GB/T 4509-2010 Determination of Penetration of Bitumen

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Card type: Test method

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

• Standard number: GB/T 4509—2010
• Chinese title: Determination of Penetration of Bitumen
• English title: Standard test method for penetration of bitumen
• Replacement relationship: replaces GB/T 4509—1998; previous versions are GB/T 4509—1984, GB/T 4509—1998
• Adoption relationship: modified adoption of ASTM D5:2006 "Determination of Penetration of Bitumen" (English version), redrafted according to ASTM D5:2006
• Publication/implementation: published on 2011-01-10, implemented on 2011-05-01
• Proposal/administration: proposed by the National Technical Committee for Standardization of Petroleum Products and Lubricants; administered by the Subcommittee on Petroleum Asphalt of the National Technical Committee for Standardization of Petroleum Products and Lubricants
• Drafting organization: Heavy Oil Research Institute, China University of Petroleum (East China)
• Main drafters: Zhang Xiaoying, Gao Qilin

2. Scope of application and non-applicability

• This standard specifies the standard needle, sample container and other test conditions for a penetration range of (0~500)1/10 mm.
• It is applicable to the determination of the penetration of solid and semi-solid bituminous materials with a penetration range from (0~500)1/10 mm.
• Note: For the preparation and testing of emulsified asphalt residue samples used in this method, reference may be made to test method SH/T 0099.4.
• Not applicable: no explicit non-applicability clause is provided in the available source.

3. Method principle

• The penetration of bitumen is expressed as the depth to which a standard needle vertically penetrates the bitumen sample under specified load, time and temperature conditions, in units of 1/10 mm.
• Unless otherwise specified, the total mass of the standard needle, needle holder and additional weight is (100±0.05)g, the temperature is (25±0.1)°C, and the time is 5 s.
• Other conditions that may be used for specific tests are shown in Table 1.

Table 1 Specific test conditions

Note: For specific tests, the test conditions shall be stated in the report.

4. Reagents and materials (purity / preparation)

• Water for water bath: distilled water is recommended; be careful not to contaminate the water with surfactants, release agents or other chemical reagents, as the presence of these substances will affect the measured penetration value.
• Low-temperature determination: it is recommended that when the penetration measurement temperature is less than or equal to 0°C, salt be used to adjust the freezing point of the water so as to meet the constant-temperature requirement of the water bath; when determining penetration at low temperature, salt water is placed in the water bath.
• Solvent: used to wipe the standard needle clean (the specific solvent name and purity are not provided in the available source).
• Other reagents: not provided in the available source.

5. Apparatus and equipment

5.1 Penetrometer

• Any instrument that can make the needle holder move vertically without obvious friction and can indicate the penetration depth to an accuracy of 0.1 mm may be used.
• Needle holder mass: (47.5±0.05)g.
• Total mass of needle and needle holder: (50±0.05)g.
• One weight each of (50±0.05)g and (100±0.05)g is provided, which can form loads of (100±0.05)g and (200±0.05)g (the load tolerance is unclear in the source transcription and remains unverified).
• The instrument is provided with a platform for placing a flat-bottomed glass dish and a mechanism for level adjustment; the needle holder shall be perpendicular to the platform.
• The instrument is provided with a needle holder release button; when the button is pressed firmly, the needle holder can fall freely.
• The needle holder shall be easy to disassemble so that its mass can be checked periodically.

5.2 Standard needle

• The 5.2.1 standard needle shall be made of hardened and tempered stainless steel, of steel grade 440-C or equivalent material, with a Rockwell hardness of 54~60 (see Figure 1).
• The needle length is about 50 mm, the long needle length is about 60 mm, and the diameter of all needles is 1.00 mm~1.02 mm.
• One end of the needle shall be ground into a cone of 8.7~9.7° (Figure 1 is marked 8°40′~9°40′).
• The cone shall be coaxial with the needle body, and the maximum axial deviation of the boundary line between the conical surface and the needle body surface shall not be greater than 0.2 mm.
• The diameter of the flat-cut conical end shall be between 0.14 mm~0.16 mm, and the angle formed with the needle axis shall not exceed 2°.
• The periphery of the flat-cut conical surface shall be sharp and free from burrs.
• The arithmetic mean roughness of the conical surface shall be 0.2 μm~0.3 μm (the original source-text extraction is "0.2pm~0.3pm", requires confirmation against the source standard (source-text extraction)).
• The needle shall be mounted in a brass or stainless steel ferrule; the ferrule diameter is (3.20±0.05)mm, the length is (38±1)mm, and the needle shall be firmly mounted in the ferrule.
• The needle tip and any other part of the needle shall not deviate from the ferrule axis by more than 1 mm.
• The total mass of the needle ferrule and its accessories is (2.50±0.05)g.
• Holes may be drilled in one end of the needle ferrule or its edge may be ground flat to control the mass.
• A separate identification number shall be stamped on each needle ferrule.
• 5.2.2 To ensure the uniformity of needles used for testing, the inspection results of the needles by the national metrology department shall meet the requirements of 5.2.1, and an inspection certificate from the national metrology department shall be attached to each needle.

5.3 Sample container

• A cylindrical flat-bottomed container made of metal or glass with minimum dimensions meeting the requirements of Table 2 shall be used.

Table 2 Sample container dimensions

(Note: In Table 2, the diameter in the "350~500" row is originally 55, and its correspondence with 55~75 in the "200~350" row is suspected to be misaligned by source-text extraction, requires confirmation against the source standard (source-text extraction).)

5.4 Constant-temperature water bath

• A water bath with a capacity of not less than 10 L and capable of maintaining the temperature within ±0.1°C of the test temperature.
• In the water bath, at a distance of 50 mm from the bottom of the water, there is a perforated support, and this support is at least 100 mm from the water surface.
• If the penetration determination is carried out in the water bath, the support shall be sufficient to support the penetrometer.
• When determining penetration at low temperature, salt water is placed in the water bath.

5.5 Flat-bottomed glass dish

• Capacity not less than 350 mL, and the depth shall cover the largest sample container.
• A stainless steel triangular support is provided inside to ensure the stability of the sample container.

5.6 Timer

• Any timing device with a scale of 0.1 s or less than 0.1 s, and an accuracy within 60 s of ±0.1 s may be used.
• Any timing device connected directly to the penetrometer shall be accurately calibrated to provide a time interval of ±0.1 s.

5.7 Thermometer

• Liquid-in-glass thermometer, meeting the following standards: scale range: -8°C~55°C, graduation value 0.1°C.
• Or any temperature-measuring device meeting this accuracy, precision and sensitivity may be used.
• The thermometer or temperature-measuring device shall be calibrated periodically according to the inspection method.

6. Recommended operating conditions

• Standard conditions: temperature (25±0.1)°C, load (100±0.05)g, time 5 s.
• Specific test conditions are shown in Table 1 (0°C/200 g/60 s; 46°C/50 g/60 s; 5°C/100 g/5 s, the last row requires confirmation against the source standard (source-text extraction)).
• For specific tests, the test conditions shall be stated in the report.

7. Sampling and sample preparation

6.1 Heating

• Heat the sample carefully with continuous stirring to prevent local overheating, and heat until the sample can flow easily.
• During heating, the heating temperature of tar asphalt shall not exceed 60°C of the softening point, and that of petroleum asphalt shall not exceed 90°C of the softening point.
• The heating time shall be as short as possible on the basis of ensuring sufficient flow of the sample.
• Avoid introducing air bubbles into the sample during heating and stirring.

6.2 Pouring

• Pour the sample into a pre-selected sample container; the sample depth shall be at least 120% of the expected penetration depth.
• If the diameter of the sample container is less than 65 mm and the expected penetration is higher than 200, three samples shall be poured for each test condition.
• If sufficient sample is available, the poured sample shall reach the edge of the sample container.

6.3 Cooling and constant-temperature conditioning

• Cover the sample container loosely to prevent dust from falling in.
• At room temperature of 15°C~30°C:
  • Samples in small sample containers (φ33 mm×16 mm) are cooled for 45 min~1.5 h;
  • Samples in medium sample containers (φ55 mm×35 mm) are cooled for 1 h~1.5 h;
  • Samples in larger sample containers are cooled for 1.5 h~2.0 h.
• After cooling is completed, place the sample container together with the flat-bottomed glass dish into a water bath at the test temperature; the water surface shall be at least 10 mm above the sample surface.
• Maintain constant temperature at the specified test temperature:
  • Small sample containers are held at constant temperature for 45 min~1.5 h;
  • Medium sample containers are held at constant temperature for 1 h~1.5 h;
  • Constant temperature of a larger sample container 1.5 h~2.0 h.

8. Analysis Procedure

• 7.1 Adjust the level of the penetrometer, check the needle link and guide rail to ensure there is no water or other substances on them. If the predicted penetration exceeds 350, a long needle should be selected; otherwise, use the standard needle. First wipe the needle clean with a suitable solvent, then dry it with a clean cloth, then insert the needle into the needle link and secure it. Select the appropriate weight according to the test conditions and place the weight properly.
• 7.2 If the penetrometer is in a water bath during the test, place the sample container directly on the support immersed in water so that the sample is completely immersed in water. If the penetrometer is not in a water bath during the experiment, place the sample container that has been brought to the test temperature on the triangular support in the flat-bottomed glass dish, completely cover the sample with water at the same temperature as the water bath, and place the flat-bottomed glass dish on the platform of the penetrometer. Slowly lower the needle link so that the needle tip just contacts the surface of the sample; if necessary, use a light source placed in a suitable position to observe the needle tip position until the needle tip just contacts the projection of the needle in the water. Gently pull down the release rod so that it contacts the top of the needle link, and adjust the dial reading on the penetrometer to zero or reset it to zero.
• 7.3 Quickly release the needle link within the specified time, and at the same time start the stopwatch or timing device, so that the standard needle falls freely and penetrates into the asphalt sample, and stop the movement of the standard needle at the specified time.
• 7.4 Pull down the release rod and bring it into contact with the top of the needle link again; at this time, the reading of the dial pointer is the penetration of the sample, or in automatic mode the cone penetration is stopped, and the cone penetration depth value is read directly through the data display device to obtain the penetration, expressed in 1/10 mm.
• 7.5 Repeat the measurement at least three times for the same sample. The distance between each test point and the distance between the test point and the edge of the sample container shall not be less than 10 mm. Before each test, the sample and the flat-bottomed glass dish shall be placed in a constant-temperature water bath, and a clean needle shall be used for each measurement. When the penetration is less than 200, the needle may be removed, wiped clean with a suitable solvent, and then continued to be used. When the penetration exceeds 200, one needle is inserted in each sample container, and three sample containers give three data. Alternatively, at least three needles are used for each sample, and the needle used in each test remains in the sample until all three needles have been inserted, and then the needles are removed from the sample. However, the difference between the highest value and the lowest value of the penetration measured in this way shall not exceed the provision in 9.1.

9. Qualitative and Quantitative and Calculation Formula

• 8.1 Report the average value of three penetration measurements, rounded to an integer, as the experimental result. The difference among the three penetration values shall not be greater than the value in Table 3.

Table 3 Maximum Difference of Three Penetration Measurements (Unit: 1/10 mm)

(Note: The original Table 3 source-text extraction is garbled in layout; the line “150~249 5420250~350350~500 6 8 20” needs to be split according to the above table, requires confirmation against the source standard (source-text extraction); in addition, the interval “20~49” is not provided in the available source.)

• 8.2 If the error exceeds this range, repeat the test using the second sample in 6.2.
• 8.3 If the result again exceeds the allowable value, cancel all test results and conduct the test again.
• Calculation formula: not provided in the available source (expressed as the average of three measurements rounded to an integer).

10. Precision

• 9.1 Repeatability: The difference between two results obtained by the same operator in the same laboratory using the same instrument on the same sample shall not exceed 4% of the average value.
• 9.2 Reproducibility: The difference between two results obtained by different operators in different laboratories using different instruments of the same type on the same sample shall not exceed 11% of the average value.
• 9.3 Because the test measurement value is defined by the test method, the data obtained by this test method has no bias.

11. Report

• Report the average value of three penetration measurements, rounded to an integer, as the experimental result (see 8.1).
• The difference among the three penetration values shall not be greater than the value in Table 3 (see 8.1).
• For specific tests, the test conditions shall be stated in the report (see the note to Table 1).
• Other reporting requirements: not provided in the available source.

12. Normative References

• GB/T 4507 Test Method for Softening Point of Asphalt
• SH/T 0099.4 Test Method for Evaporated Residue Content of Emulsified Asphalt
• Note: Chapter 2 of the original text is Normative References; ASTM D5:2006 is the original document modified and adopted (see Foreword).

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