CN103196783A - Method for determining content of silicon carbide in temperature raising agent - Google Patents
Method for determining content of silicon carbide in temperature raising agent Download PDFInfo
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- CN103196783A CN103196783A CN2013101015442A CN201310101544A CN103196783A CN 103196783 A CN103196783 A CN 103196783A CN 2013101015442 A CN2013101015442 A CN 2013101015442A CN 201310101544 A CN201310101544 A CN 201310101544A CN 103196783 A CN103196783 A CN 103196783A
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Abstract
The invention discloses a method for determining the content of silicon carbide in a temperature raising agent. The method comprises the following steps of: firing a temperature raising agent sample for the first time to remove free carbon in the sample; adding an acid solution into the fired sample, dissolving, and filtering to obtain sediment; adding a fluxing agent into the sediment, firing for the second time to oxidize carbon in the sediment o form carbon dioxide, and determining the quantity of the carbon dioxide; correspondingly performing a blank experiment without addition of the temperature raising agent sample, and determining the quantity of carbon dioxide in the blank experiment; and calculating the content of the silicon carbide in the temperature raising agent according to the quantity of the carbon dioxide obtained in the sample, and the quantity of the carbon dioxide obtained in the blank experiment. By using the technical scheme disclosed by the invention, the content of the silicon carbide in the temperature raising agent can be quickly and accurately determined.
Description
Technical field
The present invention relates to technical field of ferrous metallurgical analysis, particularly relate to a kind of method of utilizing the content of silit in the burning gases volumetric determination temperature raising agent.
Background technology
At present, for the existing national standard of the mensuration of carborundum content in the fire resistive materials such as silit, the standard of the carbon-silicon carbide materials such as temperature raising agent that contain magnesium oxide, calcium oxide and alundum (Al is but set up as yet.Measure the content of silit in the temperature raising agent and generally all use the silica weight method, the method is measured the long flow path of silit, just can analyze a collection of result in 3~4 days; And use a large amount of perchloric acid, complex operation step needs to consume a large amount of chemicalss, when causing final measuring error bigger, and environmental protection not enough, energy-conservation.
The existing method of measuring the content of silit in the temperature raising agent has silica weight method and infrared absorption method, and concrete assay method is as follows:
(1) silica weight method:
Required reagent: density is the hydrochloric acid of 1.19g/mL, and density is the hydrofluorite of 1.13g/mL, and density is the nitric acid of 1.42g/mL, and density is the perchloric acid of 1.68g/mL, the aqueous sulfuric acid that sulfuric acid mixes with the water equal-volume; Hydrochloric acid: water volume ratio is the watery hydrochloric acid of 5:95.
Measuring process: take by weighing the temperature raising agent sample and in the platinum ware, place 800 ± 10 ℃ muffle furnace to lead to the oxygen calcination, after taking out cooling, wetting with low amounts of water, add nitric acid, hydrofluorite and 8 aqueous sulfuric acids, being evaporated to the white cigarette of sulfuric anhydride in the Low-temp. electrothermal plate emits to the greatest extent, take off coldly slightly, add the aqueous hydrochloric acid solution that hydrochloric acid mixes with the water equal-volume, heated several minutes, make the impurity dissolving, filter with the middling speed quantitative filter paper while hot, use hot watery hydrochloric acid washing platinum diss and residue for several times, in company with doing blank assay; Residue and filter paper are put into the porcelain crucible that burns to constant weight, prior to behind the low-temperature carbonization filter paper in 750 ℃ of high temperature furnaces calcination 40min, take out and to put into exsiccator and be cooled to room temperature, weighing crucible and residue are done blank assay in company with sample; Residue is placed in nickel or the corundum crucible through ashing, calcination and adds NaOH and sodium peroxide 700~720 ℃ of fusions, the cooling back washes out crucible with hot water and is acidified to about pH=3.5, add perchloric acid, be heated to perchloric acid and emit dense white cigarette and the 10~15min that refluxes, take off cold slightly, add hydrochloric acid and hot water, stirring makes its dissolved salts, filter with the middling speed quantitative filter paper, clean beaker, be washed till no ferric ion with hot hydrochloric acid, then with hot water wash to there not being chlorion, to precipitate together with in the filter paper immigration porcelain crucible, ashing is at 950 ℃ of calcination 40min.Taking-up is chilled to room temperature, weighing, and the calcination weighing is to constant weight repeatedly.Calculate the content of silit in the temperature raising agent sample with residue weight.
(2) infrared absorption method
Required reagent and instrument: infrared determination of carbon and sulfur instrument CS-444; Ceramic crucible: 25 * 25mm places exsiccator standby through 1200 ℃ of calcinations; The pure iron flux, tungsten powder, needle-like tin grain; Oxygen output is pressed 35psi is set, and nitrogen output is pressed 35psi is set.
Measuring process: take by weighing Elema and temperature raising agent sample respectively and lead to oxygen calcination 1.0h in ceramic crucible in 800 ℃ ± 10 ℃ muffle furnaces, take out cooling and add the pure iron flux, vanadium pentoxide covers tungsten powder again and measures carbon content in infrared carbon sulfur analyzer.With BaCO
3The N Reference Alignment curve, the sample analysis time is set to 50s, and comparison level is 1%, and smoothly and at the 60s inner analysis finish sample burning rear surface, calculates the content of silit with the carbon content of measuring.
Summary of the invention
The Determination on content method that the purpose of this invention is to provide silit in a kind of temperature raising agent can be measured the content of silit in the temperature raising agent accurately, fast.
Technical scheme is specific as follows:
The Determination on content method of silit in a kind of temperature raising agent comprises:
The temperature raising agent of calcination for the first time sample is to remove the uncombined carbon in the described sample;
Add the acid solution dissolving in the sample after the calcination, filter, obtain precipitation;
Add flux in described precipitation, calcination for the second time makes the oxidation of coal in the described precipitation become carbon dioxide, measures the amount of described carbon dioxide;
In company with doing blank assay, do not add the temperature raising agent sample, measure the amount of carbon dioxide in the blank assay;
Calculate the content of silit in the described temperature raising agent with the amount of the carbon dioxide that obtains in sample and the blank assay.
Further: in the described calcination first time process, place 800 ± 10 ℃ muffle furnace to lead to oxygen calcination 1.0-1.5h the porcelain boat that described temperature raising agent sample is housed.
Further: obtain in the described precipitation process, add the aqueous hydrochloric acid solution that 40mL hydrochloric acid mixes with the water equal-volume in the sample after the calcination, 0.2 restrains sodium fluoride, covers surface plate, 200 ℃~250 ℃ following heating for dissolving; Add hot water 50mL after the dissolving, boil 5min, with being covered with the ceramics funnel filtration with holes that thickness is the acid-washed asbestos of 10mm; Be the aqueous hydrochloric acid solution washing funnel 5~6 times of 5:95 with hydrochloric acid and water volume ratio, and all wash on the asbestos, be precipitated to neutrality with 70~80 ℃ hot wash again, will precipitate together with asbestos with tweezers and place porcelain boat.
Further: in the described calcination second time process, the porcelain boat that precipitation is housed is placed baking oven, 110~115 ℃ of oven dry 1~1.5 hour; Add flux, with long hook porcelain boat is pushed into the centre position of 1250 ℃ of electric tube furnaces, the jam-pack plug, preheating 3min leads to oxygen combustion 5min, makes the oxidation of coal in the described precipitation become carbon dioxide.
Further: described flux is the potpourri of 0.5000 gram red copper and 0.1000 gram vanadium pentoxide.
Further: the amount of carbon dioxide records by carbometer, and the eudiometer tube rod reading of temperature raising agent sample is designated as X; The eudiometer tube rod reading of blank assay is designated as X
0
Further: the content of silit is calculated as follows in the described temperature raising agent,
W
SIC(%)=3.339(X-X
0)×f÷m
In the formula, m is sample size; F is temperature and pressure correcting coefficient, calculates according to existing method; 3.339 be converted into the coefficient of silit for carbon.
Beneficial effect of the present invention:
1, the present invention adopts gas volumetric method to measure silit in the temperature raising agent, avoids the silica weight method to use a large amount of perchloric acid, uses chemical reagent few, has the advantage of energy-saving and environmental protection.
2, method of the present invention is not only highly sensitive, and detection limit is low, and finding speed is fast, and is easy and simple to handle and little with respect to the additive method interference, has good selectivity.
3, adopt assay method of the present invention, the content of silit in experiment measuring temperature raising agent repeatedly, the standard deviation of measurement result is 0.1449, and relative standard deviation is 0.6858%, illustrates that method accuracy height, measurement result that technical solution of the present invention provides are stable.
4, the measurement range of the method that provides of technical solution of the present invention: SiC content≤45.00% in the temperature raising agent sample.
Embodiment
The total thinking of the present invention is: because sample contains small amount of carbonate, earlier sample is claimed in porcelain boat, remove uncombined carbon 800 ℃ of logical oxygen burnings, add the hydrochloric acid heating for dissolving and remove carbonate, filter to such an extent that precipitate, will precipitate oven dry and be pushed into calcination in the electric tube furnace again, make the carbon in the precipitation be converted into carbon dioxide, measure the content of carbon dioxide, with the content of the amount conversion silit of carbon dioxide.
In the embodiment of the invention, agents useful for same and instrument are preferred:
First Drexel bottle in the carbometer: interior dress is added with the potassium permanganate saturated solution of NaOH to high 1/3 place of bottle; Second Drexel bottle: dress sulfuric acid is to high 1/3 place of bottle; Drying tower: upper strata dress alkali asbestos, lower floor's dress anhydrous calcium chloride, middle interval glass wool;
Porcelain boat: 1200~1300 ℃ of calcinations, cooling is placed in the exsiccator standby before using;
Acid-washed asbestos: 900 ℃ of calcinations, cooling is placed in the exsiccator standby.
In the embodiment of the invention, the Determination on content method of silit in the temperature raising agent adopts gas volumetric method, and step is as follows:
Take by weighing the temperature raising agent sample in porcelain boat, place 800 ± 10 ℃ muffle furnace to carry out the calcination first time porcelain boat that sample is housed, logical oxygen calcination 1.0-1.5h, after sample is placed the 250mL beaker, add the aqueous hydrochloric acid solution that 40mL hydrochloric acid mixes with the water equal-volume, 0.2 gram sodium fluoride, cover surface plate, 200 ℃~250 ℃ heating for dissolving, add hot water 50mL after the dissolving, boil 5min, while hot with being covered with the ceramics funnel filtration with holes that thickness is the acid-washed asbestos of 10mm.Be the aqueous hydrochloric acid solution washing funnel 5~6 times of 5:95 with hydrochloric acid and water volume ratio, and all wash on the asbestos, be precipitated to neutrality with 70~80 ℃ hot wash again, will precipitate together with asbestos with tweezers and place porcelain boat.
The porcelain boat that precipitation is housed is placed baking oven, 110~115 ℃ of oven dry 1~1.5 hour, add 0.5000 gram red copper and 0.1000 gram vanadium pentoxide as flux, porcelain boat is pushed into the centre position of 1250 ℃ of electric tube furnaces with long hook, the centre position is the highest position of electric tube furnace temperature, carry out the calcination second time, jam-pack plug immediately, preheating 3min, logical oxygen combustion 5min, make oxidation of coal become carbon dioxide, with the potassium hydroxide solution absorbing carbon dioxide, repeat to absorb twice.According to the operation of carbometer working specification, measured quantity tracheae rod reading.When carborundum content was higher in the sample, logical oxygen burning again with the potassium hydroxide solution absorbing carbon dioxide, was write down the eudiometer tube rod reading as stated above.Repeatedly repeating above-mentioned experiment, is zero to the eudiometer tube reading, and repeatedly the reading addition is designated as X.
In company with doing blank assay, do not add the temperature raising agent sample, repeat above-mentioned experimental procedure, the eudiometer tube rod reading of blank assay is designated as X
0
The content of silit is calculated as follows:
W
SIC(%)=3.339(X-X
0)×f÷m
In the formula, m is sample size; X is the eudiometer tube rod reading; X
0Eudiometer tube rod reading for blank assay; F is temperature and pressure correcting coefficient, calculates according to existing method; 3.339 be converted into the coefficient of silit for carbon.
Selection of experiment conditions
1, silit decomposition starting temperature
The resistance Elema is high-purity silicon carbide, and purity is more than 90%.Elema was pulverized 200 orders places exsiccator standby in 100~105 ℃ of oven dry 2h.
Claim Elema and temperature raising agent sample to put into porcelain boat respectively by table 1, behind ℃ logical oxygen calcination 1.0h of muffle furnace temperature rise to 800 ± 10, do not add flux, preheating 10min in electric tube furnace, logical oxygen burning 5min, gas volumetric method is measured carbon content, and the result is as shown in table 1.
Table 1
Sample | Design temperature | Coefficient | Reading | Carbon content | Sample weighting amount g |
Elema | 950℃ | 0.875. | 0.000 | 0.000 | 0.0500 |
Elema | 1000℃ | 0.875 | 0.000 | 0.000 | 0.0500 |
Elema | 1030℃ | 0.875 | 0.000 | 0.000 | 0.0500 |
Elema | 1050℃ | 0.875 | 0.020 | 0.350 | 0.0500 |
Elema | 1100℃ | 0.875 | 0.040 | 0.700 | 0.0500 |
Temperature raising agent | 950℃ | 0.875 | 0.000 | 0.000 | 0.1500 |
Temperature raising agent | 1000℃ | 0.875 | 0.000 | 0.000 | 0.1500 |
Temperature raising agent | 1050℃ | 0.875 | 0.015 | 0.088 | 0.1500 |
Conclusion: find out that from The above results silit begins during greater than 1050 ℃ to decompose in temperature.
2, the complete decomposition temperature of silit
Claim Elema and temperature raising agent sample to put into porcelain boat respectively by table 2, after muffle furnace is warmed up to 800 ± 10 ℃ of logical oxygen calcination 1.0h, add 0.5000 gram red copper and 0.1000 gram vanadium pentoxide as flux, measure carborundum content in electric tube furnace, the results are shown in Table 2.
Table 2
Sample | Design temperature ℃ | Coefficient | Reading | Carbon content % | Silit amount % | Sample weighting amount g |
Temperature raising agent | 1200 | 0.870 | 0.900 | 5.22 | 17.40 | 0.1500 |
Temperature raising agent | 1230 | 0.870 | 0.920 | 5.336 | 17.79 | 0.1500 |
Temperature raising agent | 1250 | 0.866 | 1.110 | 6.408 | 21.38 | 0.1500 |
Temperature raising agent | 1280 | 0.859 | 1.105 | 6.328 | 21.12 | 0.1500 |
Temperature raising agent | 1280 | 0.859 | 1.110 | 6.356 | 21.21 | 0.1500 |
Elema | 1200 | 0.888 | 2.020 | 25.62 | 85.55 | 0.0700 |
Elema | 1230 | 0.888 | 2.015 | 25.56 | 85.34 | 0.0700 |
Elema | 1250 | 0.888 | 2.220 | 27.53 | 91.90 | 0.0700 |
Elema | 1280 | 0.859 | 2.230 | 27.37 | 91.37 | 0.0700 |
Conclusion: the data of Elema, temperature raising agent sample as can be seen from table 2, silit is at 1200 ℃ and 1230 ℃ of incomplete combustions, the recovery is low, and logical oxygen combustion decomposes fully in the time of 1250 ℃, the carbon that 1280 ℃ of logical oxygen combustions are measured and carborundum content and 1250 ℃ record basically identical as a result, so the logical oxygen combustion temperature of sample can be set at 1250 ℃.
3, the selection of preheating time and sample weighting amount
Draw by experiment, temperature raising agent sample silicon carbide-containing claims 0.1500 gram sample about 20%, and preheating time is when being 1~2min, logical oxygen combustion, do twice absorption after, also need again logical oxygen combustion, do twice absorption; And be 3~4min preheating time, behind the logical oxygen combustion, does twice absorption and get final product.So, be decided to be 3min preheating time.
Carborundum content is more than 20%, and the sample sample weighting amount is at 0.1000 gram, and 0.1500 gram during 0.2000 gram, can be read behind the logical oxygen combustion and absorbs reading accurately; And sample weighting amount is 0.2500 gram, absorbs reading behind the logical oxygen combustion and surpasses 1.500, because reading that eudiometer tube marks is accurate below 1.500, reading 1.500 above resultant errors are bigger, so the standard of sample weighting amount is as shown in table 3.The measurement range of this method: SiC content≤45.00% in the temperature raising agent sample.
Table 3
SiC content % | Sample weighting amount (gram) |
≤15.00 | 0.2500 |
>15.00~20.00 | 0.2000 |
>20.00~25.00 | 0.1500 |
≥25.00 | 0.1000 |
4, accuracy experiment
With silica weight method, infrared absorption method same temperature raising agent sample is measured with gas volumetric method and to be compared.
The silica weight method is measured the content of silit in the temperature raising agent, the results are shown in Table 4.
Table 4
Sample | Sample weighting amount (gram) | Weight after the calcination (gram) | Coefficient | Carborundum content % |
Temperature raising agent | 1.000 | 0.2956 | 67.10 | 19.83 |
Temperature raising agent | 1.000 | 0.2988 | 67.10 | 20.05 |
Infrared absorption method is measured the content of silit in the temperature raising agent, the results are shown in Table 5.
Table 5
Sample | Sample weighting amount (gram) | Analysis result (carbon) % | Carbon and silit conversion coefficient | Carborundum content % |
Temperature raising agent | 0.1500 | 6.396 | 3.339 | 21.36 |
Temperature raising agent | 0.1500 | 6.456 | 3.339 | 21.55 |
Silit records result and silica weight method measurement result with infrared absorption method and differs and surpassed tolerance 0.3% in the temperature raising agent, and be positive error 1.29%, reason is to contain some difficult carbonate that decompose in the temperature raising agent sample, adopts gas volumetric method to measure and can solve the problem that contains carbonate.Gas volumetric method is measured the content of silit in the temperature raising agent, result such as table 6.
Table 6
Sample | Sample weighting amount g | Reading | Coefficient | Carbon content % | Carborundum content % |
Temperature raising agent | 0.0556 | 0.400 | 0.874 | 6.288 | 20.99 |
Temperature raising agent | 0.0556 | 0.395 | 0.874 | 6.209 | 20.73 |
Temperature raising agent | 0.1825 | 1.300 | 0.881 | 6.276 | 20.95 |
Temperature raising agent | 0.1825 | 1.290 | 0.881 | 6.227 | 20.79 |
Test findings shows, carbonate content seldom in the temperature raising agent sample, consistent with silica weight method result with silit in the gas volumetric method mensuration temperature raising agent, so reliable and stable with carborundum content result in the higher carbon-silicon carbide material of gas volumetric method mensuration free carbon content.
5, the experiment of precision
The temperature raising agent sample is done repeated experiments, measure the content of its silit, analyze accuracy and the stability of this method from measurement result.
Take by weighing the temperature raising agent sample and in 800 ± 10 ℃ of muffle furnaces, behind the logical oxygen calcination 1.5h, add 0.5000 gram red copper and 0.1000 gram vanadium pentoxide as flux, in 1250 ℃ of electric tube furnaces, preheating 3min, lead to oxygen combustion 5min then, measure the content of silit, the results are shown in Table 7.
Table 7
Coefficient | Reading | Carbon content % | Silit amount % | Mean value | Standard deviation | Relative standard deviation % |
0.859 | 1.105 | 6.328 | 21.12 | ? | ? | ? |
0.859 | 1.110 | 6.356 | 21.21 | ? | ? | ? |
0.866 | 1.110 | 6.408 | 21.28 | ? | ? | ? |
0.866 | 1.090 | 6.293 | 21.02 | ? | ? | ? |
0.866 | 1.100 | 6.350 | 21.20 | ? | ? | ? |
0.866 | 1.100 | 6.350 | 21.20 | 21.13 | 0.1449 | 0.6858 |
0.866 | 1.115 | 6.437 | 21.29 | ? | ? | ? |
0.866 | 1.080 | 6.235 | 20.92 | ? | ? | ? |
0.866 | 1.105 | 6.380 | 21.30 | ? | ? | ? |
0.866 | 1.085 | 6.264 | 20.91 | ? | ? | ? |
0.866 | 1.090 | 6.293 | 21.02 | ? | ? | ? |
Conclusion: the data from table 7 as can be seen, adopt assay method of the present invention, the content of silit in 11 experiment measuring temperature raising agents, the standard deviation of measurement result is 0.1449, relative standard deviation is 0.6858%, illustrate that this method measurement result accuracy height, measurement result are stable, disturb in the measuring process for a short time that selectivity is good.
Claims (7)
1. the Determination on content method of silit in the temperature raising agent comprises:
The temperature raising agent of calcination for the first time sample is to remove the uncombined carbon in the described sample;
Add the acid solution dissolving in the sample after the calcination, filter, obtain precipitation;
Add flux in described precipitation, calcination for the second time makes the oxidation of coal in the described precipitation become carbon dioxide, measures the amount of described carbon dioxide;
In company with doing blank assay, do not add the temperature raising agent sample, measure the amount of carbon dioxide in the blank assay;
Calculate the content of silit in the described temperature raising agent with the amount of the carbon dioxide that obtains in sample and the blank assay.
2. the Determination on content method of silit in the temperature raising agent as claimed in claim 1 is characterized in that: in the described calcination first time process, place 800 ± 10 ℃ muffle furnace to lead to oxygen calcination 1.0-1.5h the porcelain boat that described temperature raising agent sample is housed.
3. the Determination on content method of silit in the temperature raising agent as claimed in claim 1, it is characterized in that: obtain in the described precipitation process, add the aqueous hydrochloric acid solution that 40mL hydrochloric acid mixes with the water equal-volume in the sample after the calcination, 0.2 gram sodium fluoride, cover surface plate, 200 ℃~250 ℃ following heating for dissolving; Add hot water 50mL after the dissolving, boil 5min, with being covered with the ceramics funnel filtration with holes that thickness is the acid-washed asbestos of 10mm; Be the aqueous hydrochloric acid solution washing funnel 5~6 times of 5:95 with hydrochloric acid and water volume ratio, and all wash on the asbestos, be precipitated to neutrality with 70~80 ℃ hot wash again, will precipitate together with asbestos with tweezers and place porcelain boat.
4. the Determination on content method of silit in the temperature raising agent as claimed in claim 1 is characterized in that: in the described calcination second time process, the porcelain boat that precipitation is housed is placed baking oven, 110~115 ℃ of oven dry 1~1.5 hour; Add flux, with long hook porcelain boat is pushed into the centre position of 1250 ℃ of electric tube furnaces, the jam-pack plug, preheating 3min leads to oxygen combustion 5min, makes the oxidation of coal in the described precipitation become carbon dioxide.
5. as the Determination on content method of silit in claim 1 or the 4 described temperature raising agents, it is characterized in that: described flux is the potpourri of 0.5000 gram red copper and 0.1000 gram vanadium pentoxide.
6. the Determination on content method of silit in the temperature raising agent as claimed in claim 1, it is characterized in that: the amount of carbon dioxide records by carbometer, and the eudiometer tube rod reading of temperature raising agent sample is designated as X; The eudiometer tube rod reading of blank assay is designated as X
0
7. the Determination on content method of silit in the temperature raising agent as claimed in claim 6, it is characterized in that: the content of silit is calculated as follows in the described temperature raising agent,
W
SIC(%)=3.339(X-X
0)×f÷m
In the formula, m is sample size; F is temperature and pressure correcting coefficient, calculates according to existing method; 3.339 be converted into the coefficient of silit for carbon.
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CN103439213A (en) * | 2013-09-02 | 2013-12-11 | 武汉钢铁(集团)公司 | System detection method for components in industrial silicon carbide |
CN106769982A (en) * | 2016-12-12 | 2017-05-31 | 中核北方核燃料元件有限公司 | The assay method of carborundum content in a kind of composite material of silicon carbide |
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CN103439213A (en) * | 2013-09-02 | 2013-12-11 | 武汉钢铁(集团)公司 | System detection method for components in industrial silicon carbide |
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CN106769982A (en) * | 2016-12-12 | 2017-05-31 | 中核北方核燃料元件有限公司 | The assay method of carborundum content in a kind of composite material of silicon carbide |
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