CN118225542A - Method for detecting silicon dioxide content in limestone and dolomite - Google Patents
Method for detecting silicon dioxide content in limestone and dolomite Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 108
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 54
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 30
- 235000019738 Limestone Nutrition 0.000 title claims abstract description 27
- 239000006028 limestone Substances 0.000 title claims abstract description 27
- 239000010459 dolomite Substances 0.000 title claims abstract description 20
- 229910000514 dolomite Inorganic materials 0.000 title claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 77
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 61
- 238000002156 mixing Methods 0.000 claims abstract description 60
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000007788 liquid Substances 0.000 claims abstract description 34
- 238000002835 absorbance Methods 0.000 claims abstract description 22
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 17
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 17
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 17
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 17
- IMBKASBLAKCLEM-UHFFFAOYSA-L ferrous ammonium sulfate (anhydrous) Chemical compound [NH4+].[NH4+].[Fe+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O IMBKASBLAKCLEM-UHFFFAOYSA-L 0.000 claims abstract description 17
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 17
- 238000001816 cooling Methods 0.000 claims abstract description 15
- 238000005303 weighing Methods 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 239000002253 acid Substances 0.000 claims abstract description 8
- 238000009736 wetting Methods 0.000 claims abstract description 8
- 239000003513 alkali Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 111
- 239000000523 sample Substances 0.000 claims description 54
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 239000012153 distilled water Substances 0.000 claims description 19
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 230000037452 priming Effects 0.000 claims description 9
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 7
- 238000004458 analytical method Methods 0.000 claims description 7
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 7
- 238000004090 dissolution Methods 0.000 claims description 7
- 239000012488 sample solution Substances 0.000 claims description 7
- 229910052709 silver Inorganic materials 0.000 claims description 7
- 239000004332 silver Substances 0.000 claims description 7
- 239000012086 standard solution Substances 0.000 claims description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 229940010514 ammonium ferrous sulfate Drugs 0.000 claims description 5
- 239000002585 base Substances 0.000 claims description 2
- 238000011010 flushing procedure Methods 0.000 claims description 2
- -1 polytetrafluoroethylene Polymers 0.000 claims description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 21
- 238000012545 processing Methods 0.000 abstract description 8
- 229940079593 drug Drugs 0.000 abstract description 2
- 239000003814 drug Substances 0.000 abstract description 2
- 238000004364 calculation method Methods 0.000 description 6
- 238000009835 boiling Methods 0.000 description 5
- 238000011161 development Methods 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- 238000011895 specific detection Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 4
- 238000004737 colorimetric analysis Methods 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for detecting the content of silicon dioxide in limestone and dolomite, belonging to the technical field of analytical chemistry. Firstly accurately weighing a sample in a crucible, adding water for wetting, adding strong alkali, heating to be liquid for a plurality of minutes, transferring the crucible into a beaker after cooling, adding water into the crucible, adding dilute hydrochloric acid into the beaker, pouring the crucible into the beaker to enable the sample to be dissolved in acid, heating the solution to be boiled for a plurality of minutes, cooling, transferring into a volumetric flask, fixing the volume, transferring a certain amount of liquid to be measured into the volumetric flask, sequentially adding water and ammonium molybdate solution, uniformly mixing, keeping the temperature at 30-40 ℃, adding oxalic acid solution, uniformly mixing, immediately adding ferrous ammonium sulfate solution, fixing the volume, measuring the absorbance of the solution at 680nm of a spectrophotometer, finding the corresponding silicon dioxide content from a standard curve, and calculating the silicon dioxide content in the sample. The invention simplifies the processing steps of colorimetric detection of silicon dioxide in limestone and dolomite, reduces the use of medicines and improves the detection efficiency.
Description
Technical Field
The invention belongs to the technical field of analytical chemistry, and particularly relates to a method for detecting the content of silicon dioxide in limestone and dolomite.
Background
Limestone and dolomite are one of important auxiliary materials for sintering and steelmaking in the metallurgical industry, and have huge consumption in steel production. The main components of limestone and dolomite are carbonate, and also contain other components such as silicon dioxide. In the prior art, the detection of silicon dioxide in limestone and dolomite is generally carried out by adopting a gravimetric method and a colorimetric method. When the content of silicon dioxide in the limestone and dolomite is more than 2%, the method can be used for detecting by a weight method; when the content of silicon dioxide in the limestone and dolomite is more than 0.05% and less than 4%, the method can be used for colorimetric detection. When the colorimetric method is used for detecting the silicon dioxide in the limestone and the dolomite, a platinum crucible and a mixed flux are adopted to melt the sample in a high-temperature furnace, the sample treatment steps are complicated, the detection time is long, the used chemicals are more, the detection efficiency is low, the normal steel smelting is seriously affected, and the method for detecting the silicon dioxide content in the limestone and the dolomite, which has the advantages of simple treatment steps, low cost, rapid detection and accurate detection result, is urgently needed to be developed.
Disclosure of Invention
In view of the above, the invention aims to provide a method for detecting the content of silicon dioxide in limestone and dolomite, which simplifies the processing steps of colorimetry for detecting the silicon dioxide in limestone and dolomite, reduces the use of medicines and improves the detection efficiency.
The invention aims at realizing the following steps:
the invention provides a method for detecting the silicon dioxide content in limestone and dolomite, which comprises the following steps:
(1) Accurately weighing 0.1-0.5 g of sample in a crucible, adding 1-2 drops of water for wetting, adding 4-10 g of strong alkali, covering a crucible cover, heating to be liquid, keeping for 8-15 minutes, and cooling;
(2) Transferring the crucible in the step (1) into a beaker, adding water with the volume of 1/3-2/3 of the crucible into the crucible, adding 20-80 mL of diluted hydrochloric acid into the beaker, pouring the crucible into the beaker, heating, shaking the beaker to dissolve a sample into acid, flushing the crucible and a crucible cover with distilled water and flowing into the beaker, heating the sample solution to boil, keeping for 1-5 minutes, cooling to room temperature, transferring the solution into a volumetric flask, fixing the volume, and uniformly mixing to obtain a to-be-tested solution;
(3) Transferring 2-30 mL of the solution to be tested into a 100mL volumetric flask, adding 5-20 mL of water, adding 5-10 mL of ammonium molybdate solution, uniformly mixing, carrying out water bath heat preservation at 30-40 ℃ for 5-15 minutes, adding 20-30 mL of oxalic acid solution, uniformly mixing, immediately adding 5-10 mL of ferrous ammonium sulfate solution, uniformly mixing, standing for 10 minutes, fixing the volume, uniformly mixing, transferring part of the obtained solution to be tested into a 1cm cuvette, taking blank as a reference, measuring absorbance at 680nm of a spectrophotometer, obtaining the corresponding silicon dioxide content from a standard curve of silicon dioxide, and calculating the content of silicon dioxide in the sample.
Based on the technical scheme, further, the granularity of the sample in the step (1) is less than or equal to 0.125mm.
Based on the technical scheme, further, before analysis, the sample is baked for 1-3 hours at 105-110 ℃, and then is placed in a dryer to be cooled to room temperature.
Based on the technical scheme, the crucible in the step (1) further comprises a silver crucible and a polytetrafluoroethylene crucible.
Based on the above technical solution, further, the strong base in step (1) includes sodium hydroxide and potassium hydroxide.
Based on the technical scheme, further, the water in the step (1) and the step (2) comprises distilled water and deionized water.
Based on the technical scheme, further, the dilute hydrochloric acid in the step (2) is prepared from concentrated hydrochloric acid and water, wherein the volume ratio of the concentrated hydrochloric acid to the water is 1:1 to 1:2.
Based on the technical scheme, in the step (2), the volume of the volumetric flask is 100-500 mL.
Based on the technical scheme, further, the concentration of the ammonium molybdate solution in the step (3) is 2.5 to 5 weight percent, the concentration of the oxalic acid solution is 2 to 3 weight percent, and the concentration of the ferrous ammonium sulfate solution is 3 to 6 weight percent.
Based on the above technical solution, further, the manufacturing of the standard curve in the step (3) includes the following steps: weighing high-purity calcium carbonate, adding hydrochloric acid solution for dissolution, and preparing priming solution with the concentration of 0.5-2 mg/mL; respectively transferring a series of silica standard solutions with different volume concentrations of 100 mug/mL into 5-8 volumetric flasks with 100mL, adding 2-5 mL of priming solution, 0.8mL of hydrochloric acid, 5-20 mL of water and 5-10 mL of ammonium molybdate solution, uniformly mixing, carrying out water bath heat preservation at 30-40 ℃ for 5-15 minutes, adding 20-30 mL of oxalic acid solution, uniformly mixing, immediately adding 5-10 mL of ammonium ferrous sulfate solution, uniformly mixing, standing for 10 minutes, and fixing the volume to prepare a series of standard curve solutions; the standard curve solutions are respectively transferred into a cuvette of 1cm, the absorbance of the standard curve solutions is measured at 680nm of a spectrophotometer by taking a blank as a reference, the absorbance is taken as an ordinate, and the mass concentration is taken as an abscissa, so that a standard curve is drawn.
Based on the above technical solution, further, the formula used in the calculation of the silica content in the sample in step (3) is as follows:
Wherein: m 1 -the amount of silica is found from the standard curve in g;
m-is the sample amount, and the unit is g;
v-the volume of the liquid to be tested is determined in mL;
v 1 -the volume of the solution to be tested is taken in mL.
Compared with the prior art, the invention has the following beneficial effects:
1. The detection method has the advantages of simple sample processing steps, less chemical reagents, less influence on environment, high detection efficiency and low sample processing cost.
2. The detection result of the detection method provided by the invention is very close to the standard value of the sample, and the detection accuracy is high.
3. The detection method of the invention only needs laboratory basic equipment and is suitable for most laboratories.
Detailed Description
The following detailed description of the invention is provided in connection with examples, but the implementation of the invention is not limited thereto, and it is obvious that the examples described below are only some examples of the invention, and that it is within the scope of protection of the invention to those skilled in the art to obtain other similar examples without inventive faculty.
Example 1
Processing a limestone sample YSB14711-96 into a sample with granularity smaller than 0.125mm according to GB/T2007.2, drying for 2 hours at 105-110 ℃ before analysis, and cooling to room temperature in a dryer; performing a blank experiment along with the sample; the specific detection process is as follows:
Accurately weighing 0.1g (accurate to 0.0001 g) of the sample in a silver crucible, adding 1-2 drops of distilled water for wetting, adding 3g of sodium hydroxide, covering a crucible cover, placing the crucible on an electric furnace, heating to be in a liquid state, keeping for 8 minutes, and taking down. The crucible is placed in cold water for cooling, the crucible is moved into a beaker, distilled water is slowly added into the crucible for about half of the volume of the crucible, 30mL (the volume ratio of concentrated hydrochloric acid to deionized water is 1:2) of diluted hydrochloric acid is added into the beaker, the crucible is placed in the beaker, the crucible is heated at a low temperature, and the beaker is shaken to dissolve the sample in acid. The crucible and the lid were rinsed with distilled water. The sample solution was heated to boiling for about 2 to 3 minutes, removed, and cooled to room temperature. The solution was transferred to a 100mL volumetric flask, to volume, and mixed well. Is the liquid to be tested.
Transferring 10mL of the solution to be tested into a 100mL volumetric flask, adding 10mL of water and 5mL of ammonium molybdate solution (5%), uniformly mixing, preserving heat for 10 minutes in a water bath at 30-40 ℃, taking down, adding 20mL of oxalic acid solution (3%), uniformly mixing, immediately adding 5mL of ammonium ferrous sulfate solution (6%), and uniformly mixing. Standing for 10 minutes. Constant volume and uniform mixing.
Part of the chromogenic solution is transferred into a cuvette of 1cm, the absorbance is measured at 680nm of a spectrophotometer by taking a blank as a reference, and the corresponding silicon dioxide amount is obtained from a standard curve.
The standard curve is prepared as follows:
0.1g of high-purity calcium carbonate is weighed into a glass beaker, 10mL (the volume ratio of concentrated hydrochloric acid to deionized water is 1:1) of diluted hydrochloric acid solution is added for dissolution, a bottoming liquid is prepared, and the solution is transferred into a 100mL volumetric flask for constant volume.
Respectively transferring 100 mug/mL of silica standard solution 0mL, 1mL, 3mL, 5mL, 7mL and 10mL, placing in 6 volumetric flasks of 100mL, adding 2mL of priming solution, 0.8mL of hydrochloric acid, 10mL of water and 5mL of ammonium molybdate solution (5%), uniformly mixing, carrying out water bath heat preservation at 30-40 ℃ for 10 minutes, taking down, adding 20mL of oxalic acid solution (3%), uniformly mixing, immediately adding 5mL of ferrous ammonium sulfate solution (6%), and uniformly mixing. Standing for 10 minutes. Constant volume and uniform mixing. And preparing a standard curve color development liquid.
And (3) transferring part of the standard curve chromogenic liquid into a cuvette of 1cm, taking a blank as a reference, measuring the absorbance at 680nm of a spectrophotometer, taking the absorbance as an ordinate and the mass concentration as an abscissa, and drawing a standard curve.
The calculation formula of the silicon dioxide content in the limestone sample is as follows:
wherein: m 1 -finding the silicon dioxide amount from a standard curve, wherein the unit is g;
m-weighing the sample, wherein the unit is g;
v-the volume of the liquid to be tested is determined in mL;
v 1 -the volume of the solution to be tested is taken in mL.
The detection method of the invention detects that the silicon dioxide content in the limestone YSB14711-96 is 1.78 percent and the standard value is 1.80 percent. The error of the result measured by the method meets the requirement of the standard GB/T3286.
Example 2
Processing a limestone sample YSBC16703-01 into a sample with granularity smaller than 0.125mm according to GB/T2007.2, drying for 2 hours at 105-110 ℃ before analysis, and cooling to room temperature in a dryer; performing a blank experiment along with the sample; the specific detection process is as follows:
Accurately weighing 0.2g (accurate to 0.0001 g) of the sample in a silver crucible, adding 1-2 drops of distilled water for wetting, adding 4g of sodium hydroxide, covering a crucible cover, placing the crucible on an electric furnace, heating to be in a liquid state, keeping for 8 minutes, and taking down. The crucible is placed in cold water for cooling, the crucible is moved into a beaker, distilled water is slowly added into the crucible for about half of the volume of the crucible, 40mL (the volume ratio of concentrated hydrochloric acid to deionized water is 1:1) of diluted hydrochloric acid is added into the beaker, the crucible is placed in the beaker, the crucible is heated at a low temperature, and the beaker is shaken to dissolve the sample in acid. The crucible and the lid were rinsed with distilled water. The sample solution was heated to boiling for about 2 to 3 minutes, removed, and cooled to room temperature. The solution was transferred to a 200mL volumetric flask, to volume, and mixed well. Is the liquid to be tested.
Transferring 10mL of the solution to be tested into a 100mL volumetric flask, adding 10mL of water and 10mL of ammonium molybdate solution (2.5%), uniformly mixing, preserving heat in a water bath at 30-40 ℃ for 10 minutes, taking down, adding 30mL of oxalic acid solution (2%), uniformly mixing, immediately adding 10mL of ferrous ammonium sulfate solution (3%), and uniformly mixing. Standing for 10 minutes. Constant volume and uniform mixing.
Part of the chromogenic solution is transferred into a cuvette of 1cm, the absorbance is measured at 680nm of a spectrophotometer by taking a blank as a reference, and the corresponding silicon dioxide amount is obtained from a standard curve.
The standard curve is prepared as follows:
0.1g of high-purity calcium carbonate is weighed into a glass beaker, 10mL (the volume ratio of concentrated hydrochloric acid to deionized water is 1:1) of diluted hydrochloric acid solution is added for dissolution, a bottoming liquid is prepared, and the solution is transferred into a 100mL volumetric flask for constant volume.
Respectively transferring 100 mug/mL of silica standard solution 0mL, 1mL, 2mL, 4mL, 6mL and 8mL, placing in 6 volumetric flasks of 100mL, adding 5mL of priming solution, 0.8mL of hydrochloric acid, 10mL of water and 10mL of ammonium molybdate solution (2.5%), uniformly mixing, carrying out water bath at 30-40 ℃ for 10 minutes, taking down, adding 30mL of oxalic acid solution (2%), uniformly mixing, immediately adding 10mL of ferrous ammonium sulfate solution (3%), and uniformly mixing. Standing for 10 minutes. Constant volume and uniform mixing. And preparing a standard curve color development liquid.
And (3) transferring part of the standard curve chromogenic liquid into a cuvette of 1cm, taking a blank as a reference, measuring the absorbance at 680nm of a spectrophotometer, taking the absorbance as an ordinate and the mass concentration as an abscissa, and drawing a standard curve.
The calculation formula of the silicon dioxide content in the limestone sample is as follows:
wherein: m 1 -finding the silicon dioxide amount from a standard curve, wherein the unit is g;
m-weighing the sample, wherein the unit is g;
v-the volume of the liquid to be tested is determined in mL;
v 1 -the volume of the solution to be tested is taken in mL.
The detection method of the invention detects that the silicon dioxide content in the limestone sample YSBC16703-01 is 2.28% and the standard value is 2.24%. The error of the result measured by the method meets the requirement of the standard GB/T3286.
Example 3
Processing limestone sample YSBC28711-93 into a sample with granularity smaller than 0.125mm according to GB/T2007.2, drying at 105-110 ℃ for 2h before analysis, and cooling to room temperature in a dryer; performing a blank experiment along with the sample; the specific detection process is as follows:
Accurately weighing 0.4g (accurate to 0.0001 g) of the sample in a silver crucible, adding 1-2 drops of distilled water for wetting, adding 4g of sodium hydroxide, covering a crucible cover, placing the crucible on an electric furnace for heating to be in a liquid state, keeping for 8 minutes, and taking down. The crucible is placed in cold water for cooling, the crucible is moved into a beaker, distilled water is slowly added into the crucible for about half of the volume of the crucible, 60mL (the volume ratio of concentrated hydrochloric acid to deionized water is 1:1) of diluted hydrochloric acid is added into the beaker, the crucible is placed in the beaker, the crucible is heated at a low temperature, and the beaker is shaken to dissolve the sample in acid. The crucible and the lid were rinsed with distilled water. The sample solution was heated to boiling for about 2 to 3 minutes, removed, and cooled to room temperature. The solution was transferred to a 200mL volumetric flask, to volume, and mixed well. Is the liquid to be tested.
Transferring 5mL of the solution to be tested into a 100mL volumetric flask, adding 10mL of water and 10mL of ammonium molybdate solution (2.5%), uniformly mixing, preserving heat in a water bath at 30-40 ℃ for 10 minutes, taking down, adding 30mL of oxalic acid solution (2%), uniformly mixing, immediately adding 10mL of ferrous ammonium sulfate solution (3%), and uniformly mixing. Standing for 10 minutes. Constant volume and uniform mixing.
Part of the chromogenic solution is transferred into a cuvette of 1cm, the absorbance is measured at 680nm of a spectrophotometer by taking a blank as a reference, and the corresponding silicon dioxide amount is obtained from a standard curve.
The standard curve is prepared as follows:
0.2g of high-purity calcium carbonate is weighed into a glass beaker, 10mL (the volume ratio of concentrated hydrochloric acid to deionized water is 1:1) of diluted hydrochloric acid solution is added for dissolution, a bottoming liquid is prepared, and the solution is transferred into a 200mL volumetric flask for constant volume.
Respectively transferring 100 mug/mL of silica standard solution 0mL, 1mL, 2mL, 4mL, 6mL and 8mL, placing in 6 volumetric flasks of 100mL, adding 5mL of priming solution, adding 0.8mL of hydrochloric acid, 10mL of water and 10mL of ammonium molybdate solution (2.5%), uniformly mixing, carrying out water bath at 30-40 ℃ for 10 minutes, taking down, adding 30mL of oxalic acid solution (2%), uniformly mixing, immediately adding 10mL of ferrous ammonium sulfate solution (3%), and uniformly mixing. Standing for 10 minutes. Constant volume and uniform mixing. And preparing a standard curve color development liquid.
And (3) transferring part of the standard curve chromogenic liquid into a cuvette of 1cm, taking a blank as a reference, measuring the absorbance at 680nm of a spectrophotometer, taking the absorbance as an ordinate and the mass concentration as an abscissa, and drawing a standard curve.
The calculation formula of the silicon dioxide content in the limestone sample is as follows:
wherein: m 1 -finding the silicon dioxide amount from a standard curve, wherein the unit is g;
m-weighing the sample, wherein the unit is g;
v-the volume of the liquid to be tested is determined in mL;
v 1 -the volume of the solution to be tested is taken in mL.
The detection method of the invention detects that the silicon dioxide content in limestone samples YSBC28711-93 is 3.42% and the standard value is 3.40%. The error of the result measured by the method meets the requirement of the standard GB/T3286.
Example 4
Dolomite samples YSBC28721a-2013 are processed into samples with granularity smaller than 0.125mm according to GB/T2007.2, and are dried for 2 hours at 105-110 ℃ before analysis, and are cooled to room temperature in a dryer; performing a blank experiment along with the sample; the specific detection process is as follows:
accurately weighing 0.25g (accurate to 0.0001 g) of the sample in a silver crucible, adding 1-2 drops of distilled water for wetting, adding 5g of sodium hydroxide, covering a crucible cover, placing the crucible on an electric furnace, heating to be in a liquid state, keeping for 12 minutes, and taking down. The crucible is placed in cold water for cooling, the crucible is moved into a beaker, distilled water is slowly added into the crucible for about half of the volume of the crucible, 50mL (the volume ratio of concentrated hydrochloric acid to deionized water is 1:1) of diluted hydrochloric acid is added into the beaker, the crucible is placed in the beaker, the crucible is heated at a low temperature, and the beaker is shaken to dissolve the sample in acid. The crucible and the lid were rinsed with distilled water. The sample solution was heated to boiling for about 2 to 3 minutes, removed, and cooled to room temperature. Transferring the solution into a 250mL volumetric flask, fixing the volume, and uniformly mixing to obtain the solution to be tested.
Transferring 10mL of the solution to be tested into a 100mL volumetric flask, adding 10mL of water and 10mL of ammonium molybdate solution (2.5%), uniformly mixing, preserving heat in a water bath at 30-40 ℃ for 10 minutes, taking down, adding 30mL of oxalic acid solution (2%), uniformly mixing, immediately adding 10mL of ammonium ferrous sulfate solution (3%), uniformly mixing, standing for 10 minutes, fixing the volume, and uniformly mixing.
Part of the chromogenic solution is transferred into a cuvette of 1cm, the absorbance is measured at 680nm of a spectrophotometer by taking a blank as a reference, and the corresponding silicon dioxide amount is obtained from a standard curve.
The standard curve is prepared as follows:
0.2g of high-purity calcium carbonate is weighed into a glass beaker, 10mL (the volume ratio of concentrated hydrochloric acid to deionized water is 1:1) of diluted hydrochloric acid solution is added for dissolution, a bottoming liquid is prepared, and the solution is transferred into a 200mL volumetric flask for constant volume.
Respectively transferring 100 mug/mL of silica standard solution 0mL, 1mL, 2mL, 4mL, 6mL and 8mL, placing in 6 volumetric flasks of 100mL, adding 4mL of priming solution, adding 0.8mL of hydrochloric acid, 10mL of water and 10mL of ammonium molybdate solution (2.5%), uniformly mixing, carrying out water bath heat preservation at 30-40 ℃ for 10 minutes, taking down, adding 30mL of oxalic acid solution (2%), uniformly mixing, immediately adding 10mL of ferrous ammonium sulfate solution (3%), uniformly mixing, standing for 10 minutes, fixing volume and uniformly mixing. And preparing a standard curve color development liquid.
And (3) transferring part of the standard curve chromogenic liquid into a cuvette of 1cm, taking a blank as a reference, measuring the absorbance at 680nm of a spectrophotometer, taking the absorbance as an ordinate and the mass concentration as an abscissa, and drawing a standard curve.
The calculation formula of the silicon dioxide content in the limestone sample is as follows:
wherein: m 1 -finding the silicon dioxide amount from a standard curve, wherein the unit is g;
m-weighing the sample, wherein the unit is g;
v-the volume of the liquid to be tested is determined in mL;
v 1 -the volume of the solution to be tested is taken in mL.
The detection method of the invention detects that the content of silicon dioxide in dolomite samples YSBC28721a-2013 is 1.46%, and the standard value is 1.48%. The error of the result measured by the detection method meets the requirement of the standard GB/T3286.
Example 5
Processing dolomite sample BH0119-2 into a sample with granularity less than 0.125mm, drying at 105-110 ℃ for 2h before analysis, and cooling to room temperature in a dryer; performing a blank experiment along with the sample; the specific detection process is as follows:
Accurately weighing 0.5g (accurate to 0.0001 g) of the sample in a silver crucible, adding 1-2 drops of distilled water for wetting, adding 10g of sodium hydroxide, covering a crucible cover, placing the crucible on an electric furnace for heating to be in a liquid state, keeping for 15 minutes, and taking down. The crucible is placed in cold water for cooling, the crucible is moved into a beaker, distilled water is slowly added into the crucible for about half of the volume of the crucible, 80mL (the volume ratio of concentrated hydrochloric acid to deionized water is 1:1) of diluted hydrochloric acid is added into the beaker, the crucible is placed in the beaker, the crucible is heated at a low temperature, and the beaker is shaken to dissolve the sample in acid. The crucible and the lid were rinsed with distilled water. The sample solution was heated to boiling for about 2 to 3 minutes, removed, and cooled to room temperature. Transferring the solution into a 500mL volumetric flask, fixing the volume, and uniformly mixing to obtain the solution to be tested.
Transferring 10mL of the solution to be tested into a 100mL volumetric flask, adding 10mL of water and 10mL of ammonium molybdate solution (2.5%), uniformly mixing, preserving heat in a water bath at 30-40 ℃ for 10 minutes, taking down, adding 20mL of oxalic acid solution (3%), uniformly mixing, immediately adding 5mL of ammonium ferrous sulfate solution (6%), and uniformly mixing. Standing for 10 min, fixing volume, and mixing.
Part of the chromogenic solution is transferred into a cuvette of 1cm, the absorbance is measured at 680nm of a spectrophotometer by taking a blank as a reference, and the corresponding silicon dioxide amount is obtained from a standard curve.
The standard curve is prepared as follows:
0.5g of high-purity calcium carbonate is weighed into a glass beaker, 15mL (the volume ratio of concentrated hydrochloric acid to deionized water is 1:1) of diluted hydrochloric acid solution is added for dissolution, a bottoming liquid is prepared, and the solution is transferred into a 500mL volumetric flask for constant volume.
Respectively transferring 100 mug/mL of silica standard solution 0mL, 2mL, 4mL, 6mL, 8mL and 10mL, placing in 6 volumetric flasks of 100mL, adding 3mL of priming solution, 0.8mL of hydrochloric acid, 10mL of water and 10mL of ammonium molybdate solution (2.5%), uniformly mixing, carrying out water bath at 30-40 ℃ for 10 minutes, taking down, adding 20mL of oxalic acid solution (3%), uniformly mixing, immediately adding 5mL of ferrous ammonium sulfate solution (6%), and uniformly mixing. Standing for 10 min, fixing volume, and mixing. And preparing a standard curve color development liquid.
And (3) transferring part of the standard curve chromogenic liquid into a cuvette of 1cm, taking a blank as a reference, measuring the absorbance at 680nm of a spectrophotometer, taking the absorbance as an ordinate and the mass concentration as an abscissa, and drawing a standard curve.
The calculation formula of the silicon dioxide content in the limestone sample is as follows:
wherein: m 1 -finding the silicon dioxide amount from a standard curve, wherein the unit is g;
m-weighing the sample, wherein the unit is g;
v-the volume of the liquid to be tested is determined in mL;
v 1 -the volume of the solution to be tested is taken in mL.
The detection method of the invention detects that the content of silicon dioxide in dolomite sample BH0119-2 is 0.25%, and the standard value is 0.25%. The error of the result measured by the method meets the requirement of the standard GB/T3286.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (10)
1. A method for detecting the content of silicon dioxide in limestone and dolomite, which is characterized by comprising the following steps:
(1) Accurately weighing 0.1-0.5 g of sample in a crucible, adding 1-2 drops of water for wetting, adding 4-10 g of strong alkali, covering a crucible cover, heating to be liquid, keeping for 8-15 minutes, and cooling;
(2) Transferring the crucible in the step (1) into a beaker, adding water with the volume of 1/3-2/3 of the crucible into the crucible, adding 20-80 mL of diluted hydrochloric acid into the beaker, pouring the crucible into the beaker, heating, shaking the beaker to dissolve a sample into acid, flushing the crucible and a crucible cover with distilled water and flowing into the beaker, heating the sample solution to boil, keeping for 1-5 minutes, cooling to room temperature, transferring the solution into a volumetric flask, fixing the volume, and uniformly mixing to obtain a to-be-tested solution;
(3) Transferring 2-30 mL of the solution to be tested into a 100mL volumetric flask, adding 5-20 mL of water, adding 5-10 mL of ammonium molybdate solution, uniformly mixing, carrying out water bath heat preservation at 30-40 ℃ for 5-15 minutes, adding 20-30 mL of oxalic acid solution, uniformly mixing, immediately adding 5-10 mL of ferrous ammonium sulfate solution, uniformly mixing, standing for 10 minutes, fixing the volume, uniformly mixing, transferring part of the obtained solution to be tested into a 1cm cuvette, taking blank as a reference, measuring absorbance at 680nm of a spectrophotometer, obtaining the corresponding silicon dioxide content from a standard curve of silicon dioxide, and calculating the content of silicon dioxide in the sample.
2. The method according to claim 1, wherein the particle size of the sample in step (1) is less than or equal to 0.125mm, and the sample is baked at 105 to 110 ℃ for 1 to 3 hours before analysis, and then cooled to room temperature in a dryer.
3. The method of claim 1, wherein the crucible of step (1) comprises a silver crucible and a polytetrafluoroethylene crucible.
4. The method of claim 1, wherein the strong base in step (1) comprises sodium hydroxide and potassium hydroxide.
5. The method of claim 1, wherein the water in step (1) and step (2) comprises distilled water and deionized water.
6. The method of claim 1, wherein the diluted hydrochloric acid in step (2) is prepared from concentrated hydrochloric acid and water, and the volume ratio of the concentrated hydrochloric acid to the water is 1:1 to 1:2.
7. The method of claim 1, wherein the volumetric flask in step (2) has a volume of 100mL to 500mL.
8. The method according to claim 1, wherein the concentration of the ammonium molybdate solution in the step (3) is 2.5 to 5wt%, the concentration of the oxalic acid solution is 2 to 3wt%, and the concentration of the ferrous ammonium sulfate solution is 3 to 6wt%.
9. The method of claim 1, wherein the step (3) of creating the standard curve comprises the steps of: weighing high-purity calcium carbonate, adding hydrochloric acid solution for dissolution, and preparing priming solution with the concentration of 0.5-2 mg/mL; respectively transferring a series of silica standard solutions with different volume concentrations of 100 mug/mL into 5-8 volumetric flasks with 100mL, adding 2-5 mL of priming solution, 0.8mL of hydrochloric acid, 5-20 mL of water and 5-10 mL of ammonium molybdate solution, uniformly mixing, carrying out water bath heat preservation at 30-40 ℃ for 5-15 minutes, adding 20-30 mL of oxalic acid solution, uniformly mixing, immediately adding 5-10 mL of ammonium ferrous sulfate solution, uniformly mixing, standing for 10 minutes, and fixing the volume to prepare a series of standard curve solutions; the standard curve solutions are respectively transferred into a cuvette of 1cm, the absorbance of the standard curve solutions is measured at 680nm of a spectrophotometer by taking a blank as a reference, the absorbance is taken as an ordinate, and the mass concentration is taken as an abscissa, so that a standard curve is drawn.
10. The method of claim 1, wherein the formula used in step (3) to calculate the silica content of the sample is as follows:
Wherein: m 1 -the amount of silica is found from the standard curve in g;
m-is the sample amount, and the unit is g;
v-the volume of the liquid to be tested is determined in mL;
v 1 -the volume of the solution to be tested is taken in mL.
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