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Fundamental Properties of Asphalts and Modified Asphalts, III

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100<br />

1% Innovalt W in AAM-1<br />

1% PPA(115%) <strong>and</strong><br />

1% Innovalt W in AAM-1<br />

1% PPA(115%) in AAM-1<br />

75<br />

50<br />

25<br />

Figure 2-5.7. 31 P NMR spectra <strong>of</strong> Innovalt W <strong>and</strong> KAO Gripper antistrip agents in<br />

PPA modified asphalt AAM-1.<br />

31P NMR Moisture determination<br />

0<br />

Some exploratory work was performed to determine if 31 P NMR could be used to determine the<br />

residual moisture content <strong>of</strong> asphalt. In part, this work was initiated because previous work had<br />

shown that PPA reacts with residual water in asphalt to form orthophosphoric acid. However,<br />

the extent <strong>of</strong> hydrolysis cannot be predicted apriori because the amount <strong>of</strong> residual water in<br />

asphalts is generally not known. A simple method for determining moisture may be useful in<br />

providing more quantitative data about the reaction.<br />

The 31 P NMR method is based on the use <strong>of</strong> phosphorous compounds that react with water to<br />

form anhydrides. For the moisture determinations, diphenylphosphinic chloride (Ph2POCl), here<br />

referred to as DPPC, was used as the derivatizing agent [Dadey et al. 1988; Wroblewski et al.<br />

1991a,b]. DPPC reacts with water in the presence <strong>of</strong> base (pyridine) to form the anhydride,<br />

Ph2P(O)OP(O)Ph2 ( 1,1,3,3-tetraphenyldiphosphoxane 1,3-dioxide) according to Scheme I,<br />

2Ph2POCl + H2O + Ph2P(O)OP(O)Ph2 + 2<br />

N<br />

-25<br />

-50<br />

Scheme I<br />

-75<br />

-100<br />

65<br />

100<br />

KAO Gripper in AAM-1<br />

1% PPA(115%) <strong>and</strong><br />

1% KAO Gripper in AAM-1<br />

1% PPA(115%) in AAM-1<br />

Phosphorous Chemical Shift, ppm Phosphorous Chemical Shift, ppm<br />

75<br />

50<br />

25<br />

N +<br />

H Cl -<br />

0<br />

-25<br />

-50<br />

-75<br />

-100

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