Commission Regulation (EC) No 2799/1999 of 17 December 1999 laying down detailed rules for applying Regulation (EC) No 1255/1999 as regards the grant of aid for skimmed milk and skimmed-milk powder intended for animal feed and the sale of such skimmed-milk powder
Date: 1999-12-17
Institutions: European Commission
Subjects: EU aid, animal feedingstuffs, award of contract, butter, eligibility criteria, invitation to tender, production aid, skimmed milk, skimmed milk powder

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COMMISSION REGULATION (EC) No 2799/1999

of 17 December 1999

laying down detailed rules for applying Regulation (EC) No 1255/1999 as regards the grant of aid
for skimmed milk and skimmed-milk powder intended for animal feed and the sale of such
skimmed-milk powder

THE COMMISSION OF THE EUROPEAN COMMUNITIES,

(3)

Having regard to the Treaty establishing the European
Community,

Having regard to Council Regulation (EC) No 1255/1999 of 17
May 1999 on the common organisation of the market in milk
and milk products (1), and in particular Articles 10 and 15
thereof,

Whereas:

(1)

feed (4), as

for use as

Regulation (EC) No 1255/1999 replaces Council Regula-
tion (EEC) No 804/68 (2), as last amended by Regulation
(EC) No 1587/96 (3), and, among others, Council Regu-
lation (EEC) No 986/68 of 15 July 1968 laying down
general rules for granting aid for skimmed milk and
skimmed-milk powder
last
amended by Commission Regulation (EC) No 1802/
95 (5). To take account of the new arrangements and of
past experience, Commission Regulation (EEC) No 1725/
79 of 26 July 1979 on the rules for granting aid to
skimmed milk processed into compound feedingstuffs
and skimmed-milk powder
feed for
calves (6), as last amended by Regulation (EC) No 83/
96 (7), should be amended and, where necessary, simpli-
fied. At the same time as amending that Regulation, in
the interests of clarity, it should also be recast to incor-
porate Commission Regulations (EEC) No 3398/91 of
20 November 1991 on the sale by invitation to tender
of
the manufacture of
compound feedingstuffs and amending Regulation (EEC)
No 569/88 (8), as last amended by Regulation (EC) No
124/1999 (9), and (EEC) No 1634/85 of 17 June 1985
fixing the amount of the aid for skimmed milk and
skimmed-milk powder
last
amended by Regulation (EEC) No 1802/95;

skimmed-milk powder

intended for

feed (10), as

for use as

for

(2)

the goal of the aid measure provided for in Article 11 of
Regulation (EC) No 1255/1999 is to enable the best
return to be obtained from milk proteins. It is therefore
appropriate to link payment of the aid to the milk-
protein content of the skimmed milk or skimmed-milk
powder used;

(1) OJ L 160, 26.6.1999, p. 48.
(2) OJ L 148, 28.6.1968, p. 13.
(3) OJ L 206, 16.8.1996, p. 21.
(4) OJ L 169, 18.7.1968, p. 4.
(5) OJ L 174, 26.7.1995, p. 27.
(6) OJ L 199, 7.8.1979, p. 1.
(7) OJ L 17, 23.1.1996, p. 3.
(8) OJ L 320, 22.11.1991, p. 16.
(9) OJ L 16, 21.1.1999, p. 19.
(10) OJ L 158, 18.6.1985, p. 7.

it is necessary to ensure that the skimmed milk and
skimmed-milk powder for which aid is granted are in
fact used as feed. To that end, aid should be granted
only for skimmed milk and skimmed-milk powder
processed into compound feedingstuffs or denatured in
accordance with certain requirements. It is also neces-
sary to prevent aid being paid more than once for the
same product;

Commission Regulation (EC) No 1043/97 (11) derogates
from some of the monitoring provisions in Regulation
(EEC) No 1725/79. The checks provided for in this
Regulation should take that derogation into account and
Regulation (EC) No 1043/97 should be repealed;

aid should be granted only if the compound feeding-
regards
stuffs meet certain minimum standards as
composition customarily observed in the industry and if
they have reached the final stage of industrial manufac-
ture. For inspection purposes, the products should be
packaged in a way that enables them to be identified.
Member States should be allowed to specify how the
above requirements are to be satisfied;

special packing is not necessary for compound feeding-
stuffs which have had lucerne meal added to them.
Furthermore, such a requirement would not be appro-
priate in cases of transportation by tanker or container
as practised by certain users. That method of transport
should therefore be subject to special inspection arrange-
ments and aid should be paid only after inspection;

the final use of cut-price skimmed milk and skimmed-
milk powder can be monitored only if the undertakings
benefiting from aid offer adequate guarantees. Processing
undertakings should be approved by the competent
agency of the Member State concerned and have an
accounting system adapted to the requirements of the
aid arrangements;

as regards the reference methods applicable to the
analyses provided for in this aid scheme, reference
should be made to the list published each year under
Commission Regulation (EC) No 2721/95 of 24
November 1995 establishing rules for the application of
reference and routine methods for the analysis and
quality evaluation of milk and milk products under the

(4)

(5)

(6)

(7)

(8)

(11) OJ L 152, 11.6.1997, p. 6.

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(9)

(10)

(11)

common market organisation (1). However, since no
reference methods have been laid down for determining
the quantity of skimmed-milk powder in compound
feedingstuffs, the presence of rennet whey powder in
skimmed-milk powder or
starch in
skimmed-milk powder, the appropriate methods should
be laid down in this Regulation;

the quality of

HAS ADOPTED THIS REGULATION:

CHAPTER I

GENERAL PROVISIONS

Article 1

a standing invitation to tender should be organised for
the sale of skimmed-milk powder from public stocks, in
order to ensure equality of access for all potential
purchasers, to arrive at a selling price reflecting market
conditions and to verify the actual end use of skimmed-
milk powder intended for use in the manufacture of
compound feedingstuffs. The prices offered can differ
considerably according, in particular, to the age of the
powder offered for sale and its location. It should there-
fore be possible to fix differentiated minimum prices;

This Regulation lays down detailed rules for applying Regula-
tion (EC) No 1255/1999 as regards:

(a) the grant of aid for skimmed milk, skimmed-milk powder,
buttermilk and buttermilk powder intended for use as
animal feed under Article 11 of that Regulation;

(b) the sale of skimmed-milk powder intended for use as

animal feed under Article 7(4) of that Regulation.

this Regulation should set the time limit for entry into
storage for the purposes of sale. Commission Regulation
(EEC) No 3536/91 of 2 December 1991 setting the
latest
time of entry into storage for skimmed-milk
powder sold under Regulation (EEC) No 3398/91 (2), as
last amended by Regulation (EC) No 2508/1999 (3),
should therefore be repealed;

the arrangements laid down in Commission Regulation
(EEC) No 1105/68 of 27 July 1968 on detailed rules for
granting aid for skimmed milk for use as feed (4), as last
amended by Regulation (EEC) No 1802/95, have proved
difficult to implement and checks on beneficiaries are
problematic. Moreover, the quantities of skimmed milk
benefiting from this measure have fallen sharply in
the scheme now has only a
recent years, so that
marginal impact on the balance on the market in milk
products. In addition, the market in skimmed milk will
continue to be supported by the aid granted when
skimmed milk is incorporated into compound feeding-
stuffs. The aid measure provided for in Regulation (EEC)
No 1105/68 should therefore be abolished and the said
Regulation repealed;

Article 2

For the purposes of this Regulation:

(a) ‘Milk’ means the product obtained from milking one or
more cows, to which nothing has been added and which
has at most been only partially skimmed;

(b) ‘Skimmed milk’ means milk with a fat content of no more
than 1 % and a protein content of not less than 31,4 % of
the non-fatty dry extract;

(c) ‘Skimmed-milk powder’ means the product obtained by
removing the water from milk, with a maximum fat
content of 11 %, a maximum moisture content of 5 % and
a protein content of not less than 31,4 % of the non-fatty
dry extract;

(d) ‘Buttermilk’ means the by-product of butter manufacture
obtained after churning the cream and separating the solid
fat, with a maximum fat content of 1 % and a protein
content of not less than 31,4 % of the non-fatty dry extract;

(e) ‘Buttermilk powder’ means

the product obtained by
removing the water from buttermilk, with a maximum fat
content of 11 %, a maximum moisture content of 5 % and
a protein content of not less than 31,4 % of the non-fatty
dry extract.

Article 3

For the purposes of applying this Regulation, buttermilk and
buttermilk powder shall be treated as skimmed milk and
skimmed-milk powder, respectively.

(12)

the Management Committee for Milk and Milk Products
has not delivered an opinion within the time limit set by
its chairman,

Article 4

(1) OJ L 283, 25.11.1995, p. 7.
(2) OJ L 335, 6.12.1991, p. 8.
(3) OJ L 304, 27.11.1999, p. 21.
(4) OJ L 184, 29.6.1968, p. 24.

‘Mixtures intended for the manufacture of compound feeding-
stuffs’ (hereinafter called ‘mixtures’) means products containing
the following ingredients:

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(a) skimmed-milk powder;

and

(b) fat;

(c) vitamins;

(d) minerals;

(e) sucrose;

(f) anti-caking agents and/or free-flowing agents (maximum

0,3 %);

(g) other liposoluble technical agents, including anti-oxidants

and emulsifiers.

Article 5

1.

‘Compound feedingstuffs’ means products:

(a) which contain, per 100 kilograms of finished product,

(i) not less than 50 kilograms and not more than 80

kilograms of skimmed-milk powder,

and

(ii) not less than 5 kilograms of non-butter fats and at

least 2 kilograms of starch or puffed starch,

or

(iii) not less than 2,5 kilograms of non-butter fats and at
least 2 kilograms of starch or puffed starch in cases
where 5 kilograms of
lucerne meal or grass meal
containing at
least 50 % (m/m) of particles not
exceeding 300 microns are incorporated per 100 kilo-
grams of skimmed-milk powder. The particles not
exceeding 300 microns must be uniformly distributed
in the mixture;

(b) which can be used directly as feed and which will not be
processed or mixed before they reach the end user.

2. Where it is established that the manufactured product
contains a quantity of skimmed-milk powder exceeding the
maximum quantity of 80 kilograms referred to in paragraph 1
(a)(i) but not exceeding 81 kilograms, the aid may nevertheless
be granted on the basis of a skimmed-milk powder content of
80 kilograms.

Where the manufactured product does not contain the
minimum quantity of 50 kilograms of skimmed-milk powder
referred to in paragraph 1 (a)(i), aid minus 15 % shall be
granted for the skimmed-milk powder actually incorporated
provided that the skimmed-milk powder content is equal to at
least 45 kilograms per 100 kilograms of finished product.

(ii) at least 2 kilograms of starch or puffed (pregelatinised)

starch;

(b) Formula B: 100 kilograms of skimmed-milk powder, plus:
(i) at least 5 kilograms of lucerne meal or grass meal
least 50 % (m/m) of particles not

containing at
exceeding 300 microns,
and

(ii) at least 12 kilograms of fish meal, non-deodorised or
with a strong smell, containing at least 30 % (m/m) of
particles not exceeding 300 microns,
and

(iii) at least 2 kilograms of starch or puffed (pregelatinised)

starch.

The particle sizes which, according to BS standard 410-1976,
to the maximum sizes laid down for the
are the closest
particles of the product concerned, without being smaller than
them, shall be regarded as equivalent thereto.

The substances added to the skimmed-milk powder must

2.
be uniformly distributed in the mixture.

Skimmed-milk powder may not be put through any process,
either before or after denaturing, that will weaken or neutralise
the effects of the denaturing, in particular by using deodorising
agents, changing the taste and smell by eliminating the compo-
nents responsible for gustatory and/or olfactory perception, or
adding ingredients giving a taste and smell that mask those of
the fish meal.

CHAPTER II

AID FOR SKIMMED-MILK POWDER

S e c t i o n 1

Amount of aid and implementing conditions

Article 7

1.

Aid is hereby fixed at:

(a) EUR 5,80 per 100 kilograms of skimmed milk with a
protein content of not less than 35,6 % of the non-fatty dry
extract;

(b) EUR 5,12 per 100 kilograms of skimmed milk with a
less than

less than 31,4 % but

protein content of not
35,6 % of the non-fatty dry extract;

Article 6

‘Denatured skimmed-milk powder’ means products
the following

1.
manufactured in accordance with one of
formulae:

(a) Formula A: 100 kilograms of skimmed-milk powder, plus:

(c) EUR 71,51 per 100 kilograms of skimmed-milk powder
with a protein content of not less than 35,6 % of the
non-fatty dry extract;

(d) EUR 63,07 per 100 kilograms of skimmed-milk powder
with a protein content of not less than 31,4 % but less than
35,6 % of the non-fatty dry extract.

(i) at least 9 kilograms of lucerne meal or grass meal
least 50 % (m/m) of particles not

containing at
exceeding 300 microns,

2.
In the case of skimmed-milk powder with a moisture
content exceeding 5 %, the aid shall be reduced by 1 % for each
additional 0,2 % of moisture.

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Article 8

(c) an indication identifying the undertaking by reference to its

approval number.

To qualify for aid, skimmed-milk powder must meet at least
the following conditions:

(a) it must be used in an undertaking approved in accordance

with Article 9:

2. Without prejudice to Article 11 and Council Directive
79/373/EEC (1), compound feedingstuffs shall be packed in
sacks or other closed or sealed containers containing not more
than 50 kilograms showing the following information:

(i) either unaltered or incorporated in a mixture,

(a) one or more of the statements listed in Annex II.B;

or

(b) an indication identifying the undertaking by reference to its

(ii) unaltered for the manufacture of denatured skimmed-

approval number;

milk powder;

(b) it may not have benefited from aid or a reduction in price

under other Community measures.

(c) the skimmed-milk powder content;

(d) the manufacturing batch number;

Article 9

1.
Undertakings producing mixtures, compound feeding-
stuffs or denatured skimmed-milk powder must have been
approved for that purpose by the competent agency of the
Member State on whose territory production takes place.

2.

Approval shall be granted to undertakings which:

(a) have suitable technical equipment and administrative and
accounting methods which make it possible to comply
with both this Regulation and the additional requirements
laid down by the Member State;

(b) submit to an inspection by the competent agency.

3.
Except in cases of force majeure, where it is found that an
undertaking no longer meets the conditions laid down in para-
graph 2 or has failed to comply with another obligation under
this Regulation, approval shall be suspended for a period of
one to twelve months, depending on the seriousness of the
irregularity.

If, at the end of that period, the conditions laid down in
paragraph 2 are not met, approval
shall be withdrawn.
Approval may be reinstated after no less than six months, at
the request of the undertaking concerned, following an in-
depth inspection.

Member States may decide not to impose such a suspension if
it is established that the irregularity was not committed deliber-
ately or through serious negligence and that its consequences
are marginal.

(e) the date of manufacture,

if this is not indicated in the

manufacturing batch number.

The above information must be clearly legible and indelibly
marked on the package or container or on a label affixed
thereto.

The Member States may lay down detailed rules for
3.
marking the packages as prescribed in paragraph 2, as well as
any additional information which may be given on the pack-
aging or container or on a label. They shall
inform the
Commission of any measures which they take to that end.

Article 11

Article 10(2) shall not apply to compound feedingstuffs:

(a) containing lucerne meal or grass meal under the conditions

laid down in Article 5(1)(a)(iii);

(b) delivered by tanker or container to a farm or a breeding or
fattening concern which uses these compound feedingstuffs
on the conditions laid down in Articles 12 and 13.

Article 12

Undertakings receiving the aid shall, on application, be author-
ised to deliver compound feedingstuffs by tanker or container.
Such authorisation shall be granted by the competent authority
of the Member State on whose territory the undertaking is
established.

Delivery shall take place under administrative supervision to
ensure, in particular, that it is made to a farm or breeding or
fattening concern which uses feedingstuffs.

Article 10

Article 13

Packages containing mixtures must show the following

1.
information:

(a) one or more of the statements listed in Annex II.A;

(b) an indication of the skimmed-milk powder content, the
added mineral and sucrose content and the fat content,
including liposoluble technical agents;

1. When delivery by tanker or container takes place in a
Member State other than the producer Member State, proof of
delivery under administrative supervision as referred to in
Article 12 shall be furnished by production of the control copy
referred to in Articles 471 to 495 of Commission Regulation
(EEC) No 2454/93 (2).

(1) OJ L 86, 6.4.1979, p. 30.
(2) OJ L 253, 11.10.1993, p. 1.

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Section 104 of the control copy must contain one or

2.
more of the statements listed in Annex II.C.

Article 16

3.
the
The importing Member State shall check that
consignee complies with the conditions set out in the second
paragraph of Article 12.

S e c t i o n 2

Inspection measures

Article 14

1.
Undertakings producing compound feedingstuffs may
receive aid only if they keep records, based on their accounts,
corresponding to the payment schedule fixed by the Member
State and including at least the following information:

(a) the quantities of milk products purchased or manufactured,

and the date of delivery or production;

(b) the date of delivery and quantities of skimmed milk and
skimmed-milk powder manufactured or received unaltered
or in a mixture used to manufacture compound feeding-
stuffs, together with the name and address of the supplier
and the milk-protein content of the products;

(c) the date of manufacture of compound feedingstuffs and the
quantities manufactured, with particulars of their composi-
tion and the percentage of each ingredient, and in partic-
ular the quantities of casein and/or caseinates added unal-
tered or in a mixture;

(d) the date of sale of skimmed milk, skimmed-milk powder
and compound feedingstuffs and the quantity sold, together
with the name and address of the consignee;

(e) losses, samples, returns and exchanges of skimmed milk,
skimmed-milk powder and compound feedingstuffs.

The information listed in paragraph 1 shall be supported

2.
by delivery vouchers and invoices.

3. Member States may require undertakings to keep specific
stock accounts showing, in particular, any additional informa-
tion they deem necessary to facilitate application of this Regu-
lation.

1.
Subject to paragraph 2, as regards compliance with the
protein, moisture and fat content of the skimmed milk or
skimmed-milk powder incorporated, the inspection shall be
made before, or at the latest at the time of, their use, whether
unaltered or in the form of a mixture, in the manufacture of
compound feedingstuffs or their use unaltered in the manufac-
ture of denatured skimmed-milk powder.

2. Where the skimmed-milk powder used, whether unal-
tered or in a mixture, comes directly from the factory premises
in which it is produced, the inspection referred to in paragraph
1 may be made before the powder leaves the said factory
premises. In that case, the following rules shall apply:

(a) the inspecting agency concerned shall take all necessary
action to ensure that the quantity of skimmed-milk powder
checked is actually used in the manufacture of compound
feedingstuffs or denatured skimmed-milk powder;

(b) the sacks, packaging and containers in which the skimmed-
milk powder is put up shall bear the relevant information
identifying the powder and the factory premises and shall
show the date of manufacture, the net weight and the
protein, moisture and fat content of the powder;

(c) the inspection records drawn up by the inspecting agency

must:

(i) identify the skimmed-milk powder and state, in partic-
ular, the quantity of powder, its protein, moisture and
fat content and the date of manufacture,

(ii) accompany the skimmed-milk powder until it is incor-

porated into compound feedingstuffs,

(iii) be annexed to the records referred to in Article 14(1).

Article 17

1.
The arrangements for inspecting the use of skimmed milk
and skimmed-milk powder, whether unaltered or in a mixture,
in the manufacture of compound feedingstuffs, shall be deter-
mined by the Member State concerned and must fulfil at least
the conditions set out in paragraphs 2 to 5.

Article 15

Inspection of the undertakings concerned shall cover, in

2.
particular:

In order to ensure compliance with this chapter, the Member
States shall carry out, in particular, the inspections provided for
in Articles 16 to 18.

(a) the composition of the skimmed milk and skimmed-milk

powder used unaltered;

(b) the composition of mixtures used;

The agency responsible for inspection shall record the results
of the inspections in reports containing, in particular, the infor-
mation provided for in Annex I to this Regulation.

(c) the composition of the compound feedingstuffs manufac-

tured.

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Inspection of undertakings shall take place on the prem-
3.
ises and shall relate in particular to the manufacturing condi-
tions as established by:

list drawn up pursuant to Article 2 of Commission Regulation
(EC) No 2721/95.

(a) inspecting the raw materials used;

(b) checking incoming and outgoing products;

(c) sampling;

(d) checking the records referred to in Article 14(1).

4.
Inspections shall be unannounced and shall be made at
least once in every 14 days of manufacture. Their frequency
shall be determined on the basis of the quantities of skimmed-
milk powder used by the undertaking and the frequency with
which its accounts are scrutinised under paragraph 5.

Undertakings not constantly using skimmed milk or skimmed-
milk powder shall forward their manufacturing programme to
the inspecting agency of the Member State concerned so that
the latter may arrange the corresponding inspections.

The above inspection frequency shall not apply in cases where
the manufacture of compound feedingstuffs is the subject of
continuous inspection on the premises.

5.
The inspections referred to in paragraph 4 shall be
supplemented by thorough and unannounced scrutiny of
commercial documents and of the records referred to in Article
14(1).

Such scrutiny shall be carried out at
least once every 12
months. Where it is carried out at least once every three
months, the frequency of the inspections referred to in para-
graph 3 may be reduced from at least once in every 14 days to
at least once in every 28 days of manufacture.

Article 18

The manufacture of denatured skimmed-milk powder
1.
shall be inspected on the premises at least once a day during
the denaturing operation.

2.
Undertakings manufacturing denatured skimmed-milk
powder shall notify the competent agency, before manufacture,
by letter or by any other means of written telecommunication,
of:

(a) the factory's approval number;

(b) the quantity of skimmed-milk powder to be denatured;

(c) the place where denaturing will take place;

(d) the planned dates when denaturing will take place.

The competent agency shall
fix the deadline for notifying
manufacturing dates and may request additional information.

Article 19

Subject to Article 20, the reference methods to be used for the
analyses provided for by this Regulation shall be those in the

Article 20

The skimmed-milk powder content

1.
in mixtures and
compound feedingstuffs shall be determined by testing each
sample at least in duplicate in accordance with the method of
analysis specified in Annex III, supplemented by the checks
provided for in Article 17(3). Should there be a discrepancy
between the results of these checks, the result of the on-the-
spot inspection shall be conclusive.

The absence of rennet whey shall be proven by the

2.
procedure outlined in Annex IV.

The starch content of compound feedingstuffs shall be
3.
determined by the checks provided for in Article 17(3), which
must be supplemented with qualitative analysis using the
method set out in Annex V.

The moisture content of acid buttermilk powder shall be

4.
determined using the method described in Annex VI.

The grass meal or lucerne meal content,

the starch
5.
content and the fish-meal content of denatured skimmed-milk
powder shall be determined either by laboratory analysis or by
the on-the-spot inspection provided for in Article 18(1).

Article 21

In order to carry out the analytical tests provided for in this
chapter, Member States may, after obtaining the Commission's
consent, set up under their supervision a system of self
checking for certain approved undertakings.

S e c t i o n 3

Payment of aid

Article 22

The amount of aid shall be that applicable either on the
1.
day on which the skimmed milk or skimmed-milk powder is
processed into compound feedingstuffs or on the day on which
the skimmed-milk powder is denatured, as the case may be.

The aid shall be paid by the competent authority desig-
2.
nated by the Member State in whose territory the manufacturer
using the skimmed milk or skimmed-milk powder either to
manufacture compound feedingstuffs or for denaturing, as the
case may be,

is situated.

3.
The aid shall be paid on the basis of applications
submitted by manufacturers of compound feedingstuffs or
denatured skimmed-milk powder (hereinafter called ‘beneficiar-
ies’) to the competent authority,

indicating:

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(a) the name and address of the beneficiary;

less than that referred to in the first subparagraph, the amount
to be recovered shall be adjusted accordingly.

(b) the quantity of skimmed milk or skimmed-milk powder for

which aid is requested,

indicating the protein content;

(c) where applicable, the quantity of compound feedingstuffs
into which the skimmed milk or skimmed-milk powder
referred to at (b) is incorporated, indicating any relevant
manufacturing batch numbers.

4.
The aid shall be paid at intervals to be fixed by the
Member State, but the period covered by the payment applica-
tion may not exceed one month.

Article 25

Where the condition laid down in Article 23(3) is met, Member
States shall be authorised to pay an advance, within the
meaning of Article 18 of Commission Regulation (EEC) No
2220/85 (1), for an amount equal to the amount of aid applied
for, subject to the lodging of a security equal to 110 % of the
amount of the advance.

In this case, the supporting documents proving entitlement to
the aid shall be supplied within six months following payment
of the advance.

Article 23

Payment of the aid shall be subject to the conditions set

1.
out in paragraphs 2 to 4.

SALES OF SKIMMED-MILK POWDER FROM PUBLIC STORAGE

CHAPTER III

The results of the analyses provided for in this chapter
2.
and the checks referred to in Article 15 relating to the payment
period immediately prior to that for which the aid is requested
must show that
this chapter have been
complied with.

the provisions of

Beneficiaries must

show to the satisfaction of

the
3.
competent authority that
the corresponding quantity of
skimmed milk or skimmed-milk powder has been processed
into compound feedingstuffs or denatured during the period
covered by the aid application.

4.
In cases covered by Article 12, beneficiaries shall supply
supporting documents establishing to the satisfaction of the
competent authority that
the compound feedingstuffs have
actually been delivered by tanker or container to a farm or
breeding or fattening concern which uses such feedingstuffs.

Article 24

1. Without prejudice to Article 25,
if the results of the
analyses provided for in this chapter and the checks referred to
in Article 15 show that the applicant has not complied with
this chapter during the previous payment period, payment of
the aid for the period covered by the current application shall
be suspended pending the results of the checks made during
the period in question. In addition, any aid unduly paid for the
previous period concerned shall be recovered.

2.
The amount of aid unduly paid out shall be that paid for
all the skimmed milk or skimmed-milk powder used during the
period between the date of the last inspection giving rise to no
observations and the date of the inspection indicating that the
beneficiary is again complying with this Regulation.

However, if the beneficiary so requests, the authority respon-
sible for inspections shall carry out a special enquiry as soon as
possible, at the former's expense. If the quantity is shown to be

S e c t i o n 1

Organisation of and participation in tendering procedures

Article 26

1.
Skimmed-milk powder shall be sold by means of a
standing invitation to tender organised by each intervention
agency.

Sales shall concern skimmed-milk powder taken into

2.
storage before 31 December 1997.

A standing invitation to tender shall be published in the
3.
Official Journal of the European Communities at least eight days
before the first closing date laid down for the submission of
tenders.

The intervention agencies shall draw up a notice of invi-
4.
tation to tender indicating in particular the closing date and
address for submission of tenders.

They shall also indicate, for the skimmed-milk powder they
hold:

(a) the locations of the warehouses where the powder to be

sold is in store,

(b) the quantity for sale in each warehouse.

5.
Intervention agencies shall keep an up-to-date list of the
information referred to in paragraph 4, which they shall make
available to interested parties on request. They shall also
publish regular updates of the list in an appropriate form, to be
indicated in the notice of invitation to tender.

Intervention agencies shall make the necessary arrange-

6.
ments to enable interested parties:

(a) to examine samples of the skimmed-milk powder put up
for sale at their own expense before submitting a tender;

(1) OJ L 205, 3.8.1985, p. 5.

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(b) to verify the results of the analyses referred to in Article 3

of Commission Regulation (EC) No 322/96 (1).

Article 27

1.
Intervention agencies shall organise individual tendering
rounds during the term of validity of the standing invitation to
tender.

2.
The closing date for submission of tenders for each indi-
vidual round shall be 12 noon (Brussels time) on the second
and fourth Tuesday of
for the second
Tuesday of August and the fourth Tuesday of December. If
Tuesday is a public holiday the time limit shall be 12 noon
(Brussels time) on the previous working day.

the month, except

Article 28

The skimmed-milk powder sold under this chapter shall

1.
qualify for the aid provided for in Article 1(a).

2.
Tenders under each individual round shall be submitted
by registered letter or delivered by hand to the intervention
agency against acknowledgement of receipt, or by any other
means of written telecommunication.

Tenders shall be submitted to the intervention agency holding
the skimmed-milk powder for which an offer is made.

3.

Tenders shall state:

(a) the name and address of the tenderer;

(b) the quantity desired;

(c) the price in euro tendered per 100 kilograms, not including

national taxes and charges, ex-warehouse;

(d) the Member State in which processing into compound

feedingstuffs or denaturing is to take place;

(e) if appropriate,

the warehouse where the skimmed-milk

powder is held and,

if desired, a substitute warehouse.

4.

Tenders shall not be valid unless:

(a) they relate to at least 10 tonnes; however, if the quantity
the
available in a warehouse is less than 10 tonnes,
minimum quantity for which an offer may be made shall
be the actual amount available;

(b) they are accompanied by the tenderer's written undertaking

to comply with the following requirements:

(i) to process

the skimmed-milk powder or have it
processed into compound feedingstuffs or denatured
skimmed-milk powder within 60 days of the closing
date for the submission of tenders in response to each
individual tendering round as specified in Article 27(2);

(ii) to comply with this Regulation or ensure that it is

complied with.

(c) proof is provided that the tenderer has lodged a tendering
security of EUR 36 per tonne, in the Member State where
the tender is submitted, for the tendering round in question
before the closing date for submission of tenders.

Tenders may not be withdrawn after the closing date

5.
provided for in Article 27(2).

Article 29

For the purposes of the tendering security provided for in
Article 28(4)(c), the primary requirements within the meaning
of Article 20 of Regulation (EEC) No 2220/85 shall be that
tenders are maintained after the closing date for submission of
tenders, that the processing security referred to in Article 30(3)
is lodged and that the price is paid.

S e c t i o n 2

Implementation of the tendering procedure

Article 30

1.
On the closing date referred to in Article 27(2), the
Member States shall inform the Commission of the quantities
and prices offered by tenderers and the quantity of skimmed-
milk powder offered for sale.

2.
The Commission shall fix a minimum selling price for the
skimmed-milk powder on the basis of the tenders received
under each round and in accordance with the procedure laid
down in Article 42 of Regulation (EEC) No 1255/1999. This
price may vary according to the age and location of the quant-
ities of skimmed-milk powder offered for sale.

It may be decided to make no award under the round.

3.
The Commission shall fix the amount of the processing
security per 100 kilograms of skimmed-milk powder at the
same time as the minimum selling price and in accordance
with the same procedure.

The purpose of the processing security shall be to ensure
fulfilment of the primary requirement, within the meaning of
Article 20 of Regulation (EEC) No 2220/85, that the skimmed-
milk powder be used in accordance with the undertaking
provided for in Article 28(4)(b). This security shall be lodged in
the Member State in which processing into compound feeding-
stuffs or denaturing is to take place, with the body designated
by that Member State.

Article 31

Tenders shall be rejected if the price offered is lower than the
minimum price.

Article 32

(1) OJ L 45, 23.2.1996, p. 5.

The intervention agency shall make the award in accord-

1.
ance with the rules laid down in paragraphs 2 to 5.

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The skimmed-milk powder shall be allocated on the basis
2.
of
its date of entry into storage, starting with the oldest
product of the total quantity available in the warehouse(s)
designated by the tenderer.

3. Without prejudice to Article 31, the successful tenderer
shall be the tenderer offering the highest price.
If the full
quantity available is not allocated,
the remainder shall be
awarded to the other tenderers on the basis of the prices
tendered, starting with the highest price.

4. Where acceptance of a tender would result in contracts
being awarded in excess of
the quantity of skimmed-milk
powder available in a particular warehouse, only the quantity
available shall be awarded to the tenderer in question.

However, the intervention agency may designate other ware-
houses to make up the quantity set out in the tender, provided
the tenderer agrees.

5. Where acceptance of two or more tenders offering the
same price for skimmed-milk powder in a particular warehouse
would lead to contracts being awarded in excess of the quantity
available, the award shall be made by allocating the quantity
available in proportion to the quantities tendered for.

However, should such allocation lead to the award of quantities
of less than five tonnes, the award shall be made by drawing
lots.

Article 33

Rights and obligations arising in connection with the invitation
to tender shall not be transferable.

security referred to in Article 29 and issue a removal order
indicating:

(a) the quantity in respect of which the abovementioned

requirements have been met;

(b) the warehouse in which the skimmed-milk powder is in

store;

(c) the final date for removal of the skimmed-milk powder;

(d) the final date for processing into compound feedingstuffs

or denaturing.

tenderers

Successful

2.
remove the skimmed-milk
shall
powder awarded to them within 30 days of the closing date for
the submission of tenders. Removal may be effected by instal-
ments.

Except in cases of force majeure, if the skimmed-milk powder
has not been removed within the period laid down in the first
subparagraph, the cost of storing it shall be borne by the
successful tenderer, at his own risk, from the day following that
on which the period expired.

3.
The skimmed-milk powder shall be handed over by the
intervention agency in packages bearing a reference to this
Regulation in clearly visible and legible characters.

At the request of the interested party, the intervention agency
shall issue a copy of the certificate indicating the composition
of the products purchased, as provided for in Article 3 of
Regulation (EC) No 322/96.

4.
In addition to the information provided for in Commis-
sion Regulation (EEC) No 3002/92 (1), Section 104 of the T5
control copy must contain one or more of the statements listed
in Annex II.D. Section 106 must show the final date for
processing into compound feedingstuffs or denaturing.

CHAPTER IV

TRANSITIONAL AND FINAL PROVISIONS

Article 34

Article 36

The

intervention agency

1.
inform
tenderers of the outcome of their participation in the invitation
to tender.

immediately

shall

Securities as referred to in Article 29 lodged for unsuccessful
tenders shall be released immediately.

2.
Before removing the skimmed-milk powder and within
the period specified in Article 35(2), successful tenderers shall
pay the intervention agency the amount corresponding to their
tender for each quantity that they wish to withdraw and shall
lodge the processing tender provided for in Article 30(3).

Article 35

1.
Once the amount referred to in Article 34(2) has been
paid and the security provided for in Article 30(3) has been
the intervention agency shall release the tendering
lodged,

Regulations (EEC) No 1105/68, (EEC) No 1725/79, (EEC) No
1634/85, (EEC) No 3398/91, (EEC) No 3536/91 and (EC) No
1043/97 are hereby repealed.

References to Regulations (EEC) No 1725/79 and (EEC) No
3398/91 shall be construed as references to this Regulation.

Article 37

Pre-printed packages as referred to in Article 4(2) and (4) of
Regulation (EEC) No 1725/79 may continue to be used until
30 June 2000.

Approval granted under Article 4(5) and Article 8(2) of Regula-
tion (EEC) No 1725/79 shall remain valid for the purposes of
applying this Regulation.

Regulation (EEC) No 1725/79 shall continue to apply to quant-
ities of skimmed-milk powder awarded under Regulation (EEC)
No 3398/91.

(1) OJ L 301, 17.10.1992, p. 17.

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This Regulation shall enter into force on 1 January 2000.

Article 38

It shall apply only to quantities of skimmed milk and skimmed-milk powder processed into compound
feedingstuffs or denatured skimmed-milk powder from that date.

This Regulation shall be binding in its entirety and directly applicable in all Member States.

Done at Brussels, 17 December 1999.

For the Commission

Franz FISCHLER

Member of the Commission

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ANNEX I

ANALYTICAL TESTS

The provisions adopted in accordance with 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 (OJ L 170, 3.8.1970, p. 21) shall
apply to sampling under this Regulation.

A. Unaltered skimmed-milk powder

1. Determination of:

(a) moisture content

(b) protein content

(c) fat content.

2. Detection of other products in accordance with the arrangements laid down by the national authorities:

(a) starch and puffed starch

(b) grass meal or lucerne meal

(c) rennet whey

(d) fish meal

(e) other substances,

in particular acid whey, which the national authorities require to be detected.

B. Skimmed-milk powder incorporated in a mixture

Tests in addition to those referred to at A.

Determination of:

(a) skimmed-milk powder content

(b) fat content,

including liposoluble technical agents.

C. Denatured skimmed-milk powder

Tests in addition to those referred to at A.

1. Where the powder is denatured using formula A:

Determination of:

(a) grass meal or lucerne meal content

(b) starch content.

Measurement of the particle size of grass meal or lucerne meal.

2. Where the powder is denatured using formula B:

Determination of:

(a) grass meal or lucerne meal content

(b) starch content

(c) fish meal content.

Measurement of the particle sizes of:

(a) grass meal or lucerne meal

(b) fish meal.

Smell may be tested by adding an inert powder before denaturing (dilution 1:20) or after denaturing (dilution 1:2).
A characteristic, strong smell must still be detectable.

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D. Compound feedingstuffs

Determination of:

(a) skimmed-milk powder content

(b) grass meal or lucerne meal content

(c) fat content.

Detection of starch.

Measurement of the particle size of grass meal or lucerne meal (checked before incorporation).

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A. Information to be shown on packaging of mixtures

ANNEX II

— Mezcla destinada a la fabricación de piensos compuestos — Reglamento (CE) no 2799/1999

— Blanding bestemt til fremstilling af foderblandinger — Forordning (EF) nr. 2799/1999

— Mischung zur Herstellung von Mischfutter — Verordnung (EG) Nr. 2799/1999

— Μείγµα που προορίζεται για την παρασκευή συνθέτων ζωοτροφών — Κανονισµός (ΕΚ) αριθ. 2799/1999

— Mixture intended for the manufacture of compound feedingstuffs — Regulation (EC) No 2799/1999

— Mélange destiné à la fabrication d'aliments composés — Règlement (CE) no 2799/1999

— Miscela destinata alla fabbricazione di alimenti composti — Regolamento (CE) n. 2799/1999

— Voor de vervaardiging van mengvoeders bestemd mengsel — Verordening (EG) nr. 2799/1999

— Mistura destinada ao fabrico de alimentos compostos — Regulamento (CE) n.o 2799/1999

— Rehuseosten valmistukseen tarkoitettu esiseos — asetus (EY) N:o 2799/1999

— Blandning avsedd för framställning av foderblandningar — Förordning (EG) nr 2799/1999

B. Information to be shown on packaging of compound feedingstuffs

— Pienso compuesto que contiene leche desnatada en polvo — Reglamento (CE) no 2799/1999

— Foderblanding med indhold af skummetmælkspulver — Forordning (EF) nr. 2799/1999

— Magermilchpulver enthaltendes Mischfutter — Verordnung (EG) Nr. 2799/1999

— Σύνθετη ζωοτροφή που περιέχει αποκορυφωµένο γάλα σε σκόνη — Κανονισµός (ΕΚ) αριθ. 2799/1999

— Compound feedingstuff containing skimmed-milk powder — Regulation (EC) No 2799/1999

— Aliment composé pour animaux contenant du lait écrémé en poudre — Règlement (CE) no 2799/1999

— Alimento composto per animali contenente latte scremato in polvere — Regolamento (CE) n. 2799/1999

— Mageremelkpoeder bevattend mengvoeder — Verordening (EG) nr. 2799/1999

— Alimento composto para animais com leite em pó desnatado — Regulamento (CE) n.o 2799/1999

— Rasvatonta maitojauhetta sisaltavä rehuseos — asetus (EY) N:o 2799/1999

— Foderblandning innehållande skummjölkspulver — Förordning (EG) nr 2799/1999

C. Specific information to be entered in Section 104 of the T5 control copy if the product is delivered by tanker

or container

— Piensos compuestos destinados a una explotación agraria o una explotación pecuaria o de engorde que utilice los

piensos compuestos — Reglamento (CE) no 2799/1999

— Foderblanding til brug på en landbrugsbedrift, en opdrætnings- eller en opfedningsvirksomhed — Forordning (EF)

nr. 2799/1999

— Für landwirtschaftliche Betriebe bzw. Aufzucht- oder Mastbetriebe bestimmtes Mischfutter — Verordnung (EG) Nr.

2799/1999

— Σύνθετες ζωοτροφές που θα χρησιµοποιηθούν από γεωργική εκµετάλλευση ή κτηνοτροφική εκµετάλλευση ή εκµετάλ-

λευση παχύνσεως — Κανονισµός (ΕΚ) αριθ. 2799/1999

— Compound feedingstuffs bound for a farm or breeding or fattening concern which uses feedingstuffs — Regulation

(EC) No 2799/1999

— Aliments composés pour animaux destinés à une exploitation agricole ou à une exploitation d'élevage ou

d'engraissement utilisatrice — Règlement (CE) no 2799/1999

— Alimenti composti per animali destinati ad un'azienda agricola o ad un'azienda dedita all'allevamento o all'ingrasso

che utilizzano gli alimenti composti — Regolamento (CE) n. 2799/1999

— Mengvoeder, bestemd voor een dit voeder gebruikend landbouwbedrijf of veeteelt- of veemesterijbedrijf —

Verordening (EG) nr. 2799/1999

— Alimentos compostos para animais destinados a uma exploração agrícola, pecuária ou de engorda utilizadora —

Regulamento (CE) n.o 2799/1999

— Maatilalle,

jalostuskarjatilalle tai

lihakarjatilalle tarkoitettu rehuseos — asetus (EY) N:o 2799/1999

— Foderblandningar avsedda att användas i ett jordbruksföretag, eller för uppfödning eller gödning — Förordning

(EG) nr 2799/1999

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D. Specific information to be entered in Section 104 of the T5 control copy in the case of skimmed-milk

powder sold from public storage

— Debe transformarse en piensos compuestos o desnaturalizarse — Reglamento (CE) no 2799/1999

— Skal forarbejdes til foderblandinger eller denatureres — Forordning (EF) nr. 2799/1999

— Zur Verarbeitung zu Mischfutter oder zur Denaturierung — Verordnung (EG) Nr. 2799/1999

— Να µεταποιηθεί σε σύνθετες ζωοτροφές ή να µετουσιωθεί — Κανονισµός (ΕΚ) αριθ. 2799/1999

— To be processed into compound feedingstuffs or denatured — Regulation (EC) No 2799/1999

— À transformer en aliments composés pour animaux ou à dénaturer — Règlement (CE) no 2799/1999

— Da trasformare in alimenti composti per animali o da denaturare — Regolamento (CE) n. 2799/1999

— Moet tot mengvoeder worden verwerkt of worden gedenatureerd — Verordening (EG) nr. 2799/1999

— Para transformação em alimentos compostos para animais ou desnaturação — Regulamento (CE) n.o 2799/1999

— Rehuseoksiksi

jalostettavaksi tai denaturoitavaksi — asetus (EY) N:o 2799/1999

— För bearbetning till foderblandningar eller denaturering — Förordning (EG) nr 2799/1999

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QUANTITATIVE DETERMINATION OF SKIMMED-MILK POWDER IN COMPOUND FEEDINGSTUFFS BY
ENZYMATIC COAGULATION OF PARA-CASEIN

ANNEX III

1.

Purpose

Quantitative determination of skimmed-milk powder in compound feedingstuffs by enzymatic coagulation of
para-casein.

2.

Scope

This method applies to compound feedingstuffs containing at least 10 % skimmed-milk powder; large quantities of
buttermilk and/or of certain non-milk proteins may lead to interferences.

3.

Principle of the method

3.1. Dissolving of casein contained in the compound feedingstuff by extraction with sodium citrate solution.

3.2. Adjustment of the calcium ion concentration to the required level to precipitate para-casein; by addition of rennet

para-casein is obtained from casein.

3.3.

The nitrogen content of the para-casein precipitate is determined by the Kjeldahl method as described by IDF
standard 20A 1986; the quantity of skimmed-milk powder is calculated on the basis of a minimum casein content
of 27,5 % (see 9.1).

4.

Reagents

The reagents used must be of analytical grade. The water used must be distilled water or water of equivalent purity.
With the exception of the rennet (4.5), all the reagents and solutions must be free of nitrogenous substances.

4.1.

Trisodium citrate, dihydrate (1 % w/v solution).

4.2.

Calcium chloride (2M solution). Weigh 20,018 g of CaCO
3 (analytical grade) in a porcelain vessel of suitable size
(150 to 200 ml) or in a beaker. Cover with distilled water and transfer onto a boiling water bath. Add slowly 50
to 60 ml of HCl solution (conc. HCl:water = 1:1) to solubilise the carbonate completely. Keep on the boiling
water bath until the CaCl
2 is dried, to eliminate the HCl which has not reacted. Transfer with distilled water to a
100 ml measuring flask and dilute to the mark. Measure the pH value, which must be not lower than 4,0. Store
the solution in a refrigerator.

4.3.

0,1 N sodium hydroxide.

4.4.

0,1 N hydrochloric acid.

4.5.

Liquid calf rennet (standard strength of 1:10 000). Store in a refrigerator at 4 to 6 °C.

4.6.

Reagents for the quantitative determination of nitrogen according to the Kjeldahl method as described by IDF
standard 20A 1986.

5.

Apparatus

Common laboratory apparatus,

including:

5.1. Mortar or homogeniser

5.2. Analytical balance

5.3.

Bench-top centrifuge (2 000 to 3 000 rpm) with 50 ml tubes

5.4. Magnetic stirrer with (10 to 15 mm) followers

5.5.

150 to 200 ml beakers

5.6.

250 and 500 ml flasks

5.7. Glass funnels of 60 to 80 mm diameter

5.8.

Fast-filtering ashless filters of diameter 150 mm (S.S. 5892, S.S. 595 1/2)

5.9.

Pipettes of various nominal volume

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5.10. Thermostatically controlled water bath at 37 °C

5.11. pH meter

5.12. Kjeldahl digestion and distillation assembly with fittings

5.13. 25 ml graduated burette

5.14. Plastic wash bottle for distilled water

5.15. Stainless steel spatulas

5.16. Thermometers

5.17. Temperature-controlled drying oven.

6.

Procedure

6.1.

Preparation of the sample.

Grind in the mortar or homogenise in the mill 10 to 20 g of the sample to obtain a homogeneous mixture.

6.2. Dissolving of milk powder and separation of the insoluble residue.

6.2.1. Weigh 1,000 ± 0,002 g of well-homogenised compound feedingstuff (6.1) directly into a 50 ml centrifuge tube.
Add 30 ml of trisodium citrate solution (4.1) previously heated to 45 °C. Mix with the aid of the magnetic stirrer
for at least five minutes.

6.2.2. Centrifuge at 500 g (2 000 to 3 000 rpm) for 10 minutes and decant the clear aqueous supernatant into a 150 to

200 ml beaker, taking care that no loose material on the bottom goes over.

6.2.3. Carry out two further extractions on the residue, according to the same procedure, adding the extracts to the first

one.

6.2.4. If a layer of oil forms at the surface, cool in the refrigerator until the fat solidifies and remove the solid layer with a

spatula.

6.3.

Coagulation of casein with the enzymes of rennet.

6.3.1. While stirring continuously, add dropwise 3,4 ml of a saturated solution of calcium chloride (4.2) to the total
aqueous extract (about 100 ml). Adjust the pH to 6,4-6,5 with solutions of NaOH (4.3) or HCl (4.4). Place in the
thermostatically-controlled water bath at 37 °C for 15 to 20 minutes to obtain saline balance. It becomes more
evident by the formation of a light turbidity.

6.3.2. Transfer the liquid into one (or two) centrifuge tubes and centrifuge at 2 000 g for 10 minutes in order to remove
the precipitated material. Transfer the supernatant, without washing the sediment, into one (or two) centrifuge
tubes.

6.3.3. Bring the temperature of the supernatant back to 37 °C. While stirring the extract, add, dropwise, 0,5 ml of the

liquid rennet (4.5). Coagulation occurs in one or two minutes.

6.3.4. Return the sample to the water bath and leave at a temperature of 37 °C for 15 minutes. Remove the sample from
the bath and break the coagulum by stirring. Centrifuge at 2 000 g for 10 minutes. Filter the supernatant through
a suitable filter paper (1) (Whatman No 541 or equivalent) and retain the filter paper. Wash the precipitate in the
centrifuge tube with 50 ml of water at approximately 35 °C by stirring the precipitate.

Centrifuge again at 2 000 g for 10 minutes. Filter the supernatant through the filter paper retained previously.

6.4. Determination of casein nitrogen.

6.4.1. After washing, transfer quantitatively the precipitate to the filter paper retained from 6.3.4 using distilled water.
Transfer the filter paper to the Kjeldahl flask. Determine the nitrogen by the Kjeldahl method as described by IDF
standard 20A 1986.

7.

Blank test

7.1. A blank test shall be made regularly using an ashless filter paper (5.8) moistened with a mixture of 90 ml (4.1)
sodium citrate solution, 1 ml saturated solution of calcium chloride (4.2), 0,5 ml of liquid rennet (4.5), and
washed with 3 × 15 ml of distilled water before mineralisation by the Kjeldahl method as described at IDF
standard 20A 1986.

7.2.

The volume of acid used for the blank test must be subtracted from the volume of acid (4.4) used for titration of
the sample.

(1) As fast filtering ashless paper should be used.

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8.

8.1.

Control test

To test the abovementioned procedure and reagents, make a determination on a standard compound feedingstuff
with a known skimmed-milk powder content as established by collaborative study. The average result of a
duplicate determination should not differ by more than 1 % from that of the collaborative study.

9.

Expression of results

9.1.

The percentage of skimmed-milk powder in the compound feedingstuff is calculated by the following formula:

( N × 6,38

27,5

× 100 ) − 2,81

0,908

% MMP =

where N is the percentage of para-casein nitrogen; 27,5 is the factor for converting determined casein into the
percentage of skimmed-milk powder; 2,81 and 0,908 are correction factors obtained from regression analysis.

10.

Accuracy of the method

10.1. Repeatability

In at least 95 % of the cases studied duplicate analysis of the same sample by the same operator in the same
laboratory must give differences in the results equivalent to no greater than 2,3 g of skimmed-milk powder in
100 g of compound feedingstuff.

10.2. Reproducibility

In at least 95 % of the cases studied, the same sample analysed by two laboratories, must give differences in the
results no greater than 6,5 g of skimmed-milk powder in 100 g of compound feedingstuff.

11.

Tolerance limit

The CrD95

CrD95 =

value (critical difference; 95 % confidence limit) is calculated using the formula (ISO 5725):

1
√2

√ R2 − r2( n − 1

n

)

(R: reproducibility; r: repeatability)

Double determination: CrD

95

= 4,5 g

Where the result of the chemical analysis differs from the declared content of skimmed-milk powder by not more
than 4,5 g (double determination) the consignment of compound feedingstuff is deemed to comply with this
provision of the Regulation.

12. Observations

12.1. The addition of large percentages of certain non-milk proteins and especially of soya proteins, when heated
together with skimmed-milk powder, may lead to too high results due to co-precipitation with the para-casein of
milk.

12.2. Addition of buttermilk may lead to somewhat low figures, due to the fact that only the non-fat portion is
determined. Addition of certain acid buttermilk may give considerably low figures, due to incomplete dissolving in
the citrate solution.

12.3. Lecithin additions of 0,5 % or more may also lead to low results.

12.4.

Incorporation of high-heat skimmed-milk powder may lead to too high figures due to the co-precipitation of
certain whey proteins with the para-casein of milk.

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ANNEX IV

DETERMINATION OF RENNET WHEY SOLIDS IN SKIMMED-MILK POWDER AND MIXTURES UNDER
REGULATION (EEC) No 1725/79

1.

Scope: Detection of the addition of rennet whey solids to:

(a) skimmed-milk powder as defined in Article l of Regulation (EEC) No 986/68, and

(b) mixtures as defined in Article 1(3) of Regulation (EEC) No 1725/79.

2.

References: International standard ISO 707.

Milk and milk products — methods of sampling, conforming to the guidelines contained in Annex I(2)(c) to
Regulation (EEC) No 625/78.

3.

Definition

The content of rennet whey solids is defined as the percentage by mass as determined by the procedure
described.

4.

Principle

Determination of the amount of glycomacropeptide A pursuant to Annex V to Regulation (EEC) No 625/78.
Samples giving positive results are analysed for glycomacropeptide A by a reversedphase high-performance liquid
chromatography procedure (HPLC-procedure). Evaluation of the result obtained by reference to standard samples
consisting of skimmed-milk powder with and without a known percentage of whey powder. Results higher than
1 % (m/m) show that rennet whey solids are present.

5.

Reagents

All reagents must be of recognised analytical grade. The water used must be distilled water or water of at least
equivalent purity. Acetonitrile should be of spectroscopic or HPLC quality.

Reagents needed for the procedure described in Regulation (EEC) No 625/78 are described in Annex V to that
Regulation.

Reagents for reversed-phase HPLC.

5.1.

Trichloroacetic acid solution

Dissolve 240 g of trichloroacetic acid (CCI3COOH) in water and make up to 1 000 ml.

5.2.

Eluent A and B

,) and 1,00 ml trifluoroacetic
CHOHCH
Eluent A: 150 ml of acetonitrile (CH3
3
COOH) are made up with water to 1 000 ml. Eluent B: 550 ml of acetonitrile, 20 ml of
acid (TFA, CF
3
isopropanol and 1,00 ml TFA are made up with water to 1 000 ml. Filter the eluent solution, prior to use,
through a membrane filter with a 0,45 µm pore diameter.

CN), 20 ml of isopropanol (CH
3

5.3.

Conservation of the column

After the analyses the column is flushed with eluent B (via a gradient) and subsequently flushed with acetonitrile
(via a gradient in 30 minutes). The column is stored in acetonitrile.

5.4.

Standard samples

5.4.1.

Skimmed-milk powder meeting the requirements of Regulation (EEC) No 625/78 (i. e. (0)).

5.4.2.

5.4.3.

The same skimmed-milk powder adulterated with 5 % (m/m) rennet-type whey powder of standard composition
(i. e. (5)).

The same skimmed-milk powder adulterated with 50 % (m/m) rennet-type whey powder of standard composi-
tion (i. e. (50)) (*).

6.

Apparatus

Apparatus needed for the procedure described in Regulation (EEC) No 625/78 is described in Annex V to that
Regulation.

Apparatus for reversed-phase HPLC.

(*) Rennet-type whey powder of standard composition and also the adulterated skimmed-milk powder are available from NIZO, Kern-
hemseweg 2, PO Box 20 - NL-6710 BA Ede. However, powders giving equivalent results to the NIZO powders must also be used.

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L 340/21

6.1.

6.2.

6.3.

6.4.

6.5.

6.6.

6.7.

6.8.

Analytical balance.

Centrifuge, capable of attaining a centrifugal force of 2 200 g, fitted with stoppered centrifuge tubes of about
50 ml.

Mechanical shaker with a provision to shake at 50 °C.

Magnetic stirrer.

Glass funnels, diameter about 7 cm.

Filter papers, medium filtration, diameter about 12,5 cm.

Glass filtration equipment with 0,45 µm pore diameter membrane filter.

Graduated pipettes, allowing delivery of 10 ml (ISO 648, Class A, or ISO/R 835), or a system capable of
deliverying 10,0 ml

in two minutes.

6.9.

Thermostatic waterbath, set at 25 ± 0,5 °C.

6.10.

HPLC-equipment, consisting of:

6.10.1. Binary gradient pumping system.

6.10.2.

Injector, hand or automatic, with a 100 µl capacity.

6.10.3. Column Dupont Protein Plus (2 × 0,46 cm I.D.) or an equivalent wide-pore silica based reversedphase column.

6.10.4. Thermostatic column oven, set at 35 ± 1 °C.

6.10.5. Variable wavelength UV detector, permitting measurements at 210 nm (if necessary, a higher wavelength up to

220 nm may be used) with a sensitivity of 0,02 A.

6.10.6.

Integrator capable of peak height measurement.

Note

Operation of the column at room temperature is possible, provided that the room temperature does not fluctuate
more than 1 °C, otherwise too much variation in the retention time of GMPA takes place.

7.

7.1.

Sampling

International standard ISO 707 — Milk and milk products — Methods of sampling, conforming to the guidelines
contained in Annex I(2)(c) of Regulation (EEC) No 625/78.

7.2.

Store the sample in conditions which preclude any deterioration or change in composition.

8.

Procedure

8.1.

Preparation of the test sample

Transfer the powder into a container with a capacity of about twice the volume of the powder, fitted with an
airtight lid. Close the container immediately. Mix the milk powder well by means of repeated inversion of the
container.

8.2.

Test portion

Weigh 2,000 ± 0,001 g of test sample into a centrifuge tube (6.2) or suitable stoppered flask (50 ml).

8.3.

Removal of fat and proteins

8.3.1. Add 20,0 g of warm water (5O °C) to the test portion. Dissolve the powder by shaking for five minutes or 30
minutes in the case of acid buttermilk using a mechanical shaker (6.3). Place the tube into the waterbath (6.9)
and allow to equilibrate to 25 °C.

8.3.2. Add 10.0 ml of the trichloroacetic acid solution of 25 °C (5.1) constantly over two minutes, while stirring
vigorously with the aid of the magnetic stirrer (6.4). Place the tube in a waterbath (6.9) and leave for 60 minutes.

8.3.3.

Centrifuge (6.2) for 10 minutes at 2 200 g, or filter through paper (6.6), discarding the first 5 ml of filtrate.

8.4.

Chromatographic determination

8.4.1.

Perform HPLC-analysis as described in Regulation (EEC) No 625/78, Annex V. If a negative result is obtained, the
sample analysed does not contain rennet-whey solids in detectable amounts. In case of positive results the
reversed-phase HPLC-procedure described below has to be applied. The presence of acid buttermilk powder may
give rise to false-positive results. The reversed-phase HPLC method excludes this possibility.

L 340/22

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8.4.2.

Before the reversed phase HPLC-analysis is carried out, the gradient conditions should be optimised. A retention
time of 26 ± 2 minutes for GMPA is optimal for gradient systems with a dead volume of about 6 ml (volume
from the point where the solvents come together to the volume of the injector loop, inclusive). Gradient systems
with a lower dead volume (e.g. 2 ml) should used 22 minutes as an optimal retention time.

Take solutions of the standard samples (5.4) without and with 50 % rennet whey.

Inject 100 µl of supernatant or filtrate (8.3.3) into the HPLC apparatus operating at the scouting gradient
conditions given in Table 1.

Table 1. Scouting gradient conditions for optimisation of the chromatography.

Time
(minutes)

Flow
(ml/minutes)

Init

27

32

37

42

1,0

1,0

1,0

1,0

1,0

% A

90

60

10

10

90

% B

10

40

90

90

10

Curve

*

lin

lin

lin

lin

Comparison of the two chromatograms should reveal the location of the (peak of GMP
A

.

Using the formula given below, the initial solvent composition to be used for the normal gradient (see 8.4.3) can
be calculated

% B = 10 – 2,5 + (13,5 + (RTgmpA – 26)/6)*30/27

% B = 7,5 + (13,5 + (RTgmpA – 26)/6)*1.11

Where:

RTgmpA:

retention time of GMP

A in the scouting gradient

10:

2,5:

13,5:

26:

6:

30:

27:

the initial % B of the scouting gradient

% B at midpoint minus % B at initial

in the normal gradient

midpoint time of the scouting gradient

required retention time of GMP
A

ratio of slopes of the scouting and normal gradient

% B at initial minus % B at 27 minutes in the scouting gradient

run-time of the scouting gradient.

8.4.3.

Take solutions of the test samples

Inject 100 µl of accurately measure supernatant or filtrate (8.3.3) into the HPLC apparatus operating at a flow
rate of 1,0 ml of eluent solution (5.2) per minute.

The composition of the eluent of the start of the analysis is obtained from 8.4.2. It is normally close to
A:B = 76:24 (5.2). Immediately after the injection a linear gradient is started, which results in a 5 % higher
percentage of B after 27 minutes. Subsequently a linear gradient is started, which brings the eluent composition
to 90 % B in five minutes. This composition is maintained for five minutes, after which the composition is
changed, via a linear gradient in five minutes to the initial composition. Depending on the internal volume of the
pumping system, the next injection can be made 15 minutes after reaching the initial conditions.

Remarks

1. The retention time of the glycomacropeptide should be 26 ± two minutes. This can be achieved by varying
the initial and end conditions of the first gradient. However, the difference in the % B for the initial and end
conditions of the first gradient must remain 5 % B.

2. The eluents should be degassed sufficiently and should also remain degassed. This is essential for proper
functioning of the gradient pumping system. The standard deviation for the retention time of the GMP peak
should be smaller than 0,1 minutes (n = 10).

3. Every five samples the reference sample (5) should be injected and used to calculate a new response factor R.

(9.1.1).

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8.4.4.

The results of the chromatographic analysis of the test sample (E) are obtained in the form of a chromatogram in
which the GMP peak is identified by its retention time of about 26 minutes.

The integrator (6.40.6) automatically calculates the peak height H of the GMP peak. The baseline location should
be checked in every chromatogram. The analysis or the integration should be repeated if the baseline was
incorrectly located.

It is essential to examine the appearance of each chromatogram prior to quantitative interpretation, in order to
detect any abnormalities due either to malfunctioning of the apparatus or the column, or to the origin and
nature of the sample analysed. If in doubt, repeat the analysis.

8.5.

Calibration

8.5.1. Apply exactly the procedure described from point 8.2 to point 8.4.4 to the standard samples (5.4.1 to 5.4.2). Use
freshly prepared solutions, because GMP degrades in an 8 % trichloroacetic acid environment at room tempera-
ture. At 4 °C the solution remains stable for 24 hours. In the case of long series of analyses the use of a cooled
sample tray in the automatic injector is desirable.

Note

8.4.2 may be omitted if the % B at initial conditions is known from previous analyses.

The chromatogram of the reference sample (5) should be analogous to Figure. 1. In this figure the GMP
preceded by two small peaks. It is essential to obtain a similar separation.

A peak is

8.5.2.

Prior to chromatographic determination of the samples inject 100 µl of the standard sample without rennet
whey (0) (5.4.1).

The chromatogram should not show a peak at the retention time of the GMPA peak.

8.5.3. Determine the response factors R by injecting the same volume of filtrate (8.5.1) as used for the samples.

9.

Expression of results

9.1.

Method of calculation and formulae

9.1.1.

Calculation of the response factor R:
GMP peak: R = W/H

Where

R = the response factor of the GMP peak
H = the height of the GMP peak
W = the quantity of whey in the standard sample (5).

9.2.

Calculation of the percentage of rennet whey powder in the sample

W(E) = R × H(E)

Where:

W(E) =
R =
H(E) =

the percentage (m/m) of rennet whey in the sample (E).
the response factor of the GMP peak (9.1.1)
the height of the GMP peak of the sample (E)

If W(E) is greater than 1 % and the difference between the retention time and that of the standard sample (5) is
smaller than 0,2 minutes then rennet whey solids are present.

9.3.

Accuracy of the procedure

9.3.1.

Repeatability

The difference between the results of two determinations carried out simultaneously or in rapid succession by the
same analyst using the same apparatus on identical test material shall not exceed 0,2 % m/m.

9.3.2.

Reproducibility

Not yet determined.

9.3.3.

Linearity

From 0 to 16 % of rennet whey a linear relationship should be obtained with a coefficient of correlation > 0,99.

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9.4.

Interpretation

9.4.1. Whey is considered to be present if the result obtained in 9.2 is higher than 1 % m/m and the retention time of
the GMP peak differs less than 0,2 minutes from that of the standard sample (5). The 1 % limit is fixed in
agreement with the provisions of points 9.2 and 9.4.1 of Annex V to Regulation (EEC) No 625/78.

31. 12. 1999

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Official Journal of the European Communities

L 340/25

QUALITATIVE DETERMINATION OF STARCH IN SKIMMED-MILK POWDER, DENATURED MILK POWDER
AND COMPOUND FEEDINGSTUFFS

ANNEX V

1.

Scope

This method is for the detection of starch which is isued as a tracer in denatured milk powders.

Limit of detection of the method is approximately 0,05 g of starch per 100 g of sample.

2.

Principle

The reaction is based on the one used in iodometry:

— fixation by the colloids of the free iodine in aqueous solution,

— absorption by the starch micelles and by colour formation.

3. Reagents

3.1. Iodine solution

— iodine. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

— potassium iodine. . . . . . . . . . . . . . . . . . . .

1 g,

2 g,

— distilled water . . . . . . . . . . . . . . . . . . . . . 100 ml.

4. Apparatus

4.1. Analytical balance

4.2. Water bath

4.3. Test tubes, 25 mm × 200 mm

5.

Procedure

Weight 1 g of the sample and transfer it into the test tube (4.3).

Add 20 ml of distilled water and shake in order to disperse the sample.

Place in the boiling water bath (4.2) and leave for 5 minutes.

Remove from the bath and cool to room temperature.

Add 0,5 ml of the iodine solution (3.1), shake and observe the resulting colour.

6.

Expression of results

A blue colouration indicates the presence of native starch in the sample.

When the sample contains modified starch the colour may not be blue.

7. Remarks

The colour, the intensity of the colour and the microscopic appearance of the starch, will vary depending on the
origin of native starch (e.g. maize or potato) and the type of modified starch present in the sample.

In the presence of modified starches the colour produced turns violet, red or brown, according to the degree of
modification of the crystalline structure of native starch.

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ANNEX VI

DETERMINATION OF MOISTURE IN ACID BUTTERMILK POWDER

1.

Scope

To determine the moisture content of acid buttermilk powder intended for animal feedingstuffs.

2.

Principle

The sample is dried under vacuum. The loss of mass is determined by weighing.

3. Apparatus

3.1. Analytical balance

3.2. Dry containers of non-corrodible metal or of glass with lids ensuring airtight closure; working surface allowing the

test sample to be spread at about 0,3 g/cm2.

3.3. Adjustable electrically heated vacuum oven fitted with an oil pump and either a mechanism for introducing hot dried

air or a drying agent (e.g. calcium oxide).

3.4. Desiccator with an efficient drying agent.

3.5. Drying oven ventilated, thermostatically controlled, at 102 ± 2 °C.

4.

Procedure

Heat a container (3.2) with its lid in the oven (3.5) for at least one hour. Place the lid on the container, immediately
transfer to a desiccator (3.4) allow to cool to room temperature and weigh to the nearest 0,5 mg.

Weigh a container (3.2) with its lid to the nearest 0,5 mg. Weight in the weighted container, to the nearest 1 mg,
about 5 g of the sample and spread evenly. Place the conainer without its lid, in the vacuum oven (3.3) preheated to
83 °C. To prevent the oven temperature from falling unduly,

introduce the container as rapidly as possible.

Bring the pressure up to 100 Torr (13,3 kPa) and leave to dry for four hours at this pressure, either in a current of
hot, dry air or using a drying agent (about 300 g for 20 samples). In the latter instance, disconnect the vacuum
pump when the prescribed pressure has been reached. Reckon drying time from the moment when the oven
temperature returns to 83 °C. Carefully bring the oven back to atmospheric pressure. Open the oven, place the lid
on the container immediately, remove the container from the oven, leave to cool for 30 to 45 minutes in the
desiccator (3.4) and weigh to the nearest 1 mg. Dry for an additional 30 minutes in the vacuum oven (3.3) at 83 °C
and reweigh. The difference between the two weighings must not exceed 0,1 % of moisture.

5. Calculation

(E – m) ·

100
E

where

E

= initial mass,

in grammes of the test sample,

m = mass,

in grammes, of the dry test sample.

6.

Precision

6.1. Repeatability limit

The difference between the results of two determinations carried out within the shortest feasible time interval, by one
operator using the same apparatus on identical test material shall not exceed 0,4 g water/100 g acid buttermilk
powder.

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L 340/27

6.2. Reproducibility limit

The difference between the results of two determinations carried out by operators in different laboratories, using
different apparatus on identical test material shall not exceed 0,6 g water/100 g acid buttermilk powder.

6.3. Source of precision data

The precision data were determined from an experiment conducted in 1995 involving eight laboratories and 12
samples (6 blind duplicates).