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Commission Regulation (EEC) No 000/90 (repealed)Show full title

Commission Regulation (EEC) No 000/90 of 17 September 1990 determining Community methods for the analysis of wines (repealed)

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  1. Introductory Text

  2. Article 1.. . . . . . . . . ....

  3. Article 2.. . . . . . . . . ....

  4. Article 3.. . . . . . . . . ....

  5. Article 4.. . . . . . . . . ....

  6. Article 5.. . . . . . . . . ....

  7. Article 6.. . . . . . . . . ....

  8. Signature

    1. ANNEX

      1. 1. DENSITY AND SPECIFIC GRAVITY AT 20 °C

        1. 1. DEFINITIONS

        2. 2. PRINCIPLE OF METHODS

        3. 3. PRELIMINARY TREATMENT OF SAMPLE

        4. 4. REFERENCE METHOD

          1. 4.1. Apparatus:

            1. 4.1.1. . . . . . . . . . ....

            2. 4.1.2. . . . . . . . . . ....

            3. 4.1.3. . . . . . . . . . ....

          2. 4.2. Calibration of pycnometer

            1. 4.2.1. Method using a twin-pan balance

            2. 4.2.2. Method using a single-pan balance

          3. 4.3. Method of measurement

            1. 4.3.1. Method using twin-pan balance

            2. 4.3.2. Method using a single-pan balance

            3. 4.3.3. . . . . . . . . . ....

            4. 4.3.4. . . . . . . . . . ....

        5. 5. USUAL METHODS

          1. 5.1. Hydrometry

            1. 5.1.1. Apparatus

              1. 5.1.1.1. . . . . . . . . . ....

              2. 5.1.1.2. . . . . . . . . . ....

              3. 5.1.1.3. . . . . . . . . . ....

            2. 5.1.2. Procedure

              1. 5.1.2.1. Method of measurement

          2. 5.2. Densimetry using a hydrostatic balance

            1. 5.2.1. Apparatus

              1. 5.2.1.1. . . . . . . . . . ....

              2. 5.2.1.2. . . . . . . . . . ....

            2. 5.2.2. Procedure

              1. 5.2.2.1. Standardization of a hydrostatic balance

              2. 5.2.2.2. Method of measurement

        6. 6. EXAMPLE OF THE CALCULATION OF THE DENSITY AT 20 °C AND...

          1. 6.1. Pycnometry using a twin-pan balance

            1. 6.1.1. Standardization of the pycnometer:

              1. 1. . . . . . . . . . ....

              2. 2. . . . . . . . . . ....

              3. 3. . . . . . . . . . ....

              4. 4. . . . . . . . . . ....

            2. 6.1.2. Determination of the density and specific gravity at 20 °C/20 °C of...

          2. 6.2. Pycnometry using a single-pan balance

            1. 6.2.1. Standardization of the pycnometer:

              1. 1. . . . . . . . . . ....

              2. 2. . . . . . . . . . ....

              3. 3. . . . . . . . . . ....

              4. 4. . . . . . . . . . ....

            2. 6.2.2. Determination of the density and specific gravity at 20° C...

        7. TABLE I F factors by which the mass of water contained in...

        8. TABLE II Temperature corrections c to the density of alcohol-free dry wines...

        9. TABLE III Temperature corrections c to the density of natural musts and...

        10. TABLE IV Temperature corrections c to the density of wines of 13 %...

        11. TABLE V Temperature corrections c to the density of dry wines and...

        12. TABLE VI Temperature corrections c to the density of natural musts and...

        13. TABLE VII Temperature corrections c to the density of wines of 13 %...

      2. 2. EVALUATION BY REFRACTOMETRY OF THE SUGAR CONCENTRATION IN GRAPE MUSTS,...

        1. 1. PRINCIPLE OF THE METHOD

        2. 2. APPARATUS

          1. 2.1. Abbé refractometer

        3. 3. PREPARATION OF THE SAMPLE

          1. 3.1. Must and concentrated must

          2. 3.2. Rectified concentrated must

        4. 4. PROCEDURE

        5. 5. CALCULATION

          1. 5.1. Temperature correction

            1. 5.1.1. . . . . . . . . . ....

            2. 5.1.2. . . . . . . . . . ....

          2. 5.2. Sugar concentration in must and concentrated must

          3. 5.3. Sugar concentration in rectified concentrated must

          4. 5.4. Refractive index of must, concentrated must and rectified concentrated must...

        6. TABLE I Correction to be made when the percentage by mass of...

        7. TABLE II Table giving the sugar concentration in must and concentrated must...

        8. TABLE III Table giving the sugar concentration in rectified concentrated must in...

      3. 3. ALCOHOLIC STRENGTH BY VOLUME

        1. 1. DEFINITION

        2. 2. PRINCIPLE OF METHODS

          1. 2.1. . . . . . . . . . ....

          2. 2.2. Reference methods:

          3. 2.3. Usual methods:

            1. 2.3.1. . . . . . . . . . ....

            2. 2.3.2. . . . . . . . . . ....

            3. 2.3.3. . . . . . . . . . ....

        3. 3. METHOD OF OBTAINING DISTILLATE

          1. 3.1. Apparatus

            1. 3.1.1. . . . . . . . . . ....

            2. 3.1.2. . . . . . . . . . ....

          2. 3.2. Reagents

            1. 3.2.1. . . . . . . . . . ....

          3. 3.3. Preparation of sample

          4. 3.4. Procedure

        4. 4. REFERENCE METHODS

          1. 4–A Measurement of the alcoholic strength of the distillate using a...

            1. 4.1. Apparatus

              1. 4.1.1. . . . . . . . . . ....

            2. 4.2. Procedure

            3. 4.3. Expression of results

              1. 4.3.1. Method of calculation

              2. 4.3.2. . . . . . . . . . ....

              3. 4.3.3. . . . . . . . . . ....

          2. 4–B Measurement of the alcoholic strength of wines using a hydrostatic...

            1. 1. METHOD OF MEASUREMENT

              1. 1.1. Introduction

              2. 1.2. Object and field of application

              3. 1.3. Principle and definitions

              4. 1.4. Reagents

                1. 1.4.1. Float-cleaning solution (sodium hydroxide, 30 % w/v)

              5. 1.5. Apparatus and equipment

                1. 1.5.1. . . . . . . . . . ....

                2. 1.5.2. . . . . . . . . . ....

                3. 1.5.3. . . . . . . . . . ....

                4. 1.5.4. . . . . . . . . . ....

                5. 1.5.5. . . . . . . . . . ....

              6. 1.6. Procedure

                1. 1.6.1. Calibration of the balance

                2. 1.6.2. Calibration of the float

                  1. 1.6.2.1. . . . . . . . . . ....

                  2. 1.6.2.2. . . . . . . . . . ....

                3. 1.6.3. Control using a water-alcohol solution

                  1. 1.6.3.1. . . . . . . . . . ....

                  2. 1.6.3.2. . . . . . . . . . ....

                4. 1.6.4. Measurement of the density of a distillate (or of its...

                  1. 1.6.4.1. . . . . . . . . . ....

                  2. 1.6.4.2. . . . . . . . . . ....

                  3. 1.6.4.3. . . . . . . . . . ....

                5. 1.6.5. Cleaning of float and measuring cylinder

                  1. 1.6.5.1. . . . . . . . . . ....

                  2. 1.6.5.2. . . . . . . . . . ....

                  3. 1.6.5.3. . . . . . . . . . ....

                  4. 1.6.5.4. . . . . . . . . . ....

                6. 1.6.6. Result

            2. 2. COMPARISON OF MEASUREMENTS MADE USING A HYDROSTATIC BALANCE WITH PROCEDURES...

              1. 2.1. Samples

              2. 2.2. Laboratories

              3. 2.3. Equipment

                1. 2.3.1. . . . . . . . . . ....

                2. 2.3.2. . . . . . . . . . ....

              4. 2.4. Analysis

              5. 2.5. Result

              6. 2.6. Evaluations of the results

                1. 2.6.1. . . . . . . . . . ....

                2. 2.6.2. Repeatability (r) and reproducibility (R)

                3. 2.6.3. Interlaboratory precision

                4. 2.6.4. Fidelity parameters

              7. 2.7. Conclusion

          3. 4–C Measurement of the alcoholic strength of wines by electronic densimetry...

            1. 1. Method of measurement

              1. 1.1. Title and introduction

              2. 1.2. Purpose and scope

              3. 1.3. Principle and definitions

              4. 1.4. Reagents and products

                1. 1.4.1. Reference fluids

                2. 1.4.2. Cleaning and drying products

              5. 1.5. Apparatus

                1. 1.5.1. Electronic densimeter using a frequency oscillator

                2. 1.5.2. Controlling the temperature in the measuring cell

                3. 1.5.3. Calibration of the apparatus

                4. 1.5.4. Checking the calibration

                5. 1.5.5. Checks

              6. 1.6. Sampling and preparation of the samples

              7. 1.7. Procedure

              8. 1.8. Expression of results

              9. 1.9. Remarks

              10. 1.10. Precision

            2. 2. Interlaboratory trials. Precision and accuracy on adjuncts

        5. 5. USUAL METHODS

          1. 5.1. Hydrometry

            1. 5.1.1. Apparatus

              1. 5.1.1.1. . . . . . . . . . ....

              2. 5.1.1.2. . . . . . . . . . ....

              3. 5.1.1.3. . . . . . . . . . ....

            2. 5.1.2. Procedure

          2. 5.2. Densimetry using a hydrostatic balance

            1. 5.2.1. Apparatus

              1. 5.2.1.1. . . . . . . . . . ....

            2. 5.2.2. Procedure

            3. 5.2.3. Expression of results

          3. 5.3. Refractometry

            1. 5.3.1. Apparatus

              1. 5.3.1.1. . . . . . . . . . ....

            2. 5.3.2. Procedure

            3. 5.3.3. Expression of results

        6. 6. EXAMPLE OF THE CALCULATION OF THE ALCOHOLIC STRENGTH OF A...

          1. 6.1. Measurement by pycnometer on a twin-pan balance

            1. 6.1.1. . . . . . . . . . ....

            2. 6.1.2. Weighing of pycnometer filled with distillate

            3. 6.1.3. Calculation of alcoholic strength

          2. 6.2. Measurement by pycnometer on a single pan balance

            1. 6.2.1. . . . . . . . . . ....

            2. 6.2.2. Weighing of the pycnometer filled with distillate

            3. 6.2.3. Calculation of alcoholic strength

        7. FORMULA FROM WHICH TABLES OF ALCOHOLIC STRENGHTS OF ETHANOL-WATER MIXTURES...

        8. TABLE I INTERNATIONAL ALCOHOLIC STRENGTH AT 20 °C

        9. TABLE II INTERNATIONAL ALCOHOLIC STRENGTH AT 20 °C

        10. TABLE III INTERNATIONAL ALCOHOLIC STRENGTH AT 20 °C

        11. TABLE IV Table giving the refractive indices of pure ethanol-water mixtures and...

      4. 4. TOTAL DRY EXTRACT

        1. 1. DEFINITION

        2. 2. PRINCIPLE OF THE METHOD

        3. 3. METHOD OF CALCULATION

        4. 4. EXPRESSION OF RESULTS

        5. TABLE I for the calculation of the content total dry extract (g/l)...

      5. 5. REDUCING SUGARS

        1. 1. DEFINITION

        2. 2. PRINCIPLE OF THE METHODS

          1. 2.1. Clarification

            1. 2.1.1. . . . . . . . . . ....

            2. 2.1.2. . . . . . . . . . ....

              1. 2.1.2.1. . . . . . . . . . ....

              2. 2.1.2.2. . . . . . . . . . ....

          2. 2.2. . . . . . . . . . ....

            1. 2.2.1. . . . . . . . . . ....

        3. 3. CLARIFICATION

          1. 3.1. Reference method

            1. 3.1.1. Reagents

              1. 3.1.1.1. . . . . . . . . . ....

              2. 3.1.1.2. . . . . . . . . . ....

              3. 3.1.1.3. . . . . . . . . . ....

              4. 3.1.1.4. . . . . . . . . . ....

              5. 3.1.1.5. . . . . . . . . . ....

                1. Preparation of the anion exchange resin column

                2. Regeneration of the resin

              6. 3.1.1.6. . . . . . . . . . ....

              7. 3.1.1.7. . . . . . . . . . ....

            2. 3.1.2. Procedure

              1. 3.1.2.1. Dry wines

              2. 3.1.2.2. Musts, mistelles, sweet and semi-sweet wines:

                1. 1. . . . . . . . . . ....

                2. 2. . . . . . . . . . ....

                3. 3. . . . . . . . . . ....

          2. 3.2. Usual methods

            1. 3.2.1. Clarification by neutral lead acetate

              1. 3.2.1.1. Reagents

              2. 3.2.1.2. Procedure

                1. 3.2.1.2.1. . . . . . . . . . ....

                2. 3.2.1.2.2. . . . . . . . . . ....

                  1. 1. . . . . . . . . . ....

                  2. 2. . . . . . . . . . ....

                  3. 3. . . . . . . . . . ....

            2. 3.2.2. Clarification by zinc 2-hexacyanoferrate

              1. 3.2.2.1. Reagents

                1. 3.2.2.1.1. . . . . . . . . . ....

                2. 3.2.2.1.2. . . . . . . . . . ....

              2. 3.2.2.2. Procedure

                1. 1. . . . . . . . . . ....

                2. 2. . . . . . . . . . ....

                3. 3. . . . . . . . . . ....

                4. 4. . . . . . . . . . ....

        4. 4. DETERMINATION OF SUGARS

          1. 4.1. Reagents

            1. 4.1.1 Alkaline copper salt solution:

            2. 4.1.2. 30 % potassium iodide solution:

            3. 4.1.3. 25 % sulphuric acid:

            4. 4.1.4. 5 g/l starch solution:

          2. 4.2. Procedure

          3. 4.3. Expression of results

            1. 4.3.1. Calculations

            2. 4.3.2. Repeatability

            3. 4.3.3. Reproducibility

      6. 6. SUCROSE

        1. 1. PRINCIPLE OF METHODS

          1. I. . . . . . . . . . ....

          2. II. . . . . . . . . . ....

        2. 2. QUALITATIVE TESTING BY THIN-LAYER CHROMATOGRAPHY

          1. 2.1. Equipment

            1. 2.1.1. . . . . . . . . . ....

            2. 2.1.2. . . . . . . . . . ....

            3. 2.1.3. . . . . . . . . . ....

            4. 2.1.4. . . . . . . . . . ....

          2. 2.2. Reagents

            1. 2.2.1. . . . . . . . . . ....

            2. 2.2.2. . . . . . . . . . ....

            3. 2.2.3. Developing agent

            4. 2.2.4. Reference solutions

          3. 2.3. Procedure

            1. 2.3.1. Preparation of sample

            2. 2.3.2. Obtaining the chromatogram

          4. 2.4. Results

        3. 3. TESTING AND DETERMINATION BY HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

          1. 3.1. Equipment

            1. 3.1.1. . . . . . . . . . ....

              1. 1. . . . . . . . . . ....

              2. 2. . . . . . . . . . ....

              3. 3. . . . . . . . . . ....

              4. 4. . . . . . . . . . ....

              5. 5. . . . . . . . . . ....

              6. 6. . . . . . . . . . ....

              7. 7. . . . . . . . . . ....

            2. 3.1.2. . . . . . . . . . ....

          2. 3.2. Reagents

            1. 3.2.1. . . . . . . . . . ....

            2. 3.2.2. . . . . . . . . . ....

            3. 3.2.3. . . . . . . . . . ....

            4. 3.2.4. . . . . . . . . . ....

          3. 3.3. Procedure

            1. 3.3.1. Preparation of sample:

            2. 3.3.2. Chromatographic determination

          4. 3.4. Calculations

            1. 3.4.1. . . . . . . . . . ....

            2. 3.4.2. . . . . . . . . . ....

          5. 3.5. Expression of results

      7. 7. GLUCOSE AND FRUCTOSE

        1. 1. DEFINITION

        2. 2. PRINCIPLE OF THE METHOD

        3. 3. APPARATUS

        4. 4. REAGENTS

          1. 4.1. . . . . . . . . . ....

          2. 4.2. . . . . . . . . . ....

          3. 4.3. . . . . . . . . . ....

          4. 4.4. . . . . . . . . . ....

          5. 4.5. . . . . . . . . . ....

        5. 5. PROCEDURE

          1. 5.1. Preparation of sample

          2. 5.2. Determination

          3. 5.3. Expression of results

            1. 5.3.1. Calculation

            2. 5.3.2. Repeatability (r)

            3. 5.3.3. Reproducibility (R)

      8. 8. DETECTING ENRICHMENT OF GRAPE MUSTS, CONCENTRATED GRAPE MUSTS, RECTIFIED CONCENTRATED...

        1. 1. DEFINITION

        2. 2. PRINCIPLE

        3. 3. PREPARATION OF THE SAMPLE FOR ANALYSIS

          1. 3.1. Extraction of ethanol and water in the wine

            1. 3.1.1. Apparatus and reagents

            2. 3.1.2. Procedure

              1. 3.1.2.1. . . . . . . . . . ....

              2. 3.1.2.2. Extraction of the ethanol

              3. 3.1.2.3. Determination of the alcoholic strength of the alcohol extracted

          2. 3.2. Fermentation of musts, concentrated musts and rectified concentrated musts

            1. 3.2.1. Apparatus and reagents

            2. 3.2.2. Procedure

              1. 3.2.2.1. Musts

              2. 3.2.2.2. Concentrated musts

              3. 3.2.2.3. Rectified concentrated musts

          3. 3.3. Preparation of alcohol sample for NMR measurement

            1. 3.3.1. Reagents

            2. 3.3.2. Procedure

          4. 3.4. Preparation of a water sample for the NMR measurement, for...

            1. 3.4.1. Reagents

            2. 3.4.2. Procedure

        4. 4. RECORDING OF 2H NMR SPECTRA OF THE ALCOHOL AND THE...

          1. 4.1. Apparatus

          2. 4.2. Standardization of spectrometer and checks

            1. 4.2.1. Standardization

            2. 4.2.2. Checking the validity of the standardization

          3. 4.3. Conditions for obtaining NMR spectra

        5. 5. EXPRESSION OF RESULTS

          1. 5.1. Ethanol

          2. 5.2. Water

          3. 5.3. . . . . . . . . . ....

        6. 6. INTERPRETATION OF RESULTS

          1. 6.1. Addition of beet sugar, cane sugar or maize glucose

            1. 6.1.1. Wines

            2. 6.1.2. Musts, concentrated musts and rectified concentrated masts

          2. 6.2. Addition of a mixture of beet sugar and cane sugar...

      9. 9. ASH CONTENT

        1. 1. DEFINITION

        2. 2. PRINCIPLE OF THE METHOD

        3. 3. APPARATUS

          1. 3.1. . . . . . . . . . ....

          2. 3.2. . . . . . . . . . ....

          3. 3.3. . . . . . . . . . ....

          4. 3.4. . . . . . . . . . ....

          5. 3.5. . . . . . . . . . ....

          6. 3.6. . . . . . . . . . ....

        4. 4. PROCEDURE

        5. 5. EXPRESSION OF RESULTS

          1. 5.1. . . . . . . . . . ....

      10. 10. ALKALINITY OF THE ASH

        1. 1. DEFINITION

        2. 2. PRINCIPLE OF THE METHOD

        3. 3. REAGENTS AND APPARATUS

          1. 3.1. . . . . . . . . . ....

          2. 3.2. . . . . . . . . . ....

          3. 3.3. . . . . . . . . . ....

          4. 3.4. . . . . . . . . . ....

        4. 4. PROCEDURE

        5. 5. EXPRESSION OF RESULTS

      11. 11. CHLORIDES

        1. 1. PRINCIPLE

        2. 2. APPARATUS

          1. 2.1. . . . . . . . . . ....

          2. 2.2. . . . . . . . . . ....

          3. 2.3. . . . . . . . . . ....

          4. 2.4. . . . . . . . . . ....

          5. 2.5. . . . . . . . . . ....

        3. 3. REAGENTS

          1. 3.1. . . . . . . . . . ....

          2. 3.2. . . . . . . . . . ....

          3. 3.3. . . . . . . . . . ....

        4. 4. PROCEDURE

          1. 4.1. . . . . . . . . . ....

          2. 4.2. . . . . . . . . . ....

          3. 4.3. . . . . . . . . . ....

        5. 5. EXPRESSION OF RESULTS

          1. 5.1. Calculations

          2. 5.2. Repeatability (r):

          3. 5.3. Reproducibility (R):

        6. 6.

      12. 12. SULPHATES

        1. 1. PRINCIPLE

          1. 1.1. Reference method

          2. 1.2. Quick test method

        2. 2. REFERENCE METHOD

          1. 2.1. Reagents

            1. 2.1.1. . . . . . . . . . ....

            2. 2.1.2. . . . . . . . . . ....

          2. 2.2. Procedure

            1. 2.2.1. General procedure:

            2. 2.2.2. . . . . . . . . . ....

          3. 2.3. Expression of results

            1. 2.3.1. Calculations:

            2. 2.3.2. Repeatability

            3. 2.3.3. Reproducibility

        3. 3. QUICK TEST METHOD

          1. 3.1. Reagents

            1. 3.1.1. . . . . . . . . . ....

            2. 3.1.2. . . . . . . . . . ....

          2. 3.2. Procedure

      13. 13. TOTAL ACIDITY

        1. 1. DEFINITION

        2. 2. PRINCIPLE OF THE METHOD

        3. 3. REAGENTS

          1. 3.1. . . . . . . . . . ....

          2. 3.2. . . . . . . . . . ....

          3. 3.3. . . . . . . . . . ....

        4. 4. APPARATUS

          1. 4.1. . . . . . . . . . ....

          2. 4.2. . . . . . . . . . ....

          3. 4.3. . . . . . . . . . ....

          4. 4.4. . . . . . . . . . ....

        5. 5. PROCEDURE

          1. 5.1. Preparation of sample:

            1. 5.1.1. Wines

            2. 5.1.2. Rectified concentrated musts

          2. 5.2. Potentiometric titration

            1. 5.2.1. Calibration of pH meter

            2. 5.2.2. Method of measurement

          3. 5.3. Titration with indicator (bromothymol blue)

            1. 5.3.1. Preliminary test: end-point colour determination.

            2. 5.3.2. Measurement

        6. 6. EXPRESSION OF RESULTS

          1. 6.1. Method of calculation

            1. 6.1.1. Wines

            2. 6.1.2. Rectified concentrated musts

          2. 6.2. Repeatability (r) for titration with the indicator:

          3. 6.3. Reproducibility (R) for titration with the indicator (5.3):

      14. 14. VOLATILE ACIDITY

        1. 1. DEFINITION

        2. 2. PRINCIPLE OF THE METHOD

        3. 3. REAGENTS

          1. 3.1. . . . . . . . . . ....

          2. 3.2. . . . . . . . . . ....

          3. 3.3. . . . . . . . . . ....

          4. 3.4. . . . . . . . . . ....

          5. 3.5. . . . . . . . . . ....

          6. 3.6. . . . . . . . . . ....

          7. 3.7. . . . . . . . . . ....

          8. 3.8. . . . . . . . . . ....

        4. 4. APPARATUS

          1. 4.1. . . . . . . . . . ....

          2. 4.2. . . . . . . . . . ....

          3. 4.3. . . . . . . . . . ....

        5. 5. PROCEDURE

          1. 5.1. . . . . . . . . . ....

          2. 5.2. Steam distillation

          3. 5.3. Titration

        6. 6. EXPRESSION OF RESULTS

          1. 6.1. Method of calculation

          2. 6.2. Repeatability (r)

          3. 6.3. Reproducibility (R)

          4. 6.4. Wine with sorbic acid present

        7. 7. DETERMINATION OF SALICYLIC ACID ENTRAINED IN THE DISTILLATE FROM THE...

          1. 7.1. Principle

          2. 7.2. Reagents

            1. 7.2.1. . . . . . . . . . ....

            2. 7.2.2. . . . . . . . . . ....

            3. 7.2.3. . . . . . . . . . ....

            4. 7.2.4. . . . . . . . . . ....

          3. 7.3. Procedure

            1. 7.3.1. Identification of salicylic acid in the volatile acidity distillate.

            2. 7.3.2. Determination of salicylic acid

            3. 7.3.3. Correction to the volatile acidity

      15. 15. FIXED ACIDITY

        1. 1. PRINCIPLE

        2. 2. EXPRESSION OF RESULTS

      16. 16. TARTARIC ACID

        1. 1. PRINCIPLE OF METHODS

          1. 1.1. Reference method

          2. 1.2. Usual method

        2. 2. REFERENCE METHOD

          1. 2.1. Gravimetric method

            1. 2.1.1. Reagents

              1. 2.1.1.1. . . . . . . . . . ....

              2. 2.1.1.2. . . . . . . . . . ....

              3. 2.1.1.3. . . . . . . . . . ....

            2. 2.1.2. Procedure

              1. 2.1.2.1. Wines with no added mesotartaric acid

              2. 2.1.2.2. Wines to which mesotartaric acid has been added

            3. 2.1.3. Expression of results

          2. 2.2. Comparative volumetric analysis

            1. 2.2.1. Reagents

              1. 2.2.1.1. . . . . . . . . . ....

              2. 2.2.1.2. . . . . . . . . . ....

              3. 2.2.1.3. . . . . . . . . . ....

              4. 2.2.1.4. . . . . . . . . . ....

            2. 2.2.2. Procedure

            3. 2.2.3. Expression of results

        3. 3. USUAL METHOD

          1. 3.1. Reagents

            1. 3.1.1. For preliminary treatment of the wine

              1. 3.1.1.1. . . . . . . . . . ....

              2. 3.1.1.2. . . . . . . . . . ....

              3. 3.1.1.3. . . . . . . . . . ....

              4. 3.1.1.4. . . . . . . . . . ....

            2. 3.1.2. For the determination of tartaric acid

              1. 3.1.2.1. . . . . . . . . . ....

              2. 3.1.2.2. . . . . . . . . . ....

              3. 3.1.2.3. . . . . . . . . . ....

              4. 3.1.2.4. . . . . . . . . . ....

              5. 3.1.2.5. . . . . . . . . . ....

              6. 3.1.2.6. . . . . . . . . . ....

              7. 3.1.2.7. . . . . . . . . . ....

              8. 3.1.2.8. . . . . . . . . . ....

              9. 3.1.2.9. . . . . . . . . . ....

              10. 3.1.2.10. . . . . . . . . . ....

          2. 3.2. Apparatus

            1. 3.2.1. . . . . . . . . . ....

            2. 3.2.2. . . . . . . . . . ....

          3. 3.3. Procedure

            1. 3.3.1. Preparation of the ion exchange column

            2. 3.3.2. Separation of organic acids

            3. 3.3.3. Determination of tartaric acid

              1. 3.3.3.1. Wines with no added mesotartaric acid

              2. 3.3.3.2. Wines to which mesotartaric acid has been added

            4. 3.3.4. Plotting the calibration curve

            5. 3.3.5. Expression of results

      17. 17. CITRIC ACID

        1. 1. PRINCIPLE OF THE METHOD

        2. 2. REAGENTS

          1. 2.1. . . . . . . . . . ....

          2. 2.2. . . . . . . . . . ....

          3. 2.3. . . . . . . . . . ....

          4. 2.4. . . . . . . . . . ....

          5. 2.5. . . . . . . . . . ....

        3. 3. APPARATUS

          1. 3.1. . . . . . . . . . ....

          2. 3.2. . . . . . . . . . ....

          3. 3.3. . . . . . . . . . ....

        4. 4. PREPARATION OF THE SAMPLE

        5. 5. PROCEDURE

        6. 6. EXPRESSION OF RESULTS

          1. 6.1. Method of calculation

          2. 6.2. Repeatability (r)

          3. 6.3. Reproducibility (R)

      18. 18. LACTIC ACID

        1. 1. PRINCIPLE OF THE METHOD

          1. 1.2. Usual method

        2. 2. REFERENCE METHOD

          1. 2.1. Reagents

            1. 2.1.1. . . . . . . . . . ....

            2. 2.1.2. . . . . . . . . . ....

            3. 2.1.3. . . . . . . . . . ....

            4. 2.1.4. . . . . . . . . . ....

            5. 2.1.5. . . . . . . . . . ....

          2. 2.2. Apparatus

            1. 2.2.1. . . . . . . . . . ....

            2. 2.2.2. . . . . . . . . . ....

            3. 2.2.3. . . . . . . . . . ....

          3. 2.3. Preparation of the sample

          4. 2.4. Procedure

            1. 2.4.1. Determination of total lactic acid

            2. 2.4.2. Determination of L-lactic acid and D-lactic acid

          5. 2.5. Expression of results

            1. 2.5.1. Method of calculation

              1. 2.5.1.1. Total lactic acid and D-lactic acid

              2. 2.5.1.2. L-lactic acid

            2. 2.5.2. Repeatability (r)

            3. 2.5.3. Reproducibility (R)

        3. 3. USUAL METHOD

          1. 3.1.1. For preliminary treatment of the wine

          2. 3.1.2. For the determination of lactic acid

            1. 3.1.2.1. . . . . . . . . . ....

            2. 3.1.2.2. . . . . . . . . . ....

            3. 3.1.2.3. . . . . . . . . . ....

            4. 3.1.2.4. . . . . . . . . . ....

            5. 3.1.2.5. . . . . . . . . . ....

            6. 3.1.2.6. . . . . . . . . . ....

            7. 3.1.2.7. . . . . . . . . . ....

            8. 3.1.2.8. . . . . . . . . . ....

          3. 3.2. Apparatus

            1. 3.2.1. . . . . . . . . . ....

            2. 3.2.2. . . . . . . . . . ....

            3. 3.2.3. . . . . . . . . . ....

          4. 3.3. Procedure

            1. 3.3.1. Preparation of the ion exchange column

            2. 3.3.2. Separation of organic acids

            3. 3.3.3. Determination of lactic acid

            4. 3.3.4. Plotting the calibration curve

          5. 3.4. Expression of results

      19. 19. L-MALIC ACID

        1. 1. PRINCIPLE OF THE METHOD

        2. 2. REAGENTS

          1. 2.1. . . . . . . . . . ....

          2. 2.2. . . . . . . . . . ....

          3. 2.3. . . . . . . . . . ....

          4. 2.4. . . . . . . . . . ....

        3. 3. APPARATUS

          1. 3.1. . . . . . . . . . ....

          2. 3.2. . . . . . . . . . ....

          3. 3.3. . . . . . . . . . ....

        4. 4. PREPARATION OF THE SAMPLE

        5. 5. PROCEDURE

        6. 6. EXPRESSION OF RESULTS

          1. 6.1. Method of calculation

          2. 6.2. Repeatability (r)

          3. 6.3. Reproducibility (R)

      20. 20. D-MALIC ACID

        1. 1. PRINCIPLE

        2. 2. REAGENTS

          1. Preparation of the solutions

            1. 1. . . . . . . . . . ....

            2. 2. . . . . . . . . . ....

            3. 3. . . . . . . . . . ....

          2. Stability of the solutions

        3. 3. APPARATUS

          1. 3.1. . . . . . . . . . ....

          2. 3.2. . . . . . . . . . ....

          3. 3.3. . . . . . . . . . ....

        4. 4. PREPARATION OF THE SAMPLE

        5. 5. PROCEDURE

        6. 6. EXPRESSION OF THE RESULTS

        7. 7. ACCURACY

          1. 7.1. Repeatability

          2. 7.2. Reproducibility

        8. 8. DOSAGE OF D-MALIC ACID (D(+)-MALIC ACID) IN WINES WITH LOW...

          1. 8.1. Field of application

          2. 8.2. Principle

          3. 8.3. Reagents

          4. 8.4. Apparatus

          5. 8.5. Preparation of the sample

          6. 8.6. Procedure

          7. 8.7. Internal validation

      21. Appendix A

        1. How to deal with side reactions

      22. Appendix B

      23. 21. TOTAL MALIC ACID

        1. 1. PRINCIPLE

        2. 2. APPARATUS

          1. 2.1. . . . . . . . . . ....

          2. 2.2. . . . . . . . . . ....

          3. 2.3. . . . . . . . . . ....

          4. 2.4. . . . . . . . . . ....

        3. 3. REAGENTS

          1. 3.1. . . . . . . . . . ....

          2. 3.2. . . . . . . . . . ....

          3. 3.3. . . . . . . . . . ....

          4. 3.4. . . . . . . . . . ....

          5. 3.5. . . . . . . . . . ....

          6. 3.6. . . . . . . . . . ....

          7. 3.7. . . . . . . . . . ....

          8. 3.8. . . . . . . . . . ....

          9. 3.9. . . . . . . . . . ....

        4. 4. PROCEDURE

          1. 4.1. Preparation of ion exchange resin

          2. 4.2. Preparation of ion exchange column

          3. 4.3. Separation of DL-malic acid

          4. 4.4. Determination of malic acid

          5. 4.5. Plotting the calibration curve

        5. 5. EXPRESSION OF RESULTS

          1. Repeatability:

          2. Reproducibility:

      24. 22. SORBIC ACID

        1. 1. PRINCIPLE OF METHODS

          1. 1.1. Determination by ultraviolet absorption spectrophotometry

          2. 1.2. Determination by gas chromatography

          3. 1.3. Identification of traces by thin-layer chromatography

        2. 2. DETERMINATION BY ULTRAVIOLET ABSORPTION SPECTROPHOTOMETRY

          1. 2.1. Reagents

            1. 2.1.1. . . . . . . . . . ....

            2. 2.1.2. . . . . . . . . . ....

            3. 2.1.3. . . . . . . . . . ....

          2. 2.2. Apparatus

            1. 2.2.1. . . . . . . . . . ....

            2. 2.2.2. . . . . . . . . . ....

            3. 2.2.3. . . . . . . . . . ....

          3. 2.3. Procedure

            1. 2.3.1. Distillation

            2. 2.3.2. Preparation of the calibration curve

            3. 2.3.3. Determination

          4. 2.4. Expression of results

            1. 2.4.1. Calculation

        3. 3. DETERMINATION BY GAS CHROMATOGRAPHY

          1. 3.1. Reagents

            1. 3.1.1. . . . . . . . . . ....

            2. 3.1.2. . . . . . . . . . ....

            3. 3.1.3. . . . . . . . . . ....

          2. 3.2. Apparatus

            1. 3.2.1. . . . . . . . . . ....

            2. 3.2.2. . . . . . . . . . ....

          3. 3.3. Procedure

            1. 3.3.1. Preparation of sample to be analysed

            2. 3.3.2. Preparation of the reference solution

            3. 3.3.3. Chromatography

          4. 3.4. Expression of results

            1. 3.4.1. Calculation

        4. 4. IDENTIFICATION OF TRACES OF SORBIC ACID BY THIN LAYER CHROMATOGRAPHY...

          1. 4.1. Reagents

            1. 4.1.1. . . . . . . . . . ....

            2. 4.1.2. . . . . . . . . . ....

            3. 4.1.3. . . . . . . . . . ....

            4. 4.1.4. . . . . . . . . . ....

          2. 4.2. Apparatus

            1. 4.2.1. . . . . . . . . . ....

            2. 4.2.2. . . . . . . . . . ....

            3. 4.2.3. . . . . . . . . . ....

            4. 4.2.4. . . . . . . . . . ....

          3. 4.3. Procedure

            1. 4.3.1. Preparation of sample to be analysed

            2. 4.3.2. Preparation of dilute reference solutions

            3. 4.3.3. Chromatography

          4. 4.4. Expression of results

      25. 23. L-ASCORBIC ACID

        1. 1. PRINCIPLE OF METHODS

          1. 1.1. Reference method (fluorimetry)

          2. 1.2. Usual method (colorimetry)

        2. 2. REFERENCE METHOD (fluorimetric method)

          1. 2.1. Reagents

            1. 2.1.1. . . . . . . . . . ....

            2. 2.1.2. . . . . . . . . . ....

            3. 2.1.3. . . . . . . . . . ....

            4. 2.1.4. . . . . . . . . . ....

            5. 2.1.5. . . . . . . . . . ....

            6. 2.1.6. . . . . . . . . . ....

          2. 2.2. Apparatus

            1. 2.2.1. . . . . . . . . . ....

            2. 2.2.2. . . . . . . . . . ....

            3. 2.2.3. . . . . . . . . . ....

            4. 2.2.4. . . . . . . . . . ....

          3. 2.3. Procedure

            1. 2.3.1. Preparation of the sample of wine or must

            2. 2.3.2. Preparation of the calibration curve

            3. 2.3.3. Fluorimetric determination

            4. 2.3.4. Expression of results

        3. 3. USUAL METHOD (colorimetric method)

          1. 3.1. Reagents

            1. 3.1.1. . . . . . . . . . ....

            2. 3.1.2. . . . . . . . . . ....

            3. 3.1.3. . . . . . . . . . ....

            4. 3.1.4. . . . . . . . . . ....

            5. 3.1.5. . . . . . . . . . ....

            6. 3.1.6. . . . . . . . . . ....

            7. 3.1.7. . . . . . . . . . ....

            8. 3.1.8. . . . . . . . . . ....

            9. 3.1.9. . . . . . . . . . ....

            10. 3.1.10. . . . . . . . . . ....

            11. 3.1.11. . . . . . . . . . ....

            12. 3.1.12. . . . . . . . . . ....

            13. 3.1.13. . . . . . . . . . ....

          2. 3.2. Apparatus

            1. 3.2.1. . . . . . . . . . ....

            2. 3.2.2. . . . . . . . . . ....

            3. 3.2.3. . . . . . . . . . ....

            4. 3.2.4. . . . . . . . . . ....

            5. 3.2.5. . . . . . . . . . ....

            6. 3.2.6. . . . . . . . . . ....

            7. 3.2.7. . . . . . . . . . ....

          3. 3.3. Procedure

            1. 3.3.1. Oxidation of the L-ascorbic acid to dehydroascorbic acid

            2. 3.3.2. Formation and extraction of the bis(2,4-dinitrophenylhydrazone) derivative of diketogulonic acid...

            3. 3.3.3. Separation of the bis(2,4-dinitrophenylhydrazone) by chromatography; this is to be...

            4. 3.3.4. Preparation of the calibration curve

            5. 3.3.5. Expression of results

              1. 3.3.5.1. Calculation

      26. 24. pH

        1. 1. PRINCIPLE

        2. 2. APPARATUS

          1. 2.1. . . . . . . . . . ....

          2. 2.2. Electrodes:

            1. 2.2.1. . . . . . . . . . ....

            2. 2.2.2. . . . . . . . . . ....

            3. 2.2.3. . . . . . . . . . ....

        3. 3. REAGENTS

          1. 3.1. Buffer solutions

            1. 3.1.1. . . . . . . . . . ....

            2. 3.1.2. . . . . . . . . . ....

            3. 3.1.3. . . . . . . . . . ....

        4. 4. PROCEDURE

          1. 4.1. Preparation of the sample for analysis

            1. 4.1.1. . . . . . . . . . ....

            2. 4.1.2. . . . . . . . . . ....

          2. 4.2. Zeroing of the apparatus

          3. 4.3. Calibration of the pH meter

          4. 4.4. Determination

        5. 5. EXPRESSION OF RESULTS

      27. 25. SULPHUR DIOXIDE

        1. 1. DEFINITIONS

        2. 2. FREE AND TOTAL SULPHUR DIOXIDE

          1. 2.1. Principle of the methods

            1. 2.1.1. Reference method

              1. 2.1.1.1. For wines and musts

              2. 2.1.1.2. For rectified concentrated musts

            2. 2.1.2. Rapid method of determination (for wines and musts)

          2. 2.2. Reference method

            1. 2.2.1. Apparatus

              1. 2.2.1.1. . . . . . . . . . ....

              2. 2.2.1.2. . . . . . . . . . ....

            2. 2.2.2. Reagents

              1. 2.2.2.1. . . . . . . . . . ....

              2. 2.2.2.2. . . . . . . . . . ....

              3. 2.2.2.3. . . . . . . . . . ....

              4. 2.2.2.4. . . . . . . . . . ....

            3. 2.2.3. Procedure

              1. 2.2.3.1. Determination of free sulphur dioxide

              2. 2.2.3.2. Expression of results

                1. 2.2.3.2.1. . . . . . . . . . ....

              3. 2.2.3.3. Determination of total sulphur dioxide

                1. 2.2.3.3.1. . . . . . . . . . ....

                2. 2.2.3.3.2. . . . . . . . . . ....

              4. 2.2.3.4. Expression of results

                1. 2.2.3.4.1. . . . . . . . . . ....

                2. 2.2.3.4.2. . . . . . . . . . ....

                3. 2.2.3.4.3. . . . . . . . . . ....

          3. 2.3. Rapid method of determination

            1. 2.3.1. Reagents

              1. 2.3.1.1. . . . . . . . . . ....

              2. 2.3.1.2. . . . . . . . . . ....

              3. 2.3.1.3. . . . . . . . . . ....

              4. 2.3.1.4. . . . . . . . . . ....

              5. 2.3.1.5. . . . . . . . . . ....

            2. 2.3.2. Apparatus

              1. 2.3.2.1. . . . . . . . . . ....

              2. 2.3.2.2. . . . . . . . . . ....

              3. 2.3.2.5. . . . . . . . . . ....

            3. 2.3.3. Procedure

              1. 2.3.3.1. Free sulphur dioxide

              2. 2.3.3.2. Sulphur dioxide

            4. 2.3.4. Expression of results

              1. 2.3.4.1. Calculation:

        3. 3. MOLECULAR SULPHUR DIOXIDE

          1. 3.1. Principle of the method

          2. 3.2. Calculation

      28. 26. SODIUM

        1. 1. PRINCIPLE OF THE METHODS

          1. 1.1. Reference method: atomic absorption spectrophotometry

          2. 1.2. Usual method: flame photometry

        2. 2. REFERENCE METHOD

          1. 2.1. Reagents

            1. 2.1.1. Solution containing 1 g of sodium per litre:

            2. 2.1.2. Matrix (model) solution:

            3. 2.1.3. Caesium chloride solution containing 5 % caesium:

          2. 2.2. Apparatus

            1. 2.2.1. . . . . . . . . . ....

            2. 2.2.2. . . . . . . . . . ....

          3. 2.3. Procedure

            1. 2.3.1. Preparation of sample

            2. 2.3.2. Calibration

            3. 2.3.3. Determination

          4. 2.4. Expression of results

            1. 2.4.1. Method of calculation

            2. 2.4.2. Repeatability (r)

            3. 2.4.3. Reproducibility (R)

        3. 3. USUAL METHOD

          1. 3.1. Reagents

            1. 3.1.1. Reference solution containing 20 mg sodium per litre

            2. 3.1.2. Dilution solution

          2. 3.2. Apparatus

            1. 3.2.1. . . . . . . . . . ....

          3. 3.3. Procedure

            1. 3.3.1. Calibration

            2. 3.3.2. Determination

          4. 3.4. Expression of results

            1. 3.4.1. Method of calculation

            2. 3.4.2. Repeatability (r)

            3. 3.4.3. Reproducibility (R)

      29. 27. POTASSIUM

        1. 1. PRINCIPLE OF THE METHODS

          1. 1.1. Reference method

          2. 1.2. Usual method

        2. 2. REFERENCE METHOD

          1. 2.1. Reagents

            1. 2.1.1. Solution containing 1 g of potassium per litre:

            2. 2.1.2. Matrix (model) solution:

            3. 2.1.3. Caesium chloride solution containing 5 % caesium:

          2. 2.2. Apparatus

            1. 2.2.1. . . . . . . . . . ....

            2. 2.2.2. . . . . . . . . . ....

          3. 2.3. Procedure

            1. 2.3.1. Preparation of sample

            2. 2.3.2. Calibration

            3. 2.3.3. Determination

          4. 2.4. Expression of results

            1. 2.4.1. Method of calculation

            2. 2.4.2. Repeatability (r)

            3. 2.4.3. Reproducibility (R)

            4. 2.4.4. Other ways of expressing results

        3. 3. USUAL METHOD: FLAME PHOTOMETRY

          1. 3.1. Reagents

            1. 3.1.1. Reference solution containing 100 mg potassium per litre

            2. 3.1.2. Dilution solution

          2. 3.2. Apparatus

            1. 3.2.1. . . . . . . . . . ....

          3. 3.3. Procedure

            1. 3.3.1. Calibration

            2. 3.3.2. Determination

          4. 3.4. Expression of results

            1. 3.4.1. Method of calculation

            2. 3.4.2. Repeatability (r)

            3. 3.4.3. Reproducibility (R)

            4. 3.4.4. Other ways of expressing results:

      30. 28. MAGNESIUM

        1. 1. PRINCIPLE OF THE METHOD

        2. 2. REAGENTS

          1. 2.1. Concentrated standard solution containing 1 g magnesium per litre

          2. 2.2. Dilute standard solution containing 5 mg magnesium per litre.

        3. 3. APPARATUS

          1. 3.1. . . . . . . . . . ....

          2. 3.2. . . . . . . . . . ....

        4. 4. PROCEDURE

          1. 4.1. Preparation of sample

          2. 4.2. Calibration

          3. 4.3. Determination

        5. 5. EXPRESSION OF RESULTS

          1. 5.1. Method of calculation

          2. 5.2. Repeatability (r)

          3. 5.3. Reproducibility (R)

      31. 29. CALCIUM

        1. 1. PRINCIPLE OF THE METHOD

        2. 2. REAGENTS

          1. 2.1. Standard solution containing 1 g calcium per litre

          2. 2.2. Dilute standard solution containing 50 mg calcium per litre

          3. 2.3. Lanthanum chloride solution containing 50 g lanthanum per litre

        3. 3. APPARATUS

          1. 3.1. . . . . . . . . . ....

          2. 3.2. . . . . . . . . . ....

        4. 4. PROCEDURE

          1. 4.1. Preparation of sample

          2. 4.2. Calibration

          3. 4.3. Determination

        5. 5. EXPRESSION OF RESULTS

          1. 5.1. Method of calculation

          2. 5.2. Repeatability (r)

          3. 5.3. Reproducibility (R)

      32. 30. IRON

        1. 1. PRINCIPLE OF THE METHODS

        2. 2. REFERENCE METHOD

          1. 2.1. Reagents

            1. 2.1.1. . . . . . . . . . ....

            2. 2.1.2 . . . . . . . . . ....

          2. 2.2. Apparatus

            1. 2.2.1 . . . . . . . . . ....

            2. 2.2.2. . . . . . . . . . ....

            3. 2.2.3. . . . . . . . . . ....

          3. 2.3. Procedure

            1. 2.3.1. Preparation of sample

            2. 2.3.2. Calibration

            3. 2.3.3. Determination

          4. 2.4. Expression of results

            1. 2.4.1. Method of calculation

        3. 3. USUAL METHOD

          1. 3.1. Reagents

            1. 3.1.1. . . . . . . . . . ....

            2. 3.1.2. . . . . . . . . . ....

            3. 3.1.3. . . . . . . . . . ....

            4. 3.1.4. . . . . . . . . . ....

            5. 3.1.5 . . . . . . . . . ....

            6. 3.1.6. . . . . . . . . . ....

            7. 3.1.7. . . . . . . . . . ....

            8. 3.1.8. . . . . . . . . . ....

            9. 3.1.9. . . . . . . . . . ....

            10. 3.1.10. . . . . . . . . . ....

          2. 3.2. Apparatus

            1. 3.2.1. . . . . . . . . . ....

            2. 3.2.2. . . . . . . . . . ....

          3. 3.3. Procedure

            1. 3.3.1. Digestion

              1. 3.3.1.1. For wines with sugar content below 50 g/l:

              2. 3.3.1.2. For musts and wines with sugar content above 50 g/l:

                1. 3.3.1.2.1. . . . . . . . . . ....

                2. 3.3.1.2.2. . . . . . . . . . ....

            2. 3.3.2. Blank experiment

            3. 3.3.3. Determination

            4. 3.3.4. Calibration

          4. 3.4. Expression of results

            1. 3.4.1. Method of calculation

      33. 31. COPPER

        1. 1. PRINCIPLE OF THE METHOD

        2. 2. APPARATUS

          1. 2.1. . . . . . . . . . ....

          2. 2.2. . . . . . . . . . ....

          3. 2.3. . . . . . . . . . ....

          4. 2.4. . . . . . . . . . ....

        3. 3. REAGENTS

          1. 3.1. . . . . . . . . . ....

          2. 3.2. . . . . . . . . . ....

          3. 3.3. . . . . . . . . . ....

          4. 3.4. . . . . . . . . . ....

          5. 3.5. . . . . . . . . . ....

        4. 4. PROCEDURE

          1. 4.1. Preparation of sample and determination of copper

          2. 4.2. Calibration

          3. 4.3. . . . . . . . . . ....

        5. 5. EXPRESSION OF RESULTS

          1. 5.1. Method of calculation

      34. 32. CADMIUM

        1. 1. Principle

        2. 2. APPARATUS

          1. 2.1. . . . . . . . . . ....

          2. 2.2. . . . . . . . . . ....

          3. 2.3. . . . . . . . . . ....

        3. 3. REAGENTS

          1. 3.1. . . . . . . . . . ....

          2. 3.2. . . . . . . . . . ....

          3. 3.3. . . . . . . . . . ....

          4. 3.4. . . . . . . . . . ....

          5. 3.5. . . . . . . . . . ....

          6. 3.6. . . . . . . . . . ....

          7. 3.7. . . . . . . . . . ....

        4. 4. PROCEDURE

          1. 4.1. Preparation of the sample

          2. 4.2. Preparation of the calibration range of solutions

          3. 4.3. Determination

            1. 4.3.1. Programming of oven (for guidance only):

            2. 4.3.2. Atomic absorption measurements:

        5. 5. EXPRESSION OF RESULTS

          1. 5.1. Method of calculation

      35. 33. SILVER

        1. 1. PRINCIPLE OF THE METHOD

        2. 2. APPARATUS

          1. 2.1. . . . . . . . . . ....

          2. 2.2. . . . . . . . . . ....

          3. 2.3. . . . . . . . . . ....

          4. 2.4. . . . . . . . . . ....

          5. 2.5. . . . . . . . . . ....

          6. 2.6. . . . . . . . . . ....

        3. 3. REAGENTS

          1. 3.1. . . . . . . . . . ....

          2. 3.2. . . . . . . . . . ....

          3. 3.3. . . . . . . . . . ....

          4. 3.4. . . . . . . . . . ....

          5. 3.5. . . . . . . . . . ....

        4. 4. PROCEDURE

          1. 4.1. Preparation of sample

          2. 4.2. Calibration

          3. 4.3. . . . . . . . . . ....

        5. 5. EXPRESSION OF RESULTS

          1. 5.1. Method of calculation

      36. 34. ZINC

        1. 1. PRINCIPLE OF THE METHOD

        2. 2. REAGENTS

          1. 2.1. . . . . . . . . . ....

          2. 2.2. . . . . . . . . . ....

        3. 3. APPARATUS

          1. 3.1. . . . . . . . . . ....

          2. 3.2. . . . . . . . . . ....

          3. 3.3. . . . . . . . . . ....

        4. 4. PROCEDURE

          1. 4.1. Preparation of sample

          2. 4.2. Calibration

          3. 4.3. Determination

        5. 5. EXPRESSION OF RESULTS

          1. 5.1. Method of calculation

      37. 35. LEAD

        1. 1. PRINCIPLE

        2. 2. APPARATUS

          1. 2.1. . . . . . . . . . ....

          2. 2.2. . . . . . . . . . ....

          3. 2.3. . . . . . . . . . ....

        3. 3. REAGENTS

          1. 3.1. . . . . . . . . . ....

          2. 3.2. . . . . . . . . . ....

          3. 3.3. . . . . . . . . . ....

          4. 3.4. . . . . . . . . . ....

        4. 4. PROCEDURE

          1. 4.1. Preparation of the sample

          2. 4.2. Preparation of the calibration range of solutions

          3. 4.3. Determination

            1. 4.3.1 Programming of oven (for guidance only):

            2. 4.3.2. Measurements

        5. 5. EXPRESSION OF RESULTS

          1. 5.1. Method of calculation

      38. 36. FLUORIDES

        1. 1. PRINCIPLE

        2. 2. APPARATUS

          1. 2.1. . . . . . . . . . ....

          2. 2.2. . . . . . . . . . ....

          3. 2.3. . . . . . . . . . ....

          4. 2.4. . . . . . . . . . ....

          5. 2.5. . . . . . . . . . ....

          6. 2.6. . . . . . . . . . ....

        3. 3. REAGENTS

          1. 3.1. . . . . . . . . . ....

          2. 3.2. . . . . . . . . . ....

          3. 3.3. . . . . . . . . . ....

        4. 4. PROCEDURE

          1. 4.1. Direct method

          2. 4.2. The known additions method

        5. 5. CALCULATIONS

      39. 37. CARBON DIOXIDE

        1. 1. PRINCIPLE OF THE METHOD

          1. 1.1. Reference method

            1. 1.1.1. Still wines (CO2 over pressure ≤ 0,5 × 105 Pa)

            2. 1.1.2. Sparkling and semi-sparkling wines

          2. 1.2. Usual method: sparkling and semi-sparkling wines

        2. 2. REFERENCE METHOD

          1. 2.1. . . . . . . . . . ....

            1. 2.1.1. Apparatus

              1. 2.1.1.1. . . . . . . . . . ....

              2. 2.1.1.2. . . . . . . . . . ....

            2. 2.1.2. Reagents

              1. 2.1.2.1. . . . . . . . . . ....

              2. 2.1.2.2. . . . . . . . . . ....

              3. 2.1.2.3. . . . . . . . . . ....

            3. 2.1.3. Procedure

            4. 2.1.4. Expression of results

          2. 2.2. Sparkling and semi-sparkling wines

            1. 2.2.1. Apparatus

              1. 2.2.1.1. . . . . . . . . . ....

              2. 2.2.1.2. . . . . . . . . . ....

            2. 2.2.2. Reagents

              1. 2.2.2.1. . . . . . . . . . ....

              2. 2.2.2.2. . . . . . . . . . ....

              3. 2.2.2.3. . . . . . . . . . ....

            3. 2.2.3. Procedure

            4. 2.2.4. Expression of results

          3. 2.3. Calculation of the theoretical excess pressure

        3. 3. USUAL METHOD: SPARKLING AND SEMI-SPARKLING WINES

          1. 3.1. Apparatus

            1. 3.1.1. Aphrometer

          2. 3.2. Procedure

          3. 3.3. Expression of results

        4. 4. RELATIONSHIP BETWEEN THE PRESSURE AND THE QUANTITY OF CARBON DIOXIDE...

      40. 37a — MEASURING EXCESS PRESSURE IN SPARKLING AND SEMI-SPARKLING WINES

        1. 1. PRINCIPLE

        2. 2. EQUIPMENT

          1. 2.1. Bottles with capsules

          2. 2.2. Bottles with corks

        3. 3. PROCEDURE

          1. 3.1. Bottles with capsules

          2. 3.2. Bottles with corks

        4. 4. EXPRESSION OF RESULTS

        5. 5. CONTROLLING THE RESULTS

      41. 38. CYANIDE DERIVATIVES

        1. 1. PRINCIPLE

        2. 2. APPARATUS

          1. 2.1. Distillation apparatus

          2. 2.2. . . . . . . . . . ....

          3. 2.3. . . . . . . . . . ....

          4. 2.4. . . . . . . . . . ....

          5. 2.5. . . . . . . . . . ....

        3. 3. REAGENTS

          1. 3.1. . . . . . . . . . ....

          2. 3.2. . . . . . . . . . ....

          3. 3.3. . . . . . . . . . ....

          4. 3.4. . . . . . . . . . ....

          5. 3.5. . . . . . . . . . ....

          6. 3.6. . . . . . . . . . ....

        4. 4. PROCEDURE

          1. 4.1. Distillation

          2. 4.2. Measurement

        5. 5. DETERMINING THE CALIBRATION CURVE

          1. 5.1. Argentometric titration of the potassium cyanide

          2. 5.2. Standard curve

            1. 5.2.1. Preparation of standard solutions

            2. 5.2.2. Titration

        6. 6. EXPRESSION OF RESULTS

          1. 6.1. Method of calculation

      42. 39. ALLYL ISOTHIOCYANATE

        1. 1. PRINCIPLE OF THE METHOD

        2. 2. REAGENTS

          1. 2.1. . . . . . . . . . ....

          2. 2.2. . . . . . . . . . ....

          3. 2.3. . . . . . . . . . ....

        3. 3. APPARATUS

          1. 3.1. . . . . . . . . . ....

          2. 3.2. . . . . . . . . . ....

          3. 3.3. . . . . . . . . . ....

          4. 3.4. . . . . . . . . . ....

          5. 3.5. . . . . . . . . . ....

          6. 3.6. . . . . . . . . . ....

        4. 4. PROCEDURE

      43. 40. CHROMATIC PROPERTIES

        1. 1. WINES AND MUSTS

          1. 1.1. Definitions

          2. 1.2. Principle of the methods

            1. 1.2.1. Reference method

            2. 1.2.2. Usual method (applicable to red and rosé wines)

          3. 1.3. Reference method

            1. 1.3.1. Apparatus

              1. 1.3.1.1. . . . . . . . . . ....

              2. 1.3.1.2. . . . . . . . . . ....

            2. 1.3.2. Procedure

              1. 1.3.2.1. Preparation of the sample

              2. 1.3.2.2. Measurements

            3. 1.3.3. Calculations

            4. 1.3.4. Expression of results

              1. 1.3.4.1. . . . . . . . . . ....

              2. 1.3.4.2. . . . . . . . . . ....

              3. 1.3.4.3. . . . . . . . . . ....

          4. 1.4. Usual method

            1. 1.4.1. Apparatus

              1. 1.4.1.1. . . . . . . . . . ....

              2. 1.4.1.2. . . . . . . . . . ....

            2. 1.4.2. Preliminary preparation of the sample

            3. 1.4.3. Procedure

            4. 1.4.4. Expression of results

              1. 1.4.4.1. Calculations

          5. TABLE 1 Transformation of absorbences to transmittances (T%)

            1. Method of use

            2. Example:

        2. 2. RECTIFIED CONCENTRATED MUSTS

          1. 2.1. Principle of the method

          2. 2.2. Apparatus

            1. 2.2.1. . . . . . . . . . ....

            2. 2.2.2. . . . . . . . . . ....

            3. 2.2.3. . . . . . . . . . ....

          3. 2.3. Procedure

            1. 2.3.1. Preparation of the sample

            2. 2.3.2. Determination of absorbence

          4. 2.4. Expression of results

      44. 41. FOLIN-CIOCALTEU INDEX

        1. 1. DEFINITION

        2. 2. PRINCIPLE OF THE METHOD

        3. 3. REAGENTS

          1. 3.1. Folin-Ciocalteu reagent

          2. 3.2. . . . . . . . . . ....

        4. 4. APPARATUS

          1. 4.1. . . . . . . . . . ....

          2. 4.2. . . . . . . . . . ....

        5. 5. PROCEDURE

          1. 5.1. Red wine

          2. 5.2. White wine

          3. 5.3. Rectified concentrated must

            1. 5.3.1. Preparation of sample

            2. 5.3.2. Measurement

        6. 6. EXPRESSION OF RESULTS

          1. 6.1. Method of calculation

          2. 6.2. Repeatability

      45. 42. SPECIAL METHODS OF ANALYSIS FOR RECTIFIED CONCENTRATED GRAPE MUST

        1. (a) TOTAL CATIONS

          1. 1. PRINCIPLE OF THE METHOD

          2. 2. APPARATUS

            1. 2.1. . . . . . . . . . ....

            2. 2.2. . . . . . . . . . ....

            3. 2.3. . . . . . . . . . ....

          3. 3. REAGENTS

            1. 3.1. . . . . . . . . . ....

            2. 3.2. . . . . . . . . . ....

            3. 3.3. . . . . . . . . . ....

          4. 4. PROCEDURE

            1. 4.1. Preparation of sample

            2. 4.2. Preparation of the ion exchange column

            3. 4.3. Ion exchange

          5. 5. EXPRESSION OF RESULTS

            1. 5.1. . . . . . . . . . ....

        2. (b) CONDUCTIVITY

          1. 1. PRINCIPLE OF THE METHOD

          2. 2. APPARATUS

            1. 2.1. . . . . . . . . . ....

            2. 2.2. . . . . . . . . . ....

          3. 3. REAGENTS

            1. 3.1. . . . . . . . . . ....

            2. 3.2. . . . . . . . . . ....

          4. 4. PROCEDURE

            1. 4.1. Preparation of the sample to be analysed

            2. 4.2. Determination of conductivity

          5. 5. EXPRESSION OF RESULTS

            1. 5.1. Calculations

        3. (c) HYDROXYMETHYLFURFURAL (HMF)

          1. 1. PRINCIPLE OF THE METHODS

            1. 1.1. Colorimetric method

            2. 1.2. High-performance liquid chromatography (HPLC)

          2. 2. COLORIMETRIC METHOD

            1. 2.1. Apparatus

              1. 2.1.1. . . . . . . . . . ....

              2. 2.1.2. . . . . . . . . . ....

            2. 2.2. Reagents

              1. 2.2.1. Barbituric acid, 0,5 % solution (m/v).

              2. 2.2.2. Paratoluidine solution, 10 % (m/v).

              3. 2.2.3. Ethanal (acetaldehyde), CH3CHO, 1 % (m/v) aqueous solution.

              4. 2.2.4. Hydroxymethylfurfural, C6O3H6, 1 g/l aqueous solution.

            3. 2.3. Procedure

              1. 2.3.1. Preparation of sample

              2. 2.3.2. Colorimetric determination

              3. 2.3.3. Preparation of the calibration curve

            4. 2.4. Expression of results

              1. 2.4.1. Method of calculation

          3. 3. HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

            1. 3.1. Apparatus

              1. 3.1.1. High-performance liquid chromatograph equipped with:

              2. 3.1.2. . . . . . . . . . ....

            2. 3.2. Reagents

              1. 3.2.1. . . . . . . . . . ....

              2. 3.2.2. . . . . . . . . . ....

              3. 3.2.3. . . . . . . . . . ....

              4. 3.2.4. . . . . . . . . . ....

              5. 3.2.5. . . . . . . . . . ....

            3. 3.3. Procedure

              1. 3.3.1. Preparation of sample

              2. 3.3.2. Chromatographic determination

            4. 3.4. EXPRESSION OF RESULTS

              1. 3.4.1. Method of calculation

        4. (d) HEAVY METALS

          1. 1. PRINCIPLE OF THE METHODS

            1. I. Rapid method for evaluation of heavy metals

            2. II. Determination of lead content by atomic absorption spectrophotometry

          2. 2. RAPID METHOD FOR EVALUATION OF HEAVY METALS

            1. 2.1. Reagents

              1. 2.1.1. Dilute hydrochloric acid, 70 % (m/v).

              2. 2.1.2. Dilute hydrochloric acid, 20 % (m/v).

              3. 2.1.3. . . . . . . . . . ....

              4. 2.1.4. pH 3,5 buffer solution.

              5. 2.1.5. . . . . . . . . . ....

              6. 2.1.6. . . . . . . . . . ....

              7. 2.1.7. Thioacetamide reagent.

              8. 2.1.8. Solution containing 0,002 g/l of lead.

            2. 2.2. Procedure

            3. 2.3. Calculations

          3. 3. DETERMINATION OF LEAD CONTENT BY ATOMIC ABSORPTION SPECTROPHOTOMETRY

            1. 3.1. Apparatus

              1. 3.1.1. . . . . . . . . . ....

              2. 3.1.2. . . . . . . . . . ....

            2. 3.2. Reagents

              1. 3.2.1. Dilute acetic acid.

              2. 3.2.2. . . . . . . . . . ....

              3. 3.2.3. . . . . . . . . . ....

              4. 3.2.4. . . . . . . . . . ....

            3. 3.3. Procedure

              1. 3.3.1. Preparation of solution to be examined

              2. 3.3.2. Preparation of reference solutions

              3. 3.3.3. Control

              4. 3.3.4. Determination

            4. 3.4. Expression of results

              1. 3.4.1. Calculations

        5. (e) CHEMICAL DETERMINATION OF ETHANOL

          1. 1. PRINCIPLE OF THE METHOD

          2. 2. APPARATUS

            1. 2.1. . . . . . . . . . ....

          3. 3. REAGENTS

            1. 3.1. Potassium dichromate solution.

            2. 3.2. Iron (II) ammonium sulphate solution.

            3. 3.3. Potassium permanganate solution.

            4. 3.4. Dilute sulphuric acid, 1:2 (v/v).

            5. 3.5. Ferrous orthophenanthroline reagent.

          4. 4. PROCEDURE

            1. 4.1. Distillation

            2. 4.2. Oxidation

            3. 4.3. Titration

          5. 5. EXPRESSION OF RESULTS

            1. 5.1. Method of calculation

        6. (f) MESO-INOSITOL, SCYLLO-INOSITOL AND SUCROSE

          1. 1. PRINCIPLE

          2. 2. REAGENTS

            1. 2.1. . . . . . . . . . ....

            2. 2.2. . . . . . . . . . ....

            3. 2.3. . . . . . . . . . ....

            4. 2.4. . . . . . . . . . ....

            5. 2.5 . . . . . . . . . ....

          3. 3. APPARATUS

            1. 3.1. . . . . . . . . . ....

            2. 3.2. . . . . . . . . . ....

            3. 3.3. . . . . . . . . . ....

            4. 3.4. . . . . . . . . . ....

            5. 3.5. . . . . . . . . . ....

            6. 3.6. . . . . . . . . . ....

            7. 3.7. . . . . . . . . . ....

          4. 4. METHOD OF OPERATION

          5. 5. CALCULATION OF RESULTS

            1. 5.1. . . . . . . . . . ....

          6. 6. EXPRESSION OF RESULTS

            1. 6.1. . . . . . . . . . ....

      46. 43. DETERMINATION OF THE ISOTOPIC RATIO 18O/16O OF THE WATER CONTENT...

        1. I. DESCRIPTION OF THE METHOD

          1. 1. Method objective

          2. 2. Principle

          3. 3. Reagents

          4. 4. Laboratory equipment

          5. 5. Experimental determinations

            1. 5.1. Manual method

              1. Operational mode of the equilibration method

              2. Degasing of the ramp

              3. Equilibration of the water and the CO2

              4. Transfer of the CO2 exchanged in the measuring cells

            2. 5.2. Use of an automatic exchange apparatus

          6. 6. Calculation and expression of the results

          7. 7. Fidelity

      47. 44. DETERMINATION OF ETHYL CARBAMATE IN WINE: SELECTIVE DETECTION METHOD USING...

        1. A. Principle

        2. B. Apparatus and chromatographic conditions (example)

        3. C. Reagents

        4. D. Preparation of the test sample

        5. E. Extraction

        6. F. GC/MS analysis

        7. G. Collaborative analysis

      48. 45. DETERMINATION BY ISOTOPE MASS SPECTROMETRY OF THE 13C/12C RATIO IN...

        1. 1. FIELD OF APPLICATION

        2. 2. REFERENCE STANDARDS

        3. 3. TERMS AND DEFINITIONS

        4. 4. PRINCIPLE

        5. 5. REAGENTS

        6. 6. APPARATUS AND EQUIPMENT

          1. 6.1. Isotope ratio mass spectrometer (IRMS)

          2. 6.2. Combustion apparatus

            1. 6.2.1. Continuous-flow systems

            2. 6.2.2. Separate preparation system

        7. 7. PREPARATION OF SAMPLES FOR TESTS

        8. 8. PROCEDURE

        9. 9. CALCULATION

        10. 10. QUALITY ASSURANCE AND CONTROL

        11. 11. PERFORMANCE CHARACTERISTICS OF THE METHOD (Accuracy)

          1. 11.1. Joint study on distillates

          2. 11.2. Interlaboratory study on two wines and one alcohol

          3. 11.3. Results of the exercises carried out to monitor proficiency in...

          4. 11.4. Limits of repeatability and reproducibility

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