CN108398481B - A kind of method of inclusion gas phase constituent in analysis metal sulfide - Google Patents
A kind of method of inclusion gas phase constituent in analysis metal sulfide Download PDFInfo
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- CN108398481B CN108398481B CN201810060425.XA CN201810060425A CN108398481B CN 108398481 B CN108398481 B CN 108398481B CN 201810060425 A CN201810060425 A CN 201810060425A CN 108398481 B CN108398481 B CN 108398481B
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Abstract
本发明公开了一种分析金属硫化物中的包裹体气相成分的方法，该方法包括：采用一种提取流体包裹体气体的真空研磨装置对样品（4）进行研磨以提取所述样品（4）中的流体包裹体气体，所述样品（4）中包括金属硫化物；以及采用四极质谱仪对提取出的所述流体包裹体气体进行分析以分析所述金属硫化物中的包裹体气相成分。
The invention discloses a method for analyzing the gas phase composition of inclusions in metal sulfide, the method comprising: grinding a sample (4) with a vacuum grinding device for extracting fluid inclusion gas to extract the sample (4) The fluid inclusion gas in the sample (4) includes metal sulfide; and the extracted fluid inclusion gas is analyzed by a quadrupole mass spectrometer to analyze the inclusion gas phase composition in the metal sulfide .
Description
Technical field
The present invention relates to geological sample analysis field, in particular to the inclusion gas in a kind of analysis metal sulfide coordinates
The method divided.
Background technique
The fluid (being properly termed as fluid inclusion) of mineral trap during the growth process saves each of geological environment at that time
Kind GEOLOGICAL AND GEOCHEMICAL information (such as temperature, pressure, system ingredient, pH value).Material composition in fluid inclusion is related
The password of geological process.Therefore system research is carried out to fluid inclusion, can obtain temperature in diagenesis and mineralizing process and
The information such as pressure condition, the chemical composition of fluid and fluid origin, to find out diagenesis, in mineralizing process geologic fluids behavior
And effect, explain diagenesis and the process and condition at mine.
It is multiple that Fluid-inclusion analysis has been widely used for geological and mineral, petroleum gas, construction material, gem and jade etc.
Research field.Theoretically, inclusion enclave is all contained in all mineral, but for generally occurring in mainly rock and the ore of research
And mineral of rich content, such as quartz, fluorite, calcite, halite, apatite, barite, cassiterite, zincblende etc..
As shown in Figure 1, generally being realized using common quadrupole mass spectrometer at present to fluid inclusion (such as Fluid inclusions
Gaseous composition in body is properly termed as fluid inclusion gas) mass spectral analysis.In geological analysis field, quadrupole mass spectrometer is
The important instrument of analysis of fluid inclution composition, main component are by four straight pole sticks as mass analyzer, this four
The straight pole stick of root is parallel with axis and equidistantly suspends；And it is identical to apply amplitude on this four straight pole sticks
DC current and radio-frequency voltage.At this point, the alternating electric field that the particle of different charge-mass ratios can be generated in this four parallel pole sticks
Middle movement, and mass separation is realized according to its motion profile, then after testing after device detection, so that it may obtain sample molecule
The mass spectrogram of (or atom).Since the mass spectrogram of sample includes the qualitative and quantitative information of sample, can then pass through
Data processing obtains the mass spectrometry results of sample.
Specifically, quadrupole mass spectrometer common shown in Fig. 1 includes with flowering structure: SV1, SV2, SV3, SV4, ISV
For gas control valve；DG is film pressure meter；VLV is needle-valve；IG is vacuum ionization ga(u)ge；QMS is four-electrode spectrum；TMP is molecule valve；
TV1, TV2, FV are solenoid valve；RP1, RP2 are mechanical pump.Connection relationship between these components is as shown in Figure 1.
When using quadrupole mass spectrometer shown in Fig. 1, the sample Jing Guo pre-treatment can be placed in quartz glass tube 500
It is interior, so that the sample in quartz glass tube 500 is reached 100 DEG C by the heating of heating furnace 600, then open SV2, is just taken out using RP2
Vacuum.Then, SV2 is closed, SV1 is opened, is further vacuumized using RP1, vacuum degree reaches 5x10 in system to be analyzed-6Pa
When, it opens SV3 and removes sample adsorbed gas.Then, SV1 is closed, furnace temp is raised to the heating rate of 1 DEG C/5s and is set
Determine temperature, then open VLV, the gas phase composition in different temperatures section is detected using QMS, finally passes through corresponding data processing
(such as processing software) calculates the molar content of gas with various component.
Since existing quadrupole mass spectrometry technology is by obtaining transparent gangue mineral (such as stone raw with spatially (companion)
English, fluorite, apatite, garnet, barite etc., wherein using quartz as optimal selection) in fluid inclusion feature come between
It is reversed to answer fluid inclusion natures, therefore infer that ore mineral (is largely opaque metal from birth by (companion) altogether spatially
Sulfide mineral) with gangue mineral (being largely transparent mineral) from same phase BIFhosted gold deposit and meanwhile precipitating be inaccurate.This example
Such as show as that pyrite, fluid inclusions homogenization temperature is higher than the fluid inclusion in gangue mineral (quartz) in cassiterite mineral
50-100 DEG C, the higher 2-10wt% of salinity.
Therefore, existing quadrupole mass spectrometry technology can only obtain gangue mineral raw with ore mineral total (companion) (such as
Above-mentioned quartz, fluorite, apatite, barite, calcite etc., wherein using quartz as optimal selection) characteristic of fluid come between it is reversed
Answer fluid inclusion natures, however, both only infer by ore mineral and gangue mineral (companion) altogether raw relationship spatially from
Precipitating is inaccurate simultaneously in same phase BIFhosted gold deposit.In order to solve this problem, directly carry out the survey to metal sulfide ore
Examination, is just particularly important with obtaining the positive evidence of reacting fluid property.
However, directly analyzing metal sulfide ore using existing quadrupole mass spectrometer, there are technology limitations.This is because golden
Belonging to the fluid inclusion in sulfide mineral cannot extract with Vacuum Heat decrepitation method, since these mineral are in higher burst temperature
Under can discharge a large amount of hydrogen sulfide (or other sulfurous gas), and hydrogen sulfide 300 DEG C or so at a temperature of can decompose reaction
Generate hydrogen and solid sulfur (i.e. H2S→H2+ S), thus hardly result in fluid inclusion in an experiment true gas componant and
Content.Moreover, because solid sulfur subparticle is easy to the flue of jam detection instrument (such as existing quadrupole mass spectrometer)
Road and each control valve (example SV1 ~ SV4 gas control valve as shown in figure 1, ISV gas control valve, VLV needle-valve etc.), therefore use
Vacuum Heat decrepitation method extraction metal sulfide ore (as shown in Figure 1) is simultaneously infeasible.In addition, Vacuum Heat decrepitation method is produced when heated
Raw a large amount of sulfurous gas also can have corrosivity to instrument (such as corresponding pipeline and mass spectrograph), to reduce instrument
Service life.
Summary of the invention
The main object of the present invention is to provide a kind of method for analyzing the inclusion gas phase constituent in metal sulfide, with solution
Certainly problem above and other potential problems in the prior art.
In order to achieve the above object, the invention proposes a kind of sides of the inclusion gas phase constituent in analysis metal sulfide
Method, which comprises a kind of vacuum grinding device for extracting fluid inclusion gas is used to grind to mention sample (4)
The fluid inclusion gas in the sample (4) is taken, includes metal sulfide in the sample (4)；And use four-electrode spectrum
Instrument analyzes to analyze the inclusion gas phase constituent in the metal sulfide fluid inclusion gas extracted；
Wherein, the vacuum grinding device for extracting fluid inclusion gas includes: pedestal (1), internal to have cavity (2), described
Cavity (2) has opening (11) on the top (10) of the pedestal (1)；Sample jar (3), is arranged to through the opening
(11) it is put into the cavity (2), and for sample (4) to be contained in the sample jar (3)；Motor (5), removably
It is installed on the top (10) of the pedestal (1), and closes the opening (11) so that the sample (4) is enclosed in the cavity
(2) in；And grinding tup (6), it is connected with each other via the output shaft of shaft coupling (7) and the motor (5)；The wherein bottom
It is additionally provided with the side-wall hole (13) being connected to the cavity (2) on the side wall (12) of seat (1), is connected on the side-wall hole (13)
Have vacuum valve (8), the vacuum valve (8) is provided so that the cavity (2) can be evacuated；The wherein grinding
Tup (6) is arranged under the driving of the motor (5) and under the drive of the shaft coupling (7), to the sample jar (3)
The interior sample (4) is ground to extract the fluid inclusion gas in the sample (4).
In accordance with an embodiment of the present disclosure, the vacuum grinding device of the extraction fluid inclusion gas further include: pressure is adjusted
Knob (9) has the first end (91) suitable for rotating and the second end (92) for installing spring (90), the spring (90)
The bottom (30) of the sample jar (3) is abutted to, the pressure adjustment knob (9) is arranged to be used for adjusting the spring (90)
Abut the support force of the bottom (30) of the sample jar (3).
In accordance with an embodiment of the present disclosure, the bottom (14) of the pedestal (1) is equipped with bottom opening (15), the second end
(92) bottom opening (15) are passed through and are connected with the spring (90).
In accordance with an embodiment of the present disclosure, the bottom (30) of the sample jar (3) is equipped with counterbore (31), the spring (90)
One end abut in the counterbore (31), the other end is connected with the second end (92).
In accordance with an embodiment of the present disclosure, the periphery of the spring (90) is additionally provided with seal bellows (93), the pressure
Adjusting knob (9) is arranged to be used for adjusting stroke of the spring (90) in the seal bellows (93), to adjust
State the support force that spring (90) abut the bottom (30) of the sample jar (3).
In accordance with an embodiment of the present disclosure, heating plate (40), the heating plate are additionally provided on the bottom (14) of the pedestal (1)
(40) it is installed on the bottom (14) of the pedestal (1) by heat source mounting flange (50)；The heat source mounting flange (50)
Lower part is additionally provided with hexagon socket head cap screw, and the hexagon socket head cap screw enables to the vacuum grinding dress for extracting fluid inclusion gas
It sets and is fixed on experimental bench.
In accordance with an embodiment of the present disclosure, be additionally provided between the motor (5) and the top (10) of the pedestal (1) for pair
The sealing magnetic fluid (60) that the opening (11) is sealed；The longitudinal section of the cavity (2) is T-shaped so that the pedestal
(1) there are stage portion (16) on inner wall, the sample jar (3) is fixed on the stage portion by the flange (32) at the top of it
(16) on；The motor includes frequency modulation stepper motor；The sample jar is made by best bright finish material；The pedestal (1) is by height
The production of intensity stainless steel material.
In accordance with an embodiment of the present disclosure, the quadrupole mass spectrometer includes with flowering structure: gas control valve SV1, gas control
Valve SV2, gas control valve SV3, gas control valve SV4, gas control valve ISV, film pressure meter DG, needle-valve VLV, vacuum ionization ga(u)ge
IG, four-electrode spectrum QMS, molecule valve TMP, solenoid valve TV1, solenoid valve TV2, solenoid valve FV, mechanical pump RP1 and mechanical pump
RP2；The vacuum valve (8) connect with the gas control valve SV3 so that the cavity (2) can be by the four-electrode spectrum
Instrument vacuumizes.
In accordance with an embodiment of the present disclosure, wherein described using a kind of vacuum grinding device for extracting fluid inclusion gas
Sample (4) is ground to extract the fluid inclusion gas in the sample (4), comprising: be put by the sample (4)
After in the sample jar (3), the vacuum grinding device for extracting fluid inclusion gas is assembled, and by the vacuum valve
Door (8) is connect with the gas control valve SV3；The vacuum valve (8) and the gas control valve SV3 are opened to utilize institute
It states mechanical pump RP1 and the mechanical pump RP2 vacuumizes the vacuum grinding device, reach 5x10 to vacuum degree-6Institute is closed after Pa
State vacuum valve (8) and the gas control valve SV3；And the starting motor (5), initial grinding rate is set as
1r/min is gradually increased grinding rate after the grinding tup (6) rotation, needed for being then ground to the sample (4) again
The motor (5) is turned off when granularity to extract the fluid inclusion gas in the sample (4)；Wherein, according to the sample (4)
Difference set different grinding rates.
In accordance with an embodiment of the present disclosure, wherein it is described using quadrupole mass spectrometer to the fluid inclusion gas extracted
Body is analyzed to analyze the inclusion gas phase constituent in the metal sulfide, comprising: opens the vacuum valve (8) and institute
Gas control valve SV3 is stated so that the fluid inclusion gas extracted enters the quadrupole mass spectrometer；And open institute
Needle-valve VLV is stated, so that the fluid inclusion gas extracted is diffused into the four-electrode spectrum QMS due to pressure difference
In, so that the inclusion gas phase constituent and Mole percent that are detected in the metal sulfide using the four-electrode spectrum QMS are contained
Amount.
Compared with prior art, the invention has the following advantages that the inclusion gas in the analysis metal sulfide of the disclosure
The method of phase constituent can be to fluid packet due to using a kind of vacuum grinding device for extracting fluid inclusion gas
Wrap up in body (it may include metal sulfide) all gas component (comprising in metal sulfide inclusion gas phase constituent or
Rare gas) it is tested, therefore application range is wider.Moreover, because using lapping mode, therefore it is more efficient, speed is more
Fastly；And the granularity after grinding can thinner (such as reach 150 mesh to 200 mesh or so), so 90% Fluid inclusions can be made
Body is opened, and can thus reduce sample size.Further, since can be replaced manually with automatic, therefore automatization level is improved,
It is more efficient.
Detailed description of the invention
Illustrate technical solution of the present invention in order to clearer, it below will be to attached drawing needed in embodiment description
It is briefly described, it is clear that, drawings in the following description are only some embodiments of the invention, general for this field
For logical technical staff, without creative efforts, it is also possible to obtain other drawings based on these drawings.
Fig. 1 is the structural schematic diagram of existing quadrupole mass spectrometer.
Fig. 2 is the structural schematic diagram according to the vacuum grinding device of the extraction fluid inclusion gas of the embodiment of the present disclosure.
Fig. 3 is the structural schematic diagram according to the vacuum grinding device of the extraction fluid inclusion gas of the embodiment of the present disclosure.
Fig. 4 is the vacuum grinding device according to the extraction fluid inclusion gas of the embodiment of the present disclosure for analyzing metal sulphur
Change structural schematic diagram when fluid inclusion gas phase composition in mineral.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Whole description, it is clear that the described embodiments are merely a part of the embodiments of the present invention, the embodiment being not all of, and is based on this hair
Embodiment in bright, those of ordinary skill in the art's every other implementation obtained under that premise of not paying creative labor
Example, shall fall within the protection scope of the present invention.
Present disclose provides a kind of methods of the inclusion gas phase constituent in analysis metal sulfide to solve the prior art
Problem above and other potential problems in (as shown in Figure 1) extract the true of fluid inclusion gas the process employs a kind of
Empty grinding device overcomes the problems, such as brought by Vacuum Heat decrepitation method.
Specifically, in order to solve in Fig. 1 in the presence of existing quadrupole mass spectrometer the technical issues of, each reality of the disclosure
It applies example and provides a kind of method for analyzing the inclusion gas phase constituent in metal sulfide, which comprises mentioned using one kind
The vacuum grinding device of fluid inclusion gas is taken to grind sample 4 to extract the fluid inclusion gas in the sample 4
Body includes metal sulfide in the sample 4；And using quadrupole mass spectrometer to the fluid inclusion gas extracted into
Row analysis is to analyze the inclusion gas phase constituent in the metal sulfide.
Fig. 2 shows the structures of the vacuum grinding device according to an embodiment of the present disclosure for extracting fluid inclusion gas to show
It is intended to.Fig. 3 shows the example sizes of the vacuum grinding device of the disclosure (unit of its numerical value is, for example, millimeter).The disclosure
Extract the vacuum grinding device of fluid inclusion gas, including pedestal 1, sample jar 3, motor 5 and grinding tup 6.
As shown in Fig. 2-Fig. 3, the inside of pedestal 1 has cavity 2, and the cavity 2 has on the top 10 of the pedestal 1
Opening 11.Sample jar 3 is arranged to be put into the cavity 2 through the opening 11, and for sample 4 to be contained in the sample
In tank 3.
In accordance with an embodiment of the present disclosure, the longitudinal section of the cavity 2 is T-shaped so that the pedestal 1 has on inner wall
Stage portion 16, the sample jar 3 are fixed in the stage portion 16 by the flange 32 at the top of it.
For example, the longitudinal section of cavity 2 is T-shaped, such as T-shaped (for example, cavity 2 can along the section of the central axis of pedestal 1
To be set as top diametrically biggish cylinder, lower part diametrically lesser cylinder).For example, the step for passing through the disclosure
Sample jar 3 is passed through 11 cavitys 2 being put into the inside of pedestal 1 that are open with can be convenient by the mutual cooperation in portion 16 and flange 32
It is interior.For example, the production of best bright finish material can be used in sample jar 3, gas absorption is prevented.
In accordance with an embodiment of the present disclosure, motor 5 is releasably attached on the top 10 of the pedestal 1, and described in closing
Opening 11 is the sample 4 to be enclosed in the cavity 2.
For example, motor 5 can be releasably attached on the top 10 of the pedestal 1, and close the opening 11 with
The sample 4 is enclosed in the cavity 2, after can making in the cavity 2 that sample jar 3 is put into pedestal 1 in this way, is made
It is sealed in the cavity 2 of pedestal 1, facilitates subsequent vacuumize and ground sample.
In accordance with an embodiment of the present disclosure, heating plate 40 is additionally provided on the bottom 14 of the pedestal 1, the heating plate 40 passes through
Heat source mounting flange 50 is installed on the bottom 14 of the pedestal 1.
For example, heat source mounting flange can heat the sample in sample jar 3, after being heated by being equipped with heating plate
Gas in cavity 2 is not easy to be adsorbed on sample, is easy to be taken away by vacuum mechanical pump, to keep the high vacuum ring in cavity 2
Border.
In accordance with an embodiment of the present disclosure, the lower part of the heat source mounting flange 50 is additionally provided with hexagon socket head cap screw, it is described in six
Angle screw enables to the vacuum grinding device for extracting fluid inclusion gas to be fixed on experimental bench.
For example, hexagon socket head cap screw is arranged at the lower part of heat source mounting flange 50, the vacuum grinding device of the disclosure can be fixed
On experimental bench.
As shown in Fig. 2-Fig. 3, in accordance with an embodiment of the present disclosure, grinding tup 6 is defeated via shaft coupling 7 and the motor 5
Shaft is connected with each other.The side-wall hole 13 being connected to the cavity 2 is additionally provided on the side wall 12 of the pedestal 1, the side wall is opened
Vacuum valve 8 is connected on hole 13, the vacuum valve 8 is provided so that the cavity 2 can be evacuated；It is wherein described
Grinding tup 6 is arranged under the driving of the motor 5 and under the drive of the shaft coupling 7, in the sample jar 3
The sample 4 is ground to extract the fluid inclusion gas in the sample 4.
For example, shaft coupling 7 is used to connect the output shaft and grinding tup 6 of motor 5, effect is to make to grind tup 6 always
Holding center rotation, without deflecting.For example, pedestal 1 can be made by high-strength stainless steel, the side wall 12 of pedestal 1
On can connect vacuum valve 8.
In accordance with an embodiment of the present disclosure, it is additionally provided between the motor 5 and the top 10 of the pedestal 1 for opening described
Mouthfuls 11 sealing magnetic fluid 60(sealing magnetic fluids 60 being sealed are in existing equipment and are not present, and leakproofness can be with
Reach 5x10-12Pa.Corresponding sealing flange can also be arranged in the top of sealing magnetic fluid 60).
In accordance with an embodiment of the present disclosure, the motor includes frequency modulation stepper motor；The vacuum valve 8 and vacuum pump (example
Such as mechanical pump RP1, RP2 in quadrupole mass spectrometer) connection so that the cavity 2 can be vacuumized by the vacuum pump (such as
It is connect with the gas control valve SV3 in quadrupole mass spectrometer, so that the cavity 2 can be by the machinery in the quadrupole mass spectrometer
Pumping vacuum)；The sample jar is made by best bright finish material；The pedestal 1 is made by high-strength stainless steel material.
For example, the motor of the disclosure is frequency modulation stepper motor, variable speed is used, and reversion can be rotated forward, it can
Accomplish to adjust revolving speed in real time and rotary speed parameter can be with real-time display on the control panel.
As shown in Fig. 2-Fig. 3, the vacuum grinding device of the extraction fluid inclusion gas of the disclosure can also include: pressure
Adjusting knob 9, has suitable for the first end 91 of rotation and the second end 92 for installing spring 90, the spring 90 abut to
The bottom 30 of the sample jar 3, the pressure adjustment knob 9, which is arranged to be used for adjusting the spring 90, abuts the sample jar
The support force of 3 bottom 30.
For example, being rotated by the first end 9 in pressure adjustment knob 9 (it is provided with screw thread, conveniently for example uses hand
The rotation of fingering row), the spring 90 in adjustable second end 92 abuts the support force of the bottom 30 of the sample jar 3, in this way may be used
Different support forces (power pushed up upwards) is used with different according to sample, to adjust between sample jar and grinding tup
Different grinding dynamics is arranged to adapt to different sample needs in grinding dynamics.
In accordance with an embodiment of the present disclosure, the bottom 14 of the pedestal 1 is equipped with bottom opening 15, and the second end 92 passes through
The bottom opening 15 is simultaneously connected with the spring 90.
For example, can 14 aperture of bottom to the pedestal 1, so as to connect pressure adjustment knob.Pressure adjusts rotation
Spring 90 is placed in the top of button, and the top of spring withstands on the bottom of sample jar.
In accordance with an embodiment of the present disclosure, the bottom 30 of the sample jar 3 is equipped with counterbore 31, and one end of the spring 90 is supported
It is connected in the counterbore 31, the other end is connected with the second end 92.
For example, counterbore 31 can be equipped on the bottom 30 of sample jar 3, so that one end of spring 90 abuts to described sink
In hole 31, the other end is connected with the second end 92, and the top of spring can be made to withstand on the bottom of sample jar in this way.
In accordance with an embodiment of the present disclosure, the periphery of the spring 90 is additionally provided with seal bellows 93, and the pressure is adjusted
Knob 9 is arranged to be used for adjusting stroke of the spring 90 in the seal bellows 93, is supported with adjusting the spring 90
Connect the support force of the bottom 30 of the sample jar 3.
For example, the periphery of spring can be encased with seal bellows 93, such pressure adjustment knob 9 can be adjusted when rotated
Stroke of the spring in seal bellows 93 is saved, so that elastic force also correspondingly changes when the stroke of spring changes, from
And to change to the support force of sample jar, to adapt to different sample needs, different grinding dynamics is set.
Based on described above, for example, the disclosure extraction fluid inclusion gas vacuum grinding device at work, can
With using stepper motor rotate drive grinding tup rotation, shaft coupling can real-time ensuring grinding tup carry out center rotating and
It does not deflect.Stepper motor can adjust slewing rate in real time, can be continuously adjusted to 100r/min from 1r/min, grind to drive
Mill tup carrys out ground sample.
Simultaneously as being also set up below pedestal in the vacuum grinding device of the extraction fluid inclusion gas of the disclosure
There is pressure adjustment knob, which is connected with spring, and spring resists sample jar, therefore can be according to different samples
The power that product are pushed up upwards using difference, so as to adjust sample jar in real time and grind the grinding dynamics between tup.
After vacuum grinding device using the extraction fluid inclusion gas of the disclosure, sample can be for example set most to exist slowly
Grinding finishes in 0.5h, and can most grind and finish in 5min fastly, therefore save time cost.And due to grinding after
Granularity can thinner (such as reach 150 mesh to 200 mesh or so), so 90% fluid inclusion can be made to be opened, thus
Sample size can be reduced.Further, since can be replaced manually with automatic, therefore automatization level is improved, it is more efficient.
In accordance with an embodiment of the present disclosure, in the vacuum grinding using extraction fluid inclusion gas shown in Fig. 2-Fig. 3
After device grinding sample, quadrupole mass spectrometer can be used to analyze to analyze the fluid inclusion gas extracted
Inclusion gas phase constituent in the metal sulfide.
As an example, as shown in figure 4, quadrupole mass spectrometer employed in the disclosure includes with flowering structure: gas control valve
SV1, gas control valve SV2, gas control valve SV3, gas control valve SV4, gas control valve ISV, film pressure meter DG, needle-valve
VLV, vacuum ionization ga(u)ge IG, four-electrode spectrum QMS, molecule valve TMP, solenoid valve TV1, solenoid valve TV2, solenoid valve FV, mechanical pump
RP1 and mechanical pump RP2；In the disclosure extraction fluid inclusion gas vacuum grinding device in vacuum valve (8) with
Gas control valve SV3 connection in quadrupole mass spectrometer is so that the cavity (2) can be vacuumized by the quadrupole mass spectrometer.
In accordance with an embodiment of the present disclosure, the vacuum grinding device using a kind of extraction fluid inclusion gas is to sample
(4) it is ground to extract the fluid inclusion gas in the sample (4), comprising: the sample (4) is being put into the sample
After in product tank (3), the vacuum grinding device for extracting fluid inclusion gas is assembled, and by the vacuum valve (8)
It is connect with the gas control valve SV3；The vacuum valve (8) and the gas control valve SV3 are opened to utilize the machinery
The pump RP1 and mechanical pump RP2 vacuumizes the vacuum grinding device, reaches 5x10 to vacuum degree-6The vacuum is closed after Pa
Valve (8) and the gas control valve SV3；And the starting motor (5), initial grinding rate is set as 1r/min,
It is gradually increased grinding rate again after the grinding tup (6) rotation, then the pass when sample (4) is ground to required granularity
The motor (5) break to extract the fluid inclusion gas in the sample (4)；Wherein, according to the difference of the sample (4) come
Set different grinding rates.
As an example, the embodiment of the present disclosure provide extraction fluid inclusion gas vacuum grinding device in use,
It can be operated using following steps:
1, stepper motor (thereon with structures such as sealing magnetic fluids 60) is removed, sample jar is taken out.
2, stepper motor is covered after 5g sample being put into sample jar and fixes (such as tightening screw).
3, power on, open heating plate, temperature is set in 50 DEG C, after reaching set temperature, constant temperature 10min.At this time
Vacuum valve is opened, is vacuumized with vacuum mechanical pump (such as vacuum mechanical pump RP1, the RP2 being had in quadrupole mass spectrometer).In this way
Sample surfaces can be excluded, the gas that the vacuum grinding device inner wall of the disclosure adsorbs, in the vacuum grinding device of the disclosure
Vacuum degree reaches 5x10-6Vacuum valve is closed after Pa.
4, start stepper motor, initial rate is set as 1r/min, after determining grinding tup rotation, then start gradually to add
Big rate.Different grinding rates can be set according to different samples.After grinding a period of time, sample is ground into required grain
It spends, the fluid inclusion in sample is opened, gas release.
5, vacuum valve is opened, gas slowly is made to enter external mass spectrograph (such as quadrupole mass spectrometer) by vacuum valve
In, to measure the ingredient of gas with various and the molar content of gas with various ingredient.
In accordance with an embodiment of the present disclosure, described that the fluid inclusion gas extracted is carried out using quadrupole mass spectrometer
Analysis is to analyze the inclusion gas phase constituent in the metal sulfide, comprising: opens the vacuum valve (8) and the gas
Control valve SV3 is so that the fluid inclusion gas extracted enters the quadrupole mass spectrometer；And open the needle-valve
VLV, so that the fluid inclusion gas extracted is diffused into the four-electrode spectrum QMS due to pressure difference, thus
Inclusion gas phase constituent and the molar content in the metal sulfide are detected using the four-electrode spectrum QMS.
As an example, as shown in figure 4, the vacuum grinding device of the extraction fluid inclusion gas of the disclosure, such as especially
The fluid inclusion gas phase composition suitable for analysis metal sulfide ore.This is because existing quadrupole mass spectrometer is generally all adopted
Fluid inclusion gas is extracted with Vacuum Heat decrepitation method, and as previously mentioned, metal sulfide ore cannot use Vacuum Heat decrepitation method
It extracts.Therefore, Vacuum Heat decrepitation method can be evaded using the vacuum grinding device of the disclosure and extracts lacking for fluid inclusion gas
It falls into, thus especially suitable for fluid inclusion gas phase composition in analysis metal sulfide ore, to overcome existing quadrupole mass spectrometer
Technological deficiency.
For example, in high vacuum (such as 10-6Pa it) under environment, is ground using the vacuum of the extraction fluid inclusion gas of the disclosure
Mill apparatus can open fluid inclusion (such as fluid inclusion in metal sulfide ore) in a manner of grinding, so as to
Directly carry out the analysis to fluid inclusion gas phase composition in opaque metal sulfide ore.When specific operation, it can use
Following steps:
1. weighing about 5g sample, it is put into the vacuum grinding device of the extraction fluid inclusion gas in the embodiment of the present disclosure
In sample jar in, assemble the vacuum grinding device of the disclosure, and it is passed through into vacuum valve and mass spectrometer (such as four
Pole mass spectrograph) it is connected with each other (as shown in figure 4, the vacuum valve and four-electrode spectrum of the vacuum grinding device of the disclosure can be passed through
The SV3 of instrument is connected with each other)；
2. opening SV2, just vacuumized using RP2；It is then shut off SV2, SV1 is opened, is further vacuumized using RP1, to
Vacuum degree reaches 10 in pipeline-5SV3 is opened when Pa, the gas adsorbed on sample to remove is then shut off SV3；
3. starting the vacuum grinding device in the embodiment of the present disclosure, sample is ground broken, inclusion enclave after a period of time
It is opened, internal gas release；
4. being again turned on SV3 at this time, SV1 is closed, opens VLV, gas is because pressure difference is diffused into QMS, to utilize QMS
Carry out detection gas component, such as can know in inclusion enclave the ingredient and molar content (such as Mole percent of different gas phases
Than)；
Compared with prior art, the vacuum grinding device shown in Fig. 4 using in the embodiment of the present disclosure analyzes metal sulphur
The embodiment for changing fluid inclusion gas phase composition in mineral, has the advantage that
1, it can will be suitable for the mineral species of quadrupole mass spectrometry technology by transparent minerals such as single quartz, calcites
It is expanded to most metal sulfide ore (such as pyrite, chalcopyrite, galena).
2, it in geological research field, is capable of providing Diagenesis And Mineralization fluid properties and positive evidence that activity is developed (such as is made
For the metal sulfide ore for reacting fluid inclusion's charcters positive evidence), to eliminate circumstantial evidence bring inaccuracy.
Through the above description of the embodiments, those skilled in the art can be understood that the present invention can be with
It is realized by other structures, feature of the invention is not limited to above-mentioned preferred embodiment.It is any to be familiar with this technology
Personnel are in technical field of the invention, the changes or modifications that can be readily occurred in, and should all cover in patent protection model of the invention
Within enclosing.
Claims (4)
1. a kind of method of the inclusion gas phase constituent in analysis metal sulfide, which comprises
A kind of vacuum grinding device for extracting fluid inclusion gas is used to grind to extract the sample sample (4)
(4) the fluid inclusion gas in includes metal sulfide in the sample (4)；And
Quadrupole mass spectrometer is used to analyze to analyze in the metal sulfide fluid inclusion gas extracted
Inclusion gas phase constituent；
Wherein, the vacuum grinding device for extracting fluid inclusion gas includes:
Pedestal (1), internal to have cavity (2), the cavity (2) has opening on the top (10) of the pedestal (1)
(11)；
Sample jar (3) is arranged to be put into through the opening (11) in the cavity (2), and for sample (4) to be contained in
In the sample jar (3)；
Motor (5) is releasably attached on the top (10) of the pedestal (1), and closes the opening (11) with by institute
Sample (4) is stated to be enclosed in the cavity (2)；And
It grinds tup (6), is connected with each other via the output shaft of shaft coupling (7) and the motor (5)；
Wherein the side-wall hole (13) being connected to the cavity (2), the side wall are additionally provided on the side wall (12) of the pedestal (1)
It is connected in aperture (13) vacuum valve (8), it is true that the vacuum valve (8) is provided so that the cavity (2) can be taken out
It is empty；
Wherein grinding tup (6) is arranged to the drive under the driving of the motor (5) and in the shaft coupling (7)
Under, the sample (4) in the sample jar (3) is ground to extract the fluid inclusion gas in the sample (4)；
Wherein, the vacuum grinding device for extracting fluid inclusion gas further include: pressure adjustment knob (9) has suitable
In the first end (91) of rotation and second end (92) for installing spring (90), the spring (90) abuts to the sample jar
(3) bottom (30), the pressure adjustment knob (9) are arranged to be used for adjusting the spring (90) abutting sample jar
(3) support force of bottom (30)；
Wherein, the bottom (14) of the pedestal (1) is equipped with bottom opening (15), and the second end (92) passes through the bottom and opens
Hole (15) is simultaneously connected with the spring (90)；
Wherein, the bottom (30) of the sample jar (3) is equipped with counterbore (31), and one end of the spring (90) abuts to described heavy
In hole (31), the other end is connected with the second end (92)；
Wherein, the periphery of the spring (90) is additionally provided with seal bellows (93), and the pressure adjustment knob (9) is arranged to
For adjusting stroke of the spring (90) in the seal bellows (93), the sample is abutted to adjust the spring (90)
The support force of the bottom (30) of product tank (3)；
Wherein, it is additionally provided with heating plate (40) on the bottom (14) of the pedestal (1), the heating plate (40) passes through heat source fixation
Blue (50) are installed on the bottom (14) of the pedestal (1)；It is characterized in that, the lower part of the heat source mounting flange (50) is also set
There is hexagon socket head cap screw, the hexagon socket head cap screw enables to the vacuum grinding device for extracting fluid inclusion gas to be fixed to
On experimental bench；
Wherein, it is additionally provided between the motor (5) and the top (10) of the pedestal (1) close for being carried out to the opening (11)
The sealing magnetic fluid (60) of envelope；The longitudinal section of the cavity (2) is T-shaped so that the pedestal (1) has step on inner wall
Portion (16), the sample jar (3) are fixed on the stage portion (16) by the flange (32) at the top of it；The motor includes adjusting
Frequency stepper motor；The sample jar is made by best bright finish material；The pedestal (1) is made by high-strength stainless steel material.
2. the method for the inclusion gas phase constituent in analysis metal sulfide according to claim 1, which is characterized in that institute
Stating quadrupole mass spectrometer includes with flowering structure: gas control valve SV1, gas control valve SV2, gas control valve SV3, gas control valve
SV4, gas control valve ISV, film pressure meter DG, needle-valve VLV, vacuum ionization ga(u)ge IG, four-electrode spectrum QMS, molecule valve TMP, electromagnetism
Valve TV1, solenoid valve TV2, solenoid valve FV, mechanical pump RP1 and mechanical pump RP2；The vacuum valve (8) and the gas control
Valve SV3 connection processed is so that the cavity (2) can be vacuumized by the quadrupole mass spectrometer.
3. the method for the inclusion gas phase constituent in analysis metal sulfide according to claim 2, which is characterized in that its
In, it is described that a kind of vacuum grinding device for extracting fluid inclusion gas is used to grind to extract the sample sample (4)
Fluid inclusion gas in product (4), comprising:
After the sample (4) is put into the sample jar (3), the vacuum for extracting fluid inclusion gas is assembled
Grinding device, and the vacuum valve (8) is connect with the gas control valve SV3；
The vacuum valve (8) and the gas control valve SV3 are opened to utilize the mechanical pump RP1 and mechanical pump RP2
The vacuum grinding device is vacuumized, reaches 5x10 to vacuum degree-6The vacuum valve (8) and gas control are closed after Pa
Valve SV3；And
Start the motor (5), initial grinding rate be set as 1r/min, after the grinding tup (6) rotation after again by
Grinding rate is gradually increased, turns off the motor (5) when the sample (4) is ground to required granularity then to extract the sample
(4) the fluid inclusion gas in；Wherein, different grinding rates is set according to the difference of the sample (4).
4. the method for the inclusion gas phase constituent in analysis metal sulfide according to claim 3, which is characterized in that its
In, it is described that quadrupole mass spectrometer is used to analyze to analyze the metal sulfide fluid inclusion gas extracted
In inclusion gas phase constituent, comprising:
Open the vacuum valve (8) and the gas control valve SV3 so that the fluid inclusion gas extracted into
Enter the quadrupole mass spectrometer；And
The needle-valve VLV is opened, so that the fluid inclusion gas extracted is diffused into described four due to pressure difference
In the mass spectrum QMS of pole, to detect the inclusion gas phase constituent in the metal sulfide using the four-electrode spectrum QMS and rub
That percentage composition.
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| CN201810060425.XA CN108398481B (en) | 2018-01-22 | 2018-01-22 | A kind of method of inclusion gas phase constituent in analysis metal sulfide |
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| CN110187011B (en) * | 2019-07-03 | 2024-04-16 | 新疆维吾尔自治区煤田地质局煤层气研究开发中心 | Simulation experimental device and simulation method for dynamic adsorption and desorption research |
| CN113567212B (en) * | 2021-07-29 | 2022-03-08 | 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 |
| CN115808340B (en) * | 2022-12-27 | 2023-11-03 | 内蒙古工业大学 | A device and method for gas extraction from metallic mineral inclusions |
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| JP2000079352A (en) * | 1998-08-11 | 2000-03-21 | Loesche Gmbh | Grinding plant and raw material grinding method |
| CN201143450Y (en) * | 2007-11-29 | 2008-11-05 | 华东师范大学 | A screw grinder |
| CN102600937A (en) * | 2012-03-28 | 2012-07-25 | 中国石油天然气股份有限公司 | Ball mill tank and method for preparing rare gas in rock inclusions |
| CN104383988A (en) * | 2014-09-15 | 2015-03-04 | 昆山熙勤自动化设备有限公司 | Spring compression type milling equipment |
| CN104407089A (en) * | 2014-12-09 | 2015-03-11 | 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 degassing high-sensitivity gas chromatography-mass spectrometry coupling analysis system and use method thereof |
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|---|---|---|---|---|
| CN2154482Y (en) * | 1993-04-27 | 1994-01-26 | 祝学禹 | Grind machine for analysing sample |
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|---|---|---|---|---|
| JP2000079352A (en) * | 1998-08-11 | 2000-03-21 | Loesche Gmbh | Grinding plant and raw material grinding method |
| CN201143450Y (en) * | 2007-11-29 | 2008-11-05 | 华东师范大学 | A screw grinder |
| CN102600937A (en) * | 2012-03-28 | 2012-07-25 | 中国石油天然气股份有限公司 | Ball mill tank and method for preparing rare gas in rock inclusions |
| CN104383988A (en) * | 2014-09-15 | 2015-03-04 | 昆山熙勤自动化设备有限公司 | Spring compression type milling equipment |
| CN104407089A (en) * | 2014-12-09 | 2015-03-11 | 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 degassing high-sensitivity gas chromatography-mass spectrometry coupling analysis system and use method thereof |
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