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Commission Regulation (EC) No 152/2009 of 27 January 2009 laying down the methods of sampling and analysis for the official control of feed (Text with EEA relevance)
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Article 1.Sampling for the official control of feed, as regards the...
Article 2.Preparation of samples for analysis and expression of results shall...
Article 3.Analysis for the official control of feed shall be carried...
Article 4.The energy value of compound poultry feed shall be calculated...
Article 5.The methods of analysis to control illegal presence of no...
Article 6.Directives 71/250/EEC, 71/393/EEC, 72/199/EEC, 73/46/EEC, 76/371/EEC, 76/372/EEC, 78/633/EEC, 81/715/EEC, 84/425/EEC,...
Article 7.This Regulation shall enter into force on the twentieth day...
METHODS OF ANALYSIS TO CONTROL THE COMPOSITION OF FEED MATERIALS AND COMPOUND FEED
3.1. Crusher of non-moisture-absorbing material which is easy to clean, allows...
3.3. Dry containers of non-corrodible metal or of glass with lids...
3.4. Electrically heated isothermal oven (± 2 oC) properly ventilated and ensuring...
3.5. Adjustable electrically heated vacuum oven fitted with an oil pump...
3.6. Desiccator with a thick perforated metal or porcelain plate, containing...
B. DETERMINATION OF MOISTURE IN ANIMAL AND VEGETABLE FATS AND OILS...
C. DETERMINATION OF THE CONTENT OF CRUDE PROTEIN
3.2. Catalyst: copper (II) oxide CuO or copper (II) sulphate pentahydrate,...
3.5. Sulphuric acid, standard volumetric solution, c(H2SO4) = 0,25 mol/l.
3.6. Sulphuric acid, standard volumetric solution, c(H2SO4) = 0,1 mol/l.
3.7. Sulphuric acid, standard volumetric solution, c(H2SO4) = 0,05 mol/l.
3.8. Methyl red indicator; dissolve 300 mg of methyl red in...
3.9. Sodium hydroxide solution (Technical grade may be used) β =...
3.10. Sodium hydroxide, standard volumetric solution c(NaOH) = 0,25 mol/l.
3.11. Sodium hydroxide, standard volumetric solution c(NaOH) = 0,1 mol/l.
3.12. Granulated pumice stone, washed in hydrochloric acid and ignited.
3.16. Methyl red indicator solution: dissolve 100 mg methyl red in...
3.17. Bromocresol green solution: dissolve 100 mg bromocresol green in 100...
3.18. Boric acid solution (10 g/l to 40 g/l depending on the apparatus...
3.19. Hydrochloric acid standard volumetric solution c(HCl) = 0,1 mol/l.
F. DETERMINATION OF AMINO ACIDS (EXCEPT TRYPTOPHANE)
3.13. Norleucine, or other compound suitable for use as internal standard....
3.16.1. Standard substances listed under paragraph 1. Pure compounds containing no water...
3.20. Hydrolysis mixture, c = 6 mol HCl/l containing 1 g phenol/l:...
3.21. Extraction mixture, c = 0,1 mol HCl/l containing 2 % thiodiglycol:...
3.25. Elution buffers, prepared according to conditions for the analyser used...
3.26. Ninhydrin reagent, prepared according to conditions for the analyser used...
3.27. Standard solutions of amino acids. These solutions shall be stored...
3.27.2. Stock standard solution of cysteic acid and methionine sulphone, c...
3.27.3. Stock standard solution of the internal standard e.g. norleucine, c...
3.27.4. Calibration solution of standard amino acids for use with hydrolysates,...
3.27.5. Calibration solution of standard amino acids for use with hydrolysates...
G. DETERMINATION OF TRYPTOPHAN
3.1. Double distilled water or water of equivalent quality must be...
3.2. Standard substance: tryptophan (purity/content ≥ 99 %) dried under vacuum over...
3.3. Internal standard substance: α-methyl-tryptophan (purity/content ≥ 99 %), dried under vacuum...
3.4. Barium hydroxide octa-hydrate (care shall be taken not to expose...
3.15. Concentrated solution of tryptophan (3.2), c = 2,5 μmol/ml:
3.16. Concentrated internal standard solution, c = 2,5 μmol/ml:
3.17. Calibration standard solution of tryptophan and internal standard:
3.21. Solution of 1 g 1,1,1-trichloro-2-methyl-2-propanol (3.19) in 100 ml methanol (3.8)....
3.22. Mobile phase for HPLC: 3,0 g acetic acid (3.18) + 900...
I. DETERMINATION OF CRUDE FIBRE
4.1. Heating unit for digestion with sulphuric acid and potassium hydroxide...
4.2. Glass filter crucible with fused sintered glass filter plate pore...
4.3. Cylinder of at least 270 ml with a reflux condenser,...
4.6. Extraction unit consisting of a support plate for the filter...
4.7. Connecting rings to assemble the heating unit (4.1), crucible (4.2)...
8.1. Feed containing more than 10 % crude fat must be defatted...
8.2. Feed containing fats which cannot be extracted directly with light...
8.3. If the feed contains over 5 % of carbonates, expressed as...
8.5. If after boiling it is difficult to filter the acidic...
8.6. The temperature for ashing shall not be higher than 500 oC...
3.1. Ethanol solution 40 % (v/v) density: 0,948 g/ml at 20 oC, neutralised to...
3.2. Carrez solution I: dissolve in water 21,9 g of zinc acetate...
3.3. Carrez solution II: dissolve in water 10,6 g of potassium ferrocyanide...
3.8.1. Copper sulphate solution: dissolve 25 g of copper sulphate, Cu SO4...
3.8.2. Citric acid solution: dissolve 50 g of citric acid, C6H8O7·H2O in...
3.8.3. Sodium carbonate solution: dissolve 143,8 g of anhydrous sodium carbonate in...
3.10. Starch solution: add a mixture of 5 g of soluble starch...
3.13. Granulated pumice stone boiled in hydrochloric acid, washed in water...
8.2. The difference between the content of total sugars after inversion,...
8.3. In order to determine the content of reducing sugars, excluding...
8.3.1. For an approximate calculation, multiply by 0,675 the lactose content...
8.3.2. For an accurate calculation of reducing sugars, excluding lactose, the...
3.1. Suspension of Saccharomyces cerevisiae: suspend 25 g of fresh yeast in...
3.2. Carrez solution I: dissolve in water 21,9 g of zinc acetate,...
3.3. Carrez solution II: dissolve in water 10,6 g of potassium ferrocyanide...
3.4.1. Copper sulphate solution: dissolve 25 g of copper sulphate Cu SO4...
3.4.2. Citric acid solution: dissolve 50 g of citric acid C6H8O7·H2O in...
3.4.3. Sodium carbonate solution: dissolve 143,8 g of anhydrous sodium carbonate in...
3.5. Granulated pumice stone boiled in hydrochloric acid, washed in water...
3.9. Starch solution: add a mixture of 5 g of soluble starch...
N. DETERMINATION OF ASH WHICH IS INSOLUBLE IN HYDROCHLORIC ACID
O. DETERMINATION OF CARBONATES
P. DETERMINATION OF TOTAL PHOSPHORUS
3.2. Hydrochloric acid, ρ20 = 1,1 g/ml (approx 6 mol/litre).
3.6. Molybdovanadate reagent: mix 200 ml of ammonium heptamolybdate solution (3.6.1),...
3.6.1. Ammonium heptamolybdate solution: dissolve in hot water 100 g of ammonium...
3.6.2. Ammonium monovanadate solution: dissolve 2,35 g of ammonium monovanadate NH4VO3 in...
3.7. Standard solution of 1 mg phosphorus per ml: dissolve 4,387 g...
METHODS OF ANALYSIS TO CONTROL THE LEVEL OF AUTHORISED ADDITIVES IN FEED
3.5. Sodium ascorbate solution, c = 10 g/100 ml (see 7.7 observations)...
3.6.1. Sodium sulphide solution, c = 0,5 mol/l in glycerol, ß...
3.7. Phenolphthalein solution, c = 2 g/100 ml in ethanol (3.1)
3.9. Mobile phase for HPLC: mixture of methanol (3.3) and water,...
3.11. All-trans-vitamin A acetate, extra pure, of certified activity, e.g. 2,8...
3.11.1. Stock solution of all-trans-vitamin A acetate: Weigh to the nearest...
3.12. All-trans-vitamin A palmitate, extra pure, of certified activity, e.g. 1,8...
3.12.1. Stock solution of all-trans-vitamin A palmitate: Weigh to the nearest...
3.13. 2,6-Di-tert-butyl-4-methylphenol (BHT) (see 7.5 observations)
4.2.1. Flat bottom or conical flasks, 500 ml, with ground-glass socket...
4.2.2. Graduated flasks with ground-glass stoppers, narrow-necked, 10, 25, 100 and...
4.2.3. Separating funnels, conical, 1 000 ml, with ground-glass stoppers
4.2.4. Pear shaped flasks, 250 ml, with ground-glass sockets
4.3. Allihn condenser, jacket length 300 mm, with ground-glass joint, with adapter...
4.4. Pleated filter paper for phase separation, diameter 185 mm (e.g. Schleicher...
4.5.1. Liquid chromatographic column, 250 mm x 4 mm, C18, 5 or 10...
4.5.2. UV or fluorescence detector, with variable wavelength adjustment
4.8.1. Glass cylinder of 1 l capacity fitted with a ground...
4.8.2. Ground glass insert equipped with a side-arm and an adjustable...
7.1. For samples with low vitamin A concentration it may be...
7.2. The weight of the sample taken for the analysis shall...
7.3. If phase separation does not occur add approximately 10 ml...
7.4. With cod-liver oil and other pure fats the saponification time...
7.6. Using a normal phase-column the separation of retinol isomers is...
7.7. Approximately 150 mg ascorbic acid can be used instead of...
7.8. Approximately 50 mg EDTA can be used instead of sodium...
7.9. In cases of analysis of vitamin A in milk replacers,...
3.5. Sodium ascorbate solution, c = 10 g/100 ml (see 7.7 observations)....
3.6.1. Sodium sulphide solution, c = 0,5 mol/l in glycerol, β...
3.7. Phenolphthalein solution, c = 2 g/100 ml in ethanol (3.1).
3.8. Mobile phase for HPLC: mixture of methanol (3.3) and water,...
3.10. DL-α-tocopherol acetate, extra pure, of certified activity.
3.10.1. Stock solution of DL-α-tocopherol acetate: Weigh to the nearest 0,1 mg,...
3.11.1. Stock solution of DL-α-tocopherol: Weigh to the nearest 0,1 mg,...
3.12. 2,6-Di-tert-butyl-4-methylphenol (BHT) (see 7.5 observations).
4.2.1. Flat bottom or conical flasks, 500 ml, with ground-glass socket....
4.2.2. Graduated flasks with ground-glass stoppers, narrow-necked, 10, 25, 100 and...
4.2.3. Separating funnels, conical, 1 000 ml, with ground-glass stoppers.
4.2.4. Pear shaped flasks, 250 ml, with ground-glass sockets.
4.3. Allihn condenser, jacket length 300 mm, with ground-glass joint, with adapter...
4.4. Pleated filter paper for phase separation, diameter 185 mm (e.g. Schleicher...
4.5.1. Liquid chromatographic column, 250 mm × 4 mm, C18, 5 or 10...
4.5.2. Fluorescence or UV detector, with variable wavelength adjustment.
4.8.1. Glass cylinder of 1 l capacity fitted with a ground...
4.8.2. Ground glass insert equipped with a side-arm and an adjustable...
7.1. For samples with low vitamin E concentration it may be...
7.2. The weight of the sample taken for the analysis shall...
7.3. If phase separation does not occur add approximately 10 ml...
7.4. After the spectrophotometric measurement of the DL-α-tocopherol acetate or DL-α-tocopherol...
7.6. Using a normal phase-column the separation of α-, β-, γ-...
7.7. Approximately 150 mg ascorbic acid can be used instead of...
7.8. Approximately 50 mg EDTA can be used instead of sodium...
7.9. Vitamin E acetate hydrolyses very fast under alkaline conditions and...
C. DETERMINATION OF THE TRACE ELEMENTS IRON, COPPER, MANGANESE AND ZINC...
3.6. Hydrogen peroxide (approximately 100 volumes of oxygen (30 % by weight))....
3.7. Standard iron solution (1 000 μg Fe/ml) prepared as follows...
3.7.1. Working standard iron solution (100 μg Fe/ml) prepared by diluting...
3.8. Standard copper solution (1 000 μg Cu/ml) prepared as follows...
3.8.1. Working standard copper solution (10 μg Cu/ml) prepared by diluting...
3.9. Standard manganese solution (1 000 μg Mn/ml) prepared as follows...
3.9.1. Working standard manganese solution (10 μg Mn/ml) prepared by diluting...
3.10. Standard zinc solution (1 000 μg Zn/ml) prepared as follows...
3.10.1. Working standard zinc solution (10 μg Zn/ml) prepared by diluting...
3.11. Lanthanum chloride solution: dissolve 12 g of lanthanum oxide in 150...
D. DETERMINATION OF HALOFUGINONE
E. DETERMINATION OF ROBENIDINE
F. DETERMINATION OF DICLAZURIL
G. DETERMINATION OF LASALOCID SODIUM
METHODS OF ANALYSIS TO CONTROL UNDESIRABLE SUBSTANCES IN FEED
A. DETERMINATION OF FREE AND TOTAL GOSSYPOL
3.1. Propan-2-ol-hexane mixture: mix 60 parts by volume of propan-2-ol with...
3.2. Solvent A: Place in a 1 litre graduated flask approximately...
3.3. Solvent B: Pipette 2 ml of 3-aminopropan-1-ol and 10 ml...
3.4. Aniline: If the optical density in the blank test exceeds...
3.5. Standard gossypol solution A: Place 27,9 mg of gossypol acetate...
3.6. Standard gossypol solution B: Place 27,9 mg of gossypol acetate...
(B) DETERMINATION OF THE LEVELS OF DIOXINS (PCDD/PCDF) AND DIOXIN-LIKE PCBs...
I. METHODS OF SAMPLING AND INTERPRETATION OF ANALYTICAL RESULTS
II. SAMPLE PREPARATION AND REQUIREMENTS FOR METHODS OF ANALYSIS USED IN...
5.1. Analytical balance (accuracy of 0,01 g except for the concentrated sediment:...
5.2. Material for grinding (grinding mill or a mortar, especially for...
5.3. Sieve fitted with sieve mesh with square meshes of width...
5.6. Compound microscope (minimum 400' magnification), transmitted light or polarised light....
METHODS OF ANALYSIS TO CONTROL ILLEGAL PRESENCE OF NO LONGER AUTHORISED ADDITIVES IN FEED
A. DETERMINATION OF METHYL BENZOQUATE
B. DETERMINATION OF OLAQUINDOX
4.3. Glass column (length 300 to 400 mm, internal diameter approximately 10 mm)...
4.4. HPLC equipment with injection system, suitable for injection volumes of...
4.4.1. Liquid chromatographic column: 300 mm x 4 mm, C18, 10 μm packing...
4.4.2. UV detector with variable wavelength adjustment or diode array detector...
CORRELATION TABLES REFERRED TO IN ARTICLE 6
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