CN116067753A - Sample melting method for measuring silicon content in ferrosilicon by perchloric acid dehydration gravimetric method - Google Patents
Sample melting method for measuring silicon content in ferrosilicon by perchloric acid dehydration gravimetric method Download PDFInfo
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- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 51
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 27
- 239000010703 silicon Substances 0.000 title claims abstract description 27
- 229910000519 Ferrosilicon Inorganic materials 0.000 title claims abstract description 21
- 230000018044 dehydration Effects 0.000 title claims abstract description 19
- 238000006297 dehydration reaction Methods 0.000 title claims abstract description 19
- 238000001304 sample melting Methods 0.000 title claims abstract description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 42
- 230000004907 flux Effects 0.000 claims abstract description 18
- 238000002844 melting Methods 0.000 claims abstract description 13
- 230000008018 melting Effects 0.000 claims abstract description 13
- 238000005406 washing Methods 0.000 claims abstract description 12
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 8
- 239000000956 alloy Substances 0.000 claims abstract description 8
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 9
- 239000002244 precipitate Substances 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- 238000010306 acid treatment Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 238000010000 carbonizing Methods 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 abstract description 12
- 238000003763 carbonization Methods 0.000 abstract description 11
- 238000001514 detection method Methods 0.000 abstract description 9
- 239000000203 mixture Substances 0.000 abstract description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract description 3
- 238000005485 electric heating Methods 0.000 abstract description 3
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 abstract description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 10
- 229910052697 platinum Inorganic materials 0.000 description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 239000011521 glass Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 239000006210 lotion Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000000779 smoke Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 238000005201 scrubbing Methods 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000009628 steelmaking Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- SOIFLUNRINLCBN-UHFFFAOYSA-N ammonium thiocyanate Chemical compound [NH4+].[S-]C#N SOIFLUNRINLCBN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- JRACIMOSEUMYIP-UHFFFAOYSA-N bis($l^{2}-silanylidene)iron Chemical compound [Si]=[Fe]=[Si] JRACIMOSEUMYIP-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000003670 easy-to-clean Effects 0.000 description 1
- -1 iron (nickel) ions Chemical class 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 238000007619 statistical method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- 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
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a sample melting method for measuring the silicon content in ferrosilicon alloy by a perchloric acid dehydration gravimetric method, which adopts sodium hydroxide flux to replace a sodium carbonate-sodium peroxide mixed flux melting sample, thereby realizing the purpose that the sample cannot be boiled and splashed in the process of melting the sample by an electric heating plate and a muffle furnace. The dehydration effect and the recovery rate are improved by reducing the adding amount of perchloric acid, the proper sample melting temperature is adjusted, the sample loss caused by the mixture of the flux and the sample after being splashed in a high-temperature furnace is prevented, the dehydration rate after the silicon is converted into silicic acid is improved, and the washing time of chloride ions is reduced. The carbonization temperature of the filter paper is adjusted to ensure complete carbonization, thereby improving the analysis accuracy. The sample melting method has the advantages that the analysis precision of the detection result is good, the analysis accuracy meets the production requirement, and the national standard requirement is met.
Description
Technical Field
The invention belongs to the technical field of chemical analysis, and particularly relates to a sample melting method for measuring the silicon content in ferrosilicon alloy by a perchloric acid dehydration gravimetric method.
Background
Ferrosilicon alloy is used as deoxidizer and alloy additive in steelmaking smelting, and in order to obtain steel with qualified chemical components and ensure the quality of the steel, deoxidization must be carried out in the final stage of steelmaking smelting, and ferrosilicon is relatively expensive, so that accurate detection of ferrosilicon content is very important. The laboratory usually adopts a powder tabletting method to measure, but the content of a calibration standard sample is required to be verified, and a sample melting method is clear in GB/T4333.1-2019 'perchloric acid dehydration weight method for measuring silicon iron silicon content and potassium fluosilicate capacity method', but sodium carbonate-sodium peroxide mixed flux given in the standard is easy to bumping in the actual test process to cause sample splashing, so that test failure or detection result is greatly lower, and the whole test operation is difficult to master. Therefore, it is necessary to study a new sample melting method.
Disclosure of Invention
The invention aims to provide a sample melting method for measuring the silicon content in ferrosilicon by a perchloric acid dehydration gravimetric method.
The invention aims to realize the method for measuring the silicon content in the ferrosilicon by a perchloric acid dehydration gravimetric method, which adopts sodium hydroxide solid as a flux to melt a sample, and comprises the following specific steps: mixing 0.2000-0.3000g of sample with 3g of sodium hydroxide solid flux, baking for 50-60 minutes at 200-300 ℃ by using an electric hot plate, melting for 5-10 minutes at 340-360 ℃, and then gradually heating to 640-660 ℃ to melt for 14-20 minutes.
The principle of the invention is as follows:
1. according to the invention, sodium hydroxide solid is adopted to replace sodium carbonate-sodium peroxide mixed flux, the sodium hydroxide solid is baked for 50-60 minutes at 200-300 ℃ and then melted for 5-10 minutes at 350 ℃ and then gradually heated to 650 ℃ to be melted for 15 minutes, so that the moisture contained in the sodium hydroxide flux is baked to be nearly dry, the baking and melting temperatures are gradual, the whole melting process flux and sample mixture cannot be subjected to bumping splashing, the sodium hydroxide melting sample is more complete than sodium carbonate-sodium peroxide, the leaching effect is better, the nickel crucible is easy to clean, and a foundation is laid for the accuracy of test results;
2. under the condition of the same sample amount, the more the perchloric acid is added, the better the dehydration effect is, but the more the chloridion is brought into the filtrate when the perchloric acid is excessively added, the longer the time of the lotion is, the invention reduces the volume of perchloric acid added per gram of sample, the silicon content in the filtrate is quite stable and tends to be stable compared with the adding of 80ml of perchloric acid when 60ml of perchloric acid is added into 0.3 gram of sample, compared with the standard, the method only needs the chloridion of the lotion, and the lotion time is reduced from about 10 hours of 80ml to 7-8 hours.
3. The carbonization temperature before firing the filter paper after filtering and drying is particularly important, when the carbonization temperature is directly 600 ℃, substances generated by the excessive carbonization temperature are fired at a high temperature, and a small amount of black small particles are generated by volatilizing and firing hydrofluoric acid, so that the final detection result is low. According to the invention, the sample is ashed by burning at 400-500 ℃ for 5 minutes and then slowly heating to 1100 ℃ for burning.
The beneficial effects of the invention are as follows:
1. the invention adopts sodium hydroxide flux to replace sodium carbonate-sodium peroxide mixed flux to melt the sample, thereby realizing the purpose that the sample cannot be boiled and splashed in the process of melting the sample by the electric heating plate and the muffle furnace. The dehydration effect is improved and the recovery rate is improved by reducing the adding amount of perchloric acid; the proper melting sample temperature is adjusted, so that the sample loss caused by the splashing of the flux and the sample mixture in a high-temperature furnace is prevented, the dehydration rate after the silicon is converted into silicic acid is improved, and the washing time of chloride ions is reduced.
2. According to the method, the carbonization temperature of the filter paper is adjusted, so that the carbonization is complete, and the analysis accuracy is improved.
3. The sample melting method has the advantages that the analysis precision of the detection result is good, the analysis accuracy meets the production requirement, and the national standard requirement is met.
Detailed Description
The invention is further illustrated, but is not limited in any way, by the following examples, and any alterations or substitutions based on the teachings of the invention are within the scope of the invention.
The invention relates to a sample melting method for measuring the silicon content in ferrosilicon by a perchloric acid dehydration gravimetric method, which adopts sodium hydroxide solid as a flux to melt a sample, and comprises the following specific steps: mixing 0.2000-0.3000g of sample with 3g of sodium hydroxide solid flux, baking for 50-60 minutes at 200-300 ℃ by using an electric hot plate, melting for 5-10 minutes at 340-360 ℃, and then gradually heating to 640-660 ℃ to melt for 14-20 minutes.
The invention also provides a method for measuring the silicon content in the ferrosilicon based on the sample melting method, which is realized by the following steps: and (3) acidifying the fused sample by hydrochloric acid, dehydrating by perchloric acid, filtering and washing, carbonizing and burning the precipitate in a high-temperature furnace at 400-500 ℃ for 5-7 minutes, slowly heating to 1100 ℃ and burning for 30 minutes to constant quantity, and finally calculating the mass fraction of silicon by using the mass difference before and after hydrofluoric acid treatment.
In the perchloric acid dehydration step, perchloric acid was added in a volume of 60mL.
In the filtering and washing step, the washing time is 7-8h.
Example 1
1. Weighing a 0.3000g ferrosilicon sample (accurate to 0.0001 g), placing the ferrosilicon sample in a nickel crucible which is filled with 3g of sodium hydroxide in advance, placing the crucible on a low-temperature electric heating plate with the voltage of 100V (about 300 ℃), slowly heating for about 50 minutes, and baking to dry water; covering the crucible cover (with a gap), melting at 350 deg.C for about 5min, slowly heating to 650 deg.C, melting for 15min, and taking out.
2. After dipping and washing the bottom and the outer wall of the crucible with water, placing the crucible in a 500mL glass beaker, adding 40mL of hot dilute hydrochloric acid (5+95) for leaching, after the reaction is stopped, scrubbing the crucible with a glass rod sleeved with a silicone tube, and washing the crucible and the cover with hot water.
3. 60mL of perchloric acid was added, placed on a hot plate, heated to smoke the perchloric acid and refluxed for a period of time (about 15 minutes) until the residue was viscous, removed, and cooled. 20mL of hydrochloric acid (1+1) was added along the wall of the cup, 100mL of hot water (80 ℃ above) was added, and the salt was dissolved by stirring.
4. Filtering the mixture in a 500mL conical flask with medium-speed quantitative filter paper while the mixture is hot, carefully scrubbing the glass rod and the cup wall, cleaning the beaker and the glass rod with hot hydrochloric acid (5+95), washing the precipitate for 6-8 times until no iron (nickel) ions exist, and checking the precipitate with an ammonium thiocyanate solution (50 g/L). Then, the mixture was washed with hot water until no chloride ion was present, and was inspected with a silver nitrate solution (20 g/L). The filter paper and the precipitate were retained.
5. The filtrate and the washing solution were transferred to a beaker for initial dehydration, and when the solution was evaporated to about 100mL under heating, 20mL of perchloric acid was added thereto, and the dehydration with perchloric acid was repeated.
6. The twice precipitate together with the filter paper is placed in a platinum crucible and is placed on an electric hot plate to be baked to be nearly dry. The filter paper was ashed at 450 ℃ with careful heating for about 5 minutes. Gradually heating to ash, slowly heating muffle furnace to 1100deg.C, burning for 30min, taking out, cooling, placing in a dryer, cooling to room temperature, weighing, and repeatedly burning to constant weight (m) 1 ）。
7. The sample is moistened by a plurality of drops of water in a crucible, 4 drops of sulfuric acid (1+1) and 6mL of hydrofluoric acid are added, the crucible is placed on an electric plate or a low-temperature electric furnace, the mixture is evaporated until the smoke of sulfuric acid is generated, 4mL of hydrofluoric acid is added again, and the mixture is heated and evaporated continuously until the smoke of sulfuric acid is generated. Burning crucible in 1100 deg.c furnace for 30min, taking out, cooling to room temperature, weighing, and burning repeatedly to constant weight (m) 2 ）。
8. Blank test
A blank test was performed along with the sample.
9. Calculation and representation of results
9.1 Calculation of silicon content
The following is calculatedSilicon content omega in sample Si Expressed as mass fraction (%);
wherein:
m 1 -mass of platinum crucible and precipitate in grams (g) before hydrofluoric acid treatment;
m 2 -the mass of platinum crucible and residue after hydrofluoric acid treatment in grams (g);
m 3 -mass of platinum crucible and blank with sample before hydrofluoric acid treatment in grams (g);
m 4 -the mass of the platinum crucible and the blank with the sample after hydrofluoric acid treatment in grams (g);
m-sample mass in grams (g);
0.4674-conversion factor of silicon dioxide to silicon.
9.2 Representation of results
And if the absolute value of the difference value of the two independent analysis results of the same sample is not greater than the repeatability limit r, taking an arithmetic average value as an analysis result. If the absolute value of the difference between the two independent analysis results is larger than the repeatability limit r, the measurement times are added according to the rule of the annex A, and the analysis result is determined.
The analysis results refine the values to approximately two digits. The precision of the data was determined according to prior art statistical methods, see table 1.
Under the repeatability condition, the absolute difference value of the obtained two independent test results is not more than the repeatability limit r, and is not more than 5% when the absolute difference value is more than the repeatability limit r.
Under the condition of reproducibility, the absolute difference value of the obtained two independent test results is not more than the reproducibility limit R, and is not more than 5 percent.
TABLE 1 precision
Example 2
The method is the same as in example 1, except that in step 1, after baking at 200 ℃ for 60 minutes by a hot plate, melting at 340 ℃ for 10 minutes, and then gradually heating to 640 ℃ for melting for 20 minutes;
in the step 4, the filter paper and the precipitate are put into a platinum crucible for drying, and then are placed into a high-temperature furnace at 400 ℃ for carbonization and burning for 7 minutes, and then are slowly heated to 1100 ℃ for burning for 30 minutes.
Example 3
The method was the same as in example 1 except that in step 1, the temperature was gradually increased to 660℃for 14 minutes after being baked on a 300℃electric plate for 60 minutes and then being melted at 360℃for 5 minutes;
in the step 4, the filter paper and the precipitate are put into a platinum crucible for drying, and then are placed into a high-temperature furnace with the temperature of 500 ℃ for carbonization and burning for 5 minutes, and then are slowly heated to the temperature of 1100 ℃ for burning for 30 minutes.
Comparative example 1 the silicon content in ferrosilicon alloy was determined according to GB/T4333.1-2019 method for determination of ferrosilicon content by perchloric acid dehydration gravimetric method and Potassium fluosilicate Capacity method.
Comparative example 2
The procedure is as in example 1, except that the flux added in step 1 is sodium peroxide-sodium carbonate.
Comparative example 3
The procedure is as in example 1, except that the volume of perchloric acid added in step 3 is 40mL.
Comparative example 4
The procedure is as in example 1, except that the volume of perchloric acid added in step 3 is 50mL.
Comparative example 5
The procedure is as in example 1, in step 6, the twice precipitated, together with the filter paper, is placed in a platinum crucible and dried on an electric hot plate. The filter paper was ashed at 650 ℃ with careful heating for about 5 minutes. Gradually heating to ash, slowly heating muffle furnace to 1100deg.C, burning for 30min, taking out, cooling, placing in a dryer, cooling to room temperature, weighing, and repeatedly burning to constant weight (m) 1 ）。
Detection example 1
The same ferrosilicon samples were examined by the methods of examples 1-3 and comparative examples 1-5, and the measured silicon contents are shown in Table 2.
TABLE 2 silicon content measured for examples 1-3 and comparative examples 1-5
As can be seen from Table 2, the RSD values of the silicon content values measured by the methods of examples 1-3 are significantly smaller than those of the prior art, indicating that the process of the present invention is good in reproducibility.
Detection example 2
To examine the accuracy of the detection methods of examples 1 to 3 and comparative examples 1 to 5, three ferrosilicon standard samples (silicon content 77.42%,66.18%,51.46%, respectively) were subjected to silicon content measurement by the methods of examples 1 to 3 and comparative examples 1 to 5, respectively, and the measurement results are shown in Table 3.
TABLE 3 accuracy of the detection methods of examples 1-3 and comparative examples 1-5
As can be seen from Table 3, the deviations of the silicon content measured by the methods of examples 1-3 of the present invention are smaller than the allowable deviations of the national standard, and the accuracy meets the requirements of the national standard method.
In conclusion, the silicon content determination method has accurate and stable results. The method of the invention is characterized in that the mixed flux is changed from sodium peroxide-sodium carbonate into sodium hydroxide, perchloric acid is increased from 40ml to 60ml, the carbonization temperature of filter paper is adjusted from 650 ℃ to 450 ℃ for burning, and then the temperature is gradually increased for carbonization, so that the stability and the accuracy of test results can be improved.
Claims (4)
1. A sample melting method for measuring the silicon content in ferrosilicon by a perchloric acid dehydration gravimetric method is characterized in that sodium hydroxide solid is adopted as a flux to melt a sample, and the specific method comprises the following steps: mixing 0.2000-0.3000g of sample with 3g of sodium hydroxide solid flux and a nickel crucible, baking for 50-60 minutes at 200-300 ℃ by using an electric hot plate, melting for 5-10 minutes at 340-360 ℃, and then gradually heating to 640-660 ℃ to melt for 14-20 minutes.
2. A method for determining the silicon content in a ferrosilicon alloy based on the sample melting method of claim 1, which is characterized by the following steps: and (3) acidifying the fused sample by hydrochloric acid, dehydrating by perchloric acid, filtering and washing, carbonizing and burning the precipitate in a high-temperature furnace at 400-500 ℃ for 5-7 minutes, slowly heating to 1100 ℃ and burning for 30 minutes to constant quantity, and finally calculating the mass fraction of silicon by using the mass difference before and after hydrofluoric acid treatment.
3. The method for determining the silicon content of a ferrosilicon alloy according to claim 2, wherein the perchloric acid is added in a volume of 60mL in the perchloric acid dehydration step.
4. The method for determining the silicon content of a ferrosilicon alloy according to claim 2, wherein the washing time period in the filtering washing step is 7-8 hours.
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