GB/T 2001-2013Coke-Determination of proximate analysis (English PDF)

3.1 General rule

This Clause specifies the determination method of coke's total moisture and air dried basis moisture.

3.2 Principle

Weigh a certain mass of coke sample; place in the pre-blast drying oven. At a certain temperature, dry it to constant mass. Calculate moisture's mass score by mass loss of coke sample.

3.3 Reagents

3.4 Apparatus

3.4.1 Drying oven. equipped with automatic temperature control and ventilation device; and be able to maintain the temperature within 170°C ~ 180°C and 105°C ~ 110°C.

3.4.5 Analytical balance. sensitivity is 0.0001 g.

3.4.6 Industrial balance. sensitivity is 0.1 g

3.5 Sample's sampling and preparation

Conduct sample's sampling and preparation according to the provisions in GB/T 1997.

3.6 Test steps

3.6.1 Determination of total moisture

3.6.1.1 Use dry and clean tray (see 3.4.2) of known mass to weigh (500±10) g of coke sample, of which the granularity is less than 13 mm, accurate to 0.1 g; make it paved in the tray.

3.6.2 Determination of air dried moisture

3.6.2.1 In the pre-dried and weighed weighing bottle, weigh 1g±0.5g of analytical sample of which the granularity is less than 0.2 mm, accurate to 0.0001 g; pave in the weighing bottle.

3.6.2.2 Remove the cover of the weighing bottle that holds sample into the pre-blasted drying oven that has been previously heated to 105°C ~ 110°C. Dry it for 1 h under the conditions of the blasting.

3.7 Calculation of results

3.7.1 Calculate the total moisture, according to equation (1).

3.7.2 Calculate coke's air dried basis moisture, according to equation (2).

3.7.3 Take arithmetic mean value of two test results as the test result.

3.7.4 Precision. repeatability of moisture determination must not exceed the stipulated values in Table 1.

4.1 General rule

This Clause specified two determination methods of coke ash content. Method 1 and Method 2.Method 1 is the arbitration method.

4.2 Principle

Weigh a certain mass of coke sample. Gradually put it into the muffle furnace that has been pre-heated to (815±10) °C for ashing. Burn it till mass is constant.

Take the mass score of residue mass that accounts for coke sample mass AS the coke's ash content.

4.3 Reagents

4.4 Apparatus

4.4.1 Muffle furnace. equipped with temperature measurement and temperature control devices, is able to maintain the temperature within 815°C±10°C. Furnace has sufficient temperature zone.

4.4.2 Cupel. porcelain, shape and inner diameter size are shown in Figure 3.

4.4.3 Cupel clamp. made of heat-resistant metal wire; shape is shown in Figure 4. It can also use crucible clamp.

4.4.4 Dryer. built-in with allochroic silica gel or granular anhydrous calcium chloride desiccant.

4.4.5 Analytical balance. sensitivity is 0.0001 g.

4.4.6 Heat-resistant porcelain or asbestos slate.

4.5 Sample's sampling and preparation

Sample's sampling and preparation shall be conducted according to the provisions in GB/T 1997.

4.6 Test steps

4.6.1 Method 1 (arbitration method)

4.6.1.4 Conduct inspection burning at 815°C±10°C, 15 min for each time till the sample mass difference between 2 consecutive times does not exceed 0.001 g or till the mass increases. When calculating, take the last mass. If the mass increases, take the mass before it increases as calculation basis.

4.6.2 Method 2

4.6.2.1 In the cupel that has been pre-burnt to constant mass, weigh 0.5±0.05 g of coke sample of which the granularity is less than 0.2 mm and has been evenly stirred, accurate to 0.0001 g; nicely pave it in the cupel, so as to make the mass per cm2 not exceed 0.10 g.

4.7 Calculation of results

4.7.1 Calculate air dried ash content of coke, according to equation (3).

5.1 Principle

Weigh a certain mass of coke sample. Put it in a porcelain crucible with cover.

At 900°C±10°C, heat it while isolating air for 7 min. The mass score of reduced mass that accounts for coke sample mass MINUS air dried basis moisture content of this coke sample EQUALS to the coke volatilization content.

5.2 Regents

5.3 Apparatus

5.3.1 Volatilization content crucible. equipped with porcelain crucible with tight cover; shape and size are shown in Figure 5. Crucible's total mass is 18 g ~ 22 g, and the cover's mass is 5 g ~ 6 g. The volatilization content crucible must closely coordinate with crucible cover. The selection of crucible cover must make vertical clearance between the cover and the crucible not greater than 0.5 mm. The crucible and the crucible cover shall be used in conjunction. Mixed use is not allowed.

5.3.3 Crucible holder. made of nickel-chromium wire or other heat-resistant metal wires. Its shape and size are shown in Figure 6. Its size enables all crucibles in the constant temperature zone. The distance between crucible bottom on crucible holder and furnace bottom shall be 30 mm ~ 40 mm.

5.3.4 Crucible holder clamp. made of nickel-chromium wire or other heat-resistant metal wires. Its shape and size are shown in Figure 7. It also can use crucible clamp.

5.3.5 Analytical balance. sensitivity is 0.0001 g.

5.3.6 Stopwatch.

5.3.7 Dryer. built-in with allochroic silica gel or granular anhydrous calcium chloride.

5.4 Sample sampling and preparation

Conduct sample sampling and preparation according to the provisions in GB/T 1997.

5.5 Test steps

5.5.1 In the porcelain crucible with cover that has been pre-burnt to constant mass at 900°C±10°C, weigh evenly stirred coke sample of which the granularity is less than 0.2 mm, accurate to 0.0001 g; gently vibrate the crucible, so as to make the sample paved. Cover the cover and place in on the crucible holder. If samples for determination is less than 6, then place empty crucibles on the holder to fill the vacancy.