This standard specifies the method summary, reagents, instruments and equipment, samples, analysis steps, expression of analysis results and tolerance for the determination of silicon carbide content by high pressure dissolution method. This standard is applicable to the determination of silicon carbide content in silicon nitride bonded silicon carbide products. Determination range: silicon carbide 60.00% to 80.00%. YB/T 174.2-2000 Chemical analysis method for silicon nitride bonded silicon carbide products High pressure dissolution method to determine silicon carbide content YB/T174.2-2000 Standard download decompression password: www.bzxz.net

ICS 81. OBD
Ferrous metal industry standard of the People's Republic of China Y5/T 174.22000
Chemical analysis for silicon nitride bonded silicon carbide product--High pressure dissolve specimen method
2000-07-26 Issued
State Metallurgical Industry Bureau Issued
2000-12-01 Implementation
YB/T174.2—2000
This standard adopts a test method which is completely different from the method for measuring silicon carbide content in silicon carbide products. The high pressure dissolve specimen method avoids the determination of total carbon and free carbon, and can also determine the content of nitride at the same time. Since aluminum has a great influence on the test results of silicon carbide, the lead content in silicon carbide is reported by comparing two test standards.
This standard is the only standard issued by the National Technical Committee for Standardization of Pyrotechnic Materials and is regulated by 1. The unit of this standard is: Pyrotechnic Materials Research Institute. The author of this standard is Wu Yudong. Yin Mingxiu. 1. Scope
Chemical analysis for nitrilin bonded silicon carbide product
Deterininatian of silicon carbide content High pressure dissolution method
B/T174.2--2000
This standard specifies the requirements for the high pressure dissolution method for the determination of silicon carbide content. Reagents, preparation, testing, analysis and screening, analysis results and allowable error.
This standard is applicable to the determination of the chemical content of dried silicon carbide bonded silicon carbide products. Determination range: 60.00%-0.Cc%. 2 Reference standards
The following standards contain gold clauses, which constitute the clauses of this standard through the six standards listed in the standard. This standard is published. All the six standards are valid. All standards will be used, and all parties using the standard should explore the use of the following standards. The possible use of new versions of the standard is recorded: GB/2007.2:1997 Sampling of sensitive products, G/5059.6-1985 Analysis method for iron content before ignition - Determination of % oxidation by EA plate method G3/T8170198? Standard value compensation for thermal preparation GH/T10325—1988 Standard requirements for sampling, acceptance, storage and disposal B/1555.1995 Chemical analysis method for determination of silicon carbide in refractory materials G1777155F YT172, 1200C cylinder chemical analysis method for determination of silicon hydride 3 Method Summary
The test product is decomposed under high pressure and the silicon carbide is transferred into a liquid in the form of a wire. The decomposition is not equal to that of the nitric acid. The free silicon is separated from the test material by pressure and the magnetic resonance 4 is obtained by subtraction. Reagents
4.1 Acid (AR).
4.2 Prepare the reagent: 2.5 parts of sodium hydroxide, 1.5 parts of anhydrous carbonyl and 0.7 parts of boric acid, mix in a spoon and pour into a bottle. 4.3 Hydrochloric acid = -,13 g/m*.
4.4 Magnesium chloride (MgSO4/).
4.5 Hydrogen phosphate (MgSO4=1.11 g/cm2)
4.6 Hydrogen phosphate (MgSO4/).
State Metallurgical Industry Bureau 20000726 approved
200C-12-01 implementation
4.7 Salt (5+95)
5 Instruments and equipment
5. 1 liter (accuracy 0.000 1 g).
YB/T174:2—2000
5.2 High temperature dissolving sampler, as shown in Figure 1, with stainless steel rods and outer cups, and tetraethylene inner rods. The maximum annual pressure is 15, and when in use, it is monitored by personnel to prevent the oven temperature from being disturbed. 0
: New standard
National" High temperature dissolving sampler sound diagram
5.3 Drying heating power teaching kW + maximum T working temperature). 5.4 Put a tetrachloroethylene beaker [300ml.>,
6 Sample
Take the sample and connect it to YE/T174.1-2000 respectively. 7.1 and 4.2 carry out 7 analysis steps
7.1 Sample
Use one sample for determination, take 0.20g of each sample and grind it to more than 0.000 1, 7.2 Empty testbzxZ.net
Carry out empty test with the sample, and the reagents are from the same test bottle. 7.3 Calibration test
Treat the sample with the standard sample.
￥H/T174.2—2000
7.4.1 Place the sample (7.1) in a high pressure dissolver 5.), add 5 mL of hydrochloric acid (4.3) and 5 mL of hydrochloric acid (4.5). Decompose the sample in a 1Y oven at 169℃:2. Take out when it reaches the warm point and cool. Wash the tetrafluoroethylene in the high-pressure sampler with water, transfer all the precipitates to a 1000 m3 tetrahydrofuran (4.1% ethyl acetate) beaker, filter with slow quantitative filter paper (add paper pulp if necessary). Collect the filtrate in a 5m2 flask, wash with hydrochloric acid (4.7% HCl) 3-4 times, wipe the filter paper twice, transfer all the precipitates to a flask, wash with hot water (4.7% HCl) 4 times, and then wash the precipitate with water 3-4 times, and control the liquid volume to about 2m2. The filtrate is used for filtering and filtering with anti-flow. 7.4.2 Wrap the newly obtained precipitate with filter fiber, heat it in a constant temperature, carefully dry it, and place it at high temperature until it gradually cools to 750°C. Cool it, moisten it with water, and add 4 drops of nitric acid (4.4), 4 vegetable acid 4.5), add about 10L of hydrogen peroxide (4.5) on a low humidity evaporator, raise the humidity for a period of time, then burn it out at 750℃ for 10 minutes, cool it in a desiccator to room temperature, and then weigh it in a car. 7.3 Test the chemical content (A1), 30%), add 2-3 mixing agents to the mixture after 7.3 determination, and cover it with a filter containing flux, cover it with a cap and leave it in the original state. Then put it in a high temperature plate, heat it from low temperature to 11G2%, keep it for 30-40min., wait for the sample to be completely decomposed, take it out, cool it and separate the total amount of GR/T1e555.S, collect 300mL of the filtrate, concentrate the net amount to 15ml. Measure the amount of A according to the EDTA method of GH/T5069.6, and divide the amount by the corresponding amount , get SC content. B Analysis results and expression
Day.1 Calculation of analysis value
Day.1.1 Calculate the mass content of silicon dioxide according to the formula: w(%)..=mxIn
Formula: W is the mass percentage of silicon dioxide, %m-the mass percentage of the blank:
the mass of the block flow
m the mass of the sample.
The result is B/91,1S. The selection rule is corrected to a decimal of 81.2. If the value of the two is (A1.%), then the formula (2) is used to calculate the mass content of silicon dioxide: W(%)
1-4×1CC,-A,0.%
W-the mass percentage of silicon dioxide, %; The length refers to the mass percentage of the sample and the amount of precipitation g.
The result obtained shall be rounded to two decimal places according to the standard of GB/T8170997. 6.2 The score value shall be rounded to two decimal places according to the standard of GB/T8170997. The score value selected in the test shall be consistent with the standard value. Only when the selected score is consistent with its standard, the analysis of the component in the test sheet is invalid, and the final result of the component can be calculated. Otherwise, the determination of the separated component shall be carried out. 8.3 The final result shall be calculated. When the absolute values ​​of the two valid analysis cases are not larger than the corresponding allowable values ​​(Table 1), the average of them shall be calculated and rounded to two decimal places according to the standard of GB/T317-197 as the final result of the component. The product shall be processed according to the standard (Table 1) and the average shall be calculated according to the standard.Modulo the required decimal places as the final result of the component.
9 Allowable pad
YH/T174.2-2000
The allowable difference between the two single analysis values ​​under the condition of weight is shown in Table 1.
Net quantity range
60. 0u~ 80. 00
Standard sample is used for evaluation
Sample is used in the above process
Order or deduction;
Allowed and,
YB/T174.2-2000
Appendix A
(Standard Supplement)
Additional analysis and data processing procedures
Link, median
FI+Ixs
t,It, ft.-
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