Analytical Instrumentation concentrations of Zinc, Phosphorus, Calcium and potentially
Molybdenum metals in these Asphalt samples as well. Historical testing has shown the following metals to be present in bitumen in mg/kg. The four samples represent bitumen samples taken from Nigerian Bitumen outcrops (5) - see Table 2
The following metal levels are found in Recycled Motor Oils Table 3 – Levels of elements of interest in REOB materials
Elements S P
Ca V
Fe
Cu Zn
Mo
Low Value 0.1%
0,005% 0.005% 0.0010% 0.005% 0.005% 0.005% 0.005%
High Value 5.00% 2.00% 2.00%
0.100% 0.200% 0.050% 1.00%
0.050%
Using XRF to Quantify the Metal Content of Asphalt Binders
The use of bench top EDXRF to characterize binders before blending them into asphalt cements is possible because the metal values are in the 10s – 1000s of ppms and are readily monitored. The characterization of Asphalt and Bitumen is also possible by using the internal ratio method available on most EDXRF systems. Sample preparation consists of transferring a constant mass to the cup to keep the mass of sample constant – the volume occupied would be a function of the density of the material.
The data generated in this study was collected on a Xenemetrix X-Cite Benchtop using the Analytix software package which has both empirical and fundamental parameter processes for evaluating data. Matrix effects were compensated for using the de Jongh algorithm and the data acquisition was accomplished in three segments providing optimal excitation conditions for the metals measured. Synthetic crude oil standards with multi- element compositions that varied independently were used to establish calibration curves and NIST reference standards were used to validate the method.
Validation Results on NIST Standards - See Table 5
Two NIST standards were used to validate the method Summary
The monitoring of metals in asphalt additives and ultimately in roadway runoff is able to be monitored using a very simple technique that is both robust and precise if calibrated correctly
Author Details
Laura Oelofse, XRF Sales and Consultants • Manor TX USA • Email:
laura@xrfsco.com
•
www.xenemetrix.com
Orly Jacobs, Xenemetrix • Migdal Haemek, Israel • Email:
info@xenemetrix.com
EDXRF elemental analysis spectrometers
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Element Calcium
Phosphorus Sulfur Zinc
Table 4 – Typical ranges of elements of interest to Asphalt producers
Elements S P
Ca V
Fe
Cu Zn
Mo
Low Value 0.1%
0,005% 0.005% 0.0010% 0.005% 0.005% 0.005% 0.005%
High Value 5.00% 2.00% 2.00%
0.100% 0.200% 0.050% 1.00%
0.050%
57
and the interelement effects are correctly assessed and compensated for. Multi element capability as well as very precise excitation conditions characterize EDXRF and make it the ideal instrument for routine laboratory measurements with the higher end EDXRF systems having the capability to quantify the carbon content of solid asphalt aggregate compacted into a briquette under substantial hydraulic pressure. In central laboratory facilities where the price of a 4kW WDXRF can be justified, the use of these instruments can be to measure secondary standards to be used for in-type material validation in solid form and disseminated to satellite instruments for real time in situ measurements.
Conclusion
XRF is a very cost effective method for characterizing the metal content in asphalt and asphalt related materials. Relatively simple sample preparation steps and sophisticated matrix correction methods can lead to highly accurate and precise results. Cross checking by ICP would be a good practice for any large scale XRF monitoring program but essentially well characterized samples that are products of round robin analysis as run through the Federal Highways Department can serve as check standards in XRF protocols.
References
1. The Effect of Asphalt Pavement on Stormwater Contamination - Andrew F. Nemeth Devon A. Ward Walter G.Woodington Worcester Polytechnic Institute May , 2010
2. Int. J. Environ. Res. Public Health 2012, 9, 1715-1731; doi:10.3390/ijerph9051715
3. The State of Knowledge Series – The use of REOB /VTAE in Asphalt – Asphalt Institute April 2016
4. International Conference on Environmental Forensics 2015 (iENFORCE2015), Concentration of heavy metals in virgin, used, recovered and waste oil: a spectroscopic study Munirah Abdul Zalia*,Wan Kamaruzaman Wan Ahmada, Ananthy Retnama, Ng Catrinab
5. Journal of Egytian Petroleum , Characterization of bitumen samples from four deposits in southwest, Nigeria using trace metals M.C. Onojake *, Leo C. Osuji, C.O. Ndubuka August 2016;
Figure 2 - Calibration Coefficients and Resultant Calibration Lines Table 5 - Comparison of values for NIST certified reference materials 1085-c and 1848 SRM 1085-c
Metals in Lubricating Oil mg/kg 299 304
285 Measured on X-cite
298 299
286 SRM1848 Lube Oil Addidtives
mg/kg except * m/m% 0.359* 0.788*
2.3270* 0.873*
0.355 0.783 2.345 0.860
Measured on the X-cite
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