CN106168545A - A kind of dynamic leaching residue sampler - Google Patents
A kind of dynamic leaching residue sampler Download PDFInfo
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- CN106168545A CN106168545A CN201610841389.1A CN201610841389A CN106168545A CN 106168545 A CN106168545 A CN 106168545A CN 201610841389 A CN201610841389 A CN 201610841389A CN 106168545 A CN106168545 A CN 106168545A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N1/20—Devices for withdrawing samples in the liquid or fluent state for flowing or falling materials
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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Abstract
The invention discloses a kind of dynamic leaching residue sampler, including leaching post and the sample holder being placed in described leaching post；Described leaching post upper end mounting spray head, draining pipe is installed in lower end；Being provided with load sample platform in described leaching post, described load sample number of units amount is the integer more than or equal to 1, and each load sample platform is placed a sample holder；Pod apertures is had on described load sample platform；It is provided with pod apertures bottom described sample holder.Assembly of the invention, in same set of leaching system, completes the sampling of the dynamic leaching residue to test sample with eluviation process, saves leaching liquor, it is not necessary to make parallel leaching system.Device is simple, it is easy to operation, reproducible, technical staff is easy to learn, easily grasp.
Description
Technical field
The invention belongs to chemical extraction experimental technique field, specifically, relate to a kind of dynamic leaching residue sampling dress
Put.
Background technology
In Epigentic Geochemistry is studied, it is completely dependent on the development characteristics of field weathering profile, is sometimes difficult to truly disclose
Geochemical behaviour of element and mineralogical corrosion mechanism during rock decay.Its reason is: rock decay forms air slaking and cuts open
During face, along with air slaking fluid permeates downwards, from the fine mineral component (such as colloidal solid) of section top leaching at section
Bottom deposits；It addition, the lateral migration of air slaking fluid is likely to cause Exterior component to be brought into weathering profile.Due to foreign substance
Deposit in weathering profile, masks element geochemistry and the real information of mineralogy change during rock decay.For
This, utilize leaching simulation experiment, dynamically analyzes protolith and forms with the leaching residue of eluviation (i.e. weathering) process, is
Geochemical behaviour of element and the effective means of mineralogy change during spike rock decay.
Sampling currently for dynamic leaching residue generally uses batch experiment, i.e. protolith sample by broken and abundant
Mixing retraction is divided into some equal portions (i.e. increment, the No.1 that numbers in order, No.2 ...), under identical experiment condition, each son
Sample, respectively as an independent experimental considerations unit, synchronizes to carry out Leaching Experiments.Reaching a certain stage with leaching process, No.1 stops
Leaching, collects leaching residue standby；Entering next stage with Leaching Experiments, No.2 stops leaching, collects leaching with No.1 residual
Excess is standby；By that analogy, until last part sample terminates leaching.Theoretically, according to No.1, the order of No.2 ...,
Protolith is increased by the intensity of weathering successively, therefore, by analyze protolith → No.1 → No.2 →... ... material composition
Change, it is possible to obtain element geochemistry and the information of mineralogy change during rock decay.
In above experimental program, it is both needed to each increment prepare a set of independent Leaching Experiments system, and needs
Consuming substantial amounts of leaching liquor, uneconomical, operation is loaded down with trivial details.
Summary of the invention
In view of this, the invention solves the problems that existing Leaching Experiments system needs to consume substantial amounts of leaching liquor, uneconomical, operation
Loaded down with trivial details technical problem.There is provided a set of device being available for extracting dynamic leaching residue, i.e. in same set of leaching system, with pouring
Molten effect process completes the sampling of the dynamic leaching residue to test sample.
In order to solve above-mentioned technical problem, the invention discloses a kind of dynamic leaching residue sampler, including leaching
Post and the sample holder being placed in described leaching post；Described leaching post upper end mounting spray head, draining pipe is installed in lower end；Described pouring
Being provided with load sample platform in dissolved pillar, described load sample number of units amount is the integer more than or equal to 1, each load sample platform is placed one and contains sample
Device；Pod apertures is had on described load sample platform；It is provided with pod apertures bottom described sample holder.
Further, described sample holder bottom is covered with microporous filter membrane, and described microporous filter membrane is covered with glassfibre filters, institute
State placement sample on glassfibre filters；Glassfibre filters, described glassfibre filters upper berth are installed in described sample holder upper end
There is quantitative filter paper.
Further, the leaching post sidewall of described sample holder correspondence position offers sampling window, and sampling window side is by closing
Page is connected with leaching post, and opposite side is provided with switch handle；The surrounding that described sampling window is connected with leaching post is also equipped with sealing
Cushion rubber.
Further, described load sample platform is fixed in leaching post by dop.
Further, the described upper and lower two ends of leaching post are provided with rubber stopper.
Further, described shower nozzle is arranged on the rubber stopper of leaching post upper end, and the rubber stopper of described leaching post upper end is also
Barometric pipe is installed.
Further, the rubber stopper of described leaching post lower end is provided with draining pipe.
Further, rayon balls is filled in described barometric pipe.
Further, described shower nozzle is provided with flow control valve.
Further, described sample holder uses politef to make, tapered for upper coarse and lower fine cylinder, sample holder upper end
Diameter be slightly less than leaching column internal diameter.
Further, described microporous filter membrane is the acetate fiber microporous filter membrane in 0.45 μm aperture.
Further, described leaching post transparent organic glass is made.
Compared with prior art, the present invention can obtain and include techniques below effect:
1) assembly of the invention, from top to bottom sets gradually multiple sample holder in leaching post, invades when having certain chemistry
The leaching liquor of erosion intensity is injected by leaching capital end, first drips and is sprinkled upon the quantitative filter paper table that No.1 sample holder top horizontal is laid
Face, leaching liquor through penetrating into sample after quantitative filter paper in planar, so makes leaching liquor be fully contacted with sample surfaces, is conducive to promoting
Enter the carrying out of water_rock interaction.It is tapered that sample holder is designed to upper coarse and lower fine cylinder, it is ensured that leaching liquor is penetrated down into by top layer sample
During be fully contacted with deep sample.Leachate after water_rock interaction is micro-through being laid on the acetate fiber bottom sample holder
After the filter membrane of hole, the pod apertures bottom sample holder it is that planar is discharged.In the process, the effect of microporous filter membrane was drainage-rock
The colloidal mineral particles produced in reaction, in case taking away with leachate.The leachate discharged bottom No.1 sample holder flows into
, there is water-rock effect as leaching liquor and sample therein in No.2 sample holder, leachate flows into next Sheng sample further successively
Device, until discharging from leaching column bottom after last part sample generation water_rock interaction, flows into liquid waste collector.
2), in assembly of the invention, disposing glassfibre filters in sample holder upper end is to support quantitative filter paper, is containing
Glassfibre filters laid by sample device bottom is to prevent sample from directly contacting with microporous filter membrane and then protecting microporous filter membrane.
3), in assembly of the invention after leaching liquor and No.1 example reaction, the chemical erosion ability of leachate can reduce, so
After afterwards as leaching liquor and No.2 example reaction, the chemical erosion ability of leachate weakens further, the like.I.e. same
Individual leaching batch, water-rock action intensity is according to No.1 → No.2 →... ... the order of → No.n gradually weakens.Therefore, through certain
The Leaching Experiments in cycle, the rate of decay of test sample is with No.1 for the strongest, then with No.2 → No.3 →... ... → No.n's
Order weakens successively.
4) assembly of the invention is in same set of leaching system, completes the dynamic pouring to test sample with eluviation process
The sampling of molten residue, saves leaching liquor, it is not necessary to making parallel leaching system, device is simple, it is easy to operation, reproducible,
Technical staff is easy to learn, easily grasp.
Certainly, the arbitrary product implementing the present invention must be not necessarily required to reach all the above technique effect simultaneously.
Accompanying drawing explanation
Accompanying drawing described herein is used for providing a further understanding of the present invention, constitutes the part of the present invention, this
Bright schematic description and description is used for explaining the present invention, is not intended that inappropriate limitation of the present invention.In the accompanying drawings:
Fig. 1 is the overall structure schematic diagram of the embodiment of the present invention 1；
Fig. 2 is sample holder structural representation in the embodiment of the present invention 1；
Fig. 3 is sample holder sectional view in the embodiment of the present invention 1；
Fig. 4 is the structure for amplifying schematic diagram of sampling window in the embodiment of the present invention 1；
Fig. 5 be in the embodiment of the present invention 2 protolith to the Weathering indices CIA changing trend diagram of dynamic leaching residue；
Fig. 6 be in the embodiment of the present invention 2 protolith to the Weathering indices SiO of dynamic leaching residue2/Al2O3Variation tendency
Figure.
Detailed description of the invention
Describe embodiments of the present invention in detail below in conjunction with drawings and Examples, thereby how the present invention is applied
Technological means solves technical problem and reaches the process that realizes of technology effect and can fully understand and implement according to this.
Embodiment 1
As it is shown in figure 1, the dynamic leaching residue sampler of the present invention, including leaching post 1 be placed in leaching post
Sample holder 2.Leaching post 1 is made for transparent organic glass, it is possible to Real Time Observation water_rock interaction process and progress in an experiment.
Sample holder 2 uses politef to make, tapered in upper coarse and lower fine cylinder, and the diameter of upper end is slightly less than leaching column internal diameter, the end
Portion leaves pod apertures (being not drawn in figure).Politef has the strongest anti acid alkali performance energy, good stability, is difficult to and leaching liquor
React, not contaminated samples；The tapered design of upper coarse and lower fine cylinder, makes to be added dropwise to planar to ooze under the leaching liquor of top layer sample
During can be fully contacted with the sample of deep layer, make water_rock interaction the most abundant.
Leaching post about 1 two ends are provided with rubber stopper 3, make leaching post 1 become closed system, prevent the dust in environment from entering
Enter system and then contaminated samples.
Being provided with shower nozzle 4 and barometric pipe 5 on the rubber stopper 3 of leaching post 1 upper end, shower nozzle is for equal in leaching post 1
Even is spilt leaching liquor, and barometric pipe 5 can balance leaching post 1 inner and outer air pressure, it is ensured that Leaching Experiments is implemented smoothly.On shower nozzle 4
Being provided with flow control valve 6, scalable drips the leaching liquor uninterrupted spilt；Rayon balls 7 it is filled with in barometric pipe 5, anti-
Dust in stop ring border enters leaching post 1.
Being provided with draining pipe 8 on the rubber stopper 3 of leaching post 1 lower end, draining pipe 8 connects liquid waste collector 9, is used for receiving
Collection leachate.
Being provided with N number of load sample platform 10 (N is the integer more than or equal to 1) in leaching post 1, load sample platform 10 is for having pod apertures
The PVC board of (being not drawn in figure), is fixed in leaching post 1 by the dop 11 in leaching post 1.One is placed on each load sample platform 10
Individual sample holder 2.
As shown in Figures 2 and 3, sample holder 2 bottom is covered with the acetate fiber microporous filter membrane 17 in 0.45 μm aperture, microporous filter membrane 17
On be coated with layer of glass filter screen 16, laboratory sample is placed on glassfibre filters 16；Sample holder top horizontal covers
Two membranes, upper strata is quantitative filter paper 15, and lower floor is glassfibre filters 16.
As shown in figs. 1 and 4, leaching post 1 sidewall of sample holder 2 correspondence position offers sampling window 12, sampling window 12 side
Being connected with leaching post 1 by hinge 14, opposite side is provided with switch handle 13；The surrounding that sampling window 12 is connected with leaching post 1 is also
O-ring seal (being not drawn in figure) is installed.
The acetate fiber microporous filter membrane 17 in the 0.45 μm aperture laid bottom sample holder 2, it is possible to prevent in water-rock effect
The cosmid level colloidal solid produced is taken away with leachate.And overlying layer of glass filter screen 16 is to protect microporous filter membrane
17, to prevent sample from directly contacting, with microporous filter membrane 17, the Latent destruction that it is produced.At determining that sample holder 2 top horizontal covers
Amount filter paper 15, receives the solution instilled from top, and forms planar percolating fluid, can be sprinkled upon whole sample surfaces by cloth equably.
The glassfibre filters 16 of lower floor, has certain mechanical strength, can support the quantitative filter paper 15 of overlying.The design of sampling window 12
Sample holder 2 and sample it is removed or placed in time in can conveniently testing.
The specification of this Leaching Experiments device or size depend on the purpose that sample is studied.Generally do general and trace elements and
Mineralogical analysis (XRD), it is thus achieved that the solid sample of the leaching remnants of about 10g is sufficient to.For silicates material, erodable
Difference, is often equal-volume air slaking, so the sample that sample holder can accommodate about 15g just can meet analysis requirement.So, sample is contained
Device can be according to bore 5cm, the specifications design of base diameter 3cm, highly 5cm；The internal diameter of lucite post slightly ratio sample holder mouth
Footpath thick 1～2mm, can insert smoothly, take out sample holder.About the distance between sample holder, to facilitate use as principle.Extremely
In the length of lucite post, depend on gathering how many dynamic leaching residue sample.For solubility sample, such as carbonate
Rock, due to its acid non-soluble substance content the most extremely low (generally < 5%), when acid non-soluble substance is analyzed and researched by needs, it may be necessary to
Corrosion sample reaches n × 102G, therefore, the specification of Leaching Experiments device the most also to increase.
Embodiment 2
Choosing of 2.1 Weathering indices
Utilize chemical index of alteration (CIA) and silica alumina ratio (SiO2/Al2O3) etc. two geochemistry Weathering indices judge
The weathering groove of dynamic leaching residue.
(1)CIA
CIA is used to the rate of decay of quantitative assessment feldspar silicate component, and its expression formula is:
CIA=[Al2O3/(Al2O3+CaO*+Na2O+K2O)]×100
In formula, each oxide is molal quantity (mol)；CaO* is the CaO in silicate phase, if containing carbonic acid in sample
Salt or phosphatic Ca need deduction.In practice, as CaO (mol) >=Na2During O (mol), CaO*=Na2O；When CaO (mol) <
Na2During O (mol), CaO*=CaO.
During chemical weathering, with the base cation gradually leaching losses such as the decomposition of feldspar silicate mineral, Ca, Na, K, Al
Being enriched with in weathering residue, CIA value is in the trend increased, as the complete leaching loss of base cation, CIA=100.
(2)SiO2/Al2O3
In silicate efflorescence, Si is released and with silicate solution leaching loss from mineral, and Al is rich in residual solid phase
Collection, therefore the air slaking of silicate show the feature of desiliconization allitization.Along with the air slaking of silicate mineral, in residue
SiO2/Al2O3Ratio (for content ratio) is in the trend being gradually lowered.
2.2 experimentations and result
Acquire arenaceous shale as test sample, broken after cross 20 mesh sieves, fully mix by quartering, be prepared for 5
Increment, every sample weight 15g, wherein 1 increment is as protolith (Y), and other 4 increments (numbered No.1～No.4) are for dynamically
The extraction of leaching residue.Utilizing the experimental system of Fig. 1, using the hydrochloric acid solution of 1mol/L as leaching liquor, leaching speed is 4L/
D, the Leaching Experiments cycle is 10d.After Leaching Experiments terminates, to protolith sample (Y) and 4 leaching residue increments (No.1～
No.4) carry out x-ray fluorescence spectrometry (XRF), measure Main elements content.
The part Main elements content of protolith sample and dynamic leaching residue and relevant Weathering indices are shown in Table 1.Fig. 5 and
Fig. 6 shows by the Weathering indices variation tendency of protolith to dynamic leaching residue.It can be seen that according to Y → No.4 → No.3
The order of → No.2 → No.1, CIA value is in the trend (Fig. 5) being gradually increased, and SiO2/Al2O3Ratio is in the trend being gradually lowered
(Fig. 6), illustrate that the degree of the chemical weathering with Main elements sign is in the trend increased successively.Above the results show this
Bright device is feasible.
The part Main elements content of table 1 arenaceous shale sample and dynamic leaching residue thereof and Weathering indices
Note: in sample number into spectrum, Y represents arenaceous shale (test sample), No.1～No.4 represents dynamic leaching residue.
Assembly of the invention, from top to bottom sets gradually multiple sample holder in leaching post, when having certain chemical erosion
The leaching liquor of intensity is injected by leaching capital end, first drips and is sprinkled upon the quantitative filter paper surface that No.1 sample holder top horizontal is laid,
Leaching liquor, through penetrating into sample after quantitative filter paper in planar, so makes leaching liquor be fully contacted with sample surfaces, may advantageously facilitate
The carrying out of water_rock interaction.It is tapered that sample holder is designed to upper coarse and lower fine cylinder, it is ensured that leaching liquor was penetrated down into by top layer sample
Journey is fully contacted with deep sample.Leachate after water_rock interaction is through being laid on the acetate fiber micropore bottom sample holder
After filter membrane, the pod apertures bottom sample holder it is that planar is discharged.In the process, the effect of microporous filter membrane was that drainage-rock is anti-
The colloidal mineral particles produced in should, in case taking away with leachate.The leachate discharged bottom No.1 sample holder penetrates into No.2
, there is water-rock effect as leaching liquor and sample therein in sample holder, leachate flows into next sample holder further successively,
Until discharging from leaching column bottom after last part sample generation water_rock interaction, flow into liquid waste collector.
In device after leaching liquor and No.1 example reaction, the chemical erosion ability of leachate can reduce, then as leaching
After liquid and No.2 example reaction, the chemical erosion ability of leachate weakens further, the like.I.e. criticize at same leaching
Secondary, water-rock action intensity is according to No.1 → No.2 →... ... the order of → No.n gradually weakens.Therefore, through the pouring of some cycles
Molten experiment, the rate of decay of test sample is with No.1 for the strongest, then with No.2 → No.3 →... ... the order of → No.n is successively
Weaken.
Assembly of the invention, in same set of leaching system, completes the dynamic leaching to test sample with eluviation process
The sampling of residue, saves leaching liquor, it is not necessary to make parallel leaching system.Device is simple, it is easy to operation, reproducible, skill
Art personnel are easy to learn, easily grasp.
As employed some vocabulary in the middle of description and claim to censure special component or method, art technology
Personnel are it is to be appreciated that same composition may be called with different nouns in different regions.This specification and claims are not
In the way of the difference of title is used as distinguishing composition." comprising " as mentioned by the middle of description and claim in the whole text is
One open language, therefore " comprise but be not limited to " should be construed to." substantially " refer in receivable range of error, this area
Technical staff can solve described technical problem in the range of certain error, basically reaches described technique effect.Description is follow-up
It is described as implementing the better embodiment of the present invention, for the purpose of right described description is the rule so that the present invention to be described, not
In order to limit the scope of the present invention.Protection scope of the present invention is when being as the criterion depending on the defined person of claims.
Also, it should be noted term " includes ", " comprising " or its any other variant are intended to nonexcludability
Comprise, so that include that the commodity of a series of key element or system not only include those key elements, but also include the most clearly
Other key elements listed, or also include the key element intrinsic for this commodity or system.In the feelings not having more restriction
Under condition, statement " including ... " key element limited, it is not excluded that in the commodity including described key element or system also
There is other identical element.
Described above illustrate and describes some preferred embodiments of the present invention, but as previously mentioned, it should be understood that the present invention
Be not limited to form disclosed herein, be not to be taken as the eliminating to other embodiments, and can be used for other combinations various,
Amendment and environment, and can be in invention contemplated scope described herein, by above-mentioned teaching or the technology of association area or knowledge
It is modified.And the change that those skilled in the art are carried out and change are without departing from the spirit and scope of the present invention, the most all should be at this
In the protection domain of bright claims.
Claims (10)
1. a dynamic leaching residue sampler, it is characterised in that include leaching post and be placed in described leaching post
Sample holder；Described leaching post upper end mounting spray head, draining pipe is installed in lower end；Load sample platform is installed in described leaching post, described
Load sample number of units amount is the integer more than or equal to 1, and each load sample platform is placed a sample holder；Pod apertures is had on described load sample platform；
It is provided with pod apertures bottom described sample holder.
2. dynamic leaching residue sampler as claimed in claim 1, it is characterised in that described sample holder bottom is covered with micro-
Hole filter membrane, described microporous filter membrane is covered with glassfibre filters, and described glassfibre filters is placed sample；On described sample holder
End installs glassfibre filters, and described glassfibre filters is covered with quantitative filter paper.
3. dynamic leaching residue sampler as claimed in claim 2, it is characterised in that described sample holder correspondence position
Leaching post sidewall offers sampling window, and sampling window side is connected with leaching post by hinge, and opposite side is provided with switch handle；Institute
State the surrounding that sampling window is connected with leaching post and be also equipped with O-ring seal.
4. dynamic leaching residue sampler as claimed in claim 3, it is characterised in that described load sample platform is solid by dop
It is scheduled in leaching post.
5. dynamic leaching residue sampler as claimed in claim 4, it is characterised in that the described upper and lower two ends of leaching post are pacified
Equipped with rubber stopper.
6. dynamic leaching residue sampler as claimed in claim 5, it is characterised in that described shower nozzle is arranged on leaching post
On the rubber stopper of upper end, the rubber stopper of described leaching post upper end is also equipped with barometric pipe；The rubber of described leaching post lower end
Draining pipe is installed beyond the Great Wall.
7. dynamic leaching residue sampler as claimed in claim 6, it is characterised in that fill in described barometric pipe
Rayon balls.
8. dynamic leaching residue sampler as claimed in claim 7, it is characterised in that be provided with flow on described shower nozzle
Regulation valve.
9. dynamic leaching residue sampler as claimed in claim 8, it is characterised in that described sample holder uses polytetrafluoro
Ethylene is made, tapered for upper coarse and lower fine cylinder, and the diameter of sample holder upper end is slightly less than leaching column internal diameter.
10. dynamic leaching residue sampler as claimed in claim 9, it is characterised in that described microporous filter membrane is 0.45 μ
The acetate fiber microporous filter membrane in m aperture.
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Cited By (3)
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| CN106840759A (en) * | 2016-12-27 | 2017-06-13 | 南华大学 | A kind of soil infiltration water original position layered sampling device |
| CN109596462A (en) * | 2018-10-25 | 2019-04-09 | 中国辐射防护研究院 | A kind of three-dimensional radioactivity Leaching Experiments equipment |
| CN111487180A (en) * | 2020-03-31 | 2020-08-04 | 河海大学 | Experimental device and experimental method for simulating natural weathering of silicate rock |
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