SH/T 0018-2007 Standard Test Method for Apparent Viscosity of Petroleum Waxes Containing Additives (Hot Melt Adhesives)

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Card type: Test method

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

• Standard number: SH/T 0018-2007
• Chinese title: Standard Test Method for Apparent Viscosity of Petroleum Waxes Containing Additives (Hot Melt Adhesives)
• English title: Standard test method for apparent viscosity of petroleum waxes compounded with additives (hot melts)
• Replacement relationship: replaces SH/T 0018-1990; previous versions are SH/T 0018-1987, SH/T 0018-1990
• Adoption relationship: modified adoption of ASTM D2669-2006 (English version), redrafted according to ASTM D2669-2006
• Main differences from ASTM D2669-2006: referenced standards adopt corresponding Chinese standards; the appendix is removed, and the appendix "Relationship between measurement spindle number, viscosity, and maximum apparent viscosity" is incorporated into the main text; the conversion relationship between millipascal·second (mPa·s) and centipoise (cP) is removed
• Main changes compared with SH/T 0018-1990: safety-related explanations are added; significance and use, and bias clauses are added; the thermometer usage range is changed from 0℃~300℃ to 10℃~200℃; the hot melt formulation used in the precision test differs from the original standard
• Publication/implementation: published on 2007-08-01, implemented on 2008-01-01
• Responsible committee: Fushun Research Institute of Petroleum and Petrochemicals, China Petroleum & Chemical Corporation
• Drafting organization: Fushun Research Institute of Petroleum and Petrochemicals, China Petroleum & Chemical Corporation
• Main drafters: Luo Yadong, Gao Junxing

2. Scope of application and non-applicability

• Applicable to liquid hot melts (1.1) with an apparent viscosity lower than 20Pa·s at temperatures below 175℃.
• Note: For samples with low apparent viscosity (less than 15mPa·s), the method of GB/T 265 may be used (1.1 note).
• This standard specifies the International System of Units as the standard units of measurement (1.2).
• Safety precaution: This standard may involve certain hazardous materials, equipment, and operations, but it is not intended to address all safety issues associated with them; before use, users are responsible for establishing appropriate safety and protective measures and formulating applicable management systems (1.3).
• Non-applicability scope: no explicitly listed non-applicable clauses are provided in the available source.

3. Method principle

Heat and melt about 800g of the sample, pour it into a 800mL glass beaker, and heat it in an electric heating mantle so that the liquid level is about 25mm from the top of the beaker; place the viscometer with the measurement spindle and guard sleeve at the specified position in the sample. Begin heating and stirring; when the sample temperature rises to slightly above the test temperature, stop heating, continue stirring until the test temperature is reached, stop stirring, and measure the apparent viscosity. As the sample temperature decreases, perform multiple measurements within a certain temperature range; plot the measured values of temperature and apparent viscosity on semi-logarithmic coordinate paper, and the apparent viscosity at any temperature can be obtained from the curve (Chapter 4).

4. Reagents and materials (purity / preparation)

• Standard viscosity oil: used for viscometer calibration (7.2). Purity/specifications are not provided in the available source.
• Hot melt formulation for precision test (Table 2):
  • High-viscosity sample: 68 wax 58% (mass fraction), ethylene-vinyl acetate copolymer 42% (mass fraction) (ethylene acetate content is 27%~29%, melt index is 12-18)
  • Medium-viscosity sample: 60 wax 72% (mass fraction), ethylene-vinyl acetate copolymer 28% (mass fraction) (ethylene acetate content is 27%~29%)
  • Low-viscosity sample: microcrystalline wax with a melting point of 77℃ 96.3% (mass fraction), butyl rubber 2.7% (mass fraction)
  • Low-viscosity sample: 68 wax 80% (mass fraction), polyethylene 20% (mass fraction) (relative molecular mass is 5000, melting point is 107℃~111℃, relative density is 0.92, viscosity at 140℃ is 4Pa·s)
• Purity of other reagents and preparation methods: not provided in the available source.

5. Apparatus and equipment

• 6.1 Viscometer: Brookfield viscometer, equipped with graduated stainless steel spindles No. 1, 2, 3, 4, and equipped with a V type stand with leveling screws.
• 6.2 Glass beaker: 800mL.
• 6.3 Electric heating mantle: for heating the 800mL glass beaker.
• 6.4 Autotransformer: 1kVA.
• 6.5 Thermometer: 10℃~200℃, minimum division 1℃.
• 6.6 Variable-speed stirrer.
• 6.7 Stainless steel stirring rod: length 475mm, diameter 7.9mm, with three 51mm blades welded at one end (original text "5Imm" requires confirmation against the source standard (source-text extraction)).
• 6.8 Heating plate: with continuously adjustable temperature control device.
• 6.9 Scissor lift platform.
• 6.10 Ring stand and universal clamp: used to secure the stirrer and thermometer.
• 6.11 Semi-logarithmic coordinate paper: 2 revolutions (cycles).

6. Recommended operating conditions

• Viscometer installation: install the viscometer on the V type stand and adjust it to level (7.1).
• Viscometer calibration: use standard viscosity oil and, using the parameters in Table 1, select the appropriate spindle and speed to calibrate the viscometer (7.2).
• Spindle selection: according to the estimated sample viscosity, use Table 1 to select the appropriate spindle and speed, and install the measurement spindle and guard sleeve on the viscometer (7.3).
• Table 1 Relationship between measurement spindle number, speed, and maximum apparent viscosity (the original table source-text extraction is noisy; the following is the identifiable content, requires confirmation against the source standard (source-text extraction)):

Note: The original text of Table 1 source-text extraction has misalignment and noise (such as "maximum knot degree", "station large viscosity", "sensitive large viscous quality", etc.); the above correspondences require confirmation against the source standard (source-text extraction).

7. Sampling and sample preparation

• 7.4 Sample preparation: place a container with about 800g of sample on an electric heating plate to melt and stir evenly; be careful not to stir air bubbles into the molten sample; pour the molten sample into the 800mL beaker used for the test so that the liquid level is about 25mm from the top of the beaker.
• 7.5 Place the beaker containing the sample into the electric heating mantle on the lift platform; the electric heating mantle is connected to the transformer, and the transformer and viscometer are connected to the power supply; install the viscometer with the measurement spindle and guard sleeve, the stirrer, and the thermometer according to Figures A1.1 and A1.2; keep the mercury bulb of the thermometer at the same level as the middle of the measurement portion of the measurement spindle, and make its distance from the measurement spindle approximately equal to the distance between the measurement spindle and the guard sleeve (about 13mm); the stirring rod blades are positioned midway between the bottom of the guard sleeve and the bottom of the beaker; adjust the position of the entire assembly so that the measurement portion of the measurement spindle maintains a distance of about 19mm from the beaker wall. Use the lift platform to adjust the position of the beaker so that the spindle enters the sample and the liquid level is 6mm below the immersion line; begin stirring and adjust the stirring speed to the minimum, but such that no vortex or bubbles are generated.

8. Analytical procedure

• 7.6 Use the transformer to adjust the sample heating temperature so that its temperature rises to more than 5℃ above the test temperature; maintain stirring during heating, and be careful to prevent the sample from being carried out with air foam.
  • Note: As the temperature rises, the liquid level will reach the spindle immersion line due to expansion of the sample volume. Be careful to prevent the liquid level from exceeding the spindle immersion line; before measurement, make a display adjustment to the immersion line.
• 7.7 Viscosity measurement:
  • When the sample temperature is more than 5℃ above the test temperature, turn off the transformer, start the viscometer motor, and continue stirring; the sample temperature begins to decrease; when it is 0.5℃ above the test temperature, stop stirring, but the measurement spindle continues to rotate; after 5 seconds, adjust the viscometer to the spindle immersion line, then rotate the spindle one full turn; when the indicator pointer is seen, simultaneously turn off the indicator, clutch, and viscometer motor, and record the dial reading; restart the viscometer motor and clutch, rotate the spindle one full turn, and when the indicator pointer is seen, simultaneously turn off the indicator, clutch, and viscometer motor, and record the second reading; repeat the above steps, obtaining three readings within 1 minutes; during this period, the sample temperature decrease should not be less than 0.5℃. Record the three measured readings and the test temperature.
  • Immediately after obtaining the last reading, start the stirrer and the viscometer motor with clutch, allow the sample temperature to decrease by about 15℃, repeat the same test procedure at a lower temperature, and continue in this way to obtain readings at 4 or more different test temperatures, with each temperature interval about 15% lower than the previous test temperature.
  • Note: The test temperature range should include all temperatures at which the apparent viscosity needs to be determined. As the temperature decreases, the sample volume shrinks; therefore, to ensure the rotor is at the correct immersion position, the rotor needs to be adjusted up and down slightly.

9. Qualitative and Quantitative and Calculation Formula

• The apparent viscosity of the 8.1 sample at temperature t is calculated according to the following formula:
  • η_t = R · n
  • Where:
    • η_t —— apparent viscosity at temperature t, mPa·s;
    • R —— the average value of one reading measured at temperature t;
    • n —— coefficient given by the rotor number and rotational speed.
• 8.2 Plot the viscosity-temperature curve: on semi-logarithmic coordinate paper, plot the obtained apparent viscosity on the logarithmic scale coordinate, and plot the corresponding test temperature on the linear coordinate (plot the viscosity-temperature curve). From the curve graph, the apparent viscosity of the sample at any temperature within the test temperature range can be found.

10. Precision

• When determining different types of samples, the hot-melt components will affect precision; therefore, the following data (see Table 2) should be used to judge the reliability of the determination results of 4 different types of hot-melt materials (95% confidence level).
• 10.1 Repeatability: The difference between parallel determination results shall not be greater than the repeatability allowable error given in Table 2.
• 10.2 Reproducibility: The difference between reproducibility determination results shall not be greater than the reproducibility allowable error given in Table 2.
• Table 2 Precision table:

Note: In Table 2, "low-viscosity sample" corresponds to two samples with different formulations; the original table does not clearly distinguish row attribution, requires confirmation against the source standard (source-text extraction).

11. Report

• Use the average of the two determination results as the determination result, and also report the determination temperature, rotor number, and rotational speed, such as apparent viscosity: 325mPa·s, 120℃ (rotor number: 2; rotational speed: 30r/min) (Chapter 9).

12. Normative References

• GB/T 265 Petroleum products — Determination of kinematic viscosity and calculation of dynamic viscosity
• GB/T 514 Specification for liquid-in-glass thermometers for petroleum product testing
• Note: For undated reference documents, the latest version applies to this standard; for dated reference documents, all subsequent amendments (excluding corrigenda) or revisions do not apply to this standard (Chapter 2).

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