Standard Method of Test for

Polymer Content of Polymer-Modified

Emulsions and Asphalt Binders
AASHTO Designation: T 302-04
SCOPE

1.1.

This test method is used to determine the percent concentration of a Styrene-Butadiene-Rubber

(SBR), Styrene-Butadiene (SB), or Styrene-Butadiene-Styrene (SBS) polymer in a polymermodified asphalt binder or emulsion residue. By using the infrared spectrum and the principles of
Beers Law, the polymer content of the asphalt material can be determined.

1.2.

This test method implies that the equipment used for the analysis is operated by experienced
personnel according to the manufacturers directions for optimum performance.

1.3.

This standard involves hazardous materials, operations, or equipment. This standard does not
purport to address all of the safety concerns associated with its use. It is the responsibility of the
user of this standard to establish appropriate safety and health practices and determine the
applicability of regulatory limitations prior to use.

2.

REFERENCED DOCUMENTS

2.1.

AASHTO Standards:
 M 231, Weighing Devices Used in The Testing of Materials

2.2.

Other Documents:
 Infrared Spectrophotometer Operators Manual

3.

APPARATUS

3.1.

Infrared Spectrophotometercapable of recording spectrum from a wavelength of the 1800 to

600 cm1 region.

3.2.

Variable speed shearing mixer.

3.3.

Heating coil with variable rheostat.

3.4.

Thermometer for determining temperatures at 4305C (40580F).

3.5.

Infrared windowspolished sodium chloride or potassium chloride windows, or other suitable

medium for casting of infrared specimens.

3.6.

Eyedroppers.

TS-2a
Copyright American Association of State Highway and Transportation Officials
Provided by IHS under license with AASHTO
No reproduction or networking permitted without license from IHS

T 302-1
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1.

AASHTO

Glass vial with leak resistant top.

3.8.

Infrared heat lamp.

3.9.

High-temperature vacuum oven.

3.10.

Balance conforming to the requirements of M 231, Class G1.

3.11.

Solvent.
Note 1Trichloroethane, technical grade or Tetrahydrofuran (THF) have been shown as suitable
solvents that do not interfere with the infrared spectrum. Other appropriate solvents may be used.

3.12.

Containers for blending the asphalt material with polymermetal pint (0.47 L) cans with lids are
suitable.

4.

PREPARATION OF CONTROL SAMPLES

4.1.

Weigh 300 5 g of asphalt binder or emulsion into a container suitable for mixing for each
standard. Record the weight to the nearest gram.

4.2.

Heat the asphalt binder until fluid, at a temperature not to exceed 163C (325F). An emulsion
should be heated to 82 1C (180 2F). Maintain this temperature while adding the polymer.

4.3.

Mix a minimum of three standards containing from 0 to 5 percent polymer (rubber solids) in equal
increments.
Note 2The standards are prepared on a weight to weight (w/w) percentage. This percentage is
based on the solids weight of the polymer and the weight of the base asphalt binder or the asphalt
emulsion residue. If the polymer is in an emulsified form and/or the standards are being made with
an asphalt emulsion, an accurate determination of the rubber solids and/or percent asphalt residue
must be made in order to prepare accurate standards.

4.4.

Example calculation:

( E )( R )(100)
A

(1)

= Percent polymer standard

where:
E = mass of emulsified polymer
R = Percent rubber solids in decimal form
A = mass of base asphalt binder or emulsion
Example:
(15.1)(0.60 )(100 ) = 3%
302.0
E = 15.1 g
R = 60 percent
A = 302.0 g

TS-2a
Copyright American Association of State Highway and Transportation Officials
Provided by IHS under license with AASHTO
No reproduction or networking permitted without license from IHS

T 302-2
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AASHTO

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3.7.

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4.5.

While maintaining heat, slowly add the calculated amount of polymer for each standard to the
appropriate weighed container of base asphalt binder or emulsion with the mixer in operation.
Allow the materials to mix thoroughly.

4.6.

While the standards are still in a homogeneous and liquid state, remove approximately 1 g from
each standard and place in an appropriately labeled vial with a leak-resistant top.

4.7.

If there is any residual moisture in the standards, place the vials in a vacuum oven set at
approximately 20 mm of Hg vacuum at 104 2C (220 4F) until constant mass is achieved.

4.8.

After drying, remove the vials from the oven and cool to room temperature before making the
dilutions necessary for infrared scanning.

5.

PREPARATION OF POLYMER SAMPLES

5.1.

Heat asphalt binder until fluid, at a temperature not to exceed 163C (325F), or if emulsion, heat
to 82 1C (180 2F), stirring to achieve a homogeneous state.

5.2.

After the sample is thoroughly mixed, place approximately 1 g in a glass vial.

5.3.

If there is any residual moisture in the sample, place the vials in a vacuum oven set at
approximately 20 mm of Hg, vacuum at 104 2C (220 4F) until constant mass is achieved.

5.4.

After drying, remove the samples from the oven and cool to room temperature before making the
dilutions for infrared scanning.

6.

DILUTIONS FOR INFRARED SCAN

6.1.

Dilute contents of each glass vial containing standards and samples with 10 mL of the solvent.

6.2.

Shake the vials until the sample is completely dissolved in the solvent.

7.

PROCEDURE

7.1.

Preparing Thin Films:

7.1.1.

Place drops of the diluted standards and sample on individual infrared windows using an
eyedropper. Insure that an even smear is placed on the windows. At a wavelength of 1460 cm1,
the transmittance level should be approximately 40 percent 5 percent for a good scan.

7.1.2.

Allow the solvent to evaporate at room temperature or place the windows under a heat lamp for
approximately 10 minutes to drive off any residual solvent.

7.2.

Analysis of the Standards:

7.2.1.

Scan the prepared infrared window for each standard from a wavelength of 1800 cm1 to 600 cm1.

TS-2a
Copyright American Association of State Highway and Transportation Officials
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T 302-3
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AASHTO

Determine the absorbance of the peaks at a wavelength of 965 cm1 for the SBR, SB or SBS and at
a wavelength of 1375 cm1 for base asphalt binder or emulsion on each standard. (See example in
Figure 1.)

7.2.2.

0.5

Absorbance

0.4

Absorbance Ratio = A1 / A2

0.3

-1

1375 cm (A2)

0.2
-1

0.1

965 cm (A1)

0.0
1800

1600

Mattson GL- 3025

Resolution: 4.0
Gain: 1 Scans: 32

1400

1200

1000

800

600

Wavenumbers (cm-1)
Iris: 0

Figure 1Infrared Scan of a Polymer Modified Asphalt Material

Divide the value of the peak at 965 cm1 (A1) by the peak at 1375 cm1 (A2) to obtain the ratio of
the relative peak values (A1/A2) of each standard.

7.2.3.

A1
= absorbance ratio
A2
where:

(2)

7.2.4.

Plot the ratio of the relative peak values (A1/A2) versus the corresponding percent polymer
content of each standard.

7.2.5.

Plot the first-order curve fit on the data to generate a standard curve. (See example in Figure 2.)

Table 1Typical Data for Standard Curve Development

Standard, %
Polymer

Absorbance Ratio
(A1/A2)

0.02

0.065

0.11

0.155

0.20

0.245

TS-2a
Copyright American Association of State Highway and Transportation Officials
Provided by IHS under license with AASHTO
No reproduction or networking permitted without license from IHS

T 302-4
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AASHTO

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A1 = peak value at 965 cm1

A2 = peak value at 1375 cm1

Absorbance Ratio (A1/A2)

0.3
0.25
0.2
X = Y 0.02
0.045
X=Yb
m

0.15
0.1
0.05
0
0

% Polymer

Figure 2Percent Polymer Content vs. Absorbance Ratio (A1/A2)

7.3.

Analysis of Sample:

7.3.1.

Perform Sections 7.2.1 through 7.2.3 for each sample and obtain the relative ratio (A1/A2) of the
sample.

7.3.2.

Determine the percent polymer content of the sample from the standard graph or mathematically.

7.3.2.1.

Example mathematical calculation:

Absorbance Ratio on Sample
A1 0.025
=
= 0.126
A2 0.199
Calculation of Percent Polymer Content
y b
m

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x=

(3)

where:
y = Absorbance Ratio (A1/A2)
m = 0.045
b = 0.02
x=

0.1260.02
0.045

(4)

x = 2.4 % Polymer

8.

REPORT

8.1.

The values determined for the polymer content shall be reported to the nearest 0.1 percent.

9.

PRECISION AND BIAS

9.1.

Information is not available to make a precision and bias statement.

TS-2a
Copyright American Association of State Highway and Transportation Officials
Provided by IHS under license with AASHTO
No reproduction or networking permitted without license from IHS

T 302-5
Licensee=Fluor Corporation/2110503106, User=Melendez, Segundo
Not for Resale, 07/06/2015 10:29:50 MDT

AASHTO