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Fundamental Properties of Asphalts and Modified Asphalts, III

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KAO Gripper. The minor resonance was not assigned, but is assumed to be due to a dimer <strong>of</strong> the<br />

2-ethyl hexanol phosphate formed during preparation <strong>of</strong> the antistrip. The spectra <strong>of</strong> the Innovalt<br />

W <strong>and</strong> KAO gripper show partial hydrolysis <strong>of</strong> the PPA caused by residual water which is<br />

present in the antistrip agents. This is shown by the increase <strong>of</strong> the phosphoric acid resonance at<br />

~1.7 ppm relative to the phosphate ester resonance at ~0.7 pm with time <strong>of</strong> setting.<br />

There do not appear to be any reactions between the Innovalt W <strong>and</strong> KAO Gripper phosphate<br />

ester antistrip agents <strong>and</strong> PPA. Presumably, there would not be any such reactions when the<br />

antistrip <strong>and</strong> PPA were added to asphalt. To test this assumption, Innovalt W <strong>and</strong> KAO Gripper<br />

antistrips were added to asphalt AAM followed by PPA (115%) addition (figure 2-5.7). Both the<br />

antistrips <strong>and</strong> PPA were added at a level <strong>of</strong> 1 wt %. The purpose <strong>of</strong> these experiments was<br />

tw<strong>of</strong>old: (1) to determine if 31 P NMR can detect signals at the 1% level in a reasonable amount<br />

<strong>of</strong> time, <strong>and</strong> (2) to determine if there might possibly be reactions between the PPA <strong>and</strong> antistrip<br />

in asphalt.<br />

In the case <strong>of</strong> the phosphate ester antistrip agents, there is a single resonance at a chemical shift<br />

(~1.7 ppm) near that <strong>of</strong> phosphoric acid (~1.4.ppm). In both cases spectra with reasonable<br />

signal-to-noise, S/N, ratios were obtained after 3 h <strong>of</strong> signal averaging. When added to asphalt<br />

in the presence <strong>of</strong> PPA, the ester antistrip resonance could not be resolved from that <strong>of</strong><br />

phosphoric acid at the resolution <strong>of</strong> the WRI magnet. Under high resolution conditions, it is<br />

expected that these resonances could be resolved.<br />

Innovalt W in<br />

PPA (115%)<br />

At 99 h<br />

Innovalt W in<br />

PPA (115%)<br />

at 0 h<br />

Innovalt W neat<br />

30 25 20 15 10 5 0 -5 -10 -15 -20 -25 -30 -35 -40 -45 -50 30 25 20 15 10 5 0 -5 -10 -15 -20 -25 -30 -35 -40 -45 -50<br />

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

Figure 2-5.6. 31 P NMR spectra <strong>of</strong> phosphate ester antistrips, neat <strong>and</strong> with PPA (115%)<br />

at different times.<br />

64<br />

KAO Gripper in<br />

PPA (115%)<br />

At 360 h<br />

KAO Gripper<br />

In PPA (115%)<br />

At 0 h<br />

KAO Gripper neat

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