quartz capillary-gas fused quartz kapillary inclusion standard specimen, with the liquid water, gas is that carbon dioxide is that example describes.
Wherein, step
(1) intercepting kapillary-(8), calcination coating, sealing, cleaning kapillary top layer, insert fluid media (medium), centrifugal, body formula microscopy survey identical with embodiment 1 with the operation of extracting vacuum, unique different be the padding of increase gas, operate as follows:
(9) frozen liquid medium: aqueous water in the kapillary is cooled off, make it condense into solid-state ice;
(10) extracting vacuum again: the control vacuum valve vacuumizes processing again, and it is retained to tube sealing finishes;
(11) thaw: close vacuum valve, reduce lifting table, make fused quartz kapillary sealing end leave liquid nitrogen in the Platinum crucible, leave standstill for a moment, allow solid ice is melted into liquid water in the pipe;
(12) blanketing gas: open gas cylinder valve, regulate the operation valve of vacuum system, be filled with quartz capillary and be retained to step (13) with the carbon dioxide calibrating gas and finish, carbon dioxide gas pressure is 8Mpa;
(13) frozen liquid medium: promote lifting table, again sealing end is immersed in the liquid nitrogen, the air-water fluid media (medium) in the freezing kapillary again, the solution-air two-phase that the interior carbon dioxide of kapillary and water are consisted of all becomes solid-state, keep sealing end to step (15) to finish, if liquid nitrogen is not enough in the Platinum crucible, should add at any time liquid nitrogen, immerse again in the liquid nitrogen from the kapillary more than the sealing end 20mm with assurance;
(14) vacuumize: after closing gas filling valve, regulate vacuum valve, again vacuumize, can remain on kapillary in because water and carbon dioxide are solid-state this moment;
(15) tube sealing: under fused quartz kapillary destination end immerses the liquid level of liquid nitrogen in the Platinum crucible fill liquid nitrogen, with flame to approximately carrying out the calcination tube sealing in the 10mm place from fused quartz kapillary sealing end; If the quantity not sufficient of liquid nitrogen in the Platinum crucible should be filled it up with then tube sealing of liquid nitrogen;
(16) detect: whether tightly under stereoscope, detect sealing, at cold and hot---the parameter qualification of microscopically testing product.
Carried out first the operation of thawing of step (11) before blanketing gas, compare with the direct blanketing gas that do not thaw, yield rate can improve several times when tube sealing.
Claims (10)
1. the preparation method of a fused quartz kapillary synthetic inclusion standard specimen comprises the steps:
(1) the long fused quartz kapillary of intercepting 45-60mm;
(2) with oxyhydrogen flame burn off fused quartz kapillary one end surfaces coating, keep the other end from the coating of port one 0-15mm, and with burn off surface coating fused quartz kapillary one end closure;
(3) utilize siphon principle to pass through fused quartz capillary coating end and in kapillary, suck appropriate amount of fluid;
(4) with hydro-extractor the fused quartz kapillary that is filled with liquid is carried out centrifugal treating, make liquid fully be sunken to fused quartz kapillary sealing end bottom;
(5) carry out freezingly with being contained in liquid nitrogen in the Platinum crucible, liquid is undergone phase transition condense into solid-state;
(6) with vacuum equipment the air in the fused quartz kapillary is taken out to the greatest extent, made in the fused quartz kapillary to keep vacuum state;
(7) under vacuum state and freezing state fused quartz kapillary openend being carried out tube sealing processes.
2. preparation method as claimed in claim 1, it is characterized in that: after described step (6) liquid freezing vacuumizes processing, also in the fused quartz kapillary, be filled with gas, and then the freezing so that gas that is filled with becomes also solid-stately, again vacuumize processing.
3. preparation method as claimed in claim 2 is characterized in that: under vacuum state first with in the fused quartz kapillary freezing fluid media (medium) thaw, and then be filled with required target criteria gas.
4. such as described preparation method one of in the claims 1 to 3, it is characterized in that: described fused quartz kapillary is the quartz capillary that gas chromatographic column is used, and removes surface coating with the flame calcination first before sealing.
5. method as claimed in claim 4 is characterized in that: described calcination is the flame envelope calcination with the hydrogen flame gun.
6. such as described preparation method one of in the claims 1 to 3, it is characterized in that: described sealing operation is to rotate the fused quartz kapillary and with the internal flame heating of hydrogen flame gun.
7. such as described preparation method one of in the claims 1 to 3, it is characterized in that: behind calcination fused quartz kapillary, also the kapillary top layer is cleaned and made its dry tack free.
8. method as claimed in claim 7, it is characterized in that: described cleaning is to use the wet tissue wiped clean, and described drying is to dry with dust-free paper.
9. such as described preparation method one of in the claims 1 to 3, it is characterized in that: the method for filling liquid is in the described step (3): gently bake the kapillary sealing end to discharge inner air tube with flame, then the kapillary openend is stretched in the liquid, utilize pressure official post liquid to enter in the kapillary by siphon.
10. such as described preparation method one of in the claims 1 to 3, it is characterized in that: after step (4) is centrifugal, before step (5) is freezing also with body formula microscopy survey the tightness of sealing end and liquid whether all by centrifugal in manage the end, the liquid that the sucks situation such as an amount of whether, if sealing is not tight or liquid is all not centrifugal to managing at the end, the liquid of suction is crossed and is done over again at most or discarded this fused quartz kapillary.
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| CN201210439778.3A CN102928276B (en) | 2012-11-07 | 2012-11-07 | Manufacturing method of inclusion standard sample synthesized by fused silica capillary |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104535367A (en) * | 2014-12-24 | 2015-04-22 | 中国科学院地球化学研究所 | Synthetic inclusion in-situ sampling device suitable for high-temperature and high-pressure hydrothermal environments |
| CN107402148A (en) * | 2016-05-20 | 2017-11-28 | 中国石油化工股份有限公司 | A kind of method and device of artificial synthesized oil gas inclusion |
| CN108375491A (en) * | 2018-01-23 | 2018-08-07 | 中国石油天然气股份有限公司 | Micro- visual fluid mothballed plant and assay method |
| CN112014185A (en) * | 2020-09-06 | 2020-12-01 | 中国科学院地球化学研究所 | Artificial synthesis method of fluid inclusion in quartz |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104535367A (en) * | 2014-12-24 | 2015-04-22 | 中国科学院地球化学研究所 | Synthetic inclusion in-situ sampling device suitable for high-temperature and high-pressure hydrothermal environments |
| CN107402148A (en) * | 2016-05-20 | 2017-11-28 | 中国石油化工股份有限公司 | A kind of method and device of artificial synthesized oil gas inclusion |
| CN107402148B (en) * | 2016-05-20 | 2020-11-13 | 中国石油化工股份有限公司 | Method and device for artificially synthesizing oil gas inclusion |
| CN108375491A (en) * | 2018-01-23 | 2018-08-07 | 中国石油天然气股份有限公司 | Micro- visual fluid mothballed plant and assay method |
| CN112014185A (en) * | 2020-09-06 | 2020-12-01 | 中国科学院地球化学研究所 | Artificial synthesis method of fluid inclusion in quartz |
| CN112014185B (en) * | 2020-09-06 | 2021-06-25 | 中国科学院地球化学研究所 | Artificial synthesis method of fluid inclusion in quartz |
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