This standard specifies the method summary, reagents, instruments, samples, analysis steps, expression of analysis results and tolerance for the determination of ferric oxide by o-phenanthroline photometric method. This standard is applicable to the determination of ferric oxide in silicon nitride bonded silicon carbide products. Determination range: ferric oxide 0.10%~1.50%. YB/T 174.4-2000 Chemical analysis method for silicon nitride bonded silicon carbide products o-phenanthroline photometric method for determination of ferric oxide content YB/T174.4-2000 Standard download decompression password: www.bzxz.net

IL8 81.080
Ferrous Metallurgy Industry Standard of the People's Republic of China YR/T 174. 4—2000
Chemical analysis for silicon nitride bonded silicon carbideproduct:Determination of iron oxide content-o-Phcnanthroline photometric method2000-07-26 Issued
Issued by State Bureau of Metallurgical Industry
Implemented on 2000-12-01
YB/T174.4—2000
When silicon content is high, the determination of iron oxide will be affected. The standard is to use the o-nitrogen separation method with a smaller value of PII to separate silicon carbide. The resistance of silicon can be measured. The analysis result is reliable. The technical standard A is the requirement of the standard. Www.bzxZ.net
This standard is issued by the Technical Committee of Refractory Standardization and is drafted by: This standard was drafted by: Ling Jiaqian, Yuan Mingxiu 1 Scope
Metallurgical Industry Standard of the People's Republic of China Chemical Analysis Method for Silicon Carbide Bonded Silicon Carbide Product Determine Natlon or Iron Oxide Content by Photometric Method
Chemical analysls for silicon carbide bonded sillcon carbide product Determine natlon or iron oxdde content by o-Pheuanihroline photometric method YB/T*74.4--2000
This standard specifies the following three requirements for the method: formula, reagent, solution, test steps, analysis results and acceptable solutions.
This standard is applicable to the determination of ferrous oxide in silicon carbide products in the general field. Source: Trichloroethane 0.10%~1.FC%.? Cited Standards
The following standards contain the provisions of this standard that are referenced in this standard and are defined as the provisions of this standard. When this standard was published, the versions shown were valid. The standard department will revise the number of standards and promote the discussion of the various components of the standard. The latest versions of the following standards are used as possible parts: G1/T2207.3-1S87 Bulk code product sampling, sample preparation method GB/TR170187 Principles of revision of paragraph value
GB: T103251888 Increase of fire-resistant products, acceptance, storage and transportation rules GB/T17317-1558 Sampling of fire-resistant raw materials and amorphous refractory materials YT1/T:7-.1-2000 Nitriding station chemical analysis of carbonized products Bridge point method High pressure dissolution method Determination of effective 3 methods Summary
The sample is treated with nitric acid and sulfuric acid. The sample is washed with hydrochloric acid, filtered, and filtered. The test solution is melted with a mixed flux tower to obtain the residual iron dioxide. The lack of 1> reaches the original For the nature ("), in a weakly acidic solution, (1) with o-dimethoxyphene or extremely red complex, dry spectrometer and measure its absorbance at wavelength Umn. The main trioxide ratio of iron oxide is 4 parts of iron oxide, the total amount of titanium oxide is 4 reagents || tt || 4.1 mixed reagent: 1.5 parts of acid-free water, 0.5 parts of carbon-free potassium hydroxide and 0.7 parts of non-acidic solution and 1.2 parts of acid (a = 1.42g/cm
4.3 Hydrogen oxychloride = 1.13g.
4.4 Hydrogen oxychloride (+1).
4. Yimo 5+35
1.6 Salt shock (=11)
4.7 Salt cost Hydroxylamine solution 1U.1g/mL1.
National Institute of Mineral Resources 2000-07-26 Approved 2000-12-01 Bottled
YB/T 174.42000
4.8 Prepare diisocyanate (3.011.) with 10% alcohol to prepare 4.9 ammonium acetate (.2g/m,1
4.10 Standard stock solution of ferric oxide: weigh 31.900g of ferric oxide (standard reagent) pre-heated at 6C9C for 30min in a cup, add a little water, add 40mL of (4.6), heat at low temperature to dissolve until clear, cool, transfer to a 100mL volumetric flask and dilute with water to a dense concentration, adjust, and transfer 1:1 of this solution to ferric oxide 4.11 standard solution. Transfer 51.00mL of ferric oxide standard solution to (4.1) at 3C tmL of the customer's dosage, dilute with a small amount to 400°C - mix well, this solution 1ml into 10c.20 titanium trioxide 4.12 = titanium dioxide standard solution 1 transfer to FU.00mL ferric oxide standard solution (4.12 = 1! In a 500nl. equal volume bottle, add water to the scale, mix until the iron content is 5. Instruments
5.1 Balance (accuracy c.53016
5.2 Spectrophotometer
6 Sample
Sampling and sample preparation are carried out according to 7.1 and 7.2 of YB/174.1-2601. 7. Analysis Step
Use two samples for determination. Transfer 0.35 ml to each sample and adjust to 0.GC518. 7.2 Empty Test
Carry out empty test with the sample. The reagents are taken from the same reagent plate. 7.3 Calibration Test
Analyze the sample with the same type. 7.4 Determination
7.4.1 Add the test bone-platinum blood, add about 10 drops of acid (4.3), 4-5 drops of sulphuric acid (4.4), and evaporate to dryness at low temperature on an electric furnace. Increase the concentration as much as possible. White smoke, remove and cool: virtual acid 4.6>ml heat 10mia~15mim. Remove, cool, use slow fixed paper to be full, can bear to 25. Mother bottle, use hot plate (4.5) to wash platinum and slag 7 times, book small piece of paper to wipe the blood and then open hot water to kill 5 times, cool to room temperature, dilute with water to degree, mix, thank the main test trihydride ferrous raw
7.4.2 will line and filter paper transfer dust fine adjustment. Low temperature and high temperature furnace meter burnt into powder, take out and cool: add 2-3 mixed flux (1.1> mix: 2 mixed dense moist blue its On the whole, place the cover pin in a high-temperature furnace at about 400°C, gradually raise the temperature to 1:30 and hold for 3min-min, and take out the sample after it is completely decomposed. Cool part. 7.4.3 Place 5L of water and 5L of hydrochloric acid (4.6) in a 20) [. beaker and heat until the sample is completely dissolved. Heat with warm water and transfer to a 250-capacity bottle. Cool in a room and dilute to the scale. The residual oxide amount is measured:
7.4.2 7.4.1 Test 1al-10cm㎡. Add about 5L. Transfer 50 ml of 7.4.3 solution into the certified volumetric flask: add 5 ml of hydrochloric acid and amine solution (4.7) ml each into each volumetric flask. Fill the flask with water ([methylenediamine] 0.9 ml). The solution should be within 3-10% of the original volume. Check the release rate with test paper. Check for 0 min. 7.1.5 Suitable chromatic aberrations (see Table III): Spectrophotometer at wavelength 51°C with the empty space in the test column as reference. Measure the photometric value of hydrogen and iron. Compare with the standard curve YA/T 174.4-200°C 5. 14: ~ 3. 25
juice: northern rat oxidized iron, containing 10% iron oxide, see 7.5 standard curve drawing
.25~1.5
7.5.1 Transfer 50.10, 1.0c1.10, 2.0c.2.50ro1. ferric dioxide standard solution 1 (4, 12). Place in two 100ml volumetric flasks, add about 50mL of water. Follow 7.4.4, open 5cm colorimetric, install a photometer with 51Cnm as the reagent, measure the absorbance at the port and draw a standard curve. 7.5.2 Transfer 0, 0.5r.=.00, 1.50, 2.00.2.50ml. ferric dioxide: standard solution 1 (4.11> Place in a group of 100ml bottles, add water to about mL., follow 7.1.1 In parallel. Use a 0.5 cm colorimetric tube, at the spectrophotometer length of 51 nm, with the reagent white fire as reference, measure the absorbance, and then prepare a standard curve. 8 Expression of analysis results
B.1 Calculation of analysis values ​​
The formula (1) is used to calculate the mass percentage of trioxide: m×V.-mxV/v×100-.
Formula: W The mass percentage of titanium dioxide, 141
The main "titanium dioxide" content is obtained from the standard curve: the residual "emulsified titanium dioxide" content is obtained from the standard curve; the main three-titanium dioxide content is determined by the test method, and the residual titanium dioxide content is determined by the test solution: the volume of the test sample is:
The test solution is designed to be heated to a temperature m.
The obtained value is rounded to a decimal point according to the content rule of G/T6170-1987, and the analysis value of the test product is consistent with the standard value according to the variation correction test result! Only if the analysis value of the standard sample is consistent with the standard value, the analytical information of the component in the sample is valid and the calculation of the component can be carried out according to 83. Otherwise, the new method should be considered in the determination.
B-3 Calculation of final result
When the absolute difference between the two valid analysis values ​​is not acceptable (according to Table 2, the arithmetic mean of the six values ​​shall be rounded to two decimal places before calibration (GB/T91) 17) as the final result of the component. Otherwise, the addition and data processing shall be carried out directly. The average value 817-187 obtained by the vertical method is rounded to two decimal places as the total value of the result. The allowable difference between the two monitoring values ​​​​obtained in the vertical component 1 is shown in Table 9. Table of allowable difference
Including standard
3. 5C -- 1. 5C
Standard wine, especially the film
Trial release price evaluation
Carry out,
Single government office value:
Allow and.
YR/T174-4—2000
Appendix A
(Standard)
Additional analysis and data processing procedures
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