SH/T 0029-1990 Determination of Ash in Petroleum Coke

AI-translated method card — human verification pending. This is not an official translation of the standard. Unclear source values remain unverified; check the original standard and product certificate before use.

Card type: Test method

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

• Standard number: SH/T 0029-90
• Chinese name: Determination of Ash in Petroleum Coke
• English name: not provided in the available source
• Replacement relationship: not provided in the available source (the additional notes state that "this standard refers to and adopts the Soviet national standards ГОСТ 22898—78 'Technical Conditions for Low-Sulfur Petroleum Coke' and ГОСТ 5889—67 'Determination of Ash in Coal Coke'", which is not a replacement relationship)
• Approval/implementation: approved by China Petrochemical Corporation 1991-03-27, implemented on 1992-04-01

2. Scope of application and non-applicability

• Applicable to: delayed petroleum coke.
• Not applicable to: not provided in the available source.

3. Method principle

The petroleum coke sample is calcined in a muffle furnace at 850℃±20℃, ashed and calcined at the same temperature to constant weight, and its ash content is calculated from the difference in mass of the sample before and after calcination.

4. Reagents and materials (purity / preparation)

• 5.1 Hydrochloric acid: chemically pure.
• 5.2 Silica gel or calcium chloride: chemically pure, used as desiccant.
• Dilute hydrochloric acid: volume ratio 1:4 (used for pretreatment of porcelain boats, see 6.2).
• Distilled water: no explicit purity requirement provided in the available source (6.2 used for rinsing).

5. Instruments and equipment

• 4.1 Muffle furnace: capable of maintaining constant temperature at 850℃±20℃.
• 4.2 Analytical balance: sensitivity 0.1mg.
• 4.3 Porcelain boat or quartz boat: rectangular, top opening length 55–60mm, width 25–30mm, bottom length 45–50mm, width 20–22mm, height 14~16mm; its size should ensure that when loaded with no less than 2g of sample, the sample per square centimeter is no greater than 0.2g.
• 4.4 Desiccator: with stopcock (or other type).
• 4.5 Crucible tongs: nickel-plated crucible tongs.
• 4.6 Horn spoon.

6. Recommended operating conditions

• Calcination temperature: 850℃±20℃.
• Porcelain boat pretreatment calcination: 850℃±20℃, 30min (6.3).
• Sample calcination: at least 2h (7.2).
• Check calcination: each time 30min (7.4).
• Cooling: cool in air 5min; cool in desiccator 30~40min.

7. Sampling and sample preparation

• 6.1 Prepare the sample according to method A in SY 2871.
• 7.1 Thoroughly stir the prepared petroleum coke sample with a horn spoon, take 2g±0.01g of petroleum coke sample from two or three places at different depths below the sample surface, place it into a pre-constant-weight porcelain boat, and weigh to the nearest 0.0002g.

8. Analysis procedure

• 6.2 Place a new porcelain boat into dilute hydrochloric acid (volume ratio 1:4) and boil for several minutes, then wash clean with water, rinse several times with distilled water, and dry in an oven.
• 6.3 Place the washed and dried porcelain boat in a high-temperature furnace and calcine at 850℃±20℃ for 30min. Remove and cool in air for 5min, then transfer the porcelain boat into a desiccator, cool for 30~40min, and weigh to the nearest 0.0002g. Repeat calcination, cooling, and weighing until the difference between two consecutive weighings is no greater than 0.0004g.
• 7.2 Place the porcelain boat containing the petroleum coke sample on the front edge of the furnace chamber of the 850℃±20℃ high-temperature furnace, gradually move the porcelain boat into the fully incandescent zone of the high-temperature furnace within 3min, then close the furnace door and calcine for at least 2h.
• 7.3 Remove the porcelain boat, cool in air for 5min, then transfer the porcelain boat into a desiccator, cool for 30~40min, and weigh to the nearest 0.0002g.
• 7.4 After weighing, perform check calcination again, each time for 30min, until the difference between two weighings is less than 0.001g, and take the last mass for calculation.

9. Qualitative/quantitative determination and calculation formula

Petroleum coke ash X [% (m/m)] is calculated according to the following formula:

X = (m₁ / m) × 100

Where:

• m—— mass of the petroleum coke sample, g
• m₁——mass of petroleum coke ash residue, g

(Note: the original source-text extraction formula appears as "X- parts × 100", suspected to be X = m₁/m × 100 with source-text extraction noise, requires confirmation against the source standard (source-text extraction).)

10. Precision

Repeatability: the difference between two results of repeated determination shall not exceed the following values.

11. Report

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

12. Referenced documents

• SY 2871 Petroleum Coke Inspection Method (editor's note: original standard number SY 2871, current standard number SH/T 0313, current standard name Petroleum Coke Inspection Method)
• Referenced and adopted: ГОСТ 22898—78 'Technical Conditions for Low-Sulfur Petroleum Coke', ГОСТ 5889—67 'Determination of Ash in Coal 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 Q&A