YB/T 174.1-2000 Chemical analysis methods for silicon nitride bonded silicon carbide products - Determination of silicon nitride content by high pressure dissolution method
Some standard content:
81.080
Ferrous Metallurgy Industry Standard of the People's Republic of China YB/T 174. 1 2000
Chemical analysis for silicon nitride bonded silicon carbidc productDetermination of silicon nitride contentHigh pressure dissolve specimen method2000-07-26 Issued
State Metallurgical Industry Bureau Issued
2000-12-01 Implementation
YB/T 174.12000
Guangzeng Zhu installed bone allowed applicable film, will reduce the standard "the amount of sample taken, the end of the reputation to 2S, the increase in average negative pressure device: for the medical exploration of the continent in this standard in the steam bottle live set of limbs from the ball. This liquid is the Appendix A standard
This standard is the national standard of the six members of the old out of 11. Car logo from grams unit: Luo San Shi Huo Yi - Research Institute, this standard single is Beijing Energy, Zhou Shi.
1 Fan Yuan
People's Republic of China black metallurgy industry standard number silicon bonded silicon carbide products chemical analysis method high pressure dissolution method to determine the content of silicon nitride
Chenifeal aialvsils for silicon nllride bonded silon carbideproduci-Tetermina1ion af slllcou nitrlde coulnt-High pressure dissolve specimen metbudYB/T 174.12000
This standard specifies the method for determining the amount of hydrogen peroxide by high pressure sampling, reagents, standards, equipment, samples, analysis steps, expression of analytical results and allowable errors.
This standard applies to the determination of hydrogen peroxide in various micro-silicon products, the measurement range: hydrogen peroxide 13.Co%u.00,
2 Referenced Standards
The provisions contained in the following standards, which have been approved for use in this standard, constitute the text of this standard. When this standard is revised, the latest version shown is valid. All standards are subject to revision and the provisions of this standard shall be discontinued. The latest version of the standard book may be produced, GB/T2007.2-1987 Bulk, * product joint sample, company sample general method for sample preparation GH/17:18? Numerical rounding rules
GB/T10325-1S8 Only refractory products are allowed to be placed, selected, accepted, stored and transported GB/1176171SSR refractory materials are not refractory materials before 3 methods Summary
Test price Use high pressure to reduce the sample step decomposition, generate chain war, separate aging silicon and, in the presence of sodium hydroxide to make the oxygen escape, use acid liquid to gradually absorb·Repair the film, use the neutral method to determine the nitrogen content, and replace the net SiN. 4 Reagents
4.1 Acid AR
4.2 Hydrogenated phthalate (GR!).
4.3 Sodium complex (AR)
4.4 Salt cost 0.110g1.
4-5 Oxo-1.1/am
4.6 Banyin (5195)
4.7 Oxidized molten stock (0.)
4.8 Boric acid solution 1 (g/)
4.9 The pure precipitate was mixed with methyl red to pick up the indicator. The two green (.1% ethyl sa solution) 501m l. and methyl red (10ml with 1% ethanol). Haijie
Approved by the State Metallurgical Industry Bureau on July 26, 2000 and implemented on December 1, 2000
YB/17,1700
4.10 Incubate vanilla extract with phenol red solution as indicator: Take vanilla blue and phenol red (0.05g/ml) in 100ml of 23% ethanol, dissolve evenly, and mix with sodium chloride (0.1mnl/ml). 4.11 Salt standard3-3 Use 0.5u gate. Calculate the oxygen standard solution to turn purple, which is the end point. Formula 1: The concentration of the labeled solution. 2XOH
1 ×G
204.2 × V
Formula, .-room oxygen ratio standard solution mo!/LG
The mass basis
End time is the volume of sodium chloride consumed in the room. m..1m dimethicone potassium permanganate, 6/mol?
5.2n.1rm/1. Standard lysate of pulmonary gland standard wave. 11) 10m in a 31m. beaker, add 2 drops of bromine and red filter (4.10). Use organic sodium hydroxide standard concentration (4 .12> Titrate until the red color turns into a blue-purple color: Calculate the concentration of the hydrochloric acid standard solution according to formula (2).
In the formula: cHaI
The concentration of the standard solution of nitrification, mol/mol. Vca
The volume of the standard solution of nitrification during titration, ml.: The volume of the hydrochloric acid standard solution, ml..3.1mal The concentration of the hydrochloric acid standard solution for nitrification can be calculated by technology (calculation) 14 × cx 2. 50h 1
Wherein: 14
En's mass mo.
The concentration of the salt solution. n!/T..
2.5951 is calculated as the conversion efficiency of silicon chloride. G Instrument setting
6. 1($ 0. OUu 1 R)
6.2 High pressure sampler, as shown in Figure 1, six steel cups, poly bottle usually consists of three parts, the outer wing four need to be B smoke inside and outside, the working pressure is 1SMPa, when in use, there should be someone to monitor, kidney mountain full box temperature should be controlled. $1t
Stainless steel cup
6.3 Cai Chao installation: as shown in Figure 2.
YB/T174.12000
Figure high pressure sampler parts show production Peng
Polymer can be used
1-·Cold real life: 2-dimensional bottle collection system.-Moisture proof: 4--burning type pressure ear deionization request| |tt||Figure 2 Schematic diagram of Yingdi equipment
6. Oven heat power kW. Product temperature 33:
6.5 Flask ml.
6.6 Tetraethylene beaker 330.
For the sample
Semi-shaped products, take samples according to GB/T105251338 Section 5. After the relevant materials are drilled and adjusted, remove the surface of the part, and then take 1Wg more as the experimental sample. For the amorphous materials, you can lose 51717GB:T:2007.2 for joint sampling and sample preparation, 7.2 samples
YB/T 1/4. 1 2000
For shaped products, grind the laboratory sample obtained in 7.1 to less than 2.0 μm, reduce it to 100: then grind it with calcium sulfate to less than C.9mm, reduce it to 255: then grind it with calcium sulfate while sieving until all of it passes through 0.1bmm sieve. For amorphous materials, divide 25 of the laboratory sample obtained in 7.1, grind it with calcium sulfate while sieving until all of it passes through 0.15 μm, finally put the test piece into (20,000) fuel, and cool it in a dryer to a thickness of 8. Analysis steps
8-1 Test sample
Use two test samples for analysis, weigh U.2)g from each sample, and weigh n(00)g. 6.2. Complete white test
Use the same test bottle as the test sample to make a blank test. 8.3 Calibration test
Then the sample is divided into the standard mix of the same type
8.4.1 Place the sample (R1) in a high-pressure dissolver, add 5 mL of slow (4.4), add 5 mL of hydrofluoric acid (4.5). Decompose the sample in an oven (6.1) at 160 (local: ℃) for 12 minutes. When warm, take it out and cool it. Use hot water to dissolve the sample in the capsule of the high-pressure dissolver. In the polyethylene cup, there is 1 300 mL of boric acid (4.1). In the national model B operation cup (e.6), use: * small piece of German low-intake flow cup inner wall, make the solution and wash all transferred to the beaker, while washing, control the solution level to about 75 =., now half, use slow quantitative filter (if necessary, we pulp filter + more to take over in the new (6.5). Use hot hydrochloric acid (4.) to wash the beaker and select 3~1 times, 2-small piece of pond paper to wipe the filter cup 2 times. Transfer all the objects to the stagnation bucket, wash the precipitate once with hot hydrochloric acid (4.6), Then use hot water to precipitate 3-1 times, control the filtrate to about 2C9ml. Dissolve for testing Si.V, use for testing, add effective sodium oxide solution (.m), add tri-la small slope glass ball (earth explosion Buddha), and add dropwise. 8.4.3 Take 1) 250ml of orthoboric acid solution (4.5) in a cup. Add 3 drops of diancresol green and methyl red indicator (4.9) in a button bottle. Use the required acid to increase When the solution is completely red, adjust the zero point of the burette, connect this bottle to the lower end of the burette, and drain. When the blue color appears, add the standard salt (4.11) until it turns red, until the red color disappears within 5min. After the evaporation, record the number.
9 Expression of the results
9.1 Calculation of the value
Direct ratio (calculate the mass content of hydrogenated base: W4 - TV × =9
Wherein: percentage of the nitrogen base, %; standard hydrochloric acid used to determine the concentration of the chemical partner/ml.: V-volume of silver standard solution consumed during titration: m-test mass.
The results of the test are in accordance with T/T8170-987. 9.2 Acceptance of analysis value
Check whether the analysis value of the standard sample in the calibration test is consistent with its standard value. When the analysis value of the standard sample is consistent with its standard value, the analysis of the component in the sample is valid, and the final result of the component can be calculated. Otherwise, the determination of the component should be repeated.
9.3 Calculation of the final result
YD,T 174,2000
When the difference between the two valid analysis values is not greater than the corresponding allowable difference (see Table 1), calculate the arithmetic mean, according to (a/T8170-1987, rounded to the first decimal place, and shall be used as the final difference of the component, otherwise Appendix A (marked when indicated) reverse: additional analysis data processing, the average value obtained is rounded to the second decimal place according to G/T8170.17 as the node of the component,
10 allowable difference
The allowable difference of the two single-time discount values obtained under the condition of recurrence is shown in Table 1. 1 allowable coupons
standard non-yuan allowable view
215. 0U ~2U, 69
to. om- so, o
The sample is likely to be
the new
special difference.
YB/T 174.1
Appendix 4
(Standard Supplementary Elements
Additional Analysis and Data Processing Procedureswww.bzxz.net
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