SH/T 0215-1999 Determination of precipitation value and abrasiveness of rust-preventive oils and greases

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Card type: Test method

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

• Standard number: SH/T 0215-1999
• Chinese title: Determination of precipitation value and abrasiveness of rust-preventive oils and greases
• English title: Rust preventive oils and grease — Determination of precipitation number and wearability
• Replacement relationship: replaces SH/T 0215-1992 (the source text writes “replaces SrvT 0215-1992”, requires confirmation against the source standard (source-text extraction))
• Adoption relationship: equivalent adoption of the “precipitation value test method” in clause 5.10 and the “abrasiveness test method” in clause 5.24 of Japanese Industrial Standard JIS K2246-1994 Rust Preventive Oil
• First issued: 1992 year 5 month
• Approval/implementation: approved by the State Bureau of Petroleum and Chemical Industry 1999-12-08, implemented on 2000-05-01

2. Scope of application and non-applicability

• This standard specifies the method for determining the volume of sediment in rust-preventive oils and greases by centrifugal separation and whether the sediment scratches a glass surface.
• This standard applies to rust-preventive oils and rust-preventive greases.
• Not applicable: not provided in the available source.

3. Method principle

• After diluting a certain amount of sample with solvent, the sediment is separated under specified conditions, and the precipitation value of the rust-preventive oil or grease is expressed by the volume of the sediment (mL).
• The obtained sediment is placed between two microscope glass slides, and after rubbing, the scratching condition of the slides is inspected to determine the abrasiveness of the sample.

4. Reagents and materials (purity / preparation)

• 5.1 Precipitation naphtha: specifications are given in Table 4.
  • Density (15℃), g/cm³: 0.692～0.702; test methods GB/T 1884, GB/T 1885
  • Aniline point, ℃: 58～unclear in the source text (requires confirmation against the source standard (source-text extraction), suspected to be 58～?); test method GB/T 262 (the source text writes “GBmonth 262”, requires confirmation against the source standard (source-text extraction))
  • Distillation range: initial boiling point, ℃ not lower than 50; 50% distillation temperature, ℃ 70～80; dry point, ℃ not higher than 130; test method GB/T 6536
• 5.2 Industrial white oil: grade 10 premium white oil conforming to the provisions of SH 0006.
• 5.3 Toluene: analytical reagent.
• 5.4 95% ethanol: analytical reagent.
• Other materials: lens cleaning paper (4.7).

5. Apparatus and equipment

• 4.1 Centrifuge tube: shape and dimensions are shown in Figure 1 and Figure 2. The scale is 100 mL, and it is equipped with a suitable cork stopper. The centrifuge tube scale is calibrated with distilled water at 20℃, and the allowable error is given in Table 1 and Table 2.
• 4.2 Centrifuge: should meet all safety requirements for normal use. It can hold an even number of two or more test tubes, and during rotation the relative centrifugal force at the tip of the graduated test tube should be 600～700. The rotating head and trunnion cups (including rubber pads) should have a good structure and be able to withstand the maximum centrifugal force. During centrifugation, the trunnion cups and rubber pads should firmly support the centrifuge tubes. The rotational speed of the centrifuge head n (r/min) is calculated according to formula (1):
  • n = 1335 √(ref/d) ……(1)
  • Where: ref—— relative centrifugal force; d—— distance between the tips of two opposite test tubes in the rotating state (rotation diameter), mm.
  • Table 3 gives the relationship among rotation diameter, relative centrifugal force, and revolutions per minute.
• 4.3 Constant-temperature water bath: temperature can be controlled at 32～35℃ and 80℃±2℃ (the water-bath temperatures and tolerance are garbled in the source transcription and require verification).
• 4.4 Balance: sensitivity 0.1 g.
• 4.5 Microscope glass slide: 75 mm × 25 mm × 1.2 mm, inspected and free of scratches.
• 4.6 Pipette: 1 mL.
• 4.7 Lens cleaning paper.

6. Recommended operating conditions

• Centrifugation: relative centrifugal force at the tip of the centrifuge tube 600～700, centrifuge 10 min.
• Water bath temperature: after dilution of rust-preventive oil, let stand at 32～35℃; dissolution and standing of rust-preventive grease at 80℃±2℃.
• Drying: naturally dry under 23℃±3℃ (the source text “23'C 3 3℃”, requires confirmation against the source standard (source-text extraction)) for 10 min.
• Rubbing: slide left and right to rub 10 times.
• Other conditions are given in Section 8.

7. Sampling and sample preparation

• Rust-preventive oil: add 10 mL sample (at room temperature) to each of two clean, dry test tubes.
• Rust-preventive grease: weigh 5 g sample in each of two beakers, accurate to ±0.1 g, then add white oil to each of the two beakers (the white-oil addition instruction is garbled in the source transcription and requires verification), dissolve the sample at 80℃±2℃, pour the solution into two centrifuge tubes, and add white oil to 100 mL.
• Other sampling requirements: not provided in the available source.

8. Analytical procedure

8.1 Determination of precipitation value

8.1.1 Rust-preventive oil

• 6.1.1.1 When the estimated precipitation value is above 0.05 mL, both type I and type II centrifuge tubes may be used; when below 0.05 mL, use type II centrifuge tubes (the source text “1 9type” and “I Rtype”, requires confirmation against the source standard (source-text extraction)).
• 6.1.1.2 Add 10 mL sample (at room temperature) to each of two clean, dry test tubes, dilute with precipitation naphtha to 100 mL, and close tightly with a cork stopper. Shake vigorously 20 times to fully mix the sample and naphtha, then place the centrifuge tubes in a water bath at 32～35℃ and let stand for 5 min. Slightly open the cork stopper to reduce the pressure inside the centrifuge tubes, then close the cork stopper tightly and shake vigorously 20 times or more to mix completely and uniformly.
  • Note: To check whether the sample and naphtha are uniformly mixed, invert the centrifuge tube; if no sample remains at the tip of the centrifuge tube, the mixture is considered uniform.
• 6.1.1.3 Place the two centrifuge tubes containing the uniformly mixed sample symmetrically and evenly into the trunnions (the mass difference between the two sides should not exceed 0.5 g), and centrifuge for 10 min at a speed giving a relative centrifugal force at the tip of the centrifuge tube of 600～700, then read.
• 6.1.1.4 Repeat the operation of 6.1.1.3 three times until the volume of sediment in the centrifuge tubes reads a constant value for three consecutive times. If the volume of sediment is less than 0.005 mL, observe whether there is black sediment or fibrous material at the bottom of the centrifuge tube and record it.

8.1.2 Rust-preventive grease

• 6.1.2.1 Weigh 5 g sample in each of two beakers, accurate to ±0.1 g, then add white oil to each of the two beakers, dissolve the sample at 80℃±2℃, pour the solution into two centrifuge tubes, and add white oil to 100 mL.
• 6.1.2.2 Place the above centrifuge tubes containing the sample in a water bath at 80℃±2℃ and keep for 16 h; after removal, immediately read the sediment volume. That is, in this case centrifugal separation is not required.

8.2 Determination of abrasiveness

• 7.1.1 For the sample after completion of Chapter 6, immediately pour off the upper liquid, leaving several milliliters at the bottom, then add toluene to 100 mL, and place on the centrifuge at a speed giving a relative centrifugal force at the tip of the centrifuge tube of 600～700, and centrifuge for 10 min.
• 7.1.2 For the sample after completion of the centrifugal separation in 7.1.1, pour off the upper liquid, leaving about 1 mL at the bottom, use a pipette to take several drops of the residue and place them on a new glass slide that has been washed with 95% ethanol and wiped dry with lens cleaning paper, and naturally dry under 23℃±3℃ for 10 min.
• 7.1.3 On the glass slide to which the residue has adhered, cover with a new clean glass slide, press tightly with fingers, and slide left and right to rub 10 times. Visually inspect whether the glass slides are scratched after rubbing.

9. Qualitative and quantitative determination and calculation formulas

• Expression of precipitation value results:
  • 6.2.1 When the difference in sediment volume between the two centrifuge tubes is less than 0.1 mL, if the average value is less than 0.05 mL, the result is accurate to 0.01 mL; if the average value is between 0.05～0.5 mL, the result is accurate to 0.05 mL; if the average value is greater than 0.5 mL, the result is accurate to 0.1 mL.
  • 6.2.2 When the difference in sediment volume between the two centrifuge tubes is greater than 0.1 mL, repeat the test with another two centrifuge tubes, take the average value of the four centrifuge tubes as the reading, and report the result as described in 6.2.1.
  • 6.2.3 When the sediment volume is below 0.005 mL, visually inspect the bottom of the centrifuge tube for black sediment or fibrous material and record it.
• Expression of abrasiveness results:
  • 7.2 If the glass slide is scratched, it is judged as scratched; if not scratched, it is judged as not scratched.
• Formula for calculating centrifuge speed: n = 1335 √(ref/d) ……(1), for the meanings of symbols see Section 5.

10. Precision

• Judge the reliability of the precipitation value test results according to the following provisions (confidence level of 95%); this precision applies to rust-preventive oil samples whose test results are between 0.05～1.20 mL.
• 6.3.1 Repeatability: in the same laboratory, by the same operator using the same test apparatus in a short continuous period, the difference between two test results obtained from the same sample should not exceed the value specified in Table 5.
• 6.3.2 Reproducibility: In different laboratories, with different operators using different instruments, the difference between two test results obtained from a single test each on the same sample shall not exceed the value specified in Table 5.
• Table 5 Precision:
  • Sediment value: Repeatability, mL: take the larger value between 0.05 mL or 10% of the mean; Reproducibility, mL: take the larger value between 0.15 mL or 30% of the mean (original text: "take the larger value between 0.15.L or 3 0% of the mean", requires confirmation against the source standard (source-text extraction)).
• Abrasiveness precision: not provided in the available source.

11. Report

• Not provided in the available source (the main body of the standard does not have a separate "Report" section; for expression of results see Section 9).

12. Normative References

• GB/T 262 Determination of aniline point of petroleum products
• GB/T 1884 Determination of density of petroleum and liquid petroleum products (hydrometer method)
• GB/T 1885 Petroleum measurement tables
• GB/T 6536 Determination of distillation of petroleum products
• SH 0006 Industrial white oil
• Editor's note: The standard numbers and standard names of the referenced standards in this standard have changed as follows:
  • Original standard number GB/T 1894 → Current standard number GB/T 1884, current standard name: Determination of density of crude petroleum and liquid petroleum products in the laboratory (hydrometer method)

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 Q&A