CN112284990A - Method for separating and measuring content of clay particles - Google Patents
Method for separating and measuring content of clay particles Download PDFInfo
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- CN112284990A CN112284990A CN202011119278.2A CN202011119278A CN112284990A CN 112284990 A CN112284990 A CN 112284990A CN 202011119278 A CN202011119278 A CN 202011119278A CN 112284990 A CN112284990 A CN 112284990A
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- 239000002245 particle Substances 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 49
- 239000004927 clay Substances 0.000 title claims abstract description 30
- 239000002734 clay mineral Substances 0.000 claims abstract description 38
- 239000000843 powder Substances 0.000 claims abstract description 37
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 21
- 239000011707 mineral Substances 0.000 claims abstract description 21
- 239000004576 sand Substances 0.000 claims abstract description 17
- 238000004062 sedimentation Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000004445 quantitative analysis Methods 0.000 claims abstract description 8
- 238000005259 measurement Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000000926 separation method Methods 0.000 claims description 7
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 7
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 7
- 239000004575 stone Substances 0.000 claims description 7
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 7
- 238000002441 X-ray diffraction Methods 0.000 claims description 6
- 238000005070 sampling Methods 0.000 claims description 6
- 238000001228 spectrum Methods 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000010813 internal standard method Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 abstract description 10
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 229960000907 methylthioninium chloride Drugs 0.000 description 4
- 238000010998 test method Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000003556 assay Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 235000019738 Limestone Nutrition 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000006028 limestone Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/04—Investigating sedimentation of particle suspensions
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/10—Investigating individual particles
-
- 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 invention provides a method for separating and measuring content of clay particles, which relates to the technical field of particle number measurement, and comprises the following steps: determining the content X1 of a main mineral phase and the content X2 of a secondary mineral phase in the machine-made sandstone powder; dissolving machine-made sand powder in the solution to form turbid liquid so as to dissolve clay minerals; separating the solution containing clay minerals by a natural sedimentation method; drying the separated solution; repeating the separating step for multiple times, and collecting the particles separated for multiple times; and (4) quantitatively analyzing the content x2 of the clay minerals to obtain the clay mineral content in the machine-made sandstone powder. The natural sedimentation method can be used for extracting particles smaller than 5 mu m, and the accuracy can reach 80-90% by combining with the quantitative analysis method to process the content determination of the clay mineral, so that the content of the clay particles in the machine-made sand is more accurately separated and determined, and misjudgment is not easy to cause.
Description
Technical Field
The invention relates to the technical field of particle number measurement, in particular to a method for separating and measuring content of clay particles.
Background
In the prior art, in order to separate and measure the clay particle content of the machine-made sandstone powder, a sand equivalent test method or a methylene blue value test method is generally adopted. The sand equivalent test method is used for measuring the content of cohesive soil or impurities contained in various fine aggregates such as natural sand, artificial sand, stone chips and the like so as to evaluate the cleanliness of the aggregates. The methylene blue value test method is a method for determining whether expansive clay minerals exist in fine aggregates, fine powders and mineral powders and determining an overall index of the contents thereof.
However, neither the sand equivalent test detection method nor the methylene blue value test detection method can effectively separate and measure the mud content in the machine-made sand powder, and the qualified aggregate is easily detected as unqualified according to the detection indexes required by the current specifications, thereby causing misjudgment.
Disclosure of Invention
The invention aims to provide a method for separating and measuring content of clay particles, which aims to solve the technical problems that in the prior art, a methylene blue value test detection method cannot effectively separate and measure the mud content in machine-made sandstone powder, and qualified aggregate is easily detected as unqualified, so that misjudgment is caused.
The invention provides a method for separating and measuring the content of clay particles, which comprises the following steps:
1) determining the content X1 of a main mineral phase and the content X2 of a secondary mineral phase in the machine-made sandstone powder; wherein, X1+ X2 is 100%; the secondary mineral contains clay mineral;
2) dissolving machine-made sand powder in a solution to form turbid solution, and adding sodium hexametaphosphate into the turbid solution to dissolve clay minerals;
3) separating the solution containing clay minerals by a natural sedimentation method;
4) drying the separated solution;
5) repeating the step 3-4 for a plurality of times, and collecting the particles separated for a plurality of times;
6) sampling the separated particles, and quantitatively analyzing the content X2 of the clay mineral to obtain the content (X2X 2/100)% of the clay mineral in the machine-made sandstone powder.
Further, before the step 1), the following steps are included: the machine-made sandstone powder in the stone chips is prepared by a water washing method.
Further, in the step 1), after the machine-made sandstone powder is dried to constant weight at 60 ℃, sampling and quantitative analysis are carried out on the machine-made sandstone powder, and full spectrum fitting is carried out according to an XRD (X-ray diffraction) spectrum, so as to obtain the main mineral phase content X1 and the minor mineral phase content X2.
Further, in the step 1), the machine-made sandstone powder is sampled by a quartering method.
Further, in the step 1), analysis and quantitative analysis are carried out by using a type X-ray diffractometer, and the scanning speed is 2 degrees/min.
Further, in the step 2), the machine-made sand powder is dissolved in deionized water to form turbid liquid, 4% of sodium hexametaphosphate is added, and the mixture is shaken and shaken uniformly.
Further, in the shaking process, the solution is continuously shaken for 48 hours and then shaken for 30 minutes by ultrasonic wave.
Further, before the step 4), the following steps are included: the solution containing clay minerals is separated by centrifugation.
Further, in the step 4), the separated solution is placed in an environment with the temperature of less than 40 ℃ for drying.
Further, in step 6), 15% ZnO was added to the sample, and the content x2 of the clay mineral was quantitatively analyzed by an internal standard method.
According to the method for separating and measuring the content of the clay particles, the natural sedimentation method is adopted to extract particles smaller than 5 microns, so that the clay minerals are extracted from the sand making stone powder, and meanwhile, the content of the clay minerals is processed by combining a quantitative analysis method, so that the accuracy can reach 80% -90%, the content of the clay particles in the machine-made sand is more accurately separated and measured, and misjudgment is not easily caused.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a block diagram of the steps of a method for separation and assay of clay particles according to an embodiment of the present invention;
fig. 2 is a block diagram of the steps of a method for separating and measuring the content of clay particles according to another embodiment of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
FIG. 1 is a block diagram of the steps of a method for separation and assay of clay particles according to an embodiment of the present invention; as shown in fig. 1, the method for separating and measuring content of clay particles provided by the embodiment of the present invention includes the following steps:
1) determining the content X1 of a main mineral phase and the content X2 of a secondary mineral phase in the machine-made sandstone powder; wherein, X1+ X2 is 100%; the secondary mineral contains clay mineral;
2) dissolving machine-made sand powder in a solution to form turbid solution, and adding sodium hexametaphosphate into the turbid solution to dissolve clay minerals;
3) separating the solution containing clay minerals by a natural sedimentation method;
4) drying the separated solution;
5) repeating the step 3-4 for a plurality of times, and collecting the particles separated for a plurality of times;
6) sampling the separated particles, and quantitatively analyzing the content X2 of the clay mineral to obtain the content (X2X 2/100)% of the clay mineral in the machine-made sandstone powder.
According to the method for separating and measuring the content of the clay particles, provided by the embodiment of the invention, the particles with the particle size smaller than 5 microns can be extracted by adopting a natural sedimentation method, so that the clay minerals are extracted from the sand making stone powder, and meanwhile, the content of the clay minerals is processed by combining a quantitative analysis method, so that the accuracy can reach 80% -90%, the content of the clay particles in the machine-made sand is more accurately separated and measured, and misjudgment is not easily caused.
FIG. 2 is a block diagram of the steps of a method for separation and assay of clay particles according to another embodiment of the present invention; as shown in fig. 2, on the basis of the above embodiment, further, before step 1), the following steps are included: the machine-made sandstone powder in the stone chips is prepared by a water washing method.
Wherein, the water washing method comprises the following steps: and a method in which two types of substances having different solubilities are simultaneously passed through water, one of the two types being capable of dissolving in water and the other of the two types being incapable of dissolving, and then the aqueous layer is removed by a liquid separation method.
Further, in the step 1), after the machine-made sandstone powder is dried to constant weight at 60 ℃, sampling and quantitative analysis are carried out on the machine-made sandstone powder, and full spectrum fitting is carried out according to an XRD (X-ray diffraction) spectrum, so as to obtain the main mineral phase content X1 and the minor mineral phase content X2.
Wherein, the machine-made sand powder is dried in an oven.
Further, in the step 1), the machine-made sandstone powder is sampled by a quartering method.
The quartering method is also called a cone quartering method, and is a division operation method in which each sample is piled into a uniform cone shape, pressed into a frustum, and divided into quarters by a cross-shaped frame.
Further, in the step 1), analysis and quantitative analysis are carried out by using a type X-ray diffractometer, and the scanning speed is 2 degrees/min.
In this example, step 1) enables the determination of the content X1 of the main mineral phase and the content X2 of the secondary mineral (clay-containing mineral) phase, on the basis of the subsequent determination of the content of clay minerals.
On the basis of the above embodiment, further, in step 2), the machine-made sandstone powder is dissolved in deionized water to form a turbid solution, 4% of sodium hexametaphosphate is added, and the turbid solution is shaken and shaken up.
In the shaking process, the solution is continuously shaken for 48h and then shaken for 30min by ultrasonic wave.
Drying a machine-made sandstone powder sample at 60 ℃ to constant weight, sampling by adopting a quartering method, weighing 20g of the limestone powder, dissolving in 1000ml of deionized water to form turbid liquid, adding 3ml of 4% sodium hexametaphosphate into the solution, shaking the solution uniformly by uninterrupted oscillation for 48 hours, and then oscillating for 30 minutes by ultrasonic waves to completely dissolve clay minerals in the solution.
In this embodiment, step 2) is to dissolve the clay mineral in the solution, so that the clay mineral can be separated by a separation method.
As shown in fig. 2, on the basis of the above embodiment, further, before step 4), the following steps are further included: the solution containing clay minerals is separated by centrifugation.
Specifically, taking out the turbid liquid from the conical flask, pouring the turbid liquid into a first beaker, calculating the time required for 5-micrometer particles to naturally settle to a position 10cm away from the liquid level, naturally settling the particles, inserting a siphon pipe of 10cm into the beaker after the settling time is up, sucking out the turbid liquid at the position 10cm away from the liquid level, putting the turbid liquid in a second beaker into a high-speed centrifuge in batches, centrifuging until the upper-layer solution is clear, and putting a sample obtained by centrifuging into an oven (the oven temperature is less than 40 ℃) for drying.
The calculation method of the time required by natural sedimentation comprises the following steps:
according to the stokes (Stockers) natural sedimentation principle, dispersed particles uniformly distributed in a medium are sedimented under the action of gravity, when the gravity and the viscosity coefficient of the medium reach equilibrium, the dispersed particles are sedimented uniformly, and the sedimentation velocity of the particles is in direct proportion to the square of the radius of the particles and in inverse proportion to the viscosity coefficient of the medium, and the relationship can be represented by the following formula:
wherein v is the free settling velocity, cm/s; r-radius of dispersed particles, cm; d 1-density of dispersed particles, g/cm 3; d 2-density of media, g/cm 3; eta-viscosity coefficient of the medium, g/(cm · s).
When the particles move at a constant speed, the relationship between the constant-speed movement time t of the particles and the constant-speed movement distance s of the particles can be obtained, as shown in the following formula. Thus, the time required for the clay particles (<5 μm particles) in the stone dust to settle to a certain depth can be calculated at a certain temperature, so that the clay particles are separated out.
In addition, three simultaneous experiments were performed per set of samples and all isolated particles <5 μm were collected.
It is also possible to add a step of chemical separation before step 4).
Further, in the step 4), the separated solution is placed in an environment with the temperature of less than 40 ℃ for drying.
In this embodiment, during the test, the tester may select to separate the clay mineral solution by natural sedimentation and/or centrifugation of the sample according to the range of the precision requirement. In general, the measurement accuracy is higher by performing the centrifugation after the natural sedimentation.
On the basis of the above examples, further, in step 6), 15% ZnO was added to the sample, and the content x2 of the clay mineral was quantitatively analyzed by the internal standard method.
In this embodiment, ZnO can mark the clay mineral in the sample, which is helpful for identifying the clay mineral by using an internal standard method.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A method for separating and measuring the content of clay particles is characterized by comprising the following steps:
1) determining the content X1 of a main mineral phase and the content X2 of a secondary mineral phase in the machine-made sandstone powder; wherein, X1+ X2 is 100%; the secondary mineral contains clay mineral;
2) dissolving machine-made sand powder in a solution to form turbid solution, and adding sodium hexametaphosphate into the turbid solution to dissolve clay minerals;
3) separating the solution containing clay minerals by a natural sedimentation method;
4) drying the separated solution;
5) repeating the step 3-4 for a plurality of times, and collecting the particles separated for a plurality of times;
6) sampling the separated particles, and quantitatively analyzing the content X2 of the clay mineral to obtain the content (X2X 2/100)% of the clay mineral in the machine-made sandstone powder.
2. The method for separating and measuring the content of clay particles according to claim 1, further comprising the following steps before step 1):
the machine-made sandstone powder in the stone chips is prepared by a water washing method.
3. The method for separating and measuring the content of clay particles according to claim 1, wherein in the step 1), after the machine-made sandstone powder is dried to constant weight in an environment of 60 ℃, the machine-made sandstone powder is sampled and quantitatively analyzed, and a full spectrum fitting according to an XRD (X-ray diffraction) spectrum is carried out to obtain the main mineral phase content X1 and the secondary mineral phase content X2.
4. The method for separating and measuring the content of clay particles according to claim 3, wherein in the step 1), the machine-made sandstone powder is sampled by a quartering method.
5. The method for separation and content measurement of clay particles according to claim 3, wherein in step 1), analytical quantitative analysis is performed using a type X-ray diffractometer with a scanning speed of 2 °/min.
6. The method for separating and measuring the content of clay particles according to claim 1, wherein in the step 2), the machine-made sandstone powder is dissolved in deionized water to form a turbid solution, 4% of sodium hexametaphosphate is added, and the turbid solution is shaken up.
7. The method for separating and measuring the content of clay particles according to claim 6, wherein the solution is shaken for 48 hours without interruption during shaking and then is shaken for 30min by ultrasonic waves.
8. The method for separating and measuring the content of clay particles according to claim 1, further comprising the following steps before the step 4):
the solution containing clay minerals is separated by centrifugation.
9. The method for separating and measuring the content of clay particles according to claim 8, wherein in the step 4), the separated solution is dried in an environment of less than 40 ℃.
10. The method for separating and measuring the content of clay particles according to claim 1, wherein 15% ZnO is added to the sample in step 6), and the content x2 of the clay mineral is quantitatively analyzed by an internal standard method.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112945824A (en) * | 2021-02-24 | 2021-06-11 | 西安欧中材料科技有限公司 | Method for detecting inclusions in fine-particle-size nickel-based superalloy powder |
| CN115124268A (en) * | 2022-06-29 | 2022-09-30 | 长江水利委员会长江科学院 | Machine-made sand, preparation method and concrete prepared from machine-made sand |
| CN115321859A (en) * | 2022-07-25 | 2022-11-11 | 武汉理工大学 | Method for separating superfine stone powder and nano clay from limestone mine tailings |
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