Chlorine and Sulfur in Cement

    Application Note EDXRF1250

    EDXRF1250 bannerScope

    The analysis of chlorine (Cl) and sulfur (as SO₃) in cement is demonstrated.

    Background

    Monitoring proper levels of chlorine is especially vital in producing cement. Soluble chlorine, most often CaCl₂, can be added to concretes and cements as an accelerating agent for faster strength development or shorter setting times. However, the presence of chlorine in reinforced concrete can cause corrosion of the steel reinforcing material, possibly causing premature structural damage. Sulfur in cement is often monitored during the addition of gypsum to the mixtures. The sulfur content in part determines drying rates and strength, as well as the ability of the cement to dry under water. For these reasons it is vital to monitor and control both the chlorine and sulfur levels. To meet this analytical need, Applied Rigaku Technologies offers a small, simple to use, benchtop EDXRF system ideal for use along the production and QC processes in a cement plant.

    800x610 NEX QC+ (S in Crude screen)_picture_2020.06.25Model: NEX QC

    Calibration

    Nine assayed cement samples were used to develop empirical calibrations for Cl and SO₃. The results of the calibrations are reported below. Mg, Al, Si, K, Ca, Fe, and Sr were also measured, without the need to have assay values. It is important to measure the elements present in the cement mix to enable alpha correction that compensate for matrix effects due to variations in X-ray absorption/enhancement effects. To model the sample set shown here, only two alpha corrections were required for the Cl and SO₃ fits. Different cement mixtures and calibration sets may require different sets of alpha corrections.

    Cl calibration

    Element: Cl
    Units: %
    Sample I.D. Standard value Calculated value
    1 0.020 0.0188
    2 0.012 0.0119
    3 0.013 0.0144
    5 0.044 0.0442
    6 0.030 0.0289
    7 0.021 0.0209
    8 0.032 0.0330
    9 0.056 0.0559

    EDXRF1250 Correlation plot ClCorrelation plot Cl

    SO₃ calibration

    Element: SO₃
    Units: %
    Sample I.D. Standard value Calculated value
    1 2.34 2.348
    2 2.10 2.125
    3 1.91 1.894
    4 0.89 0.895
    5 3.42 3.434
    6 2.70 2.730
    7 2.50 2.489
    8 3.04 3.012
    9 2.50 2.474

    EDXRF1250 Correlation plot SO3Correlation plot SO₃

    Repeatability

    To demonstrate recovery and repeatability (precision), two calibration standards were selected. Each was measured in 10 repeat analyses without moving the sample between measurements.

    Sample ID: 2
    Units: %
    Element STD value NEX QC value STD dev
    Cl 0.012 0.0104 0.0006
    SO₃ 2.10 2.089 0.027

    Sample ID: 9
    Units: %
    Element STD value NEX QC value STD dev
    Cl 0.056 0.0526 0.0009
    SO₃ 2.50 2.540 0.025

    Conclusion

    The results show NEX QC provides excellent performance for the measurement of Cl and SO₃ in cement using matrix-matched standards to model the particular clinker or cement type. The NEX QC offers a simple and fast means of analysis during the QA/QC process in the production of cement.