CN102600937A - Ball milling tank and method for preparing rare gas in rock inclusion - Google Patents
Ball milling tank and method for preparing rare gas in rock inclusion Download PDFInfo
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- CN102600937A CN102600937A CN2012100866236A CN201210086623A CN102600937A CN 102600937 A CN102600937 A CN 102600937A CN 2012100866236 A CN2012100866236 A CN 2012100866236A CN 201210086623 A CN201210086623 A CN 201210086623A CN 102600937 A CN102600937 A CN 102600937A
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- 239000011435 rock Substances 0.000 title claims abstract description 135
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000000498 ball milling Methods 0.000 title abstract description 9
- 239000007789 gas Substances 0.000 claims abstract description 153
- 238000010438 heat treatment Methods 0.000 claims abstract description 52
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 29
- 239000010959 steel Substances 0.000 claims abstract description 29
- 238000000227 grinding Methods 0.000 claims description 39
- 241000475481 Nebula Species 0.000 claims description 23
- 210000004907 gland Anatomy 0.000 claims description 18
- 239000011261 inert gas Substances 0.000 claims description 8
- 238000000605 extraction Methods 0.000 claims description 5
- 230000008878 coupling Effects 0.000 claims description 4
- 238000010168 coupling process Methods 0.000 claims description 4
- 238000005859 coupling reaction Methods 0.000 claims description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 3
- 238000003801 milling Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 2
- 238000007789 sealing Methods 0.000 abstract description 16
- 239000012535 impurity Substances 0.000 abstract 1
- 238000004458 analytical method Methods 0.000 description 8
- 238000005086 pumping Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 238000003780 insertion Methods 0.000 description 4
- 230000037431 insertion Effects 0.000 description 4
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- 238000000746 purification Methods 0.000 description 2
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 238000000429 assembly Methods 0.000 description 1
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- 238000002474 experimental method Methods 0.000 description 1
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Abstract
The invention discloses a ball milling tank and a method for preparing rare gas in a rock inclusion, wherein the ball milling tank for preparing the rare gas in the rock inclusion comprises the following components: the sample tank is provided with a tank body and a top cover, wherein the top cover is arranged above the tank body in a sealing manner, the tank body is provided with an accommodating cavity, and more than one first steel ball is placed in the accommodating cavity; the high vacuum valve is connected to the top cover, a through hole is formed in the top cover, and an air inlet of the high vacuum valve is communicated with the accommodating cavity of the tank body through the through hole; and the heating assembly is sleeved outside the sample tank. The ball milling tank and the method for preparing the rare gas in the rock inclusion can remove various impurity gases and moisture on the surface of a rock inclusion sample, and can always keep a sealing state in the ball milling process of the rock inclusion sample, so that the prepared rare gas is not polluted by the rare gas in the outside air.
Description
Technical field
The present invention is relevant for a kind of ball grinder and method that is used to prepare rare gas, especially relevant for a kind of ball grinder and method that in oil-gas geology experiment field, is used for preparing rock inclusion enclave rare gas.
Background technology
Rare gas (claiming inert gas again) becomes the important tracer of geology course because of its unique chemical inertia.In oil-gas exploration, rare gas component in the rock inclusion enclave and isotope are containing abundant oil-gas geology information, and they become the Tibetan phase all to have important spike indicative function for the origin cause of formation of research oil gas with source, oil-gas-source contrast and oil gas.Therefore, the preparation to rare gas in the rock inclusion enclave is the precondition and guarantee of carrying out rare gas component and isotope analysis.
Concerning rock inclusion enclave solid sample, carrying out ball mill grinding is the important step of preparation rare gas pre-treatment.In the oil-gas geology field, on the one hand, because the rare gas abundance that contains in the rock inclusion enclave is extremely low; And the surface of rock inclusion enclave sample is adsorbed with various foreign gases and moisture through regular meeting; In the ball mill grinding process, the various foreign gases and the moisture of rock inclusion enclave sample surfaces can hinder the release of rare gas in the rock inclusion enclave; Cause still containing rare gas in the part rock inclusion enclave after ball mill grinding, the rare gas in the sample does not fully discharge; And; Along with constantly carrying out of ball mill grinding; The various foreign gases and the moisture of rock inclusion enclave surface adsorption also can together be produced out; This just makes and also contains various foreign gases of other the rare gas and moisture in the rock inclusion enclave in the prepared gas that comes out, and the rare gas that causes preparing receives the pollution of rare gas in the air, has a strong impact on follow-up to rare gas component and isotopic analysis result and accuracy thereof.
On the other hand; At present in commercial production such as food, chemical industry, agricultural chemicals, coating, printing ink; Being widely used has various types of grinding pots or ball grinder because there is the not salable online defective such as vacuumize of maybe can't carrying out in those ball grinders, make the rock inclusion enclave carry out at a high speed, when high efficiency is pulverized; Sample jar can not keep the state that seals constantly; Rare gas in the rock inclusion enclave is prone to leak to outside the sample jar, and simultaneously, the rare gas in the outside air also can get in the sample jar and pollute the rare gas that rock inclusion enclave sample is discharged; Have again; Because sample jar can not keep the state of high vacuum; Before ball mill grinding; The air that itself exists in the sample jar also can exert an influence to the rare gas that the rock inclusion enclave is discharged, and influences the preparation purity of rare gas, and the purification and the enrichment of rare gas handled in the follow-up rock inclusion enclave.
Therefore, be necessary to provide a kind of new ball grinder and preparation method, overcome above-mentioned defective.
Summary of the invention
The purpose of this invention is to provide a kind of ball grinder that is used for preparing rock inclusion enclave rare gas; This ball grinder can remain sealing state in rock inclusion enclave sample carries out the process of ball milling; And can remove the various foreign gases and the moisture of rock inclusion enclave sample surfaces; Make the rare gas of preparing not receive the pollution of rare gas in the air, satisfy and carry out the rare gas component and the isotope analysis requirement of high accuracy, high accuracy.
Another object of the present invention provides a kind of method that is used for preparing rock inclusion enclave rare gas; This method can remain sealing state in rock inclusion enclave sample carries out the process of ball milling; And can remove the various foreign gases and the moisture of rock inclusion enclave sample surfaces; Make the rare gas of preparing not receive the pollution of rare gas in the air, satisfy and carry out the rare gas component and the isotope analysis requirement of high accuracy, high accuracy.
Above-mentioned purpose of the present invention can adopt following technical proposal to realize:
The present invention provides a kind of said ball grinder that is used for preparing rock inclusion enclave rare gas to comprise:
Sample jar, it has the top cover that tank body and seal cover are located at said tank body top, and said tank body has container cavity, is placed with first steel ball more than in the said container cavity;
High vacuum valve, it is connected on the said top cover, offers perforation on the said top cover, and the air inlet of said high vacuum valve is connected with the container cavity of said tank body through said perforation;
Heating component, it is set in outside the tank body of said sample jar.
In preferred embodiment, between the tank body of said sample jar and said top cover, be folded with seal washer.
In preferred embodiment, be placed with second steel ball more than in the container cavity of said sample jar, the diameter of said second steel ball is less than the diameter of said first steel ball.
In preferred embodiment, said first steel ball is two, and its diameter is 8mm; Said second steel ball is two, and its diameter is 2mm.
In preferred embodiment; Said heating component comprises heating jacket and tightens part; Said heating jacket is around on the outer surface of said tank body; Two ends of said heating jacket radially outward convex with connecting portion respectively, and the said part of tightening is connected between said two connecting portions, and the outer surface of said heating jacket is connected with heated coupling.
In preferred embodiment, between said heating jacket and said tank body, be folded with thermocouple.
In preferred embodiment, perforation place of said top cover is connected with tube connector, and the air inlet of said high vacuum valve links to each other with said tube connector through the attaching nut.
In preferred embodiment, the outside of said high vacuum valve is arranged with gland, and said gland is connected the top of said top cover.
In preferred embodiment, the top of said gland offers connecting hole, and the gas outlet of said high vacuum valve is stretched in the said connecting hole.
In preferred embodiment, the tank base of said sample jar is provided with three reference columns, and said three reference columns along the circumferential direction are evenly distributed on the bottom of said tank body.
The present invention also provides a kind of method that is used for preparing rock inclusion enclave rare gas, and the said method that is used for preparing rock inclusion enclave rare gas comprises:
A) select rock inclusion enclave sample, the particle diameter size of said rock inclusion enclave sample is 0.125mm～1mm;
B) the said rock inclusion enclave sample of select is put into like each described tank body that is used for preparing the ball grinder of rock inclusion enclave rare gas of claim 1～10, the amount of putting into of said rock inclusion enclave sample is 10～15 grams;
C) open said high vacuum valve, said sample jar is vacuumized, through said heating component said tank body is heated simultaneously;
D) close said heating component, continue said tank body is vacuumized;
E) close said high vacuum valve; The said ball grinder that is used for preparing rock inclusion enclave rare gas is placed on the grinding plate of nebula formula ball mill device; Clamping device through said nebula formula ball mill device is fixed on said grinding plate with the said ball grinder that is used for preparing rock inclusion enclave rare gas; Open said nebula formula ball mill device, the said ball grinder that is used for preparing rock inclusion enclave rare gas is rotated on said grinding plate.
In preferred embodiment, in said step c, the pressure after treating to vacuumize in the said tank body reaches 10
-1During Pa, carry out said steps d again.
In preferred embodiment, in said steps d, the pressure after treating to vacuumize in the said tank body reaches 10
-4During Pa, carry out said step e again.
In preferred embodiment, in said step c, the heating-up temperature of said heating component is 100 ℃～150 ℃.
In preferred embodiment, in said step e, be 10 minutes to the said milling time that is used for preparing the ball grinder of rock inclusion enclave rare gas through said nebula formula ball mill device, the grinding rotating speed is 400rpm.
In preferred embodiment; After said step e, also comprise step f: close said nebula formula ball mill device; The said ball grinder that is used for preparing rock inclusion enclave rare gas is taken off; Inert gas extraction is linked to each other with said high vacuum valve with the sample-preparing system that separates, open said high vacuum valve, the interior rare gas of said tank body extracts through said inert gas and the zirconium base stove of the sample-preparing system that separates etc. purifies with enrichment and handles.
Of the present inventionly be used for preparing the ball grinder of rock inclusion enclave rare gas and the characteristics and the advantage of method is:
One, ball grinder and the method that is used for preparing rock inclusion enclave rare gas of the present invention; Because top cover and tank body are that sealing is provided with each other; Therefore ball grinder has good sealing property; Can effectively prevent rock inclusion enclave sample the leaking outside or the inflow of outside air of rare gas in the process of ball mill grinding, thereby guarantee that prepared rare gas does not receive the pollution of outside air; In addition, ball grinder can connect outside vaccum-pumping equipment through high vacuum valve, utilizes outside vaccum-pumping equipment that the container cavity of tank body is vacuumized, and has further guaranteed the purity of prepared rare gas; Have, heating component can effectively be removed various foreign gases and the moisture attached to rock inclusion enclave sample surfaces again, guarantees for the abundant release of rare gas in the rock inclusion enclave provides prerequisite.
Two, ball grinder and the method that is used for preparing rock inclusion enclave rare gas of the present invention; In the sample jar of ball grinder, be placed with the steel ball of two kinds of diameter; Under same grinding rotating speed; Can further promote grinding of the interior rock inclusion enclave sample of sample jar, farthest to discharge the rare gas in the rock inclusion enclave.
Three, ball grinder and the method that is used for preparing rock inclusion enclave rare gas of the present invention, the gland that is connected on the top cover is covered with high vacuum valve within it, and it can play the effect of protection high vacuum valve air inlet; In addition, be arranged on three reference columns of tank base, can with the corresponding one by one buckle of three fixed grooves on the grinding plate of nebula formula ball mill device, avoid ball grinder in nebula formula ball mill device, to carry out shaking when high speed is rotated.
Description of drawings
In order to be illustrated more clearly in the technical scheme in the embodiment of the invention; The accompanying drawing of required use is done to introduce simply in will describing embodiment below; Obviously, the accompanying drawing in describing below only is some embodiments of the present invention, for those of ordinary skills; Under the prerequisite of not paying creative work, can also obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 looks half sectional view for the master who is used for preparing the ball grinder of rock inclusion enclave rare gas of the present invention.
Fig. 2 is the tank body cutaway view that is used for preparing the ball grinder of rock inclusion enclave rare gas of the present invention.
Fig. 3 is the top cover cutaway view that is used for preparing the ball grinder of rock inclusion enclave rare gas of the present invention.
Fig. 4 is the heating component front view that is used for preparing the ball grinder of rock inclusion enclave rare gas of the present invention.
Fig. 5 is the heating component vertical view that is used for preparing the ball grinder of rock inclusion enclave rare gas of the present invention.
Fig. 6 is the gland half sectional view that is used for preparing the ball grinder of rock inclusion enclave rare gas of the present invention.
Fig. 7 is the gland vertical view that is used for preparing the ball grinder of rock inclusion enclave rare gas of the present invention.
Fig. 8 is placed on the sketch map on the grinding plate of nebula formula ball mill device for the ball grinder that is used for preparing rock inclusion enclave rare gas of the present invention.
The specific embodiment
To combine the accompanying drawing in the embodiment of the invention below, the technical scheme in the embodiment of the invention is carried out clear, intactly description, obviously, described embodiment only is the present invention's part embodiment, rather than whole embodiment.Based on the embodiment among the present invention, those of ordinary skills are not making the every other embodiment that is obtained under the creative work prerequisite, all belong to the scope of the present invention's protection.
Embodiment 1
As shown in Figure 1, the present invention provides a kind of ball grinder that is used for preparing rock inclusion enclave rare gas, and it comprises sample jar 1, high vacuum valve 2 and heating component 3.Wherein: sample jar 1 has the top cover 12 that tank body 11 and seal cover are located at said tank body 11 tops, and said tank body 11 has container cavity 111, is placed with first steel ball 13 more than in the said container cavity 111; High vacuum valve 2 is connected on the said top cover 12, offers perforation 121 on the said top cover 12, and the air inlet 21 of said high vacuum valve 2 is connected with the container cavity 111 of said tank body 11 through said perforation 121; Heating component 3 is set in outside the tank body 11 of said sample jar 1.
Specifically be, please cooperate and consult Fig. 2 that the tank body of sample jar 1 11 is processed by stainless steel material; It is rounded cup-shaped substantially, tank body 11 open upper end, and the center is formed with container cavity 111; Be placed with a plurality of first steel balls 13 in the container cavity 111, the open upper end edge of tank body 11 extends radially outwardly and is formed with connecting portion 112, along the circumferential direction evenly offers the connection screw 113 of a plurality of columniform perforations on the connecting portion 112; In the present invention, offer eight on the connecting portion 112 and connect screw 113.In this embodiment, the inner diameter d of tank body 11 is 5.5cm, and D outer diameter is 6.7cm, and the D outer diameter 1 of connecting portion 112 is 9cm, and its thickness h is 1cm, and the diameter d 1 that connects screw 113 is 0.8cm, and height h1 is 1cm.
As shown in Figure 3, the top cover of sample jar 1 12 is processed by stainless steel material, and it is in the form of annular discs substantially; The middle part of top cover 12 convexes with insertion section 122 downwards; The middle part of top cover 12 offers perforation 121, and perforation 121 is connected with container cavity 111, along the circumferential direction offers the fixing threaded hole 123 of a plurality of columniform perforations on the outer peripheral edges of top cover 12; In the present invention, offer eight fixing threaded holes 123 on the outer peripheral edges of top cover 12.In this embodiment, the diameter D2 of insertion section 122 is 5.2cm, and high h2 is 0.5cm, and the diameter d 2 of perforation 121 is 4mm.
High vacuum valve 2 is connected on the top cover 12 of sample jar 1, and its air inlet 21 121 is connected with the container cavity 111 of sample jar 1 through boring a hole.In the present invention; The perforation 121 of top cover 12 is designed to the structure of its upper end diameter greater than its lower end diameter; Can be connected with tube connector 22 at perforation 121 upper end through seamless welding manner like this, tube connector 22 is processed by stainless steel material, and the air inlet 21 of high vacuum valve 2 is fixedly connected on the tube connector 22 through attaching nut 23; Attaching nut 23 can firmly be connected high vacuum valve 2 on the top cover 12 with tube connector 22, and guarantees the sealing that is connected between high vacuum valve 2 and the top cover 12.High vacuum valve 2 of the present invention can be used for connecting exterior mechanical pump or molecular pump equipment, opens high vacuum valve 2, can the air in the container cavity 111 be extracted out through mechanical pump or molecular pump, reaches the purpose that makes container cavity 111 form high vacuum state.
The present invention is before ball mill grinding; At first a plurality of first steel balls 13 and rock inclusion enclave sample to be pulverized are put into the tank body 11 of sample jar 1; Then top cover 12 lids are located at tank body 11 tops; This moment, inserted in the container cavity 111 of tank bodies 11 insertion section 122 of top cover 12, afterwards with on the fixing threaded hole on the top cover 12 123 and the tank body 11 to be connected screw 113 relative one by one, and insert attachment screw 14 respectively and be fastenedly connected; At last high vacuum valve 2 is fixedly connected on the top cover 12 with attaching nut 23 through tube connector 22, accomplishes the sealing assembling of ball grinder.
When ball mill grinding, ball grinder of the present invention is connected to outside vaccum-pumping equipments such as mechanical pump or molecular pump through high vacuum valve 2, open high vacuum valve 2; Utilize mechanical pump or molecular pump that the container cavity 111 of tank body 11 is vacuumized, when vacuumizing, open 3 pairs of sample jars 1 of heating component and heat, at this moment; Rock inclusion enclave sample in the tank body 11; The various foreign gases of its surface attachment and moisture will evaporate in the container cavity 111 under the effect of heat, and along with the effect of mechanical pump or molecular pump is drawn out of outside the sample jar 1, after being vacuumized fully in the container cavity 111 of sample jar 1; Close high vacuum valve 2; Ball grinder of the present invention is placed on the grinding plate of nebula formula ball mill device, carries out high speed, efficient, pulverizing fast, the ball milling device is remaining high vacuum and high sealing state in crushing process; Gas in the tank body 11 can not leak outside; Extraneous air, particularly airborne rare gas can not get in the tank body 11 and pollutes the gas in the tank body 11; Thereby guaranteed that the rare gas of preparing in the sample jar 1 does not receive the pollution of rare gas in the air, carried out in the rock inclusion enclave analysis of rare gas full constituent and isotope analysis provides precondition and guarantee for follow-up.
The present invention is used for preparing the ball grinder of rock inclusion enclave rare gas; Because top cover 12 is that sealing is provided with each other with tank body 11; Therefore ball grinder has good sealing property; Can effectively prevent rock inclusion enclave sample the leaking outside or the inflow of outside air of rare gas in the process of ball mill grinding, guarantee that prepared rare gas does not receive the pollution of rare gas in the air; In addition, heating component 3 can carry out the temperature control heating to the rock inclusion enclave sample in the sample jar 1, with various foreign gases and the moisture of effective removal attached to rock inclusion enclave sample surfaces, for the abundant release of rare gas in the rock inclusion enclave provides prerequisite to guarantee.
According to an embodiment of the invention, between the tank body 11 of said sample jar 1 and said top cover 12, be folded with seal washer 15.Specifically be, seal washer 15 is processed by oxygenless copper material, and it is the annulus bodily form substantially, and in this embodiment, the external diameter of seal washer 15 is 6cm, and internal diameter is 5.2cm, and thickness is 2mm.The two ends up and down of seal washer 15 closely contact with the bottom surface of top cover 12 and the end face of tank body 11 respectively.
Further, in the present invention, be concaved with circular groove 114 downwards, the convex ring fin 115 that is provided with on this circular groove 114 in the end face center of tank body 11; The bottom center place of top cover 12 upwards is concaved with circular groove 124; On this circular groove 124, convex with ring fin 125 downwards; Seal washer 15 is folded between the ring fin 125 of ring fin 115 and top cover 12 of tank body 11; And ring fin 115 all is designed to tip-angled shape with ring fin 125 relative ends, the consolidation more through seal washer 15 sealings between the tank body 11 that can guarantee sample jar 1 like this and the top cover 12, the sealing property of raising ball grinder.
According to an embodiment of the invention, be placed with second steel ball 16 more than in the container cavity 111 of said sample jar 1, the diameter of said second steel ball 16 is less than the diameter of said first steel ball 13.In sample jar 1, place two kinds of steel balls that diameter is different, under same grinding rotating speed, can further promote grinding of sample jar 1 interior rock inclusion enclave sample, farthest discharge the rare gas in the rock inclusion enclave sample.In this embodiment, the diameter that in sample jar 1, is placed with two first steel balls 13 and two second steel ball 16, the first steel balls 13 is 8mm, and the diameter of second steel ball 16 is 2mm.
Like Fig. 4, shown in 5; According to an embodiment of the invention; Said heating component 3 comprises heating jacket 31 and tightens part 32, and said heating jacket 31 is around on the outer surface of said tank body 11, and two ends of said heating jacket 31 radially outward convex with connecting portion 33 respectively; The said part 32 of tightening is connected between said two connecting portions 33, and the outer surface of said heating jacket 31 is connected with heated coupling 34.
Specifically be; Tightening part 32 can closely be fixed on heating jacket 31 on tank body 11 outer surfaces of sample jar 1; The heated coupling 34 that is arranged on heating jacket 31 outsides is used to heat this heating jacket 31; Heating jacket 31 after heating can be with heat transferred tank body 11, and then the rock inclusion enclave sample in the heating tank body 11, makes the various foreign gases and moisture disengaging rock inclusion enclave sample of rock inclusion enclave sample outer surface.
Further, between said heating jacket 31 and said tank body 11, also be folded with thermocouple 35.Thermocouple 35 is used to detect the temperature of tank body 11, for the heating-up temperature of controlling heating component 3 at any time provides the numerical value support.
Like Fig. 1,6, shown in 7, according to an embodiment of the invention, the outside of said high vacuum valve 2 is arranged with gland 4, and said gland 4 is connected the top of said top cover 12.Specifically be; Gland 4 is processed by stainless steel material, and it is cylinder barrel shaped substantially, and the sidewall bottom of gland 4 convexes with curved edge 41; On top cover 12 end faces of sample jar 1 to being provided with annular groove 126 by curved edge 41; Curved edge 41 embeds in the annular groove 126 of top cover 12, and gland 4 is connected on the top cover 12 and with high vacuum valve 2 and is covered with within it, and gland 4 plays protection high vacuum valve 2 air inlets 21; The sidewall of gland 4 is provided with opening 42, and in the present invention, high vacuum valve 2 is made up of valve body 24 and control handle 25, and control handle 25 stretches out outside the opening 42, and the air inlet 21 of valve body 24 is connected on the top cover 12 with attaching nut 23 through tube connector 22.
Further, the top of said gland 4 offers the connecting hole 43 of perforation, and the gas outlet 26 of said high vacuum valve 2 is stretched in the said connecting hole 43.Connecting hole 43 can be protected the gas outlet 26 of high vacuum valve 2, and plays the effect of the connecting interface of protection gas outlet 26 and outside vaccum-pumping equipment.In this embodiment, the D outer diameter 3 of gland 4 is 6cm, and inner diameter d 3 is 4.4cm, and high h3 is 6.5cm, and opening 42 height h4 are 5cm, and opening 42 width b are 3cm, and the diameter d 4 of connecting hole 43 is 1.5cm, and high h5 is 1.1cm.
According to an embodiment of the invention, tank body 11 bottoms of said sample jar 1 are provided with three reference columns 116, and said three reference columns 116 along the circumferential direction are evenly distributed on the bottom of said tank body 11.When ball grinder of the present invention is placed on when carrying out ball mill grinding on the nebula formula ball mill device; The corresponding one by one buckle of three holddown grooves on the grinding plate of these three reference columns 116 and nebula formula ball mill device, it mainly plays situation fixing, that avoid shaking in sample jar 1 crushing process and takes place.In this embodiment, the diameter d 5 of reference column 116 is 1.5cm, and height h6 is 0.4cm, and this reference column 116 is 4cm with tank body 11 outer lateral extent a.
Embodiment 2
See also shown in Fig. 1-8, the present invention also provides a kind of method that is used for preparing rock inclusion enclave rare gas, and the said method that is used for preparing rock inclusion enclave rare gas comprises:
A) select rock inclusion enclave sample, the particle diameter size of said rock inclusion enclave sample is 0.125mm～1mm;
B) the said rock inclusion enclave sample of select is put into like each described tank body 11 that is used for preparing the ball grinder of rock inclusion enclave rare gas of claim 1～10, the amount of putting into of said rock inclusion enclave sample is 10～15 grams;
C) open said high vacuum valve 2, said sample jar 1 is vacuumized, heat through 3 pairs of said tank bodies 11 of said heating component simultaneously;
D) close said heating component 3, continue said tank body 11 is vacuumized;
E) close said high vacuum valve 2; The said ball grinder that is used for preparing rock inclusion enclave rare gas is placed on the grinding plate 5 of nebula formula ball mill device; Clamping device 51 through said nebula formula ball mill device is fixed on said grinding plate 5 with the said ball grinder that is used for preparing rock inclusion enclave rare gas; Open said nebula formula ball mill device, the said ball grinder that is used for preparing rock inclusion enclave rare gas is rotated on said grinding plate 5.
Specifically be that ball grinder structure, operation principle and the beneficial effect of this embodiment 2 are identical with the ball grinder of embodiment 1, repeat no more at this.
Before ball mill grinding; Elder generation packs 10～15 gram rock inclusion enclave samples of preliminary select in sample jar 1 tank body 11; And be respectively charged into two piece of first steel ball 13 and two piece of second steel ball 16, and seal washer 15 is placed on tank body 11 end faces and buckles top cover 12, insert in the container cavity 111 of tank bodies 11 insertion section 122 of top cover 12; Seal washer 15 is folded between the ring fin 115 of ring fin 125 and tank body 11 of top cover 12; Afterwards, the fixing threaded hole on the top cover 12 123 is corresponding one by one with connection screw 113 on the tank body 11, and penetrate attachment screw 14 respectively and be fixedly connected; At last heating component 3 is socketed in the outside of tank body 11, promptly accomplishes the pre-treatment step of rare gas in the preparation rock inclusion enclave sample.
In the ball mill grinding process, at first, ball grinder is connected to outside vaccum-pumping equipments such as mechanical pump or molecular pump through high vacuum valve 2; In this embodiment; Ball grinder is connected to the vaccum-pumping equipment of inert gas extraction and the sample-preparing system that separates (it can be 201020269937.6 patent referring to the patent No. that this inert gas extracts with the concrete structure of the sample-preparing system that separates, and its concrete structure repeats no more at this) through high vacuum valve 2, opens high vacuum valve 2; Utilize this vaccum-pumping equipment that the container cavity 111 of tank body 11 is vacuumized; When vacuumizing, open the 3 pairs of sample jars 1 of heating component that are set on the tank body 11 and heat, at this moment, the rock inclusion enclave sample in the tank body 11; The various foreign gases of its surface attachment and moisture will evaporate under the effect of heat in the container cavity 111; And, close heating component 3 this moment along with the effect of vaccum-pumping equipment is drawn out of outside the sample jar 1, continue container cavity 111 is vacuumized; Can fully the material in the sample jar 1 be extracted out like this, so that container cavity 111 reaches high vacuum state; After being vacuumized fully in the container cavity 111 of sample jar 1; Close high vacuum valve 2, ball grinder is placed on the grinding plate 5 of nebula formula ball mill device, with three corresponding buckles of respective slot (not shown) on three reference columns 116 of tank body 11 bottoms and the grinding plate 5; Be fixed on ball grinder on three lock bracket 52 of grinding plate 5 through clamping device 51 simultaneously; After treating fixedly to finish, start nebula formula ball mill device, ball grinder is rotation at a high speed on grinding plate; Rock inclusion enclave sample in the ball grinder will be efficiently, ground fast under the effect of first steel ball 13 and second steel ball 16.In the ball mill grinding process of rock inclusion enclave sample; This ball grinder is remaining the state of high vacuum and high sealing; Therefore, the gas in the tank body 11 can not leak outside extraneous air; Particularly airborne rare gas; Can not get in the tank body 11 and pollute the gas in the tank body 11, thereby guarantee that the rare gas of preparing in the sample jar 1 does not receive the pollution of rare gas in the outside air, carry out in the rock inclusion enclave analysis of rare gas full constituent and isotope analysis provides precondition and guarantee for follow-up.At last; Ball grinder is taken out in nebula formula ball mill device; And its high vacuum valve 2 is connected to the purification assemblies such as zirconium base stove of inert gas extraction and the sample-preparing system that separates; In order to the rare gas that discharges in the ball grinder is carried out purified treatment, make the rare gas in the rock inclusion enclave reach maximum enrichment and purifying.
The present invention is used for preparing the method for rock inclusion enclave rare gas; Because holding the top cover 12 of the ball grinder of rock inclusion enclave sample is that sealing is provided with each other with tank body 11; Therefore in preparation rock inclusion enclave during rare gas; Ball grinder can have good sealing property, can effectively prevent rock inclusion enclave sample the leaking outside or the inflow of outside air of rare gas in the process of ball mill grinding, has guaranteed that prepared rare gas does not receive the pollution of rare gas in the outside air; In addition, heating component 3 can carry out the temperature control heating to the rock inclusion enclave sample in the sample jar 1, with various foreign gases and the moisture of effective removal attached to rock inclusion enclave sample surfaces, for the abundant release of rare gas in the rock inclusion enclave provides prerequisite to guarantee.
According to an embodiment of the invention, in said step c, the pressure after treating to vacuumize in the said tank body 11 reaches 10
-1During Pa, carry out said steps d again.When the pressure of tank body 11 reaches 10
-1During Pa, can various foreign gases and moisture that the rock inclusion enclave sample surfaces that evaporate in the container cavity 111 adheres to be extracted out basically basically.
Further, in said steps d, the pressure after treating to vacuumize in the said tank body 11 reaches 10
-4During Pa, carry out said step e again.Can further container cavity 111 remaining various foreign gases be extracted out like this, to ensure the high vacuum state of container cavity 111.
According to an embodiment of the invention, in said step c, the heating-up temperature of said heating component 3 is 100 ℃～150 ℃.In preferred embodiment, this heating-up temperature is 110 ℃, can make the various foreign gases of rock inclusion enclave sample surfaces and the outer surface that moisture fully breaks away from the rock inclusion enclave like this.
According to an embodiment of the invention, in said step e, be 10 minutes to the said milling time that is used for preparing the ball grinder of rock inclusion enclave rare gas through said nebula formula ball mill device, the grinding rotating speed is 400rpm.Can fully grind the rock inclusion enclave sample in the tank body 11 like this, the rare gas in the rock inclusion enclave sample is fully discharged.
The above is merely several embodiments of the present invention, and those skilled in the art can carry out various changes or modification to the embodiment of the invention according to the disclosed content of application documents and not break away from the spirit and scope of the present invention.
Claims (16)
1. a ball grinder that is used for preparing rock inclusion enclave rare gas is characterized in that, the said ball grinder that is used for preparing rock inclusion enclave rare gas comprises:
Sample jar, it has the top cover that tank body and seal cover are located at said tank body top, and said tank body has container cavity, is placed with first steel ball more than in the said container cavity;
High vacuum valve, it is connected on the said top cover, offers perforation on the said top cover, and the air inlet of said high vacuum valve is connected with the container cavity of said tank body through said perforation;
Heating component, it is set in outside the tank body of said sample jar.
2. the ball grinder that is used for preparing rock inclusion enclave rare gas as claimed in claim 1 is characterized in that, between the tank body of said sample jar and said top cover, is folded with seal washer.
3. the ball grinder that is used for preparing rock inclusion enclave rare gas as claimed in claim 1 is characterized in that, is placed with second steel ball more than in the container cavity of said sample jar, and the diameter of said second steel ball is less than the diameter of said first steel ball.
4. the ball grinder that is used for preparing rock inclusion enclave rare gas as claimed in claim 3 is characterized in that, said first steel ball is two, and its diameter is 8mm; Said second steel ball is two, and its diameter is 2mm.
5. the ball grinder that is used for preparing rock inclusion enclave rare gas as claimed in claim 1; It is characterized in that; Said heating component comprise heating jacket with tighten part, said heating jacket is around on the outer surface of said tank body, two ends of said heating jacket radially outward convex with connecting portion respectively; The said part of tightening is connected between said two connecting portions, and the outer surface of said heating jacket is connected with heated coupling.
6. the ball grinder that is used for preparing rock inclusion enclave rare gas as claimed in claim 5 is characterized in that, between said heating jacket and said tank body, is folded with thermocouple.
7. the ball grinder that is used for preparing rock inclusion enclave rare gas as claimed in claim 1 is characterized in that perforation place of said top cover is connected with tube connector, and the air inlet of said high vacuum valve links to each other with said tube connector through the attaching nut.
8. the ball grinder that is used for preparing rock inclusion enclave rare gas as claimed in claim 1 is characterized in that the outside of said high vacuum valve is arranged with gland, and said gland is connected the top of said top cover.
9. the ball grinder that is used for preparing rock inclusion enclave rare gas as claimed in claim 8 is characterized in that the top of said gland offers connecting hole, and the gas outlet of said high vacuum valve is stretched in the said connecting hole.
10. the ball grinder that is used for preparing rock inclusion enclave rare gas as claimed in claim 1 is characterized in that, the tank base of said sample jar is provided with three reference columns, and said three reference columns along the circumferential direction are evenly distributed on the bottom of said tank body.
11. a method that is used for preparing rock inclusion enclave rare gas is characterized in that, the said method that is used for preparing rock inclusion enclave rare gas comprises:
A) select rock inclusion enclave sample, the particle diameter size of said rock inclusion enclave sample is 0.125mm～1mm;
B) the said rock inclusion enclave sample of select is put into like each described tank body that is used for preparing the ball grinder of rock inclusion enclave rare gas of claim 1～10, the amount of putting into of said rock inclusion enclave sample is 10～15 grams;
C) open said high vacuum valve, said sample jar is vacuumized, through said heating component said tank body is heated simultaneously;
D) close said heating component, continue said tank body is vacuumized;
E) close said high vacuum valve; The said ball grinder that is used for preparing rock inclusion enclave rare gas is placed on the grinding plate of nebula formula ball mill device; Clamping device through said nebula formula ball mill device is fixed on said grinding plate with the said ball grinder that is used for preparing rock inclusion enclave rare gas; Open said nebula formula ball mill device, the said ball grinder that is used for preparing rock inclusion enclave rare gas is rotated on said grinding plate.
12. the method that is used for preparing rock inclusion enclave rare gas as claimed in claim 11 is characterized in that, in said step c, the pressure after treating to vacuumize in the said tank body reaches 10
-1During Pa, carry out said steps d again.
13. the method that is used for preparing rock inclusion enclave rare gas as claimed in claim 12 is characterized in that, in said steps d, the pressure after treating to vacuumize in the said tank body reaches 10
-4During Pa, carry out said step e again.
14. the method that is used for preparing rock inclusion enclave rare gas as claimed in claim 11 is characterized in that, in said step c, the heating-up temperature of said heating component is 100 ℃～150 ℃.
15. the method that is used for preparing rock inclusion enclave rare gas as claimed in claim 11; It is characterized in that; In said step e; Is 10 minutes through said nebula formula ball mill device to the said milling time that is used for preparing the ball grinder of rock inclusion enclave rare gas, and the grinding rotating speed is 400rpm.
16. the method that is used for preparing rock inclusion enclave rare gas as claimed in claim 11; It is characterized in that; After said step e, also comprise step f: close said nebula formula ball mill device; The said ball grinder that is used for preparing rock inclusion enclave rare gas is taken off; The inert gas extraction is linked to each other with said high vacuum valve with the sample-preparing system that separates, open said high vacuum valve, the rare gas in the said tank body purifies with enrichment with the zirconium base stove of the sample-preparing system that separates through said inert gas extraction and handles.
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| CN103323305A (en) * | 2013-05-24 | 2013-09-25 | 中国石油天然气股份有限公司 | Sample preparation device and method for preparing rare gas in rock |
| CN103406178A (en) * | 2013-08-02 | 2013-11-27 | 浙江大学 | Ball milling pot used for preparing metal coordination hydride nanorod |
| CN103698166A (en) * | 2012-09-27 | 2014-04-02 | 中国科学院地质与地球物理研究所兰州油气资源研究中心 | Rock analysis gas high-vacuum degassing and gas-collecting device |
| CN105107590A (en) * | 2015-07-16 | 2015-12-02 | 中国地质大学（武汉） | Grinding device and method for oil gas-containing rock inclusion |
| CN108387413A (en) * | 2018-01-22 | 2018-08-10 | 中国科学院地质与地球物理研究所 | A kind of vacuum grinding device of extraction fluid inclusion gas |
| CN108398481A (en) * | 2018-01-22 | 2018-08-14 | 中国科学院地质与地球物理研究所 | A kind of method of inclusion gas phase constituent in analysis metal sulfide |
| CN108956836A (en) * | 2018-05-18 | 2018-12-07 | 中国石油化工股份有限公司 | The release of hydrocarbon gas and extraction element and method in inclusion enclave |
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| CN108956836B (en) * | 2018-05-18 | 2020-07-14 | 中国石油化工股份有限公司 | Device and method for releasing and extracting hydrocarbon gas in inclusion |
| CN113567212A (en) * | 2021-07-29 | 2021-10-29 | 中国地质科学院矿产资源研究所 | Device and method for extracting rare gas in rock mineral sample inclusion |
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Inventor after: Wang Dongliang Inventor after: Wang Xiaobo Inventor after: Li Zhisheng Inventor after: Zhang Ying Inventor after: Li Jian Inventor after: Sun Mingliang Inventor after: Li Jin Inventor after: Wang Yifeng Inventor before: Wang Dongliang Inventor before: Wang Xiaobo Inventor before: Li Zhisheng Inventor before: Zhang Ying Inventor before: Li Jian Inventor before: Sun Mingliang Inventor before: Li Jin Inventor before: Yang Chunxia Inventor before: Wang Yifeng |
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Free format text: CORRECT: INVENTOR; FROM: WANG DONGLIANG WANG XIAOBO LI ZHISHENG ZHANG YING LI JIAN SUN MINGLIANG LIJIN YANG CHUNXIA WANG YIFENG TO: WANG DONGLIANG WANG XIAOBO LI ZHISHENG ZHANG YING LI JIAN SUN MINGLIANG LI JIN WANG YIFENG |
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