SH/T 0327-1992 (2004) Determination of Ash in Lubricating Grease

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 title / English name / replacement relationship

• Standard number: SH/T 0327-92 (confirmed in 2004)
• Full title: Determination of Ash in Lubricating Grease
• English name: not provided in the available source
• Replacement relationship: replaces SY 2703—82
• Approval/implementation: approved by China Petrochemical Corporation 1992-05-20, implemented on 1992-05-20
• First issued: 1954

2. Scope of application and non-applicability

• This standard specifies the determination method for ash in lubricating grease.
• This standard applies to lubricating grease.
• Not applicable: not provided in the available source.

3. Method principle

Use quantitative filter paper as an ignition wick, burn the sample, and calcine the solid residue to ash, expressed as a mass percentage.

4. Reagents and materials (purity / preparation)

• 3.1.1 Hydrochloric acid: chemically pure; prepare dilute hydrochloric acid by mixing hydrochloric acid and distilled water in a volume ratio of 1:4.
• 3.1.2 Ammonium nitrate: analytical reagent (should be ash-free); prepare an aqueous solution of 10%.
• 3.2 Material: quantitative filter paper, diameter 9cm.

5. Apparatus and equipment

• 4.1 Covered porcelain crucible: 30mL. Note: the porcelain crucible may be used until the porcelain glaze inside it is damaged.
• 4.2 Desiccator.
• 4.3 Electric hot plate, electric furnace, or other heat source.
• 4.4 Crucible tongs.
• 4.5 Beaker: 500mL.
• 4.6 High-temperature electric furnace or crucible furnace: capable of maintaining constant temperature at 600°C±20°C and 800°C±20°C. Requires confirmation against the source standard (source-text extraction): the source text reads “600°CC 20° seven and 800°C 20°C”.

6. Recommended operating conditions

• Calcination temperature: 600°C±20°C (test procedure 6.2); 800°C±20°C (crucible constant-weight treatment 5.2).
• During burning, the flame height should not exceed the upper edge of the crucible by 10cm.
• 6.2 at 600°C±20°C for at least 1.5h, until the residue is completely ashed.
• 6.3 then place in a high-temperature furnace or crucible furnace and calcine for 15min.
• Cooling: cool in air for 3min, transfer to a desiccator and cool for 30~40min.

7. Sampling and sample preparation

• 5.1 Use a spatula to scrape off the surface layer of the sample, then take approximately equal amounts of sample from at least three locations not close to the container wall, place in a small beaker, and stir uniformly.
• 6.1 According to the ash content, weigh 2~5g of sample in a crucible that has been brought to constant weight, weighed to the nearest 0.01g.

8. Analysis procedure

• 5.2 Place the porcelain crucible in a beaker containing dilute hydrochloric acid (1:4), heat to boiling for several minutes, remove, wash with water and distilled water, dry, then place in a high-temperature electric furnace or crucible furnace heated to 800°C±20°C, calcine for at least 10min, remove and cool in air for 3min, then transfer to a desiccator, cool for 30~40min, and then weigh, weighed to the nearest 0.0002g. Repeat the calcination, cooling, and weighing until the difference between consecutive weighings is not greater than 0.0004g.
• 6.1 Take a piece of quantitative filter paper, fold it in two, roll it into a cone, use scissors to cut off the part from 5~10mm from the tip, place it in the crucible so that the conical filter paper covers the surface of the sample. Place on an electric furnace or hot plate and heat; after the filter paper is soaked with the sample, ignite and burn.
• 6.2 After the sample has finished burning and the flame has extinguished, carefully transfer the crucible containing the carbonized residue into a high-temperature electric furnace at 600°C±20°C, and maintain at this temperature for at least 1.5h until the residue is completely ashed. If the carbonized residue is difficult to ash, after the crucible has cooled, add a few drops of ammonium nitrate solution to wet the residue, then slowly evaporate to dryness and continue calcination.
• 6.3 After the residue has become ash, remove and cool in air for 3min, then transfer to a desiccator, cool for 30~40min, and then weigh, weighed to the nearest 0.0002g. Then place in a high-temperature furnace or crucible furnace and calcine for 15min. Repeat the calcination, cooling, and weighing until the difference between consecutive weighings is not greater than 0.0004g.

9. Qualitative/quantitative determination and calculation formula

The ash content of the sample X [% (m/m)] is calculated according to the following formula:

X = (m₁ - m₂) / m × 100

Where:

• m₁ — mass of sample ash and filter paper ash, g;
• m₂ — mass of filter paper ash, g;
• m — mass of sample, g.

Requires confirmation against the source standard (source-text extraction): the source formula is typeset as “X=m-W2×100”; the symbols in the formula are given in the source as “m mass of sample ash and filter paper ash”, “m2 one mass of filter paper ash”, “m— mass of sample”; the symbol subscripts and formula form are subject to the source text.

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 determination result.

12. Referenced documents

not provided in the available source.

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