SH/T 0191-1992 Determination of Demulsibility of Lubricating Oils

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 0191-92 (confirmed in 2000)
• Chinese title: Determination of Demulsibility of Lubricating Oils
• English title: not provided in the available source (the main text does not give an English title)
• Replacement relationship: replaces zB E34([unreadable character])-87 (original text as such, source-text extraction doubtful point: requires confirmation against the source standard (source-text extraction))
• Adoption relationship: identically adopts British Standard BS 2000 part 19:1982 "Demulsibility of Lubricating Oils"
• Technical committee: Technical committee of the Research Institute of Petroleum Processing
• Drafting organization: Research Institute of Petroleum Processing is responsible for drafting
• Main drafter: Hou Shulan
• Approval/implementation: approved by China Petrochemical Corporation 1992-05-20, implemented on 1992-05-20

2. Scope of application and non-applicability

• Applicable to turbine oils and other lubricating oils.
• Used turbine oils may also be used, but due to oil aging and contamination, the precision is lower than specified.
• Note: Oils containing antioxidants may give higher results than corresponding oils without antioxidants, and their precision may also be unsatisfactory.
• Non-applicable scope: not provided in the available source.

3. Method principle

20mL The sample is emulsified with steam at a temperature of about 90℃, then the emulsion is placed in a bath at about 94℃, and the time required to separate 20mL oil is measured.

4. Reagents and materials (purity / preparation)

• Solvent oil: for washing (purity and preparation not provided in the available source).
• Distilled water: for washing and the steam generator (5.3).
• Boiling stones or glass capillaries: added to the steam generator (5.3).
• Chromic acid cleaning solution: for cleaning the apparatus (5.2).

5. Apparatus and equipment

• 4.1.1 Steam generator: made of metal or glass; metal ones should be equipped with a water level gauge; glass ones may use a short-neck, wide-mouth flask with a capacity of not less than 1000mL.
• 4.1.2 Separation bath and emulsification bath: made of glass, or 3000mL beakers may be used; equipped with wooden or metal covers that can vertically fix the oil container and thermometer in the bath.
• 4.1.3 Heat source: blowtorch or electric hot plate or other heating method.
• 4.1.4 Oil container: a test tube with length 200mm, inner diameter 23mm, wall thickness 0.8～1.4mm; marked with lines every 1mL between 10～50mL, with a line around the test tube every 5mL, and the distance between the 10～50mL lines is 98mm±5mm (the original text "t 5mm" is suspected to be ±5mm, requires confirmation against the source standard (source-text extraction)).
• 4.1.5 Thermometer: for the oil container, see Appendix A; for the emulsification bath and separation bath, use a thermometer with a range of 0～100℃ and a scale division of 1℃.
• 4.1.6 Steam conduit and steam tube: see figure (figure omitted in the original text).
• Composition of the demulsibility tester (figure caption): 1— thermometer (0～100℃); 2— wooden or metal cover; 3— auxiliary steam line; 4— screw clamp; 5— rubber tube; 6,8— steam conduit; 7— thermometer (-1～105℃); 9— oil container; 10— emulsification bath; 11— steam generator, minimum capacity 1L; 12— separation bath; 13— detail of the end of the steam conduit.

6. Recommended operating conditions

• Emulsification bath water temperature: 19～26℃ (original text "19 - - 26cC", requires confirmation against the source standard (source-text extraction)).
• Separation bath water temperature: 93～95℃.
• Sample amount: 20mL.
• After steam is introduced, the oil temperature rises to 88～91℃ (original text "88[unreadable separator]9130", suspected to be 88～91℃, requires confirmation against the source standard (source-text extraction)), generally requiring 45～75s.
• With continuous steam introduction, within 4～6.5min the volume of condensed water and oil in the oil container should reach 40mL±3mL (the volume of the steam conduit and thermometer should be deducted, about 12～15mL).
• If the time is less than 4min, it may be because the steam flow rate is too fast, or water in the steam conduit has not been completely blown out by the steam; this test should be discarded.
• Separation bath temperature: 93～95℃.
• Recording interval: record the volume of separated oil layer once every 30s.

7. Sampling and sample preparation

• 5.1 The sample should avoid contamination, and care should be taken to avoid light.
• 5.2 Wash all apparatus that contacts the sample, such as the oil container and steam conduit, sequentially with solvent oil, chromic acid cleaning solution, and tap water, then wash with distilled water and dry.
• 5.3 Add distilled water to half the capacity of the steam generator, and put in several boiling stones or glass capillaries. Add 3000mL±50mL water to each of the emulsification bath and separation bath (original text "3000n[unreadable characters]ML", requires confirmation against the source standard (source-text extraction)). Install the apparatus as shown in the figure.
• 5.4 Boil the water in the steam generator, keep the water temperature of the emulsification bath at 19～26℃, and raise the water temperature of the separation bath to 93～95℃.

8. Analysis procedure

• 6.1 Pour 20mL of sample into the oil container, cover the oil container with a cork stopper having two holes, insert a thermometer through one hole, adjust the bottom of the thermometer mercury bulb to a distance of 20～25mm from the bottom of the test tube, and place it in the rack of the emulsification bath.
• 6.2 Pass steam through the steam conduit until the condensate disappears. Quickly insert the steam conduit into the oil container so that the tip of the tube touches the center of the bottom of the oil container (the fit between the steam conduit and the cork stopper should not be too tight). Control the temperature by adjusting the screw clamp on the steam conduit and the steam outlet. The steam flow rate should cause the oil temperature in the oil container to rise to 88～91℃, generally requiring 45～75s. Throughout the test, sufficient steam should be discharged from the steam outlet of the steam generator. With continuous steam introduction, within 4～6.5min the volume of condensed water and oil in the oil container should reach 40mL±3mL (the volume of the steam conduit and thermometer should be deducted, about 12～15mL). If the time is less than 4min, it may be caused by the steam flow rate being too fast, or water in the steam conduit not being completely blown out by the steam; this test should be discarded.
• 6.3 Remove the steam conduit from the rubber tube, and immediately start the stopwatch, quickly transfer the oil container to the separation bath at 93～95℃, and remove the thermometer and steam conduit from the oil container. Record the volume of separated oil layer once every 30s. If the interface between the oil layer and the emulsion is not a clear, straight horizontal line, treat any lacy emulsion layer as part of the water layer. The position of this line should be read to 0.5mL, and record the time required to separate 20mL oil (s). If no 20mL oil has separated within 20min, stop the test and record the volume of separated oil layer.
• Note: During observation, do not take the oil container out of the separation bath.

9. Qualitative and quantitative determination and calculation formula

• Definition: Demulsibility value—the time required for an oil to separate from an emulsion after being emulsified with steam under specified conditions, expressed in seconds (s)).
• The result is expressed as the time required to separate 20mL oil (s)).
• Calculation: calculate the average of two determination results (8.1).
• Reporting: report the average value, rounded to 15s (original text "rounded to 15s", requires confirmation against the source standard (source-text extraction)), as the determination result. If no 20mL oil has separated within 20min, report greater than 1200s.
• Formula: not provided in the available source.

10. Precision

Judge the reliability of test results according to the following provisions (95% confidence level). For unused oil, the difference between two determination results should not exceed the following values:

• Repeatability: 30s or 20% of the average (whichever is greater)
• Reproducibility: 60s or 30% of the average (whichever is greater)
• 8.1 Calculate the average of two determination results. If the difference between the two results and their average is greater than 15s, or greater than 10% of the average (if this value is greater), conduct a third test.

11. Report

• 8.1 Calculate the average of two determination results. If the difference between the two results and their average is greater than 15s, or greater than 10% of the average (if this value is greater), conduct a third test.
• 8.2 Report the average value, rounded to 15s, as the determination result. If no 20mL oil has separated within 20min, report greater than 1200s.

12. Referenced documents

• Appendix A Technical specifications for thermometer used in oil container (supplementary document).
• Adopted standard: BS 2000 part 19:1982 "Demulsibility of Lubricating Oils".
• Other 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 Q&A