Application note issue #5 Cement Analysis August 2017 Cement analysis using FP program (Fundamental Parameters) Cement is a blend of several minerals. It is critical to control the elemental composition and properties such as strength, setting, time and color. ED-XRF is being used to analyze the raw components, raw meal, clinker, and the final cement product (Na, Mg, Al, Si, S, K, Ca, and Fe in Cement, Clinker, and Raw Meal). XRF is at the heart of the control of the production process in any modern cement works and is central to the ability of the cement maker to produce a consistent product. All measurements were conducted on Xenemetrix X-Calibur analyzer, using fundamental parameters program. The X-Calibur is an excellent bench-top EDXRF analyzer for qualitative and quantitative elemental analysis. It offers an accurate, precise, fast, simple and non-destructive analysis technique. Advanced Fundamental Parameters Software is a complete XRF analysis tool enabling quantitative analysis of various samples. This program provides strong analytical tools and abilities in R&D, Geological applications, Reverse engineering, process control and other applications. The sample preparation conducted on Equilab systems - Pressed pellet preparation on EQP-100 and fused beads preparation on induction fluxer F1. X-Calibur EQP-100 induction fluxer F1 1
The Unknown Sample Cement 1885A (Table 1) was used as unknow sample and was analysed in: 1. Pressed pellet form 2. Fused bead form The Standards The quantification was done using FP program with one standard for the pressed pellet (Table 2) and one standard for the fused bead (Table 3) for calibration. 2
Sample preparation Pressed pellet preparation Both samples (unknow and standard) were pressed the same way. Fused beads preparation Samples (unknow and standards) were prepared the same way. Sample were mixed with a fluxer (lithium borate) at the ratio of- 1 (sample): 10 (fluxer). Cement Fluxer Fluxer 3
Acquisition of the pellet The Xenemetrix X-Calibur measured and provided Spectrum for 12 different acquisitions: 2 in press pellets form (unknown and standard) and 2 in fused beads form (unknown and standard). Each pair measured in 3 different system configurations (see conditions): Each sample (fused bead and pressed pellet) was analysed separately, each one using a calibration file created with one standard. Three acquisition conditions were used in order to see all the elements in an optimal way (Table 4). Table 4 Excitation mode Voltage [kv] Current [μa] Environment Element of interest Condition 1 No filter 8 30 He Mg, Al, Si, S, Ca, Ti, Fe Condition 2 No filter 4 900 He Na Condition 3 Ti filter 10 900 Air K Fundamental parameters (FP) analysis The first file opened template file is the calibration file created with one certified standard for the fused bead and one certified standard for the pressed pellet. Fundamental Parameter method correlates between the measured X-ray intensities and the elemental concentrations in samples, based on X-ray physics and measured values of fundamental atomic parameters in the ED-XRF region of the spectra. FP program are the correct and accurate solution in case a series of standards are unavailable, and the absence of a calibration curve. 4
Results Fused bead Pressed pellet Comparison Fused bead Pressed pellet Certified value SiO2 20.541 20.812 20.909 Al2O3 5.915 5.857 4.026 Fe2O3 1.827 1.722 1.929 CaO 60.952 60.020 62.39 MgO 4.353 4.905 4.03 SO3 2.765 2.892 2.83 Na2O 1.195 1.255 1.068 K2O 0.367 0.261 0.206 TiO2 0.217 0.177 0.195 *Enhanced accuracy can be achieved by using additional standards. Conclusion Cement material can be accurately analysed by EDXRF technology. The preferred sample preparation method can be either press pellets or fused beads. Fundamental Parameters algorithmically calculates the concentration and provides precise and accurate results which correlate to the expected concentrations. EDXRF is recommended as a simple and easy method to quantify metals in cement and can be a reliable tool to monitor the production of a consistent product. Email: info@xenemetrix.com www.xenemetrix.com Tel: +972-4-9891313 Fax: +972-4-9891323 Ramat Gabriel Industrial Zone, 6 Hatikshoret St., Migdal Haemek 2310901, Israel Copyright Xenemetrix 2008. All rights reserved 5