GB/T 269-2023 Determination of Cone Penetration of Lubricating Greases and Petrolatum

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

• Standard number: GB/T 269—2023
• Chinese name: Determination of Cone Penetration of Lubricating Greases and Petrolatum
• English name: Determination of cone penetration of lubricating greases and petrolatum
• Replacement relationship: replaces GB/T 269—1991 "Determination of Cone Penetration of Lubricating Greases and Petrolatum"
• Adoption relationship: modified adoption of ISO 2137:2020 (MOD)
• Previous versions: GB 269—1985, GB 5017—1985; GB 269—1985 and GB 5017—1985 were modified and merged into GB/T 269—1991; this is the third revision
• Publication/implementation: published on 2023-05-23, implemented on 2023-12-01
• Proposing and secretariat: National Technical Committee for Standardization of Petroleum Products and Lubricants (SAC/TC 280)
• Drafting organization: Sinopec Research Institute of Petroleum Processing
• Main drafter: Jiang Liang

2. Scope of application and non-applicability

• This document describes the method for determining the consistency of lubricating greases and petrolatum by the cone penetration method.
• Applicable to lubricating greases and petrolatum (petroleum jelly).
• Chapter 8: full-scale cone penetration into lubricating grease to determine consistency, including unworked, worked, extended worked, and block penetration 4 methods, with penetration values measured to 500 units.
• Chapter 9: determination of small-sample lubricating grease using 1/2 or 1/4 scale cones, only applicable to lubricating greases with full-scale penetration values from 175 units to 385 units, and only used when the test sample size is not suitable for Chapter 8; it cannot replace the full-scale cone method.
• Chapter 10: full-scale cone penetration into petrolatum to determine consistency, with full-scale penetration values up to 300 units; this method can also determine the consistency of slack wax.
• Not applicable/limitations: the 1/4 scale cone has poor precision and its use should be restricted as much as possible; after mechanical shear testing in bearings or specific test rigs, it is not advisable to use the 1/4 scale cone to measure changes in lubricating grease penetration.
• Certain petrolatum containing higher melting point waxes may require higher flow temperatures; the precision values in Table 3 are not applicable to the determination results of such petrolatum.
• No other explicit non-applicable scope is provided in the available source.

3. Method principle

• Lubricating grease penetration: at 25 °C, release the cone assembly from the penetrometer, allow the cone to fall for 5 s, measure the depth of penetration into the sample; 3 determinations should be made and the average of the results reported.
  • Unworked penetration: the sample is transferred to a suitable test container with as little agitation as possible for determination.
  • Worked penetration: determined after the sample has been subjected to 60 double strokes in a lubricating grease worker.
  • Extended worked penetration: determined after the sample has been subjected to more than 60 double strokes in a lubricating grease worker.
  • Block penetration: cut block-shaped lubricating grease with a lubricating grease cutter and determine on the newly cut cube surface.
• Petrolatum penetration: the sample is first melted and cooled under specified conditions, then determined according to the lubricating grease penetration method.

4. Reagents and materials (purity / preparation)

• Cleaning solvent: volatile non-gumming solvents such as petroleum ether should be used (see 8.1.2).
• No other reagents and their purity or preparation provisions are provided in the available source.

5. Apparatus and equipment

• 6.1 Penetrometer: capable of measuring the depth of cone penetration into the sample, in 0.1 mm units; the cone assembly or platform can move vertically; adjustable so that the cone tip is at the grease surface and the indicator reads "zero"; when the cone is released, it should be able to fall at least 62 mm without appreciable friction; the cone tip should not strike the bottom of the sample container; equipped with leveling screws and a spirit level. A mechanical or digital indicator may be used.
• 6.2 Cone:
  • 6.2.1 Full-scale cone: consists of a cone made of magnesium or other suitable material and a detachable hardened steel tip; the total mass of the cone shall be 102.50 g±0.05 g, and the mass of the cone rod shall be 47.50 g±0.05 g; the outer surface is polished. For penetration determinations in the range of 400 units, an optional cone may be used (Figure 3), with a total cone mass of 102.50 g±0.05 g and a total movable assembly mass of 47.50 g±0.05 g.
  • 6.2.2 1/2 scale cone and cone rod: the cone is made of steel, stainless steel, or brass, with a hardened steel tip having a Rockwell hardness C of 45 to 50; the cone rod may be made of stainless steel; the total mass of the cone and cone rod shall be 37.50 g±0.05 g; the mass of the cone shall be 22.500 g±0.025 g; the mass of the cone rod shall be 15.000 g±0.025 g.
  • 6.2.3 1/4 scale cone and cone rod: the cone is made of plastic or other low-density material, with a hardened steel tip having a Rockwell hardness C of 45 to 50; the cone rod may be made of magnesium alloy; the total mass of the cone and cone rod shall be 9.380 g±0.025 g, adjustable by adding small pellets into the cavity of the cone rod.
• 6.3 Lubricating grease worker:
  • 6.3.1 Full-scale lubricating grease worker: conforms to the dimensions in Figure 6; the working speed shall reach 60 strokes/min±10 strokes/min, with a minimum working stroke distance of 63 mm; equipped with a suitable thermometer calibrated at 25 °C, inserted through the vent valve.
  • 6.3.2 1/2 scale lubricating grease worker: conforms to the dimensions in Figure 7, made of stainless steel, with a volume of 50 mL; the working speed shall reach 60 strokes/min±10 strokes/min, with a minimum working stroke of 35 mm.
  • 6.3.3 1/4 scale lubricating grease worker: made of stainless steel, conforms to the dimensions in Figure 8; the working speed shall reach 60 strokes/min±10 strokes/min, with a minimum working stroke of 14 mm; the internal dimensions of the worker grease cup are φ19.0 mm × height 17.5 mm, and the volume including the grease orifice plate is 4 mL.
  • 6.3.4 Overflow ring (optional): when determining penetration, it should be placed at least 13 mm below the edge of the worker grease cup; the edge height of the overflow ring is 13 mm.
• 6.4 Lubricating grease cutter: has a firmly mounted sharp blade with a beveled knife; the blade should be straight and sharp; grind both sides to a thickness of 1.2 mm and grind the lower edge; the supporting wooden table should be perpendicular to the blade.
• 6.5 Air bath or constant-temperature laboratory: capable of maintaining 25.0 °C±0.5 °C and accommodating the assembled lubricating grease worker; the water bath should be equipped with facilities to prevent the sample surface from contacting water, and with a cover to maintain the air temperature above the sample at 25 °C; for block penetration determination, an air bath capable of maintaining 25.0 °C±0.5 °C is required, or a sealed container placed in a water bath may be used; a water bath or constant-temperature laboratory may be used instead of an air bath.
• 6.6 Thermometer: a thermometer calibrated at 25 °C, for use in a water bath or air bath.
• 6.7 Oven: capable of maintaining 85 °C±2 °C, used for melting petrolatum samples.
• 6.8 Spatula: a suitable corrosion-resistant square-ended hard blade (e.g., width 32 mm, length not less than 150 mm); for 1/2 and 1/4 scale cone tests, the spatula width should be 13 mm.
• 6.9 Stopwatch: with a division of 0.1 s.
• 6.10 Petrolatum sample container: a flat-bottomed cylindrical container with a diameter of 100 mm±5 mm and a depth of 65 mm or greater than 65 mm, made of metal with a thickness of at least 1.6 mm, and capable of providing a suitable waterproof cover; flexible "ointment box" type containers should not be used.

6. Recommended operating conditions

• Lubricating grease penetration determination temperature: 25.0 °C±0.5 °C.
• Cone falling time: 5.0 s±0.1 s.
• Number of strokes for worked penetration: 60 double strokes; minimum stroke not less than 63 mm, maximum stroke not greater than 71.5 mm.
• Extended worked penetration: perform the specified or agreed number of double strokes; immediately after completing the working, place in a constant-temperature air bath or water bath so that the sample reaches 25.0 °C±0.5 °C within 1.5 h; after removal, perform 60 more double strokes within about 1 min.
• Laboratory temperature before extended worked penetration test: 15 °C to 30 °C, and the sample should be left in the laboratory long enough for the grease temperature to reach 15 °C to 30 °C.
• Block penetration: place the sample in a constant-temperature air bath at 25.0 °C±0.5 °C for at least 1 h.
• Petrolatum melting: oven 85 °C±2 °C; cooling: cool without ventilation at a controlled temperature of 25 °C±2 °C for 16 h to 18 h; before testing, use a water bath at 2 h to bring the temperature to 25.0 °C±0.5 °C.
• Petrolatum container filling: fill to within 6 mm of the container rim.
• 1/2 and 1/4 scale cone worked penetration: pile the center portion to a height of about 6 mm, without using a thermometer.
• No other recommended operating conditions are provided in the available source.

7. Sampling and sample preparation

• 7 Sampling: unless otherwise specified in the product specification, sampling shall be carried out in accordance with SH/T 0229; the sample should be inspected for any signs of non-uniformity, such as oil separation, phase change, or severe contamination; if abnormalities are found, resampling should be carried out.
• 8.1.1 Preparation of unworked penetration sample:
  • Take enough sample (at least 0.5 kg) to fill the grease worker cup; if the sample penetration is greater than 200 units, the amount of sample taken must be at least three times the amount needed to fill the worker cup.
  • Place the assembled empty grease worker or a metal container of the same internal dimensions and an appropriate amount of sample in a 25.0 °C±0.5 °C air bath for a sufficient time so that the sample temperature reaches 25.0 °C±0.5 °C.
  • The sample should preferably be transferred as a whole block, so that the filled amount overfills the container and is subjected to as little agitation as possible; vibrate the container to remove entrained air, press firmly with a spatula, and obtain a full cup of sample free of air pockets; hold the spatula at an angle of 45° to the direction of movement and scrape it across the edge of the worker cup to remove excess sample; immediately carry out the penetration determination.
  • For greases with an unworked penetration greater than 265 units, the determination should be carried out in a container having the same diameter as the grease worker cup.
• 8.2.1 Sample preparation for worked penetration: Take enough sample (at least 0.5 kg) to fill the grease worker cup; during filling, heap the central portion to a height of about 13 mm, and press firmly with a spatula to avoid entraining air; assemble with the perforated plate in the raised position, open the vent valve, and press the perforated plate to the bottom of the cup; insert a thermometer so that its top is at the center of the sample; place in a 25.0 °C±0.5 °C bath until the temperature reaches 25.0 °C±0.5 °C.
• 8.2.2 Sample preparation after working: Vigorously vibrate the worker cup, and use a spatula to fill the sample into the holes left by the perforated plate and remove air pockets; scrape off excess sample above the edge of the worker cup to form a flat surface.
• 8.3.1 Sample preparation for extended worked penetration: According to 8.2.1.2, fill a clean worker cup with sample, assemble the worker, and perform the specified or agreed number of double strokes.
• 8.4.1 Sample preparation for block penetration: Take a grease hard enough to retain its shape, and use a grease cutter to cut it at room temperature into a cube with an edge length of about 50 mm; cut off a layer about 1.5 mm thick from each of the three faces adjacent to one corner; take care not to touch the portion of the newly exposed face to be used for the test; place in a 25.0 °C±0.5 °C constant-temperature air bath for at least 1 h.
• 9.2.1 Sample preparation for unworked penetration with 1/2 and 1/4 ratio cones: Take enough sample to fill the grease worker cup; if the 1/4 penetration is greater than 47 units or the 1/2 penetration is greater than 97 units, only 1 tests should be performed in 1 cups, and at least the amount of sample needed to fill 3 worker cups is required; operate according to 8.1.1.2.
• 9.3.1 Sample preparation for worked penetration with 1/2 and 1/4 ratio cones: Take enough sample to fill a suitable grease worker cup; operate according to 8.2.1.2, but heap the central portion to a height of about 6 mm, and do not use a thermometer.
• 10.1 Sample preparation for petrolatum:
  • For penetration greater than 200 units, take about 1 kg of sample; for penetration not greater than 200 units, take about 700 g of sample.
  • For penetration greater than 200 units, prepare 3 samples separately; for penetration not greater than 200 units, prepare one sample.
  • Place the sample in a 85 °C±2 °C oven to melt, heating the sample together with its container to 85 °C; after removal, fill the container to within 6 mm of the rim; cool in a draft-free place at 25 °C±2 °C for 16 h～18 h; before testing, place in a water bath for 2 h so that the temperature reaches 25.0 °C±0.5 °C; the sample surface should not be smoothed or the sample worked in any other way.
  • Some synthetic petrolatums will be affected by contact with water and should be covered with a sealing lid according to the grease test method; non-synthetic petrolatums are not affected by water and need not be covered.
  • If the room temperature deviates from 25 °C by 2 °C or 2 °C or more, immediately before the determination place the cone in a water bath to equilibrate to 25.0 °C±0.5 °C, then dry it with a lint-free cloth or paper.

8. Analytical procedure

• 8.1 Unworked penetration:
  • 8.1.2 Clean the cone and cone shaft: Check whether the cone tip is damaged; carefully clean the cone before each test; during cleaning, the cone shaft may be fixed in the raised position; remove all grease or oil from the cone shaft; do not rotate the cone shaft; take care not to damage the cone tip.
  • 8.1.3 Penetration determination: Place the worker cup on the penetrometer platform and adjust it to be completely level; adjust the measuring mechanism so that the cone is held at the "zero" position; bring the cone tip just into contact with the sample surface; for samples with penetration greater than 400 units, the cone tip should be aligned with the center of the worker cup, with a deviation within 0.3 mm; quickly release the cone shaft, allow it to fall for 5.0 s±0.1 s, then clamp the cone shaft; gently press down the indicator shaft until it is stopped by the cone shaft, and read the penetration value from the indicator dial.
  • If the sample penetration exceeds 200 units, carefully align the cone with the center of the container; only 1 test may be performed on this sample.
  • If the sample penetration is not greater than 200 units, 3 tests may be carried out in the same container; the measurement points are located at the midpoints of the 3 radii of each container sector 120°.
  • Perform a total of 3 determinations on the sample and record the measured values.
• 8.2 Worked penetration:
  • Work according to 8.2.1.2: Subject the sample to 60 full double strokes of the perforated plate in about 1 min, then return the perforated plate to the top position; open the vent valve, remove the top cover and perforated plate, and scrape as much as possible of the easily removable sample adhering to the perforated plate back into the worker cup; immediately determine according to 8.2.2 and 8.2.3.
  • 8.2.2 Sample preparation: Vigorously vibrate the worker cup, and use a spatula to fill the sample into the holes left by the perforated plate and remove air pockets; scrape off excess sample above the edge of the worker cup to form a flat surface.
  • 8.2.3 Penetration determination: Determine according to 8.1.2 and 8.1.3; immediately carry out 2 or more successive determinations in the same sample; record 3 measured values.
• 8.3 Extended worked penetration:
  • Fill with sample according to 8.2.1.2, assemble the worker, and perform the specified or agreed number of double strokes; during working, keep the pressure cap on the worker cover tightly sealed.
  • Immediately after completing the working, place the worker in a constant-temperature air bath or water bath so that the sample reaches 25.0 °C±0.5 °C within 1.5 h; after removal, subject the sample to 60 more double strokes in about 1 min; carry out sample preparation and penetration determination according to 8.2.2 and 8.2.3.
• 8.4 Block penetration:
  • Place the sample on the penetrometer platform that has been adjusted to be completely level, with one test face upward, and press its corners so that the sample remains level and stable; adjust the measuring mechanism so that the cone is at the "zero" position, and bring the cone tip just into contact with the center surface of the sample; determine according to 8.1.2 and 8.1.3.
  • Perform a total of 3 determinations on one exposed face of the sample; the measurement points should be at least 6 mm from the edge and as far apart from each other as possible, and should not touch areas that have been disturbed, air holes, or other obvious surface defects.
  • If any one result differs from the other results by more than 3 units, supplementary tests should be carried out until the difference among the 3 values obtained does not exceed 3 units; take the average of the 3 values as the penetration value of the tested surface.
  • 8.4.3 Supplementary determination: To balance the effect of fiber orientation in testing fiber greases, repeat the determination on the other two test faces of the sample and record the average values; when agreed by both parties, smooth, non-fibrous greases may be tested on one face.
• 9 Method for 1/2 and 1/4 ratio cones:
  • 9.2 Unworked penetration: Carefully clean the cone before each test; fix the cone shaft in the raised position; remove all grease or oil from the cone shaft; do not rotate the cone; use the cone to make one preliminary penetration determination at the center of the sample surface; if the 1/4 penetration is greater than 47 units or the 1/2 penetration is greater than 97 units, only one test may be performed on this sample; otherwise, 3 tests may be performed in the same container; operate according to 8.1.3.1 and 8.1.3.4.
  • 9.3 Worked penetration: Operate according to 8.2.1.2, but heap the central portion to a height of about 6 mm, and do not use a thermometer; prepare according to 8.2.2; immediately determine according to 9.2.2 and 9.2.3.1～9.2.3.3; operate according to 8.1.3.1; immediately carry out two or more successive determinations in the same sample; record 3 measured values.
• 10 Determination of petrolatum penetration: Operate according to 8.1.2 and 8.1.3; some harder petrolatums tend to form a pronounced depression at the center when solidified, and testing should not be carried out in the depression.

9. Qualitative and quantitative and calculation formulas

• 11.1 Calculation of full-scale cone penetration: Calculate the average of the recorded values obtained from the determinations.
• 11.2 Conversion of 1/2 and 1/4 penetration to full-scale penetration:
  • 11.2.2 1/4 ratio cone: P₁ = 3.75p₁ + 24
    • P₁: approximate full-scale penetration, in units of 0.1 mm;
    • p₁: 1/4 penetration, in units of 0.1 mm.
  • 11.2.3 1/2 ratio cone: P₂ = 2p₂ + 5
    • P₂: approximate full-scale penetration, in units of 0.1 mm;
    • p₂: 1/2 penetration, in units of 0.1 mm.
• 12 Expression of results: Round the result to an integer (in units of 0.1 mm).
• Note: Penetration 1 units = 0.1 mm (see 3.2 note).

10. Precision

• 13.1 General: Precision is determined based on ISO 4259:2006 through interlaboratory statistical analysis results; judge the reliability of test results according to 13.2 and 13.3 (95% confidence level).
• 13.2 Repeatability (r): the difference between two test results obtained by the same operator, in the same laboratory, using the same instrument, following the same test method, on the same test sample in successive determinations shall not be greater than the values specified in Table 1, Table 2 and Table 3.
• 13.3 Reproducibility (R): the difference between two single, independent results obtained by different operators, in different laboratories, using different instruments, following the same test method, on the same test sample in separate determinations shall not be greater than the values specified in Table 1, Table 2 and Table 3.
• Table 1 Precision of full-scale cone penetration of lubricating grease (unit is 0.1 mm):
  • Unworked, penetration range 85～475, repeatability r = 8, reproducibility R = 19
  • Worked, penetration range 130～475, repeatability r = 15, reproducibility R = 20
  • Extended worked, penetration range 130～475, repeatability r = ?, reproducibility R = 270
  • Block, penetration range below 85, repeatability r = ?, reproducibility R = 11
  • Note: the precision for penetration above 475 units has not yet been determined; room temperature within the range of 15 °C～30 °C, penetration measured after 100000 reciprocating working strokes.
  • Requires confirmation (source-text extraction): in Table 1, the values for extended worked repeatability and block repeatability are originally source-text extraction as “?”, and cannot be confirmed.
• Table 2 Precision of penetration of lubricating grease with 1/2 and 1/4 ratio cones (unit is 0.1 mm):
  • Unworked, 1/2 ratio, repeatability r = 5 (10), reproducibility R = 13 (26)
  • Worked, 1/2 ratio, repeatability r = 3 (6), reproducibility R = 10 (20)
  • Unworked, 1/4 ratio, repeatability r = 3 (11), reproducibility R = 10 (38)
  • Worked, 1/4 ratio, repeatability r = 3 (11), reproducibility R = 7 (26)
  • Note: the numbers in parentheses indicate the corresponding precision values after conversion to full-scale penetration values.
• Table 3 Precision of petrolatum penetration:
  • Repeatability r = 2 + 0.05X₁
  • Reproducibility R = 9 + 0.12X₂
  • Note: X₁ is the average of two replicate test results; X₂ is the average of two single, independent test results.
  • Unit is 0.1 mm.

11. Report

• 14 The test report shall contain at least the following information:
  • a) state this document;
  • b) the test procedure used (as described in Chapter 8, Chapter 9 or Chapter 10), the method used (worked, worked, extended worked or block) and the cone used (full-scale cone, optional cone, 1/2 ratio cone or 1/4 ratio cone);
  • c) sample type and identification method;
  • d) test results (see Chapter 12);
  • e) state any differences from the specified test procedure by agreement or otherwise;
  • f) date of test.
• Requires confirmation (source-text extraction): in b), “worked, worked, extended worked or block” is suspected to be “unworked, worked, extended worked or block”.

12. Normative references

• SH/T 0229 Sampling method for solid and semi-solid petroleum products (normative reference)
• GB/T 7631.8—1990 (Chapter 5 informative reference)
• ISO 4259:2006 Petroleum products—Determination and application of precision data in relation to methods of test (Bibliography)
• ISO 6743-99 Lubricants, industrial oils and related products (class L)—Classification—Part 99: General (Bibliography)
• ISO 12924 Lubricants, industrial oils and related products (Class L)—Family X (Greases)—Specification (Bibliography)
• Technical differences between this document and ISO 2137:2020: replaced ISO 23572 with the normative references SH/T 0229 (see Chapter 7).
• Editorial modifications of this document compared with ISO 2137:2020: added an informative reference to GB/T 7631.8—1990 in Chapter 5, and added “Bibliography”.

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