GB/T 5686.6-1988 Chemical analysis methods for manganese silicon alloys - Determination of carbon content by gas volumetric method

GB/T 5686.6-1988 Chemical analysis methods for manganese-silicon alloys - Determination of carbon content by gas volumetric method GB/T5686.6-1988 Standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Chemical analysis method of silicomanganese alloy
Gas volumetric method for the determination of carbon content
This standard is applicable to the determination of carbon content in silicomanganese alloy. Determination range: 0.100% ~ 4.000%, UDC 669. 74' 782
GB 5686. 6 --- 88
This standard complies with GB1467-...78 General Principles and General Provisions of Metallurgical Product Chemical Analysis Method Standard". 1 Method Summary
The sample is placed in a tubular combustion furnace for heating and combustion through oxygen. The generated mixed gas such as carbon monoxide is collected in a gas measuring tube after desulfurization, and then the carbon dioxide in it is absorbed by potassium monoxide solution. The difference in volume before and after absorption is the carbon monoxide volume, which is then converted into carbon content. 2 Reagents and materials
Flux: pot particles (0.4~0.8 mm), copper, iron powder, five chemical second, etc., the carbon content in the flux is not more than 0.002%. 2.2 Asbestos fiber.
2.3 Soda lime or pseudo hydroxide,
2.4 Alumina: active, granular.
Manganese dioxide: active, granular.
Sulfuric acid (p 1.84 g/mL).
Sulfuric acid (0.1±100): add methyl red solution to turn red 2.8 Chromic acid saturated sulfuric acid solution: add potassium hydroxide or chromic anhydride to saturated nitric acid (2.6) and use the above clear solution. 2.9 Potassium hydroxide solution (40%).
Sodium chloride solution (26%): use methyl red solution as an indicator and add sulfuric acid (11) until acidic, oxygen: purity greater than 99.5%.
3 Instruments and equipment
3.1 Gas container carbonization is shown in the figure below.
3.1.1 Washing bottle (5): Contains saturated sulfuric acid solution (2.8) with chromic acid. 3.1.2 Washing bottle (6): Contains broken stone fire or hydroxide 3.1.3 Drying tower (7.8): Contains lead oxide (2.4). High temperature combustion tube (9): Φ×T,, mn; 23～24×600. 3. 1. 4
Tubular combustion furnace (10): The current can be adjusted to ensure the required temperature for burning the sample. 3.1.6 Asbestos fiber (11): Burn until there is no carbon. 3.1.7 Brown sulfur tube (12): Contains manganese hydride (2.5) Approved by the Ministry of Metallurgical Industry of the People's Republic of China on February 2, 1958 and implemented on March 1, 1989
1 Oxygen cylinder: 2 Oxygen meter 18 Flushing bottle: 4 Micro-flow meter, 6 Washing bottle: 10 Drying cake; 9 High temperature environment tube; 10 Tube or combustion furnace, 1 Rock sugar red fiber, 12 Desulfurization tube, 15 Closed carbon position (including; condenser a, air pipe b, level bottle c, absorber d, small case c, three-way piston f, oscillometer g), 14 High temperature control ink, 15 Frosted glass case, 16 Porcelain boat
3.1.8 Porcelain boat (16): 88mm or 97mm long, should be pre-tested: 1200℃ tube Burn in a combustion furnace with oxygen until there is no carbon. It can also be burned in a high-temperature furnace at 1000℃ for more than 4 hours. After cooling, place in a non-grease-coated desiccator containing alkali asbestos (or city coal) and anhydrous calcium hydroxide.
3.1.9 Gas measuring tube (b): Contain sodium chloride solution (2.10) or sulfuric acid solution (2.7). Each grid scale is 0.05mL, which is engraved under standard conditions of 16℃ and 101.32kPa (760mmHg). 3.1.10 Absorber (d): Contain potassium hydroxide solution (2.9). 3.1.71 Small piston (e), only with - can pass through the atmosphere. 3.2 Long hook, made of low-carbon nickel-chromium wire or heat-resistant alloy wire. 3.3 Mercury barometer: The air pressure value should be calibrated according to formula (1): P -P/ (1—0. 000 163 t -0. 002 6 c8s240. 000 000 2 11) In the play, P
-corrected air bed value, kPa,
-air pressure measured by mercury barometer, kPa, t-temperature at the location of mercury barometer, ℃;
-latitude at the location of mercury barometer.;
4 Sample
Height of the mercury barometer, m. All rust-silicon samples passed the 0.125mm sieve. 5 Analysis steps
5. 1 Sample quantity
Weigh the sample and flux according to Table 1.
0. 400~1. 200
>1.200-2, 50
>2.50~4.00
5.2 Blank test
Sample area
Carry out a blank test together with the sample.
5.3 Preparation before analysis
GB 5686.6-88
Copper oxide
0. 5--1, 0
Rat oxide + pentoxide
Iron powder + hydrogenated steel
Vanadium divanadium
(1: 1)
0. b~1, 0
0. 5-~1. 0
+iron powderbZxz.net
0, 5 --1, c
Raise the furnace temperature to 1200～1350℃, check if the pipeline and piston are leaking, whether the device is working properly, burn the standard sample, and check the instrument and operation.
5. 4 Determination
Put the sample 5.1) in the porcelain plate (3.1.8), cover the baking agent according to Table 1, push the porcelain boat into the highest temperature of high-temperature combustion, immediately plug the frosted plug (15), open the three-way valve (f) on the carrier gas meter, and adjust the oxygen flow rate to 120140 mL/min. Keep the oxygen flowing for about 3 minutes to keep the temperature of the high-temperature combustion tube constant. According to the operating procedures of the volumetric carbon analyzer, the mixed gas is introduced into the gas tube. After narrowing and absorption, the reading is measured. After confirming that the residual gas volume has not changed, the frosted glass is opened and the porcelain boat is pulled with a long hook to check the block. After confirming that the combustion is complete, the residual gas is vented. 6 Calculation
Calculate the percentage of carbon according to formula (2): C (%) - :A=4)-Y4×IX100
Wherein: A
16℃ air pressure 101.32kPa, when acidic water is used as the sealing liquid, the carbon content A value per milliliter of carbon dioxide on the closed filter surface is 0.00050008: when sodium fluoride acid solution is used as the sealing liquid, the A value is 0.001522g: the volume of the mixed gas, L;
W, the volume of the residual gas, n!.;
-the volume of the gas in the vacuum test, mL:
m-the voltage of the sample, B:
W--the overflow and air pressure correction coefficient, see Appendix A Table A1 or Table A2. 7 Allowable difference
The difference in analysis results between laboratories should not be larger than the allowable difference listed in Table 2 below. Table 2
400~1.205
>1.200~2.503
>2. 54--4. 06
Gk 5686.6—88
Gas volumetric method for measuring carbon temperature
Gas pressure correction coefficient table
(This table uses 1:1000
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sulfuric acid solution as sealing liquid)
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