S.L. 437.67 · Methods Of Analysis For The Official (S.L. 437.67)
S.L. 437.67 Art. 1Title, scope and applicability. I. 1. This method It does not of mineral the analysis of olaginous fruit on the The described in September the oil content, 2. The sample nature of the necessary to which have a 3. 3.1. rapid, even with the and 4.1.2. (e.g. motion or 3.2. 3.3. Dry closure; 3.4. rapid
(1) The title of these rules is the Methods of Analysis for the Official Control of Feedingstuffs Rules.
(2) The scope of these rules is to implement the rules found under EU Commission Directive 71/393/EEC establishing EC methods for the official control of feedingstuffs.
(3) The Member States shall require that analyses for official controls of feedingstuffs as regards their contents of moisture, volatile nitrogenous bases, total phosphorus and crude oils and fats be carried out according to the methods described in the Schedule.
*These rules have been repealed by Legal Notice 37 of 2025. SCHEDULE
DETERMINATION OF MOISTURE Purpose and Scope makes it possible to determine the moisture content of feedingstuffs. cover the analysis of milk products as straight feedingstuffs, the analysis substances and mixtures composed predominantly of mineral substances, animal and vegetable fats and oils or the analysis of the oil seeds and defined in Council Regulation No 136/66/EEC of 22 September 1966 establishment of a common organization of the market in oils and fats. determination of the moisture content of oil seeds and oleaginous fruit is Annex III to Commission Regulation (EEC) No 1470/68 of 23 1968 on the drawing and reduction of samples and the determination of impurities and moisture in oil seeds. Principle is desiccated under specified conditions which vary according to the feedingstuff. The loss in mass is determined by weighing. It is carry out preliminary drying when dealing with solid feedingstuffs high moisture content. Apparatus Crusher of non moisture-absorbing material which is easy to clean, allows crushing without producing any appreciable heating, prevents contact outside air as far as possible and meets the requirements laid down in 4.1.1. hammer or watercooled micro-crushers, collapsible cone mills, slow cogwheeled crushers). Analytical balance, accurate to 0ꞏ5 mg.
containers of non-corrodible metal or of glass with lids ensuring airtight working surface allowing the test sample to be spread at about 0ꞏ3 g/cm2.
Electrically heated isothermal oven (± 1ºC) properly ventilated and ensuring temperature regulation*.
Adjustable electrically heated vacuum oven fitted with an oil pump and mechanism for introducing hot dried air or a drying agent (e.g. calcium
Desiccator with a thick perforated metal or porcelain plate, containing an agent. Procedure operations described in this section must be carried out immediately the packages of samples. Analysis must be carried out at least in
Preparation Feedingstuffs other than those coming under 4.1.2 and 4.1.3 50 g of the sample. If necessary, crush or divide in such a way as to of cereals, flour, groats and meal, the oven must have a thermal capacity such that, when it will return to that temperature in less than 45 minutes after the maximum number of test been placed inside to dry simultaneously. Ventilation must be such that, when as many common wheat as it can contain are dried for two hours, the results differ from those obtained drying by less than 0ꞏ15%. avoid any variation in moisture content (see 6).
4.1.2. Cereals and groats Take at least 50 g of the sample. Grind into particles of which at pass through a 0ꞏ5 mm mesh sieve and will leave no more than 10% reject round-meshed sieve.
4.1.3. Feedingstuffs in liquid or paste form, feedingstuffs predominantly of oils and fats Take about 25 g of the sample, weigh to the nearest 10 mg, add quantity of anhydrous sand weighed to the nearest 10 mg an homogeneous product is obtained. 4.2. Drying 4.2.1. Feedingstuffs other than those coming under 4.2.2 and 4.2.3 Weigh a container (3.3) with its lid to the nearest 0ꞏ5 mg. Weigh into container, to the nearest 1 mg, about 5 g of the sample and spread evenly. container, without its lid, in the oven preheated to 103ºC. To prevent temperature from falling unduly, introduce the container as rapidly Leave to dry for four hours reckoned from the time when the oven returns to 103ºC. Replace the lid on the container, remove the latter leave to cool for 30 to 45 minutes in the desiccator (3.6) and weigh to mg. For feedingstuffs composed predominantly of oils and fats, dry in additional 30 minutes at 130ºC. The difference between the two weighings exceed 0ꞏ1% of moisture.
4.2.2. Cereals, flour, groats and meal Weigh a container (3.3) with its lid to the nearest 0ꞏ5 mg. Weigh into container, to the nearest 1 mg, about 5 g of the crushed sample and Place the container, without its lid, in the oven preheated to 130ºC. oven temperature from falling unduly, introduce the container as rapidly Leave to dry for two hours reckoned from the time when the oven returns to 130ºC. Replace the lid on the container, remove the latter leave to cool for 30 to 45 minutes in the desiccator (3.6) and weigh to mg. 4.2.3. Compound feedingstuffs containing more than 4% of sucrose straight feedingstuffs such as locust beans, hydrolyzed cereal products, dried beet chips, fish and sugar solubles; compound feedingstuffs containing than 25% of mineral salts including water of crystallization. Weigh a container (3.3) with its lid to the nearest 0ꞏ5 mg. Weigh into container, to the nearest 1 mg, about 5 g of the sample and spread evenly. container, without its lid, in the vacuum oven (3.5) preheated to between 85ºC. To prevent the oven temperature from falling unduly, introduce as rapidly as possible. Bring the pressure up to 100 Torr and leave to dry for four hours at either in a current of hot, dry air or using a drying agent (about samples). In the latter instance, disconnect the vacuum pump when pressure has been reached. Reckon drying time from the moment temperature returns to 80ºC to 85ºC. Carefully bring the oven back pressure. Open the oven, place the lid on the container immediately, container from the oven, leave to cool for 30 to 45 minutes in the desiccator the nearest 1 mg. Dry for an additional 30 minutes in the vacuum oven 85ºC and reweigh. The difference between the two weighings must not of moisture.
Preliminary drying
Feedingstuffs other than those coming under 4.3.2 feedingstuffs with a high moisture content which makes crushing difficult subjected to preliminary drying as follows:
g of uncrushed sample to the nearest 10 mg (compressed or feedingstuffs may be roughly divided if necessary) in a suitable a 20 × 12 cm aluminium plate with a 0ꞏ5 cm rim). Leave to dry in an 60ºC to 70ºC until the moisture content has been reduced to between 8% Remove from the oven, leave to cool uncovered in the laboratory for one weigh to the 10 mg. Crush immediately as indicated in 4.1.1 and dry as 4.2.1 or 4.2.3 according to the nature of the feedingstuff.
Cereals a moisture content of over 17% must be subjected to preliminary follows: of grain to the nearest 10 mg in a suitable container (e.g. a unground aluminium plate with a 0ꞏ5 cm rim). Leave to dry for 5 to 7 minutes in an Remove from the oven, leave to cool uncovered in the laboratory for weigh to the nearest 10 mg. Grind immediately as indicated in 4.1.2 indicated in 4.2.2. Calculation of results moisture content, as a percentage of the sample, is calculated by using the formulae:
without preliminary drying 100
E
mass, in grammes, of the test sample, in grammes, of the dry test sample.
with preliminary drying - m)M ] 100 ( Mm ) + E - M . = 100 1 -M' E EM'
mass, in grammes, of the test sample, in grammes, of the test sample after preliminary drying, in grammes, of the test sample after crushing or grinding, in grammes, of the dry test sample.
Repeatibility difference between the results of two parallel determinations carried out on sample should not exceed 0ꞏ2% of moisture.