CN117330698A - Chemical analysis method for checking cement raw material composition - Google Patents
Chemical analysis method for checking cement raw material composition Download PDFInfo
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- CN117330698A CN117330698A CN202311051980.3A CN202311051980A CN117330698A CN 117330698 A CN117330698 A CN 117330698A CN 202311051980 A CN202311051980 A CN 202311051980A CN 117330698 A CN117330698 A CN 117330698A
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- 239000004568 cement Substances 0.000 title claims abstract description 29
- 238000009614 chemical analysis method Methods 0.000 title claims abstract description 17
- 239000002994 raw material Substances 0.000 title abstract description 23
- 239000000203 mixture Substances 0.000 title description 5
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 79
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 75
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 40
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000011591 potassium Substances 0.000 claims abstract description 39
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 39
- 239000001103 potassium chloride Substances 0.000 claims abstract description 39
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 39
- 239000002244 precipitate Substances 0.000 claims abstract description 31
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000007787 solid Substances 0.000 claims abstract description 21
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 20
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 19
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims abstract description 19
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 238000001914 filtration Methods 0.000 claims abstract description 16
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 239000004111 Potassium silicate Substances 0.000 claims abstract description 13
- 239000002253 acid Substances 0.000 claims abstract description 13
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 claims abstract description 13
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 13
- 229910052913 potassium silicate Inorganic materials 0.000 claims abstract description 13
- 238000005406 washing Methods 0.000 claims abstract description 12
- 229910000027 potassium carbonate Inorganic materials 0.000 claims abstract description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 9
- 238000004448 titration Methods 0.000 claims abstract description 9
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011698 potassium fluoride Substances 0.000 claims abstract description 7
- 235000003270 potassium fluoride Nutrition 0.000 claims abstract description 7
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 5
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 4
- 238000002844 melting Methods 0.000 claims abstract description 4
- 230000008018 melting Effects 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 37
- 239000012086 standard solution Substances 0.000 claims description 13
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 claims description 12
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000009835 boiling Methods 0.000 claims description 8
- 238000006386 neutralization reaction Methods 0.000 claims description 6
- 229910052697 platinum Inorganic materials 0.000 claims description 6
- WSPDUNQYYCIPFG-UHFFFAOYSA-M potassium ethanol chloride Chemical compound [Cl-].[K+].C(C)O WSPDUNQYYCIPFG-UHFFFAOYSA-M 0.000 claims description 5
- -1 potassium fluorosilicate Chemical compound 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 238000004458 analytical method Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 239000013049 sediment Substances 0.000 claims description 3
- 235000012054 meals Nutrition 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims 1
- 238000007689 inspection Methods 0.000 abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 abstract 1
- 238000001514 detection method Methods 0.000 description 9
- 239000002245 particle Substances 0.000 description 5
- 239000002910 solid waste Substances 0.000 description 5
- 238000001354 calcination Methods 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 239000002893 slag Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000004927 clay Substances 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000001304 sample melting Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
-
- 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
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Molecular Biology (AREA)
- Biophysics (AREA)
- Engineering & Computer Science (AREA)
- Biomedical Technology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a chemical analysis method for detecting components of cement raw materials, which comprises the steps of sample pretreatment; adding anhydrous potassium carbonate into a sample, performing a melting reaction to generate potassium silicate, cooling, and then placing into a plastic beaker; adding nitric acid into a plastic beaker to fully dissolve potassium silicate; adding potassium fluoride, standing and reacting to generate potassium fluosilicate precipitate; cooling to below 30 ℃, adding solid potassium chloride, and fully reacting to generate potassium fluosilicate precipitate; filtering the solution by using quick filter paper to obtain solid potassium chloride and potassium fluosilicate precipitate, and washing and dissolving the solid potassium chloride by using a potassium chloride solution to obtain the potassium fluosilicate precipitate; neutralizing residual acid in potassium fluosilicate precipitate in potassium chloride solution environment; hydrolyzing potassium fluosilicate precipitate into hydrogen fluoride and silicic acid; by usingSodium hydroxide titration was used to neutralize the hydrogen fluoride and the silica content of the sample was calculated based on the amount of sodium hydroxide used. The invention solves the problem of SiO in the existing cement raw material inspection method 2 Inaccurate inspection and low inspection efficiency.
Description
Technical Field
The invention belongs to the technical field of analysis and assay methods, and particularly relates to a chemical analysis method for detecting components of cement raw materials.
Background
In the cement industry, the inspection of cement raw materials basically implements the GB176-2017 detection standard of the cement chemistry analysis method, which is mainly aimed at the inspection of traditional clay raw materials and mine raw materials. With the rapid development of industry, the types of solid waste generated by different industries are more, and due to the 'inclusion' of cement on the treatment of large amount of solid waste and the requirements of cost reduction and synergy, a large amount of industrial waste residues enter the field of view of cement, and carbide slag, fly ash, steel slag, magnesium slag and the like are favored by the modern cement raw materials.
Aiming at the cement raw materials prepared by the existing bulk solid wastes, the traditional inspection method is time-consuming, and can cause inaccurate inspection and mislead the quality control precision of cement technicians. For example, in the course of carrying out the raw material SiO 2 In the inspection of (2), the traditional gravimetric method needs to be evaporated, filtered and calcined, and part of acid insoluble matters cannot be thoroughly dissolved, so that the insoluble matters are retained on the filter paper, and the insoluble matters remain in the filter paper in the calcination process, so that the detection value of the silicon dioxide is higher; however, the conventional capacity rule can increase a large amount of hydrochloric acid and constant volume, which results in long test time.
Disclosure of Invention
The invention aims to provide a chemical analysis method for detecting components of cement raw materials, which solves the problems of SiO in the existing cement raw material detection method 2 Inaccurate inspection and low inspection efficiency.
The technical scheme adopted by the invention is as follows: a chemical analysis method for inspecting components of a cement raw meal comprising the steps of:
step 1, sample pretreatment;
step 2, adding anhydrous potassium carbonate into the sample, performing a melting reaction to generate potassium silicate, cooling, and then placing into a plastic beaker;
step 3, adding nitric acid into the plastic beaker to fully dissolve potassium silicate; adding potassium fluoride, standing and reacting to generate potassium fluosilicate precipitate;
step 4, cooling the product obtained in the step 3 to below 30 ℃, and adding solid potassium chloride to fully react to generate potassium fluosilicate precipitate;
step 5, filtering the solution in the product obtained in the step 4 by using quick filter paper to obtain solid potassium chloride and potassium fluosilicate precipitate, and washing and dissolving the solid potassium chloride by using a potassium chloride solution to obtain the potassium fluosilicate precipitate;
step 6, neutralizing residual acid in potassium fluosilicate precipitation in a potassium chloride solution environment;
step 7, hydrolyzing the potassium fluosilicate precipitate obtained in the step 6 into hydrogen fluoride and silicic acid;
and 8, titrating the product obtained in the step 7 by using a sodium hydroxide standard solution to enable sodium hydroxide to completely neutralize hydrogen fluoride, and calculating the silicon dioxide content in the sample according to the dosage of the sodium hydroxide.
The present invention is also characterized in that,
the step 1 specifically comprises the following steps: weighing 0.2g of sample, placing into a platinum crucible, placing into a 950-1000 ℃ high temperature furnace for presintering for more than 5min, and taking out.
The step 2 is specifically as follows: adding 0.2-0.5g of anhydrous potassium carbonate into the sample obtained in the step 1, then placing the sample into a high-temperature furnace, burning for 15min for melt reaction to generate potassium silicate, cooling and placing the sample into a plastic beaker.
The adding amount of nitric acid in the step 3 is 10-15ml; the addition amount of potassium fluoride is 10-15ml, and the concentration is 150g/L.
And (4) adding solid potassium chloride in the step (4) and reacting for 15-20min.
The step 5 is specifically as follows: filtering by using quick filter paper, filtering the solution, and reserving solid potassium chloride and potassium fluosilicate sediment at the bottom of a plastic beaker cup; the plastic beaker is washed twice by using a potassium chloride solution with the concentration of 50g/L, the total amount of washing liquid is not more than 25ml, so that solid potassium chloride is dissolved, and the obtained potassium fluosilicate precipitate is filtered on filter paper.
The step 6 is specifically as follows: placing filter paper attached with potassium fluosilicate precipitate in a plastic beaker, and adding 10-15ml of potassium chloride-ethanol solution with the concentration of 50g/L and 1ml of phenolphthalein indicator solution with the concentration of 10g/L along the wall of the beaker; the filter paper was then unrolled and the solution was titrated with 0.1mol/L sodium hydroxide standard solution to neutralize residual acid that was not washed out, the filter paper was stirred and squeezed, and the walls of the cup were then scrubbed until the solution became red.
The step 7 is specifically as follows: 200ml of boiling water was added to a plastic beaker to hydrolyze the potassium fluorosilicate precipitate obtained in step 6 into hydrogen fluoride and silicic acid.
The step 8 is specifically as follows: and (3) titrating the product obtained in the step (7) to red by using a 0.1mol/L sodium hydroxide standard solution, and carrying out a neutralization reaction on sodium hydroxide and hydrogen fluoride, wherein the titration end point is red, so that the reaction of the hydrogen fluoride is proved to be complete.
The beneficial effects of the invention are as follows: according to the chemical analysis method for detecting the components of the cement raw material, the sample is dissolved more thoroughly in the sample melting process, the solution is clearer after dissolution, and the solution after dissolution is directly titrated, so that the detection time is shortened, the problems that part of insoluble matters are remained on filter paper in the prior art, the insoluble matters remain in the filter paper in the calcining process, the silicon dioxide detection value is higher and the titration is accurate are avoided.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
Example 1
The invention provides a chemical analysis method for checking components of cement raw materials, which comprises the following steps:
step 1, sample pretreatment, which is used for removing structural water and volatile gases; the method comprises the following steps: weighing 0.2g of sample, placing into a platinum crucible, placing into a 950-1000 ℃ high temperature furnace for presintering for more than 5min, and taking out.
Step 2, adding anhydrous potassium carbonate (K) into the sample 2 CO 3 ) The melting reaction produces potassium silicate (K) 2 SiO 3 ) The sample is melted more thoroughly by using strong alkali weak acid salt potassium carbonate, so that insoluble silicon dioxide (SiO) is converted into soluble siliconAcid salt, cooling and putting into a plastic beaker; the method comprises the following steps: adding 0.2-0.5g of anhydrous potassium carbonate into the sample obtained in the step 1, then placing the sample into a high-temperature furnace, burning for 15min for melt reaction to generate potassium silicate, cooling and placing the sample into a plastic beaker.
Step 3, potassium silicate reacts with excessive potassium ions and fluoride ions in nitric acid (HNO) medium to generate potassium fluosilicate (K) 2 SiF 6 ) And (5) precipitation. Adding 10-15ml of nitric acid into a plastic beaker to fully dissolve potassium silicate; then 10-15ml of potassium fluoride (KF) with the concentration of 150g/L is added for standing reaction to generate potassium fluosilicate precipitate.
And 4, cooling the product obtained in the step 3 to below 30 ℃, adding potassium chloride (KCl) particles, carefully stirring, crushing large particles, and saturating the potassium chloride and separating out 1-3g of potassium chloride. The reaction of potassium fluoride and potassium silicate in nitric acid medium belongs to exothermic reaction, the reaction is more thorough by lowering the temperature, and the hydrolysis of potassium fluosilicate can be restrained by adding potassium chloride particles, so that the reaction is more thorough. Placing the mixture for reaction for 15-20min after the temperature is lower than 30 ℃ so that the generation reaction of potassium fluosilicate precipitate is thoroughly carried out.
Step 5, filtering the solution in the product obtained in the step 4 by using quick filter paper to obtain solid potassium chloride and potassium fluosilicate precipitate, and washing and dissolving the solid potassium chloride by using a potassium chloride solution to obtain the potassium fluosilicate precipitate; the method comprises the following steps: filtering by using quick filter paper, filtering the solution, and reserving solid potassium chloride and potassium fluosilicate sediment at the bottom of a plastic beaker cup; the plastic beaker is washed twice by using a potassium chloride solution with the concentration of 50g/L, the total amount of washing liquid is not more than 25ml, so that solid potassium chloride is dissolved, and the obtained potassium fluosilicate precipitate is filtered on filter paper. The filtering time can be shortened by both rapid filter paper filtration and control of the total washing amount, the dissociation time of potassium fluosilicate is reduced, and inaccurate detection is avoided.
Step 6, neutralizing residual acid in potassium fluosilicate precipitation in a potassium chloride solution environment; the method comprises the following steps: placing filter paper attached with potassium fluosilicate precipitate in a plastic beaker, adding 10-15ml of potassium chloride-ethanol solution with the concentration of 50g/L and 1ml of phenolphthalein indicator solution with the concentration of 10g/L along the wall of the beaker, and inhibiting hydrolysis of potassium fluosilicate in the subsequent neutralization process by adopting the potassium chloride-ethanol solution; the filter paper was then unrolled and the solution was titrated with 0.1mol/L sodium hydroxide standard solution to neutralize residual acid that was not washed out, the filter paper was stirred and squeezed, the walls of the cup were then scrubbed until the solution appeared reddish, thereby completely neutralizing residual acid on the filter paper and in the beaker.
Step 7, hydrolyzing the potassium fluosilicate precipitate obtained in the step 6 into Hydrogen Fluoride (HF) and silicic acid (H SiO); the method comprises the following steps: adding 200ml of boiling water into a plastic beaker to hydrolyze the potassium fluosilicate precipitate obtained in the step 6 into hydrogen fluoride and silicic acid, wherein the boiling water is boiled and then is neutralized by a sodium hydroxide standard solution until the phenolphthalein is reddish, and after the boiling water is added, the potassium fluosilicate is hydrolyzed into the hydrogen fluoride and the silicic acid, and the solution turns white.
Step 8, titrating the product obtained in the step 7 by using a sodium hydroxide (NaOH) standard solution to completely neutralize hydrogen fluoride by using sodium hydroxide, and calculating the silicon dioxide content in the sample according to the using amount of the sodium hydroxide; the method comprises the following steps: and (3) titrating the product obtained in the step (7) to reddish color by using a 0.1mol/L sodium hydroxide standard solution, and carrying out a neutralization reaction on sodium hydroxide and hydrogen fluoride, wherein the titration end point is reddish color, so that the reaction of the hydrogen fluoride is proved to be complete. (the three colors of the neutralization water, the residual acid and the titration end point need to be kept consistent, so as to avoid titration errors)
In the above manner, the chemical analysis method for inspecting the components of cement raw materials of the present invention is based on K 2 SiF 6 The basic principle of SiO measurement by the capacity method is as follows:
SiO 3 2- +6F - +6H + →SiF 6 2- +3H 2 O
SiF 6 2- +2K + →K 2 SiF 6 ↓
K 2 SiF 6 ↓+3H 2 o (heat) →2KF+H 2 SiO 3 +4HF
HF+NaOH＝NaF+H 2 O
But differs therefrom as shown in table 1:
TABLE 1 comparison of the method of the invention with the prior art test methods
The potassium carbonate adopted in the sample melting process is stronger in alkalinity and more thoroughly reacts with the sample, so that the sample is more thoroughly dissolved, and the solution after dissolution is more clear. The dissolved solution is directly titrated, so that the detection time is shortened, compared with the traditional weight method, the steps of evaporating, filtering and calcining are omitted, the problem that part of insoluble matters are remained on filter paper in the prior art, so that the insoluble matters remain as silicon dioxide in the calcining process of the filter paper is avoided, the problem that the detection value of the silicon dioxide is higher is solved, and the titration is accurate; compared with the traditional capacity method, the method omits the steps of constant volume and cooling, greatly shortens the inspection time, and avoids the problem of inaccurate inspection caused by long time.
Example 2
a. Weighing a 0.2 sample, placing the sample into a platinum crucible, then placing the platinum crucible into a high-temperature furnace with the temperature of 950-1000 ℃ for presintering for 5min, and then taking out the platinum crucible. Adding 0.2-0.5g anhydrous potassium carbonate, burning in a high temperature furnace for 15min, taking out, cooling, and placing in a plastic beaker. 12ml of nitric acid and 10ml of potassium fluoride (150 g/L) were added, and the mixture was allowed to stand. Cooling to below 30deg.C, adding potassium chloride particles, stirring, crushing large particles, and saturated and small amount of potassium chloride is separated out.
b. Placing at a temperature less than 30deg.C for 15-20min, filtering with rapid filter paper, filtering, collecting solid potassium chloride and precipitate at the bottom of cup, washing plastic cup with potassium chloride (50 g/L) solution for 2 times, dissolving solid potassium chloride during washing, and keeping the total volume of washing liquid not more than 25ml.
c. The filter paper was removed and placed in a beaker, and 10ml of potassium chloride-ethanol solution 50g/L and 1ml of phenolphthalein indicator solution (10 g/L) were added along the wall of the beaker.
d. The filter paper was unrolled, the unwashed acid was neutralized by dropping a standard solution of 0.1mol/L sodium hydroxide into a constant volume, carefully stirred, pressed, triturated and the walls of the cup were then scrubbed until the solution became reddish (filtration, washing, neutralization of residual acid should be rapid to prevent precipitation and dissolution of potassium fluorosilicate).
e. 200ml of boiling water was added, and after boiling, the mixture was neutralized with a sodium hydroxide standard solution to a boiling water in which phenolphthalein was reddish.
f. Titration was performed with 0.1mol/L sodium hydroxide standard solution to reddish.
Example 3
SiO in raw material 2 Content determination method precision verification, for SiO in raw material 2 The content was measured and the analysis of the measured data is shown in Table 2.
TABLE 2 SiO in raw materials 2 Method precision verification data
As is clear from Table 2, siO in the raw material 2 The content is 0.10% extremely poor in 6 times of measurement results, 0.10% meets the requirements within the range of the repeatability error +/-0.20%, and SiO in the raw material is 2 The content results are reliable. The method solves the problem that the traditional clay raw material inspection method is not applicable to industrial solid waste detection, solves the problem that the cement industry utilizes industrial solid waste as raw material ingredients accurately, and has substantial guiding significance.
Claims (9)
1. A chemical analysis method for inspecting components of a cement raw meal, comprising the steps of: step 1, sample pretreatment; step 2, adding anhydrous potassium carbonate into the sample, performing a melting reaction to generate potassium silicate, cooling, and then placing into a plastic beaker; step 3, adding nitric acid into the plastic beaker to fully dissolve potassium silicate; adding potassium fluoride, standing and reacting to generate potassium fluosilicate precipitate; step 4, cooling the product obtained in the step 3 to below 30 ℃, and adding solid potassium chloride to fully react to generate potassium fluosilicate precipitate; step 5, filtering the solution in the product obtained in the step 4 by using quick filter paper to obtain solid potassium chloride and potassium fluosilicate precipitate, and washing and dissolving the solid potassium chloride by using a potassium chloride solution to obtain the potassium fluosilicate precipitate; step 6, neutralizing residual acid in potassium fluosilicate precipitation in a potassium chloride solution environment; step 7, hydrolyzing the potassium fluosilicate precipitate obtained in the step 6 into hydrogen fluoride and silicic acid; and 8, titrating the product obtained in the step 7 by using a sodium hydroxide standard solution to enable sodium hydroxide to completely neutralize hydrogen fluoride, and calculating the silicon dioxide content in the sample according to the dosage of the sodium hydroxide.
2. The chemical analysis method for inspecting components of raw cement according to claim 1, wherein said step 1 is specifically: weighing 0.2g of sample, placing into a platinum crucible, placing into a 950-1000 ℃ high temperature furnace for presintering for more than 5min, and taking out.
3. The chemical analysis method for inspecting components of raw cement according to claim 1, wherein said step 2 is specifically: adding 0.2-0.5g of anhydrous potassium carbonate into the sample obtained in the step 1, then placing the sample into a high-temperature furnace, burning for 15min for melt reaction to generate potassium silicate, cooling and placing the sample into a plastic beaker.
4. The chemical analysis method for inspecting components of raw cement according to claim 1, wherein the nitric acid is added in an amount of 10 to 15ml in the step 3; the addition amount of potassium fluoride is 10-15ml, and the concentration is 150g/L.
5. The chemical analysis method for inspecting components of raw cement according to claim 1, wherein the step 4 is carried out for 15 to 20 minutes after adding solid potassium chloride.
6. The chemical analysis method for inspecting components of raw cement according to claim 1, wherein said step 5 is specifically: filtering by using quick filter paper, filtering the solution, and reserving solid potassium chloride and potassium fluosilicate sediment at the bottom of a plastic beaker cup; the plastic beaker is washed twice by using a potassium chloride solution with the concentration of 50g/L, the total amount of washing liquid is not more than 25ml, so that solid potassium chloride is dissolved, and the obtained potassium fluosilicate precipitate is filtered on filter paper.
7. The chemical analysis method for inspecting components of raw cement according to claim 6, wherein said step 6 is specifically: placing filter paper attached with potassium fluosilicate precipitate in a plastic beaker, and adding 10-15ml of potassium chloride-ethanol solution with the concentration of 50g/L and 1ml of phenolphthalein indicator solution with the concentration of 10g/L along the wall of the beaker; the filter paper was then unrolled and the solution was titrated with 0.1mol/L sodium hydroxide standard solution to neutralize residual acid that was not washed out, the filter paper was stirred and squeezed, and the walls of the cup were then scrubbed until the solution became red.
8. The method for chemical analysis of components of raw cement according to claim 7, wherein said step 7 is specifically: 200ml of boiling water was added to a plastic beaker to hydrolyze the potassium fluorosilicate precipitate obtained in step 6 into hydrogen fluoride and silicic acid.
9. The chemical analysis method for inspecting components of raw cement according to claim 1, wherein said step 8 is specifically: and (3) titrating the product obtained in the step (7) to red by using a 0.1mol/L sodium hydroxide standard solution, and carrying out a neutralization reaction on sodium hydroxide and hydrogen fluoride, wherein the titration end point is red, so that the reaction of the hydrogen fluoride is proved to be complete.
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| CN202311051980.3A CN117330698A (en) | 2023-08-21 | 2023-08-21 | Chemical analysis method for checking cement raw material composition |
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| CN202311051980.3A CN117330698A (en) | 2023-08-21 | 2023-08-21 | Chemical analysis method for checking cement raw material composition |
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