NB/SH/T 0324-2010 Determination of oil separation from lubricating grease — Cone mesh method

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: NB/SH/T 0324—2010
• Chinese title: Determination of oil separation from lubricating grease — Cone mesh method
• English title: Standard test method for oil separation from lubricating grease (Conical sieve method)
• Replacement relationship: replaces SH/T 0324-1992
• Publication/implementation: published on 2011-01-09, implemented on 2011-05-01
• Issuing authority: National Energy Administration
• ICS 75.100; F 36

2. Scope of application and non-applicability

• 1.1 is applicable to the determination of the oil separation tendency of lubricating grease at high temperature. Unless the lubricating grease specification requires other test conditions, the test conditions of this standard are a temperature of 100 °C and a time of 30 h.
• 1.2 is not applicable to lubricating grease products with a cone penetration greater than 340 (1/10 mm) (test method GB/T 269, which is softer than lubricating grease of grade NLGI II).
• 1.3 uses International System of Units [SI] units.
• 1.4 may involve certain hazardous materials, operations and equipment, but does not purport to address all safety problems associated with them; users should establish appropriate safety and protective measures before use and determine the applicability of relevant regulatory limitations.

3. Method principle

A weighed test sample is placed in a conical mesh made of nickel wire, nickel-copper alloy wire or stainless steel wire, suspended over a beaker, and heated to the specified time and temperature. Unless the lubricating grease specification has special requirements, the standard test conditions for the test sample are constant temperature at 100 °C ± 0.5 °C for 30 h ± 0.25 h, after which measurement is carried out. The separated oil is weighed and reported as the mass fraction of the test sample at the start of the measurement.

4. Reagents and materials (purity / preparation)

• Solvent: used for cleaning the cone mesh, beaker and cover (8.1); the specific type and purity are not provided in the available source.
• Test sample: lubricating grease; the volume required for each test is approximately the same, and the mass range is about 8 g to 12 g (7.3).
• Other reagents and materials: not provided in the available source.

5. Apparatus and equipment

• 6.1 Cone mesh test apparatus: consists of a conical mesh formed from corrosion-resistant wire of about 70 (the original text appears to be a value related to aperture size; requires confirmation against the source standard (source-text extraction)), a 200 mL tall-form beaker without a spout and a cover, with a hook at the center of the cover. The structure and dimensions are shown in Figure 1. Units are millimeters. The dimensions marked in the detailed drawing of the cone mesh include 9.7±3.3, 8.1±0.3, about 36, etc. (requires confirmation against the source standard (source-text extraction)).
• 6.2 Mesh: a conical mesh, in accordance with the provisions of GB/T 10611, made of medium-coarse 248 μm stainless steel, nickel-copper alloy or nickel wire, as shown in Figure 1. The original text mentions “always use graded products or wire mesh ... conforming to this standard” (wording requires confirmation against the source standard (source-text extraction)).
• 6.3 Constant-temperature oven: temperature capable of being controlled at 100 °C ± 0.5 °C.
• Balance: minimum weighing 250 g, readability 0.01 g.
• Others: not provided in the available source.

6. Recommended operating conditions

• Standard test conditions: temperature 100 °C ± 0.5 °C, time 30 h ± 0.25 h (1.1, 4, 9.1).
• Unless the lubricating grease specification has special requirements, carry out the test under the above standard conditions.

7. Sampling and test sample preparation

• 7.1 Inspect the sample for non-uniformity, such as oil separation, phase change, or significant contamination. If any abnormal condition is found, a new sample should be obtained.
• 7.2 The amount of sample used for analysis shall at least be sufficient to meet the needs of repeat testing.
• 7.3 Although the mass of lubricating grease required for the test has been determined, the amount of lubricating grease used to fill the cone mesh will still be somewhat greater than the amount required for the test. Each test requires a sufficient amount of lubricating grease to fill the cone mesh, with the filling height approximately as shown in Figure 1 (about 10 mL). Regardless of the lubricating grease, the volume of lubricating grease required for each test is approximately the same; the mass range is between 8 g and 12 g.

8. Analytical procedure

• 8.1 Carefully clean the cone mesh, beaker and cover with a suitable solvent. Allow the cone mesh to air-dry naturally. Note: Cleaning the cone mesh with solvent in an ultrasonic bath is very effective.
• 8.2 Inspect the cone mesh to confirm that it is clean and free of residue so that separated oil can seep through. If the cone mesh surface shows irregularities such as broken seams, dents, creases, or if the mesh openings are enlarged or reduced, it should be replaced.
• 9.1 Pre-heat the constant-temperature oven to the test temperature. Unless otherwise specially required, the test is carried out under the standard conditions of 100 °C ± 0.5 °C for 30 h ± 0.25 h.
• 9.2 Weigh the beaker to the nearest 0.01 g.
• 9.3 Assemble as shown in Figure 1.
• 9.4 Using a suitable spatula (original text “using a suitable spat...” requires confirmation against the source standard (source-text extraction)), fill the lubricating grease test sample into the mesh as far as possible to the level shown in Figure 1, avoiding the formation of air bubbles. Handle carefully so that the test sample is not forced out through the mesh openings. Smooth the top of the test sample into a convex rounded shape to prevent separated oil from accumulating.
• 9.5 The fully assembled apparatus is shown in Figure 1; weigh to the nearest 0.01 g. Use the difference to calculate the mass of the lubricating grease test sample W.
• 9.6 Place the assembled cone mesh oil separation apparatus into the constant-temperature oven controlled at the specified temperature and leave it for the specified time.
• 9.7 Remove the cone mesh oil separation apparatus from the constant-temperature oven and cool to room temperature. Remove the cover from the beaker and tap gently so that oil on the tip of the cone mesh flows down the wall of the beaker into the beaker, thereby avoiding separated oil remaining on the tip of the cone mesh. Weigh the beaker including the collected separated oil to the nearest 0.01 g.
• 9.8 After the test is completed, clean the apparatus promptly in accordance with the requirements of Chapter 8 to prepare for the next test.

9. Qualitative and quantitative determination and calculation formula

• The oil separation amount X [% (mass fraction)] is calculated according to formula (1):
  • X = 100 × (W₂ − W₁) / W ...... (1)
  • Where: W₁ — mass of the empty beaker before heating, g; W₂ — mass of the beaker after heating, g; W—— mass of the test sample, g.
  • Note: The subscript source-text extraction of the symbol in the original text is unclear (W-W/W); it has been organized according to context and requires confirmation against the source standard (source-text extraction).
• Expression of results: to the nearest 0.1% (mass fraction) (see Chapter 11).

10. Precision

• 12.1 Precision: based on a statistical test of oil separation by eight test participants on eight test samples, with all tests repeated; the mass fraction range of oil separation of the test samples is 0.% to 23% (the original values require confirmation against the source standard (source-text extraction)). The reliability of test results is judged according to the following provisions (95% confidence level; the original text “65%” requires confirmation against the source standard (source-text extraction)).
• Table 1 Typical precision values for determination of oil separation

• 12.1.1 Repeatability (r): in the same laboratory, by the same operator using the same apparatus, under the same operating conditions, for repeated determinations on the same test sample, the difference between the two results obtained shall not exceed the requirement of formula (2).
  • r = 1.151 × X^0.5 ...... (2)
  • Where: X—— arithmetic mean of the two repeat determination results.
  • Note: The exponent source-text extraction in the original text is “X0s”; based on the repeatability coefficient 1.151 and the values in Table 1, it is inferred to be X^0.5; requires confirmation against the source standard (source-text extraction).
• 12.1.2 Reproducibility (R): for tests on the same test sample under specified test conditions by different operators in different laboratories using different apparatus, the difference between the two single independent results obtained shall not exceed the requirement of formula (3).
  • R = 1.517 × X^0.5 ...... (3)
  • Where: X—— arithmetic mean of the two single independent results.
  • Note: The exponent source-text extraction in the original text is “XS”; based on the reproducibility coefficient 1.517 and the values in Table 1, it is inferred to be X^0.5; requires confirmation against the source standard (source-text extraction).
• 12.2 Bias: there is no bias in the method for determining oil separation from lubricating grease, because the oil separation of the test sample is defined solely by this test method.

11. Report

The report shall include the following information:

• Nature of the sample.
• Test date.
• Test temperature and duration.
• Results: to the nearest 0.1% (mass fraction).
• Note: In the original text, clause numbers source-text extraction of Chapter 11 are missing (11, 11.1, 11.4, etc.); requires confirmation against the source standard (source-text extraction).

12. Normative references

• GB/T 269 Standard test method for cone penetration of lubricating grease and petrolatum (GB/T 269—1991, eqv ISO 2137:1985)
• GB/T 10611 Industrial wire mesh — Designation method and mesh size series (GB/T 10611-2003, ISO 2194:1991, MOD)
• Reference: [1]SH/T 0682 Standard test method for oil separation from lubricating grease during storage

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 questions and answers