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GB/T 6432-2018Determination of crude protein in feeds—Kjeldahl method (English PDF)

饲料中粗蛋白的测定 凯氏定氮法

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Issued by

SAMR; SAC

Level / Type

National · Recommended

Issue date

September 17, 2018

Implementation date

April 1, 2019

Scope

GB/T 6432-2018 is the English-translated version of 饲料中粗蛋白的测定 凯氏定氮法.

GB/T 6432-2018 is the Chinese national Kjeldahl method for determining the crude protein content of feeds.

The sample is digested with sulfuric acid in the presence of a catalyst so that its nitrogen compounds turn into ammonium sulfate; the ammonia freed by adding alkali is distilled, absorbed in boric acid and titrated with a hydrochloric acid standard solution.

The standard lists the reagents and instruments, sampling and reduction by quartering, and two procedures, a semi-micro method used for arbitration and a full-volume method, with a check of the distillation step on ammonium sulfate, a blank determination with sucrose, the calculation of the result and the precision requirements.

It applies to feed raw materials, compound feeds, concentrated feeds, concentrate supplements and additive premixes. It replaces GB/T 6432-1994, was issued on 17 September 2018 and has applied since 1 April 2019.

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Document preview — GB/T 6432-2018

National Standard of the People's Republic of China

ICS
65.120
Classification
B 46
Replacing
GB/T 6432-1994

Issued by: State Administration for Market Regulation; Standardization Administration of the PRC

Contents

  • Foreword3
  • 1 Scope4
  • 2 Normative references4
  • 3 Principle4
  • 4 Reagents or materials4
  • 5 Instruments and equipment5
  • 6 Sample6
  • 7 Test steps6
  • 8 Test data processing8
  • 9 Precision9

Foreword

This Standard was drafted in accordance with the rules given in GB/T 1.1-2009.

This Standard replaces GB/T 6432-1994 Method for the determination of crude protein in feedstuffs.

Compared with GB/T 6432-1994, the main technical changes, except editorial changes, are as follows.

-- Modify the standard name (see cover);

-- Modify the scope of application (see Chapter 1);

-- Add provisions on significant figures of calculation results (see Chapter 8).

1 Scope

This Standard specifies the Kjeldahl method for the determination of crude protein in feeds.

This Standard applies to the determination of crude protein in feed raw materials, compound feeds, concentrated feeds, concentrate supplements and additive premixed feeds.

2 Normative references

The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies to this document. For undated references, the latest edition (including any amendment) applies to this document.

GB/T 601, Chemical reagent - Preparations of reference titration solutions

GB/T 6682, Water for analytical laboratory use - Specification and test methods

GB/T 14699.1, Feeding stuffs - Sampling

GB/T 20195, Animal feeding stuffs - Preparation of test samples

3 Principle

The sample is digested by sulfuric acid under the action of the catalyst, and the nitrogen-containing compound is converted into ammonium sulfate. Add alkali to distill to make ammonia escape;

4 Reagents or materials

Unless otherwise stated, only use analytical reagents.

4.1 Water. GB/T 6682, grade 3.

4.2 Boric acid. chemical pure.

4.3 Sodium hydroxide. chemical pure.

4.4 Sulfuric acid. chemical pure.

4.5 Ammonium sulfate.

4.11 Hydrochloric acid standard titration solution. c(HCl) = 0.1 mol/L or 0.02 mol/L, prepared and calibrated according to GB/T 601.

4.12 Methyl red ethanol solution. Weigh 0.1 g of methyl red; use ethanol to dissolve and dilute to 100 mL.

4.13 Bromocresol green ethanol solution. Weigh 0.5 g of bromocresol green; use ethanol to dissolve and dilute to 100 mL.

5 Instruments and equipment

5.1 Analytical balance. sensitivity 0.000 1g.

5.2 Boiling sterilizer or electric furnace.

5.3 Kjeldahl flask. 250 mL.

5.4 Boiling and sterilization tube. 250 mL.

6 Sample

Take representative feed samples according to GB/T 14699.1; use the quartering method to reduce the sampling.

7 Test steps

7.1 Semi-micro method (arbitration method)

7.1.1 Sample boiling and sterilization
7.1.1.1 Kjeldahl flask boiling and sterilization

Perform two tests in parallel. Weigh 0.5 g ~ 2 g of the sample (nitrogen content 5 mg ~ 80 mg, accurate to 0.000 1 g);

7.1.2 Distillation of ammonia

After the boiled-and-sterilized solution of the sample is cooled, add 20 mL of water; transfer it to a 100 mL volumetric flask; after cooling, use water to dilute to the mark; shake well; use it as the sample decomposition solution. Immerse the end of the condenser tube of the semi-micro distillation device into the Erlenmeyer flask filled with 20 mL of boric acid absorption solution I (4.8) and 2 drops of mixed indicator (4.14).

7.1.3 Titration

Immediately use 0.1 mol/L or 0.02 mol/L of hydrochloric acid standard titration solution (4.11) to titrate the absorption solution after distillation in 7.1.2. The solution changes from blue-green to gray-red as the titration end point.

7.2 Full volume method

7.2.1 Sample boiling and sterilization

Follow the steps in 7.1.1.

7.2.2 Distillation of ammonia

7.2.2.3 When using an automatic Kjeldahl nitrogen analyzer, carry out the measurement according to the instrument operation manual.

7.2.3 Titration

Use 0.1 mol/L hydrochloric acid standard titration solution (4.11) to titrate the absorption solution. The solution changes from blue-green to gray-red as the end point.

7.3 Distillation step verification

Accurately weigh 0.2 g of ammonium sulfate (accurate to 0.000 1 g), to replace the sample; operate according to the steps in 7.1 or 7.2. The measured nitrogen content of ammonium sulfate shall be (21.19±0.2) %. Otherwise, check whether the steps of the addition of alkali, distillation and titration are correct.

7.4 Blank determination

Accurately weigh 0.5 g of sucrose (accurate to 0.000 1 g), to replace the sample; carry out blank determination according to 7.1 or 7.2.

8 Test data processing

The crude protein content in the sample is expressed in mass fraction w, and the value is expressed in mass fraction (%), and calculated according to Formula (1).

9 Precision

Under repeatability conditions, the ratio of the absolute difference between two independent measurement results and their arithmetic mean TO the mean shall meet the following requirements. […]

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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 15 pages — is available in the English PDF.

Referenced standards

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Editions of GB/T 6432

EditionTitleRevisionStatus
GB/T 6432-2018Determination of crude protein in feeds—Kjeldahl methodcurrent editionCurrent
GB/T 6432-1994Determination of crude protein in feeds—Kjeldahl methodprevious editionSuperseded

This page sells the current edition, GB/T 6432-2018. Earlier editions are listed for reference only.

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