CN103041895B - Vacuum ball-milling degassing tank for rare gas analysis, and analysis method - Google Patents
Vacuum ball-milling degassing tank for rare gas analysis, and analysis method Download PDFInfo
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- CN103041895B CN103041895B CN201110310605.7A CN201110310605A CN103041895B CN 103041895 B CN103041895 B CN 103041895B CN 201110310605 A CN201110310605 A CN 201110310605A CN 103041895 B CN103041895 B CN 103041895B
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Abstract
The invention discloses a vacuum ball-milling degassing tank for rare gas analysis, and an analysis method. The degassing tank comprises a tank body and an upper cover, wherein a pipe is arranged on the upper cover, one end of the pipe is inserted into the tank body, the pipe is in tight coupling with the upper cover, and the other end of the pipe is provided with a vacuum valve which is in tight coupling with the pipe and is sheathed inside a pressing sleeve with a bucket-shaped structure; the pressing sleeve is arranged on the upper cover; an opening is formed in the side surface of the pressing sleeve, and the vacuum valve penetrates through the opening to be communicated with the outside; a steel ball is arranged inside the tank body; and the tank body is connected with the upper cover in a fastening manner and is provided with a seal. The analysis method comprises the following steps of: sealing a sample in the tank body, crushing the sample by the degassing tank in a ball-milling instrument, collecting rare gas, and then connecting the vacuum ball-milling degassing tank into a gas analysis device for analysis. The degassing tank provided by the invention is simple in structure and convenient to operate, is provided with an interface shared with the analysis device, simultaneously can meet the requirements on high vacuum tightness and of analysis of the rare gas, and has low air background.
Description
Technical field
The present invention relates to geology field, say further, relate to a kind of vacuum ball milling degassing tank for rare gas analysis and analytical method.
Background technology
Geological research field, because rare gas is very large in the partition coefficient difference of solid phase and liquid phase, rare and refractory metals in rock in liquid phase inclusion enclave can well be preserved, it is the important means of spike Mantle Fluids, but it is very difficult for isolating rare gas from rock sample, first must be broken to solid sample.The instrument that current pulverizing is milled has a lot, abroad representative and advanced is the PM200 planet-shaped ball milling instrument that German Retsch company manufactures, this equipment is to the fine gtinding of solid matter, high fineness of grind can be reached, until submicron order, but the milling tank configured (see Fig. 1), to mill cylindrical shell by 101; 102 O shape circles; 103 mill upper cover composition.Just to mill design for the ultra-fine grinding of general solid matter, do not consider the problems referred to above.Therefore, there is following shortcoming in the device of this structure: its structure of this device is simple, and poor sealing performance, can not vacuumize, and lacks the interface be connected with ancillary equipment and cannot carry out lower step analysis.
Summary of the invention
For solving problems of the prior art, the invention provides a kind of vacuum ball milling degassing tank for rare gas analysis and analytical method.Structure is simple, easy to operate, have with analytical instrument connecting interface, can meet the airtight requirement of high vacuum, lower air background simultaneously, meets the analysis requirement of rare gas.
An object of the present invention is to provide a kind of vacuum ball milling degassing tank analyzed for rare gas.
Comprise tank body and upper cover,
Cover on described and be provided with pipe, pipe one end is inserted in tank body, and pipe and upper cover are tightly connected, and the other end is provided with vacuum valve, and vacuum valve is connected with pipe sealing; Described vacuum valve is enclosed within gland, and gland is barrel-like structure, is placed in and covers, and gland side is provided with opening, and vacuum valve is in communication with the outside through opening; When degassing tank is placed on ball milling instrument, use gland to be fixed on ball milling instrument, prevent from occurring in process of lapping to loosen;
Described tank interior is provided with steel ball; Described tank body and upper cover are fastenedly connected.
Described tank body inner bottom part arranges circular arc chamfering;
Described tank body is that anti-ballistic materials is made, can preferred stainless steel material;
Described steel ball number can be preferably three;
Be provided with sealing ring between described upper cover and tank body, described sealing ring is preferably oxygen-free copper sealing ring, and the compacting of stainless steel cutting edge seals.
Two of object of the present invention is to provide a kind of rare gas analytical method.
Comprise:
Sample is placed in sealing in tank body, described vacuum ball milling degassing tank is put into ball milling instrument and pulverizes sample, collects rare gas, is then analyzed by vacuum ball milling degassing tank access gas analyzing apparatus.
Can be preferred:
Put into ball milling instrument again after first being vacuumized by described vacuum ball milling degassing tank and pulverize sample, vacuum is 1 × 10
-4pa ~ 1 × 10
-3pa.
Specifically can adopt following steps:
(1) solid matter sample and steel ball are placed in hermetically sealed can, put sealing ring, tighten fastening bolt and grinding pot is sealed, cover upper cover, prevent milling tank from High Rotation Speed disrupted sample process, having loosening possibility;
(2) open vacuum valve, by vavuum pump, degassing tank is vacuumized, be evacuated to 10
-4pa, valve-off;
(3) be placed on degassing tank by gland and cover, what degassing tank was placed on ball milling instrument mills on platform, acts on gland, be fixed on by degassing tank on ball milling instrument by the mechanical part on ball milling instrument; Open ball milling instrument sample comminution in tank to the powder being less than 1um sample comminution in tank to the fine powder being less than 1um;
(4) degassing tank is accessed rare gas purification enrichment device, carry out gas composition and isotopic analysis.
In described step (3),
After on the platform of milling vacuum sphere grinding jar being placed in ball milling instrument, act on gland by the mechanical part on ball milling instrument, degassing tank is fixed on ball milling instrument, gland is while protection vacuum valve, also mechanical component ball milling instrument playing fixation can be made, act on gland, prevent ball grinder in process of lapping from occurring to loosen; Open ball milling instrument, vacuum ball milling degassing tank round axle rotation, and runs up around common axis in the opposite direction, ball of so milling starts to move in tank, discharge the impact momentum of huge amount, there is high strength crushing effect, finally go out sample size in 10 minutes and be less than 1 micron.The gas composition that tax like this is stored in rock sample progressively discharges desorption out, and concentrate be stored in milling tank.Tank body upper cover axle center is connected to vacuum valve, is connected carries out rare gas analysis with rare gas purification enrichment device sample introduction interface.
Above-described ball milling instrument preferably can adopt PM200 planet-shaped ball milling instrument.
Compared to the prior art the present invention, has following advantage:
(1) vacuum electromagnetic ball mill device has that structure is simple, easy for operation, the feature of good leak tightness.
(2) have and analytical instrument connecting interface, there is low air background, meet the analysis requirement of rare gas.
Accompanying drawing explanation
Grinding pot structural representation in Fig. 1 prior art
Fig. 2 vacuum ball milling of the present invention degassing tank structural representation
Description of reference numerals:
101-grinding cylinder; 102-O type circle; 102-grinds upper cover;
1-steel ball; 2-inclusion enclave sample; 3-tank body; 4-sealing ring; 5-upper cover;
6-fastening bolt; 7-welded pipe; 8-attaching nut; 9-vacuum valve; 10-gland
Detailed description of the invention
Below in conjunction with embodiment, further illustrate the present invention.
Embodiment:
As shown in Figure 2, a kind of vacuum ball milling degassing tank analyzed for rare gas, described upper cover 5 is provided with welded pipe 7, and welded pipe 7 one end is inserted in tank body 3, with upper cover 5 seal welding; The other end is provided with vacuum valve 9, by the airtight connection of valve securing member; Described vacuum valve 9 is enclosed within gland 10, and gland 10 is barrel-like structure, is placed on upper cover 5, and gland 10 side is provided with opening, and vacuum valve 9 can be in communication with the outside through opening; Described tank body 3 inside is provided with steel ball 1, and the quantity of steel ball 1 is three; Described tank body 3 is connected by fastening bolt 6 with upper cover 5.
Tank body 3 inner bottom part arranges circular arc chamfering; Tank body 3 is shock proof stainless steel material;
Be provided with sealing ring 4 between described upper cover 5 and tank body 3, described sealing ring 4 is oxygen-free copper sealing ring, and the compacting of stainless steel cutting edge seals;
Vacuum valve 9 is SS-4H (swagelok) bellow sealed valve, is fixed in welded pipe 7 by attaching nut 8, and vacuum valve 9 is connected with rare gas purity analysis device.
When carrying out sample analysis,
(1) solid matter sample and steel ball are placed in hermetically sealed can, put sealing ring, tighten fastening bolt and grinding pot is sealed, cover upper cover, prevent milling tank from High Rotation Speed disrupted sample process, having loosening possibility.
(2) open vacuum valve, by vavuum pump, degassing tank is vacuumized, be evacuated to 10
-4pa, valve-off;
(3) gland is placed on degassing tank covers, what degassing tank was placed on PM200 planet-shaped ball milling instrument mills on platform, act on gland by the mechanical part on ball milling instrument, degassing tank is fixed on ball milling instrument, prevent from occurring in process of lapping to loosen, open ball milling instrument, vacuum ball milling degassing tank is round axle rotation, and run up around common axis in the opposite direction, ball of so milling starts to move in tank, discharge the impact momentum of huge amount, there is high strength crushing effect, finally go out sample size in 10 minutes and be less than 1 micron.The gas composition that tax like this is stored in rock sample progressively discharges desorption out, and concentrate be stored in milling tank;
(4) degassing tank is accessed rare gas purification enrichment device, carry out gas composition and isotopic analysis.
Claims (8)
1., for the vacuum ball milling degassing tank that rare gas is analyzed, comprise tank body and upper cover, it is characterized in that:
Cover on described and be provided with pipe, pipe one end is inserted in tank body, and pipe and upper cover are tightly connected, and the other end is provided with vacuum valve, and vacuum valve is connected with pipe sealing; Described vacuum valve is enclosed within gland, and gland is barrel-like structure, is placed in and covers, and gland side is provided with opening, and vacuum valve can be in communication with the outside through opening;
Described tank interior is provided with steel ball;
Described tank body and upper cover are fastenedly connected and seal.
2. vacuum ball milling degassing tank as claimed in claim 1, is characterized in that:
Described tank body inner bottom part arranges circular arc chamfering.
3. vacuum ball milling degassing tank as claimed in claim 2, is characterized in that:
Described tank body is stainless steel material.
4. vacuum ball milling degassing tank as claimed in claim 1, is characterized in that:
Described steel ball number is three.
5. vacuum ball milling degassing tank as claimed in claim 1, is characterized in that:
Sealing ring is provided with between described upper cover and tank body.
6. vacuum ball milling degassing tank as claimed in claim 5, is characterized in that:
Described sealing ring is oxygen-free copper sealing ring, and the compacting of stainless steel cutting edge seals.
7. adopt an analytical method for the vacuum ball milling degassing tank as described in one of claim 1 ~ 6, comprising:
Sample is placed in sealing in tank body, described vacuum ball milling degassing tank is put into ball milling instrument and pulverizes sample, collects rare gas, is then analyzed by vacuum ball milling degassing tank access gas analyzing apparatus;
Put into ball milling instrument again after first being vacuumized by described vacuum ball milling degassing tank and pulverize sample, vacuum is 1 × 10
-4pa ~ 1 × 10
-3pa.
8. analytical method as claimed in claim 7, is characterized in that described method is specially:
(1) solid matter sample and steel ball are placed in tank body, put sealing ring, tank body is sealed, cover upper cover, degassing tank is vacuumized;
(2) be placed on degassing tank by gland and cover, what degassing tank was placed on ball milling instrument mills on platform, acts on gland, be fixed on by degassing tank on ball milling instrument by the mechanical part on ball milling instrument;
(3) ball milling instrument is opened sample comminution in tank body to the powder being less than 1um;
(4) degassing tank is accessed rare gas purification enrichment device, carry out gas composition and isotopic analysis.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110310605.7A CN103041895B (en) | 2011-10-13 | 2011-10-13 | Vacuum ball-milling degassing tank for rare gas analysis, and analysis method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110310605.7A CN103041895B (en) | 2011-10-13 | 2011-10-13 | Vacuum ball-milling degassing tank for rare gas analysis, and analysis method |
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| Publication Number | Publication Date |
|---|---|
| CN103041895A CN103041895A (en) | 2013-04-17 |
| CN103041895B true CN103041895B (en) | 2015-05-06 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201110310605.7A Active CN103041895B (en) | 2011-10-13 | 2011-10-13 | Vacuum ball-milling degassing tank for rare gas analysis, and analysis method |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104677777B (en) * | 2013-11-29 | 2017-10-27 | 中国石油化工股份有限公司 | Rock remnants air content test devices and its method of testing |
| CN107597308B (en) * | 2017-11-13 | 2023-04-25 | 福州大学 | Ventilated reaction ball milling tank with reinforced double ribs on inner wall of tank body and use method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2104705U (en) * | 1991-10-30 | 1992-05-20 | 中国科学院金属研究所 | Vacuum and aerated ball grinding pot |
| CN200945443Y (en) * | 2006-05-24 | 2007-09-12 | 中国科学院上海微系统与信息技术研究所 | A ball mill jar that can withstand high pressure or vacuum |
| CN200962075Y (en) * | 2006-04-06 | 2007-10-17 | 中国石油化工股份有限公司 | A rock scraps crushing and degasing device |
| CN101722087A (en) * | 2008-10-31 | 2010-06-09 | 中国石油化工股份有限公司 | Vacuum sealing milling tank and using method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7767151B2 (en) * | 2005-08-03 | 2010-08-03 | Wildcat Discovery Technologies, Inc. | High throughput mechanical alloying and screening |
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- 2011-10-13 CN CN201110310605.7A patent/CN103041895B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2104705U (en) * | 1991-10-30 | 1992-05-20 | 中国科学院金属研究所 | Vacuum and aerated ball grinding pot |
| CN200962075Y (en) * | 2006-04-06 | 2007-10-17 | 中国石油化工股份有限公司 | A rock scraps crushing and degasing device |
| CN200945443Y (en) * | 2006-05-24 | 2007-09-12 | 中国科学院上海微系统与信息技术研究所 | A ball mill jar that can withstand high pressure or vacuum |
| CN101722087A (en) * | 2008-10-31 | 2010-06-09 | 中国石油化工股份有限公司 | Vacuum sealing milling tank and using method thereof |
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| CN103041895A (en) | 2013-04-17 |
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