JB/T 10152-2000 Silicon carbide special products Silicon nitride bonded silicon carbide plate
Some standard content:
JB/T10152--2000
Silicon nitride bonded silicon carbide plate is a widely used replacement product with good high temperature performance. This standard was formulated in combination with domestic and foreign production and sample testing conditions when international standards and foreign advanced standards have not yet been collected. Appendix A of this standard is the appendix of the standard.
This standard is proposed and managed by the National Technical Committee for Standardization of Abrasives and Grinding Tools. The responsible drafting units of this standard: Zhengzhou Abrasives and Grinding Research Institute, Boai High Temperature Materials Factory. The main drafters of this standard: Xiao Junming, Liu Feng, Ma Jinfeng, Wang Xu, Li Zhiqiang, Liu Ming. 353
Machinery Industry Standard of the People's Republic of China
Special products of silicon carbide-Slab of silicon nitride bonded silicon carbide
Special products of silicon carbide-Slab of silicon nitride bonded silicon carbideJB/T10152-2000
This standard specifies the code, size specifications, technical requirements, inspection methods, inspection rules and marking, packaging, transportation and storage of silicon nitride bonded silicon carbide plate products.
This standard is applicable to sheds, flame baffles and other boards of silicon nitride bonded silicon carbide with working temperature not higher than 1500C. 2 Referenced standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard is published, the versions shown are valid. All standards will be revised, and the parties using this standard should explore the possibility of using the latest versions of the following standards. GB191—1990 Pictorial symbols for packaging, storage and transportation
GB/T2997-1982 Test method for apparent porosity, water absorption, bulk density and true porosity of dense shaped refractory products GB/T3001-—1982 Test method for flexural strength of refractory products at room temperature GB/T3002—1982 Test method for flexural strength of refractory products at high temperature GB/T5072—1985 Test method for compressive strength of dense shaped refractory products at room temperature 3 Product classification
See Table 1 for product shape, code and mark.
Flame baffle
Approved by the State Machinery Industry Bureau on January 4, 2000354
Product marking
a/b/c/d/e
Implemented on June 1, 2000
4 Dimensions
For the dimensions of flame baffle (NC-G), see Table 2.
500～900
900～1100
11001200
1200~1500
For the dimensions of shed (NC-P), see Table 3.
JB/T10152—2000
Table 1 (end)
4.3 Shapes and dimensions not included in this standard shall be agreed upon by the supplier and the buyer. 5 Technical requirements
5:1 Chemical composition and physical properties shall comply with the provisions of Table 4. d
Product marking
Fe2O, %
Sioz, %
Dimensional deviation shall comply with the provisions of Table 5.
Length and width direction
Thickness direction
Flatness shall comply with the provisions of Table 6.
Size range
Allowable deviation
JB/T10152~-2000
Edge and corner defects shall comply with the provisions of Table 7.
Size range
Edge and corner defects
500～~1000
Apparent porosity, %
Volume density·g/cm
Flexural strength at room temperature, MPa
Flexural strength at high temperature (1400C).MPa
Compressive strength at room temperature, MPa
Size range
500～1000
500～1000
≥130
Allowable deviation
5.5 The depth of the ablation pit is less than or equal to 2.5mm, the length is less than or equal to 10mm, and the number is less than or equal to 5. 5.6
No cracks or cracks are allowed.
Testing method
The chemical composition of SiC.SiN., Fe,O;, Si, SiO, shall be tested in accordance with the provisions of Appendix A (Appendix of the standard). The apparent porosity and bulk density shall be tested in accordance with the provisions of GB/T2997. The room temperature flexural strength shall be tested in accordance with the provisions of GB/T3001. The high temperature flexural strength shall be tested in accordance with the provisions of GB/T3002. 6.4
The room temperature compressive strength shall be tested in accordance with the provisions of GB/T5072. 6.6 Dimensional inspection: Use a steel tape measure and a steel ruler with an accuracy of 0.2inm for inspection. 6.7
Flatness inspection: Place the product on the workbench and use a flat ruler and a feeler gauge to check, mm
6.8 Inspection of corner defects: Steel rulers and specially manufactured measuring devices and prism meters that can be tightly fitted on the corners of the product and have a 356
scale that slides in the specified direction can be used for inspection. JB/T10152—2000
6.9 Inspection of corrosion pits: Use a vernier caliper with a graduation value of 0.02mm for inspection. Products without obvious pitting and erosion after processing and grinding are not counted as corrosion. 6.10
Inspection of cracks and fissures: Visual inspection. If a hammer is used to knock and a dull sound is heard, it is judged to have a dark crack. 7 Inspection rules
7.1 Inspection classification
Silicon nitride bonded silicon carbide plates are divided into type inspection and factory inspection. 7.2 Type inspection
Type inspection shall be conducted in any of the following cases: a) Trial production of new products or transfer of old products to other factories for production; b) After formal production, if there are major changes in the process or raw materials, the performance of the product may be affected; c) During formal production, type inspection shall be conducted every six months; d) After a long period of suspension of production, the product is resumed; e) There is a significant difference between the factory inspection result and the last type inspection result; f) The quality supervision agency proposes a requirement for type inspection. 7.2.1 Inspection items
7.2.1.1 Appearance inspection: visual inspection.
7.2.1.2 The results of the dimensional inspection shall comply with the provisions of Table 5. 7.2.1.3 The results of the flatness inspection shall comply with the provisions of Table 6. 7.2.1.4 The results of the inspection of appearance defects, melting pits and cracks, and fissures shall comply with the provisions of 5.4 to 5.6. 7.2.7.5 The results of the inspection of the chemical composition and physical and mechanical properties of the product shall comply with the provisions of Table 4. 7.2.2 Sampling method
7.2.2.1 Determination of inspection batch
Each batch of products is an inspection batch.
7.2.2.2 Selection of samples
Randomly select 1 piece from the same batch of products, and then divide it into several small pieces and randomly select 5 pieces. 7.2.3 Judgment rule
The sample shall be executed according to the inspection judgment rule in Table 8. If the inspection fails, it is allowed to double the sampling quantity for re-inspection; if the re-inspection still fails, the batch of products shall be judged as unqualified.
Volume
Flexural strength at room temperature
7.3 Factory inspection
Sampling quantity
Factory inspection shall be carried out according to the provisions of 7.2.1.1~~7.2.1.4. Number of qualified judgments
Judgment rules
Number of unqualified judgments
8 Marking, packaging, transportation and storage
JB/T10152-2000
8.1 The name, size, quality, manufacturing date, inspector and trademark of the product should be clearly marked on one corner of each board. 8.2 The packaging should have anti-vibration and moisture-proof measures.
8.3 The packaging box should be clearly marked with specifications, quantity, quality, manufacturer, factory date, fragile, moisture-proof and other words, and comply with the provisions of GB191.
8.4 During transportation, the products must be guaranteed not to be damaged or exposed to rain, etc. 8.5 The products should be stored in a dry and ventilated warehouse. 358
A1 Preparation of sample
JB/T10152—2000
Appendix A
(Appendix of standard)
Chemical analysis method of silicon carbide bonded silicon carbide plate The sample block is broken into small pieces with a diameter of less than 3mm. Take 20g by quartering method, put it in a corundum mortar and grind it to pass through a 180-mesh screen. The iron filings are absorbed by a magnet and dried at 105-110℃ for 1h. Take it out, cool it and set it aside. A2 Determination of silicon dioxide
A2.1 Principle of method
Silicon dioxide is heated and dissolved in a hydrofluoric acid-hydrochloric acid-potassium chloride solution to form potassium fluorosilicate precipitation, which is hydrolyzed in boiling water. The generated hydrofluoric acid is titrated with a sodium hydroxide standard solution to calculate the mass fraction of silicon dioxide. A2.2 Reagentswww.bzxz.net
A2.2.1 Hydrochloric acid: p=1.18g/mL.
A2.2.2 Hydrofluoric acid: mass fraction 40%.
A2.2.3 Potassium chloride.
A2.2.4 Potassium chloride: 10%, weigh 10g potassium chloride and dissolve it in water, dilute to 100mL. A2.2.5 Potassium fluoride ethanol solution: 5%, weigh 5g potassium chloride and dissolve it in 50ml water, add 50mL ethanol and mix well. A2.2.6 Phenolic acid indicator: 1%, weigh 1g phenolic acid and dissolve it in 60mL ethanol, dilute to 100ml with water, neutralize with 0.1mol/L sodium hydroxide standard solution until it just turns red. A2.2.7 Potassium hydrogen phthalate: reference reagent A2.2.8 Sodium hydroxide standard solution: 0.1mol/L. Preparation: weigh 4g sodium hydroxide and dissolve it in freshly boiled and cooled water, add a little barium chloride, dilute to 1L, let it stand, absorb the clarified liquid and store it in a plastic bottle for later use. Calibration: Accurately weigh 0.4g of potassium hydrogen phthalate dried at 105~110℃ for 1h, and place in three 250mL conical flasks, add 100mL of freshly boiled and cooled distilled water, shake to dissolve, add 2~3 drops of phenolic acid indicator, and titrate with sodium hydroxide standard solution until the end point is slightly red.
Calculate the concentration of sodium hydroxide standard solution according to formula (A1): m
c= 0.204 0 V
-concentration of sodium hydroxide standard solution, mol/L; where: c—
m---the amount of potassium hydrogen phthalate weighed, g; V is the volume of sodium hydroxide standard solution consumed during titration, mL. A2.3 Analysis steps
?(A1)
Weigh about 0.3g of A1 preparation sample, accurate to 0.0001g, into a 250mL plastic beaker, add 10mL of hydrofluoric acid and 10mL of hydrochloric acid (1+1), heat in a constant temperature water bath at 80-90℃ for 20min, remove, stir, cool, add 0.5-1g excess of solid potassium chloride until saturated, let stand for 3-5min (the precipitation temperature of potassium fluorosilicate should be 15-20℃), filter with a plastic funnel, wash with potassium fluoride (10%) solution 2-3 times, remove the precipitate and put it into the original plastic cup, add 10ml of potassium chloride ethanol (5%) solution and 10 drops of phenolic acid indicator along the wall of the cup, titrate with sodium hydroxide standard solution until slightly red (the volume is not counted at this time), quickly add about 180mL of freshly boiled distilled water and 10 drops of indicator, titrate with sodium hydroxide standard solution until the slightly red color does not disappear. Calculate the mass fraction of silicon dioxide according to formula (A2): w(Si02) = XV× 0.01502×100m
·(A2)
JB/T 10152—2000
Wherein: c——concentration of sodium hydroxide standard solution, mol/L; V—volume of sodium hydroxide standard solution consumed during titration, mL; sample volume, g.
A2.4 The allowable error shall be as specified in Table A1.
Content range
Allowable error
A3 Determination of silicon
A3.1 Principle of the method
10. 01 ~ 30. 00
The silicon in the sample is oxidized to silicon dioxide by nitric acid. The original silicon dioxide in the sample and the newly generated silicon dioxide are dissolved in a hydrofluoric acid-hydrochloric acid-potassium chloride solution to form potassium fluosilicate precipitation, which is hydrolyzed with boiling water. The generated hydrofluoric acid is titrated with a standard sodium hydroxide solution. The original silicon dioxide in the sample is subtracted from the total amount of silicon dioxide to obtain the silicon content through conversion. A3.2 Reagents
A3.2. 1 Nitric acid: p=1. 40 g/mL.
A3.2.2 The rest is the same as A2.2.
A3.3 Analysis steps
Weigh about 0.3 g of sample prepared in A1, accurate to 0.0001 g, into a 250 mL plastic beaker, add 10 mL of hydrofluoric acid, 1 mL of nitric acid, and 10 mL of hydrochloric acid (1+1). The rest of the operation is the same as in A2.3. Calculate the mass fraction of silicon according to formula (A3):
(c×V× 0.015 02 × 100 - w(Si02)× 0.467 4w(S) =
Wherein: c—
concentration of sodium hydroxide standard solution, mol/L; V—volume of sodium hydroxide standard solution consumed in titrating silicon dioxide in A3.3, ml; m—
-sample volume in A3.3·g.
A3.4 Allowable error is as specified in Table A2.
Content range
Allowable error
A4 Determination of total silicon
A4.1 Principle of the method
0.51 ~~ 3. 00
The sample is heated and melted with sodium hydroxide and potassium nitrate, and the molten block is decomposed by hydrochloric acid. The solution is evaporated to wet salt, hydrochloric acid is added, and animal glue is used to make silica, and the precipitate is calcined to constant weight, and then treated with hydrofluoric acid-sulfuric acid to volatilize and remove silicon in the form of silicon tetrafluoride. The weight difference before and after the hydrofluoric acid treatment is the amount of silicon dioxide in the precipitate. The amount of residual silicon dioxide in the filtrate is determined by the silicon molybdenum blue spectrophotometry, and the total silicon content can be calculated by adding the two.
A4.2 Reagents
A4.2.1 Sodium hydroxide.
A4.2.2 Potassium nitrate.
Hydrochloric acid: (5+95).
Animal glue solution: 1%.
Ammonium molybdate: 5%, weigh 5g of ammonium molybdate and dissolve it in 100mL of water. JB/T 10152—-2000
A4.2.6 Ammonium ferrous sulfate: 6%, weigh 6g of ammonium ferrous sulfate and dissolve it in water, add 2-3 drops of sulfuric acid, dilute to 100mL, and prepare it before use.
A4.2.7 Oxalic-sulfur mixed acid: (1+1), measure 1 part of 5% oxalic acid and 1 part of (1+3) sulfuric acid, mix them. A4.2.8 Hydrofluoric acid: mass fraction 40%.
A4.2.9 Sulfuric acid: (1+ 1).
A4.2.10 Silicon dioxide standard solution: 1 ml. Contains 0.05 mg of silicon dioxide. Accurately weigh 0.1000 g of silicon dioxide (high purity reagent) burned at 1000°C in platinum, add 2 g of anhydrous sodium carbonate (standard reagent) and mix carefully, then cover with 0.5 g, send it into a high-temperature furnace at 860~~900°C to melt for 20 minutes, take it out, rotate it, let the molten material adhere to the inner wall of the crucible, cool it, clean the outer wall, and then Leach out with hot water in a polyethylene beaker, cool it, transfer it to a 1000mL volumetric flask, dilute it to the mark with water, shake it well and immediately transfer it to a dry plastic bottle for storage for later use. Take 100mL of the above solution and put it into a 200mL volumetric flask pre-filled with 10mL hydrochloric acid (2mol/L), dilute it to the mark with water, shake it well, and it is the silica standard solution (containing 0.05mg/mL silica). A4.3 Analysis steps
A 4.3.1 Weigh about 0.2g of the sample of A1, accurate to 0.0001g, into a crucible containing 5g of sodium hydroxide that has been dehydrated beforehand, add 2g of potassium nitrate, put it into a high-temperature furnace at room temperature, heat it from room temperature to 700℃, melt it for 10~15min, take it out, cool it, transfer it and cover it in a beaker, the beaker contains about 100mL of boiling water, heat it to dissolve the melt, wash out the crucible and cover it, add 20mL of hydrochloric acid, place it on a sand bath and evaporate it to wet salt. Then add 20mL of hydrochloric acid. Stir it evenly, heat it on a water bath for 5~10min, add 10mL of animal glue solution (1%) while it is hot, stir it thoroughly, and keep it warm on a 70℃ water bath for 10min. Remove it, add 20~30mL of hot water, stir to dissolve the salts, filter with medium-speed filter paper, collect the filtrate in a 250mL volumetric flask, wash the precipitate and beaker with hot hydrochloric acid (5+95) several times, and then wash with hot water until there is no chlorine. Move the filter paper and the precipitate into a platinum crucible, carefully dry it, put it in a high-temperature furnace, gradually increase it from room temperature to 1000℃, burn it for 1h, take it out, cool it, weigh it, and repeat the operation until constant weight. After burning, first moisten the precipitate with water, then add 5mL of hydrofluoric acid and 1~2 drops of sulfuric acid (1+1), evaporate it on a sand bath until white sulfuric acid smoke emerges, remove it, cool it, add 3~5mL of hydrofluoric acid, continue to evaporate until the white sulfuric acid smoke disappears, then place it in a high-temperature furnace, burn it at 1000C for 15min, take it out, cool it, and weigh it. Repeat the operation until constant weight. After cooling the filtrate and washings to room temperature, dilute to 250mL, draw 5mL into a 100mL volumetric flask, add 10mL of water, 5mL of ammonium molybdate (5%), shake well (when the room temperature is below 20°C, slightly warm the solution to 20°C before coloring), let it stand for 10~~15min to allow it to completely colorize. Add 20ml of grass-sulfur mixed acid (1+1)., 5mL of ammonium ferrous sulfate (6%), dilute to the mark with water, and shake well. Use water as a reference, measure the absorbance at a wavelength of 700nm on a spectrophotometer with a 1cm colorimetric filter, and subtract the blank absorbance to obtain the number of milligrams of silicon dioxide from the standard curve.
The total silica mass fraction is calculated according to formula (A4): w[SiOT}] =
Where: m2—the mass of the precipitate and the crucible before the hydrofluoric acid treatment, g, m1—the mass of the precipitate and the crucible after the hydrofluoric acid treatment, g; m3—the number of milligrams of silicon dioxide obtained from the curve; ——the mass of the sample, g.
m×250
×1000
·(A4)
A4.3.2 Working curve drawing: Take 8 portions of hydrochloric acid solution A4.2.3, 12mL each, and put them into 8 100mL volumetric flasks respectively. Use a microburette to add 0.00, 0.20, 0.50, 1.00, 2.00, 4.00, 6.00, 8.00mL of silica standard solution in sequence, add water to 35mL, and 5mL of ammonium aluminate (5%). The following operations are the same as A4.3.1. After subtracting the blank absorbance from the absorbance value at each point, draw the working curve. A4.4 The allowable error is as specified in Table A3.
A5 Determination of ferric oxide
A5.1 Principle of the method
JB/T 10152—2000
Add allowable error
In an ammonia solution (pH 8~11.5), trivalent iron ions react with sulfosalicylic acid to form yellow sulfosalicylic acid iron complex salt, and its content is determined by absorption spectrophotometry.
A5.2 Reagents
A5.2.1 Sulfosalicylic acid: 15%, weigh 15g sulfosalicylic acid and dissolve it in 100mL water. A5.2.2 Hydrochloric acid: (5+95).
A5.2.3 Ammonia water: a=0.90g/ml.
A5.2.4 Ferric oxide standard solution: 0.1mg/mL. Accurately weigh 0.1000g of dried ferric oxide (spectrally pure), place it in a 250mL beaker, add 30mL of hydrochloric acid (1+1), heat to dissolve, and transfer 1.000ml to a volumetric flask after cooling. Dilute to the mark with water and shake well. A5.3 Drawing of working curve
Put 10mL of hydrochloric acid (5+95) solution into 7 50mL volumetric flasks respectively, and use a microburette to add 0.00, 0.501.00, 2.00, 4.00.6.00.8.00mL of ferric oxide standard solution (0.1mg/mL) in sequence, develop color according to the sample operation method, and draw the working curve by subtracting the absorbance of the blank test from the measured absorbance. A5.4 Analysis steps
Pull 25mL of the solution prepared in A4.3 into a 50mL volumetric flask, add 5mL of sulfosalicylic acid (15%), add nitrogen water until it turns stable yellow, add 8-10 drops in excess, dilute with water to the mark, and shake. Dry filter into a dry beaker, use water as a reference solution, use a 1cm colorimetric tube to measure its absorbance at a wavelength of 420nm, subtract the absorbance of the blank test, and find the content of ferric oxide on the working curve. Calculate the mass fraction of ferric oxide according to formula (A5): w(Fe,O,) =
Where: m1---weighed sample amount, g;
take the amount of ferric oxide found on the working curve in the sample solution. m2---
A5.5 The allowable error is as specified in Table A4.
Content range
Allowable error
A6 Determination of silicon nitride
A6.1 Principle of the method
0.25~0.50
0. 51 ~1. 00
(A5)
The sample is decomposed with sodium hydroxide, and the escaped ammonia is absorbed by boric acid solution with nitrogen as the carrier. Then, bromocresol green and methyl red are used as indicators, and the standard hydrochloric acid solution is used to titrate until the test solution turns red but not green. The nitrogen content is calculated according to the number of milliliters of the standard hydrochloric acid solution consumed, and the mass fraction of silicon nitride can be obtained by conversion. A6.2 Reagents
A6.2.1 Sodium hydroxide.
A6.2.2 Boric acid solution: 1%, weigh 1g of boric acid and dissolve it in 100mL of water. 362
JB/T10152—2000
A6.2.3 Bromocresol green and methyl red mixed indicator: Mix 50mL of bromocresol green (0.1% ethanol solution) with 10mL of methyl red (0.1% ethanol solution).
A6.2.4 Hydrochloric acid standard solution: 0.05mol/L, take 4.2mL of hydrochloric acid, dilute to 1000ml with water, and shake well. Weigh 0.0500~0.1000g of anhydrous sodium carbonate (high purity reagent) dried at 250C in advance into a 300mL conical flask, add 100mL of freshly boiled and cooled water, shake to dissolve, add 2~3 drops of methyl orange indicator, and then titrate with hydrochloric acid standard solution until the test solution suddenly changes from yellow to orange-red as the end point.
Calculate the concentration of the hydrochloric acid standard solution according to formula (A6): m
Where: c——concentration of the hydrochloric acid standard solution, mol/I.; m
——amount of anhydrous sodium carbonate weighed, g;
V—volume of hydrochloric acid consumed in titration.mL.
A6.3 Analysis steps
·(A6)
Weigh about 0.2g of the sample prepared in A1, accurate to 0.0001g, and put it in a nickel containing 4g of sodium hydroxide, and then cover 6g of sodium hydroxide on the sample, cover it with a nickel crucible cover (with a small hole), put the nickel into a glass reaction bottle, cover it with a ground-mouth reaction bottle cover, connect one end of the reaction bottle to nitrogen with a latex tube, and connect the other end to the absorption bottle (as shown in Figure A1). The absorption bottle contains 100mL of boric acid solution (1.%), and add 3 to 5 drops of indicator. Place the reaction bottle in a furnace and slowly heat the temperature from room temperature to 550-600℃, and keep it warm at this temperature. During the heating process, the continuously escaping nitrogen turns the absorption liquid from red to green. Add hydrochloric acid standard solution in time and continuously until the absorption liquid stops turning green. Perform a blank test in the same way.
Calculate the mass fraction of nitrogen according to formula (A7):
w(N) = X (V, - V) X 0. 014 0m
Where: c—concentration of hydrochloric acid standard solution, mol/L; Vz——-volume of hydrochloric acid consumed in titration, mL;
V,-volume of hydrochloric acid consumed in blank test, mL;
sample volume in A6.3, g.
Calculate the mass fraction of silicon nitride according to formula (A8): X 100
w(Si,N,) = w(N) X 2.503 9
Glass reaction bottle
Absorption bottle
A6.4 The allowable error shall be as specified in Table A5.
Chengtae
High temperature furnace
Schematic diagram of nitrogen determination
Allowable error
(A7)
( A8 )
Determination of silicon carbide
The mass fraction of silicon carbide is calculated according to formula (A9): JB/T 10152
w(SiC) = ([SiO2(T)] - w(SiO,) -- w[SiO2(si)] - w[SiO2(sis,]) 0. 667 3 In: w[SiO2(s]=(Si) x2. 139 5;w[SiO2(sig,)]=w(SigN)x1.2849. A7.1 Allowable error is as specified in Table A6.
Allowable error90g/ml.
A5.2.4 Ferric oxide standard solution: 0.1mg/mL. Accurately weigh 0.1000g of dried ferric oxide (spectrally pure), place it in a 250mL beaker, add 30mL of hydrochloric acid (1+1), heat to dissolve, cool and transfer to 1.000ml. Dilute to the scale with water in a volumetric flask and shake well. A5.3 Drawing of working curve
Take 10mL of hydrochloric acid (5+95) solution and put it into 7 50ml volumetric flasks respectively, add 0.00, 0.501.00, 2.00, 4.00.6.00.8.00mL of ferric oxide standard solution (0.1mg/mL) in turn with a microburette, develop color according to the sample operation method, and draw the working curve by subtracting the absorbance of the blank test from the measured absorbance. A5.4 Analysis steps
Pull 25mL of the solution prepared in A4.3 into a 50mL volumetric flask, add 5mL of sulfosalicylic acid (15%), add nitrogen water until it turns stable yellow, add 8-10 drops in excess, dilute with water to the mark, and shake. Dry filter into a dry beaker, use water as a reference solution, use a 1cm colorimetric tube to measure its absorbance at a wavelength of 420nm, subtract the absorbance of the blank test, and find the content of ferric oxide on the working curve. Calculate the mass fraction of ferric oxide according to formula (A5): w(Fe,O,) =
Where: m1---weighed sample amount, g;
take the amount of ferric oxide found on the working curve in the sample solution. m2---
A5.5 The allowable error is as specified in Table A4.
Content range
Allowable error
A6 Determination of silicon nitride
A6.1 Principle of the method
0.25~0.50
0. 51 ~1. 00
(A5)
The sample is decomposed with sodium hydroxide, and the escaped ammonia is absorbed by boric acid solution with nitrogen as the carrier. Then, bromocresol green and methyl red are used as indicators, and the standard hydrochloric acid solution is used to titrate until the test solution turns red but not green. The nitrogen content is calculated according to the number of milliliters of the standard hydrochloric acid solution consumed, and the mass fraction of silicon nitride can be obtained by conversion. A6.2 Reagents
A6.2.1 Sodium hydroxide.
A6.2.2 Boric acid solution: 1%, weigh 1g of boric acid and dissolve it in 100mL of water. 362
JB/T10152—2000
A6.2.3 Bromocresol green and methyl red mixed indicator: Mix 50mL of bromocresol green (0.1% ethanol solution) with 10mL of methyl red (0.1% ethanol solution).
A6.2.4 Hydrochloric acid standard solution: 0.05mol/L, take 4.2mL of hydrochloric acid, dilute to 1000ml with water, and shake well. Weigh 0.0500~0.1000g of anhydrous sodium carbonate (high purity reagent) dried at 250C in advance into a 300mL conical flask, add 100mL of freshly boiled and cooled water, shake to dissolve, add 2~3 drops of methyl orange indicator, and then titrate with hydrochloric acid standard solution until the test solution suddenly changes from yellow to orange-red as the end point.
Calculate the concentration of the hydrochloric acid standard solution according to formula (A6): m
Where: c——concentration of the hydrochloric acid standard solution, mol/I.; m
——amount of anhydrous sodium carbonate weighed, g;
V—volume of hydrochloric acid consumed in titration.mL.
A6.3 Analysis steps
·(A6)
Weigh about 0.2g of the sample prepared in A1, accurate to 0.0001g, and put it in a nickel containing 4g of sodium hydroxide, and then cover 6g of sodium hydroxide on the sample, cover it with a nickel crucible cover (with a small hole), put the nickel into a glass reaction bottle, cover it with a ground-mouth reaction bottle cover, connect one end of the reaction bottle to nitrogen with a latex tube, and connect the other end to the absorption bottle (as shown in Figure A1). The absorption bottle contains 100mL of boric acid solution (1.%), and add 3 to 5 drops of indicator. Place the reaction bottle in a furnace and slowly heat the temperature from room temperature to 550-600℃, and keep it warm at this temperature. During the heating process, the continuously escaping nitrogen turns the absorption liquid from red to green. Add hydrochloric acid standard solution in time and continuously until the absorption liquid stops turning green. Perform a blank test in the same way.
Calculate the mass fraction of nitrogen according to formula (A7):
w(N) = X (V, - V) X 0. 014 0m
Where: c—concentration of hydrochloric acid standard solution, mol/L; Vz——-volume of hydrochloric acid consumed in titration, mL;
V,-volume of hydrochloric acid consumed in blank test, mL;
sample volume in A6.3, g.
Calculate the mass fraction of silicon nitride according to formula (A8): X 100
w(Si,N,) = w(N) X 2.503 9
Glass reaction bottle
Absorption bottle
A6.4 The allowable error shall be as specified in Table A5.
Chengtae
High temperature furnace
Schematic diagram of nitrogen determination
Allowable error
(A7)
( A8 )
Determination of silicon carbide
The mass fraction of silicon carbide is calculated according to formula (A9): JB/T 10152
w(SiC) = ([SiO2(T)] - w(SiO,) -- w[SiO2(si)] - w[SiO2(sis,]) 0. 667 3: w[SiO2(s]=(Si) x2. 139 5;w[SiO2(sig,)]=w(SigN)x1.2849. A7.1 Allowable error is as specified in Table A6.
Allowable error90g/ml.
A5.2.4 Ferric oxide standard solution: 0.1mg/mL. Accurately weigh 0.1000g of dried ferric oxide (spectrally pure), place it in a 250mL beaker, add 30mL of hydrochloric acid (1+1), heat to dissolve, cool and transfer to 1.000ml. Dilute to the scale with water in a volumetric flask and shake well. A5.3 Drawing of working curve
Take 10mL of hydrochloric acid (5+95) solution and put it into 7 50ml volumetric flasks respectively, add 0.00, 0.501.00, 2.00, 4.00.6.00.8.00mL of ferric oxide standard solution (0.1mg/mL) in turn with a microburette, develop color according to the sample operation method, and draw the working curve by subtracting the absorbance of the blank test from the measured absorbance. A5.4 Analysis steps
Pull 25mL of the solution prepared in A4.3 into a 50mL volumetric flask, add 5mL of sulfosalicylic acid (15%), add nitrogen water until it turns stable yellow, add 8-10 drops in excess, dilute with water to the mark, and shake. Dry filter into a dry beaker, use water as a reference solution, use a 1cm colorimetric tube to measure its absorbance at a wavelength of 420nm, subtract the absorbance of the blank test, and find the content of ferric oxide on the working curve. Calculate the mass fraction of ferric oxide according to formula (A5): w(Fe,O,) =
Where: m1---weighed sample amount, g;
take the amount of ferric oxide found on the working curve in the sample solution. m2---
A5.5 The allowable error is as specified in Table A4.
Content range
Allowable error
A6 Determination of silicon nitride
A6.1 Principle of the method
0.25~0.50
0. 51 ~1. 00
(A5)
The sample is decomposed with sodium hydroxide, and the escaped ammonia is absorbed by boric acid solution with nitrogen as the carrier. Then, bromocresol green and methyl red are used as indicators, and the standard hydrochloric acid solution is used to titrate until the test solution turns red but not green. The nitrogen content is calculated according to the number of milliliters of the standard hydrochloric acid solution consumed, and the mass fraction of silicon nitride can be obtained by conversion. A6.2 Reagents
A6.2.1 Sodium hydroxide.
A6.2.2 Boric acid solution: 1%, weigh 1g of boric acid and dissolve it in 100mL of water. 362
JB/T10152—2000
A6.2.3 Bromocresol green and methyl red mixed indicator: Mix 50mL of bromocresol green (0.1% ethanol solution) with 10mL of methyl red (0.1% ethanol solution).
A6.2.4 Hydrochloric acid standard solution: 0.05mol/L, take 4.2mL of hydrochloric acid, dilute to 1000ml with water, and shake well. Weigh 0.0500~0.1000g of anhydrous sodium carbonate (high purity reagent) dried at 250C in advance into a 300mL conical flask, add 100mL of freshly boiled and cooled water, shake to dissolve, add 2~3 drops of methyl orange indicator, and then titrate with hydrochloric acid standard solution until the test solution suddenly changes from yellow to orange-red as the end point.
Calculate the concentration of the hydrochloric acid standard solution according to formula (A6): m
Where: c——concentration of the hydrochloric acid standard solution, mol/I.; m
——amount of anhydrous sodium carbonate weighed, g;
V—volume of hydrochloric acid consumed in titration.mL.
A6.3 Analysis steps
·(A6)
Weigh about 0.2g of the sample prepared in A1, accurate to 0.0001g, and put it in a nickel containing 4g of sodium hydroxide, and then cover 6g of sodium hydroxide on the sample, cover it with a nickel crucible cover (with a small hole), put the nickel into a glass reaction bottle, cover it with a ground-mouth reaction bottle cover, connect one end of the reaction bottle to nitrogen with a latex tube, and connect the other end to the absorption bottle (as shown in Figure A1). The absorption bottle contains 100mL of boric acid solution (1.%), and add 3 to 5 drops of indicator. Place the reaction bottle in a furnace and slowly heat the temperature from room temperature to 550-600℃, and keep it warm at this temperature. During the heating process, the continuously escaping nitrogen turns the absorption liquid from red to green. Add hydrochloric acid standard solution in time and continuously until the absorption liquid stops turning green. Perform a blank test in the same way.
Calculate the mass fraction of nitrogen according to formula (A7):
w(N) = X (V, - V) X 0. 014 0m
Where: c—concentration of hydrochloric acid standard solution, mol/L; Vz——-volume of hydrochloric acid consumed in titration, mL;
V,-volume of hydrochloric acid consumed in blank test, mL;
sample volume in A6.3, g.
Calculate the mass fraction of silicon nitride according to formula (A8): X 100
w(Si,N,) = w(N) X 2.503 9
Glass reaction bottle
Absorption bottle
A6.4 The allowable error shall be as specified in Table A5.
Chengtae
High temperature furnace
Schematic diagram of nitrogen determination
Allowable error
(A7)
( A8 )
Determination of silicon carbide
The mass fraction of silicon carbide is calculated according to formula (A9): JB/T 10152
w(SiC) = ([SiO2(T)] - w(SiO,) -- w[SiO2(si)] - w[SiO2(sis,]) 0. 667 3 In: w[SiO2(s]=(Si) x2. 139 5;w[SiO2(sig,)]=w(SigN)x1.2849. A7.1 Allowable error is as specified in Table A6.
Allowable error1000g is placed in a 300mL conical flask, 100mL of freshly boiled and cooled water is added, shaken to dissolve, 2-3 drops of methyl orange indicator are added, and then titrated with hydrochloric acid standard solution until the test solution changes from yellow to orange-red as the end point.
Calculate the concentration of hydrochloric acid standard solution according to formula (A6): m
Where: c——concentration of hydrochloric acid standard solution, mol/I.; m
——amount of anhydrous sodium carbonate weighed, g;
V—volume of hydrochloric acid consumed in titration.mL.
A6.3 Analysis steps
·(A6)
Weigh about 0.2g of the sample prepared in A1, accurate to 0.0001g, and put it in a nickel crucible containing 4g of sodium hydroxide, and then cover the sample with 6g of sodium hydroxide, cover the nickel crucible with a lid (with a small hole), put the nickel in a glass reaction bottle, cover the ground mouth reaction bottle cap, connect one end of the reaction bottle to nitrogen with a latex tube, and the other end to the absorption bottle (as shown in Figure A1). The absorption bottle contains 100mL of boric acid solution (1.%), and 3 to 5 drops of indicator. Put the reaction bottle in a furnace, slowly heat it from room temperature to 550-600℃, and keep it warm at this temperature. During the heating process, the continuously escaping nitrogen turns the absorption liquid from red to green. Add hydrochloric acid standard solution in time and continuously until it turns red, until the absorption liquid does not turn green, which is the end point, and perform a blank test in the same way.
Calculate the mass fraction of nitrogen according to formula (A7):
w(N) = X (V, - V) X 0. 014 0m
Wherein: c—concentration of hydrochloric acid standard solution, mol/L; Vz——-volume of hydrochloric acid consumed in titration, mL;
V,-volume of hydrochloric acid consumed in blank test, mL;
Sample volume in A6.3, g.
Calculate the mass fraction of silicon nitride according to formula (A8): X 100
w(Si,N,) = w(N) X 2. 503 9
Glass reaction bottle
Absorption bottle
A6.4 The allowable error shall be as specified in Table A5.
Chengtae
High temperature furnace
Schematic diagram of nitrogen determination
Allowable error
(A7)
( A8 )
Determination of silicon carbide
The mass fraction of silicon carbide is calculated according to formula (A9): JB/T 10152
w(SiC) = ([SiO2(T)] - w(SiO,) -- w[SiO2(si)] - w[SiO2(sis,]) 0. 667 3 In: w[SiO2(s]=(Si) x2. 139 5;w[SiO2(sig,)]=w(SigN)x1.2849. A7.1 Allowable error is as specified in Table A6.
Allowable error1000g is placed in a 300mL conical flask, 100mL of freshly boiled and cooled water is added, shaken to dissolve, 2-3 drops of methyl orange indicator are added, and then titrated with hydrochloric acid standard solution until the test solution changes from yellow to orange-red as the end point.
Calculate the concentration of hydrochloric acid standard solution according to formula (A6): m
Where: c——concentration of hydrochloric acid standard solution, mol/I.; m
——amount of anhydrous sodium carbonate weighed, g;
V—volume of hydrochloric acid consumed in titration.mL.
A6.3 Analysis steps
·(A6)
Weigh about 0.2g of the sample prepared in A1, accurate to 0.0001g, and put it in a nickel crucible containing 4g of sodium hydroxide, and then cover the sample with 6g of sodium hydroxide, cover the nickel crucible with a lid (with a small hole), put the nickel in a glass reaction bottle, cover the ground mouth reaction bottle cap, connect one end of the reaction bottle to nitrogen with a latex tube, and the other end to the absorption bottle (as shown in Figure A1). The absorption bottle contains 100mL of boric acid solution (1.%), and 3 to 5 drops of indicator. Put the reaction bottle in a furnace, slowly heat it from room temperature to 550-600℃, and keep it warm at this temperature. During the heating process, the continuously escaping nitrogen turns the absorption liquid from red to green. Add hydrochloric acid standard solution in time and continuously until it turns red, until the absorption liquid does not turn green, which is the end point, and perform a blank test in the same way.
Calculate the mass fraction of nitrogen according to formula (A7):
w(N) = X (V, - V) X 0. 014 0m
Wherein: c—concentration of hydrochloric acid standard solution, mol/L; Vz——-volume of hydrochloric acid consumed in titration, mL;
V,-volume of hydrochloric acid consumed in blank test, mL;
Sample volume in A6.3, g.
Calculate the mass fraction of silicon nitride according to formula (A8): X 100
w(Si,N,) = w(N) X 2. 503 9
Glass reaction bottle
Absorption bottle
A6.4 The allowable error shall be as specified in Table A5.
Chengtae
High temperature furnace
Schematic diagram of nitrogen determination
Allowable error
(A7)
( A8 )
Determination of silicon carbide
The mass fraction of silicon carbide is calculated according to formula (A9): JB/T 10152
w(SiC) = ([SiO2(T)] - w(SiO,) -- w[SiO2(si)] - w[SiO2(sis,]) 0. 667 3 In: w[SiO2(s]=(Si) x2. 139 5;w[SiO2(sig,)]=w(SigN)x1.2849. A7.1 Allowable error is as specified in Table A6.
Allowable error
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