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Commission Regulation (EC) No 273/2008 (repealed)Show full title

Commission Regulation (EC) No 273/2008 of 5 March 2008 laying down detailed rules for the application of Council Regulation (EC) No 1255/1999 as regards methods for the analysis and quality evaluation of milk and milk products (repealed)

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  1. Introductory Text

  2. CHAPTER I GENERAL PROVISIONS

    1. Article 1.Subject matter and scope

    2. Article 2.Routine methods

  3. CHAPTER II METHODS OF ANALYSIS

    1. Article 3.Evaluation of compliance of a consignment with a legal limit

    2. Article 4.Sensory evaluation

    3. Article 5.Tracers

    4. Article 6.Detection of cows’ milk casein

    5. Article 7.Detection of coliforms

    6. Article 8.Determination of the lactose content

    7. Article 9.Detection of rennet whey

    8. Article 10.Detection of buttermilk

    9. Article 11.Detection of antimicrobiotic residues

    10. Article 12.Determination of skimmed-milk powder content

    11. Article 13.Detection of starch

    12. Article 14.Determination of moisture content in dried cream

    13. Article 15.Determination of moisture content of acid buttermilk powder

    14. Article 16.Determination of milk fat purity

  4. CHAPTER III GENERAL AND FINAL PROVISIONS

    1. Article 17.Quality assurance

    2. Article 18.Sampling and disputes over the results of analysis

    3. Article 19.Transition period

    4. Article 20.Repeals

    5. Article 21.Entry into force

  5. Signature

    1. ANNEX I

      (Article 1)

      1. LIST OF REFERENCE METHODS

        2. Notes to list of European Union reference methods:

    2. ANNEX II

      (Article 3)

      1. EVALUATION OF COMPLIANCE OF A CONSIGNMENT WITH THE LEGAL LIMIT...

        1. 1. PRINCIPLE

        2. 2. THE METHOD IS VALIDATED THROUGH INTERNATIONAL COLLABORATION

        3. 3. IN-HOUSE VALIDATION WITH CALCULATION OF INTERNAL REPRODUCIBILITY STANDARD DEVIATION

    3. ANNEX III

      (Article 4)

      1. EVALUATION OF ASSESSORS AND THE RELIABILITY OF RESULTS IN SENSORY...

        2. A. DETERMINATION OF THE ‘REPEATABILITY INDEX’

        3. B. DETERMINING THE ‘DEVIATION INDEX’

        4. C. COMPARISON OF THE RESULTS OBTAINED IN DIFFERENT REGIONS OF A...

    4. ANNEX IV

      (Article 4)

      1. SENSORY EVALUATION OF BUTTER

        1. 1. SCOPE

        2. 2. DEFINITIONS

        3. 3. TEST ROOM

        4. 4. SELECTION OF ASSESSORS

          2. 4.1. ISO/DIS 22935-1 | IDF 99-1 par 4 (recruitment) and par...

          3. 4.2. Initial training should cover the following:

        5. 5. REQUIREMENTS FOR THE PANEL

        6. 6. PERFORMANCE

        7. 7. SAMPLING AND PREPARATION OF THE SAMPLE

        8. 8. ASSESSMENT OF THE VALUE OF EACH ATTRIBUTE

          1. 8.1. The sensory evaluation is to be carried out in relation...

          2. 8.2. Each attribute has to be sensory evaluated separately. The scoring...

          3. 8.3. It may be desirable for the assessors to score together,...

          4. 8.4. Scoring for acceptance is as follows:

        9. 9. SUPERVISION

        10. 10. NOMENCLATURE

        11. 11. REFERENCE

    5. ANNEX V

      (Article 5)

      1. DETERMINATION OF THE CONTENT OF ENANTHIC ACID TRIGLYCERIDE IN BUTTER,...

        1. 1. SCOPE

        2. 2. TERMS AND DEFINITION

        3. 3. PRINCIPLE

        4. 4. REAGENTS

          2. 4.1. n-Hexane

          3. 4.2. Standard triglyceride of caproic acid, at least 99 % pure

          4. 4.3. Standard triglyceride of enanthic acid, at least 99 % pure

          5. 4.4. Anhydrous sodium sulfate (Na2SO4).

        5. 5. APPARATUS

          2. 5.1. Analytical balance precise at 1 mg

          3. 5.2. Volumetric flasks, of capacities 10 ml and 20 ml

          4. 5.3. Tubes for centrifuge, of capacity 30 ml

          5. 5.4. Rotary evaporator

          6. 5.5. Oven, capable of being maintained at a temperature of 50 °C...

          7. 5.6. Filter paper, medium porosity, of diameter about 15 cm

          8. 5.7. Gas chromatography equipment

            2. 5.7.1. Gas chromatograph equipped with a split/splitless or on-column injector and...

            3. 5.7.2. GC column, with a stationary phase which has successfully employed...

              2. 5.7.2.1. Example of applicable conditions using a split injector:

              3. 5.7.2.2. Example of applicable conditions using an on-column injector:

          9. 5.8. Injection syringe, of capacity 5 μl.

        6. 6. SAMPLING

        7. 7. PROCEDURE

          1. 7.1. Preparation of the test sample and test portion

            2. 7.1.1. Butter-oil, Butter

              1. 7.1.1.1. Melt 50 g to 100 g of test sample in the oven (5.5)...

              2. 7.1.1.2. Place 0,5 g to 1,0 g of anhydrous sodium sulfate (5.4) in a...

              3. 7.1.1.3. Filter the fat through the filter paper containing anhydrous sodium...

            3. 7.1.2. Cream

              1. 7.1.2.1. Bring the test sample to a temperature of 20 °C ±...

              2. 7.1.2.2. Mix or stir the sample thoroughly

              3. 7.1.2.3. Dilute a suitable amount of test sample so as to...

              4. 7.1.2.4. Proceed as with raw milk and homogenized milk (see ISO...

              5. 7.1.2.5. Weigh in a 10 ml volumetric flask (5.2), to the nearest...

              6. 7.1.2.6. Introduce 1 ml of the solution 7.1.1.2 in a 10 ml volumetric...

          2. 7.2. Preparation of the calibration standards

            1. 7.2.1. Dissolve 100 mg of the triglyceride of enanthic acid (4.3) in...

            2. 7.2.2. Dissolve 100 mg of the triglyceride of caproic acid (4.2) in...

            3. 7.2.3. Introduce 1 ml of the solution 7.2.2 in a 10 ml volumetric...

            4. 7.2.4. Introduce 1 ml of the solution 7.2.1 and 1 ml of the solution...

            5. 7.2.5. Introduce 1 ml of the solution 7.2.4 in a 10 ml volumetric...

          3. 7.3. Chromatographic determination

            1. 7.3.1. Inject 1 μl of the standard solution 7.2.5 twice

            2. 7.3.2. Inject 1 μl of each sample solution

            3. 7.3.3. Repeat the operation 7.3.1 every 3 samples in order to...

        8. 8. CALCULATION OF RESULTS

          2. 8.1. Calibration

            1. 8.1.1. Calculate the response factor for each duplicate of STD1, Rf1(a)...

            2. 8.1.2. Similarly, calculate the mean average response factor STD2, Rf2

            3. 8.1.3. Calculate the mean average response factor, Rf

          3. 8.2. Test samples

        9. 9. PRECISION

          2. 9.1. Repeatability

          3. 9.2. Reproducibility

        10. 10. TOLERANCE LIMITS: LOWER LIMITS (CASE OF INSUFFICIENT QUANTITIES)

          1. 10.1. Three samples must be taken from the traced product in...

          2. 10.2. Butter and concentrated butter

            1. 10.2.1. The incorporation rate is 11 kg of at least 95 % pure...

            2. 10.2.2. The results of three samples obtained from the analysis of...

          3. 10.3. Cream

            1. 10.3.1. The incorporation is 10 kg of at least 95 % pure enanthic...

            2. 10.3.2. The results of the three samples obtained from the analysis...

        11. 11. TOLERANCE LIMITS: UPPER LIMITS (CASE OF EXCEEDING QUANTITY BY MORE...

          1. 11.1. Three samples must be taken from the traced product in...

          2. 11.2. Butter and concentrated butter

            1. 11.2.1. The results of three samples obtained from the analysis of...

          3. 11.3. Cream

            1. 11.3.1. The results of three samples obtained from the analysis of...

        12. 12. ADDITIONAL INFORMATION: STATISTICAL ANALYSIS OF RESULTS ON THE DETERMINATION OF...

          2. Tests for outliers:

          3. Precision parameters

          4. Figure 1

            1. Experimental results: Sample A

            2. Experimental results: Sample B

            3. Experimental results: Sample C

            4. Experimental results: Sample D

    6. ANNEX VI

      (Article 5)

      1. DETERMINING THE VANILLIN CONTENT IN CONCENTRATED BUTTER, BUTTER OR CREAM...

        1. 1. SCOPE AND FIELD OF APPLICATION

        2. 2. PRINCIPLE

        3. 3. APPARATUS

          2. 3.1. Freezer, operating in the temperature range -15 °C to -20 °C

          3. 3.2. Syringes, disposable of 2 ml capacity

          4. 3.3. Membrane microfilters of 0,45 μm pore size, resistant to a...

          5. 3.4. Liquid chromatography system consisting of a pump (flow of 1,0...

          6. 3.5. Analytical column (250 mm × 4,6 mm ID) packed with LiChrospher RP...

          7. 3.6. Guard column (ca. 20 mm × 3 mm ID) dry-packed with LiChrospher...

          8. 3.7. Centrifuge operating at 2 000 rpm.

        4. 4. REAGENTS

          2. 4.1. Isopropanol

          3. 4.2. Ethanol 96 % (v/v)

          4. 4.3. Acetonitrile

          5. 4.4. Extraction solution

          6. 4.5. Vanillin (4-hydroxy-3-methoxybenzaldehyde) ≥ 98 %

            2. 4.5.1. Vanillin stock solution (= 500 μg/ml)

            3. 4.5.2. Vanillin standard solution (= 10 μg/ml)

            4. 4.5.3. Methanol, HPLC quality

            5. 4.5.4. Acetic acid, glacial

            6. 4.5.5. Water, HPLC quality

            7. 4.5.6. HPLC mobile phase

        5. 5. PROCEDURE

          1. 5.1. Preparation of the test sample

            1. 5.1.1. Butter

            2. 5.1.2. Concentrated butter

            3. 5.1.3. Cream

          2. 5.2. Preparation of the test solution

          3. 5.3. Calibration

          4. 5.4. Determination by HPLC

        6. 6. CALCULATION OF THE RESULTS

        7. 7. ACCURACY OF THE METHOD

          1. 7.1. Repeatability (r)

          2. 7.2. Reproducibility (R)

        8. 8. TOLERANCE LIMITS

          1. 8.1. Three samples must be taken from the traced product in...

          2. 8.2. Tracer obtained either from vanilla or from synthetic vanillin

            2. 8.2.1. The incorporation rate for 4-hydroxy-3-methoxybenzaldehyde is 250 g per tonne of...

            3. 8.2.2. The results for the three samples obtained from the analysis...

          3. 8.3. Tracer obtained exclusively from vanilla beans or integral extracts thereof:...

            2. 8.3.1. The incorporation rate for 4-hydroxy-3-methoxybenzaldehyde is 100 g per tonne of...

            3. 8.3.2. The results for the three samples obtained from the analysis...

        9. 9. NOTES

          1. 9.1. Recovery of added vanillin at a level of 250 mg/kg...

          2. 9.2. The standard solution contains 5 % extraction solution to compensate for...

          3. 9.3. The analysis is based on a linear calibration line with...

          4. 9.4. By using appropriate dilutions of the standard solution (4.5.2), the...

    7. ANNEX VII

      (Article 5)

      1. DETERMINING THE ETHYL ESTER OF BETA-APO-8'-CAROTENIC ACID IN CONCENTRATED BUTTER...

        1. 1. SCOPE AND FIELD OF APPLICATION

        2. 2. PRINCIPLE

        3. 3. APPARATUS

          1. 3.1. Pipettes — graduated, of capacity 0,25, 0,50, 0,75 and 1,0 ml

          2. 3.2. Spectrophotometer — suitable for use at 440 nm (and 447-449 nm) and...

          3. 3.3. Volumetric flasks, 20 ml and 100 ml

          4. 3.4. Analytical balance, sensitivity 0,1 mg capable of weighing to the nearest...

          5. 3.5. Oven, 45 °C ± 1 °C

          6. 3.6. Fast-filtering ashless filters.

        4. 4. REAGENTS

          2. 4.1. Apo-carotenic ester suspension (approximately 20 %)

            2. 4.1.1. Establish the content of the suspension as follows:

            3. 4.1.2. Apo-carotenic ester standard solution, approx. 0,2 mg/ml

          3. 4.2. Petroleum spirit (40-60 °C)

          4. 4.3. Sodium sulphate, anhydrous, granular, previously dried at 102 °C for two...

          5. 4.4. Chloroform

          6. 4.5. Cyclohexane

        5. 5. PROCEDURE

          1. 5.1. Preparation of the test sample

            1. 5.1.1. Concentrated butter

            2. 5.1.2. Butter

          2. 5.2. Determination

          3. 5.3. Calibration

        6. 6. CALCULATION OF THE RESULTS

          1. 6.1. Apo-carotenic ester content, expressed as mg/kg product, is given by:...

        7. 7. ACCURACY OF THE METHOD

          1. 7.1. Repeatability

            1. 7.1.1. Butter analysis

            2. 7.1.2. Concentrated butter analysis

          2. 7.2. Reproducibility

            1. 7.2.1. Butter analysis

          3. 7.3. Concentrated butter analysis

          4. 7.4. Source of precision data

        8. 8. TOLERANCE LIMITS

          1. 8.1. Three samples must be taken from the traced product in...

          2. 8.2. Butter

            1. 8.2.1. The incorporation rate for butter, taking into account background absorbance,...

            2. 8.2.2. The results for the three samples obtained from the analysis...

          3. 8.3. Concentrated butter

            1. 8.3.1. The incorporation rate for concentrated butter, taking into account background...

    8. ANNEX VIII

      (Article 5)

      1. DETERMINING SITOSTEROL OR STIGMASTEROL IN BUTTER OR CONCENTRATED BUTTER BY...

        1. 1. SCOPE AND FIELD OF APPLICATION

        2. 2. PRINCIPLE

        3. 3. APPARATUS

          1. 3.1. 150 ml saponification flask fitted with a reflux condenser having ground-glass...

          2. 3.2. 500 ml separating funnels

          3. 3.3. 250 ml flasks

          4. 3.4. Pressure equalising funnels, 250 ml or similar, to collect waste diethyl...

          5. 3.5. Glass column, 350 mm × 20 mm fitted with sintered glass plug...

          6. 3.6. Waterbath or isomantle

          7. 3.7. Reaction vials, 2 ml

          8. 3.8. Gas chromatograph suitable for use with a capillary column, provided...

            2. 3.8.1. a thermostatic chamber for columns capable of maintaining the desired...

            3. 3.8.2. a temperature-adjustable vaporisation unit

            4. 3.8.3. a flame ionisation detector and converter-amplifier

            5. 3.8.4. an integrator-recorder suitable for use with the converter-amplifier (3.8.3)

          9. 3.9. A fused-silica capillary column entirely coated with BP1 or equivalent...

          10. 3.10. A 1 μl gas chromatography microsyringe with hardened needle.

        4. 4. REAGENTS

          2. 4.1. Ethanol, at least 95 % pure

          3. 4.2. Potassium hydroxide, 60 % solution, dissolve 600 g potassium hydroxide (minimum 85 %)...

          4. 4.3. Betulin of at least 99 % purity

            2. 4.3.1. Solutions of betulin in diethyl ether (4.4)

              2. 4.3.1.1. The concentration of betulin solution used for sitosterol determination should...

              3. 4.3.1.2. The concentration of betulin solution used for stigmasterol determination should...

          5. 4.4. Diethyl ether, analytical purity (free from peroxides or residue)

          6. 4.5. Sodium sulphate, anhydrous, granular, previously dried at 102 °C for two...

          7. 4.6. Silylating reagent, for example TRI-SIL (available from Pierce Chemical Co,...

          8. 4.7. Lanosterol

          9. 4.8. Sitosterol, of known purity not less than 90 % pure (P)...

            2. 4.8.1. Sitosterol standard solution — prepare a solution containing, to the...

          10. 4.9. Stigmasterol, of known purity not less than 90 % pure (P)...

            2. 4.9.1. Stigmasterol standard solution — prepare a solution containing, to the...

          11. 4.10. Resolution test mixture. Prepare a solution containing 0,05 mg/ml lanosterol...

        5. 5. METHOD

          1. 5.1. Preparation of standard solutions for chromatography

            2. 5.1.1. Sitosterol standard chromatographic solution: transfer 1 ml of sitosterol standard solution...

            3. 5.1.2. Stigmasterol standard chromatographic solution: transfer 1 ml of stigmasterol standard solution...

          2. 5.2. Preparation of the unsaponifiables

            1. 5.2.1. Melt the butter sample at a temperature not exceeding 35 °C,...

            2. 5.2.2. Add 1,0 ml of internal standard solution (4.3.1.1) to the flask...

            3. 5.2.3. Pass the clear, soap-free ether layer through a glass column...

          3. 5.3. Preparation of trimethyl silyl ethers

            1. 5.3.1. Transfer the ether solution remaining in the flask to a...

            2. 5.3.2. Silylate the sample by addition of 1 ml TRI-SIL (4.6). Close...

          4. 5.4. Gas-chromatographic analysis

            1. 5.4.1. Choice of operating conditions

            2. 5.4.2. Analytical procedure

        6. 6. CALCULATION OF RESULTS

          1. 6.1. Determine the area of the sterol peaks and betulin peaks...

        7. 7. ACCURACY OF THE METHOD

          1. 7.1. Butter

            1. 7.1.1. Repeatability

              1. 7.1.1.1. Stigmasterol

              2. 7.1.1.2. Sitosterol

            2. 7.1.2. Reproducibility

              1. 7.1.2.1. Stigmasterol

              2. 7.1.2.2. Sitosterol

            3. 7.1.3. Source of precision data

          2. 7.2. Concentrated butter

            1. 7.2.1. Repeatability

              1. 7.2.1.1. Stigmasterol

              2. 7.2.1.2. Sitosterol

            2. 7.2.2. Reproducibility

              1. 7.2.2.1. Stigmasterol

              2. 7.2.2.2. Sitosterol

            3. 7.2.3. Source of precision data

        8. 8. TOLERANCE LIMITS

          1. 8.1. Three samples must be taken from the traced product in...

          2. 8.2. Butter

            1. 8.2.1. Stigmasterol

              1. 8.2.1.1. The incorporation rate for stigmasterol is 150 g of at least...

              2. 8.2.1.2. The results for the three samples obtained from the analysis...

            2. 8.2.2. Sitosterol

              1. 8.2.2.1. The incorporation rate for sitosterol is 600 g of at least...

              2. 8.2.2.2. The results for the three samples obtained from the analysis...

          3. 8.3. Concentrated butter

            1. 8.3.1. Stigmasterol

              1. 8.3.1.1. The incorporation rate for stigmasterol is 150 g of at least...

              2. 8.3.1.2. The results for the three samples obtained from the analysis...

            2. 8.3.2. Sitosterol

              1. 8.3.2.1. The incorporation rate for sitosterol is 600 g of at least...

              2. 8.3.2.2. The results for the three samples obtained from the analysis...

    9. ANNEX IX

      (Article 6)

      1. REFERENCE METHOD FOR THE DETECTION OF COWS’ MILK AND CASEINATE...

        1. 1. SCOPE

        2. 2. FIELD OF APPLICATION

        3. 3. PRINCIPLE OF THE METHOD

          1. 3.1. Isolation of caseins from cheese and the reference standards

          2. 3.2. Dissolving of the isolated caseins and submitting to plasmin (EC.3.4.21.7)...

          3. 3.3. Isoelectric focusing of plasmin-treated caseins in the presence of urea...

          4. 3.4. Evaluation of stained γ3 and γ2-casein patterns (evidence of cows’...

        4. 4. REAGENTS

          2. Isoelectric focusing

            1. 4.1. Reagents for production of the urea containing polyacrylamide gels

              1. 4.1.1. Stock gel solution

              2. 4.1.2. Gel solution

              3. 4.1.3. Catalyst solutions

                1. 4.1.3.1. N, N, N' N' — tetramethylethylenediamine (Temed)

                2. 4.1.3.2. 40 % w/v ammonium persulphate (PER):

            2. 4.2. Contact fluid

            3. 4.3. Anode solution

            4. 4.4. Cathode solution

          3. Sample preparation

            1. 4.5. Reagents for protein isolation

              1. 4.5.1. Dilute acetic acid (25,0 ml of glacial acetic acid made up...

              2. 4.5.2. Dichloromethane

              3. 4.5.3. Acetone

            2. 4.6. Protein dissolving buffer

            3. 4.7. Reagents for plasmin cleavage of caseins

              1. 4.7.1. Ammonium carbonate buffer

              2. 4.7.2. Bovine plasmin (EC. 3.4.21.7), activity at least 5 U/ml

              3. 4.7.3. ε-Aminocaproic acid solution for enzyme inhibition

            4. 4.8. Standards

              1. 4.8.1. Certified reference standards of a mixture of renneted ewes’ and...

              2. 4.8.2. Preparation of laboratory interim-standards of buffalos’ renneted milk containing 0 %...

          4. Reagents for protein staining

            1. 4.9. Fixative

            2. 4.10. Destaining solution

            3. 4.11. Staining solutions

              1. 4.11.1. Staining solution (stock solution 1)

              2. 4.11.2. Staining solution (stock solution 2)

              3. 4.11.3. Staining solution (working solution)

        5. 5. EQUIPMENT

          1. 5.1. Glass plates (265 × 125 × 4 mm); rubber roller (width...

          2. 5.2. Gel carrier sheet (265 × 125 mm)

          3. 5.3. Covering sheet (280 × 125 mm). Stick on strip of adhesive...

          4. 5.4. Electrofocusing chamber with cooling plate (e.g. 265 × 125 mm) and...

          5. 5.5. Circulation cryostat, thermostatically controlled at 12 ± 0,5 °C

          6. 5.6. Centrifuge, adjustable to 3 000 g

          7. 5.7. Electrode strips (≥ 265 mm long)

          8. 5.8. Plastic dropping bottles for the anode and cathode solutions

          9. 5.9. Sample applicators (10 × 5 mm, viscose or low protein-adsorption filter...

          10. 5.10. Stainless steel scissors, scalpels and tweezers

          11. 5.11. Stainless steel or glass staining and destaining dishes (e.g. 280...

          12. 5.12. Adjustable rod homogenizer (10 mm shaft diameter), rpm range 8 000...

          13. 5.13. Magnetic stirrer

          14. 5.14. Ultrasonic bath

          15. 5.15. Film welder

          16. 5.16. 25 μl micropipettes

          17. 5.17. Vacuum concentrator or freeze-dryer

          18. 5.18. Thermostatically controlled water bath adjustable to 35 and 40 ± 1 °C with...

          19. 5.19. Densitometer equipment reading at λ = 634 nm

        6. 6. PROCEDURE

          1. 6.1. Sample preparation

            1. 6.1.1. Isolation of caseins

            2. 6.1.2. Plasmin cleavage of β-caseins to intensify γ-caseins

          2. 6.2. Preparation of the urea containing polyacrylamide gels

          3. 6.3. lsoelectric focusing

            2. Conditions for isoelectric focusing:

              1. 6.3.1. Gel size 265 × 125 × 0,25 mm

              2. 6.3.2. Example of a voltage programme for an automatic electrophoresis device...

          4. 6.4. Protein staining

            1. 6.4.1. Protein fixation

            2. 6.4.2. Washing and staining the gel plate

            3. 6.4.3. Destaining the gel plate

        7. 7. EVALUATION

          2. 7.1. Visual estimation

          3. 7.2. Densitometric estimation

        8. 8. REFERENCES

    10. ANNEX X

      (Article 7)

      1. REFERENCE METHOD FOR DETECTING COLIFORMS IN BUTTER, SKIMMED-MILK POWDER, CASEIN...

        1. 1. PREPARATION OF SAMPLES

        2. 2. PROCEDURE

        3. 3. RESULTS

    11. ANNEX XI

      (Article 8)

      1. DETERMINATION OF LACTOSE IN COMPOUND FEEDINGSTUFFS

        1. 1. SCOPE AND FIELD OF APPLICATION

        2. 2. REFERENCE

        3. 3. DEFINITION

        4. 4. PRINCIPLE

        5. 5. REAGENTS

          1. 5.1. General

          2. 5.2. Lactose

          3. 5.3. Concentrated Biggs/Szijarto solution

          4. 5.4. Diluted Biggs/Szijarto solution

          5. 5.5. Preparation of HPLC grade water

        6. 6. APPARATUS

          2. 6.1. HPLC ion exchange resin column

          3. 6.2. Guard column

          4. 6.3. Column oven

          5. 6.4. HPLC pump

          6. 6.5. HPLC injection device

          7. 6.6. HPLC detector

          8. 6.7. Integrator

          9. 6.8. Water purification unit

          10. 6.9. Solvent filtration unit

          11. 6.10. Analytical balance

          12. 6.11. Water bath

          13. 6.12. Centrifuge

          14. 6.13. Volumetric flask 50 mL

          15. 6.14. Volumetric flask 100 mL

          16. 6.15. Graduated pipette

        7. 7. SAMPLING

        8. 8. PREPARATION OF LACTOSE STANDARD SOLUTION

          1. 8.1. Standard 1

          2. 8.2. Standard 2

        9. 9. PREPARATION OF THE TEST SAMPLE

          1. 9.1. Reconstitution of the sample

          2. 9.2. Sample treatment

        10. 10. HPLC DETERMINATION

          1. 10.1. Preliminary preparation of HPLC

            1. 10.1.1. Installation of the column and pre-column

            2. 10.1.2. Detector and initial flow

            3. 10.1.3. Column oven and final flow-rate

            4. 10.1.4. Integration

            5. 10.1.5. Guard column test

          2. 10.2. Running standards

          3. 10.3. Running samples

        11. 11. CALCULATION AND EXPRESSION OF THE RESULTS

          1. 11.1. Calibration

          2. 11.2. Samples

        12. 12. PRECISION

          2. 12.1. Repeatability

          3. 12.2. Reproducibility

        13. 13. REFERENCES

    12. ANNEX XII

      (Article 9)

      1. DETECTION OF RENNET WHEY IN SKIMMED-MILK POWDER FOR PUBLIC STORAGE...

        1. 1. SCOPE AND FIELD OF APPLICATION

        2. 2. REFERENCE

        3. 3. DEFINITION

        4. 4. PRINCIPLE

        5. 5. REAGENTS

          2. 5.1. Trichloroacetic acid solution

          3. 5.2. Eluent solution, pH 6,0

          4. 5.3. Flushing solvent

          5. 5.4. Standard samples

            1. 5.4.1. Skimmed-milk powder meeting the requirements of this Resolution (i.e. [0])...

            2. 5.4.2. The same skimmed-milk powder adulterated with 5 % (m/m) rennet-type whey...

        6. 6. APPARATUS

          1. 6.1. Analytical balance

          2. 6.2. Optional centrifuge capable of attaining a centrifugal force of 2...

          3. 6.3. Mechanical shaker

          4. 6.4. Magnetic stirrer

          5. 6.5. Glass funnels, diameter about 7 cm

          6. 6.6. Filter papers, medium filtration, diameter about 12,5 cm

          7. 6.7. Glass filtration equipment with 0,45 μm pore diameter membrane filter...

          8. 6.8. Graduated pipettes allowing delivery of 10 ml (ISO 648, Class A,...

          9. 6.9. Dispensing system capable of delivering 20,0 ml water at ca. 50 °C...

          10. 6.10. Thermostatic water bath, set at 25 ± 0,5 °C

          11. 6.11. HPLC equipment, consisting of:

            2. 6.11.1. Pump

            3. 6.11.2. Injector, hand or automatic, with a 15 to 30 μl capacity...

            4. 6.11.3. Two TSK 2 000-SW columns in series (length 30 cm, internal...

            5. 6.11.4. Thermostatic column oven, set at 35 ± 1 °C

            6. 6.11.5. Variable wavelength UV detector, permitting measurements at 205 nm with a...

            7. 6.11.6. Integrator capable of valley-to-valley integration

        7. 7. SAMPLING

          1. 7.1. Samples must be taken in accordance with the procedure laid...

          2. 7.2. Store the sample in conditions which preclude any deterioration or...

        8. 8. PROCEDURE

          1. 8.1. Preparation of the test sample

          2. 8.2. Test portion

          3. 8.3. Removal of fat and proteins

            1. 8.3.1. Add 20,0 ml of warm water (50 °C) to the test portion....

            2. 8.3.2. Add 10,0 ml of the trichloroacetic acid solution (5.1) of ca....

            3. 8.3.3. Centrifuge (6.2) for 10 minutes at 2 200 g, or filter through...

          4. 8.4. Chromatographic determination

            1. 8.4.1. Inject 15 to 30 μl of accurately measured supernatant or filtrate...

            2. 8.4.2. The results of chromatographic analysis of the test sample [E]...

          5. 8.5. Calibration

            1. 8.5.1. Apply exactly the procedure described from point 8.2 to point 8.4.2 to...

            2. 8.5.2. Prior to chromatographic determination of the samples, condition the columns...

            3. 8.5.3. Determine the response factors R by injecting the same volume...

        9. 9. EXPRESSION OF RESULTS

          1. 9.1. Method of calculation and formulae

            1. 9.1.1. Calculation of the response factors R:

            2. 9.1.2. Calculation of the relative area of the peaks in the...

            3. 9.1.3. Calculation of the relative retention time of peak III in...

            4. 9.1.4. Experiments have shown that there is a linear relation between...

          2. 9.2. Calculation of the percentage of rennet whey powder in the...

          3. 9.3. Accuracy of the procedure

            1. 9.3.1. Repeatability

            2. 9.3.2. Reproducibility

          4. 9.4. Interpretation

            1. 9.4.1. Assume the absence of whey if the relative area of...

            2. 9.4.2. If the relative area of peak III, SIII [E] is...

            3. 9.4.3. If the relative area of peak III, SIII [E] is...

              2. 9.4.3.1. The data obtained after analysis of samples of unadulterated skimmed-milk...

              3. 9.4.3.2. If T1 and/or T2 are zero or less, the presence...

              4. Skimmed-milk powder

              5. Skimmed-milk powder

    13. ANNEX XIII

      (Article 9)

      1. DETERMINING RENNET WHEY SOLIDS IN SKIMMED-MILK POWDER AND THE MIXTURES...

        1. 1. PURPOSE: DETECTING THE ADDITION OF RENNET WHEY SOLIDS TO:

        2. 2. REFERENCES: INTERNATIONAL STANDARD ISO 707

        3. 3. DEFINITION

        4. 4. PRINCIPLE

        5. 5. REAGENTS

          2. 5.1. Trichloroacetic acid solution

          3. 5.2. Eluents A and B

          4. 5.3. Conservation of the column

          5. 5.4. Standard samples

            1. 5.4.1. Skimmed-milk powder meeting the requirements for public storage (i e....

            2. 5.4.2. The same skimmed-milk powder adulterated with 5 % (m/m) rennet-type whey...

            3. 5.4.3. The same skimmed-milk powder adulterated with 50 % (m/m) rennet-type whey...

        6. 6. APPARATUS

          2. 6.1. Analytical balance

          3. 6.2. Optional centrifuge capable of attaining a centrifugal force of 2...

          4. 6.3. Mechanical shaker

          5. 6.4. Magnetic stirrer

          6. 6.5. Glass funnels, diameter about 7 cm

          7. 6.6. Filter papers, medium filtration, diameter about 12,5 cm

          8. 6.7. Glass filtration equipment with 0,45 μm pore diameter membrane filter...

          9. 6.8. Graduated pipettes, allowing delivery of 10 ml (ISO 648, Class A,...

          10. 6.9. Dispensing system capable of delivering 20,0 ml water at ca. 50 °C...

          11. 6.10. Thermostatic water bath, set at 25 ± 0,5 °C

          12. 6.11. HPLC equipment, consisting of:

            2. 6.11.1. Binary gradient pumping system

            3. 6.11.2. Injector, hand or automatic, with a 100 μl capacity

            4. 6.11.3. Agilent Technologies Zorbax 300 SB-C3 column (length 25 cm, 0,46 cm internal...

            5. 6.11.4. Thermostatic column oven, set at 35 ± 1 °C

            6. 6.11.5. Variable wavelength UV detector, permitting measurements at 210 nm (if necessary,...

            7. 6.11.6. Integrator capable of setting the integration to common baseline or...

        7. 7. SAMPLING

          1. 7.1. Samples must be taken in accordance with the procedure laid...

          2. 7.2. Store the sample in conditions which preclude any deterioration or...

        8. 8. PROCEDURE

          1. 8.1. Preparation of the test sample

          2. 8.2. Test portion

          3. 8.3. Removal of fat and proteins

            1. 8.3.1. Add 20,0 ml of warm water (50 °C) to the test portion....

            2. 8.3.2. Add 10,0 ml of the trichloroacetic acid solution of ca. 25 °C...

            3. 8.3.3. Centrifuge (6.2) 2 200 g for 10 minutes, or filter through paper...

          4. 8.4. Chromatographic determination

            1. 8.4.1. Perform HPLC-analysis as described in Annex XII. If a negative result...

            2. 8.4.2. Before the reversed phase HPLC-analysis is carried out, the gradient...

            3. 8.4.3. Take solutions of the test samples

            4. 8.4.4. The results of the chromatographic analysis of the test sample...

          5. 8.5. Calibration

            1. 8.5.1. Apply exactly the procedure described from point 8.2 to point 8.4.4 to...

            2. 8.5.2. Prior to chromatographic determination of the samples inject 100 μl...

            3. 8.5.3. Determine the response factors R by injecting the same volume...

        9. 9. EXPRESSION OF RESULTS

          1. 9.1. Method of calculation and formulae

            1. 9.1.1. Calculation of the response factor R:

          2. 9.2. Calculation of the percentage of rennet whey powder in the...

          3. 9.3. Accuracy of the procedure

            1. 9.3.1. Repeatability

            2. 9.3.2. Reproducibility

            3. 9.3.3. Linearity

          4. 9.4. Interpretation

            2. Table 1 Ni –4,6 standard

    14. ANNEX XIV

      (Article 10)

      1. SKIMMED-MILK POWDER: QUANTITATIVE DETERMINATION OF PHOSPHATIDYLSERINE AND PHOSPHATIDYLETHANOLAMINE

        2. 1. PURPOSE AND FIELD OF APPLICATION

        3. 2. DEFINITION

        4. 3. PRINCIPLE OF THE METHOD

        5. 4. REAGENTS

          2. 4.1. Standard material: PEDP, at least 99 % pure

          3. 4.2. Reagents for standard sample and test sample preparation

            1. 4.2.1. HPLC-grade methanol

            2. 4.2.2. HPLC-grade chloroform

            3. 4.2.3. Tryptamine-monohydrochloride

          4. 4.3. Reagents for o-phthaldialdehyde derivatisation

            1. 4.3.1. Sodium hydroxide, 12 M water solution

            2. 4.3.2. Boric acid, 0,4 M water solution adjusted to pH 10,0...

            3. 4.3.3. 2-mercaptoethanol

            4. 4.3.4. o-phthaldialdehyde (OPA)

          5. 4.4. HPLC elution solvents

            1. 4.4.1. Elution solvents must be prepared using HPLC-grade reagents.

            2. 4.4.2. HPLC-grade water

            3. 4.4.3. Methanol of fluorimetric tested purity

            4. 4.4.4. Tetrahydrofuran

            5. 4.4.5. Sodium dihydrogen phosphate

            6. 4.4.6. Sodium acetate

            7. 4.4.7. Acetic acid.

        6. 5. APPARATUS

          1. 5.1. Analytical balance, capable of weighing to the nearest 1 mg, with...

          2. 5.2. Beakers, 25 and 100 ml capacity

          3. 5.3. Pipettes, capable of delivering 1 and 10 ml

          4. 5.4. Magnetic stirrer

          5. 5.5. Graduated pipettes, capable of delivering 0,2, 0,5 and 5 ml

          6. 5.6. Volumetric flasks, 10, 50 and 100 ml capacity

          7. 5.7. Syringes, 20 and 100 μl capacity

          8. 5.8. Ultrasonic bath

          9. 5.9. Centrifuge, capable of operating at 27 000 × g

          10. 5.10. Glass vials, about 5 ml capacity

          11. 5.11. Graduated cylinder, 25 ml capacity

          12. 5.12. pH-meter, accurate to 0,1 pH units

          13. 5.13. HPLC equipment

            2. 5.13.1. Gradient pumping system, capable of operating at 1,0 ml/min at...

            3. 5.13.2. Autosampler with derivatisation capability

            4. 5.13.3. Column heater, capable of maintaining the column at 30 °C ±...

            5. 5.13.4. Fluorescence detector, capable of operating at 330 nm excitation wavelength and 440 nm...

            6. 5.13.5. Integrator or data processing software capable of peak area measurement...

            7. 5.13.6. A Lichrosphere — 100 column (250 × 4,6 mm) or an...

        7. 6. SAMPLING

        8. 7. PROCEDURE

          1. 7.1. Preparation of the internal standard solution

            1. 7.1.1. Weigh 30,0 ± 0,1 mg of tryptamine-monohydrochloride (4.2.3) into a 100 ml...

            2. 7.1.2. Pipette 1 ml (5.3) of this solution into a 10 ml volumetric...

          2. 7.2. Preparation of the test sample solution

            1. 7.2.1. Weigh 1,000 ± 0,001 g of the SMP sample into...

            2. 7.2.2. Pipette 0,2 ml (5.5) of the reconstituted milk into a 10 ml...

            3. 7.2.3. Centrifuge (5.9) at 27 000 g × g for 10 minutes...

          3. 7.3. Preparation of the external standard solution

            1. 7.3.1. Weigh 55,4 mg PEDP (4.1) into a 50 ml volumetric flask (5.6)...

            2. 7.3.2. Pipette 1 ml (5.3) of this solution into a 100 ml volumetric...

          4. 7.4. Preparation of the derivatising reagent

          5. 7.5. Determination by HPLC

            1. 7.5.1. Elution solvents (4.4)

            2. 7.5.2. Suggested eluting gradient:

            3. 7.5.3. Injection volume: 50 μl derivatising reagent and 50 μl sample solution...

            4. 7.5.4. Column equilibration

            5. 7.5.5. Determine the PS + PE content in the test sample...

            6. 7.5.6. Perform the sequence of the chromatographic analyses keeping constant the...

          6. 7.6. Integration mode

            1. 7.6.1. PEDP peak

            2. 7.6.2. Tryptamine peak

            3. 7.6.3. PS and PE peaks groups

        9. 8. CALCULATION AND EXPRESSION OF RESULTS

        10. 9. ACCURACY OF THE METHOD

          2. 9.1. Repeatability

          3. 9.2. Reproducibility

        11. 10. REFERENCES

          1. 10.1. Resmini P., Pellegrino L., Hogenboom J.A., Sadini V., Rampilli M.,...

    15. ANNEX XV

      (Article 11)

      1. DETECTION OF ANTIMICROBIAL RESIDUES IN SKIMMED MILK POWDER

        2. Positive results are to be interpreted as follows:

    16. ANNEX XVI

      (Article 12)

      1. QUANTITATIVE DETERMINATION OF SKIMMED-MILK POWDER IN COMPOUND FEEDINGSTUFFS BY ENZYMATIC...

        1. 1. PURPOSE

        2. 2. SCOPE

        3. 3. PRINCIPLE OF THE METHOD

          1. 3.1. Dissolving of casein contained in the compound feedingstuff by extraction...

          2. 3.2. Adjustment of the calcium ion concentration to the required level...

          3. 3.3. The nitrogen content of the para-casein precipitate is determined by...

        4. 4. REAGENTS

          2. 4.1. Trisodium citrate, dihydrate (1 % w/v solution)

          3. 4.2. Calcium chloride (about 5 M solution)

          4. 4.3. 0,1 N sodium hydroxide

          5. 4.4. 0,1 N hydrochloric acid

          6. 4.5. Liquid calf rennet (strength about 100 IMCU/ml according to standard...

          7. 4.6. Reagents for the quantitative determination of nitrogen according to the...

        5. 5. APPARATUS

          2. 5.1. Mortar or homogeniser

          3. 5.2. Analytical balance capable of weighing to the nearest 1 mg, with...

          4. 5.3. Bench-top centrifuge (500 g or 2 000 to 3 000 rpm) with...

          5. 5.4. Magnetic stirrer with (10 to 15 mm) followers

          6. 5.5. 150 to 200 ml beakers

          7. 5.6. 250 and 500 ml flasks

          8. 5.7. Glass funnels of 60 to 80 mm diameter

          9. 5.8. Fast-filtering ashless filters of diameter 150 mm (Whatman No 41 or equivalent)

          10. 5.9. Pipettes of various nominal volume

          11. 5.10. Thermostatically controlled water bath at 37 °C ± 1 °C

          12. 5.11. pH meter, accurate to 0,1 units

          13. 5.12. Thermometers, accurate to 1 °C.

        6. 6. PROCEDURE

          1. 6.1. Preparation of the sample

          2. 6.2. Dissolving of milk powder and separation of the insoluble residue...

            1. 6.2.1. Weigh 1,000 ± 0,002 g of well-homogenised compound feedingstuff (6.1)...

            2. 6.2.2. Centrifuge at 500 g (2 000 to 3 000 rpm) for...

            3. 6.2.3. Carry out two further extractions on the residue, according to...

            4. 6.2.4. If a layer of oil forms at the surface, cool...

          3. 6.3. Coagulation of casein with the enzymes of rennet

            1. 6.3.1. While stirring continuously, add dropwise 2 ml of calcium chloride (4.2)...

            2. 6.3.2. Transfer the liquid into one centrifuge tubes and centrifuge at...

            3. 6.3.3. Bring the temperature of the supernatant back to 37 °C ± 1 °C....

            4. 6.3.4. Return the sample to the water bath and leave at...

          4. 6.4. Determination of casein nitrogen

            1. 6.4.1. After washing, transfer quantitatively the precipitate to the filter paper...

        7. 7. BLANK TEST

          1. 7.1. A blank test shall be made regularly by submitting to...

          2. 7.2. The volume of acid used for the blank test must...

        8. 8. EXPRESSION OF RESULTS

          1. 8.1. The percentage of skimmed-milk powder in the compound feedingstuff is...

        9. 9. ACCURACY OF THE METHOD

          1. 9.1. Repeatability

          2. 9.2. Reproducibility

        10. 10. OBSERVATIONS

          1. 10.1. The addition of large percentages of certain non-milk proteins and...

          2. 10.2. Addition of buttermilk may lead to somewhat low figures, due...

          3. 10.3. Lecithin additions of 0,5 % or more may also lead to...

          4. 10.4. Incorporation of high-heat skimmed-milk powder may lead to too high...

    17. ANNEX XVII

      (Article 13)

      1. DETECTION OF STARCH IN SKIMMED-MILK POWDER, DENATURED MILK POWDER AND...

        1. 1. SCOPE

        2. 2. PRINCIPLE

        3. 3. REAGENTS

          1. 3.1. Iodine solution

        4. 4. APPARATUS

          1. 4.1. Analytical balance

          2. 4.2. Boiling water bath

          3. 4.3. Test tubes, 25 mm × 200 mm.

        5. 5. PROCEDURE

        6. 6. EXPRESSION OF RESULTS

        7. 7. REMARKS

    18. ANNEX XVIII

      (Article 14)

      1. DETERMINATION OF MOISTURE CONTENT IN DRIED CREAM

        1. 1. SCOPE

        2. 2. TERMS AND DEFINITIONS

        3. 3. PRINCIPLE

        4. 4. APPARATUS

          2. 4.1. Analytical balance, capable of weighing to the nearest 1 mg, with...

          3. 4.2. Drying oven, well ventilated, capable of being maintained thermostatically at...

          4. 4.3. Desiccator, provided with freshly dried silica gel with hygrometric indicator...

          5. 4.4. Flat-bottomed dishes, depth of approximately 25 mm, diameter of approximately 50 mm,...

          6. 4.5. Bottles, with tight-fitting stoppers, for mixing the laboratory samples.

        5. 5. SAMPLING

        6. 6. PREPARATION OF TEST SAMPLE

        7. 7. PROCEDURE

          1. 7.1. Preparation of the dish

            1. 7.1.1. Heat an uncovered dish and its lid (4.4) in the...

            2. 7.1.2. Place the lid on the dish, transfer the covered dish...

          2. 7.2. Test portion

          3. 7.3. Determination

            1. 7.3.1. Uncover the dish and place it with its lid in...

            2. 7.3.2. Replace the lid, transfer the covered dish to the desiccator,...

            3. 7.3.3. Uncover the dish and heat it again, with its lid,...

            4. 7.3.4. Repeat the heating and the weighing procedure until the mass...

        8. 8. CALCULATION AND EXPRESSION OF RESULTS

          1. 8.1. Calculation

        9. 9. PRECISION

          2. 9.1. Repeatability

          3. 9.2. Reproducibility

        10. 10. TEST REPORT

    19. ANNEX XIX

      (Article 15)

      1. DETERMINATION OF MOISTURE IN ACID BUTTERMILK POWDER

        1. 1. SCOPE

        2. 2. PRINCIPLE

        3. 3. APPARATUS

          1. 3.1. Analytical balance, capable of weighing to the nearest 1 mg, with...

          2. 3.2. Dishes of non-corrodible metal or of glass with lids ensuring...

          3. 3.3. Adjustable electrically heated vacuum oven fitted with an oil pump...

          4. 3.4. Desiccator with an efficient drying agent

          5. 3.5. Drying oven ventilated, thermostatically controlled, at 102 ± 2 °C.

        4. 4. PROCEDURE

        5. 5. CALCULATION

        6. 6. PRECISION

          1. 6.1. Repeatability limit

          2. 6.2. Reproducibility limit

          3. 6.3. Source of precision data

    20. ANNEX XX

      (Article 16)

      1. REFERENCE METHOD FOR THE DETERMINATION OF MILK FAT PURITY BY...

        1. 1. SCOPE AND FIELD OF APPLICATION

        2. 2. DEFINITION

        3. 3. PRINCIPLE OF THE METHOD

        4. 4. REAGENTS

          2. 4.1. Carrier gas: nitrogen or, alternatively, helium or hydrogen, all with...

          3. 4.2. Fat standards, for standardizing a milk fat standard according to...

            2. 4.2.1. Triglyceride standards, saturated, suited products are available commercially.

            3. 4.2.2. Cholesterol standard.

          4. 4.3. Methanol (CH3OH), free of water.

          5. 4.4. n-Hexane (CH3(CH2)4CH3).

          6. 4.5. n-Heptane (CH3(CH2)5CH3).

          7. 4.6. Other gases: hydrogen, purity at least 99,995 %, free from organic...

          8. 4.7. Anhydrous sodium sulfate (Na2SO4).

        5. 5. APPARATUS

          2. 5.1. High-temperature gas chromatograph

          3. 5.2. Chromatography column

            1. 5.2.1. Packed column

            2. 5.2.2. Capillary column

          4. 5.3. Extrelut column, of capacity 1 ml to 3 ml, filled with silica gel,...

          5. 5.4. Graphite seals, capable of withstanding temperatures of at least 400 °C;...

          6. 5.5. Water bath, capable of maintaining a temperature of 50 °C ±...

          7. 5.6. Oven, capable of operating at 50 °C ± 2 °C and 100 °C ±...

          8. 5.7. Microlitre pipette.

          9. 5.8. Graduated pipette, of capacity 5 ml.

          10. 5.9. Round-bottomed flask, of capacity 50 ml.

          11. 5.10. Erlenmeyer flask, of nominal capacity 250 ml.

          12. 5.11. Funnel.

          13. 5.12. Fine-pored filter paper.

          14. 5.13. Rotary evaporator.

          15. 5.14. Ampoules, of nominal capacity 1 ml, fitted with a polytetrafluoroethylene-lined aluminium...

          16. 5.15. Injection syringe, with syringe plunger not reaching into the tip...

          17. 5.16. Analytical balance, capable of weighing to the nearest 1 mg, with...

        6. 6. SAMPLING

        7. 7. PROCEDURE

          1. 7.1. Preparation of test samples

            2. 7.1.1. Isolation from butter or butteroil

            3. 7.1.2. Extraction according to the Röse–Gottlieb gravimetric method

            4. 7.1.3. Extraction from milk using silica gel columns

          2. 7.2. Preparation of sample solution

          3. 7.3. Chromatographic triglyceride determination

            1. 7.3.1. Baseline drift

            2. 7.3.2. Injection technique

              1. 7.3.2.1. Packed column

              2. 7.3.2.2. Capillary column

            3. 7.3.3. Calibration

              1. 7.3.3.1. General

              2. 7.3.3.2. Commercial milk fat standard

              3. 7.3.3.3. Laboratory milk fat standard

            4. 7.3.4. Chromatographic conditions

              2. 7.3.4.1. Packed column

              3. 7.3.4.2. Capillary column

        8. 8. INTEGRATION, EVALUATION AND CONTROL OF THE ANALYTICAL PERFORMANCE

        9. 9. CALCULATION AND EXPRESSION OF RESULTS

          1. 9.1. Triglyceride composition

            1. 9.1.1. Calculation

            2. 9.1.2. Expression of test results

          2. 9.2. S-values

            1. 9.2.1. Calculation

              1. 9.2.1.1. Calculate the S-values, expressed as a percentage, by inserting the...

              2. 9.2.1.2. Soy bean, sunflower, olive, rapeseed, linseed, wheat germ, maize germ,...

              3. 9.2.1.3. Coconut and palm kernel fat.

              4. 9.2.1.4. Palm oil and beef tallow.

              5. 9.2.1.5. Lard.

              6. 9.2.1.6. Total.

            2. 9.2.2. Expression of test results

          3. 9.3. Detection of foreign fat

        10. 10. PRECISION

          1. 10.1. Interlaboratory test

          2. 10.2. Repeatability

          3. 10.3. Reproducibility

        11. 11. UNCERTAINTY OF MEASUREMENT

        12. 12. TEST REPORT

      2. ANNEX A

        (normative)

        1. PREPARATION OF THE PACKED COLUMN

          1. A.1 REAGENTS AND APPARATUS

            1. A.1.1 Toluene (C6H5CH3).

            2. A.1.2 Dimethyldichlorosilane [Si(CH3)2Cl2] solution.

            3. A.1.3 Cocoa butter solution, with a mass fraction of 5 % cocoa...

            4. A.1.4 Stationary phase, 3 % OV-1 on 125 µm to 150 µm (100 to 120 mesh)...

            5. A.1.5 Glass column, of internal diameter 2 mm and length 500 mm, U-shaped....

            6. A.1.6 Apparatus, for filling the packed column.

              2. A.1.6.1 Filling column, with screwed-on end caps, provided with a mark...

              3. A.1.6.2 Fine sieve, with mesh size of about 100 µm, with screw...

              4. A.1.6.3 Silanized glass wool, deactivated.

              5. A.1.6.4 Vibrator, for uniform distribution of the stationary phase during filling....

              6. A.1.6.5 Silanizing devices, for silanizing the glass surface of the column....

              7. A.1.6.6 Woulff bottle.

              8. A.1.6.7 Water suction pump.

          2. A.2 SILANIZATION (DEACTIVATION OF THE GLASS SURFACE)

          3. A.3 FILLING

          4. A.4 CONDITIONING

      3. ANNEX B

        (informative)

        1. QUANTIFICATION OF THE FOREIGN FAT CONTENT

          1. B.1 GENERAL

          2. B.2 CALCULATION

          3. B.3 EXPRESSION OF TEST RESULTS

          4. Bibliography

    21. ANNEX XXI

      (Article 18)

      1. PROCEDURE APPLICABLE WHEN THE RESULTS OF AN ANALYSIS ARE DISPUTED...

        1. 1. A further analysis is carried out in another laboratory approved...

        2. 2. The expanded uncertainties (k = 2) of the mean y...

        3. 3. U y ‾ 1 = 2 σ 2 R  – ...

        4. 4. In order to test whether the results of the two...

        5. 5. U y ‾ 1   –  y ‾ 2 =...

    22. ANNEX XXII

      CORRELATION TABLE

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