SH/T 0801-2007 Determination of homogeneity and miscibility of engine oils

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Card type: Test method

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

• Standard number: SH/T 0801—2007
• Chinese title: Determination of homogeneity and miscibility of engine oils
• English title: Standard test method for determination of homogeneity and miscibility in automotive engine oils
• Replacement relationship: not provided in the available source (no replacement of any standard is mentioned)
• Adoption relationship: modified adoption of ASTM D6922-03 "Determination method for homogeneity and miscibility of engine oils", redrafted according to ASTM D6922-03
• Main technical differences from ASTM D6922-03:
  • Some referenced standards adopt the corresponding national standards and industry standards of our country
  • In clause 6.7 of this standard, the liquid cold bath is changed to a cooling chamber
  • In 10.4.11 of this standard, 28°C is changed to 27°C
• Editorial modifications: In Table 1, the test report form adds the description of particle size by sw as no particles; the chapter on keywords is deleted
• Appendix A is a normative appendix
• Publication/implementation: published on 2007-08-01, implemented on 2008-01-01
• Issuing body: National Development and Reform Commission of the People's Republic of China
• Custodian: Sinopec Research Institute of Petroleum Processing
• Drafting organization: Lubricant Branch of Sinopec Corp.
• Main drafters: Cui Haiou, Meng Xuemei

2. Scope of application and non-applicability

• 1.1 This standard specifies the determination method for the homogeneity of engine oils and the retention of homogeneity after a specified temperature change, as well as the determination method for the miscibility of engine oils mixed with specified standard reference oils after a specified temperature change.
• 1.2 This standard uses the International System of Units [SI] units.
• 1.3 This standard involves certain hazardous materials, operations and equipment, but does not purport to address all safety problems associated with them. Therefore, users of this standard must establish appropriate safety and protective measures and determine corresponding management systems before use.
• Non-applicable scope: not provided in the available source.

3. Method principle

• 4 Method summary: Visually determine the color and observe the test sample and six sample mixtures after the sample is mixed with different reference oils. Determine the pour point of the sample and the six sample mixtures, then warm them back to room temperature, visually determine the color, and observe them. Heat the sample and the six sample mixtures to 232°C, then cool to room temperature, store at the pour point temperature of the sample for 18h~24h, visually determine the color, and observe the separation phenomenon during the process of thawing and warming back to room temperature. (This paragraph in the original text has heavy source-text extraction noise, and some text requires confirmation against the source standard (source-text extraction))
• 5 Significance and use: The ability of engine oils from different manufacturers to maintain homogeneity and miscibility is of important significance. Since automobile drivers generally cannot predict information from engine oil manufacturers regarding oil use, if the oil cannot maintain homogeneity and have appropriate functions, it may lead to engine failure.

4. Reagents and materials (purity / preparation)

• 7 Reagents and materials: reference oils, provided by the monitoring center (TMC) of the American Society for Testing and Materials (ASTM), including HMA, HMB, HMC, HMD, HME, HMF, a total of 6 reference clear oils (the original text says "reference clear", suspected to be "reference oil", requires confirmation against the source standard (source-text extraction)).
• Purity and preparation method: not provided in the available source.

5. Instruments and equipment

• 6.1 Test tube: a cylindrical flat-bottomed test tube made of transparent glass. The inner diameter of the test tube is 30.0mm–32.4mm, the outer diameter is 33.2mm–34.8mm, the height is 115mm~125mm, and the wall thickness of the test tube does not exceed 1.6mm. There is a marked line from the bottom of the test tube to 54mm±3mm. (The original text number source-text extraction has noise, requires confirmation against the source standard (source-text extraction))
• 6.2 Thermometer: a thermometer conforming to GB-36 in GB/T 514 or other equivalent thermometers.
• 6.3 Stopper: a clean stopper, which may be perforated or have a center hole, used for inserting a thermometer.
• 6.4 Sleeve: a cylindrical sleeve with a flat bottom made of glass or metal, leakproof, with a height of about 120mm, and the inner diameter of the sleeve is about 9.0mm~12.0mm larger than the outer diameter of the test tube.
• 6.5 Disc: made of cork or felt, about 6mm thick, with a diameter the same as the inner diameter of the sleeve.
• 6.6 Gasket: ring-shaped, 5mm thick, able to fit exactly on the outside of the test tube so that it is relatively loose inside the sleeve. The purpose of the ring-shaped gasket is to prevent the test tube from contacting the sleeve.
• 6.7 Cooling chamber: any liquid cold bath and other cooling equipment capable of providing the required temperature.
• 6.8 Oven: capable of raising the temperature of the sample to 232°C±2°C within 25min~90min.
• 6.9 Pour point tester (manual or automatic optional): a pour point tester conforming to the requirements of GB/T 3535. Automatic pour point testers have advantages such as saving time and using less sample, and may also have other advantages in use. Ensure that the calibration, adjustment and operation of the automatic pour point tester follow the manufacturer's procedure requirements. However, when the pour point is reported by an automatic pour point tester, in some cases, a certain (the original text here source-text extraction is incomplete, requires confirmation against the source standard (source-text extraction)). In case of dispute, the manual instrument shall prevail for arbitration testing.

6. Recommended operating conditions

• Heating temperature: 232°C±2°C (10.5.4)
• Heating time: raise temperature to 232°C±2°C within 25min~90min (6.8, 10.5.4)
• Cooling chamber temperature: -18°C~-15°C (10.4.3, the original text says "-18C~-150", suspected to be -18°C~-15°C, requires confirmation against the source standard (source-text extraction))
• Second cooling chamber temperature: specific value not provided in the available source (source-text extraction is missing at 10.4.8, requires confirmation against the source standard (source-text extraction))
• Third cooling chamber temperature: -52°C~-49°C (10.4.10)
• Storage time at pour point temperature: 18h~24h (10.6.1)
• Pour point determination temperature interval: in multiples of 3°C (10.4.5, 10.4.9, 10.4.11)
• The total operation time from removing the test tube to returning it to the sleeve shall not exceed 3s (10.4.6)
• Keep the test tube horizontal for 5s (10.4.7)
• Temperature difference between additional cooling chambers: 17°C (10.4.11)

7. Sampling and sample preparation

• 8 Sampling: sample according to the requirements of GB/T 4756.
• 9 Test preparation:
  • 9.1 Place on the test rack (the original text is incomplete, requires confirmation against the source standard (source-text extraction))
  • 9.2 Measure and mark on each test tube (the original text source-text extraction has noise, requires confirmation against the source standard (source-text extraction))
  • 9.2.1 Measure and mark on each test tube the positions from the bottom of the test tube to 23mm and to 54mm.
  • 9.2.2 Mark the first test tube for placing the sample.
  • 9.2.3 Mark with letters A to F, designating the six test tubes for mixing the sample with reference oils.
  • 9.3 Shake the sample vigorously to homogenize it.
  • 9.4 Fill the sample into the six test tubes (test tubes A to F) to the mark at 23mm.
  • 9.5 Fill the sample into the test tube marked as the sample to the mark at 54mm.
  • 9.6 Shake the six reference oils vigorously to homogenize them.
  • 9.7 Fill the corresponding reference oil into the test tube marked as (the original text source-text extraction has noise, requires confirmation against the source standard (source-text extraction)) to the mark at 54mm, obtaining six sample mixtures.
  • 9.8 Stopper each test tube with a leakproof stopper (the original text source-text extraction has noise, requires confirmation against the source standard (source-text extraction)), and shake the test tubes vigorously.
  • 9.9 Remove each test tube (the original text is incomplete, requires confirmation against the source standard (source-text extraction))

8. Analysis procedure

• 10.1 Heat the sample and sample mixtures in the test tubes in a constant-temperature oven to 46°C±2°C (the original text says "461*21", suspected to be 46°C±2°C, requires confirmation against the source standard (source-text extraction)).
• 10.2 Remove the sample and sample mixtures from the oven and cool to room temperature.
• 10.3 Record the separation condition of the sample and each sample mixture (i.e., phase separation position, color and particle size) and appearance in Table 1.
• 10.4 Pour point determination: except as specified in Note 10.4.7, the test procedure for this pour point determination shall be carried out in accordance with the provisions of GB/T 3535.
  • 10.4.1 Place a ring-shaped gasket below the oil surface in each test tube.
  • 10.4.2 Place a calibrated thermometer on the sealing stopper of each test tube. Ensure that the temperature-sensing bulb of the thermometer is immersed and the beginning of the capillary is below the oil surface by 3mm.
  • 10.4.3 Place a calibrated thermometer in the cooling chamber and maintain the temperature between -18°C~-15°C.
  • 10.4.4 Place the test tube in the sleeve of the cooling chamber.
  • 10.4.5 The pour point is expressed as a positive or negative integer multiple of 3. Start observing the temperature of each sample and sample mixture from above the expected pour point temperature 12°C (estimated in multiples of 3). Carefully remove the test tube from the sleeve, tilt the test tube, just enough to observe whether the sample in the test tube flows.
  • 10.4.6 If the sample and sample mixture in the test tube are flowing, immediately return it to the sleeve (the total operation time from removing the test tube to returning it to the sleeve is required not to exceed 3s).
  • 10.4.7 If the sample and sample mixture in the tilted test tube cannot flow, keep the test tube horizontal for 5s and record the time with a timer. If the sample and sample mixture show any movement at this time, return the test tube to the sleeve of the cooling chamber. If the sample and sample mixture show no movement, record the test temperature of the test tube at this time on the record paper as the "pour point" (the original text here source-text extraction is incomplete, requires confirmation against the source standard (source-text extraction)) in units of °C. Then place the test tube on the test rack to thaw. Note: GB/T 3535 requires adding 3°C to the measured temperature as the test result and reporting it; this standard requires reporting the actual observed temperature.
  • 10.4.8 If the sample and sample mixture still flow when reaching -6°C, place the test tube and sleeve into the second cooling chamber and maintain the temperature at (the original text source-text extraction is missing, requires confirmation against the source standard (source-text extraction)).
  • 10.4.9 For the test sample and test sample mixtures, continue performing the steps from 10.4.5 to 10.4.7 at intervals of every 3°C.
  • 10.4.10 If the test sample and test sample mixtures are still flowing upon reaching -24°C, place the test tube and jacket in the third cooling chamber, maintaining the temperature at -52°C~-49°C.
  • 10.4.11 For each test sample and test sample mixture, continue performing the steps from 10.4.5 to 10.4.7 at intervals of every 3°C. For tests to determine ultra-high pour point and ultra-low pour point, the temperature difference between additional cooling chambers is 17°C. When the temperature of each test sample and test sample mixture is below that of the cooling chamber (original text source-text extraction noise, requires confirmation against the source standard (source-text extraction)), transfer the test tube to the appropriate cooling chamber.
  • 10.4.12 Wait for the test sample and test sample mixtures to thaw.
  • 10.4.13 When the test sample and test sample mixtures become transparent and the turbidity disappears, observe the separation phenomena (i.e., phase separation position, color, and particle size) and appearance, and record the results on the record sheet at "just warmed above the cloud point temperature" (see Table 1).
• 10.5 Heat the test sample and test sample mixtures:
  • 10.5.1 Wait for the test sample and test sample mixtures to warm to room temperature.
  • 10.5.2 Remove the thermometer and stopper from the test tube.
  • 10.5.3 Remove the ring gasket from the test tube.
  • 10.5.4 Place all test samples and test sample mixtures in a suitable oven, set its temperature so that the temperature of the test samples and test sample mixtures reaches 232°C±2°C within 90min.
  • 10.5.5 When the temperature of the test sample and test sample mixtures reaches 232°C±2°C, heating should be stopped immediately, removed from the oven, and cooled to room temperature.
• 10.6 Store the test sample and test sample mixtures at the pour point temperature:
  • 10.6.1 Place the test sample and six test sample mixtures in a suitable cooling chamber, maintained at the pour point temperature of the test sample, and store for 18h~24h.
  • 10.6.2 After storage is completed, remove the test sample and test sample mixtures from the cooling chamber and allow them to warm naturally.
  • 10.6.3 When the test sample and test sample mixtures become transparent and the turbidity disappears, observe the test sample and record the results on the report form at "heated to 232°C—, stored at pour point temperature—18h— warmed above pour point temperature" (see Table 1).
  • 10.6.4 Warm the test sample and test sample mixtures to room temperature.
  • 10.6.5 Observe the test sample and test sample mixtures and record the results on the report form at "warmed to room temperature" (see Table 1).
  • 10.6.6 Dispose of the test sample and test sample mixtures as required.

9. Qualitative and Quantitative and Calculation Formulas

• This method is a qualitative/semi-quantitative visual observation method, with no calculation formulas.
• Results are recorded in Table 1 test report form, and the recorded items include: separation phenomena, phase separation position, color, particle size, and test sample appearance.
• Table 1 judgment codes:
  • Separation phenomena: D: clear boundary; N: no clear boundary
  • Color: w: white or very light; y: yellow; b: black
  • Test sample appearance: d: too dark to transmit light; m: dark but transparent; l: light color
  • Phase separation position: T: near the top; B: near the bottom; F: fine line in the interface; U: uniformly distributed
  • Particle size: s: when at cloud point or mist-like, very small; Sp: spots or large particles; sw: no particles
• Table 1 recording stages: before treatment, cooled to pour point (°C), just warmed above cloud point temperature, heated to 232°C— stored at pour point temperature—18h— warmed above pour point temperature, warmed to room temperature.
• Table 1 test sample numbers: test sample, test sample + HMA (A), test sample + HMB (B), test sample + HMC (C), test sample + HMD (D), test sample + HME (E), test sample + HMF (F).

10. Precision

• 12 Precision and bias: Since the results of this test are non-quantitative, this test method cannot provide data on precision and bias.

11. Report

• 11 Report: Report the results of homogeneity and miscibility in the form of Table 1.
• Table 1 test report form includes: sample number, test sample number, date, thermometer number, and observation results at each stage.

12. Referenced Documents

• GB/T 514 Technical conditions for glass liquid thermometers for petroleum product testing
• GB/T 3535 Determination of pour point of petroleum products (GB/T 3535—2006, mod ISO 3016:1994)
• GB/T 4756 Manual sampling of petroleum liquids (GB/T 4756—1998, eqv ISO 3170:1988)
• SH/T 0512 Evaluation method for low-temperature rusting of gasoline engine oils (MS Procedure ID method)
• SH/T 0763 Evaluation method for rust prevention of gasoline engine oils (BRT method)
• Note: In the original text 2 normative reference documents, "CB/T 3535" is suspected to be "GB/T 3535", and "CB/T 514" is suspected to be "GB/T 514", requires confirmation against the source standard (source-text extraction).

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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