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    Metrohm - Application Work AW IC CH6-1136-112012

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    Metrohm - Application Work AW IC CH6-1136-112012

    Uploaded by

    Alaa Noureldeen
    28 views4 pages

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    © © All Rights Reserved

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    28 views4 pages

    Metrohm - Application Work AW IC CH6-1136-112012

    Uploaded by

    Alaa Noureldeen

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    © All Rights Reserved
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    of 4

    Application Work AW IC CH6-1136-112012

    Cyanide and sulfide analysis using amperometric detection and


    Metrosep A Supp 10 - 100/2.0

    Branch Reagents
    Food, stimulants, beverages, general analytical chemistry Sulfide standard, Na2S, 32 – 38 %, CAS 27610-45-3,
    Fluka 719751
    Keywords
    Potassium cyanide, KCN puriss. p.a ≥ 98%, CAS 151-
    IC; 850; 858; Metrosep A Supp 10 - 100/2.0; Cyanide;
    Sulfide; 2.850.9110; DC Mode; Ag WE; Pd Ref.; branch 1; 50-8, Fluka 60179
    ®,
    branch 7 Sodium hydroxide, NaOH, ≥ 30% TraceSELECT
    Summary CAS 1310-73-2, Fluka 13171-250ML-F

    The determination of sulfide and cyanide in tap water was Ethylenediaminetetraacetic acid disodium salt,
    investigated on the Metrosep A Supp 10 - 100/2.0 column [-CH2N(CH2CO2Na)CH2CO2H]2, 0.2 mol/L,
    using sodium hydroxide eluent and amperometric detector. CAS 139-33-3, Fluka 35102
    Ultrapure water, resistivity >18 MΩ·cm (25 °C),
    Samples
    type I grade (ASTM D1193)
    Spiked Herisau tap water.

    Solutions
    Instruments
    Eluent 100 mmol/L sodium hydroxide in
    881 Compact IC pro – Cation 2.881.0010 carbon dioxide free ultrapure
    water (resistivity >18 M )
    858 Professional Sample Processor 2.858.0020
    +0.007 mmol/L EDTA
    IC Amperometric Detector 2.850.9110 in ultra pure water (resistivity
    Wall - Jet Cell 6.1257.010 >18 M )
    Spacer 25 µm 6.1257.840 Standard solutions
    Ag Working Electrode 6.1257.240 For the 1000 ppm sulfide standard 695 mg of Sodium
    Pd Reference Electrode 6.1257.740 sulfide was diluted in a 100 mL flask with 100 mmol/L
    Metrosep A Supp 10 - 100/2.0 6.1020.210 sodium hydroxide (= 1000 ppm).
    Metrosep A Supp 10 Guard/2.0 6.1020.600
    The diluted cyanide and sulfide standards were dissolved in
    100 mmol/L sodium hydroxide.

    Concentration of cyanide and sulfide standards.


    β [µg/L] Sulfide Cyanide
    Std. 1 0.05 0.05
    Std. 2 0.10 0.10
    Std. 3 0.25 0.25
    Std. 4 0.50 0.50
    Std. 5 1.0 1.0
    Std. 6 2.0 2.0
    Std. 7 4.0 4.0
    Std. 8 8.0 8.0
    Std. 9 10.0 10.0

    Page 1 of 4
    Application Work AW IC CH6-1136-112012
    Cyanide and sulfide analysis using amperometric detection and
    Metrosep A Supp 10 - 100/2.0

    Sample preparation
    No sample preparation was required. Date
    21st of November, 2012

    Analysis
    The samples and standards were injected with the 858 Author
    Professional Sample Processor. Gabriele Zierfels
    Competence Center Ion Chromatography
    Parameters Metrohm International Headquarters

    Flow 0.25 mL/min


    Mode DC Appendix
    Result chromatograms with peak table, calibration curves.
    Cell potential 0.0 V
    Range Auto
    Channel current
    Column temperature 35 °C
    Detector temperature 35 °C
    Injection volume 20 µL

    Calculation
    Automatic integration with MagIC Net 2.3 software using
    peak area.

    Results
    Recovery of sulfide and cyanide was tested with Herisau tap
    water. The water was spiked with 8 ppb cyanide and sulfide.
    Additional 1 mL sodium hydroxide per 100 mL volume
    was added (= 100 mmol/L NaOH), then the flask was filled
    up.

    Conc. [µg/L] Mean (3) % RSD


    Cyanide 8.03 1.78
    Sulfide 5.93 1.74

    Comments
    Only before the first usage only, the column needs a
    pretreatment.
    It should be rinsed with 50 mmol/L EDTA solution with
    standard flow for 3 h, followed by conditioning with the
    eluent for 12 h. This ensured optimal measuring conditions.
    The EDTA concentration in the eluent depends on the
    column. EDTA pushes the sulfide and cyanide peaks on the
    A Supp 10 to the front of the chromatogram, while the
    system peak doesn`t move. In this case the correct
    concentration of EDTA helped to separate the sulfide from
    the system peak.

    Page 2 of 4
    Application Work AW IC CH6-1136-112012
    Cyanide and sulfide analysis using amperometric detection and
    Metrosep A Supp 10 - 100/2.0

    Appendix
    Standard 2 (the peak at 3.2 min is the system peak)

    Standard 7

    Page 3 of 4
    Application Work AW IC CH6-1136-112012
    Cyanide and sulfide analysis using amperometric detection and
    Metrosep A Supp 10 - 100/2.0

    Calibration curves:

    Page 4 of 4

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