Applications of the X-Ray Fluorescence Spectroscopy (XRF) on Chloride Binding Isotherms
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1 Applications of the X-Ray Fluorescence Spectroscopy (XRF) on Chloride Binding Isotherms Marisol Tsui Chang August 4 th, 2016
2 Research Questions: How does the x- ray fluorescence spectroscopy (XRF) measure chloride concentration for chloride binding isotherms? How does the XRF method compare to the Titration method for this analysis?
3 Objectives: To develop a protocol to accurately analyze chloride in solutions for chloride binding isotherms using the XRF
4 The Basics of XRF: Non- destructive analytical technique that determines the chemical composition of any material
5 The Basics of XRF: Excites the material with a primary x- ray source Measures the emitted fluorescent or secondary x- ray and its intensity Image taken from
6 Chloride Binding Environmental exposure of concrete to salts 2 types of chlorides in concrete: Free: chloride ions in solution Bound: chloride ions that react with mineral phases in cement paste Calcium oxychloride
7 Chloride Binding Calcium Hydroxide (Portlandite) from cement matrix Image taken from
8 Chloride Binding Calcium Chloride from deicing salts Image taken from
9 Chloride Binding Calcium Oxychloride Image taken from
10 Chloride Binding Importance: Damage in concrete due to the formation of calcium oxychloride
11 XRF for Chloride Binding Solutions: Sample Preparation of Solutions (Cody) Titration analysis of chloride concentration (Cody) Calibration of XRF (Marisol) Sample Preparation of Solutions for XRF (Marisol) XRF analysis of chloride concentration (Marisol)
12 XRF for Chloride Binding Solutions: Sample Preparation of Solutions: Mix 4 g of powdered cement paste with 10 ml of CaCl 2 solution 14 cement mixtures CaCl 2 at 18 different concentrations Three temperatures: 5 C, 23 C, 38 C Cement exposure to CaCl 2 solution for 6 weeks
13 XRF for Chloride Binding Solutions: Sample Preparation of Solutions: Top solution extracted Measure the chloride concentration of extracted solution with titration and with XRF
14 XRF for Chloride Binding Solutions: Sample Preparation for XRF Solution sample preparation with Mylar film Time of preparation: 5 minutes Calibration Calcium chloride (>99% purity) known solutions at different concentrations Analysis Time of analysis: 3 minutes
15 XRF for Chloride Binding Solutions: Analysis of bound chlorides versus calcium chloride initial concentration Bound chloride = difference between initial concentration of CaCl 2 and free chlorides in solution tested Figure 1: Difference between isotherms due to the formation of calcium oxychloride Figure taken from Effects of temperature on the chloride binding of Portland cement pastes exposed to CaCl 2 Solutions by Wei, Tao and Weiss
16 XRF for Chloride Binding: 7.00 Chloride Binding Isotherm for Mixture 1 at 5 C Bound Chloride Concentration (%) CaCl2 Concentration (%) Figure 2: Chloride concentration results from the titration versus the XRF method
17 XRF for Chloride Binding: Table 1: Chloride concentration from titration and from XRF
18 XRF versus Titration: Chloride Concentration from XRF (%) Chloride Concentration from XRF versus Titration y = x R² = Chloride Concentration from Titration (%) Figure 3: Chloride concentration results from the titration versus the XRF method
19 Solutions for Chloride Binding: XRF can be used to produce chloride binding isotherms There is a good 1:1 linear correlation between both methods results (titration and XRF) Advantages of XRF: Less time testing for chloride concentration Can detect other elements (Na, K, etc)
20 Advisors: Dr. Prannoy Suraneni post- doctoral researcher at Oregon State University Dr. W. Jason Weiss head of the Civil and Construction Engineering School at Oregon State University Weiss Research Group at Oregon State University Cody Tibbits masters student at Oregon State University
21 Questions?
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