Softening Points: Methods and Applications in Resins and Bitumen

All About Softening Point

What Is Softening Point?

What Is Softening Point

The resins are noncrystalline amorphous materials that soften gradually over a range of temperatures. Therefore, the softening point is controlled by the average molecular weight of the resin.

The softening point is also related to the intrinsic viscosity, hardness, and brittleness of resins. The softening point is defined as the temperature at which the resin flows under a given load on heating. Several standard methods have been proposed to determine the softening point of resins.

List of Proposed to Determine the Softening Point

List of Proposed to Determine the Softening Point

  1. Ring and Ball Method (R&B)
  2. Kriimer—Sarnow Method
  3. Mettler Softening Point Method
  4. Plate—Plate Stress Rheonzeter Test

Ring and Ball Method (R&B)

Ring and Ball Method (R&B)

ASTM D 3461-76, DIN ISO 4625. This method is the most frequently used to determine the softening point of resins. Show above figure illustrates the experimental device used to determine the R&B softening point. The resin is melted into a metal ring and left to cool. The ring is placed in a special metallic device, which is placed into a water or glycerol bath.

A steel ball of given diameter and mass is placed on the ring and the bath is heated at a given rate. The temperature at which the ball forces the softening resin downward is noted as the softening point.

Kreimer-Sarnow Method

Kreimer-Sarnow Method

DIN 53 180. This is the oldest method used to determine the softening point of resins and is relatively similar to the R&B method. Instead of a ring, a small glass tube that is open at both ends is used and the load is a small mercury drop. The softening point is obtained as the temperature at which the mercury drop breaks through the softening resin and falls.

Mettler Softening Point Method

Mettler Softening Point Method

1. Heating element, 2. Platinum resistance thermometer, 3. Sample, 4. Light source, 5. Furnace, 6. Sample cup, 7. Photocell, 8. Collector sleeve. ASTM D 3461-76. This is the most recent method. This automatic method measures the temperature at which the resin flows out of a sample cup under its own weight.

The temperature is recorded when the first drop crosses the light path of a photocell (show in the figure). This method is quite accurate and reproducible.

Plate—Plate Stress Rheonzeter Test.

The resin is placed between the two steel plates of a stress-controlled rheometer, maintaining a gap larger than 0.5 cm. The upper plate is oscillated at a given frequency, whereas the lower plate is heated.

The variation of the storage and loss moduli as a function of the temperature is monitored. The softening temperature can be estimated from the temperature at the cross-over between the two moduli.

Ring-Ball Test for Softening Point of Bitumen

The closely defined method used for bitumen is described in BS 4692. In the ring-and-ball test, samples of bitumen are prepared by pouring the bitumen, which has been heated under specified conditions, into metal rings which serve as molds.

Preparation of the bitumen samples must be carried out in a controlled manner detailed in BS 4692. The determination is usually carried out in duplicate and the apparatus is designed to hold two discs.

Apparatus for Softening Point of Bitumen

Apparatus for Softening Point of Bitumen

Ring

A brass shouldered ring. (Show above figure)

Ball

A steel ball, 9.53 mm (3/8”) in diameter, weighing between 3.45 and 3.55 grams. ( Show above figure)

Ball Centering Guide

A guide for centering the ball and made of brass. (Show above figure)

Ring Holder

The rings shall be supported on a brass ring holder. (Show above figure)

Brass Pouring Plate

Brass Pouring Plate

  1. A flat, smooth brass plate approximately 75 by 50 mm has been treated to prevent the bituminous material from adhering to it.
  2. Suitable treatment is to coat the plate just before use with a thin layer of a mixture of glycerin and dextrin, talc, or china clay.

Bath

Glass Vessel

A glass vessel, capable of being heated, not less than 85 mm in diameter and not less than 120 mm in depth from the bottom of the flare.

Thermometer

Thermometer

Thermometer having a range from -2 to +80°C.

Procedure for Softening Point of Bitumen

Procedure for Softening Point of Bitumen

The determination is usually carried out in duplicate and the apparatus is designed to hold two discs.

The apparatus is assembled with the rings, the appropriate thermometer, and ball guides in position, and the bath is filled to a height of 50 mm above the upper surface of the rings, as shown above, figure, with freshly boiled distilled water at a temperature of 5 °C when the softening point is below 80 °C, the water temperature being maintained at 5 °C for 15 min.

Using forceps, a steel ball, previously cooled to 5 °C, having a diameter of 9.53 mm and weighing 3.50 ± 0.05 g, is placed upon each sample disc contained within a tapered brass ring with a larger internal diameter of 17.5 mm.

A ball guide previously placed over the disc assists in placing the ball in position. The bath is then heated and the water stirred so that the temperature rises at a uniform rate of 5 ± 0.5 °C/min until the bitumen softens and allows the ball to pass through the ring.

The rate of temperature rise should not be averaged over the test period and any determination where the rate does not fall within the specified limits after the first 3 min must be rejected.

For each ring and ball, the temperature shown by the thermometer is taken at the instant the sample surrounding the ball touches the bottom plate. If, however, the difference between the values obtained in the duplicate determinations exceeds 1 °C the test must be repeated.

When the softening point is expected to be above 80 °C the water is replaced with glycerol, which is maintained at a temperature of 35 °C for 15 min before placing a steel ball at the same temperature on to the disc.

Observations & Results for Softening Point of Bitumen

Sr.No. Softening Point
°C
Mean
°C
1 45.2 °C 45.1 °C
2 45.0 °C

Softening Point of Bitumen Lab Report

The experiment has been performed successfully and the softening point came out to be 45.1oC. Bitumen having this softening point should not be used in DDIT Nadiyad as the city’s highest maximum temperature was 40.3 °C recorded on March 30, 1990 And 46 °C was recorded on May 26, 2013.

At the time the meteorological office recorded this official temperature in the shade, it reported a heat index in direct sunlight of 55 °C. So to avoid the problems of  Rutting and bleeding this bitumen should not be used in Lahore.

FAQ: Softening Points

What Is the Softening Point?

The softening point is the temperature at which a resin or bitumen begins to flow under a specified load. It is a critical property for understanding the performance and application of these materials.

How Is the Softening Point Related to Resin Properties?

The softening point of resins is influenced by their average molecular weight, intrinsic viscosity, hardness, and brittleness. These factors determine how the material will behave when heated.

What Are the Standard Methods for Determining the Softening Point of Resins?

Several methods are used to determine the softening point of resins, including:

  1. Ring and Ball Method (R&B)
  2. Kreimer-Sarnow Method
  3. Mettler Softening Point Method
  4. Plate-Plate Stress Rheometer Test

How Does the Ring and Ball Method Work?

In the Ring and Ball Method, a steel ball is placed on a sample of resin within a metal ring. The sample is heated in a water or glycerol bath. The temperature at which the ball forces the softening resin downward is recorded as the softening point.

What Is the Kreimer-Sarnow Method?

The Kreimer-Sarnow Method involves using a small glass tube and a mercury drop as a load. The temperature at which the mercury drop breaks through the softening resin and falls is noted as the softening point.

How Does the Mettler Softening Point Method Differ from Other Methods?

The Mettler Softening Point Method is an automatic technique that measures the temperature at which a resin flows out of a sample cup under its own weight. The temperature is recorded when the first drop crosses a light path of a photocell, making this method accurate and reproducible.

What Is the Plate-Plate Stress Rheometer Test?

In the Plate-Plate Stress Rheometer Test, the resin is placed between two steel plates of a stress-controlled rheometer. The upper plate oscillates at a given frequency while the lower plate is heated. The softening temperature is estimated from the temperature at the cross-over between the storage and loss moduli.

How Is the Softening Point of Bitumen Determined?

The softening point of bitumen is typically determined using the Ring and Ball Test, as described in BS 4692. This method involves heating bitumen samples in metal rings and recording the temperature at which a steel ball passes through the softened material.

What Apparatus Is Used for the Ring and Ball Test for Bitumen?

The apparatus for this test includes:

  1. Brass shouldered ring
  2. Steel ball
  3. Ball centering guide
  4. Ring holder
  5. Brass pouring plate
  6. Bath
  7. Thermometer

What Is the Procedure for Determining the Softening Point of Bitumen?

The procedure involves assembling the apparatus with rings, thermometer, and ball guides, filling the bath with water or glycerol, and heating at a controlled rate. The temperature at which the bitumen softens and allows the ball to pass through the ring is recorded.

What Were the Results of the Softening Point Test for Bitumen?

In the experiment, the softening point of bitumen was found to be 45.1°C. This bitumen should not be used in areas with temperatures exceeding this point, such as DDIT Nadiyad, where temperatures can reach up to 46°C.

Why Is the Softening Point Important for Bitumen Usage?

The softening point indicates the temperature at which bitumen can start to deform. Using bitumen with an appropriate softening point ensures durability and prevents issues like rutting and bleeding in high-temperature conditions.

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