CN111537386A - Method for analyzing content of silicon dioxide - Google Patents
Method for analyzing content of silicon dioxide Download PDFInfo
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- CN111537386A CN111537386A CN202010395433.7A CN202010395433A CN111537386A CN 111537386 A CN111537386 A CN 111537386A CN 202010395433 A CN202010395433 A CN 202010395433A CN 111537386 A CN111537386 A CN 111537386A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 19
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000005303 weighing Methods 0.000 claims abstract description 15
- 239000000706 filtrate Substances 0.000 claims abstract description 13
- 239000013049 sediment Substances 0.000 claims abstract description 10
- 238000002844 melting Methods 0.000 claims abstract description 9
- 230000008018 melting Effects 0.000 claims abstract description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 52
- 239000000919 ceramic Substances 0.000 claims description 27
- 238000010438 heat treatment Methods 0.000 claims description 27
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 26
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 24
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 22
- 238000001816 cooling Methods 0.000 claims description 22
- 238000010304 firing Methods 0.000 claims description 20
- 239000002244 precipitate Substances 0.000 claims description 19
- 239000000779 smoke Substances 0.000 claims description 18
- 239000011521 glass Substances 0.000 claims description 15
- 230000004907 flux Effects 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000010306 acid treatment Methods 0.000 claims description 8
- 239000011324 bead Substances 0.000 claims description 8
- 239000004576 sand Substances 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 235000011837 pasties Nutrition 0.000 claims description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims description 4
- 239000011733 molybdenum Substances 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 4
- 238000005375 photometry Methods 0.000 claims description 4
- 229920002620 polyvinyl fluoride Polymers 0.000 claims description 4
- 238000009736 wetting Methods 0.000 claims description 4
- 238000004380 ashing Methods 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 3
- 239000004327 boric acid Substances 0.000 claims description 3
- 238000010000 carbonizing Methods 0.000 claims description 3
- 238000005485 electric heating Methods 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
- 239000000017 hydrogel Substances 0.000 claims description 3
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 abstract description 5
- 238000004090 dissolution Methods 0.000 abstract description 5
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 3
- 238000001304 sample melting Methods 0.000 abstract description 2
- 238000007711 solidification Methods 0.000 abstract 1
- 230000008023 solidification Effects 0.000 abstract 1
- 229910052573 porcelain Inorganic materials 0.000 description 10
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- 230000018044 dehydration Effects 0.000 description 5
- 238000006297 dehydration reaction Methods 0.000 description 5
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 4
- 238000010408 sweeping Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 238000005406 washing Methods 0.000 description 2
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000007849 furan resin Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
-
- 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
- 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
- G01N1/38—Diluting, dispersing or mixing samples
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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
- G01N1/44—Sample treatment involving radiation, e.g. heat
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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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
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Abstract
The invention discloses a method for analyzing the content of silicon dioxide, which comprises the steps of adopting quantitative filter paper to hold a sample, preparing analysis filtrate and sediment, weighing a quantitative sample, wrapping the quantitative sample with the quantitative filter paper, mixing the quantitative sample with a mixed fusing agent, simultaneously adopting a graphite powder crucible to melt the sample in a high-temperature box-type resistance furnace, enabling the sample to be free of splashing in the sample melting process, achieving the solidification of the sample, dissolving the solidified standard sample, ensuring the complete melting of the sample, quickly dehydrating after the dissolution, having high speed and less splashing phenomenon, and obtaining purer silicon dioxide, thereby reducing errors and having more accurate numerical value.
Description
Technical Field
The invention relates to a method for analyzing content, in particular to a method for analyzing the content of silicon dioxide in silica sand.
Background
In the process of adopting furan resin self-hardening sand for casting, raw materials used for molding and core making mainly comprise silica sand, wherein the main component of the silica sand is silica, and the product quality is directly influenced by the content of the silica. The analysis of the content of silicon dioxide generally adopts a platinum crucible container to melt a sample in a high-temperature box type resistance furnace, a fusing agent adopts anhydrous sodium carbonate to melt the sample, the fused sample is uniformly adhered to the inner wall of the platinum crucible (the fused sample becomes a thin sheet and is easy to dissolve), and then hydrochloric acid (1+1) is added for dissolution. However, in the actual plant operation process, the use of a platinum crucible is costly and difficult to store.
The method adopts a graphite powder crucible (made of pyrolytic graphite powder containing 99.85% of carbon), melts samples in a high-temperature box-type resistance furnace, if the fusing agent adopts anhydrous sodium carbonate to melt samples, when the flat-ball fused beads are dissolved in HCl (1+1) to the samples, the dissolution speed is slow and the samples are not easy to be completely dissolved, thereby causing time and labor waste and errors in analysis.
Disclosure of Invention
The invention aims to provide a method for analyzing the content of silicon dioxide, which has the advantages of low cost, low energy consumption, easy operation and accurate analysis.
The task of the invention is achieved in that: adopting quantitative filter paper to hold samples, and preparing and analyzing filtrate and sediment, wherein the method comprises the following specific steps:
weighing a sample, wherein the mass of the sample is 0.2g and is accurate to 0.0001g of silica sand sample;
step (2), folding quantitative filter paper into a conical bag shape, filling 2g of mixed flux into a filter bag, and putting the step (1) into the filter bag to be fully and uniformly mixed with the mixed flux to obtain a sample;
step (3) covering a layer of 1g of mixed flux on the mixed sample obtained in the step (2), and folding and wrapping the filter bag to obtain a sample;
step (4), placing the sample obtained in the step (3) into a prepared graphite crucible, then placing the crucible into a high-temperature box type resistance furnace, gradually heating the crucible to 900 ℃ from low temperature, melting the crucible for 15-30 minutes, opening a furnace door, taking out the crucible, cooling the crucible to room temperature, and obtaining a standard sample, wherein the sample in the crucible is in the shape of a glass ball molten bead after high temperature and cooling, and the standard sample has certain mechanical strength and does not absorb water;
step (5), putting the standard sample obtained in the step (4) into a 250ml beaker, adding 40ml hydrochloric acid (1+1), heating the beaker on an electric furnace at about 600 ℃, raising the temperature of the hydrochloric acid (1+1) solution in the beaker to about 100 ℃, completely dissolving the standard sample for 2-3 minutes, taking off the standard sample, adding 20ml perchloric acid into the dissolved standard sample, covering a watch glass, heating and dehydrating the standard sample on an electric furnace at 700 ℃, rising the solution temperature to about 210 ℃ along with the rise of the temperature of the solution to about 120 ℃ to emit hydrochloric acid smoke, continuously refluxing the perchloric acid smoke for 10-20 minutes until the residue is pasty, folding the silicic acid out in a hydrogel state after the standard sample is heated and dehydrated at low temperature, adding 30ml hydrochloric acid (1+1) after the solution is slightly cooled, stirring, dissolving salts, adding hot water at about 80 ℃ to 150ml volume, dissolving the salt again, and taking out the solution after slight boiling to obtain a solution;
filtering the solution obtained in the step (5) by using medium-speed quantitative filter paper, checking the filtrate to be neutral by using a pH test, and measuring the content of silicon dioxide M1 in the filtrate by using a molybdenum blue absorption photometry;
and (7) transferring the precipitate and the filter paper obtained in the step (6) into a ceramic crucible, dropwise adding 2 drops of sulfuric acid (1: 1), drying, carbonizing and ashing on an electric furnace at a low temperature of 100-150 ℃, then heating to 640-650 ℃ in a gradient manner to carbonize the quantitative filter paper until no smoke exists and the filter paper can not catch fire, and then moving to a high temperature without closing the door, and gradually heating to 900 ℃ from 700 ℃ to the furnace side to completely oxidize the carbon. Firing for 30 minutes, covering the ceramic crucible with a cover, and reserving a strip gap to enable air to flow back, moving the ceramic crucible into a high-temperature furnace at 950 plus material temperature of 1000 ℃, firing for 30 minutes, taking out, cooling, weighing, and repeatedly firing until the constant weight m1 is equal to the mass of the sediment and the ceramic crucible before hydrofluoric acid treatment;
step (8), the sample obtained after the firing in the step (7) is completely swept into a polyvinyl fluoride crucible, a plurality of drops of water are used for wetting, 3 drops of sulfuric acid 1:1 and 5ml of hydrofluoric acid are added, the sample is steamed on an electric heating plate at the low temperature of less than 250 ℃ until the sample is dried, the sediment is completely swept into a ceramic crucible, the heating is continued, the heating temperature is 350-400 ℃, the ceramic crucible is fired for 15 minutes in a high-temperature furnace at 950-1000 ℃, the ceramic crucible is cooled to the room temperature in a dryer, the mass of the sediment and the ceramic crucible after the m2 hydrofluoric acid treatment is weighed,
the percentage of silica in the precipitate M2= (M1-M2) ÷ mass of the sample × 100%
The silica content in the sample = the sum of M1 + M2.
In the steps 1 and 2, quantitative filter paper is adopted to be folded into a conical bag shape to wrap the sample.
Step 2 the mixed flux used in step 3 and step 5 was made of 2.2g of anhydrous sodium carbonate and 0.8g of boric acid.
The invention has the following effects: the method comprises the steps of weighing a quantitative sample, wrapping the sample by using quantitative filter paper, mixing the sample by using a mixed flux, and simultaneously melting the sample in a high-temperature box type resistance furnace by using a graphite powder crucible, wherein the sample does not splash in the sample melting process, the sample can be solidified, the solidified standard sample is dissolved at a high dissolving speed, the sample can be completely dissolved, and the sample is quickly dehydrated after being dissolved, so that the speed is high, the splashing phenomenon is less, and pure silicon dioxide is obtained, thereby reducing errors and ensuring more accurate numerical value.
Detailed Description
Example one
Weighing a quantitative sample, wrapping the sample with quantitative filter paper, mixing with a mixed flux, placing the sample in a graphite crucible, transferring the graphite crucible into a high-temperature box type resistance furnace for melting, taking out the sample when the sample is melted into a oblate spheroid glass bead shape, dissolving with HCl (1+1), filtering with quantitative filter paper, measuring the content of silicon dioxide in the filtrate by a molybdenum blue absorption photometry, and finally obtaining the content M1 of silicon dioxide in the filtrate, wherein the content of silicon dioxide in silica sand = the sum of M1 + M2, so M2 needs to be obtained, and M2 is obtained by the mass x 100% of the sample of the percentage content M2 in the precipitate (M1-M2 divided by the sum of the mass M1 and the mass 100%, so that the precipitate and the filter paper are transferred into a clean ceramic crucible in the filtering process, adding a plurality of drops of sulfuric acid, drying, carbonizing and ashing on an electric furnace at low temperature, then transferring into the high-temperature furnace without closing the door for 30 minutes, and then moving the crucible into a high-temperature furnace to be burned for 30 minutes, taking out and cooling, weighing, repeatedly burning until the weight is constant m1, then completely sweeping m1 into a polyvinyl fluoride crucible, wetting with water, dripping sulfuric acid and hydrofluoric acid, evaporating to dryness on a low-temperature furnace, then completely sweeping the precipitate into a ceramic crucible, continuously heating, observing with naked eyes, burning the crucible in the high-temperature furnace for 15 minutes under the condition of exhausting white smoke of sulfur trioxide, slightly cooling, cooling to room temperature in a dryer, weighing, and repeatedly burning until the weight is constant m 2.
The steps of the first embodiment are as follows:
weighing a sample, wherein the mass of the sample is 0.2g and is accurate to 0.0001g of silica sand sample;
step (2), folding quantitative filter paper into a conical bag shape, filling 2g of mixed flux into a filter bag, and putting the step (1) into the filter bag to be fully and uniformly mixed with the mixed flux to obtain a sample;
step (3) covering a layer of 1g of mixed flux on the mixed sample obtained in the step (2), and folding and wrapping the filter bag to obtain a sample;
step (4), placing the sample obtained in the step (3) into a prepared graphite crucible, then placing the crucible into a high-temperature box type resistance furnace, gradually heating the crucible to 900 ℃ from low temperature, melting the crucible for 15-30 minutes, opening a furnace door, taking out the crucible, cooling the crucible to room temperature, and obtaining a standard sample after the sample in the crucible is in the shape of a glass ball molten bead after high temperature and cooling, wherein the standard sample has certain mechanical strength and does not absorb water, and hydrochloric acid (1+1) solution is added for complete dissolution;
and (5) putting the standard sample obtained in the step (4) into a 250ml beaker, adding 40ml of hydrochloric acid (1+1), heating the beaker on an electric furnace at the temperature of about 600 ℃, raising the temperature of the hydrochloric acid (1+1) solution in the beaker to 90-100 ℃, and completely dissolving and removing the standard sample after 2-3 minutes. Adding 20ml perchloric acid on the dissolved standard sample, covering a watch glass, placing the standard sample on a 700 ℃ electric furnace for heating and dehydration, and continuously refluxing for 10-20 minutes by the perchloric acid with thick white smoke at the temperature of 200-210 ℃ along with the temperature of the solution is increased to 110-120 ℃. At the moment, the standard sample is subjected to low temperature, heating and dehydration, silicic acid is folded out in a hydrogel state, the standard sample is taken down and slightly cooled, then 30ml of hydrochloric acid (1+1) is added for stirring, salts are dissolved, hot water with the temperature of about 80 ℃ is added to reach the volume of 150ml, the salts are dissolved again, and the standard sample is taken down after slight boiling, so that a solution is obtained;
filtering the solution obtained in the step (5) by using medium-speed quantitative filter paper, checking the filtrate to be neutral by using PH test paper, and measuring the content M1 of silicon dioxide in the filtrate by using a molybdenum blue absorption photometry;
and (7) transferring the precipitate and the filter paper obtained in the step (6) into a ceramic crucible, dropwise adding 2 drops of sulfuric acid (1: 1), drying the precipitate and the filter paper on an electric furnace at a low temperature (the temperature is 100-150 ℃, and then the temperature is increased to 650 ℃ in a gradient manner) to carbonize the quantitative filter paper until the quantitative filter paper is smokeless (the filter paper cannot catch fire), and then moving the precipitate and the filter paper to a high-temperature furnace side without closing the door (the temperature is gradually increased from 700 ℃ to 900 ℃) to completely oxidize the carbon. Firing for 30 minutes, covering the ceramic crucible (a strip gap should be reserved so as to enable air to flow back), then moving the ceramic crucible into a high-temperature furnace at 950-1000 ℃, firing for 30 minutes, taking out, cooling, weighing, and repeatedly firing until the constant weight m1 (the mass of the sediment and the ceramic crucible before hydrofluoric acid treatment);
step (8), sweeping the burned sample m1 obtained in step (7) into a polyvinyl fluoride crucible, wetting with a plurality of drops of water, adding 3 drops of sulfuric acid 1:1 and 5ml of hydrofluoric acid, steaming on an electric heating plate at a low temperature (less than 250 ℃) until the sample is dried, sweeping the precipitate into a ceramic crucible, continuously heating, burning the ceramic crucible in a high-temperature furnace at 950 ℃ and 1000 ℃ for 15 minutes under the condition that the ceramic crucible emits sulfur trioxide white smoke at 350-400 ℃, cooling to room temperature in a drier, weighing m2 (the mass of the precipitate and the ceramic crucible after hydrofluoric acid treatment),
the percentage of silica in the precipitate M2= (M1-M2) ÷ mass of the sample × 100%
The silica content in the sample = the sum of M1 + M2.
And (3) wrapping the mixture in the step 1 and the step 2 by using quantitative filter paper.
Step 2 the mixed flux used in step 3 and step 5 was made of 2.2g of anhydrous sodium carbonate and 0.8g of boric acid.
And 6, filtering the solution by using quantitative filter paper, placing little paper pulp in the middle of the quantitative filter paper, receiving the filtrate and the washing liquid during filtering by using a 250ml volumetric flask, wiping a surface dish by using glass with a rubber head, washing the glass rod and the beaker for 3-5 times by using hot water, and checking the filtrate to be neutral by using a pH test paper.
The content of the silicon dioxide is analyzed by the method and the steps, so that the error is reduced, the analysis speed is high, and the numerical value is more accurate.
Example II,
Melting for 15 minutes in the step (4) of the first embodiment, opening a furnace door, taking out a crucible, cooling to room temperature, obtaining a standard sample after the sample in the crucible is in a shape of a glass bead melt after high temperature and cooling, wherein the standard sample has certain mechanical strength and does not absorb water, and is completely dissolved by adding a hydrochloric acid (1+1) solution;
melting for 22 minutes, opening a furnace door, taking out the crucible, cooling to room temperature, obtaining a standard sample after the sample in the crucible is in a glass ball molten bead shape after high temperature and cooling, wherein the standard sample has certain mechanical strength and does not absorb water, and hydrochloric acid (1+1) solution is added for complete dissolution;
melting for 30 minutes, opening the furnace door, taking out the crucible, cooling to room temperature, obtaining a standard sample after the sample in the crucible is in a glass ball molten bead shape after high temperature and cooling, wherein the standard sample has certain mechanical strength and does not absorb water, and the standard sample is completely dissolved by adding a hydrochloric acid (1+1) solution.
In the step (5) of example one, the standard sample obtained in the step 4 was placed in a 250ml beaker, 40ml of hydrochloric acid (1+1) was added, and the beaker was heated on an electric furnace at 600 ℃ so that the temperature of the hydrochloric acid (1+1) solution in the beaker was raised to 90 ℃ and the standard sample was completely dissolved in 2 minutes and removed. Adding 20ml perchloric acid to the dissolved standard sample, covering a watch glass, putting the standard sample on a 700 ℃ electric furnace for heating and dehydration, and continuously refluxing for 10 minutes by emitting hydrochloric acid smoke when the temperature of the solution is increased to 110 ℃ and emitting concentrated white smoke by perchloric acid when the temperature of the solution is increased to 200 ℃ until the residue is pasty and taken down.
The standard sample obtained in step 4 was placed in a 250ml beaker, 40ml of hydrochloric acid (1+1) was added, and the beaker was heated on an electric furnace at about 600 ℃ so that the temperature of the hydrochloric acid (1+1) solution in the beaker was raised to 95 ℃ and the standard sample was completely dissolved in 2.5 minutes and removed. Adding 20ml perchloric acid to the dissolved standard sample, covering a watch glass, putting the standard sample on a 700 ℃ electric furnace for heating and dehydration, and continuously refluxing for 15 minutes by emitting hydrochloric acid smoke when the temperature of the solution is increased to 115 ℃ and emitting strong white smoke by perchloric acid when the temperature of the solution is increased to 205 ℃ until the residue is pasty and taken down.
And (3) putting the standard sample obtained in the step (4) into a 250ml beaker, adding 40ml of hydrochloric acid (1+1), heating the beaker on an electric furnace at the temperature of 600 ℃, raising the temperature of the hydrochloric acid (1+1) solution in the beaker to 100 ℃, and completely dissolving and removing the standard sample after 3 minutes. Adding 20ml perchloric acid to the dissolved standard sample, covering a watch glass, putting the standard sample on a 700 ℃ electric furnace for heating and dehydration, and continuously refluxing for 20 minutes by emitting hydrochloric acid smoke when the temperature of the solution is increased to 120 ℃ and emitting concentrated white smoke by perchloric acid when the temperature of the solution is increased to 210 ℃ until the residue is pasty and taken down.
In the step (7) of the first example, the precipitate and the filter paper obtained in the step 6 were transferred to a porcelain crucible, 2 drops of sulfuric acid (1: 1) were added dropwise, the mixture was dried in an electric furnace at a low temperature of 175 ℃, then the temperature was increased in a gradient manner to 640 ℃ to carbonize a certain amount of the filter paper until no smoke was generated and the filter paper could not catch fire, and then the mixture was transferred to a high temperature without closing the door and gradually increased from 700 ℃ to 900 ℃ to completely oxidize the carbon. Firing for 30 minutes, covering the porcelain crucible with a cover, and reserving a strip gap to enable air to flow back, moving the porcelain crucible into a high-temperature furnace at 950 ℃, firing for 30 minutes, taking out and cooling, weighing, and repeatedly firing until the constant weight m1 is equal to the mass of the sediment and the porcelain crucible before hydrofluoric acid treatment;
and (3) transferring the precipitate and the filter paper obtained in the step (6) into a ceramic crucible, dropwise adding 2 drops of sulfuric acid (1: 1), drying on an electric furnace at a low temperature of 175 ℃, then heating up to 645 ℃ in a gradient manner to carbonize the quantitative filter paper until no smoke exists and enable the filter paper to catch fire, and then moving into a furnace with a high temperature of no door, wherein the high temperature is gradually increased from 700 ℃ to 900 ℃ so as to completely oxidize the carbon. Firing for 30 minutes, covering the porcelain crucible with a cover, reserving a strip gap, enabling air to flow back, moving into a high-temperature furnace with the temperature of 975 ℃, firing for 30 minutes, taking out, cooling, weighing, and repeatedly firing until the constant weight m1 (the mass of the precipitate and the porcelain crucible before hydrofluoric acid treatment;
and (3) transferring the precipitate and the filter paper obtained in the step (6) into a ceramic crucible, dropwise adding 2 drops of sulfuric acid (1: 1), drying on an electric furnace at a low temperature of 150 ℃, then, heating up to 650 ℃ in a gradient manner to carbonize the quantitative filter paper until no smoke exists and the filter paper can not catch fire, and then, moving into a furnace with a high temperature without closing a door, and gradually heating up from 700 ℃ to 900 ℃ to completely oxidize the carbon. And (3) firing for 30 minutes, covering the porcelain crucible with a cover, reserving a strip gap, refluxing air, transferring the porcelain crucible into a high-temperature furnace at 1000 ℃, firing for 30 minutes, taking out the porcelain crucible, cooling, weighing, and repeatedly firing until the constant weight m1 is equal to the mass of the precipitate and the porcelain crucible before hydrofluoric acid treatment.
Claims (3)
1. A method of analyzing silica content, characterized by: adopting quantitative filter paper to hold samples, and preparing and analyzing filtrate and sediment, wherein the method comprises the following specific steps:
weighing a sample, wherein the mass of the sample is 0.2g and is accurate to 0.0001g of silica sand sample;
step (2), folding quantitative filter paper into a conical bag shape, filling 2g of mixed flux into a filter bag, and putting the step (1) into the filter bag to be fully and uniformly mixed with the mixed flux to obtain a sample;
step (3) covering a layer of 1g of mixed flux on the mixed sample obtained in the step (2), and folding and wrapping the filter bag to obtain a sample;
step (4), placing the sample obtained in the step (3) into a prepared graphite crucible, then placing the crucible into a high-temperature box type resistance furnace, gradually heating the crucible to 900 ℃ from low temperature, melting the crucible for 15-30 minutes, opening a furnace door, taking out the crucible, cooling the crucible to room temperature, and obtaining a standard sample, wherein the sample in the crucible is in the shape of a glass ball molten bead after high temperature and cooling, and the standard sample has certain mechanical strength and does not absorb water;
step (5), putting the standard sample obtained in the step (4) into a 250ml beaker, adding 40ml hydrochloric acid (1+1), heating the beaker on an electric furnace at about 600 ℃, raising the temperature of the hydrochloric acid (1+1) solution in the beaker to about 100 ℃, completely dissolving the standard sample for 2-3 minutes, taking off the standard sample, adding 20ml perchloric acid into the dissolved standard sample, covering a watch glass, heating and dehydrating the standard sample on an electric furnace at 700 ℃, rising the solution temperature to about 210 ℃ along with the rise of the temperature of the solution to about 120 ℃ to emit hydrochloric acid smoke, continuously refluxing the perchloric acid smoke for 10-20 minutes until the residue is pasty, folding the silicic acid out in a hydrogel state after the standard sample is heated and dehydrated at low temperature, adding 30ml hydrochloric acid (1+1) after the solution is slightly cooled, stirring, dissolving salts, adding hot water at about 80 ℃ to 150ml volume, dissolving the salt again, and taking out the solution after slight boiling to obtain a solution;
filtering the solution obtained in the step (5) by using medium-speed quantitative filter paper, checking the filtrate to be neutral by using a pH test, and measuring the content of silicon dioxide M1 in the filtrate by using a molybdenum blue absorption photometry;
step (7), transferring the precipitate and the filter paper obtained in the step (6) into a ceramic crucible, dropwise adding 2 drops of sulfuric acid (1: 1), drying, carbonizing and ashing at a low temperature of 100-150 ℃ on an electric furnace, then heating up to 640-650 ℃ in a gradient manner to carbonize the quantitative filter paper until no smoke exists and the filter paper can not catch fire, then moving into a furnace side with a high temperature of no door gradually heating up to 900 ℃ from 700 ℃ to completely oxidize the carbon, firing for 30 minutes, covering the ceramic crucible but reserving a strip gap to enable air to flow back and then moving into a 950-1000 ℃ high-temperature furnace, firing for 30 minutes, taking out, cooling, weighing and repeatedly firing until the mass of the precipitate and the ceramic crucible is equal to the mass of m1 hydrofluoric acid before treatment;
step (8), the sample obtained after the firing in the step (7) is completely swept into a polyvinyl fluoride crucible, a plurality of drops of water are used for wetting, 3 drops of sulfuric acid 1:1 and 5ml of hydrofluoric acid are added, the sample is steamed on an electric heating plate at the low temperature of less than 250 ℃ until the sample is dried, the sediment is completely swept into a ceramic crucible, the heating is continued, the heating temperature is 350-400 ℃, the ceramic crucible is fired for 15 minutes in a high-temperature furnace at 950-1000 ℃, the ceramic crucible is cooled to the room temperature in a dryer, the mass of the sediment and the ceramic crucible after the m2 hydrofluoric acid treatment is weighed,
the percentage of silica in the precipitate M2= (M1-M2) ÷ mass of the sample × 100%
The silica content in the sample = the sum of M1 + M2.
2. A method of analysing the silica content according to claim 1, characterized in that: in the steps 1 and 2, quantitative filter paper is adopted to be folded into a conical bag shape to wrap the sample.
3. A method of analysing the silica content according to claim 1, characterized in that: step 2 the mixed flux used in step 3 and step 5 was made of 2.2g of anhydrous sodium carbonate and 0.8g of boric acid.
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