SH/T 0754-2005 Evaluation method for corrosion performance of diesel engine oils under 135℃

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Card type: Test method

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

• Standard number: SH/T 0754-2005
• Chinese title: Evaluation method for corrosion performance of diesel engine oils under 135℃
• English title: Standard test method for evaluation of corrosiveness of diesel engine oil at 135℃
• Replacement relationship: not provided in the available source (the foreword only states modified adoption of ASTM D6594-00, and does not mention replacement of an old version of the standard)
• Adoption relationship: modified adoption of ASTM D6594-00 "Evaluation method for corrosion performance of diesel engine oils under 135℃"
• Publication/implementation: published by 2005-04-11, implemented by 2005-09-01
• Issuing body: National Development and Reform Commission of the People's Republic of China
• Custodian: Sinopec Research Institute of Petroleum Processing
• Drafting organization: PetroChina Lubricant Research and Development Center
• Main drafters: She Haibo, Zhang Changhe, Yu Jun
• Main differences from ASTM D6594-00: some referenced standards adopt corresponding Chinese national standards and industry standards; the data dictionary in Appendix A2 of ASTM D6594-00 is not adopted (its content is mainly explanation of abbreviations for reference); the wording of repeatability and reproducibility is modified according to Chinese practice; the keywords of Chapter 14 are deleted.
• Appendices: Appendix A and Appendix B are both normative appendices.

2. Scope of application and non-applicability

• 1.1 This standard is used to evaluate the corrosion tendency of diesel engine oils toward various metals, especially lead, copper alloys, and the like commonly used in diesel engine cam followers and bearings.
• 1.2 This standard uses International System of Units (SI) units.
• 1.3 This standard does not address all safety problems associated with its use; users should establish appropriate safety and protection measures before using this standard and formulate corresponding management systems.
• Non-applicability scope: not provided in the available source.

3. Method principle

• Chapter 4 Method summary: immerse four metal test pieces of copper, lead, tin, and phosphor bronze in a certain amount of engine oil sample, pass air into the sample at high temperature for a specified time, and after the test ends, separately conduct corrosion testing on the copper metal test piece and the sample.
• A reference oil test is conducted in each group of tests to verify whether that test is valid.
• Chapter 5 Significance and use: this test method is mainly used to simulate the corrosion process of nonferrous metals in diesel engine oils; the corrosion process studied is mainly caused by certain chemical substances in the lubricating oil rather than by degradation or contamination of the lubricating oil. A large amount of road test data proves that this test method is correlated with cam and bearing failures caused by corrosion.

4. Reagents and materials (purity / preparation)

• 7.1 Reagent purity: unless otherwise specified, analytical grade reagents may be used in all tests.
• 7.2 Metal test pieces: except that the lead test piece has dimensions 2.5cm × 2.5cm × 0.178cm, the other test pieces have dimensions 2.5cm × 2.5cm × 0.081cm, and each test piece has two holes. The material and type are copper (R401-A), lead (R401-Lead), tin (R401-tin), and phosphor bronze (R401-PRz). Note: metal test pieces can be purchased from Test Engineering INC in the United States.
• 7.3 Sandpaper: 58.5μm aluminum oxide and 35.0μm silicon carbide sandpaper; do not use sandpaper containing iron-based abrasive, such as natural emery.
• 7.4 Absorbent cotton: contains 100% cotton.
• 7.5 Acetone: sulfur-free. Warning: flammable, harmful.
• 7.6 Glassware cleaning solution: chromic acid cleaning solution, prepared by mixing 35mL saturated sodium dichromate (hydrated) and 1000mL sulfuric acid. Warning: can cause burns.
• 7.7 Tetrahydrofuran (THF). Warning: flammable, toxic and harmful.
• 7.8 Degreasing solvent: tetrahydrofuran (THF) is recommended.
• 7.9 Solvent naphtha: naphtha, containing aromatics. Warning: flammable, toxic and harmful.
• 7.10 Reference oil: provided by TMC.
• 7.11 Detergent: for cleaning glassware.

5. Apparatus and equipment

• 6.1 Standard-wall-thickness borosilicate glass apparatus, composed of the following parts:
  • 6.1.1 Sample tube: see Figure 1 (the original figure number source-text extraction is "Figure to", requires confirmation against the source standard (source-text extraction))
  • 6.1.2 Sample tube elbow: see Figure 2 (the original source-text extraction is "Figure 20", requires confirmation against the source standard (source-text extraction))
  • 6.1.3 Air tube: see Figure 3 (the original source-text extraction is "Figure 30", requires confirmation against the source standard (source-text extraction))
  • 6.1.4 Thermocouple tube: see Figure 4
  • 6.1.5 Spherical condenser tube: see Figure 5 (the original source-text extraction is "Figure 50", requires confirmation against the source standard (source-text extraction))
  • 6.1.6 Assembled apparatus: see Figure 6 (the original source-text extraction is "Figure 60", requires confirmation against the source standard (source-text extraction))
• 6.2 Other glassware and accessories
  • 6.2.1 Hooks (for metal test pieces): made of stainless steel, dimensions noted in Figure 7.
  • 6.2.2 Connector: made of polytetrafluoroethylene, 10/18 connector, used to seal the air tube and the sample tube elbow.
• 6.3 Other apparatus
  • 6.3.1 Heating bath: temperature control accuracy ±0.5℃, immersion depth 250mm±20mm, oil bath recommended. Warning: the apparatus surface temperature is high; protective measures should be taken to avoid direct skin contact.
  • 6.3.2 Fume hood: to remove fumes generated during heating.
  • 6.3.3 Dry air source: dew point −68℃ (the original source-text extraction is "one 689C", requires confirmation against the source standard (source-text extraction)).
    • 6.3.3.1 Optionally, an air dryer may be used to dry the air to meet the requirement of 6.3.3. Use a glass tube filled with anhydrous calcium sulfate as the dryer, and control the linear velocity of air passing through the tube to not exceed 1.2m/min.
  • 6.3.4 Flowmeter: measurable flow range 10L/h±1L/h (the original source-text extraction is "IOUh ± lUho", requires confirmation against the source standard (source-text extraction)).
  • 6.3.5 Balance: range 2500g, sensitivity 0.1g (the original source-text extraction is "25008, sensitivity 0. 1g", requires confirmation against the source standard (source-text extraction)).
  • 6.3.6 Syringe: capable of accurately measuring 100mL of liquid.
  • 6.3.7 Drying oven (optional): for drying glassware at high temperature.
  • 6.3.8 Tweezers: made of stainless steel; or gloves (dust-free).
  • 6.3.9 Thermocouple or equivalent: a sheathed thermocouple may be used in direct contact with the oil; for a non-sheathed thermocouple, a thermowell may be used, and the thermowell is filled with a heat transfer medium.
  • 6.3.10 Sand block and fixture: for treating test pieces.

6. Recommended operating conditions

• Sample temperature: 135℃±0.5℃ (9.6)
• Air flow rate: 5L/h±0.5L/h (9.8)
• Test time: 168h (9.8, 9.9)
• Sample tube immersion depth: 30cm±5cm (9.6)
• Heating bath temperature control accuracy: ±0.5℃ (6.3.1)
• Air source dew point: −68℃ (6.3.3)
• Dryer air linear velocity: not exceeding 1.2m/min (6.3.3.1)

7. Sampling and sample preparation

• 9.5 Use a syringe to add 100mL±1mL of sample into the sample tube, weigh again the total mass of the air tube, sample tube, and their contents, to the nearest 0.1g, and determine the sample mass.
• Metal test piece preparation (8.3):
  • 8.3.1 In all steps, test pieces must be handled with stainless steel tweezers or dust-free gloves. If there are many defects or particles on the metal test piece, first grind them off with coarse sandpaper, then polish with the 58.5μm sandpaper and 35.0μm sandpaper described in 8.3.2. Note: this operation and the following preparation process should be carried out in a fume hood.
  • 8.3.2 Use a sand block with a test piece fixture to fix the test piece; first use 58.5μm sandpaper to grind off dirt from both surfaces and the four edges of the square metal test piece, use a 0.16μm drill bit to remove burrs at the small holes, then use 35.0μm sandpaper wetted with acetone for fine grinding to remove previous grinding marks.
    • 8.3.2.1 Preferably, place the 35.0μm sandpaper flat, and rub the test piece lengthwise on the 35.0μm sandpaper in a direction perpendicular to the grinding direction of the 58.5μm sandpaper. Each sheet of sandpaper may only be used for wiping the same type of metal test piece.
    • 8.3.2.2 Ensure that all surfaces of all test pieces are ground in the same manner. Carry out this procedure under normal indoor lighting; it is not necessary to observe the grinding condition of the test piece surface under strong light, and do not scratch or mark the test piece surface.
  • 8.3.3 Place the ground test pieces in tetrahydrofuran.
  • 8.3.4 Before the test begins, remove the test pieces from the tetrahydrofuran and wipe them with clean absorbent cotton; wipe gently to remove particles on the test pieces, and do not grind the test pieces again.
  • 8.3.5 Then rinse the test pieces with tetrahydrofuran and place them in a desiccator to dry.
• Glassware cleaning (8.1):
  • 8.1.1 Clean all glassware and accessories with degreasing solvent to remove residual oil, and air dry.
  • 8.1.2 Clean the glassware and accessories with detergent, first rinse with tap water, then rinse with distilled water, and dry.
  • 8.1.3 Place the above apparatus in a dust-proof cabinet and take it out at the time of testing. If stored for more than one week, it should be cleaned with distilled water, dried, and then used.
  • 8.1.4 If there are special requirements, a further glassware cleaning procedure must be used.
    • 8.1.4.1 Soak all glassware in glassware cleaning solution (see clause 7.6) for 3h～16h.
    • 8.1.4.2 Remove the glassware, first rinse several times with tap water, then rinse with distilled water, and dry.
    • 8.1.4.3 In the case of arbitration testing, unless there is another cleaning solvent satisfactory to all parties, it is necessary to use this procedure to clean the glassware more thoroughly.

8. Analytical procedure

• 8.2 Apparatus assembly: assemble the apparatus as shown in Figure 6.
• 9.1 Put the hooks on the lower part of the air tube, and hang the test pieces on their respective hooks.
• 9.2 The order for hanging the test pieces is lead, copper, tin, phosphor bronze.
• 9.3 Place the air tube and the bundle of test pieces on it into the sample tube so that the air tube contacts the bottom of the sample tube. Attach the sample tube elbow to the sample tube.
• 9.4 Weigh the total mass of the air tube, sample tube, and their contents, to the nearest 0.1g.
• 9.5 Using a syringe, add the 100mL±1mL test sample into the sample tube, weigh again the total mass of the air tube, sample tube and their contents, to the nearest 0.1g, and determine the sample mass.
• 9.6 Place the sample tube into the heating bath, with an immersion depth of 30cm±5cm, connect the sample tube to the condenser and other components, and control the sample temperature at 135℃±0.5℃.
• 9.7 Pass cooling water through the condenser.
• 9.8 Connect the air tube to an air source that provides clean dry air. At the start of the test, introduce air into the sample at a flow rate of 5L/h±0.5L/h and maintain it for 168h. Pre-dried air or reagent-grade bottled air should be used. Use a calibrated air flow meter to control the air flow.
• 9.9 After the 135℃ test of 168h, close and disassemble the air flow meter.
  • 9.9.1 Disconnect the air source and remove the condenser.
  • 9.9.2 Remove the sample tube from the heating bath and cool for at least 15min; after cooling, wipe the exterior clean with a cloth moistened with solvent naphtha.
  • 9.9.3 Weigh again the total mass of the air tube, sample tube and their contents, to the nearest 0.1g, calculate the remaining sample mass, and determine the percentage evaporation loss of the sample mass (see 10.5.1). If the percentage evaporation loss is greater than 8%, this indicates leakage; eliminate the source of leakage and retest with a new sample and new metal test specimens.
• 10.1 Remove the air tube and the test specimen bundle from the sample tube; do not touch the test specimens with hands; retain the sample tube and sample for further testing.
• 10.2 Using tweezers or gloves, clean the copper test specimen in tetrahydrofuran; discard the other test specimens.
• 10.3 Rate the corrosion on both sides of the copper strip using the GB/T 5096 method.
• 10.4 As soon as possible, analyze the concentrations of copper, lead and tin in the sample before and after the test using the GB/T 17476 method.

9. Qualitative and Quantitative Determination and Calculation Formulas

• 10.5.1 The percentage evaporation loss of the sample L (%) is calculated according to formula (1):

  L = (W₁ − W₂) / W₃ × 100 ………………(1)

  Where:

  • W₁——total mass of the air tube, sample tube and contents (including the sample) before the test, g;
  • W₂——total mass of the air tube, sample tube and contents (including the sample) after the test, g;
  • W₃——initial mass of the sample, g.

• 10.5.2 The change in metal concentration in the sample after the test ΔC (mg/kg) is calculated according to formula (2):

  ΔC = C₂ − C₁ ………………(2)

  Where:

  • C₁——metal concentration value measured before the test of the sample (see 10.4), mg/kg;
  • C₂——metal concentration value measured after the test of the sample (see 10.4), mg/kg.

• Copper strip corrosion rating: Rate the corrosion on both sides of the copper strip according to the GB/T 5096 method (10.3); if the corrosion ratings on the two surfaces of the copper strip differ, report the corrosion rating according to the more severely corroded side (12.1).

10. Precision

• 13.1 Precision: The precision of this standard was determined in accordance with ASTM E691 as a guide, through interlaboratory statistical testing in seven cooperating laboratories. The reliability of test results can be judged according to the following provisions (95% confidence level).
• 13.1.1 Repeatability (I.P.)
  • Note: I.P. is the abbreviation of Intermediate Precision, literally translated as centered precision, commonly called repeatability.
  • For the same operator, using the same instrument, under the same operating conditions, the difference between two results obtained from the determination of the same sample shall not exceed the I.P. value in formula (3) and formula (4):
  • Change in copper metal concentration in the sample after the test ΔC (mg/kg) (natural logarithm transformation applied):
    • S_I.P. = 0.272, ln(I.P.) = 0.754 ………………(3)
  • Change in lead metal concentration in the sample after the test ΔC (mg/kg):
    • S_I.P. = 6.14, I.P. = 43.02 ………………(4)
• 13.1.2 Reproducibility (R)
  • For different operators in different laboratories, the difference between two results obtained from the determination of the same sample shall not exceed the R value in formula (5):
  • Change in copper metal concentration in the sample after the test ΔC (mg/kg) (natural logarithm transformation applied):
    • S_R = 0.400, R = 1.109 ………………(5)
• 13.1.3 If a suitable reference oil is available, the precision of the change in tin metal concentration in the sample after the test ΔC can be determined.
• 13.2 Bias cannot be determined for the time being; it will be determined after collecting a large amount of data.

11. Report

• 12 Report (for format see Appendix B)
  • 12.1 If the corrosion ratings on the two surfaces of the copper strip differ, report the corrosion rating according to the more severely corroded side (see 10.3).
  • 12.2 Report the concentrations of copper, lead and tin in the reference oil before and after the test and their changes (C₁, C₂, ΔC in 10.5.2).
  • 12.3 Report the concentrations of copper, lead and tin in the sample before and after the test and their changes (C₁, C₂, ΔC in 10.5.2).
• Appendix B (Normative Appendix) Report Format:
  • B.1 The report format for evaluating the corrosion performance of diesel engine oils is shown in Table B.1 to Table B.3.
  • Table B.1 Report cover: test validity (valid/invalid), test heat bath number, test end date, oil product designation, formulation/standard designation, distinguishing number, heat bath run number, data, heat bath position, test end time, etc.
  • Table B.2 Summary of test results: laboratory, heat bath number, heat bath run number, heat bath position, test end date, test end time, oil product designation, start date, formulation/standard designation, test duration; test oil sample characteristics (reference oil test/sample test); metal concentration change (mg/kg) (metal type: copper, lead, tin, internal standard; number of tests; pre-test concentration, average value, post-test concentration, average value, concentration change for reference oil test/sample test); GB/T 5096 copper strip corrosion rating; evaporation loss/%; metal type (copper, lead, tin, phosphor bronze) test specimen sequence number for reference oil test/sample test.
  • Table B.3 Explanation: laboratory, heat bath number, heat bath run number, heat bath position, test end date, test end time, oil product designation, start date, formulation/standard designation.

12. Referenced Documents

• GB/T 5096 Petroleum products—Copper strip corrosion test method
• GB/T 17476 Determination of additive elements, wear metals and contaminants in used lubricating oils and certain elements in base oils (inductively coupled plasma atomic emission spectrometry) (the original text source-text extraction is "inductively coupled plasma atomic emission spectrometry", requires confirmation against the source standard (source-text extraction))
• SH/T 0512 Gasoline engine oils—Low-temperature rust evaluation method (MS procedure ID method)
• SH/T 0763 Gasoline engine oils—Rust prevention evaluation method (BRT method)
• ASTM E691 Practical method for conducting interlaboratory studies to determine the precision of test methods

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.

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