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    Isocyanate Content of U: Rethane

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    swapon kumar shill
    This document describes methods for measuring the isocyanate content of urethane samples using automatic potentiometric titration. The sample is dissolved in toluene and reacted with di-n-butylamine, then back-titrated with hydrochloric acid. The isocyanate content is calculated based on the titration volume. The method shows good repeatability of 0.25% relative standard deviation. Several automatic titration systems from Kyoto Electronics are recommended for precisely analyzing urethane samples.

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    Isocyanate Content of U: Rethane

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    swapon kumar shill
    139 views4 pages
    This document describes methods for measuring the isocyanate content of urethane samples using automatic potentiometric titration. The sample is dissolved in toluene and reacted with di-n-butylamine, then back-titrated with hydrochloric acid. The isocyanate content is calculated based on the titration volume. The method shows good repeatability of 0.25% relative standard deviation. Several automatic titration systems from Kyoto Electronics are recommended for precisely analyzing urethane samples.

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    ETII-98003NCO.pdf

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    This document describes methods for measuring the isocyanate content of urethane samples using automatic potentiometric titration. The sample is dissolved in toluene and reacted with di-n-butylamine, then back-titrated with hydrochloric acid. The isocyanate content is calculated based on the titration volume. The method shows good repeatability of 0.25% relative standard deviation. Several automatic titration systems from Kyoto Electronics are recommended for precisely analyzing urethane samples.

    Copyright:

    © All Rights Reserved
    Download as PDF, TXT or read online from Scribd
    Download as pdf or txt
    139 views4 pages

    Isocyanate Content of U: Rethane

    Uploaded by

    swapon kumar shill
    This document describes methods for measuring the isocyanate content of urethane samples using automatic potentiometric titration. The sample is dissolved in toluene and reacted with di-n-butylamine, then back-titrated with hydrochloric acid. The isocyanate content is calculated based on the titration volume. The method shows good repeatability of 0.25% relative standard deviation. Several automatic titration systems from Kyoto Electronics are recommended for precisely analyzing urethane samples.

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    © All Rights Reserved
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    Download as pdf or txt
    of 4

    Plastic, Rubber Isocyanate Content of Urethane

    Acidxbase titration by
    Automatic Potentiometric Titrator
    JIS K 7301 ISO 14896
    Standards JIS K 1603
    JIS K 1556

    1.Abstract
    Measurement of isocyanate content is standardized by the below quoted test
    methods.
    Sample liquid after dissolved in dry toluene reacts with excessive di-n-Butylamine,
    and back titrate residual di-n-Butylamine with hydrochloric acid up to the endpoint.
    The content of Isocyanate is calculated from titration volume.

    2.Reference
    1) JIS K 7301-1995 Test Method for Tri-range Isocyanic Prepolymer for
    Heat-curable Urethane Elastomer
    2) JIS K 1603-1985 Test Method for Polymethylene Polyphenyl Polyisocyanate
    3) JIS K 1556-2006 Test Method for Tolunediisocyanate － Polyurethane raw
    materials （Appendix １）
    4) ISO 14896-2006 Plastics -- Polyurethane raw materials -- Determination of
    isocyanate content

    3.Cautions in measurement
    1) Repeated measurement lowers sensitivity of glass electrode, and regeneration
    process of electrode is required each time a measurement is finished.
    To regenerate the electrode, dip it in solvent once for cleaning, and then in pure
    water for 10 to 60 min. (depends on how much contaminated)
    2) Handle chemicals in a well ventilated room or use a draft.
    3) Note that organic cyanate is harmful when its fume is absorbed through skin or
    inhaled. Wear protective gloves and glasses, and work in a well ventilated room.
    4) Isocyanate reacts with ambient moisture. Keep room humidity as low as possible,
    preferably below 50% RH.

    TII-98003 Ver.01 1/4


    4.Post-measurement care
    After a series of measurements for the day is over, be sure to regenerate the
    electrode according to the preceding “3. Cautions in measurement”.

    5.Test equipment
    Main unit：Automatic potentiometric titrator （Standard preamplifier STD－）
    Electrode： Option Combination glass electrode

    6.Reagent
    Titrant ： lmo1/L Hydrochloric acid （ｆ＝1.00）
    Solvent ： Dry Toluene + Isopropyl alcohol
    Reagent ： 2mol/L di-n-Butylamine

    7.Measurement procedure
    一Measurement―
    1) Prepare 3g sample in a 200mL conical flask.
    2) Add 20mL Toluene to dissolve the sample.
    3) Add 20mL of 2mol/L di-n-Butylamine.
    4) Shake to make it even, and leave it for more than 20 minutes.
    5) Add 100mL of Isopropyl alcohol.
    6) Titrate with lmo1/L Hydrochloric acid up to the endpoint.
    7) Likewise, perform blank test.

    8. Formula
    Isocyanate content = ( SIZE / ( ( BL1 － EP1 ) × FA1 ) ) × K2

    EP1 ： Titration volume ( mL )


    BL1 ： Blank level ( 39.888mL )
    FA1 ： Titant factor ( 1.00 )
    K2 ： Coefficient ( 1000 )
    SIZE ： Sample size ( g )

    TII-98003 Ver.01 2/4


    9.Example of measurement
    －Ambient condition－
    Room temperature：25 ℃ Humidity ： 41 ％ Weather ： Fair

    - Titration parameter - - Titration curve -


    Model : AT-400
    Method No. : 18
    Titr.mode : Auto
    Intermit
    Titr.form : EP Stop

    [CALCU. PARA]
    [TITR. PARA]
    Sample Measurement
    Form : EP Stop Conc1 CalcuNo. 7
    Buret No. : 1 Conc1 Dim. []
    Preamp : STD Conc1 EP Position 1
    Detector No. : 1 Data [f(EP2-EP1)]
    Dimension : pH T.Type [Back]
    Max.Vol : 60.0mL Data [f(T.Vol)]
    W.Time : 0s Local Blank
    Direction : Auto Blank 39.888mL
    Common T.Factor
    K2 1000
    [CTRL. PARA] Temp.Comp. [Off]

    End Point No. : 1


    S(dE) : 50
    S(E/mL) : 100
    O.Titr : 0mL
    Gain : 1
    S.Pot : 4.0mV
    Stab. : 0.5mV/s
    Delay Time : 1s
    L.Time : 30s
    M.Unit : 0.5mL
    Separation : Off
    A.Simulation : Off

    (The above printout data were obtained from titration by AT-400)


    ≪TITR. PARA: titration parameter≫
    Form: of titration/ Buret No.: the burette used in titration / Detector No.: the detector used in titration
    Dimension: potential unit / Max.Vol: of titration / W.Time: before titration starts
    Direction: of titration
    ≪CTRL. PARA: control parameter≫
    End Point No.: number of EPs / S(dE): EP potential (difference) / S(E/mL): EP potential (differential)
    O.Titr: over-titration / Gain: sensitivity of detection signal /S.Pot.: potential change of sampling signal
    Stability: of EP potential / Delay Time: before stability check / Limit Time: of stability check
    M.Unit: titration volume of data sampling / Separation: of potential / A.Simulation: redetection of EP
    ≪CALCU. PARA: calculation parameter≫
    Conc.1 formula 1 /Conc1 Dim. Unit of conc 1/ Data: calculation formula of titration volume
    T.Type: normal or back titration / Blank: blank level/Common T.Factor: selection of factor
    Temp.Comp.: temperature compensation / C1(mg/mL): concentration conversion at EP1
    K2: unit conversion coefficient / Conc1 EP Position: EP position at concentration 1

    TII-98003 Ver.01 3/4


    －Measurement results－
    Sample Titration Isocyanate
    n Statistics of results
    (g) (mL) content
    1 3.0793 23.2391 184.96 Mean 185.41
    2 3.0545 23.4141 185.41 SD 0.46
    3 3.0105 23.6911 185.87 RSD 0.25 %
    ＊The above results were obtained by 3 tests of the same sample.
    ＊ Red underline shows the data from page 3/4.

    10.Summary
    Urethane is dehydrated compound of amino group and alcohol group via carbonyl,
    and Ethyl carbamate or Polyurethane (Urethane resin) is popularly called Uretahne.
    The chemical compound Isocyanate having chemical structure of −N=C=O is also
    called Isocyanic ester, which is important material for polyurethane.
    The above sample test shows a good repeatability of 0.25% relative standard
    deviation as the automated potentiometry is the most reliable measurement
    technique.
    The analysis of urethane can be easily and precisely made by any of the following
    titration systems manufactured by Kyoto Electronics (KEM).

    【AT-610】 【AT-510】 【AT-500N-1】

    Awarded Product of Supreme • Compact and cost performance • Low cost and high performance
    Technology from Kyoto City model • Easy view with back light LCD
    • Easy key entry by touch panel of • PC card expands data memory for • GLP/GMP conformed model
    large color LCD （8-inch wide） convenience and versatility.
    • Simultaneous titration in parallel
    • Both potentiometric and Karl
    Fischer moisture titration
    (coulometric・volumetric） can be
    performed at a time.

    TII-98003 Ver.01 4/4

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