Thermogravimetric Analysis of Carbonate Aggregate, HR-336, 1994

Research has shown that one of the major contributing factors in early joint deterioration of portland cement concrete (PCC) pavement is the quality of the coarse aggregate. Conventional physical and freeze/thaw tests are slow and not satisfactory in evaluating aggregate quality. In the last ten years the Iowa DOT has been evaluating X-ray analysis and other new technologies to predict aggregate durability in PCC pavement. The objective of this research is to evaluate thermogravimetric analysis (TGA) of carbonate aggregate. The TGA testing has been conducted with a TA 2950 Thermogravimetric Analyzer. The equipment is controlled by an IBM compatible computer. A "TA Hi-RES" (trademark) software package allows for rapid testing while retaining high resolution. The carbon dioxide is driven off the dolomite fraction between 705 deg C and 745 deg C and off the calcite fraction between 905 deg C and 940 deg C. The graphical plot of the temperature and weight loss using the same sample size and test procedure demonstrates that the test is very accurate and repeatable. A substantial number of both dolomites and limestones (calcites) have been subjected to TGA testing. The slopes of the weight loss plot prior to the dolomite and calcite transitions does correlate with field performance. The noncarbonate fraction, which correlates to the acid insolubles, can be determined by TGA for most calcites and some dolomites. TGA has provided information that can be used to help predict the quality of carbonate aggregate.

Investigation of Rapid Thermal Analysis Procedures for Prediction of the Service Life of PCCP Carbonate Coarse Aggregate, HR-337, 1993

The major objective of this research project was to use thermal analysis techniques in conjunction with x-ray analysis methods to identify and explain chemical reactions that promote aggregate related deterioration in portland cement concrete. Twenty-two different carbonate aggregate samples were subjected to a chemical testing scheme that included: • bulk chemistry (major, minor and selected trace elements) • bulk mineralogy (minor phases concentrated by acid extraction) • solid-solution in the major carbonate phases • crystallite size determinations for the major carbonate phases • a salt treatment study to evaluate the impact of deicer salts Test results from these different studies were then compared to information that had been obtained using thermogravimetric analysis techniques. Since many of the limestones and dolomites that were used in the study had extensive field service records it was possible to correlate many of the variables with service life. The results of this study have indicated that thermogravimetric analysis can play an important role in categorizing carbonate aggregates. In fact, with modern automated thermal analysis systems it should be possible to utilize such methods on a quality control basis. Strong correlations were found between several of the variables that were monitored in this study. In fact, several of the variables exhibited significant correlations to concrete service life. When the full data set was utilized (n = 18), the significant correlations to service life can be summarized as follows ( a = 5% level): • Correlation coefficient, r, = -0.73 for premature TG loss versus service life. • Correlation coefficient, r, = 0.74 for relative crystallite size versus service life. • Correlation coefficient, r, = 0.53 for ASTM C666 durability factor versus service life. • Correlation coefficient, r, = -0.52 for acid-insoluble residue versus service life. Separation of the carbonate aggregates into their mineralogical categories (i.e., calcites and dolomites) tended to increase the correlation coefficients for some specific variables (r sometimes approached 0.90); however, the reliability of such correlations was questionable because of the small number of samples that were present in this study.

Investigation of Rapid Thermal Analysis Procedures for Prediction of the Service Life of PCCP Carbonate Coarse Aggregate: Phase I, Progress Report, HR-337, 1992

The major objective of this research project is to utilize thermal analysis techniques in conjunction with x-ray analysis methods to identify and explain chemical reactions that promote aggregate related deterioration in Portland cement concrete. The first year of this project has been spent obtaining and analyzing limestone and dolomite samples that exhibit a wide range of field service performance. Most of the samples chosen for the study also had laboratory durability test information (ASTM C 666, method B) that was readily available. Preliminary test results indicate that a strong relationship exists between the average crystallite size of the limestone (calcite) specimens and their apparent decomposition temperatures as measured by thermogravimetric analysis. Also, premature weight loss in the thermogravimetric analysis tests appeared to be related to the apparent decomposition temperature of the various calcite test specimens.