CN110398402A - One kind being suitable for different minerals composition rock or sand sample quartz method of purification - Google Patents
One kind being suitable for different minerals composition rock or sand sample quartz method of purification Download PDFInfo
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- CN110398402A CN110398402A CN201910661695.0A CN201910661695A CN110398402A CN 110398402 A CN110398402 A CN 110398402A CN 201910661695 A CN201910661695 A CN 201910661695A CN 110398402 A CN110398402 A CN 110398402A
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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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
Abstract
The present invention provides one kind to be suitable for different minerals composition rock or sand sample quartz method of purification, it is characterized in that, the method for purification is the following steps are included: thickness measure and rock-mineral determination, crushing sample and sieving, flushing fine particle, the 1st magnetic separation separation, chloroazotic acid processing, ultrapure water cleaning, the 2nd magnetic separation separation, FLOTATION SEPARATION, HCl-H2SiF6Etching, more sodium tungstate heavy-fluid separation, ultrasonic cleaning, petrographic microscope detection, ICP-AES survey Al content.The beneficial effects of the present invention are: the present invention establishes the quartz purification for forming rock and sand sample suitable for different minerals and standardizes process；Method of the invention reduces poisonous reagent hydrofluoric acid usage amount, shortens experimental period, establish can quantification operation experiment flow, the operability and purification efficiency of experiment greatly improved.
Description
Technical field
The invention belongs to dating methods technical fields, are related to a kind of pure quartzy extracting method, and in particular to one kind is applicable in
Rock or sand sample quartz method of purification are formed in different minerals.
Background technique
For earth science research, dating technology is the basis of its research, and importance is self-evident, and development is very fast in recent years
Dating technology be original place cosmogenic nuclide10Be and26Al Exposure Ages measuring method.This dating methods need to obtain pure
For quartz as year substance is surveyed, why selecting quartz is based on following reason: first, crystal structure is fine and close, limits it
A possibility that by nucleic pollution is generated in atmosphere；Second, it is generally existing in nature, it easily acquires, has generation10Be and26Al
Target nucleus condition；Third, chemical component is simple, is easier to the calculating of nucleic generating rate；4th, Al content very low (one
As less than 200 μ g/g), be able to satisfy AMS pairs26When Al carries out precise measurement26Al/27Al ratio is not less than 10-14Requirement.
However, it is ensured that the method surveys the accuracy in year it is necessary to guarantee that used quartz has very high purity, because
The purity of quartz will affect the separating effect of Be and Al；27The pollution of Al will lead to26Al/27(potassium feldspar is about for the increase of Al statistical error
1000 μ g/g, plagioclase about 1100-1900 μ g/g)；Generating rate is to calculate calibration according to the value of the pure quartz in high latitude sea level.
Therefore the quartz specimen for obtaining high-purity, is one of key link of the dating methods, and the method requires the quartzy Al after purification
Content is that 200 μ g/g of year < is surveyed in exposure, buries and surveys 100 μ g/g of year <.
But the pure quartzy extracting method of the prior art is difficult to obtain the quartz of high-purity, if to be prepared high-purity
The sample of degree can only be using high cost and high pollution as give-and-take conditions, more especially for the extremely low sample extraction difficulty of quartz content
Greatly, but the situation of reality is to survey the sample that quartz content is low in year sample increasing, and is more effectively extracted so needing to develop
With the method for purifying quartz, the method for its andesine is especially separated.
The pure quartzy extracting method of the prior art is mainly the classical way for using Kohl and Nishiizumi
(1992), pure quartz is extracted and is primarily present following technical problem:
1., due to its mineral composition difference, processing method is also required to be adjusted, not have for different primary samples
A kind of blanket method；
2. the sample extremely low for quartz content, extracting has certain technical difficulty；
3. for non-quartz mineral content very high sample, quartz purification is needed through acid etch repeatedly, but is molten
A large amount of chemical reagent can be consumed by taking off non-quartz mineral, this will increase economy and Ecological Cost, and when sample is cleaned multiple times
Loss will also result in the reduction of quartz mineral, cause experimental error.
Summary of the invention
In order to make up for the deficiencies of the prior art, the present invention provides one kind to be suitable for different minerals composition rock or sand sample stone
English method of purification solves a series of problems present in pure quartzy extraction process.
One kind being suitable for different minerals composition rock or sand sample quartz method of purification, comprising the following steps:
(1) thickness measure and rock-mineral determination: measurement thickness of sample, and take pictures, the rock-mineral determination of aforementioned sample is carried out later,
Estimate the particle size of content and quartz quartzy in aforementioned sample；
(2) sample and sieving are crushed: if aforementioned sample is granite sample, being crushed using pulverizer and powder
It is broken, it is sieved later, obtains the component that partial size is 0.25-0.50mm；If aforementioned sample is various sedimentary formation samples, directly
Use HCl/HNO3Immersion treatment is sieved after cleaning, drying, and the component that partial size is 0.25-0.50mm is obtained；
(3) it rinses fine particle: the deionized water of beakers volume 1/6 being added in beaker, is later put into sample
In beakers, continues to add at deionized water to the 2/3 of beakers volume, be stirred with glass bar, then by aforementioned deionization
Water is poured out, and realizes the purpose for washing away tiny particles content, and repetition is washed repeatedly, until cleaning tiny particles content, obtains degranulation sample；
(4) the 1st magnetic separation separation: if can be gone by strong magnets in aforementioned degranulation sample containing a small amount of strongly magnetic mineral
It removes, magnetic separation instrument is used to separate if containing a large amount of magnetic minerals in aforementioned degranulation sample；Specific operation process is, according to aforementioned
Degranulation sample particle diameter difference selects different magnetic separation instrument revolving speeds；Magnetic separation separation is carried out using magnetic separation instrument, after obtaining magnetic separation separation
Sample after aforementioned magnetic separation separation is packed into sample sack by sample, and indicate on aforementioned sample bag sample ID, particle size and
magnetic；The dust catcher of Wet-dry is used to clean magnetic separation instrument after completing magnetic separation separation；
(5) chloroazotic acid is handled: by dense HCl and HNO3The ratio of 1:1 is configured to chloroazotic acid for removing aforementioned magnetic separation by volume
The oxide of carbonate and iron after separation in sample；Detailed process is that sample after aforementioned magnetic separation separation is put into suitable beaker
In, enough deionized waters are added and cover sample after aforementioned magnetic separation separation, and make sample surfaces after aforementioned magnetic separation separation parallel,
Record total volume V；It is repeatedly slowly added to HCl-HNO on a small quantity3, it is equal with aforementioned total volume V that volume is added；It stirs and covers later
Evaporating dish is placed in draught cupboard and stands 24 hours, until sample sufficiently reacts after aforementioned magnetic separation separation, obtains sample after chloroazotic acid processing
Product；
(6) ultrapure water cleans: pouring out residual acid, deionized water is cleaned after aforementioned chloroazotic acid processing sample 5-6 times, then by beaker
It is moved to the sink switched equipped with deionized water from draught cupboard, is repeatedly washed to neutrality, sample after being cleaned finally will be aforementioned clear
It washes rear sample to be transferred in another beaker, and beakers is placed in 80 DEG C of drying in baking oven, obtain drying sample；
(7) the 2nd magnetic separation separation: record magnetic separation instrument parameter and electric current select magnetic separation according to the partial size of aforementioned drying sample
The revolving speed of instrument carries out magnetic separation separation using aforementioned magnetic separation instrument, obtains sample after 2 magnetic separation separation, is loaded into sample sack, and
Sample ID, particle size and magnetic are indicated on aforementioned sample bag；Complete the dust suction that Wet-dry is used after magnetic separation separates
Device cleans magnetic separation instrument；
(8) FLOTATION SEPARATION: sample after aforementioned 2 magnetic separation separation biggish for feldspar and mica content, using floatation；
Specific operation process is that sample first impregnates 1 hour through 1%HF solution after aforementioned 2 magnetic separation separation, hates feldspar and mica surface
Water, and quartz surfaces are hydrophilic；Then aforementioned HF solution is outwelled, a few drop terpinols are added and mix, the CO containing saturation is added21ml/L
Glacial acetic acid solution and 1g/L lauryl amine mixed solution 1L, be sufficiently stirred and be passed through CO2, will generate largely rich in feldspar and
The foam of mica particles skims foregoing foams after several seconds, quartz will be retained in solution bottom, obtains sample after FLOTATION SEPARATION；
(9)HCl-H2SiF6Etching: weighing sample 50-100g after aforementioned FLOTATION SEPARATION, put into 250mL centrifugal bottle, and adds
Enter the HCl-H of 200mL2SiF6Acid solution, water-bath are vibrated 2 days, ultrapure water cleaning, 80 DEG C of drying；It covers and tightens later, upper roller machine
Overnight, drum temperature is controlled at 60-80 DEG C for rotation；Next day outwells solution, and new HCl-H is added2SiF6Acid solution, then upper roller machine rotation
Turn over night；Repeatedly handle 2 times, cleaning, drying observation processing after sample character, with decide whether repeat this step or into
Enter in next step；
(10) more sodium tungstate heavy-fluids more sodium tungstate heavy-fluid separation: are formulated as density 3.0g/cm3Solution for standby；It uses
The heavy caliber for the configuration polytetrafluoroethylene (PTFE) material that capacity is 500mL is switched separatory funnel and fixed by iron stand, underlying Buchner funnel,
It is separated using ordinary filter paper, and connects Suction filtration device；Before the more sodium tungstate heavy-fluids of 250mL and 60g are added in aforementioned separatory funnel
Sample after acid etching is stated, filler cap is added to screw, is vibrated to mix well, loose filler cap is stood, and density is greater than 3.0g/cm3Weight
Mineral precipitation to funnel bottom, opening funnel switch is released, the partial size phase of the separation process and sample after aforementioned acid etching
It closes, partial size is smaller, and the required sedimentation time is longer；Few drops of deionized waters are added along aforementioned separatory funnel lid with wash bottle later, cover
Oscillation shakes up, and pine lid is stood, and observes sample separate condition；This process repeatedly records each deionized water and obtains dosage, it is generally recognized that
50 drip, about 2.5mL, can reduce solution density 0.1g/cm3, this experiment quartz specimen density to be prepared section is
2.67-2.63g/cm3, concrete operations are depending on the separation situation for adding deionized water and sample after aforementioned acid etching；It will finally obtain
The quartz specimen obtained sufficiently elutes, and is dried for standby；
(11) ultrasonic cleaning: aforementioned quartz specimen is put into 1L polyethylene jar, and 150mL1%HF/HNO is added3
After acid solution plus deionized water is to 750mL, and capping is tightened, and is put into ultrasonic cleaner, and processing is overnight；Next day changes acid, repeat at
Reason 1 time, observes aforementioned quartz specimen disposition, if aforementioned quartz specimen character is uniform, powder particle is less, then a large amount of pure
Otherwise water cleaning, drying repeat ultrasonic cleaning step in case dissolution, final to obtain purification quartz；
(12) petrographic microscope detects: the purity of purification quartz is examined using petrographic microscope, determines refining effect, if
Still there are other a small amount of mineral residues, then rejected by hand, the purity of purification quartz is made to reach 100% as far as possible；
(13) ICP-AES surveys Al content: weighing 0.25g foregoing purification quartz to 25mL polytetrafluoroethylene (PTFE) crucible, 5mL is added
HF and 1mL HNO3, cover, be placed in 120 DEG C of electric hot plate and heat 2 hours, until foregoing purification quartz is completely dissolved；Lid is removed,
150 DEG C are evaporated；Addend drips HClO4It is evaporated, 1mLHCl is added and is dissolved, moves to 15mL centrifuge tube, is cleaned using ultrapure water 1mL
Aforementioned crucible, and being transferred in same centrifuge tube, then plus ultrapure water carry out ICP-AES measurement to 10mL；Aforementioned ICP-AES measurement
As a result middle Al content < 100 μ g/g, then quartz purifying has reached requirement, conversely, then return step (9) re-starts HCl-H2SiF6Erosion
Quarter and subsequent step, until Al content reaches requirement.
As a preferred solution, pulverizer described in step (2) is jaw crusher and disk crusher.
It is further preferred that various sedimentary formation samples described in step (2) include speleothems, fluvial outwash stratum
Sample.
It is further preferred that being needed if the sample is the high sample of clay content when step (3) rinses fine particle
It first to be impregnated 1-2 days with deionized water, and with ultrasonic cleaning several hours, be rinsed the step of fine particle again later
Suddenly.
It is further preferred that can increase by one between step (12) and (13) measures sample stone with X-ray diffractometer
The step of English content, specially detects mineral content using X-ray diffractometer, and calculates the purity of foregoing purification quartz.
The beneficial effects of the present invention are: it is provided by the invention a kind of quartzy suitable for different minerals composition rock or sand sample
Method of purification has the advantage that
(1) present invention establishes the quartz purification standardization process that rock and sand sample are formed suitable for different minerals；
(2) method of purification of the prior art need to repeatedly carry out hydrofluoric acid-nitric acid etch, and method of the invention reduces severe toxicity
Reagent hydrofluoric acid usage amount shortens experimental period, establish can quantification operation experiment flow, experiment greatly improved
Operability and purification efficiency.
Detailed description of the invention
Fig. 1 is a kind of stream that rock or sand sample quartz method of purification are formed suitable for different minerals of the embodiment of the present invention 1
Journey schematic diagram.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, to the technology in the embodiment of the present invention
Scheme is clearly and completely described, it is clear that and described embodiments are some of the embodiments of the present invention, rather than whole
Embodiment.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without creative efforts
The every other embodiment obtained, shall fall within the protection scope of the present invention.
Embodiment 1
One kind being suitable for different minerals composition rock or sand sample quartz method of purification, includes the following steps (referring to Fig. 1):
(1) thickness measure and rock-mineral determination: measurement thickness of sample, and take pictures, the rock-mineral determination of sample, estimation are carried out later
The particle size of quartzy content and quartz in sample；
(2) sample and sieving are crushed: if sample is granite sample, being crushed and is crushed using pulverizer, it
After be sieved, obtain partial size be 0.25-0.50mm component；If sample is various sedimentary formation samples such as speleothems, river
Alluvial formation sample etc. is flowed, then be used directly HCl/HNO3Immersion treatment is sieved after cleaning, drying, and acquisition partial size is 0.25-
The component of 0.50mm；Pulverizer is jaw crusher and disk crusher；
(3) it rinses fine particle: the deionized water of beaker volume 1/6 being added in beaker, sample is put into beaker later
In, continue to add at deionized water to the 2/3 of beaker volume, stirred with glass bar, then pour out deionized water, realization washes away thin
The purpose of small particle, repetition are washed repeatedly, until cleaning tiny particles content, obtain degranulation sample；Sample is that clay content is high
Sample then need first to be impregnated 1-2 days with deionized water, and with ultrasonic cleaning several hours, be rinsed tiny again later
The step of grain；
(4) the 1st magnetic separation separation: if can be removed by strong magnets in degranulation sample containing a small amount of strongly magnetic mineral,
Magnetic separation instrument is used to separate if containing a large amount of magnetic minerals in degranulation sample；Specific operation process is, according to degranulation sample
Partial size difference selects different magnetic separation instrument revolving speeds；Magnetic separation separation is carried out using magnetic separation instrument, sample after magnetic separation separation is obtained, by magnetic separation
Sample is packed into sample sack after separation, and sample ID, particle size and magnetic are indicated on sample sack；Complete magnetic separation separation
Magnetic separation instrument is cleaned using the dust catcher of Wet-dry afterwards；
(5) chloroazotic acid is handled: by dense HCl and HNO3The ratio of 1:1 is configured to chloroazotic acid for removing magnetic separation separation by volume
The oxide of carbonate in sample and iron afterwards；Detailed process is that sample is put into suitable beaker after separating magnetic separation, is added
Sample after enough deionized water covering magnetic separation separation, and make sample surfaces after magnetic separation separation parallel, record total volume V；It is few
Amount is repeatedly slowly added to HCl-HNO3, it is equal with total volume V that volume is added；Evaporating dish is stirred and covered later, is placed in draught cupboard
It is interior to stand 24 hours, until sample sufficiently reacts after magnetic separation separation, obtain sample after chloroazotic acid processing；
(6) ultrapure water cleans: pouring out residual acid, deionized water cleans after chloroazotic acid processing sample 5-6 time, then by beaker from leading to
Wind cupboard is moved to the sink equipped with deionized water switch, is repeatedly washed to neutrality, sample after being cleaned, sample after finally cleaning
It is transferred in another beaker, and places the beaker 80 DEG C of drying in baking oven, obtain drying sample；
(7) the 2nd magnetic separation separation: record magnetic separation instrument parameter and electric current select magnetic separation instrument according to the partial size of drying sample
Revolving speed carries out magnetic separation separation using magnetic separation instrument, obtains sample after 2 magnetic separation separation, is loaded into sample sack, and on sample sack
Indicate sample ID, particle size and magnetic；The dust catcher of Wet-dry is used to clean magnetic separation instrument after completing magnetic separation separation；
(8) FLOTATION SEPARATION: sample after 2 magnetic separation separation biggish for feldspar and mica content, using floatation；Specifically
Operating process is, sample first impregnates 1 hour through 1%HF solution after 2 magnetic separation separation, makes feldspar and mica surface hydrophobic, and stone
English surface hydrophilic；Then HF solution is outwelled, a few drop terpinols are added and mix, the CO containing saturation is added21ml/L glacial acetic acid solution
With the mixed solution 1L of the lauryl amine of 1g/L, it is sufficiently stirred and is passed through CO2, the largely bubble rich in feldspar and mica particles will be generated
Foam skims foam after several seconds, quartz will be retained in solution bottom, obtains sample after FLOTATION SEPARATION；
(9)HCl-H2SiF6Etching: sample 50-100g after FLOTATION SEPARATION is weighed, is put into 250mL centrifugal bottle, and be added
The HCl-H of 200mL2SiF6Acid solution, water-bath are vibrated 2 days, ultrapure water cleaning, 80 DEG C of drying；It covers and tightens later, upper roller machine rotation
Night is turned over, drum temperature is controlled at 60-80 DEG C；Next day outwells solution, and new HCl-H is added2SiF6Acid solution, then upper roller machine rotation
Overnight；It handles 2 times repeatedly, the character of sample after cleaning, drying observation processing, to decide whether to repeat this step or entrance
In next step；
(10) more sodium tungstate heavy-fluids more sodium tungstate heavy-fluid separation: are formulated as density 3.0g/cm3Solution for standby；It uses
The heavy caliber for the configuration polytetrafluoroethylene (PTFE) material that capacity is 500mL is switched separatory funnel and fixed by iron stand, underlying Buchner funnel,
It is separated using ordinary filter paper, and connects Suction filtration device；The more sodium tungstate heavy-fluids of 250mL and 60g acid etching are added in separatory funnel
Sample afterwards adds filler cap to screw, and vibrates to mix well, and loose filler cap is stood, and density is greater than 3.0g/cm3Heavy mineral sedimentation
To funnel bottom, to open funnel switch and released, the separation process is related to the partial size of sample after acid etching, and partial size is smaller,
The required sedimentation time is longer；Few drops of deionized waters are added along separatory funnel lid with wash bottle later, covers oscillation and shakes up, loose Gai Jing
It sets, observes sample separate condition；This process repeatedly records each deionized water and obtains dosage, it is generally recognized that and 50 drip, about 2.5mL,
Solution density 0.1g/cm can be reduced3, this experiment quartz specimen density to be prepared section is 2.67-2.63g/cm3, specifically
It operates depending on the separation situation for adding deionized water and sample after acid etching；Finally the quartz specimen of acquisition is sufficiently eluted, is dried
It does spare；
(11) ultrasonic cleaning: quartz specimen is put into 1L polyethylene jar, and 150mL1%HF/HNO is added3Acid solution
Afterwards plus deionized water is to 750mL, and capping is tightened, and is put into ultrasonic cleaner, and processing is overnight；Next day changes acid, reprocessing 1
It is secondary, quartz specimen disposition is observed, if quartz specimen character is uniform, powder particle is less, then a large amount of pure water cleanings, drying
In case dissolution, otherwise repeats ultrasonic cleaning step, it is final to obtain purification quartz；
(12) petrographic microscope detects: the purity of purification quartz is examined using petrographic microscope, determines refining effect, if
Still there are other a small amount of mineral residues, then rejected by hand, the purity of purification quartz is made to reach 100% as far as possible；
(13) X-ray diffractometer measures sample quartz content: detecting the quartzy Minerals of purification using X-ray diffractometer and contains
Amount, and calculate the purity of purification quartz；
(14) ICP-AES surveys Al content: weighing 0.25g purification quartz to 25mL polytetrafluoroethylene (PTFE) crucible, 5mL HF is added
With 1mL HNO3, cover, be placed in 120 DEG C of electric hot plate and heat 2 hours, until purification quartz is completely dissolved；Remove lid, 150 DEG C of steamings
It is dry；Addend drips HClO4It is evaporated, 1mL HCl is added and is dissolved, 15mL centrifuge tube is moved to, using ultrapure water 1mL cleaning crucible,
And be transferred in same centrifuge tube, then plus ultrapure water to 10mL carry out ICP-AES measurement；Al content in ICP-AES measurement result <
100 μ g/g, then quartz purifying has reached requirement, conversely, then return step (9) re-starts HCl-H2SiF6Etching and subsequent step,
Until Al content reaches requirement.
Comparative example 1
A kind of quartz method of purification, comprising the following steps:
(1) crush sample and sieving: coarse granule granite sample can be crushed and be sieved with pulverizer, obtain appropriate particle size
Component (0.25-0.50mm)；Various sedimentary formation samples such as speleothems, fluvial outwash formation sample etc., can directly use
HCl/HNO3Immersion treatment, cleaning, drying sieving, the component (0.25-0.50mm) for choosing appropriate particle size carry out at next step afterwards
Reason.
(2) 1:1HCl removes the oxide of carbonate and iron: sample being put into suitable beaker, enough water is added and covers
Lid sample, so that sample surfaces are parallel；The total volume V of water and sample is added in record；It is slowly added to equivalent HCl (acutely such as reaction,
It is then a small amount of to be repeatedly added), evaporating dish is stirred and covered, is heated 24 hours in 80 DEG C of heating plate, so that sample sufficiently reacts.
(3) residual acid is poured out, using deionized water by sample clean to faintly acid, is dried in baking oven in 80 DEG C.
(4) magnetic separation: record magnetic separation instrument parameter and electric current；A small amount of magnetic mineral can be removed by strong magnets, largely then use magnetic
It selects instrument to separate, pays attention to sample particle diameter with the collocation of magnetic separation instrument revolving speed；Magnetism granule is packed into sample sack, and is indicated on sack
Sample ID, particle size and magnetic；(especially paid attention to feed hopper with the dust catcher cleaning magnetic separation instrument of Wet-dry, connect sample
Hairbrush below pallet and wheel).
(5) acid etching: 100-150g sample is packed into 1L polyethylene wide-mouth bottle, and the 5%HF/HNO of about 750ml is added3Mixing
Acid solution, capping are tightened, and overnight, drum temperature is controlled at 60-80 DEG C for upper roller machine rotation.Next day outwells solution, and new acid solution is added,
Upper roller again.It handles 3-5 times repeatedly, cleaning, drying observes sample property, under deciding whether to repeat this step or enter
One step.
(6) more sodium tungstate heavy-fluid separation: this experiment uses more sodium tungstate heavy-fluids, is formulated as density 3.0g/cm3It is molten
Liquid is spare；Separatory funnel is switched using the heavy caliber for the configuration polytetrafluoroethylene (PTFE) material that capacity is 500ml, to avoid sample solid
Particle blocking and friction；Separatory funnel is fixed using iron stand, underlying cloth funnel, heavy-fluid and stream are separated using ordinary filter paper
Mineral out.250ml heavy-fluid and the sample of about 60g is added, filler cap is added to screw, vibrates to mix well, loose filler cap is stood,
Density is greater than 3.0g/cm3Heavy mineral be settled down to funnel bottom, open funnel switch discharge section heavy-fluid and be removed；Then
Few drops of pure water are added along separatory funnel lid with wash bottle, covers oscillation and shakes up, pine lid is stood, and observes sample separate condition.And this reality
Testing required quartz specimen density section is 2.67-2.63g/cm3.Concrete operations are depending on adding water and sample separation situation.It will obtain
The quartz obtained sufficiently elution, is dried for standby.
(7) 1%HF/HNO3Etching: sample is packed into 1L polyethylene wide-mouth bottle, and the 1%HF/HNO of about 750ml is added3Mixed acid
Liquid, capping are tightened, and overnight, drum temperature is controlled at 60-80 DEG C for upper roller machine rotation.Next day outwells solution, washing；Repeat 1-2
It is secondary.
(8) quartzy purity is examined under microscope: being checked under petrographic microscope, is determined refining effect.
(9) ICP-AES surveys Al content: weighing quartz, adds 5ml HF, cover and heat in electric hot plate, until sample dissolves；It removes
Lid, 150 DEG C are evaporated；Few drops of HClO4It is evaporated (except F-)；Pipettor adds HCl, moves to 15ml centrifuge tube.100 μ g/ of Al content >
G repeats to etch；100 μ g/g of Al content <, quartz purifying have reached requirement.
It should be appreciated that described above, the specific embodiments are only for explaining the present invention, is not intended to limit the present invention.By
The obvious changes or variations that spirit of the invention is extended out are still in the protection scope of this invention.
Claims (5)
1. one kind is suitable for different minerals composition rock or sand sample quartz method of purification, which is characterized in that the method for purification packet
Include following steps:
(1) thickness measure and rock-mineral determination: measurement thickness of sample, and take pictures, the rock-mineral determination of the sample is carried out later, is estimated
The particle size of quartzy content and quartz in the sample；
(2) sample and sieving are crushed: if the sample is granite sample, being crushed and is crushed using pulverizer, it
After be sieved, obtain partial size be 0.25-0.50mm component；If the sample is various sedimentary formation samples, it then be used directly
HCl/HNO3Immersion treatment is sieved after cleaning, drying, and the component that partial size is 0.25-0.50mm is obtained；
(3) it rinses fine particle: the deionized water of the beaker volume 1/6 being added in beaker, be later put into sample described
In beaker, continues to add at deionized water to the 2/3 of the beaker volume, stirred with glass bar, then fall the deionized water
Out, the purpose for washing away tiny particles content is realized, repetition is washed repeatedly, until cleaning tiny particles content, obtains degranulation sample；
(4) the 1st magnetic separation separation: if can be removed by strong magnets in the degranulation sample containing a small amount of strongly magnetic mineral,
Magnetic separation instrument is used to separate if containing a large amount of magnetic minerals in the degranulation sample；Specific operation process is to be gone according to described
Particulate samples partial size difference selects different magnetic separation instrument revolving speeds；Magnetic separation separation is carried out using magnetic separation instrument, obtains sample after magnetic separation separation
Sample after magnetic separation separation is packed into sample sack by product, and indicate on the sample sack sample ID, particle size and
magnetic；The dust catcher of Wet-dry is used to clean magnetic separation instrument after completing magnetic separation separation；
(5) chloroazotic acid is handled: by dense HCl and HNO3After the ratio of 1:1 is configured to chloroazotic acid for removing the magnetic separation separation by volume
The oxide of carbonate and iron in sample；Detailed process is that sample after magnetic separation separation is put into suitable beaker, is added
Enter enough deionized waters and cover sample after the magnetic separation separation, and makes sample surfaces after the magnetic separation separation parallel, record
Total volume V；It is repeatedly slowly added to HCl-HNO on a small quantity3, it is equal with the total volume V that volume is added；It stirs later and covers evaporation
Ware is placed in draught cupboard and stands 24 hours, until sample sufficiently reacts after magnetic separation separation, obtains sample after chloroazotic acid processing；
(6) ultrapure water cleans: pouring out residual acid, deionized water cleans after the chloroazotic acid processing sample 5-6 time, then by beaker from leading to
Wind cupboard is moved to the sink equipped with deionized water switch, is repeatedly washed to neutrality, sample after being cleaned finally will be after the cleaning
Sample is transferred in another beaker, and the beaker is placed in 80 DEG C of drying in baking oven, obtains drying sample；
(7) the 2nd magnetic separation separation: record magnetic separation instrument parameter and electric current select magnetic separation instrument according to the partial size of the drying sample
Revolving speed carries out magnetic separation separation using the magnetic separation instrument, obtains sample after 2 magnetic separation separation, is loaded into sample sack, and described
Sample ID, particle size and magnetic are indicated on sample sack；Use the dust catcher of Wet-dry clear after completing magnetic separation separation
Clean magnetic separation instrument；
(8) FLOTATION SEPARATION: sample after 2 magnetic separation separation biggish for feldspar and mica content, using floatation；Specifically
Operating process is that sample first impregnates 1 hour through 1%HF solution after 2 magnetic separation separation, makes feldspar and mica surface hydrophobic,
And quartz surfaces are hydrophilic；Then the HF solution is outwelled, a few drop terpinols are added and mix, the CO containing saturation is added21ml/L ice
The mixed solution 1L of the lauryl amine of acetum and 1g/L, is sufficiently stirred and is passed through CO2, feldspar and mica are largely rich in by generating
The foam of particle skims the foam after several seconds, quartz will be retained in solution bottom, obtains sample after FLOTATION SEPARATION；
(9)HCl-H2SiF6Etching: sample 50-100g after the FLOTATION SEPARATION is weighed, is put into 250mL centrifugal bottle, and be added
The HCl-H of 200mL2SiF6Acid solution, water-bath are vibrated 2 days, ultrapure water cleaning, 80 DEG C of drying；It covers and tightens later, upper roller machine rotation
Night is turned over, drum temperature is controlled at 60-80 DEG C；Next day outwells solution, and new HCl-H is added2SiF6Acid solution, then upper roller machine rotation
Overnight；It handles 2 times repeatedly, the character of sample after cleaning, drying observation processing, to decide whether to repeat this step or entrance
In next step；
(10) more sodium tungstate heavy-fluids more sodium tungstate heavy-fluid separation: are formulated as density 3.0g/cm3Solution for standby；Use iron stand
The heavy caliber for the configuration polytetrafluoroethylene (PTFE) material that capacity is 500mL is switched separatory funnel to fix, underlying Buchner funnel, use is general
Logical filter paper separation, and connect Suction filtration device；Acid etching described in the more sodium tungstate heavy-fluids of 250mL and 60g is added in the separatory funnel
Sample after quarter, adds filler cap to screw, and vibrates to mix well, and loose filler cap is stood, and density is greater than 3.0g/cm3Heavy mineral it is heavy
It is down to funnel bottom, funnel switch is opened and is released, the separation process is related to the partial size of sample after the acid etching, partial size
Smaller, the required sedimentation time is longer；Few drops of deionized waters are added along the separatory funnel lid with wash bottle later, covers oscillation and shakes
Even, pine lid is stood, and observes sample separate condition；This process repeatedly records each deionized water and obtains dosage, it is generally recognized that 50 drops
Water, about 2.5mL can reduce solution density 0.1g/cm3, this experiment quartz specimen density to be prepared section is 2.67-
2.63g/cm3, concrete operations are depending on the separation situation for adding deionized water and sample after the acid etching；Finally by the stone of acquisition
English sample sufficiently elutes, and is dried for standby；
(11) ultrasonic cleaning: the quartz specimen is put into 1L polyethylene jar, and 150mL1%HF/HNO is added3Acid solution
Afterwards plus deionized water is to 750mL, and capping is tightened, and is put into ultrasonic cleaner, and processing is overnight；Next day changes acid, reprocessing 1
It is secondary, the quartz specimen disposition is observed, if the quartz specimen character is uniform, powder particle is less, then a large amount of pure water
Otherwise cleaning, drying repeat ultrasonic cleaning step in case dissolution, final to obtain purification quartz；
(12) petrographic microscope detects: examining the purity of purification quartz using petrographic microscope, refining effect is determined, if still had
Other a small amount of mineral residues are then rejected by hand, and the purity of purification quartz is made to reach 100% as far as possible；
(13) ICP-AES surveys Al content: weighing purification quartz described in 0.25g and 5mL HF is added to 25mL polytetrafluoroethylene (PTFE) crucible
With 1mL HNO3, cover, be placed in 120 DEG C of electric hot plate and heat 2 hours, until the purification quartz is completely dissolved；Remove lid, 150
It DEG C is evaporated；Addend drips HClO4It is evaporated, 1mL HCl is added and is dissolved, 15mL centrifuge tube is moved to, clean institute using ultrapure water 1mL
State crucible, and be transferred in same centrifuge tube, then plus ultrapure water to 10mL carry out ICP-AES measurement；The ICP-AES measurement knot
Al content < 100 μ g/g in fruit, then quartz purifying has reached requirement, conversely, then return step (9) re-starts HCl-H2SiF6Etching
And subsequent step, until Al content reaches requirement.
2. a kind of different minerals that are suitable for according to claim 1 form rock or sand sample quartz method of purification work, special
Sign is that pulverizer described in step (2) is jaw crusher and disk crusher.
3. a kind of different minerals that are suitable for according to claim 1 form rock or sand sample quartz method of purification work, special
Sign is that various sedimentary formation samples described in step (2) include speleothems, fluvial outwash formation sample.
4. a kind of different minerals that are suitable for according to claim 1 form rock or sand sample quartz method of purification work, special
Sign is, when step (3) rinses fine particle, needs first to use deionized water if the sample is the high sample of clay content
The step of impregnating 1-2 days, and with ultrasonic cleaning several hours, being rinsed fine particle again later.
5. a kind of different minerals that are suitable for according to claim 1 form rock or sand sample quartz method of purification work, special
The step of sign is, can increase by one between step (12) and (13) with X-ray diffractometer measurement sample quartz content, tool
Body is the purity for detecting mineral content using X-ray diffractometer, and calculating the purification quartz.
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| CN111203328A (en) * | 2020-01-10 | 2020-05-29 | 中国科学院合肥物质科学研究院 | Method for purifying quartz sand |
| CN113182066A (en) * | 2021-05-18 | 2021-07-30 | 党泽发 | Gravity separation method |
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