SH/T 0033-1990 Determination of true density of petroleum coke

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Card type: Test method

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

• Standard number: SH/T 0033-90
• Chinese name: Determination of true density of petroleum coke
• English name: not provided in the available source
• Replacement relationship: not provided in the available source (the additional notes state: "by reference, adopts clause 4.4 'Determination of true density' of the Soviet national standard ГОСТ 22898-78 'Technical conditions for low-sulfur petroleum coke'")
• Approval/implementation: approved by China Petrochemical Corporation 1991-03-27, implemented on 1992-04-01

2. Scope of application and non-applicability

• Scope of application: This standard specifies the method for determining the true density of petroleum coke; it is applicable to delayed petroleum coke (green coke).
• Non-applicability: not provided in the available source.

3. Method principle

Place a calcined petroleum coke sample with a crushed particle size not greater than 0.1 mm into a density bottle, add anhydrous ethanol, and determine its true density from the mass of the sample and the volume of anhydrous ethanol it displaces.

4. Reagents and materials (purity / preparation)

• Anhydrous ethanol: analytical reagent.
• Distilled water: used for determination of the density bottle volume (7.2).
• Chromic acid cleaning solution: used for cleaning the density bottle (7.2.1).
• Preparation method: not provided in the available source.

5. Instruments and equipment

• 5.1 High-temperature furnace: box-type resistance furnace, capable of ensuring heating to 1300±25℃ within 2h; the furnace chamber dimensions shall be not less than 100mm×150mm×200mm.
• 5.2 Constant-temperature water bath: capable of maintaining a constant temperature of 20±0.1℃.
• 5.3 Density bottle: a 25 mL volumetric flask may be used, with a stopper, and the inner diameter of the neck not greater than 8 mm.
• 5.4 Thermometer: 0～50℃, with a scale division of 0.1℃.
• 5.5 Sand bath or water bath.
• 5.6 Porcelain crucible: with lid, see Figure 1.
• 5.7 Mechanical crusher or porcelain mortar.
• 5.8 Sieve: aperture 0.1mm (140 mesh).
• 5.9 Long-neck funnel.
• 5.10 Pipette: 10mL.
• 5.11 Analytical balance: sensitivity 0.1mg.

6. Recommended operating conditions

• Calcination temperature: 1300±25℃; holding time: 5h; after stopping heating, cool to below 100℃ before taking out.
• Constant-temperature water bath temperature: 20±0.1℃; constant-temperature time: 20～30min.
• Boiling conditions: boil on a sand bath or water bath for 3min.
• Frequency of density bottle volume (water value) determination: not less than once every three months.
• Frequency of anhydrous ethanol density determination: the density of each batch of anhydrous ethanol must be determined.

7. Sampling and sample preparation

• 7.1 Calcination of petroleum coke: sample according to method A in SY 2871, and prepare a sample with a particle size less than 3mm. Place the sample into a porcelain crucible, cover with a lid, put into a high-temperature furnace, and heat to 1300±25℃. Hold at this temperature for 5h, then stop heating, cool to below 100℃, and take out. From the upper layer of the cooled sample, remove a layer of height 1.0～1.5cm; grind the remainder with a mechanical crusher or porcelain mortar and sieve it entirely to prepare a sample with a particle size less than 0.1mm. If steel mechanical crushing is used, iron powder must be removed with a magnet.
• 7.2 Determination of density bottle volume:
  • 7.2.1 Before determination, carefully wash the density bottle with chromic acid cleaning solution, rinse with water, then rinse with distilled water, dry it, and weigh to the nearest 0.0002g.
  • 7.2.2 Inject freshly boiled distilled water cooled to room temperature into the density bottle to near the mark, cover with the ground stopper, and place in a constant-temperature water bath at 20±0.1℃ for 20～30min. Use a pipette to draw distilled water from a standby bottle placed in the constant-temperature water bath, inject it into the density bottle until the liquid level reaches the mark, absorb excess water with filter paper, and wipe clean the inner wall above the liquid level. After taking it out, wipe the outer wall dry with silk cloth and weigh, to the nearest 0.0002g.
  • 7.2.3 Repeat the operation of 7.2.2 until the difference in mass between replicates is not greater than 0.001g, and take the arithmetic mean.
  • 7.2.4 The density bottle volume V (cm³) is calculated according to formula (1): V = (m₁ − m) / 0.9982 Where: m — mass of the density bottle, g; m₁ — mass of the density bottle containing water, g; 0.9982 — density of water at 20℃, g/cm³.
• 7.3 Determination of anhydrous ethanol density:
  • 7.3.1 Dry the density bottle whose volume has been determined, and according to 7.2.2 and 7.2.3, use anhydrous ethanol instead of distilled water to determine the density of anhydrous ethanol.
  • 7.3.2 The density of anhydrous ethanol ρ₁ (g/cm³) is calculated according to formula (2): ρ₁ = (m₂ − m) / V Where: m — mass of the density bottle, g; m₂ — mass of the density bottle containing anhydrous ethanol, g; V — volume of the density bottle, cm³.
  • 7.3.3 Take the arithmetic mean of the replicate determination results as the density of anhydrous ethanol.

8. Analytical procedure

• 8.1 Take 2～3g of the sample prepared in clause 7.1, inject it through a long-neck funnel into a dry density bottle of known mass, and weigh to the nearest 0.0002g.
• 8.2 Inject about one third of the volume of anhydrous ethanol into the density bottle containing the petroleum coke sample, and boil on a sand bath or water bath for 3min, but do not let the anhydrous ethanol and sample escape. At the same time, boil anhydrous ethanol in another flask on the sand bath. After boiling, take out the density bottle and flask and cool in air. Following steps similar to 7.2.2, take anhydrous ethanol from the flask and inject it into the density bottle to the mark, maintain constant temperature at 20±0.1℃, adjust the liquid level, and weigh.

9. Qualitative and quantitative determination and calculation formula

The true density of petroleum coke ρ (g/cm³) is calculated according to formula (3):

ρ = m₄ / [ V − (m₅ − m₃ − m₄) / ρ₁ ]

Where:

• m₃ — mass of the density bottle containing petroleum coke, g;
• m₄ — mass of the petroleum coke sample (= m₃ − m), g;
• m₅ — mass of the density bottle containing petroleum coke and anhydrous ethanol, g;
• V — volume of the density bottle, cm³;
• ρ₁ — density of anhydrous ethanol at 20℃, g/cm³.

(Note: the original formula (3)source-text extraction contains noise; the formula form requires confirmation against the source standard (source-text extraction).)

10. Precision

Repeatability: the difference between two results of repeated determinations by the same operator shall not be greater than 0.01g/cm³.

11. Report

Take the arithmetic mean of two repeated determination results as the determination result.

12. Referenced documents

• SY 2871 Test method for petroleum coke (editor's note: current standard number SH/T 0313, current standard name Test method for petroleum coke)
• By reference, adopts: clause 4.4 'Determination of true density' in the Soviet national standard ГОСТ 22898-78 'Technical conditions for low-sulfur petroleum coke'

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 Q&A