CN107478585B - Method for testing free silicon dioxide in mica powder - Google Patents
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- CN107478585B CN107478585B CN201710637369.7A CN201710637369A CN107478585B CN 107478585 B CN107478585 B CN 107478585B CN 201710637369 A CN201710637369 A CN 201710637369A CN 107478585 B CN107478585 B CN 107478585B
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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- G—PHYSICS
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- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/22—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
Abstract
The invention provides a method for testing free silicon dioxide in mica powder, which comprises the following steps: (1) separating mica powder; (2) putting the residue settled at the bottom of the beaker into a triangular flask, adding a selective solvent, heating, cooling to room temperature, adding water for dilution, and adding concentrated nitric acid; (3) filtering the solution in the step (2), washing residues in the triangular flask by using dilute nitric acid, transferring the residues to filter paper, and washing by water; (4) putting the filter paper and the residues into a silver crucible for cooling and high-temperature burning; taking out the silver crucible, cooling to room temperature, adding a plurality of drops of absolute ethyl alcohol and sodium hydroxide, and melting at high temperature; (5) after the silver crucible in the step (4) is cooled to room temperature, adding hot water for leaching, heating until the solution is clear, and pouring the solution into a hydrochloric acid aqueous solution; (6) and (3) sucking 2-5ml of the clear liquid into a colorimetric tube, adding 1N hydrochloric acid, an ammonium molybdate solution and an ammonium persulfate solution, then adding absolute ethyl alcohol, diluting with water to scale, shaking uniformly, standing for 30-60 minutes, and measuring the extinction value.
Description
Technical Field
The invention relates to the technical field of silicon dioxide testing, in particular to a method for testing free silicon dioxide in mica powder.
Background
The sand content is one of the important indexes for evaluating the mica powder, and the main component of the sand content is quartz or opal monomer siliceous mineral-free silicon dioxide (fSiO)2) It is a bad substance directly affecting the application of mica powder in some high-grade fields, and must be strictly monitored. The test of the free silicon dioxide belongs to item analysis, however, at present, China has no unified' about fSiO in mica powder2Test method of (1). We have intensely explored and studied that established physicochemical principles are one of the effective ways to solve this problem. Firstly, adopting a physical sedimentation method to distribute fSiO in mica powder2All sand-like minerals in the sand are enriched and separated, and then the fSiO is quantitatively determined by adopting a chemical reaction test method on the basis2The actual content in the mica powder, i.e. the physicochemical process described above. The successful application of the technology in the mica powder test is still the first creation in China, and the technology plays a good role in widening the application field of the mica powder.
Disclosure of Invention
The invention aims to solve part of problems in the existing silicon dioxide testing technology and provides a method for testing free silicon dioxide in mica powder.
The purpose of the invention is realized by the following technical scheme:
a method for testing free silicon dioxide in mica powder comprises the following steps:
(1) weighing mica powder, putting into a beaker, adding water, stirring uniformly, pouring out the slurry containing the mica powder, injecting water, repeating the pouring and water injection steps for 3-4 times until the mica powder in the beaker is basically completely separated;
(2) pouring the residue settled at the bottom of the beaker into a triangular flask by using water and placing the triangular flask on an electric heating plate;
(3) adding a selective solvent into the triangular flask, then starting an electric heating plate for heating, shaking the triangular flask at intervals, heating until the violent reaction in the triangular flask stops, then maintaining for about 30 minutes, taking down, cooling to room temperature, adding water for dilution, and then adding concentrated nitric acid;
(4) filtering the solution in the step (3), washing residues in the triangular flask by using dilute nitric acid, transferring the residues to filter paper, and washing the residues in the triangular flask and the filter paper by using warm water until the residues are free from acidity;
(5) putting the filter paper and the residues into a silver crucible, putting the silver crucible into a muffle furnace for low-temperature ashing and low-temperature ashing (namely, a low-temperature ashing stage from room temperature to firing humidity after a power supply is turned on and before firing), and heating to a high temperature for firing;
(6) taking out the silver crucible, cooling to room temperature, adding a plurality of drops of absolute ethyl alcohol, weighing granular sodium hydroxide, spreading on residues of the silver crucible, and putting the silver crucible into a muffle furnace again for high-temperature melting;
(7) after the silver crucible in the step (6) is cooled to room temperature, adding hot water, placing the silver crucible on an electric hot plate, heating until the solute is clear, stirring, pouring the mixture into a volumetric flask containing hydrochloric acid water solution, diluting the mixture with water until the scales are uniformly shaken;
(8) and (3) sucking 2-5ml of the clear liquid into a colorimetric tube, adding 1N hydrochloric acid, an ammonium molybdate solution and an ammonium persulfate solution, then adding absolute ethyl alcohol, diluting with water to scale, shaking uniformly, standing for 30-60 minutes, and measuring the extinction value.
The selective solvent in the step (3) is phosphorus-nitric mixed acid, the mass-volume ratio of the mica powder to the selective solvent is 2:1.5, the mass unit is g, and the volume unit is ml.
Preferably, the volume of the slurry containing the mica powder poured in the step (1) is 80% of the total volume.
Preferably, the step (1) of pouring out adopts a siphon method.
Preferably, the volume ratio of phosphoric acid to nitric acid in the selective solvent in the step (3) is 15: 1; the mass volume ratio of the mica powder to the selective solvent is 2: 1.5.
Preferably, the heating temperature in the step (3) is 190-210 ℃, and the concentration of the concentrated nitric acid is 14N; the addition amount is 1-3 ml.
Preferably, the filtration in the step (4) is performed by using slow quantitative filter paper paved with a proper amount of paper pulp; in the step (4), the concentration of the nitric acid is 1-3%, the washing times are 3-4 times, and the concentration of the nitric acid is 1-3%, which means that 1-3ml of concentrated nitric acid, namely water, is contained in each 100ml of water solution: acid 99: 97 to volume ratio.
Preferably, the temperature of the high-temperature burning in the step (5) is 650-750 ℃ and the time is 20-60 minutes.
Preferably, the temperature of the high-temperature melting in the step (6) is 550-600 ℃, and the time is 5-10 minutes; the mass ratio of the sodium hydroxide to the mica powder is 20:1-2 (the fused matter is fSiO in the residue after the mica powder is separated2Not all mica powder).
Preferably, in the step (7), the volume ratio of the hydrochloric acid to the water in the hydrochloric acid aqueous solution is 1:1, and the addition amount of the hydrochloric acid aqueous solution is 10-15 ml.
Preferably, the concentration of the hydrochloric acid in the step (8) (volume concentration is 5-10ml of concentrated hydrochloric acid in 100ml of aqueous solution) is 5-10%, and the addition amount is 8-12 ml; the concentration of the ammonium molybdate solution is 5-10%, the adding amount is 1-8ml, the concentration of the ammonium persulfate solution is 8-12%, and the adding amount is 1-5 ml; the addition amount of the absolute ethyl alcohol is 8-10 ml; wherein ammonium molybdate and ammonium persulfate are solute gram weight g: water volume ml.
The invention has the beneficial effects that: in the step (6) of the present application, sodium hydroxide is used as a solvent, and the amount of the sodium hydroxide is different according to the property and the weight of the processed sample, and the sand content in the mica powder mainly comprises feldspar, quartz, marble, a small amount of limonite and the like. After passing through the solvent, the siliceous minerals of quartz (including opal) are remained, and other various mineral rocks are dissolved. Then filtered to separate, so that the sodium hydroxide melts at high temperature to leave little quartz (opal). The aim is to convert it into a molten state and then to assume an ionic state in the hydrochloric acid solution. The amount of sodium hydroxide added depends on the amount of quartz (including opal) ore, but not too much, which would severely corrode the silver crucible. The addition of the concentrated nitric acid in the step (3) enables the dissolved mineral components to be in an ionic state all the time, and the addition of the concentrated nitric acid can avoid hydrolysis, so that the aim of facilitating filtration and separation is fulfilled. However, the adding amount of the concentrated nitric acid cannot be too high, and the excessive nitric acid is corroded and filtered to lower the influence on the filtration. In the application, various reagents are added in the amount determined after tests, so that the requirements of a color development process are met while the reagent is saved. Of these, acidity and complex stabilization time are particularly important.
Drawings
FIG. 1 is a graph of selective solvent usage versus extinction;
FIG. 2 is a graph showing the reaction time in the flask and the extinction value in step (3);
FIG. 3 is a test result expression;
fig. 4 is a graph of the operating curve.
Detailed Description
In order to better explain the present invention, the technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the drawings in the embodiments of the present invention.
The applicant can separate the mica powder from other minerals with high specific gravity and sand grains conveniently by physical settling method, and the rest of mica powder is dissolved and separated by selective solvent2Minerals, quartz (including opal) is retained for free silica (fSiO)2) Quantitative test, (measurement of silicon, usually high content by gravimetric method, low content by colorimetric method).
Example 1
Weighing 20g of dried mica powder sample, putting the dried mica powder sample into a 1000ml beaker, adding a little water, stirring the mixture into paste, then injecting the water into the beaker to about 800ml, and fully and uniformly stirring the mixture. After a few minutes of standing until the liquid level is calm, the slurry containing the mica powder is carefully poured out to about 80% of the total volume, preferably by the siphon method. And then injecting water again, and repeating the operation steps for 4 times until the mica powder in the beaker is basically separated completely. Carefully pouring all residues settled at the bottom of the beaker into a 150ml triangular flask by using a fine water flow, and pouring off excessive water.
Placing 150ml of triangular flask containing the enriched sand content on an electric heating plate, carefully adding 15ml of selective solvent, wherein the selective solvent is mixed acid with the volume ratio of phosphoric acid to nitric acid being 15:1, and then starting the electric heating plate to heat and decompose the sample at the temperature of 200 ℃. The flask was shaken 4 times at intervals to disperse the sand grains. Heating until the violent reaction in the bottle stops, maintaining for 30 minutes, taking down the triangular flask, cooling to room temperature, adding water to dilute to about 100ml, adding 1ml of concentrated nitric acid, and shaking up. Filtering with slow quantitative filter paper spread with appropriate amount of paper pulp, washing the triangular flask and residue with 1% nitric acid for 3 times, transferring the residue in the flask onto the filter paper (wiping the inner wall of the flask with a small piece of filter paper), washing the residue in the triangular flask and the filter paper with warm water until no acidity exists, and verifying whether the residue is no acidity with pH test paper.
Putting the filter paper together with the residues (namely quartz or opal minerals) into a silver crucible, putting the silver crucible into a muffle furnace, ashing at low temperature, heating to 700 ℃, and burning for 30 minutes. Taking out the crucible, cooling to room temperature, adding a plurality of drops of absolute ethyl alcohol, weighing 1g of granular sodium hydroxide by a balance with a sensitivity of 0.1g, placing the granular sodium hydroxide on the residue, spreading, putting the crucible into a muffle furnace again, heating to 550 ℃, melting for 7 minutes, and taking out. Adding hot water into the crucible to 2/3 position after the crucible is cooled to room temperature, placing the crucible on an electric hot plate, heating and leaching until the solution is clear, stirring with a plastic stirring rod, and standing for a while. The solution was slowly poured into a 100ml volumetric flask previously containing 12ml of 1:1 hydrochloric acid and 30ml of water (shaking the flask while pouring the solution) and then diluted with water until the scale was shaken up.
2-5ml of the above clear solution (less than 5ml and 5ml of blank solution) is sucked into a 100ml colorimetric tube. 10ml of 8% hydrochloric acid, 5ml of 7% ammonium molybdate solution and 2ml of 10% ammonium persulfate solution are added, 10ml of absolute ethyl alcohol is immediately added (each reagent is added and is shaken up), diluted to the scale with water and shaken up. After standing for 30 minutes, the extinction value was measured immediately using a model 721 spectrophotometer, a 1cm cuvette with a wavelength of 420 μm, and water as a reference solution.
Drawing a working curve, absorbing a silicon dioxide standard solution: 0. 100, 300, 500, 700, 1000, 1500, 2000, 2500, 3000. mu.g of the total amount of the compound was added to a 100ml cuvette, about 30ml of water was added, a drop of 0.1% nitrophenol indicator was added and neutralized with 1N hydrochloric acid until the yellow color disappeared, and an excess of 10ml was added, followed by the same procedure as the sample, and the curve was plotted as shown in FIG. 4.
In order to ensure the authenticity and reliability of the measurement result, A, B, C three parts of the same sample are weighed simultaneously, 20mg of high-purity quartz sand of 40 meshes is accurately weighed into the sample C, and then parallel tests are carried out simultaneously. In calculating the analysis results, the arithmetic mean of A, B samples was taken, and C sample was used to examine the recovery rate of high purity silica sand. Practice shows that: the yield can reach one hundred percent, and the blank value in the test is basically zero; 1-2 blank tests are carried out simultaneously in the test.
The test results are expressed in FIG. 3.
For the test of the amount of selective solvent used in step (3): the operation is carried out according to the steps of the method of the invention, only the amount of the selected solvent is changed, and the result is shown in FIG. 1, FIG. 1 shows that the phosphorus-nitric mixed acid is a strong selective solvent, the extinction values of 20g of mica powder samples with the sand content of 10-25ml are basically consistent, and the amount of the selective solvent in the embodiment is preferably 15 ml.
Further description with respect to fig. 1:
① weighing 5 parts of dry mica powder and 5 parts of wet mica powder respectively, wherein each part is 20g, placing the dry mica powder and the wet mica powder into a beaker, separating the mica powder according to the testing method of the invention, flushing the obtained residue into a triangular flask by using water, respectively adding different amounts of selective solvents (phosphorus-nitric mixed acid), and then heating and decomposing the sample on an electric heating plate;
② proceed to complete the steps of the method of the invention.
③ the extinction values (E) measured by dry mica powder and wet mica powder with different solvent amounts are plotted in figure 1. from figure 1, the result is basically the same for the residue in 20g dry mica powder or wet mica powder with 10-25ml of selective solvent amount.
Regarding the test of the reaction time and extinction value in the flask in step (3), the reaction time was varied according to the procedure of the method of the present invention, and the results are shown in FIG. 2: FIG. 2 shows that the sand content of the 20g mica powder sample is substantially consistent with the extinction value of 20-40 min, and the preferred reaction time in this embodiment is 30 min.
Further description with respect to fig. 2:
① weighing 5 dry mica powder and 5 wet mica powder, each of which is about 20g, respectively, placing the dry mica powder and the wet mica powder into a beaker, separating the mica powder according to the test method of the invention, flushing the obtained residues into a triangular flask with water, adding 15ml of each selective solvent (phosphorus nitric mixed acid), heating on an electric heating plate to decompose a sample, heating until the violent reaction in the triangular flask stops, and continuing to heat at intervals of 10, 20, 30, 40 and 50 minutes to respectively take down one dry mica powder test sample and one wet mica powder test sample;
② proceed to complete the steps of the method of the invention.
③ the extinction values (E) measured by the dry mica powder and the wet mica powder taken down at different intervals are plotted in figure 2. As can be seen from figure 2, for the residue in 20g of dry mica powder or wet mica powder, the residue is heated until the violent reaction in the triangular flask stops, and then the residue is continuously heated for 20-40 minutes, and the test results are basically the same.
Influencing the silicon molybdenum yellow color development reaction with respect to the acidity of the solution in the step (8); the monomolecular silicic acid with too high acidity is easy to polymerize into the polymolecular silicic acid, so that the color development reaction is incomplete. If the acidity is too low, the color reaction is slow, and a small amount of high-valence metal ions existing in the solution are easy to hydrolyze to interfere with the determination. Absorbing standard SiO2Solution 1000ug in 100ml colorimetric cylinderIn this, 30ml of water were added and different amounts of 80% hydrochloric acid were added, operating according to the procedure of the process of the invention, the results are shown in Table 1.
TABLE 1
| Hydrochloric acid dosage (ml) | 2 | 4 | 6 | 8 | 10 | 15 | 20 | 25 |
| Photometer reading (E) | 0.190 | 0.204 | 0.205 | 0.205 | 0.205 | 0.200 | 0.114 | 0.017 |
Table 1 shows that the extinction values do not change much in the range of 4 to 15ml with 8% hydrochloric acid in a volume of 100ml, and the extinction values drop significantly when the amount of hydrochloric acid exceeds 15ml, 10ml with 8% hydrochloric acid being used in this example.
For the silicon clamp yellow complex stabilization time test: silicon molybdenum yellow complex [ H8Si(Mo2O7)-H2O]Before the stability of (2), a person has done too much work, and the details are not repeated here. There are data describing that addition of a certain amount of hexanol can protect the complex, but the introduction of hexanol will affect the measurement by reducing part of the silico-molybdenum yellow to silico-molybdenum blue (the lower the content is, the more obvious). For this reason, we add 0.1-0.3g ammonium persulfate before adding the existing alcohol, can receive good results, and the complex stability time is up to 3 hours invariable, this method adopts and adds 2ml of 10% ammonium persulfate solution, the result is shown in Table 2:
TABLE 2
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention disclosed herein should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. A method for testing free silicon dioxide in mica powder is characterized by comprising the following steps:
(1) weighing mica powder, putting into a beaker, adding water, stirring uniformly, pouring out the slurry containing the mica powder, injecting water, and repeating the pouring and water injection steps for 3-4 times;
(2) pouring the residue settled at the bottom of the beaker into a triangular flask by using water and placing the triangular flask on an electric heating plate;
(3) adding a selective solvent into the triangular flask, then starting an electric heating plate for heating, shaking the triangular flask at intervals, heating until the violent reaction in the triangular flask stops, then maintaining for 30 minutes, taking down and cooling to room temperature, adding water for dilution, and then adding concentrated nitric acid;
(4) filtering the solution in the step (3), washing residues in the triangular flask by using dilute nitric acid, transferring the residues to filter paper, and washing the residues in the triangular flask and the filter paper by using warm water until the residues are free from acidity;
(5) putting the filter paper and the residues into a silver crucible, putting the silver crucible into a muffle furnace for low-temperature ashing, and heating to a high temperature for firing;
(6) taking out the silver crucible, cooling to room temperature, adding a plurality of drops of absolute ethyl alcohol, weighing granular sodium hydroxide, spreading on residues of the silver crucible, and putting the silver crucible into a muffle furnace again for high-temperature melting;
(7) after the silver crucible in the step (6) is cooled to room temperature, adding hot water, placing the silver crucible on an electric hot plate, heating the silver crucible until the solution is clear, stirring the solution, pouring the solution into a volumetric flask containing hydrochloric acid water solution, diluting the solution with water until the scales are evenly shaken;
(8) sucking the clear liquid obtained in the step (7) into a colorimetric tube, adding 1N hydrochloric acid, an ammonium molybdate solution and an ammonium persulfate solution, then adding absolute ethyl alcohol, diluting with water to scale, shaking uniformly, standing for 30-60 minutes, and measuring the extinction value;
the residue in the step (2) is free of any fluorine-containing mineral component;
the selective solvent in the step (3) is phosphorus-nitric mixed acid, the mass-volume ratio of the mica powder to the selective solvent is 2: 1-2.5, the mass unit is g, and the volume unit is ml;
the volume of the clear liquid in the step (8) is 2-5 ml.
2. The method for testing free silica in mica powder according to claim 1, wherein the volume of the slurry containing mica powder poured out in the step (1) is 80% of the total volume.
3. The method for testing free silica in mica powder as claimed in claim 1, wherein the pouring out in step (1) is by siphon method.
4. The method for testing free silica in mica powder according to claim 1, wherein the volume ratio of phosphoric acid to nitric acid in the selective solvent in the step (3) is 15: 1; the mass volume ratio of the mica powder to the selective solvent is 2: 1.5.
5. The method for testing free silica in mica powder as claimed in claim 1, wherein the heating temperature in the step (3) is 190-210 ℃; the concentration of the concentrated nitric acid is 14N, and the adding amount is 1-3 ml.
6. The method for testing free silica in mica powder according to claim 1, wherein the filtering in the step (4) is performed by using a slow quantitative filter paper paved with a proper amount of paper pulp; in the step (4), the concentration of nitric acid is 1-3%, and the washing times are 3-4.
7. The method for testing free silica in mica powder as claimed in claim 1, wherein the high temperature burning in step (5) is 650-750 ℃ for 20-60 min.
8. The method for testing free silica in mica powder as claimed in claim 1, wherein the temperature of the high temperature melting in the step (6) is 550-600 ℃ for 5-10 min; the mass ratio of the mica powder to the sodium hydroxide is 20: 1-2.
9. The method for testing free silica in mica powder according to claim 1, wherein the volume ratio of hydrochloric acid to water in the hydrochloric acid aqueous solution in the step (7) is 1:1, and the addition amount of the hydrochloric acid aqueous solution is 10-15 ml.
10. The method for testing free silica in mica powder according to claim 1, wherein the concentration of hydrochloric acid in the step (8) is 5-10%, and the addition amount is 8-12 ml; the concentration of the ammonium molybdate solution is 5-10%, and the addition amount is 1-8 ml; the concentration of the ammonium persulfate solution is 8-12%, and the adding amount is 1-5 ml; the addition amount of the absolute ethyl alcohol is 8-10 ml.
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| CN101988892A (en) * | 2009-07-30 | 2011-03-23 | 中国商用飞机有限责任公司 | Method for measuring silicon dioxide content in solution |
| CN103728261A (en) * | 2013-12-14 | 2014-04-16 | 武钢集团昆明钢铁股份有限公司 | Fast and accurate detection method for silicon dioxide content in limestone, kalk and dolomite |
| CN106092922A (en) * | 2016-05-30 | 2016-11-09 | 内蒙古包钢钢联股份有限公司 | The detection method of silicon dioxide in carbide slag |
| CN106338450A (en) * | 2016-08-26 | 2017-01-18 | 内蒙古包钢钢联股份有限公司 | Continuous analysis method of calcium fluoride and silicon dioxide in fluorite |
| CN106353301A (en) * | 2016-08-14 | 2017-01-25 | 贵州开磷质量检测中心有限责任公司 | Silicon dioxide measuring method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101988892A (en) * | 2009-07-30 | 2011-03-23 | 中国商用飞机有限责任公司 | Method for measuring silicon dioxide content in solution |
| CN103728261A (en) * | 2013-12-14 | 2014-04-16 | 武钢集团昆明钢铁股份有限公司 | Fast and accurate detection method for silicon dioxide content in limestone, kalk and dolomite |
| CN106092922A (en) * | 2016-05-30 | 2016-11-09 | 内蒙古包钢钢联股份有限公司 | The detection method of silicon dioxide in carbide slag |
| CN106353301A (en) * | 2016-08-14 | 2017-01-25 | 贵州开磷质量检测中心有限责任公司 | Silicon dioxide measuring method |
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