SH/T 0557-1993 Standard Test Method for Viscosity of Petroleum Asphalt (Vacuum Capillary Method)

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Card type: Test method

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

• Standard number: SH/T 0557-93 (confirmed in 1998)
• Chinese title: Standard Test Method for Viscosity of Petroleum Asphalt (Vacuum Capillary Method)
• English title: not provided in the available source (the English title is not given in the main text)
• Supersession relationship: not provided in the available source
• Adoption relationship: This standard is identical to the American Society for Testing and Materials standard ASTM D2171-85 "Standard Test Method for Viscosity of Petroleum Asphalt Using a Vacuum Capillary Viscometer" (see additional notes)
• Approval/implementation: approved by China Petrochemical Corporation 1993-06-11, implemented on 1994-05-01

2. Applicable scope and non-applicability

• Applicable to the determination of the dynamic viscosity of petroleum asphalt when measured with a vacuum capillary viscometer at 60℃.
• May also be used to determine other substances with viscosity in the range of 0.0036～20.000 Pa·s.
• Also applicable when used at other temperatures, but the precision is based on the determination of the viscosity of asphalt at 60℃.
• Not applicable: not provided in the available source.

3. Method principle

Under strictly controlled vacuum and temperature, measure the time required for a certain volume of liquid to flow through a capillary. The viscosity of the liquid is expressed in units of Pa·s and is the flow time in seconds multiplied by the viscometer calibration coefficient.

As the liquid in the capillary rises, the shear rate decreases; using different vacuum levels or capillaries of different diameters also changes the shear rate. Therefore, this method is suitable for determining the viscosity of both Newtonian and non-Newtonian fluids.

4. Reagents and materials (purity / preparation)

• Standard viscosity sample: a standard viscosity sample with the approximate viscosity values listed in Table D1 (used for viscometer calibration).
• Cleaning solvents: toluene, petroleum ether, chromic acid cleaning solution, distilled water, residue-free acetone.
• For drying: clean dry air.
• Purity / specific preparation: not provided in the available source.

Table D1 Viscosity standard samples (excerpt from the source text)

Note: In Table D1, the 20℃ value of N190000 and the content of the third row source-text extraction have obvious noise and require confirmation against the source standard (source-text extraction).

5. Apparatus and equipment

• 3.1 Viscometer: the viscometer selected by this standard is detailed in Annex A; two viscometers recommended as equivalent for use are detailed in Annexes B and C; detailed rules regarding viscometer standards are given in Annex D.
• 3.2 Thermometer: a calibrated precision standard thermometer with a scale division of 0.02℃ or other temperature-measuring equipment with the same accuracy may be used. Thermometer specifications are given in Annex E.
• 3.3 Water bath: should be suitable for immersing the viscometer, at least so that the uppermost timing mark scale of the viscometer is immersed at least 20 mm below the water bath liquid surface, and convenient for observing the viscometer and thermometer. The viscometer should have firm support. A balance between heat input and heat loss should be ensured, and the water bath should be thoroughly stirred. The temperature difference of the medium in the water bath throughout the entire height of the viscometer or between viscometers at different positions shall not exceed 0.03℃.
• 3.4 Vacuum system: should be able to maintain the vacuum within the range of 39996 Pa±67 Pa (300 mmHg±0.5 mmHg). The basic components of the system are shown in Figure 1. The vacuum system line should use glass tubing with an inner diameter of 6.35 mm, and the glass joints used should be sealed and leak-free. When the system is closed, the vacuum indicated by the open mercury differential manometer (scale 1 mm) should not decrease. The vacuum source may be a suitable vacuum pump or suction pump.
• 3.5 Timer: a stopwatch or other timing device with a scale of 0.1 s (or smaller), an error within 0.05%, and a total timing range of not less than 15 min may be used.

Figure 1 Basic components of the vacuum system: 1— open mercury differential manometer; 2— regulating valve or stopcock valve; 3—1 liter buffer tank; 4— pressure stabilizer.

6. Recommended operating conditions

• Test temperature: 60℃ (precision is based on the viscosity of asphalt at 60℃); the water bath temperature is maintained within the range of the test temperature ±0.03℃.
• Vacuum: 39996 Pa±67 Pa (300 mmHg±0.5 mmHg).
• Flow time: select a flow time greater than 60 s; report the first flow time between the two timing mark scales that exceeds 60 s.
• Viscometer preheating temperature: 135℃±5℃.
• Time for the viscometer to remain in the water bath: 30 min±5 min.
• Other temperature conditions: not provided in the available source.

7. Sampling and sample preparation

4.1 Carefully heat the sample and stir continuously to ensure the sample is heated evenly and to prevent local overheating.

4.2 Transfer at least 20 mL of sample into a suitable container, heat to 135℃±5℃ (requires confirmation against the source standard, source-text extraction the source text reads "135`2 1 592"), stir occasionally to prevent local overheating, and stir carefully and slowly to prevent air from entering.

8. Analytical procedure

5.1 Maintain the water bath temperature within the range of the test temperature ±0.03℃, and make necessary corrections to all thermometer readings.

5.2 Select a clean, well-dried viscometer with a flow time greater than 60 s, and preheat to 135℃±5℃.

5.3 Fill the viscometer with the prepared sample to the height of the filling line E±2 mm (see Figure 2).

5.4 Place the viscometer filled with sample into an oven or oil bath at 135℃±5℃, and keep it at 10 min±2 min to expel large bubbles.

5.5 Remove the viscometer from the oven or oil bath, and within 5 min clamp the viscometer on a rack and place it vertically into the water bath so that the uppermost timing mark scale is at least 20 mm below the water bath liquid surface.

5.6 Establish a vacuum system of 39996 Pa±67 Pa (300 mmHg±0.5 mmHg), and connect the vacuum system to the viscometer using the regulating valve or stopcock valve installed on the viscometer line.

5.7 After the viscometer has been placed in the water bath for 30 min±5 min, open the regulating valve or stopcock valve on the line leading to the vacuum system so that the asphalt flows into the capillary.

5.8 Measure the time required for the leading edge of the meniscus to pass the two timing mark scales, to the nearest 0.1 s, report the first flow time between the two timing mark scales that exceeds 60 s, and note the numbers of this pair of timing mark scales.

5.9 After the test is completed, remove the viscometer from the water bath and place it upside down in an oven at 135℃±5℃ until the asphalt flows out of the viscometer. Thoroughly clean the viscometer with toluene, then rinse with petroleum ether. Pass a small flow of clean dry air through the capillary (for about 2 min or until the solvent has completely evaporated) to dry the tube. Periodically clean the viscometer with chromic acid cleaning solution to thoroughly remove organic deposits. Rinse with distilled water and residue-free acetone and blow dry with clean air.

Figure 2 Viscometer selected by this standard: 1— filling line E; 2— first timing mark F; 3—B section; 4— second timing mark G; 5—C section; 6— third timing mark H; 7—D section; 8— fourth timing mark I; 9— filling tube A; 10—24/40 ground joint; 11— vacuum tube M.

9. Qualitative and quantitative determination and calculation formula

Select the calibration coefficient corresponding to this pair of timing mark scales (e.g., 5.8), use the following formula to calculate and report the viscosity (Pa·s), retaining three significant figures:

P = k · t

Where:

• k—— the selected calibration coefficient, Pa·s/s;
• t—— flow time, s.

(The source formula source-text extraction is "P two ‘ "c"; based on the context and the formula form in Annex D, it is arranged as P = k·t, requires confirmation against the source standard (source-text extraction).)

Annex D Calibration formula:

D3.7 The capillary calibration coefficient is calculated according to formula (D1):

k = P₁ / t

Where:

• P₁——the viscosity of the standard sample at the calibration temperature, Pa·s;
• t—— flow time, s;
• k—— the calibration coefficient of the viscometer at a vacuum of 39996 Pa±67 Pa (300 mmHg±0.5 mmHg), Pa·s/s.

D4.3 The calibration coefficient k₁ is calculated according to formula (D2):

k₁ = (t₂ · k₂) / t₁

Where:

• k₁——the calibration coefficient of the viscometer being calibrated;
• t₁——the flow time of the viscometer being calibrated, s;
• k₂——the capillary coefficient of the standard viscometer;
• t₂——the corresponding flow time of the standard viscometer, s.

10. Precision

• 8.1 Repeatability: for the same operator using the same instrument, the difference between two repeated determination results shall not exceed 7% of their average value.
• 8.2 Reproducibility: for results provided by two laboratories, the error shall not exceed 10% of their average value.

11. Report

When reporting the viscosity test results, the test temperature and vacuum shall also be stated. For example: viscosity [60℃, 39996 Pa±67 Pa, Pa·s] (the source example source-text extraction is "viscosity [printed ℃, 39996Pa±67Pa, Pa- s five 60t (300manHg, poise)]", requires confirmation against the source standard (source-text extraction)).

12. Reference Documents

• ASTM D2171-85 "Determination of Viscosity of Petroleum Asphalt with Vacuum Capillary Viscometer" (identical adoption, see additional notes)
• Appendix A: Viscometer specifications selected by this standard (supplementary element)
• Appendix B: Recommended viscometer specifications for identical use (1) (supplementary element)
• Appendix C: Recommended viscometer specifications for identical use (2) (supplementary element)
• Appendix D: Calibration of viscometer (supplementary element)
• Appendix E: Thermometer specifications (supplementary element)

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