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    4.2.09 AOAC of Fi Cial Method 984.13 Pro Tein (Crude) in An I Mal Feed and Pet Food

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    estefania
    This document provides the procedure for determining crude protein content in animal feed and pet food using the copper catalyst Kjeldahl method. Key steps include: (1) digesting the sample in sulfuric acid using copper sulfate as a catalyst to convert nitrogen to ammonia, (2) distilling the ammonia and titrating with an acid, (3) calculating the percentage of nitrogen and crude protein from these values using a conversion factor. The document specifies reagents, apparatus, and provides details on sample preparation, digestion, distillation, and titration steps.

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    4.2.09 AOAC of Fi Cial Method 984.13 Pro Tein (Crude) in An I Mal Feed and Pet Food

    Uploaded by

    estefania
    2K views1 page
    This document provides the procedure for determining crude protein content in animal feed and pet food using the copper catalyst Kjeldahl method. Key steps include: (1) digesting the sample in sulfuric acid using copper sulfate as a catalyst to convert nitrogen to ammonia, (2) distilling the ammonia and titrating with an acid, (3) calculating the percentage of nitrogen and crude protein from these values using a conversion factor. The document specifies reagents, apparatus, and provides details on sample preparation, digestion, distillation, and titration steps.

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    AOAC

    Original Title

    984.13

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    This document provides the procedure for determining crude protein content in animal feed and pet food using the copper catalyst Kjeldahl method. Key steps include: (1) digesting the sample in sulfuric acid using copper sulfate as a catalyst to convert nitrogen to ammonia, (2) distilling the ammonia and titrating with an acid, (3) calculating the percentage of nitrogen and crude protein from these values using a conversion factor. The document specifies reagents, apparatus, and provides details on sample preparation, digestion, distillation, and titration steps.

    Copyright:

    © All Rights Reserved
    Download as PDF, TXT or read online from Scribd
    Download as pdf or txt
    2K views1 page

    4.2.09 AOAC of Fi Cial Method 984.13 Pro Tein (Crude) in An I Mal Feed and Pet Food

    Uploaded by

    estefania
    This document provides the procedure for determining crude protein content in animal feed and pet food using the copper catalyst Kjeldahl method. Key steps include: (1) digesting the sample in sulfuric acid using copper sulfate as a catalyst to convert nitrogen to ammonia, (2) distilling the ammonia and titrating with an acid, (3) calculating the percentage of nitrogen and crude protein from these values using a conversion factor. The document specifies reagents, apparatus, and provides details on sample preparation, digestion, distillation, and titration steps.

    Copyright:

    © All Rights Reserved
    Download as PDF, TXT or read online from Scribd
    Download as pdf or txt
    of 1

    4.2.

    09 Heat flask at 5-min boil rate (burner preheated and adjusted to


    AOAC Official Method 984.13 bring 250 mL H2O at 25°C to rolling boil in 5 min) until dense
    Protein (Crude) in Animal Feed and Pet Food white fumes clear bulb of flask, swirl gently, continue heating
    Copper Catalyst Kjeldahl Method additional 90 min. (Note: Reagent proportions, heat input, and
    First Action 1984
    di ges tion time are crit i cal fac tors—do not change.) Cool,
    Final Action 1994
    cautiously add 250 mL H2O, and cool to room temperature.
    A. Principle (Note: If bumping occurs during distillation, volume of H2O may
    Sam ple is di gested in H 2 SO 4 , us ing CuSO 4 as cat a lyst, be increased to ca 275 mL.)
    converting N to NH3 which is distilled and titrated. Pre pare ti tra tion beaker by add ing ac cu rately mea sured
    B. Reagents appropriate volume standard acid solution to amount of H2O such
    (a) So dium hy drox ide.—Pel lets, flakes, or so lu tion with that condenser tip will be sufficiently immersed. Add 3–4 drops
    spe cific grav ity ≥1.36, low N. Dis solve ca 450 g NaOH in H 2O, indicator solution, B(c).
    cool, di lute to 1 L. Add 2–3 drops of tributyl citrate to digestion flask to re duce
    (b) Alundum.—Boiling stones, 8–14 mesh (Thomas foaming; add another 0.5–1.0 g alundum granules. Slowly, down
    Sci en tific Co., No. 1590-D18). side of flask, add sufficient NaOH solution, B(a), such that
    (c) Methyl red in di ca tor.—Dissolve 1 g methyl red (Na salt) mixture will be strongly alkaline. Immediately connect flask to
    in 100 mL metha nol.
    distillation apparatus, mix completely, and distil at ca 7.5 min
    (d) Hy dro chlo ric stan dard so lu tion.—0.5M, or sul fu ric acid
    boil rate until ≥150 mL distillate is collected in titration beaker.
    stan dard so lu tion, 0.25M. Pre pare as in 936.15 (see A.1.06) or
    Titrate excess standard acid in distillate with standard NaOH
    890.01 (see A.1.14).
    solution. Correct for blank determination on reagents. Calculate % N.
    (e) So dium hy drox ide stan dard so lu tion.—0.1M. Pre pare as
    When standard HCl is used:
    in 936.16 (see A.1.12).
    After standardizing both acid and base individually, also check
    N, % (w/w) = [(Macid)(mLacid ) – (mLbk)(MNaOH)
    one against the other. In ad dition, check en tire method by
    – (mLNaOH)(MNaOH)][1400.67]/mg test portion
    analyzing NIST Standard Reference Material No. 194, NH4H2PO4,
    certified 12.15% N, and high purity lysine⋅HCl. When standard H2SO4 is used:
    C. Apparatus
    (a) Digestion.—Use Kjeldahl flasks with capacity of 500–800 mL. N, % (w/w) = [(Macid)(2)(mLacid ) – (mLbk)(MNaOH)
    (b) Distillation.—Connect digestion flask to distillation trap by – (mLNaOH)(MNaOH)][1400.67]/mg test portion
    rubber stopper and connect distillation trap to condenser with low-S
    tubing. Outlet of condenser tube should be <4 mm diameter. where mL NaOH = mL standard base needed to titrate distillate;
    mLacid = mL standard acid used for that distillate; mLbk = mL
    D. Determination standard base needed to titrate 1 mL standard acid minus mL
    Weigh 0.250–1.000 g test portion into digestion flask. Add 15 g standard base needed to ti trate re agent blank car ried through
    K2SO4, 0.04 g anhy drous CuSO4, 0.5–1.0 g alundum granules, method and dis tilled into 1 mL stan dard acid; M acid = molarity
    and 20 mL H2SO4. (Add additional 1.0 mL H2SO4 for each 0.1 g of stan dard acid; M b a s e = molarity of stan dard base.
    fat or 0.2 g other organic matter if test portion weight is >1 g.) Cal cu late per cent crude pro tein, de fined as 6.25 × percent
    ni tro gen, or 5.7 × per cent ni tro gen for wheat grains.
    Include at least one assay of high purity lysine⋅HCl in each
    day’s run as check of correctness of digestion parameters. If Reference: JAOAC 67, 869(1984).
    recovery is not complete, make appropriate adjustments. Revised: March 1996

     2005 AOAC INTERNATIONAL

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