Standard Specification for

Detecting the Presence of Phosphorous

in Asphalt Binder

AASHTO Designation: TP 78-09 1

1. SCOPE
1.1. This qualitative test method can be used to identify the presence of polyphosphoric acid (PPA) in
asphalt binder or residue. If PPA is present in the binder, a blue color is developed in
approximately 5 min. The test method is not quantitative, but it can detect PPA at concentrations
as low as 0.1 percent. The test method can only determine the presence of phosphorus. It is not
specific for the presence of PPA. A positive test result assumes that the phosphorus is from PPA.
Any additive that contains phosphorus will give a false positive for the presence of PPA.

1.2. The values stated in SI units are to be regarded as the standard.

1.3. This standard does not purport to address all of the safety concerns, if any, 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 Standard:
 T 40, Sampling Bituminous Materials

3. SUMMARY OF TEST METHOD

3.1. Butyl alcohol is used to extract some of the acid present from the asphalt. The extracted acid is
then transferred to the water phase. The presence of phosphoric acid is detected by reaction with
ammonium molybdate, potassium antimonyl tartrate, and ascorbic acid to form a blue color.

4. SIGNIFICANCE
4.1. Phosphoric acid may be added to asphalt binder to modify the physical properties of the binder.
This test method detects the presence of phosphoric acid in the asphalt binder but is not a
quantitative test. The result is either positive or negative that phosphoric acid is present.

5. APPARATUS
5.1. Pipette—Disposable, plastic transfer pipettes.

5.2. Containers—One-ounce cans, test tubes, or small beakers. Disposable cans or glassware are
recommended to avoid contamination. If glassware is reused, it must be washed with hot (1 + 3)
hydrochloric acid (1 part hydrochloric acid to 3 parts distilled water) and rinsed with distilled

TS-2b TP 78-1 AASHTO

© 2013 by the American Association of State Highway and Transportation Officials.
All rights reserved. Duplication is a violation of applicable law.
 water. Commercial detergents should not be used to clean the glassware because they may contain
phosphates, which will interfere with the results.
Note 1—One agency found that the cans they were using for this test had been lubricated during
the manufacturing process with a lubricant containing phosphates. This resulted in a positive result
in this test even with the empty can. If there is doubt about the condition of the containers being
used, then take the precaution of running a blank test with no asphalt.

6. REAGENTS AND MATERIALS

6.1. Antimonyl Tartrate/Ammonium Molybdate Solution—Dissolve 0.13 g of potassium antimonyl
tartrate hydrate [C8H4K2O12Sb2∙H2O] in 50 mL of distilled water. Add 5.6 g of ammonium
molybdate [(NH4)6Mo7O24∙4 H2O] and swirl until dissolved.

6.2. Sulfuric Acid Solution—1 N solution of sulfuric acid [H2SO4]. Sulfuric acid solution can be
purchased in 1-L polyethylene bottles.

6.3. Stock Solution—Mix the antimonyl tartrate/ammonium molybdate solution from Section 6.1 with
approximately 950 mL of 1 N sulfuric acid solution. This can be done by adding the solution from
Section 6.1 to 1 L of 1 N sulfuric acid if there is sufficient space in the bottle. The exact amount of
sulfuric acid is not critical. This solution is stable for 1 year.

6.4. Ascorbic Acid Color Reagent—Dissolve 0.50 g of L-ascorbic acid [C6H8O6] in 100 mL of the
stock solution from Section 6.3. Prepare the reagent fresh daily as needed.

6.5. Butyl Alcohol—Isobutanol [(CH3)2CHCH2OH] or n-butanol [CH3(CH2)3OH] may be used.

7. SAMPLING
7.1. Sample the material in accordance with T 40. See Note 2 regarding potential concerns regarding
contamination of sampling container.

8. PROCEDURE
8.1. Heat the asphalt and pour 1 to 2 g into a 1-oz can or other small container.

8.2. Place the container in an oven set at 163 ± 10°C for 10 min to ensure the asphalt is fluid.

8.3. Remove the container, and immediately add 2 mL of butyl alcohol while stirring the container.

8.4. Continue to stir the container and add 2 mL of distilled water.

8.5. While still stirring the container, add 2 mL of the ascorbic acid color reagent. After the addition of
the color reagent, stop stirring and allow the sample to sit for 5 to 10 min.

8.6. If phosphoric acid is present in the asphalt, a blue color will develop within 5 to 10 min. Decant
the solution into a second container if unable to see the color.
Note 2—After 30 min, the results are not reliable. The color may either fade or intensify after
30 min.

8.7. If a blue color appears, the sample is reported as “positive.” The sample is reported as “negative”
if it does not turn blue.

TS-2b TP 78-2 AASHTO

© 2013 by the American Association of State Highway and Transportation Officials.
All rights reserved. Duplication is a violation of applicable law.
 Note 3—The blue color, if present, will be in the aqueous phase, which will be at the bottom.
Often the top layer has a brown or green color.

8.8. When new reagents are prepared, prepare and run a blank (asphalt with no phosphoric acid).

9. REPORT
9.1. This report shall include the following:

9.1.1. Identification of sample.

9.1.2. “Positive” or “Negative” result.

10. PRECISION AND BIAS

10.1. Precision—The research required to develop precision estimates has not been conducted.

10.2. Bias—This test method has no bias since the values determined can only be defined in terms of
this test method.

11. KEYWORDS
11.1. Asphalt; phosphoric acid; PPA.

1
This provisional test method was adopted and first published in 2009.

TS-2b TP 78-3 AASHTO

© 2013 by the American Association of State Highway and Transportation Officials.
All rights reserved. Duplication is a violation of applicable law.