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Commission Regulation (EEC) No 000/90 (repealed)Dangos y teitl llawn

Commission Regulation (EEC) No 000/90 of 17 September 1990 determining Community methods for the analysis of wines (repealed)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.(1) The Community methods for the analysis of wine making...

  3. Article 2.For the purposes of applying this Regulation: the repeatability shall...

  4. Article 3.(1) Automated analytical methods shall be acceptable, under the responsibility...

  5. Article 4.Wherever mention is made of water for solution, dilution, or...

  6. Article 5.Regulation (EEC) No 1108/82 is repealed. However Article 1 (4) of...

  7. Article 6.This Regulation shall enter into force on the day of...

  8. Signature

    1. ANNEX

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

        1. 1. DEFINITIONS

        2. 2. PRINCIPLE OF METHODS

          1. Note:

        3. 3. PRELIMINARY TREATMENT OF SAMPLE

        4. 4. REFERENCE METHOD

          1. 4.1. Apparatus:

            1. 4.1.1. A Pyrex pycnometer, of approximately 100 ml capacity, with a removable...

            2. 4.1.2. A tare bottle, consisting of a vessel with the same...

            3. 4.1.3. A twin-pan balance with a range of at least 300 g...

          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. The repeatability of the density measurements

            4. 4.3.4. The reproducibility of the density measurements:

        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. Weighing of clean dry pycnometer:

              2. 2. Weighing of pycnometer filled with water at t °C:

              3. 3. Calculation of mass of air contained in the pycnometer:

              4. 4. Characteristic values to be retained:

            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. Weight of clean dry pycnometer:

              2. 2. Weight of pycnometer filled with water at t °C:

              3. 3. Mass of air contained in the pycnometer:

              4. 4. Characteristic values to be retained:

            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. Instruments graduated in percentage by mass of sucrose: use Table...

            2. 5.1.2. Instruments graduated in refractive index: find the index measured at...

          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

          1. Note:

        2. 2. PRINCIPLE OF METHODS

          1. 2.1. Distillation of wine made alkaline by a suspension of calcium...

          2. 2.2. Reference methods:

          3. 2.3. Usual methods:

            1. 2.3.1. Measurement of the alcoholic strength of the distillate with a...

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

            3. 2.3.3. Measurement of the alcoholic strength of the distillate by refractometry....

              1. Note:

        3. 3. METHOD OF OBTAINING DISTILLATE

          1. 3.1. Apparatus

            1. 3.1.1. Distillation apparatus, consisting of:

            2. 3.1.2. Steam-distillation apparatus consisting of:

          2. 3.2. Reagents

            1. 3.2.1. A 2 M suspension of calcium hydroxide, obtained by carefully pouring...

          3. 3.3. Preparation of sample

          4. 3.4. Procedure

            1. Note:

        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. Use the standardized pycnometer as described in the chapter ‘Density...

            2. 4.2. Procedure

            3. 4.3. Expression of results

              1. 4.3.1. Method of calculation

                1. Note:

              2. 4.3.2. Repeatability, r: r = 0,10 % vol.

              3. 4.3.3. Reproducibility, R: R = 0,19 % vol.

          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. Single-pan hydrostatic balance with a sensitivity of 1 mg.

                2. 1.5.2. Float with a volume of at least 20 ml, specially adapted...

                3. 1.5.3. Measuring cylinder bearing a level mark. The float must be...

                4. 1.5.4. Thermometer (or temperature-measuring probe) graduated in degrees and tenths of...

                5. 1.5.5. Weights, calibrated by a recognised certifying body.

              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. Fill the measuring cylinder to the mark with double-distilled water...

                  2. 1.6.2.2. Immerse the float and the thermometer, stir, read off the...

                3. 1.6.3. Control using a water-alcohol solution

                  1. 1.6.3.1. Fill the measuring cylinder to the mark with a water-alcohol...

                  2. 1.6.3.2. Immerse the float and the thermometer, stir, read off the...

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

                  1. 1.6.4.1. Pour the test sample into the measuring cylinder up to...

                  2. 1.6.4.2. Immerse the float and the thermometer, stir, read off the...

                  3. 1.6.4.3. Correct ρ t using the table of densities ρ t...

                5. 1.6.5. Cleaning of float and measuring cylinder

                  1. 1.6.5.1. Immerse the float in the float-cleaning solution in the measuring...

                  2. 1.6.5.2. Allow to soak for one hour spinning the float periodically....

                  3. 1.6.5.3. Rinse with copious amounts of tap water followed by distilled...

                  4. 1.6.5.4. Dry with soft laboratory paper which does not shed fibres....

                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. Electronic hydrostatic balance (accurate to 5 decimal places), if possible...

                2. 2.3.2. Electronic densimeter, if possible with autosampler.

              4. 2.4. Analysis

              5. 2.5. Result

              6. 2.6. Evaluations of the results

                1. 2.6.1. The trial results were examined for evidence of individual systematic...

                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

              1. Note:

        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. The constants of the pycnometer have been determined and calculated...

            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. The constants of the pycnometer have been determined and calculated...

            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. Reference method: after neutralization and removal of alcohol, the wine...

            2. 2.1.2. Usual methods: the wine is treated with one of the...

              1. 2.1.2.1. Neutral lead acetate;

              2. 2.1.2.2. Zinc 2-hexacyanoferrate.

          2. 2.2. Determination

            1. 2.2.1. Single method: the clarified wine or must is reacted with...

        3. 3. CLARIFICATION

          1. 3.1. Reference method

            1. 3.1.1. Reagents

              1. 3.1.1.1. 1 M solution hydrochloric acid (HCl);

              2. 3.1.1.2. 1 M solution sodium hydroxide (NaOH);

              3. 3.1.1.3. 4 M solution acetic acid (CH3COOH);

              4. 3.1.1.4. 2 M solution sodium hydroxide (NaOH);

              5. 3.1.1.5. Anion exchange resin (Dowex 3 (20-50 mesh) or equivalent resin)....

                1. Preparation of the anion exchange resin column

                2. Regeneration of the resin

              6. 3.1.1.6. Neutral lead acetate solution (approximately saturated)

              7. 3.1.1.7. Calcium carbonate (Ca CO3)

            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. Musts and mistelles: prepare a 10 % solution of the liquid...

                2. 2. Sweet wines, whether fortified or not, having a density between...

                3. 3. Semi-sweet wines having a density at 20 °C between 0,997 and...

          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. For qualitative testing by thin-layer chromatography: sucrose is separated from...

          2. II. For testing and determination by high-performance liquid chromatography: the sucrose...

            1. Note:

        2. 2. QUALITATIVE TESTING BY THIN-LAYER CHROMATOGRAPHY

          1. 2.1. Equipment

            1. 2.1.1. Chromatograhic plates covered with a desired thickness of cellulose powder...

            2. 2.1.2. Chromatography tank.

            3. 2.1.3. Micrometric syringe or micropipette.

            4. 2.1.4. Oven with regulation to 105 ± 2 °C.

          2. 2.2. Reagents

            1. 2.2.1. Decolourizing charcoal.

            2. 2.2.2. Mobile phase: Dichloromethane — glacial acetic acid (p20 — 1,05 g/ml)...

            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. High-performance liquid chromatograph equipped with:

              1. 1. 10 µl loop injector,

              2. 2. a detector: a differential refractometer or an interferometer refractometer,

              3. 3. an alkylamine-bonded silica column (length 25 cm, internal diameter 4 mm),

              4. 4. a guard column filled with the same phase,

              5. 5. an arrangement for insulating the guard column and analytical columns...

              6. 6. a recorder and, if required, an integrator,

              7. 7. mobile phase flow rate: 1 ml/min.

            2. 3.1.2. Arrangement for membrane filtration (0,45 µm).

          2. 3.2. Reagents

            1. 3.2.1. Doubly distilled water.

            2. 3.2.2. HPLC quality acetonitrile (CH3CN).

            3. 3.2.3. Mobile phase: acetonitrile-water, previously subjected to membrane filtration (0,45 µm), (80:20...

            4. 3.2.4. Standard solution: 1,2 g/l aqueous sucrose solution. Filter using a 0,45 µm...

          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. For wines and musts: calculate the concentration in g/l.

            2. 3.4.2. For rectified concentrated musts: let C be the sucrose concentration...

          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. Solution 1: buffer solution (0,3 M triethanolamine, pH 7,6, 4 × 10−3 M in...

          2. 4.2. Solution 2: nicotinamide adenine dinucleotide phosphate solution (about 11,5 × 10−3 M): dissolve...

          3. 4.3. Solution 3: adenosine 5′-triphosphate solution (about 81 × 10−3 M): dissolve 250 mg disodium...

          4. 4.4. Solution 4: hexokinase/glucose 6-phosphate dehydrogenase: mix 0,5 ml hexokinase (2 mg of...

          5. 4.5. Solution 5: phosphoglucose isomerase (2 mg of protein/ml or 700 U/ml). The...

            1. Note:

        5. 5. PROCEDURE

          1. 5.1. Preparation of sample

          2. 5.2. Determination

            1. Note:

          3. 5.3. Expression of results

            1. 5.3.1. Calculation

              1. Note:

            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. Note:

            2. 3.1.1. Apparatus and reagents

            3. 3.1.2. Procedure

              1. 3.1.2.1. Determine the alcoholic strength of the wine (t v) to...

              2. 3.1.2.2. Extraction of the ethanol

                1. Note:

              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

                1. Note:

          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

              1. Note:

        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. For each of the isotope parameters, calculate the average of...

            1. Note:

        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. boiling water-bath;

          2. 3.2. balance sensitive to 0,1 mg;

          3. 3.3. hot-plate or infra-red evaporator;

          4. 3.4. temperature-controlled electric muffle furnace;

          5. 3.5. desiccator;

          6. 3.6. flat-bottomed platinum dish 70 mm in diameter and 25 mm in height....

        4. 4. PROCEDURE

        5. 5. EXPRESSION OF RESULTS

          1. 5.1. Method of calculation

      10. 10. ALKALINITY OF THE ASH

        1. 1. DEFINITION

        2. 2. PRINCIPLE OF THE METHOD

        3. 3. REAGENTS AND APPARATUS

          1. 3.1. 0,05 M sulphuric acid solution (H2SO4);

          2. 3.2. 0,1 M sodium hydroxide solution (NaOH);

          3. 3.3. methyl orange, 0,1 % solution in distilled water;

          4. 3.4. boiling water-bath.

        4. 4. PROCEDURE

        5. 5. EXPRESSION OF RESULTS

      11. 11. CHLORIDES

        1. 1. PRINCIPLE

        2. 2. APPARATUS

          1. 2.1. pH/mV meter graduated at intervals of at least 2 mV.

          2. 2.2. Magnetic stirrer.

          3. 2.3. Ag/AcCl electrode with a saturated solution of nitrate potassium as...

          4. 2.4. Microburette graduated in 1/100 ml.

          5. 2.5. Chronometer.

        3. 3. REAGENTS

          1. 3.1. Standard chloride solution: 2,1027 g of potassium chloride, KCl (max. 0,005 %...

          2. 3.2. Silver nitrate titrating solution: 4,7912 g of analytical grade silver nitrate,...

          3. 3.3. Nitric acid, of at least 65 % purity ( ρ20 = 1,40 g/ml)....

        4. 4. PROCEDURE

          1. 4.1. 5,0 ml of standard chloride solution are measured into a 150 ml...

          2. 4.2. 5 ml of the standard chloride solution are measured into a...

          3. 4.3. 50 ml of wine for analysis are measured into a 150 ml...

        5. 5. EXPRESSION OF RESULTS

          1. 5.1. Calculations

          2. 5.2. Repeatability (r):

          3. 5.3. Reproducibility (R):

        6. 6. Note: For very precise determination.

      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 M solution of hydrochloric acid.

            2. 2.1.2. Barium chloride solution of 200 g/l of BaCl2 · 2H2O.

          2. 2.2. Procedure

            1. 2.2.1. General procedure:

            2. 2.2.2. Special procedure: sulphited must and wine with a high sulphur...

          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. Buffer solution pH 7,0:

          2. 3.2. 0,1 M sodium hydroxide (NaOH) solution.

          3. 3.3. 4 g/l bromothymol blue indicator solution:

        4. 4. APPARATUS

          1. 4.1. Water vacuum pump.

          2. 4.2. 500 ml vacuum flask.

          3. 4.3. Potentiometer with scale graduated in pH values, and electrodes. The...

          4. 4.4. Measuring cylinders 50 ml (wine), 100 ml (rectified concentrated must).

        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. Crystalline tartaric acid (C4H6O6).

          2. 3.2. 0,1 M sodium hydroxide solution (NaOH).

          3. 3.3. 1 % phenolphthalein solution in 96 % vol neutral alcohol.

          4. 3.4. Hydrochloric acid (ρ 20 = 1,18 to 1,19 g/ml) diluted 1/4 (v/v)....

          5. 3.5. 0,005 M iodine (I2) solution.

          6. 3.6. Crystalline potassium iodide (KI).

          7. 3.7. 5 g/l starch solution.

          8. 3.8. Saturated solution of sodium borate (Na2B4O7 · 10H2O), i.e. about 55 g/l...

        4. 4. APPARATUS

          1. 4.1. Steam distillation apparatus consisting of:

          2. 4.2. Water pump.

          3. 4.3. Vacuum flask.

        5. 5. PROCEDURE

          1. 5.1. Preparation of sample: elimination of carbon dioxide. Place about 50 ml...

          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. Hydrochloric acid (HCl) (ρ 20 = 1,18 to 1,19 g/l).

            2. 7.2.2. Sodium thiosulphate, (Na2S2O3 · 5H2O) in a 0,1 M solution.

            3. 7.2.3. 10 % (m/v) solution of iron (III) ammonium sulphate (Fe2(SO4)3 ·...

            4. 7.2.4. 0,01 M solution of sodium salicylate.

          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. Calcium acetate solution containing 10 g of calcium per litre:

              2. 2.1.1.2. Calcium (±)tartrate, crystallized: CaC4O6H4 · 4H2O:

              3. 2.1.1.3. Precipitation solution (pH 4,75):

            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. Hydrochloric acid (HCl) (1:5 v/v) (ρ20 = 1,18 to 1,19 g/ml)

              2. 2.2.1.2. EDTA solution, 0,05 M:

              3. 2.2.1.3. Sodium hydroxide solution, 40 % (m/v):

              4. 2.2.1.4. Complexometric indicator: 1 % (m/m)

            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. Buffer solution pH 7,8.

          2. 2.2. Reduced nicotinamide adenine dinucleotide (NADH) solution (approximately 6 × 10− 3 M): dissolve...

          3. 2.3. Malate dehydrogenase/lactate dehydrogenase solution (MDH/LDH, 0,5 mg MDH/ml, 2,5 mg LDH/ml): mix...

          4. 2.4. Citrate-lyase (CL, 5 mg protein/ml): dissolve 168 mg lyophilisate in 1 ml ice-cold...

          5. 2.5. Polyvinylpolypyrrolidone (PVPP)

            1. Note:

        3. 3. APPARATUS

          1. 3.1. A spectrophotometer permitting measurement to be made at 340 nm, the...

          2. 3.2. Glass cells with optical path lengths of 1 cm or single-use...

          3. 3.3. Micropipettes for pipetting volumes in the range 0,02 to 2 ml....

        4. 4. PREPARATION OF THE SAMPLE

        5. 5. PROCEDURE

          1. Note:

        6. 6. EXPRESSION OF RESULTS

          1. 6.1. Method of calculation

            1. Note:

          2. 6.2. Repeatability (r)

          3. 6.3. Reproducibility (R)

      18. 18. LACTIC ACID

        1. 1. PRINCIPLE OF THE METHOD

          1. Note:

          2. 1.2. Usual method

        2. 2. REFERENCE METHOD

          1. 2.1. Reagents

            1. 2.1.1. Buffer solution, pH 10 (glycylglycine 0,6 mol/l; L-glutamate 0,1 mol/l):

            2. 2.1.2. Nicotinamide adenine dinucleotide (NAD) solution, approximately 40 × 10− 3 M: dissolve 900 mg...

            3. 2.1.3. Glutamate pyruvate transaminase (GPT) suspension, 20 mg/ml. The suspension remains stable...

            4. 2.1.4. L-lactate dehydrogenase (L-LDH) suspension, 5 mg/ml. This suspension remains stable for...

            5. 2.1.5. D-lactate dehydrogenase (D-LDH) suspension, 5 mg/ml. This suspension remains stable for...

          2. 2.2. Apparatus

            1. 2.2.1. A spectrophotometer permitting measurements to be made at 340 nm, the...

            2. 2.2.2. Glass cells with optical path lengths of 1 cm or single-use...

            3. 2.2.3. Micropipettes for pipetting sample volumes in the range 0,02 to...

          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

              1. Note:

          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

                1. Note:

              2. 2.5.1.2. L-lactic acid

                1. Note:

            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

            1. Note:

      19. 19. L-MALIC ACID

        1. 1. PRINCIPLE OF THE METHOD

        2. 2. REAGENTS

          1. 2.1. Buffer solution, pH 10

          2. 2.2. Nicotinamide adenine dinucleotide (NAD) solution, approximately 47 × 10− 3 M:

          3. 2.3. Glutamate oxaloacetate transaminase (GOT) suspension, 2 mg/ml. The suspension remains stable...

          4. 2.4. L-malate dehydrogenase (L-MDH) solution, 5 mg/ml. This solution remains stable for...

            1. Note:

        3. 3. APPARATUS

          1. 3.1. A spectrophotometer permitting measurement to be made at 340 nm, the...

          2. 3.2. Glass cells with optical path lengths of 1 cm or single-use...

          3. 3.3. Micropipettes for pipetting sample volumes in the range 0,01 to...

        4. 4. PREPARATION OF THE SAMPLE

        5. 5. PROCEDURE

        6. 6. EXPRESSION OF RESULTS

          1. 6.1. Method of calculation

            1. Note:

          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. Use content of bottle 1 undiluted. Before using bring solution...

            2. 2. Dissolve content of bottle 2 in 4 ml double-distilled water.

            3. 3. Dissolve content of one of bottles 3 in 0,6 ml double-distilled...

          2. Stability of the solutions

        3. 3. APPARATUS

          1. 3.1. A spectrophotometer permitting measurement to be made at 340 nm, the...

          2. 3.2. Glass cuvettes with optical path lengths of 1 cm (if preferred...

          3. 3.3. Micropipettes for pipetting volumes in the range 0,01 to 2 ml....

        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. Glass column approximately 250 mm in length and 35 mm internal diameter,...

          2. 2.2. Glass column approximately 300 mm in length and 10 to 11 mm...

          3. 2.3. Thermostatically controlled water bath at 100 °C.

          4. 2.4. Spectrophotometer set to measure absorbence at 420 nm using 10 mm cells....

        3. 3. REAGENTS

          1. 3.1. A strongly basic ion exchange resin (e.g. Merck III).

          2. 3.2. Sodium hydroxide 5 % (m/v).

          3. 3.3. Acetic acid 30 % (m/v).

          4. 3.4. Acetic acid 0,5 % (m/v).

          5. 3.5. Sodium sulphate solution 10 % (m/v).

          6. 3.6. Concentrated sulphuric acid 95 to 97 % (m/m).

          7. 3.7. Sulphuric acid 86 % (m/m).

          8. 3.8. Chromotropic acid 5 % (m/v)

          9. 3.9. DL-Malic acid solution 0,5 g/l.

        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. Crystalline tartaric acid, C4H6O6.

            2. 2.1.2. Calcium hydroxide, Ca(OH)2, solution, approximately 0,02 M.

            3. 2.1.3. Reference sorbic acid solution, 20 mg/l:

          2. 2.2. Apparatus

            1. 2.2.1. Steam distillation apparatus (see chapter ‘Volatile acidity’).

            2. 2.2.2. Water bath at 100 °C.

            3. 2.2.3. Spectrophotometer enabling absorbence measurements to be made at a wavelength...

          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. Ethyl ether, (C2H5)2O, distilled just before use.

            2. 3.1.2. Internal reference solution: solution of undecanoic acid, C11H22O2, in 95 %...

            3. 3.1.3. Aqueous solution of sulphuric acid, H2SO4 (ρ20 = 1,84 g/ml) diluted 1:3...

          2. 3.2. Apparatus

            1. 3.2.1. Gas chromatograph fitted with a flame ionization detector and a...

            2. 3.2.2. Microsyringe, 10 µl capacity graduated in 0,1 µl.

          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. Ethyl ether, (C2H5)2O.

            2. 4.1.2. Aqueous sulphuric acid solution, H2SO4 (ρ20 = 1,84 g/ml), diluted 1:3 (v/v)....

            3. 4.1.3. Reference solution of sorbic acid in an approximately 10 % vol...

            4. 4.1.4. Mobile phase: hexane-pentane-acetic acid (20:20:3) (C6H14/C5H12/CH3COOH, ρ20 = 1,05 g/ml).

          2. 4.2. Apparatus

            1. 4.2.1. Precoated 20 × 20 cm plates for thin layer chromatography coated with polyamide...

            2. 4.2.2. Cell for thin layer chromatography.

            3. 4.2.3. Micropipette or microsyringe for delivering volumes of 5 µl to within...

            4. 4.2.4. Ultraviolet lamp (254 nm).

          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. Orthophenylenediamine dihydrochloride solution, C6H10Cl2N2, 0,02 g per 100 ml; prepared just before...

            2. 2.1.2. Sodium acetate trihydrate solution, CH3COONa · 3H2O, 500 g/litre.

            3. 2.1.3. Mixed solution of boric acid and sodium acetate:

            4. 2.1.4. Glacial acetic acid solution, CH3COOH (ρ20 = 1,05 g/ml), diluted to 56 %...

            5. 2.1.5. Reference solution of L-ascorbic acid, 1 g/litre:

            6. 2.1.6. Very pure analytical grade activated carbon

          2. 2.2. Apparatus

            1. 2.2.1. Fluorimeter. Use a spectrofluorimeter equipped with a lamp giving a...

            2. 2.2.2. Sintered glass filter of porosity 3.

            3. 2.2.3. Test tubes (diameter approximately 10 mm).

            4. 2.2.4. Stirring rods for test tubes.

          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

                1. Note:

      26. 24. pH

        1. 1. PRINCIPLE

        2. 2. APPARATUS

          1. 2.1. pH meter with a scale calibrated in pH units and...

          2. 2.2. Electrodes:

            1. 2.2.1. Glass electrode, kept in distilled water.

            2. 2.2.2. Calomel-saturated potassium chloride reference electrode, kept in a saturated solution...

            3. 2.2.3. Or a combined electrode, kept in distilled water.

        3. 3. REAGENTS

          1. 3.1. Buffer solutions

            1. 3.1.1. Saturated solution of potassium hydrogen tartrate, containing at least 5,7 g...

            2. 3.1.2. Solution of potassium hydrogen phthalate, 0,05 M, containing 10,211 g of potassium...

            3. 3.1.3. Solution containing:

        4. 4. PROCEDURE

          1. 4.1. Preparation of the sample for analysis

            1. 4.1.1. For must and wine: use the must or wine directly....

            2. 4.1.2. For rectified concentrated must: dilute the rectified concentrated must with...

          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. The apparatus used should conform to the diagram shown below,...

              2. 2.2.1.2. A microburette.

            2. 2.2.2. Reagents

              1. 2.2.2.1. Phosphoric acid, 85 % (H3PO4, ρ20 = 1,71 g/ml).

              2. 2.2.2.2. Hydrogen peroxide solution, 9,1 g H2O2/litre (three volumes).

              3. 2.2.2.3. Indicator reagent:

              4. 2.2.2.4. Sodium hydroxide solution, NaOH, 0,01 M

            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. Calculation

              3. 2.2.3.3. Determination of total sulphur dioxide

                1. 2.2.3.3.1. For rectified concentrated musts, use the solution obtained by diluting...

                2. 2.2.3.3.2. Wines and musts

              4. 2.2.3.4. Expression of results

                1. 2.2.3.4.1. Calculation

                2. 2.2.3.4.2. Repeatability (r)

                3. 2.2.3.4.3. Reproducibility (R)

          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:

                1. Notes:

        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. Atomic absorption spectrophotometer equipped with an air-acetylene burner.

            2. 2.2.2. Sodium hollow cathode lamp.

          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. Atomic absorption spectrophotometer, equipped with an air-acetylene burner.

            2. 2.2.2. Potassium hollow cathode lamp.

          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. Atomic absorption spectrophotometer fitted with an air-acetylene burner.

          2. 3.2. Magnesium hollow cathode lamp.

        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. Atomic absorption spectrophotometer fitted with an air-acetylene burner.

          2. 3.2. Calcium hollow cathode lamp.

        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. Concentrated standard iron solution containing 1 g Fe(III) per litre.

            2. 2.1.2 Dilute standard iron solution containing 100 mg iron per litre.

          2. 2.2. Apparatus

            1. 2.2.1 Rotary evaporator with thermostatically controlled waterbath.

            2. 2.2.2. Atomic absorption spectrophotometer equipped with an air-acetylene burner.

            3. 2.2.3. Iron hollow cathode lamp.

          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. Platinum dish.

          2. 2.2. Atomic absorption spectrophotometer.

          3. 2.3. Copper hollow cathode lamp.

          4. 2.4. Gas supplies: air-acetylene or nitrous oxide/acetylene.

        3. 3. REAGENTS

          1. 3.1. Metallic copper.

          2. 3.2. Nitric acid, HNO3, concentrated 65 %, ρ20 = 1,38 g/ml.

          3. 3.3. Dilute nitric acid, 1:2 (v/v).

          4. 3.4. Solution containing copper at 1 g/l.

          5. 3.5. Solution containing copper at 100 mg/l.

        4. 4. PROCEDURE

          1. 4.1. Preparation of sample and determination of copper

          2. 4.2. Calibration

          3. 4.3. Measure the absorbence at 324,8 nm. Set the zero with doubly...

        5. 5. EXPRESSION OF RESULTS

          1. 5.1. Method of calculation

            1. Notes:

              1. (a) Select the solutions for establishing the calibration curve and the...

              2. (b) Proceed as follows when very low copper concentrations are expected...

      34. 32. CADMIUM

        1. 1. Principle

        2. 2. APPARATUS

          1. 2.1. Atomic absorption spectrophotometer equipped with a graphite oven, background correction...

          2. 2.2. Cadmium hollow cathode lamp.

          3. 2.3. 5 µl micropipettes with special tips for atomic absorption measurements.

        3. 3. REAGENTS

          1. 3.1. 85 % phosphoric acid (ρ20 = 1,71 g/ml).

          2. 3.2. Phosphoric acid solution obtained by diluting 8 ml of phosphoric acid...

          3. 3.3. A 0,02 M solution of di-sodium salt of ethylene diamine tetra-acetic...

          4. 3.4. pH 9 buffer solution: dissolve 5,4 g of ammonium chloride in...

          5. 3.5. Eriochrome black T: 1 % (w/w) solid solution in sodium chloride....

          6. 3.6. Cadmium sulphate (CdSO4·8H2O).

          7. 3.7. Cadmium reference solution at 1 g per litre.

        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. Platinum dish.

          2. 2.2. Waterbath, thermostatically controlled to 100 °C.

          3. 2.3. Furnace controlled to 500 to 525 °C.

          4. 2.4. Atomic absorption spectrophotometer.

          5. 2.5. Silver hollow cathode lamp.

          6. 2.6. Gas supplies: air, acetylene.

        3. 3. REAGENTS

          1. 3.1. Silver nitrate, AgNO3.

          2. 3.2. Nitric acid, HNO3, concentrated 65 %, ρ20 = 1,38 g/ml.

          3. 3.3. Dilute nitric acid, 1:10 (v/v).

          4. 3.4. Solution containing silver at 1 g/l.

          5. 3.5. Solution containing silver at 10 mg/l.

        4. 4. PROCEDURE

          1. 4.1. Preparation of sample

          2. 4.2. Calibration

          3. 4.3. Set the wavelength to 328,1 nm. Set zero using doubly distilled...

        5. 5. EXPRESSION OF RESULTS

          1. 5.1. Method of calculation

            1. Note:

      36. 34. ZINC

        1. 1. PRINCIPLE OF THE METHOD

        2. 2. REAGENTS

          1. 2.1. Standard solution containing 1 g of zinc per litre:

          2. 2.2. Dilute standard solution containing 100 mg of zinc per litre.

        3. 3. APPARATUS

          1. 3.1. Rotary evaporator with thermostatically controlled waterbath.

          2. 3.2. Atomic absorption spectrophotometer equipped with an air-acetylene burner.

          3. 3.3. Zinc hollow cathode lamp.

        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. Atomic absorption spectrophotometer equipped with a graphite oven, non-specific absorption...

          2. 2.2. Lead hollow cathode lamp.

          3. 2.3. 5 µl micropipettes with special tips for atomic absorption measurements.

        3. 3. REAGENTS

          1. 3.1. 85 % phosphoric acid (ρ20 = 1,71 g/ml).

          2. 3.2. Phosphoric acid solution obtained by diluting 8 ml of phosphoric acid...

          3. 3.3. Nitric acid (ρ20 = 1,38 g/ml).

          4. 3.4. Lead solution at 1 g per litre.

        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. Fluoride-ion-selective crystal membrane electrode.

          2. 2.2. Reference electrode (calomel or Ag/AgCl).

          3. 2.3. Millivoltmeter (pH meter with extended scale in millivolts), accurate to...

          4. 2.4. Magnetic stirrer with an insulating plate to protect the analysis...

          5. 2.5. Plastic beakers with a capacity of 30 or 50 ml, and...

          6. 2.6. Precision pipettes (pipettes graduated in microlitres or any other equivalent...

        3. 3. REAGENTS

          1. 3.1. Stock fluoride solution of 1 g/l.

          2. 3.2. Standard fluoride solutions of appropriate concentration are prepared by diluting...

          3. 3.3. Buffer solution, pH 5,5

        4. 4. PROCEDURE

          1. Preliminary comment:

          2. 4.1. Direct method

          3. 4.2. The known additions method

        5. 5. CALCULATIONS

      39. 37. CARBON DIOXIDE

        1. 1. PRINCIPLE OF METHODS

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

            1. 2.1.1. Apparatus

              1. 2.1.1.1. Magnetic stirrer.

              2. 2.1.1.2. pH meter.

            2. 2.1.2. Reagents

              1. 2.1.2.1. Sodium hydroxide solution, NaOH, 0,1 M.

              2. 2.1.2.2. Sulphuric acid solution, H2SO4, 0,05 M.

              3. 2.1.2.3. Carbonic anhydrase solution, 1 g/l.

            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. Magnetic stirrer.

              2. 2.2.1.2. pH meter.

            2. 2.2.2. Reagents

              1. 2.2.2.1. Sodium hydroxide, NaOH, 50 % (m/m).

              2. 2.2.2.2. Sulphuric acid solution, H2SO4, 0,05 M.

              3. 2.2.2.3. Carbonic anhydrase solution, 1 g/l.

            3. 2.2.3. Procedure

            4. 2.2.4. Expression of results

          3. 2.3. Expression of results

        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. 38. CYANIDE DERIVATIVES

        2. 1. PRINCIPLE

        3. 2. APPARATUS

          1. 2.1. Distillation apparatus

          2. 2.2. 500-ml round-bottomed flask with standardised ground joints

          3. 2.3. Water bath thermostatically controlled at 20 °C

          4. 2.4. Spectrophotometer allowing absorbance to be measured at wavelength of 590 nm...

          5. 2.5. Glass cells or single-use cells with optical paths of 20 mm...

        4. 3. REAGENTS

          1. 3.1. Phosphoric acid (H 3 PO 4 ) at 25 % (m/v)...

          2. 3.2. Chloramine-T solution (C 7 H 7 ClNNa O 2 S,...

          3. 3.3. Solution of 1,3-dimethyl-barbituric acid: dissolve 3,658 g 1,3-dimethyl-barbituric acid (C 6 H...

          4. 3.4. Potassium cyanide (KCN)

          5. 3.5. Potassium iodide (KI) solution at 10 % (m/v)

          6. 3.6. Silver nitrate solution (AgNO 3 ), 0,1 M

        5. 4. PROCEDURE

          1. 4.1. Distillation

          2. 4.2. Measurement

        6. 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

        7. 6. EXPRESSION OF RESULTS

          1. 6.1. Method of calculation

      41. 39. ALLYL ISOTHIOCYANATE

        1. 1. PRINCIPLE OF THE METHOD

        2. 2. REAGENTS

          1. 2.1. Ethanol, absolute.

          2. 2.2. Standard solution: solution of allyl isothiocyanate in absolute alcohol containing...

          3. 2.3. Freezing mixture consisting of ethanol and dry ice (temperature −60 °C)....

        3. 3. APPARATUS

          1. 3.1. Distillation apparatus as shown in the figure overleaf. A stream...

          2. 3.2. Heating mantle, thermostatically controlled.

          3. 3.3. Flowmeter.

          4. 3.4. Gas chromatograph fitted with a flame spectrophotometer detector equipped with...

          5. 3.5. Stainless steel chromatograph column of internal diameter 3 mm and length...

          6. 3.6. Microsyringe, 10µl.

        4. 4. PROCEDURE

      42. 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. Spectrophotometer enabling measurements to be made between 300 and 700 nm....

              2. 1.3.1.2. Glass cells in pairs, with optical paths, b, equal to...

            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. The relative luminosity is given by the value of Y...

              2. 1.3.4.2. The chromaticity is expressed by the dominant wavelength and the...

              3. 1.3.4.3. Results

          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

              1. Note:

            2. Example:

        2. 2. RECTIFIED CONCENTRATED MUSTS

          1. 2.1. Principle of the method

          2. 2.2. Apparatus

            1. 2.2.1. Spectrophotometer enabling measurements to be made between 300 and 700 nm....

            2. 2.2.2. Glass cells with optical paths of 1 cm.

            3. 2.2.3. Membrane filter of pore diameter 0,45 µm.

          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

      43. 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. Anhydrous sodium carbonate, Na2CO3, made up into a 20 % m/v...

        4. 4. APPARATUS

          1. 4.1. 100 ml volumetric flasks.

          2. 4.2. Spectrophotometer capable of operating at 750 nm.

        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

      44. 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. Glass column of internal diameter 10 to 11 mm and length...

            2. 2.2. pH meter with a scale graduated at least in 0,1 pH...

            3. 2.3. Electrodes:

          3. 3. REAGENTS

            1. 3.1. Strongly acid cation exchange resin in H+ form pre-swollen by...

            2. 3.2. Sodium hydroxide solution, 0,1 M.

            3. 3.3. Paper pH indicator.

          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. Calculations

        2. (b) CONDUCTIVITY

          1. 1. PRINCIPLE OF THE METHOD

          2. 2. APPARATUS

            1. 2.1. Conductivity meter enabling measurements of conductivity to be made over...

            2. 2.2. Waterbath for bringing the temperature of samples to be analysed...

          3. 3. REAGENTS

            1. 3.1. Demineralized water with specific conductivity below 2 µS cm−1 at 20 °C....

            2. 3.2. Reference solution of potassium chloride.

          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. Spectrophotometer for making measurements between 300 and 700 nm.

              2. 2.1.2. Glass cells with optical paths of 1 cm.

            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. Membrane filtration apparatus, pore diameter 0,45 µm.

            2. 3.2. Reagents

              1. 3.2.1. Doubly distilled water.

              2. 3.2.2. Methanol, CH3OH, distilled or HPLC quality.

              3. 3.2.3. Acetic acid CH3COOH, (ρ = 1,05 g/ml).

              4. 3.2.4. Mobile phase: water-methanol (3.2.2)-acetic acid (3.2.3) previously filtered through a...

              5. 3.2.5. Reference solution of hydroxymethylfurfural, 25 mg/l (v/v).

            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. Dilute ammonia. Take 14 g of ammonia, NH3 (ρ20 = 0,931 to...

              4. 2.1.4. pH 3,5 buffer solution.

              5. 2.1.5. Thioacetamide solution C2H5 SN, 4 % (m/v).

              6. 2.1.6. Glycerol solution, C3H8O3, 85 % (m/v), ( n 20 °C D = 1,449...

              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. Atomic absorption spectrophotometer equipped with an air-acetylene burner.

              2. 3.1.2. Lead hollow cathode lamp.

            2. 3.2. Reagents

              1. 3.2.1. Dilute acetic acid.

              2. 3.2.2. Solution of ammonium pyrrolidinedithiocarbamate, C5H12N2S2, 1 % (m/v).

              3. 3.2.3. Methylisobutylketone, (CH3)2CHCH2COCH3.

              4. 3.2.4. Solution containing 0,010 g/l of lead.

            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. Use the distillation apparatus described in the chapter ‘Alcoholic strength...

          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. Internal standard: xylitol (aqueous solution of about 10 g/l to which...

            2. 2.2. Bis(trimethylsilyl)trifluoroacetamide — BSTFA — (C8H18F3NOSi2)

            3. 2.3. Trimethylchlorosilane (C3H9ClSi)

            4. 2.4. Pyridine p.A. (C5H5N)

            5. 2.5 Meso-inositol (C6H12O6)

          3. 3. APPARATUS

            1. 3.1. Gas chromatograph equipped with:

            2. 3.2. Capillary column (e.g. in fused silica, coated with OV 1,...

            3. 3.3. Integrator.

            4. 3.4. Microsyringe, 10 µl.

            5. 3.5. Micropipettes, 50, 100 and 200 µl.

            6. 3.6. 2 ml flask with Teflon stopper.

            7. 3.7. Oven.

          4. 4. METHOD OF OPERATION

          5. 5. CALCULATION OF RESULTS

            1. 5.1. A solution is prepared containing:

          6. 6. EXPRESSION OF RESULTS

            1. 6.1. Meso-inositol and scyllo-inositol are expressed in milligrams per kilogram of...

      45. 43. DETERMINATION OF THE ISOTOPIC RATIO 18 O/ 16 O OF...

        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 CO 2

              4. Transfer of the CO 2 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

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

        2. A. Principle

        3. B. Apparatus and chromatographic conditions (example)

        4. C. Reagents

        5. D. Preparation of the test sample

        6. E. Extraction

        7. F. GC/MS analysis

        8. G. Collaborative analysis

      47. 45. DETERMINATION BY ISOTOPE MASS SPECTROMETRY OF THE 13 C/ 12...

        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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