SH/T 0313-1992 Petroleum coke test methods

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Card type: Test method

1. Method number / full name / English name / replacement relationship

• Standard number: SH/T 0313-92
• Chinese name: Petroleum coke test methods
• English name: not provided in the available source
• Replacement relationship: replaces SY 2871-77 (88)
• Included method numbers:
  • Method A Sampling
  • Method B Determination of moisture in petroleum coke
  • Method C Determination of volatile matter
  • Method D Determination of ash in petroleum coke
  • Method E Determination of sulfur content in petroleum coke
  • Method F Determination of fine coke content
  • Method G Determination of density of petroleum coke after calcination

2. Scope of application and non-applicability

• This standard specifies test methods for sampling, moisture, volatile matter, ash, sulfur content, fine coke content, and density after calcination of petroleum coke.
• This standard applies to petroleum coke.
• Not applicable: not provided in the available source.

3. Method principle

• Method B (moisture): A weighed petroleum coke sample is dried in an oven to constant mass, and its mass loss is determined.
• Method C (volatile matter): A petroleum coke sample is placed in a 850℃ high-temperature furnace and heated for 3min, and its mass loss is determined.
• Method D (ash): A petroleum coke sample is ashed and calcined in a 850℃ high-temperature furnace to constant mass to determine the ash of the petroleum coke.
• Method E (sulfur content): same as GB/T 387 "Determination of sulfur content in dark petroleum products (tube furnace method)".
• Method F (fine coke content): sieve with a 25mm metal wire sieve, weigh the fine coke passing through the sieve, and calculate it as a percentage of the total mass of the sample.
• Method G (density after calcination): using the density bottle method, with anhydrous ethanol as the medium, determine the density of calcined petroleum coke powder at 15℃.
• Method A (sampling): no principled description is provided in the available source.

4. Reagents and materials (purity / preparation)

• Method G:
  • Anhydrous ethanol: chemically pure.
  • Nitrogen used during calcination: free of oxygen and trace carbon monoxide (as stated in the source text).
  • If nitrogen cannot be blown in, a covered double crucible may be used, with a finely ground and calcined carbon-containing substance sprinkled between the inner and outer crucibles.
• Other methods: not provided in the available source.

5. Instruments and equipment

• Method B:
  • 7.1 Oven: capable of maintaining a constant temperature at 105±3℃.
  • 7.2 Galvanized steel tray: 160mm×120mm×30mm; a porcelain or glass evaporating dish with a capacity of 150mL and a diameter of 100mm may also be used.
  • 7.3 Weighing bottle: with a ground stopper, diameter 50mm, height 30mm.
  • 7.4 Desiccator.
  • 7.5 Mercury thermometer: 0~150℃, scale division 1.0℃.
  • 7.6 Crucible tongs.
  • 7.7 Small spoon.
• Method C:
  • 12.1 Porcelain crucible: height 43±0.5mm, outer diameter of the upper opening 32±0.5mm, outer diameter of the bottom opening 18±0.5mm, with a crucible cover having a groove-like inner surface; mass without cover 13–14g, wall thickness 1.3–1.4mm.
  • 12.2 High-temperature furnace: capable of maintaining a constant temperature at 850±20℃; the furnace door should have an opening for volatiles to escape, and the rear wall of the furnace should have an opening for inserting a thermocouple.
  • 12.3 Rack: made of heat-resistant metal wire, used for placing crucibles; the height of the rack shall keep the distance between the bottom of the crucible placed on the rack and the furnace bottom at 20±2mm.
  • 12.4 Desiccator.
  • 12.5 Crucible tongs.
  • 12.6 Small spoon.
  • 12.7 Stopwatch.
• Method D:
  • 19.1 High-temperature furnace: capable of maintaining a constant temperature at 850±20℃.
  • 19.2 Boat-shaped porcelain dish: rectangular, upper opening length 55–60mm, width 25–30mm; bottom length 45–50mm, width 20–22mm, height 14~16mm.
  • 19.3 Desiccator.
  • 19.4 Crucible tongs.
  • 19.5 Small spoon.
• Method G:
  • 26.1 High-temperature furnace: capable of maintaining the temperature in the furnace chamber up to 1300℃.
  • 26.2 Crucible or boat-shaped dish: made of porcelain or corundum.
  • 26.3 Desiccator.
  • 26.4 Agate mortar or steel mortar.
  • 26.5 Metal mesh sieve: sieve mesh opening 0.1mm.
  • 26.6 Density bottle: 50mL or a conical narrow-neck density bottle of another volume.
• Method A, Method E, Method F: not provided in the available source (Method E cites GB/T 387).

6. Recommended operating conditions

• Method B Drying temperature: 105±3℃.
• Method C High-temperature furnace temperature: 850±20℃; heating time 3min.
• Method D High-temperature furnace temperature: 850±20℃; calcination 2h.
• Method G Calcination temperature: 1300±10℃; calcination time 5h; density measurement temperature: 15℃.
• Others: not provided in the available source.

7. Sampling and sample preparation

Method A Sampling

• 3 General provisions:
  • 3.1 The petroleum coke sampling method is based on SH 0229 and is supplemented by the provisions of this standard.
  • 3.2 In principle, petroleum coke samples should be taken from the coke stream; when conditions do not permit, they may also be taken from the top of transport vehicles (trains, trucks, etc.) and from coke piles.
  • 3.3 Samples for total moisture determination must be taken at the production plant loading point immediately before weighing.
• 4.1.1 Sampling from the coke stream: when sampling from the coke stream with a mechanical sampler or manually, the effective flow time of the petroleum coke should be calculated based on the total coke flow rate, and sampling should be carried out at equal time intervals within that time. The number of increments per lot must not be less than five, and the total sample amount must not be less than 10kg.
• 4.1.2 Sampling from the top of transport vehicles: on the same vehicle, samples must be taken from the surface layer at at least five points at equal average distances (after long-distance transport or standing, sampling should be at 0.2~0.3m below the coke layer), striving for a uniform sample and increasing its representativeness. The sampling amount per vehicle must not be less than 5kg; the number of vehicles sampled per lot is calculated as 10% of the total number of vehicles (but must not be less than two vehicles), and the total sample amount must not be less than 10kg.
• 4.1.3 Sampling from coke piles: the sampling points on the coke pile are distributed on three circumferential lines on the surface of the coke pile at distances of 0.5m from the bottom and top and at half the height of the coke pile, with three, five, and eight sampling points arranged at equal intervals respectively (see the figure below). At the surface layer of each sampling point (after long-term stacking, at 0.2~0.3m below the coke pile layer), take no less than 0.5kg of petroleum coke sample; the total sample amount must not be less than 8kg.
• 4.1.4 Divide the sample selected according to the above provisions into four portions, take any two identical portions and mix them, crush them with a hammer on a steel plate, and then remove two portions by quartering; continue crushing and dividing in this way until the coke particle size is less than 10mm and the total mass is about 1~2kg, thus obtaining the final petroleum coke sample; divide the above sample into two portions. One portion is for full-item analysis, and the other is sealed and stored for two months for rechecking and arbitration.

5 Sample preparation

• Place the 0.5kg final petroleum coke sample on a tray and dry it in an oven at 105±3℃ for more than 30min, so that the sample reaches an air-dried state.
• After removing the petroleum coke from the oven and cooling it, crush it mechanically or manually to a particle size less than 5mm, and uniformly take out a 50g sample. Continue crushing until it can completely pass through a sieve with an aperture of 0.15mm; this sample can be used for the determination of sulfur content, ash, and volatile matter of petroleum coke.

8. Analytical procedure

Method B Moisture

• 8.1 Determination of total moisture:
  • 8.1.1 Weigh 50g of the final petroleum coke sample (accurate to 0.5g) onto a pre-weighed steel tray, spread the petroleum coke evenly in the steel tray, place it in an oven preheated to 105±3℃, and open the natural ventilation holes of the oven.
  • 8.1.2 After 1h, remove the steel tray, cool in air for 30min and weigh; then dry again for 20min each time until the difference between two weighings is less than 0.5g; use the last weighing value for calculation.
• 8.2 Determination of internal moisture:
  • 8.2.1 Carefully stir the prepared sample, take about 2g of petroleum coke sample from different parts of the sample (in two or three portions), place it in a pre-constant-mass weighing bottle, place the weighing bottle in an oven at 105±3℃ and dry for 1h, remove it and cool in a desiccator for 30min, and weigh. Then dry again for 30min each time until the difference between two weighings is less than 0.001g; use the last mass for calculation (accurate to 0.0002g).
  • Note: When drying in the oven, the cover of the weighing bottle containing the petroleum coke sample should be opened halfway; when cooling and weighing in the desiccator, the cover should be closed tightly.

Method C Volatile matter

• 13 Preparatory work:
  • 13.1 Heat the high-temperature furnace to 850±20℃; the position of the thermocouple should be such that the junction is located in the constant-temperature zone at 20~30mm from the furnace bottom.
  • 13.2 The crucible must be pre-calcined in a high-temperature furnace at 850℃, cooled in a desiccator, weighed, and placed in a desiccator for later use.
• 14 Test procedure:
  • 14.1 Stir the sample prepared in Chapter 5 with a small spoon, take 1±0.05g sample from the lower part of the sample, place it in the crucible, and shake gently to spread the sample in the crucible evenly. Cover the crucible well and place the crucible on the rack.
  • 14.2 Quickly send the crucible containing the sample together with the rack to the constant-temperature zone in the high-temperature furnace, start the stopwatch at the same time, close the furnace door, and heat. When the heating time just reaches 3min, remove the volatile matter crucible from the constant-temperature zone. After cooling in air for 3min, transfer the crucible to a desiccator, cool for 30~40min, and weigh (accurate to 0.0002g).

Method D Ash

• 20.1 Stir the prepared petroleum coke sample with a small spoon, weigh 2~3g of petroleum coke from below the sample surface, and place it in a preheated and constant-mass porcelain dish.
• 20.2 Place the porcelain dish containing the petroleum coke sample on the front edge of the furnace chamber of the high-temperature furnace at 850±20℃, and gradually move the porcelain dish into the fully incandescent zone of the high-temperature furnace within 3min. Close the furnace door (the small hole in the furnace door should be opened), and calcine for 2h.
• 20.3 Take out the porcelain dish, cool in air 3min, then transfer into a desiccator, cool 30~40min, and weigh. After weighing, calcine again, each time 30min, until the difference between two weighings is less than 0.001g, take the last mass for calculation (accurate to 0.0002g).

Method E Sulfur content

• 24 Same as GB/T 387 "Determination of sulfur content in dark petroleum products (tube furnace method)".

Method F Powder coke amount

• 25 Weigh out the sample used for determining the powder coke content in petroleum coke, place it on a metal wire sieve with openings of 25mm level and sieve it. Use a shovel to take out the petroleum coke, each portion not more than 15kg, and evenly spread it over the entire surface of the sieve. Sieve each portion of petroleum coke in the sieve left and right continuously three times. After all the petroleum coke sample has been sieved, weigh the powder coke that passed through the sieve; the powder coke content in the petroleum coke is calculated as the percentage of the total mass of the sample taken.

Method G Density after calcination

• 28 Preparation work:
  • 28.1 Calcination: The calcination of the petroleum coke analytical sample may be carried out in a special calcination furnace or in other heating devices capable of adjusting and maintaining the temperature at 1300℃ or above 1300℃. Place the petroleum coke sample to be analyzed into a porcelain or corundum boat-shaped dish or crucible for calcination; the thickness of the loaded sample shall not exceed 60mm. Place the uncovered boat-shaped dish or crucible into a tube furnace; during calcination, in order to prevent oxidation of the petroleum coke, nitrogen gas free of oxygen and trace carbon monoxide must be gently blown into the furnace. If it is impossible to blow in nitrogen, calcination is allowed in a covered double-layer crucible; the outer crucible may be made of metal, and between the inner and outer crucibles a finely ground and calcined carbon-containing substance must be sprinkled. After calcination at a temperature of 1300±10℃ for 5h, transfer the sample to a cooler place on the furnace, cool to below 300℃, and then move it into a desiccator.
  • 28.2 Pulverization: Place the calcined analytical petroleum coke sample in an agate mortar or steel mortar and grind it; it must be ground very fine so that it can pass through a sieve with mesh openings of 0.1mm. The residue on the sieve must be repeatedly ground until the analytical sample completely passes through. When using a steel mortar, the ground sample must subsequently be demagnetized, and loss of sample must be avoided during grinding. The amount of sample taken for determining the density of petroleum coke depends on the volume of the density bottle used:
    • Density bottle volume 25mL, sample amount 2g
    • Density bottle volume 50mL, sample amount 3g
    • Density bottle volume 100mL, sample amount 5g
    • It is best to use a density bottle with a 50mL conical narrow neck.
• 29 Test procedure:
  • 29.1 Pour the calcined petroleum coke powder from a small long-stem funnel into a pre-weighed density bottle, and weigh the density bottle containing the petroleum coke powder to determine the amount of sample weighed, accurate to 0.0001g.
  • 29.2 Pour anhydrous ethanol into the density bottle containing the petroleum coke powder sample to two-thirds of its volume, and place it on a sand bath to boil for 3min, then let it stand in a water bath at 15℃. In addition, boil anhydrous ethanol in a flask for 3min, also place it in a water bath at 15℃, and after leaving it for 10min, remove the density bottle and flask from the bath, fill the density bottle with anhydrous ethanol so that the liquid level of anhydrous ethanol in the bottle is slightly below the mark, then place the density bottle and the flask containing boiled anhydrous ethanol into a water bath (or thermostat), and leave them at 15℃ for 20min. After the above time, remove the density bottle and flask from the water bath, quickly fill the density bottle with anhydrous ethanol to the mark, then carefully wipe dry the inner wall of the neck of the density bottle (above the anhydrous ethanol liquid level) with a strip of filter paper, while the outside of the density bottle is wiped dry with a clean soft towel, and weigh on an analytical balance. Then pour out the solution in the density bottle and carefully wash it with anhydrous ethanol.
  • 29.3 Fill the density bottle to the mark with boiled anhydrous ethanol, carefully wipe dry the inner wall of the neck of the density bottle, and weigh on an analytical balance.
  • Note: ① The density of anhydrous ethanol and the mass of the density bottle containing anhydrous ethanol are both determined at 15℃. ② The determination of the mass of the density bottle containing anhydrous ethanol must be carried out at least once in each 8h work shift.

9. Qualitative and quantitative and calculation formulas

• Total moisture X₁ [% (m/m)] is calculated according to formula (1):
  • X₁ = (m − m₁) / m × 100
  • Where: m— mass of the sample before drying, g; m₁—mass of the sample after drying, g.
  • Requires confirmation (source-text extraction): the original formula (1) source-text extraction is "X, two (0-m) 100", the numerator is suspected to be (m−m₁), the denominator is suspected to be m, requires confirmation against the source standard.
• Internal water: the mass percentage of internal water in 8.2.2, X₂, is calculated according to the calculation formula for total moisture.
• Volatile matter X₃ [% (m/m)] is calculated according to formula (2):
  • X₃ = (m₁ − m₂) / m₁ × 100 − X₂
  • Where: m₁—mass of the petroleum coke sample, g; m₂—mass of the petroleum coke residue after heating, g; X₂—water content in the petroleum coke sample, %.
  • Note: The water content in petroleum coke should be determined simultaneously with the volatile matter.
  • Requires confirmation (source-text extraction): the original formula (2) source-text extraction is "X, =002-092100 one one X:", symbols and subscripts require confirmation against the source standard.
• Ash X₄ [% (m/m)] is calculated according to formula (3):
  • X₄ = m₅ / m × 100
  • Where: m— mass of the petroleum coke sample, g; m₅—mass of the petroleum coke ash residue, g.
  • Requires confirmation (source-text extraction): the original formula (3) source-text extraction is "X, =S×100", symbols require confirmation against the source standard.
• Powder coke amount: calculated as the percentage of the mass of powder coke passing through the 25mm sieve to the total mass of the sample taken (the original text does not provide a formula number).
• Density after calcination ρ (g/cm³) is calculated according to formula (4):
  • ρ = m₆·ρ₁ / (m₇ + m₆ − m₈)
  • Where: m₆—mass of the petroleum coke powder sample, g; m₇—mass of the density bottle filled with anhydrous ethanol, g; m₈—mass of the density bottle containing anhydrous ethanol and the petroleum coke powder sample, g; ρ₁—density of anhydrous ethanol at 15℃, g/cm³.
  • Requires confirmation (source-text extraction): the original formula (4) source-text extraction is "P=- ms•Pi / m. +m, one ms", symbols and subscripts require confirmation against the source standard.

10. Precision

• Moisture (Method B) The difference between two repeated determination results shall not be greater than:
  • Total moisture: 0.3%
  • Internal water: 0.2%
• Volatile matter (Method C): the difference between two repeated determination results shall not be greater than 0.3% (m/m).
• Ash (Method D): the difference between two repeated determination results shall not be greater than 0.05% (m/m).
• Density after calcination (Method G): the difference between two repeated determination results shall not be greater than 0.02g/cm³.
• Sampling, sulfur content, powder coke amount: not provided in the available source.

11. Report

• Moisture: take the arithmetic mean of two repeated determination results as the moisture determination result of the sample.
• Volatile matter: take the arithmetic mean of two repeated determination results as the volatile matter determination result of the sample.
• Ash: take the arithmetic mean of two repeated determination results as the ash determination result of the sample.
• Density after calcination: take the arithmetic mean of two repeated determination results as the density of petroleum coke after calcination.
• Sampling, sulfur content, powder coke amount: not provided in the available source.

12. Referenced documents

• GB/T 387 Determination of sulfur content in dark petroleum products (tube furnace method)
• SH 0229 Sampling method for solid and semi-solid petroleum products

13. Source and verification

This page is an AI translation of the available Chinese method card. Human verification is pending. It is not an official translation of the standard. Check the source standard and product certificate before use.

14. Quick reference for questions and answers