Commission Directive 1999/79/EC of 27 July 1999 amending the third Commission Directive 72/199/EEC of 27 April 1972 establishing Community methods of analysis for the official control of feedingstuffs (Text with EEA relevance)
Date: 1999-07-27
Institutions: European Commission
Subjects: analytical chemistry, animal nutrition, manufactured feedingstuffs, poultry

7. 8. 1999

EN

Official Journal of the European Communities

L 209/23

COMMISSION DIRECTIVE 1999/79/EC

of 27 July 1999

amending the third Commission Directive 72/199/EEC of 27 April 1972 establishing Community
methods of analysis for the official control of feedingstuffs

(Text with EEA relevance)

THE COMMISSION OF THE EUROPEAN COMMUNITIES,

Having regard to the Treaty establishing the European
Community,

Having regard to Council Directive 70/373/EEC of 20 July
1970 on the introduction of Community methods of sampling
and analysis for the official control of feedingstuffs (1), as last
amended by the Act of Accession of Austria, Finland and
Sweden (2), and in particular Article 2 thereof,

(1) Whereas Directive 70/373/EEC stipulates that official
controls of feedingstuffs for the purpose of checking
compliance with the requirements arising under the
laws,
provisions
governing their quality and composition must be carried
out using Community methods of
sampling and
analysis;

administrative

regulations

and

(2) Whereas the third Commission Directive 72/199/EEC of
27 April 1972 establishing Community methods of
analysis for the official control of feedingstuffs (3), as last
amended by Commission Directive 98/54/EC (4), sets out
methods of analysis for, inter alia, the determination of
starch by polarimetric method;

(3) Whereas Commission Directive 86/174/EEC of 9 April
1986 fixing the method of calculation for the energy
value of compound poultryfeed (5), stipulates that for the
calculation of the energy value of compound poultry
feed,
in application of Article 10 Council Directive
79/373/EEC of 2 April 1979 on the marketing of
compound feedingstuffs (6), as last amended by Commis-
sion Directive 1999/61/EC (7), the starch content must
be determined by the polarimetric method as set out in
Commission Directive 72/199/EEC;

(4) Whereas Council Directive 96/25/EC of 29 April 1996
on the circulation of feed materials, amending Directives
70/524/EEC, 74/63/EEC, 82/471/EEC and 93/74/EEC

(1) OJ L 170, 3.8.1970, p. 2.
(2) OJ C 241, 29.8.1994, p. 1.
(3) OJ L 123, 29.5.1972, p. 6.
(4) OJ L 208, 24.7.1998, p. 49.
(5) OJ L 130, 16.5.1986, p. 53.
(6) OJ L 86, 6.4.1979, p. 30.
(7) OJ L 162, 26.6.1999, p. 67.

and repealing Directive 77/101/EEC (8) as last amended
by Directive 1999/61/EC requires the quantities of some
analytical constituents, including starch, to be compul-
sorily declared on some feed materials;

(5) Whereas in the light of the advances of scientific and
technological knowledge, the polarimetric method is no
longer appropriate to determine the starch content for
other purposes than those of
the above mentioned
Commission and Council Directives; whereas therefore it
is appropriate to limit the purpose and scope of the
polarimetric method for the determination of starch;

(6) Whereas some feed materials give rise to interferences,
whereby the polarimetric method for the determination
of starch could yield false results; whereas it is therefore
appropriate to mention these feed materials explicitly;

(7) Whereas the measures provided for in this Directive are
the Standing

in accordance with the opinion of
Committee for Feedingstuffs,

HAS ADOPTED THIS DIRECTIVE:

Article 1

Annex I
amended in accordance with the Annex to this Directive.

to Commission Directive 72/199/EEC is hereby

Article 2

Member States shall bring into force, not
than 31
December 1999, the laws, regulations or administrative provi-
sions necessary to comply with the provisions of this Directive.
They shall

immediately inform the Commission thereof.

later

They shall apply the measures from 1 January 2000.

When Member States adopt these measures, they shall contain
a reference to this Directive or shall be accompanied by such
reference at
their official publication. Member
States shall adopt the procedure for such reference.

the time of

(8) OJ L 125, 23.5.1996, p. 35.

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7. 8. 1999

This Directive shall enter into force on the 20th day following its publication in the Official Journal of the
European Communities.

Article 3

This Directive is addressed to the Member States.

Article 4

Done at Brussels, 27 July 1999.

For the Commission

Franz FISCHLER

Member of the Commission

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Official Journal of the European Communities

L 209/25

Section 1 (Determinination of starch) is replaced by the following:

ANNEX

‘1. DETERMINATION OF STARCH

POLARIMETRIC METHOD

1.

Purpose and scope

This method makes it possible to determine the levels of starch and of high molecular weight starch degradation
products in feedingstuffs for the purpose of checking compliance with Commission Directive 86/174/EEC and
Council Directive 96/25/EC.

2.

Principle

The method comprises two determinations. In the first, the sample is treated when hot with dilute hydrochloric acid.
After clarification and filtration the optical rotation of the solution is measured by polarimetry.

In the second, the sample is extracted with 40 % ethanol. After acidifying the filtrate with hydrochloric acid,
clarifying and filtering, the optical rotation is measured as in the first determination.

The difference between the two measurements, multiplied by a known factor, gives the starch content of the sample.

3.

Reagents

3.1. 25 % (w/w) hydrochloric acid, d: 1,126 g/ml.

3.2. 1,128 % (w/v) hydrochloric acid.

The concentration must be checked by titration using a sodium hydroxide solution 0,1 mol/litre in the presence of
0,1 % (w/v) methyl red in 94 % (v/v) ethanol. 10 ml = 30.94 ml of NaOH 0.1 mol/lite.

3.3. Carrez solution I: dissolve 21,9 g of zinc acetate Zn(CH3

COO)
2

.2H
2

O and 3 g of glacial acetic acid in water. Make

up to 100 ml with water.

3.4. Carrez solution II: dissolve 10,6 g of potassium ferrocyanide [K4

(Fe(CN)

].3H
6

O in water. Make up to 100 ml with
2

water.

3.5. 40 % (v/v) ethanol, d : 0,948 g/ml at 20 °C.

4. Apparatus

4.1. 250 ml erlenmeyer flask with standard ground-glass joint and with reflux condenser.

4.2. Polarimeter or saccharimeter.

5.

Procedure

5.1. Preparation of the sample

Crush the sample until

it is fine enough for all of it to pass through a 0,5 mm round-meshed sieve.

5.2. Determination of the total optical rotation (P or S) (see observation 7.1)

Weigh 2,5 g of the crushed sample to the nearest mg and place in a 100 ml graduated flask. Add 25 ml of
hydrochloric acid (3.2), shake to obtain even distribution of the test sample and add a further 25 ml of hydrochloric
acid (3.2). Immerse the flask in a boiling water bath shaking vigorously and steadily for the first three minutes to
prevent the formation of agglomerates. The quantity of water in the water bath must be sufficient for the bath to
remain at boiling point when the flask is introduced into it. The flask must not be taken out of the bath whilst being
shaken. After exactly 15 minutes, remove from the bath, add 30 ml of cold water and cool immediately to 20 °C.

Add 5 ml of Carrez solution I (3.3) and shake for one minute. Then add 5 ml of Carrez solution II (3.4) and shake
again for one minute. Make up to volume with water, mix and filter. If the filtrate is not perfectly clear (which is
rare), repeat the determination using a larger quantity of Carrez solutions I and II, for example 10 ml.

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Measure the optical rotation of the solution in a 200 mm tube with the polarimeter or saccharimeter.

5.3. Determination of the optical rotation (P' or S') of substances soluble in 40 % ethanol

Weigh 5 g of the sample to the nearest mg, place in a 100 ml graduated flask and add about 80 ml of ethanol
(3.5) (see observation 7.2). Leave the flask to stand for 1 hour at room temperature; during this time, shake
vigorously on six occasions so that the test sample is thoroughly mixed with the ethanol. Make up to volume with
ethanol (3.5), mix and filter. Pipette 50 ml of the filtrate (= 2,5 g of the sample ) into a 250 ml erlenmeyer flask,
add 2,1 ml of hydrochloric acid (3.1) and shake vigorously. Fit a reflux condenser to the erlenmeyer flask and
immerse the latter in a boiling water bath. After exactly 15 minutes, remove the erlenmeyer flask from the bath,
transfer the contents to a 100 ml graduated flask, rinsing with a little cold water, and cool to 20 °C. Clarify using
Carrez solutions I (3.3) and II (3.4), make up to volume with water, mix, filter and measure the optical rotation as
indicated in the second and third paragraphs of 5.2.

6.

Calculation of results

The starch content (%) is calculated as following:

6.1. Measurement by polarimeter

Starch content (%) =

2000 (P - P(cid:1))
[α] D

20°

P
P(cid:1)

= total optical rotation in angle degrees
= optical rotation in angle degrees of the substances soluble in 40 % (V/V) ethanol

[α] D

20° = specific optical rotation of pure starch. The numerical values conventionally accepted for factor are the

following

+ 185.9°: rice starch
+ 185.4°: potato starch
+ 184.6°: maize starch
+ 182.7°: wheat starch
+ 181.5°: barley starch
+ 181.3°: oat starch
+ 184.0°: other types of starch and starch mixtures in compound feedingstuffs

6.2. Measurement by saccharimeter

Starch content (%) =

2000
[α] D

20° ×

(2N × 0,665) × (S - S(cid:1))
100

–

26,6 N × (S - S(cid:1))
20°
[α] D

S
S(cid:1)
N

= total optical rotation in saccharimeter degrees
= optical rotation in saccharimeter degrees of the substances soluble in 40 % (V/V) ethanol
= weight (g) of saccharose in 100 ml of water yielding an optical rotation of 100 saccharimeter degrees

when measured using a 200 mm tube

16,29 g for the French saccharimeters

26,00 g for the German saccharimeters

20,00 g for mixed saccharimeters.

[α] D

20° = specific optical rotation of pure starch (see 6.1)

6.3. Repeatability

The difference between the results of two parallel determinations carried out on the same sample must not exceed
0,4 in absolute value for a starch content lower than 40 % and 1,1 % relative for starch contents equal or higher
than 40 %

7. Observations

7.1.

7.2.

If the sample contains more than 6 % of carbonates, calculated in terms of calcium carbonate, they must be
destroyed by treatment with an exactly appropriate quantity of dilute sulphuric acid before determination of the
total optical rotation.

In the case of products with a high lactose content, such as powdered milk serum or skimmed milk powder, proceed
as follows after adding 80 ml of ethanol (3.5). Fit a reflux condenser to the flask and immerse the latter in a water
bath at 50 °C for 30 minutes. Leave to cool and continue the analysis as indicated in 5.3.

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7.3. Following feed materials, in case they are present in significant amount in feedingstuffs, are known to give rise to
interferences when determining the starch content by polarimetric method and whereby incorrect results could be
yielded:

— (sugar) beet products such as (sugar) beet pulp, (sugar) beet molasses, (sugar) beet pulp-molassed, (sugar) beet

vinasse, (beet) sugar,

— citrus pulp,

— linseed;

linseed expeller;

linseed extracted,

— rape seed; rape seed expeller; rape seed extracted; rape seed hulls,

— sunflower seed; sunflower seed extracted; sunflower seed, partially decorticated, extracted,

— copra expeller; copra extracted,

— potato pulp,

— dehydrated yeast,

— products rich in inulin (e.g. chips and meal of Jerusalem artichokes);

— greaves.’