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    Determination of Iron in Cement by Photometric Titration: Titration Application Note T-80

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    Xiomara Jorga
    This document describes a photometric titration method for determining the amount of iron in cement using EDTA as the titrant and sulfosalicylic acid as the indicator. The method involves digesting a cement sample, filtering, and titrating the iron in the sample solution from reddish violet to faintly yellow. The amount of iron is calculated based on the titrant consumption and used to report the percentage of Fe2O3 in the cement sample.

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    © All Rights Reserved
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    Determination of Iron in Cement by Photometric Titration: Titration Application Note T-80

    Uploaded by

    Xiomara Jorga
    199 views2 pages
    This document describes a photometric titration method for determining the amount of iron in cement using EDTA as the titrant and sulfosalicylic acid as the indicator. The method involves digesting a cement sample, filtering, and titrating the iron in the sample solution from reddish violet to faintly yellow. The amount of iron is calculated based on the titrant consumption and used to report the percentage of Fe2O3 in the cement sample.

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    analiticas

    Original Title

    926258_AN-t080

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    This document describes a photometric titration method for determining the amount of iron in cement using EDTA as the titrant and sulfosalicylic acid as the indicator. The method involves digesting a cement sample, filtering, and titrating the iron in the sample solution from reddish violet to faintly yellow. The amount of iron is calculated based on the titrant consumption and used to report the percentage of Fe2O3 in the cement sample.

    Copyright:

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

    Determination of Iron in Cement by Photometric Titration: Titration Application Note T-80

    Uploaded by

    Xiomara Jorga
    This document describes a photometric titration method for determining the amount of iron in cement using EDTA as the titrant and sulfosalicylic acid as the indicator. The method involves digesting a cement sample, filtering, and titrating the iron in the sample solution from reddish violet to faintly yellow. The amount of iron is calculated based on the titrant consumption and used to report the percentage of Fe2O3 in the cement sample.

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    © All Rights Reserved
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    Titration Application Note T80

    Determination of iron in cement


    by photometric titration

    This Application Note describes the digestion of a cement sample and the photometric determination of iron according to DIN EN 196-2 by using the Optrode
    at 610 nm. Sulfosalicylic acid was used as indicator and EDTA as titrant.

    Method description
    Sample

    Analysis

    Portland-cement

    Titer

    Sample preparation

    2 mL CaCl2 standard are pipetted into a sample beaker,


    1.0 mL calconcarboxylic acid indicator, 120 mL dist. H2O
    and 4 mL c(NaOH) = 2 mol/L are added. The solution is
    titrated immediately with c(Na2EDTA) = 0.05 mol/L.

    Approximately 2.5 g cement are mixed with 1 g ammonium chloride and thoroughly brayed with a glass rod.
    Then, 10 mL conc. HCl and 0.5 mL conc. HNO3 are
    added. The mixture is heated in a water bath for 30
    minutes. The pasty mixture is diluted with a small
    amount of dist. H2O and quantitatively filtered through
    a coarse-pored filter (595) into a 500 mL volumetric
    flask. The filter is well rinsed with hot dist. H2O. After
    cooling, the combined filtrate and washings are made
    up to the mark with dist. H2O (sample solution).
    Configuration
    905 Titrando
    800 Dosino
    Dosing unit 5 mL
    Dosing unit 10 mL
    Dosing unit 50 mL
    802 Rod Stirrer incl. propeller
    814 USB Sample Processor
    Sample rack 12x250 mL
    Sample beaker 250 mL glass
    Optrode ( = 610 nm)
    Ecotrode plus
    Electrode cable

    2.905.0010
    4 x 2.800.0010
    2 x 6.3032.150
    1 x 6.3032.210
    1 x 6.3032.250
    2.802.0020
    2.814.0030
    6.2041.310
    6.1432.320
    6.1115.000
    6.0262.100
    6.2104.020

    Titration Application Note T80


    Version 2

    Solutions
    Titrant

    c(Na2EDTA) = 0.05 mol/L

    Ammonium chloride
    (NH4Cl)
    Hydrochloric acid (HCl),
    conc.

    CAS 12125-02-9

    Nitric acid (HNO3),conc.


    Calconcarboxylic acid
    indicator solution
    (stable only one day!)
    w(sulfosalicylic acid)
    indicator solution
    Standard solution
    6.2301.070

    CAS 7697-37-2

    c(NaOH) = 2 mol/L
    c(NaOH) = 1 mol/L
    c(NaOH) = 0.1 mol/L
    Ammonium hydroxide
    Glycine

    Sample
    25 mL of the sample solution are pipetted into a sample
    beaker and diluted with dist. H2O to approx. 120 mL.
    Then, 0.5 g glycine and 1 mL of sulfosalicylic acid indicator are added. After adjustment to pH 1.5 with 25%
    NH4OH, the solution is heated to 50 C in a water bath
    to bring glycine into solution. After cooling to room
    temperature, the mixture is titrated with c(EDTA) = 0.05
    mol/L from reddish violet to faintly yellow.
    Parameters

    Titration mode
    Stirring rate
    Pause (s)
    Signal drift (mV/min)
    Min waiting time (s)
    Max waiting time (s)
    Volume increment (mL)
    EP criterion (mV)
    EP recognition
    Wavelength Optrode (nm)

    Titer/sample
    MET U
    8
    30
    50
    0
    26
    0.1
    30
    all
    610

    Calculations

    CAS 7647-01-0

    50 mg carboxylic acid in
    100 mL of c(NaOH) = 0.1
    mol/L.
    4 g in 100 mL dist. H2O
    c(CaCl2) = 0.1 mol/L
    Metrohm
    CAS 1310-73-2
    CAS 1310-73-2
    CAS 1310-73-2
    c(NH4OH) = 25%
    CAS 56-40-6

    VEP1
    c(EDTA)
    t
    500
    159.69
    100
    Sample size
    Sample vol.
    1000
    2

    Consumption of titrant in mL
    Concentration of titrant in mol/L
    Titer of the titrant (dimensionless)
    Dilution factor in mL (here 500 mL)
    Molecular weight of Fe2O3 in g/mol
    Calculation factor for %
    Weight of sample in g used to prepare the sample solution (here 2.5 g)
    Volume of sample solution used for
    the determination in mL
    Correction factor for L
    Stoichiometric factor

    Results
    Fe2O3 in %

    2.39 0.035 (n = 6)

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