Abstract

New global tendencies for waste materials reusing in building materials are imposing the request for improved performances of chemical analysis methods and the improvements of matrices used. A new method for optical emission spectrometry with inductively coupled plasma (ICP-OES) is developed and validated for the chemical analysis (35 elements: Al, Be, Cd, So, Cr, Cu, Fe, Mn, Mo, Ni, V, Mo, Zn, Pb , Bi, Si, Zr, W, As, Se, Sb, Sn, Ti, Ba, B, Ag, Mg, Ca, K, Na, S, P, Ga, In, Li) in leachate of fly ash. Validation performances and the uncertainty ?f measurement were resolved. Uncertainty ?f measurements were resolved by three routes: validation procedure, participation in proficiency testing (PT) schemes and standard method. The obtained method is a new simple and effective analyzing route for determination of undesired trace elements and their quantity comprised in leachates of fly ash, and leachates of building materials with addition of fly ash (cement binders and mortars). In order to prove its accuracy and precision, the developed method was employed on laboratory samples of cement binders and mortars. Results were compared with limit values provided in the standard. Multivariate analyses, i.e. cluster analysis and principal component analysis, were applied to establish interrelations between analyzed samples, and to certify the developed ICP-OES method.

Highlights

  • With the rapid economic increase and the development of industry, increasingly more solid waste has been produced

  • According to EURACHEM 1998 the validation was performed by evaluating the selectivity, i.e. the ability to unequivocally assess the analyte in the presence of components that are expected to occur in the solution (Matix effect), linearity, limit of detection (LoD), limit of quantification (LoQ), precision and accuracy [22]

  • LoD, LoQ, correlation coefficients, Y-intercepts and slopes of linear function are automatically calculated by Smart Analyzer Vision software

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Summary

Introduction

With the rapid economic increase and the development of industry, increasingly more solid waste has been produced. The leaching behavior of heavy metals is dependent on physical and chemical factors. Some of chemical factors are complexation processes, availability for leaching, related with pH and redox conditions, control mechanisms such as kinetic or equilibrium, and sorption processes [6] Some elements, such as Si, Al, Ca and Fe are the major elements of fly ash which play important role on the leaching of toxic heavy metals. The ICP-OES method is a routine analytical technique for metal determination. The developed method is employed on the leachate of fly ash, and subsequently affirmed on the leachates obtained on the crushed samples of cement binders and mortars. Mortar samples were prepared and cured with respect to the method given in SRPS EN 196-1:2018 (Methods of testing cement - Part 1: Determination of strength). Water: binder ratio 0.5 was used for preparation of both mortar mixtures

Leaching test
Calibration standards
Preparation of the matrix spike standards
Statistical analysis
Validation method
Accuracy and precision
Measurement uncertainty
Measurement uncertainty calculated by validation data
Measurement uncertainty calculated by data provided in the standard method
Principal component analysis
Conclusion
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