CN117147368A - Method for measuring silicon content in carbon cored wire - Google Patents
Method for measuring silicon content in carbon cored wire Download PDFInfo
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- CN117147368A CN117147368A CN202311268631.7A CN202311268631A CN117147368A CN 117147368 A CN117147368 A CN 117147368A CN 202311268631 A CN202311268631 A CN 202311268631A CN 117147368 A CN117147368 A CN 117147368A
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- carbon
- silicon content
- cored wire
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- hydrochloric acid
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 45
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 40
- 239000010703 silicon Substances 0.000 title claims abstract description 40
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910052573 porcelain Inorganic materials 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000008188 pellet Substances 0.000 claims abstract description 8
- 239000002244 precipitate Substances 0.000 claims abstract description 8
- 238000001704 evaporation Methods 0.000 claims abstract description 7
- 239000012046 mixed solvent Substances 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 239000000155 melt Substances 0.000 claims abstract description 6
- 150000003839 salts Chemical class 0.000 claims abstract description 5
- 239000000779 smoke Substances 0.000 claims abstract description 5
- 238000004380 ashing Methods 0.000 claims abstract description 4
- 238000009835 boiling Methods 0.000 claims abstract description 4
- 229940005991 chloric acid Drugs 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 15
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 12
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 8
- 238000001556 precipitation Methods 0.000 claims description 6
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 4
- SOIFLUNRINLCBN-UHFFFAOYSA-N ammonium thiocyanate Chemical compound [NH4+].[S-]C#N SOIFLUNRINLCBN-UHFFFAOYSA-N 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- 230000000391 smoking effect Effects 0.000 claims description 4
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 3
- 239000004327 boric acid Substances 0.000 claims description 3
- 238000004364 calculation method Methods 0.000 claims description 3
- 229910001447 ferric ion Inorganic materials 0.000 claims description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- -1 iron ion Chemical class 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000012768 molten material Substances 0.000 claims 1
- 239000002245 particle Substances 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 abstract description 2
- 238000001304 sample melting Methods 0.000 abstract description 2
- XTEGARKTQYYJKE-UHFFFAOYSA-N chloric acid Chemical compound OCl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-N 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 229910000831 Steel Inorganic materials 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000007689 inspection Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 238000009628 steelmaking Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000010309 melting process Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- HXOLFXRMWWHLMH-UHFFFAOYSA-L disodium boric acid carbonate Chemical compound [Na+].[Na+].OB(O)O.[O-]C([O-])=O HXOLFXRMWWHLMH-UHFFFAOYSA-L 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000004442 gravimetric analysis Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- 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
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 relates to a method for measuring silicon content in a carbon cored wire, which comprises the following steps: 1) Taking 0.25+/-0.02 g of core powder in the carbon cored wire, and placing the core powder in a muffle furnace to burn for more than 30 minutes until no carbon exists in the sample; 2) 2-3 g of mixed solvent is put into the quantitative filter paper folded into a cone shape, ash is added, and the mixture is packed into pellets; placing the pellets and carbon powder into a porcelain crucible, heating in a muffle furnace, placing the obtained melt and hydrochloric acid into a beaker for heating, dissolving the melt, evaporating, adding chloric acid until smoke is generated, and cooling; adding boiling water, heating at low temperature to dissolve salts, and filtering with filter paper; 4) Drying the precipitate and the filter paper in a porcelain crucible, ashing, burning in a muffle furnace, and cooling to room temperature in a dryer; the silicon content was calculated. The advantages are that: the influence of carbon on the detection is eliminated, the sample melting cost is low, no impurity is introduced, and batch detection is facilitated. The accuracy and precision are high.
Description
Technical Field
The invention belongs to the field of chemical analysis of carbon cored wires, and particularly relates to a method for measuring silicon content in a carbon cored wire.
Background
The carbon cored wire is a coil material formed by crushing high-quality graphite ore into powder with certain granularity and filling the powder into a continuous narrow steel belt. The carbon-adding agent mainly plays a role of carbureting in the steelmaking process and complements the carbon content burnt in the steel smelting process. Because of the strip structure, the molten steel can be poured into the molten steel, the utilization rate is high, and the carburetion effect is good.
The silicon content of the carbon cored wire has a great influence on the carburetion effect, and the carburetion effect is poor due to the high silicon content, so that the accurate detection of the silicon content is particularly important.
Disclosure of Invention
The invention aims to provide a method for measuring the silicon content in a carbon cored wire, which is simple to operate, can accurately measure the silicon content in the carbon cored wire and meets the requirement of steelmaking production.
In order to achieve the above purpose, the present invention is realized by the following technical scheme:
a method for determining the silicon content of a carbon cored wire comprising the steps of:
1) Taking 0.25+/-0.02 g of core powder in the carbon cored wire, and placing the core powder in a muffle furnace at 850+/-50 ℃ to burn for more than 30 minutes until no carbon exists in the sample;
2) 2-3 g of mixed solvent is put into the quantitative filter paper folded into a cone shape, and ash obtained in the step 1) is added to be packed into pellets; putting the pellets and carbon powder into a porcelain crucible, putting the porcelain crucible into a muffle furnace with the temperature of 950+/-50 ℃, taking out the porcelain crucible after 35+/-2 min, cooling to room temperature, and putting the obtained melt into a 250mL beaker;
3) Adding 40+/-2 mL of hydrochloric acid into a beaker, heating to 100+/-30 ℃ in a low-temperature electric furnace to dissolve the melt, evaporating to 10+/-0.5 mL, adding 15+/-1 mL of perchloric acid, continuing to evaporate until smoking, expelling the high-chloric acid smoke, and cooling; adding 100+ -5 mL of boiling water, heating at low temperature of 100+ -30 ℃ to dissolve salts, filtering at the temperature with filter paper, washing the beaker with 80+ -10 ℃ hydrochloric acid solution for 5-7 times, washing the precipitate for 7-8 times until no ferric ion reaction occurs, and washing with 80+ -10 ℃ hot water until no chloride ion precipitation reaction occurs;
4) Placing the precipitate and filter paper into a porcelain crucible with constant weight, drying, ashing, burning in a muffle furnace with 1000+/-50 ℃ for 30+/-2 min, taking out, cooling to room temperature in a dryer, weighing, and repeatedly burning to constant quantity;
5) Calculation of
Calculating silicon content omega in sample si ：
In the formula (1): omega si Silicon content in the sample, mass percent; m is m 1 G is the mass of ash; m is the mass of the sample, g;0.4674 is the coefficient of silicon dioxide converted to silicon.
The quality of the core powder is accurate to 0.0001g.
The preparation of the mixed solvent comprises the following steps: mixing anhydrous sodium carbonate and boric acid according to a mass ratio of 2:1, grinding, putting into a drying oven with the temperature of 250+/-15 ℃ for more than 3 hours, taking out, cooling, grinding, and the granularity of the ground material is below 80 meshes.
The middle of the porcelain crucible is concave, and the melt heated by the muffle furnace is in a flat sphere shape.
The volume ratio of the concentrated hydrochloric acid to the water in the hydrochloric acid is 1:1.
The concentration of the perchloric acid is 1.67g/mL.
The hydrochloric acid solution in the step 3) is a mixed solution of concentrated hydrochloric acid and water, and the volume ratio of the concentrated hydrochloric acid to the water is 5:95.
In step 3), an ammonium thiocyanate solution is used for checking whether no iron ions react, and the concentration of the ammonium thiocyanate solution is 50g/L.
In the step 3), a silver nitrate solution is used for checking whether no chloridion precipitation reaction exists, and the concentration of the silver nitrate solution is 10g/L.
The granularity of the carbon powder in the step 2) is 7-10 mu m.
Compared with the prior art, the invention has the beneficial effects that:
the method for measuring the silicon content in the carbon cored wire is a gravimetric analysis method, and carbon removal operation is performed in the early stage to eliminate the influence of carbon on the inspection. The quantitative filter paper folded into a cone shape is adopted, the small balls are packed and placed in the ceramic crucible filled with carbon powder and pressed into a concave shape to melt the sample, the sample melting cost is low, no impurity is introduced, and batch detection is facilitated. The accuracy and the precision are high, and the steel-making production requirements can be met.
Detailed Description
The present invention will be described in detail below, but it should be noted that the practice of the present invention is not limited to the following embodiments.
A method for determining the silicon content of a carbon cored wire comprising the steps of:
1) Sieving the core powder in the carbon cored wire with a 0.097mm sieve, taking 0.25g to 0.0001g accurately, and placing the core powder in a muffle furnace at 850+/-50 ℃ to burn for more than 30min until no carbon exists in the sample.
2) 2-3 g of mixed solvent is put into the quantitative filter paper folded into a cone shape, and ash obtained in the step 1) is added to be packed into pellets; putting the pellets and carbon powder into a porcelain crucible, filling the porcelain crucible, putting the porcelain crucible into a 950+/-50 muffle furnace, taking out the porcelain crucible after 35+/-2 min, cooling to room temperature, and putting the obtained melt into a 250mL beaker; wherein, the carbon powder is put into a porcelain crucible after passing through a sieve of 0.097mm, and the preparation of the mixed solvent is carried out: mixing anhydrous sodium carbonate and boric acid according to a mass ratio of 2:1, grinding, putting into a drying oven with the temperature of 250+/-15 ℃ for more than 3 hours, taking out, cooling, crushing by a stainless steel rod, grinding by an agate mortar, and storing in a grinding bottle for standby grinding.
3) Adding 40mL of hydrochloric acid (1+1) into a beaker, heating to 100+/-30 ℃ in a low-temperature electric furnace to dissolve the melt, evaporating to 10+/-0.4 mL, adding 15+/-0.6 mL of perchloric acid (with the concentration of 1.67 g/mL), continuing evaporating until smoking, expelling the high-chloric acid smoke, and cooling; adding 100+ -10 mL of boiling water, heating at low temperature of 100+ -30 ℃ to dissolve salts, filtering at the temperature with filter paper, washing beaker with 80+ -10 ℃ hot hydrochloric acid solution (5+95) for 5-7 times, washing precipitate for 7-8 times until no ferric ion reaction, and washing with 80+ -10 ℃ hot water until no chloride ion precipitation reaction; the presence or absence of iron ion reaction was checked with an ammonium thiocyanate solution having a concentration of 50g/L. And (3) checking whether no chloridion precipitation reaction exists or not by using a silver nitrate solution, wherein the concentration of the silver nitrate solution is 10g/L.
4) Placing the precipitate and filter paper into a porcelain crucible with constant weight, drying, ashing, burning in a muffle furnace with 1000+/-50 ℃ for 30+/-2 min, taking out, cooling to room temperature in a dryer, weighing, and repeatedly burning to constant quantity; the middle of the porcelain crucible is concave, and the melt heated by the muffle furnace is in a flat sphere shape.
According to the inspection condition, when the silicon content is more than 1%, the silicon swing operation can be increased. Placing impure silicon dioxide (all of the above precipitate) in a platinum crucible, adding 3 drops of sulfuric acid (1+1) and 5mL of hydrofluoric acid (concentrated) by wetting with a little water, placing on an electric hot plate, heating and evaporating until the sulfuric acid smoke is exhausted, then placing in a 1050 ℃ high temperature furnace to burn for 15min, taking out and slightly cooling, placing in a dryer, cooling to room temperature, weighing, and repeatedly burning to constant quantity.
5) Calculation of
Calculating silicon content omega in sample si ：
In the formula (1): omega si Silicon content in the sample, mass percent; m is m 1 G is the mass of ash; m is the mass of the sample, g;0.4674 is the coefficient of silicon dioxide converted to silicon. The same sample was measured at least 2 times independently.
2 samples with different contents and one standard sample were selected, and each sample was analyzed 9 times in parallel, and the analysis results and the precision are shown in table 1. By referring to the standards of other varieties of silicon inspection, the silicon content is 1.00% -5.00%, the tolerance is basically 0.15-0.20%, and as can be seen from the table 1, the precision and accuracy of the analysis of the method can meet the requirements of similar standards, and the production and scientific research requirements can be met.
Table 1 precision and accuracy test
The method includes the steps of firstly carrying out high Wen Chutan on a sample, melting ash by using a sodium carbonate-boric acid mixed flux, leaching and acidizing by using hydrochloric acid, heating perchloric acid for dehydration, smoking and evaporating to near dryness, cooling, heating to dissolve salts, filtering, washing, drying, burning, weighing to constant quantity, and calculating the content of silicon. The accuracy and precision of the result are high, the problem of accurately measuring the silicon content in the carbon cored wire is solved, and technical support is provided for steelmaking production and scientific research.
In the detection process, carbon needs to be completely removed in the early stage, otherwise, the observation of the later stage inspection phenomenon is influenced. In the melting process, the filter paper wrapping the fluxing agent and the sample is screwed up, and after melting, the transfer is complete, so that the silicon loss in the melting process is avoided. The filtering and washing steps are carefully operated, so that the cleaning is ensured and the silicon loss is avoided. The accurate result can be obtained by the operation according to the method.
Claims (10)
1. A method for determining the silicon content of a carbon cored wire comprising the steps of:
1) Taking 0.25+/-0.02 g of core powder in the carbon cored wire, and placing the core powder in a muffle furnace at 850+/-50 ℃ to burn for more than 30 minutes until no carbon exists in the sample;
2) 2-3 g of mixed solvent is put into the quantitative filter paper folded into a cone shape, and ash obtained in the step 1) is added to be packed into pellets; putting the pellets and carbon powder into a porcelain crucible, putting the porcelain crucible into a muffle furnace with the temperature of 950+/-50 ℃, taking out the porcelain crucible after 35+/-2 min, cooling to room temperature, and putting the obtained melt into a 250mL beaker;
3) Adding 40+/-2 mL of hydrochloric acid into a beaker, heating to 100+/-30 ℃ in a low-temperature electric furnace to dissolve the melt, evaporating to 10+/-0.5 mL, adding 15+/-1 mL of perchloric acid, continuing to evaporate until smoking, expelling the high-chloric acid smoke, and cooling; adding 100+ -5 mL of boiling water, heating at low temperature of 100+ -30 ℃ to dissolve salts, filtering at the temperature with filter paper, washing the beaker with 80+ -10 ℃ hydrochloric acid solution for 5-7 times, washing the precipitate for 7-8 times until no ferric ion reaction occurs, and washing with 80+ -10 ℃ hot water until no chloride ion precipitation reaction occurs;
4) Placing the precipitate and filter paper into a porcelain crucible with constant weight, drying, ashing, burning in a muffle furnace with 1000+/-50 ℃ for 30+/-2 min, taking out, cooling to room temperature in a dryer, weighing, and repeatedly burning to constant quantity;
5) Calculation of
Calculating silicon content omega in sample si ：
In the formula (1): omega si Silicon content in the sample, mass percent; m is m 1 G is the mass of ash; m is the mass of the sample, g;0.4674 is the coefficient of silicon dioxide converted to silicon.
2. The method for determining the silicon content of a carbon cored wire of claim 1 wherein the mass of the core powder is accurate to 0.0001g.
3. The method for determining the silicon content of the carbon cored wire of claim 1 wherein the preparing of the mixed solvent comprises: mixing anhydrous sodium carbonate and boric acid according to a mass ratio of 2:1, grinding, putting into a drying oven with the temperature of 250+/-15 ℃ for more than 3 hours, taking out, cooling, grinding, and the granularity of the ground material is below 80 meshes.
4. The method for determining the silicon content of the carbon cored wire of claim 1 wherein the middle of the porcelain crucible is concave, and the molten material after being heated by the muffle furnace is in a flat sphere shape.
5. The method for determining the silicon content of the carbon cored wire of claim 1 wherein the volume ratio of concentrated hydrochloric acid to water in the hydrochloric acid is 1:1.
6. The method for determining the silicon content of a carbon cored wire of claim 1 wherein the concentration of perchloric acid is 1.67g/mL.
7. The method for determining the silicon content of a carbon cored wire of claim 1 wherein the hydrochloric acid solution in step 3) is a mixed solution of concentrated hydrochloric acid and water, and the volume ratio of the concentrated hydrochloric acid to the water is 5:95.
8. The method for determining the silicon content of a carbon cored wire of claim 1 wherein the step 3) is performed by checking whether no iron ion is reacted with an ammonium thiocyanate solution having a concentration of 50g/L.
9. The method for determining the silicon content of a carbon cored wire of claim 1 wherein the silver nitrate solution is used in step 3) to check whether no chloride ion precipitation reaction occurs, the concentration of the silver nitrate solution being 10g/L.
10. The method for determining the silicon content of a carbon cored wire of claim 1 wherein the particle size of the carbon powder in step 2) is 7 to 10 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311268631.7A CN117147368A (en) | 2023-09-28 | 2023-09-28 | Method for measuring silicon content in carbon cored wire |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311268631.7A CN117147368A (en) | 2023-09-28 | 2023-09-28 | Method for measuring silicon content in carbon cored wire |
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| Publication Number | Publication Date |
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| CN117147368A true CN117147368A (en) | 2023-12-01 |
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| CN202311268631.7A Pending CN117147368A (en) | 2023-09-28 | 2023-09-28 | Method for measuring silicon content in carbon cored wire |
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| Country | Link |
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- 2023-09-28 CN CN202311268631.7A patent/CN117147368A/en active Pending
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