This standard specifies the method summary, reagents, instruments, samples, analysis steps, expression of analysis results and tolerance for the determination of free silicon content by molybdenum blue photometry. This standard is applicable to the determination of free silicon content in silicon nitride bonded silicon carbide products. Determination range: free silicon 100%~2.00%. YB/T 174.3-2000 Chemical analysis method for silicon nitride bonded silicon carbide products Determination of free silicon content by molybdenum blue photometry YB/T174.3-2000 Standard download decompression password: www.bzxz.net

1cs 81. 080
Ferrous Metallurgy Industry Standard of the People's Republic of China YB/I 174.32000
Chemical analysis for silicon nitride bundedsilicon carbide productsDeterniination of free silicon conlent-Molybdcmum blue photometric method
Chemical analysis for silicon nitride bundedsilicon carbide productsDeterniination of free silicon conlent-Molybdcmum blue photometric method methocl2000-07-26 Issued
National Bureau of Metallurgical Industry Issued
2000-12-01 Implementation
YB/T1/4.320DG
In the past, the gas volumetric method for determining the dissociated silicon was based on the gas state parameters of the gas, which not only required some complicated measurement equipment, but also required some more parameters to be measured, and the analysis steps were too complicated. The technical standard also divided the gas volumetric method into the method for determining the dissociated silicon, which was too complicated. The technical standard A was also a standard for the single standard.
This standard puts forward and summarizes the technical requirements for material standardization. This standard was drafted by: Luoyang Refractory Research Institute. 4 Standard drafters: Guan Shineng, Zhou Ming.
1 Scope
Metallurgical industry standard of the People's Republic of China Chemical analysis method for silicon nitride boded silicon carbide products-Determination of free silicon content by molybdenum blue photometry
Chemical analysis far sillcon nitride boded silicon carbide product-
Ihe termiauion of free siliron cnntent.-Mulybdeaum blur phutumetrie raethdYB/T174.3—2000
This standard covers the main contents of the molybdenum blue photometric method for determining free siliron, reagents, transformers and equipment, test parameters, analysis steps, description of analysis results and tolerances
This standard is applicable to the determination of free silicon in silicon nitride boded silicon carbide products. The determination range is 0.10% to 3.0%. 2 Reference standards
The provisions contained in the following standards constitute the records of technical standards through reference in this standard. After the publication of this standard, the total versions shown are valid. All standards will be revised. The parties who use this standard should consider the possibility of using the following standard versions. GB/T2007.21SA7 General rules for sampling and inspection of sensitive mineral products Manual inspection method GB/T8170-1S87 Numerical diagnosis and specification GB/T10325-1985 Refractory products stacking, sampling, acceptance, storage and delivery rules: GB/1717-998 Refractory granules and amorphous refractory materials YB/1174.12C03 Silicon hydride and silicon carbide products Comparative analysis of silicon fluoride by high pressure dissolution filtration Method 3 Summary
The test is carried out by boiling the sample with sodium hydride and sodium carbonate solution to convert the free type in the sample into soluble silica gel salt and dissolve it. The chelating agent is not degraded. After the separation, the silica in the chlorine is measured by the material photometric method. The converted ions are 4 reagents
4.7 The density of oxygen is 168/cm.
4.2 Ammonium hydroxide NHMoUU solution 0/
4.3 Bisphenol A: Take 15% hydrochloric acid (HC, O, -2H) and dissolve it in 250ml sulfuric acid (1), dilute with water to 100l. Mix about.
4.4 Sulfur dioxide [FeS): (NH), S·H) (40g/) Weigh 4g of chlorinated acid and immerse it in water for 5 minutes (11). Dilute with water and filter it for 10 minutes (filter if necessary). 4.5 Hydrochloric acid (m=1.15R/cm).
4.6 Acid 1-1).
National Metallurgical Industry Weekly 2DC0-07-25 approved 2000-12-01 implementation
4.7 When acid (1-5)
YR/T174.3-2000
4.B, 1--nitro indicator minus (10) water brain 9 prepared 4.9 dioxide standard stock solution (0.500Cmgml, weigh U.S03. First, 1K0T of the burning piece and cool to room temperature, the carrying brick is placed in a car with water and sodium carbonate, very spoonful, another anhydrous limit blue is placed on it, the upper cover is left to flow, the medicine must be protected. The product is 10 melted and then cooled. Put the whole thing in a tight burning forest, Use 100ml boiling water, rinse with hot water, cover, cool to room temperature, put into 10ccml volumetric flask, add water to the mark, mix and store in a 4.0 standard silicate solution (mm25/): transfer 500ml of the standard silicate solution (4.9) to a 10-mouth bottle, dilute with water to the mark, store in a plastic bottle, 5.1 large (16c.5001g) 5-2 light welcome 5.3 agglomerate m. 5 sample sampling system YB/174. [—201 7.2 1. 7 Analysis steps
Sample
Two samples were measured, the net amount was 0.25g, and the concentration was 0. C35 1 R-7.7 Blank test monitor
Carry out blank test together with the sample. The reagents used must be taken from the reagent bottle. 7.3 According to the positive test
, analyze the sample with the standard column number:
7.4 Determination
7.4.1 Put the material cup into the material cup, add 10Wm sodium oxide solution (4.1). Set the surface of the blood on a hot bath, stir once every 1: pass the paper with a speed machine, and then put it in the cup (5.3). Oxygen oxidation method (4.1) end burns to remove the sediment 1--item: wash the anti-starch 4--5 times with hot water. 7.4.2 Method report includes 2 net 24-two sales examples (4.8. Heat test <4.) until colorless, roll on the market to reduce the body to 15ml. Then add 2 3ml1. hydrochloric acid (4.5), transfer to 230mL container bottle and cool to room temperature. Dilute to scale with water sample, transfer 7.4.3 or 5 (centiliter ml. free solution (7.4.2 month 1tm. wear element. Add 15ml. water and ml. key night according to 1.2) shake at room temperature 51 (. Then in water resources ten micro two ml grass sparse mixed acid 1.3 and ml sieve night stand (1.) month water pre-drop main column No,
7.44 in the colorimetric industry (see length 1), the wavelength of the light meter at m, with the type of self-falling liquid (7.2 as a reference to measure its absorbance and then stop the above) on the corresponding two to do, Table 1
as a detaching agent
made 5 on the safe your company
n. 1--6. 5?
0. 50 --2. 0u
7.5.1 0.0.c, ..39.1.502.00,2.=0ml. standard micro-(45) in 1-100ml bottle. Add 3
YB/T174.3-2000
2.5mL plate cut (4.71 water to below 2mL and connect 7.4.~7.4.4 with 3em comparison, spectral wavelength i93nm, measure its absorbance with reagent as reference. Prepare standard curve. 7.5.2 Collect 9.2.00, 4.00.G.0.8.0, 10.C0ml. Standard solution (1.10) is divided into 3 groups of 100ml. Place 2.5ml in volumetric bottles. Add water to less than 20ml and proceed according to 7.4.3 to 7.4.4. At 0.5 colorimetric, measure the absorbance at 69 on the spectrophotometer plate with the reagent blank H as reference and draw a standard curve. Analysis results and expression
8.1 The calculation of the free silicon mass fraction is based on formula (1): W(S)-
Wherein: w
the mass threshold content of free silicon, %;
m X 0. 4G7 2
The volume of the test sample obtained from the working curve is 1
the virtual year of the test sample + 8
, and the total volume of the test solution is ml.
The coefficient of free silicon dioxide is calculated, X
The results are in accordance with the above-mentioned /131701987 drug price specification 8-2 decimal places for acceptance of the drug vehicle state
The analysis column is marked with a zero standard. Only when the analytical value of the standard is consistent with its criterion, the analysis of the component in the medical work is valid, and the calculation of the final result of the criterion component can be carried out. This rule should be reversed for the component.3 Calculation of the final result wwW.bzxz.Net
When the absolute value of the two effective discounts is not the same as the difference in the purchase price, see Table 2, calculate the half-mean of the method, the decimal point of the B31701987 full period, the contract revision case is still established as the final result of the deduction, otherwise the appendix #A (marked appendix) is used for auction and discount data processing: the same as the current value method G/870-197 is also used as the state contract revision rate to round up the price of the public.
9 Allowable difference
Under the condition of the crown, the difference between the three single analysis values ​​is 2, and the allowable difference in Table 3 is the full value of my
1. x ~ 3. Jc
Standard element related
Test clearance
On the upper side is T——single analysis minimum:
-allowable difference,
TB/T174.3—20DC
(Standard Appendix)
Additional analysis and data processing procedures
,
++++:+,
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