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    Determination of Alkali Metals in Cement

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    Mansueta Stefanus
    This document describes a method for determining alkali metals like sodium and potassium in cement using a flame photometer. The method involves preparing aluminum nitrate and sodium/potassium standards, dissolving a cement sample, and measuring intensities to generate a standard curve. The sample reading is used to determine concentration by the calibration curve. Calcium interference is suppressed by adding aluminum to the sample. Percentages of sodium or potassium in the original sample are then calculated from ppm readings and sample weight.

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    Determination of Alkali Metals in Cement

    Uploaded by

    Mansueta Stefanus
    90 views2 pages
    This document describes a method for determining alkali metals like sodium and potassium in cement using a flame photometer. The method involves preparing aluminum nitrate and sodium/potassium standards, dissolving a cement sample, and measuring intensities to generate a standard curve. The sample reading is used to determine concentration by the calibration curve. Calcium interference is suppressed by adding aluminum to the sample. Percentages of sodium or potassium in the original sample are then calculated from ppm readings and sample weight.

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    This document describes a method for determining alkali metals like sodium and potassium in cement using a flame photometer. The method involves preparing aluminum nitrate and sodium/potassium standards, dissolving a cement sample, and measuring intensities to generate a standard curve. The sample reading is used to determine concentration by the calibration curve. Calcium interference is suppressed by adding aluminum to the sample. Percentages of sodium or potassium in the original sample are then calculated from ppm readings and sample weight.

    Copyright:

    © All Rights Reserved
    Download as PDF, TXT or read online from Scribd
    Download as pdf or txt
    90 views2 pages

    Determination of Alkali Metals in Cement

    Uploaded by

    Mansueta Stefanus
    This document describes a method for determining alkali metals like sodium and potassium in cement using a flame photometer. The method involves preparing aluminum nitrate and sodium/potassium standards, dissolving a cement sample, and measuring intensities to generate a standard curve. The sample reading is used to determine concentration by the calibration curve. Calcium interference is suppressed by adding aluminum to the sample. Percentages of sodium or potassium in the original sample are then calculated from ppm readings and sample weight.

    Copyright:

    © All Rights Reserved
    Download as PDF, TXT or read online from Scribd
    Download as pdf or txt
    of 2

    Flame Photometer PFP7 Protocol: P05-060A

    The Flame Photometric Determination of Alkali Metals in


    Cement
    Introduction
    When using a flame photometer for the determination of sodium, difficulty is experienced when lime
    (calcium) is present in appreciable amounts of more than a few per cent. This is due to the calcium emitting
    some radiation, which passes through the sodium filter to a measurable extent. This error must be taken
    into account or it can, in the case of cements, cause errors of up to 100% in the reported sodium content.

    Methods that remove the calcium from the sample, or methods that add equivalent amounts of calcium to
    the instrument calibration solutions are available, but in this method the interference is suppressed by the
    addition of aluminium to the sample.

    Materials Required
    Equipment
    Jenway flame photometer
    Accurate balance weighing to 0.0005g
    Volumetric flasks
    Whatman filter paper – No.40
    Ice bath

    Reagents
    Aluminium – Metal
    Mercury (II) Chloride – 5% solution
    Nitric Acid 70%w/w
    Hydrochloric Acid 37%w/w
    Sodium Standard – 1000ppm (Part number 025 021)
    Potassium Standard – 1000ppm (Part number 025 023)
    Deionised Water

    Method
    Aluminium nitrate solution preparation

    1. Whilst cooling in an ice bath, dissolve 30.0g of aluminium in 400ml of 1:1 nitric acid in a 1.0L volumetric
    flask. Add a few drops of 5% mercury (II) chloride solution to facilitate the dissolution of the aluminium.

    2. Allow the solution to cool to room temperature and dilute to volume with deionised water.

    Standard preparation

    1. Accurately pipette 10.0ml of the 1000ppm sodium standard and 10.0ml of the 1000ppm potassium
    standard into a 1.0 L volumetric flask containing 400ml of deionised water.

    2. Add 10ml of concentrated hydrochloric acid.

    3. Make up to volume with deionised water. This is a 10ppm sodium and potassium standard solution.

    4. From the 10ppm standard solution, prepare 100.0ml of 7.5, 5 and 2.5ppm standard solutions using
    deionised water as diluent.

    [email protected]
    www.jenway.com
    Tel: 01785 810433
    Sample preparation

    1. Mix 0.5g of cement, accurately weighed, with 45ml of deionised water and 5ml of concentrated
    hydrochloric acid.

    2. Heat the solution to boiling point and filter through a no. 40 filter paper into a 500ml volumetric flask.

    3. Wash the filter paper with 6 x 30ml aliquots of hot deionised water.

    4. Add 100ml of aluminium nitrate solution and allow the solution to cool.

    5. Once cool, dilute the solution to volume with deionised water.

    Method

    1. Set up the flame photometer as detailed in the instruction manual.

    2. Aspirate deionised water and set the zero.

    3. Aspirate the standards into the flame photometer.

    4. Plot a standard curve of sodium/potassium concentration against intensity.

    5. Aspirate the sample solution into the flame and record the reading. If the reading is above the value
    recorded for the 10ppm standard, dilute the sample until the value is within the range of the calibration
    curve.

    Calculation
    From the results obtained from the calibration graphs, the percentage of sodium or potassium in the sample
    can be determined. The results should be multiplied by any dilution factor used in the samples preparation.

    Sodium content of cement (%) = sample (ppm) x 500 x 100%


    1000000 x sample weight (g)

    Potassium content of cement (%) = sample (ppm) x 500 x 100%


    1000000 x sample weight (g)

    [email protected]
    www.jenway.com
    Tel: 01785 810433

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