2009R0606 — EN — 01.08.2009 — 000.001

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This document is meant purely as a documentation tool and the institutions do not assume any liability for its contents

►B	COMMISSION REGULATION (EC) No 606/2009 of 10 July 2009 laying down certain detailed rules for implementing Council Regulation (EC) No 479/2008 as regards the categories of grapevine products, oenological practices and the applicable restrictions (OJ L 193, 24.7.2009, p.1)

Amended by:

		Official Journal
		No	page	date
►M1	COMMISSION REGULATION (EC) No 1166/2009 of 30 November 2009	L 314	27	1.12.2009

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▼B

COMMISSION REGULATION (EC) No 606/2009

of 10 July 2009

laying down certain detailed rules for implementing Council Regulation (EC) No 479/2008 as regards the categories of grapevine products, oenological practices and the applicable restrictions

Article 1

Purpose

This Regulation lays down detailed rules for the application of Title III, Chapters I and II of Regulation (EC) No 479/2008.

Article 2

Wine-growing areas where wines may have a maximum total alcoholic strength of 20 % vol.

The wine-growing areas referred to in the first indent of point (c) of the second subparagraph of paragraph 1 of Annex IV to Regulation (EC) No 479/2008 shall be zones C I, C II and C III referred to in Annex IX to that Regulation and the areas of zone B in which white wines with the following protected geographical indications may be produced: ‘Vin de pays de Franche-Comté’ and ‘Vin de pays du Val de Loire’.

Article 3

Authorised oenological practices and restrictions

1.  The authorised oenological practices and restrictions applicable to the production and conservation of products covered by Regulation (EC) No 479/2008, referred to in Article 29(1) thereof, are laid down in Annex I hereto.

2.  The authorised oenological practices and the conditions for and the limits on their use are set out in Annex I A.

3.  The maximum sulphur dioxide contents of wines are given in Annex I B.

4.  The maximum volatile acid contents are given in Annex I C.

5.  The rules on sweetening are laid down in Annex I D.

Article 4

Experimental use of new oenological practices

1.  For experimental purposes as referred to in Article 29(2) of Regulation (EC) No 479/2008, each Member State may authorise the use of certain oenological practices or processes not provided for in that Regulation or in this Regulation, for a maximum of three years, on condition that:

‘Experiment’ shall mean an operation or operations carried out in the context of a well-defined research project with a single experimental protocol.

2.  The products obtained by the experimental use of such practices and processes may be placed on the market of a Member State other than the Member State concerned provided the Member State authorising the experiment gives prior notification to the competent authorities of the Member State of destination of the terms of the authorisation and the quantities involved.

3.  During the three months following the end of the period referred to in paragraph 1, the Member State concerned shall forward to the Commission a report on the authorised experiment and the results thereof. The Commission shall notify the other Member States of those results.

4.  Depending on these results, the Member State concerned may apply to the Commission for authorisation to continue the experiment, possibly with a larger quantity than in the original experiment, for a further maximum period of three years. The Member State shall submit an appropriate dossier in support of its application. The Commission, in accordance with the procedure referred to in Article 113(2) of Regulation (EC) No 479/2008, shall decide on the application to continue the experiment.

Article 5

Oenological practices applicable to categories of sparkling wines

The authorised oenological practices and restrictions, including enrichment, acidification and de-acidification, concerning sparkling wines, quality sparkling wines and quality aromatic sparkling wines, referred to in point (b) of the second paragraph of Article 32 of Regulation (EC) No 479/2008 are listed in Annex II hereto, without prejudice to the oenological practices and restrictions of general application laid down in Regulation (EC) No 479/2008 and in Annex I hereto.

Article 6

Oenological practices applicable to liqueur wines

The authorised oenological practices and restrictions concerning liqueur wines referred to in point (c) of the second paragraph of Article 32 of Regulation (EC) No 479/2008 are listed in Annex III hereto, without prejudice to the oenological practices and restrictions of general application laid down in Regulation (EC) No 479/2008 and in Annex I hereto.

Article 7

Definition of coupage

1.  Within the meaning of point (d) of the second paragraph of Article 32 of Regulation (EC) No 479/2008, ‘coupage’ shall mean the mixing of wines or musts of different origins, different vine varieties, different harvest years or different categories of wine or of must.

2.  The following shall be regarded as different categories of wine or must:

For the purposes of this paragraph, rosé wine shall be regarded as red wine.

3.  The following processes shall not be regarded as coupage:

Article 8

General rules on blending and coupage

1.  A wine may be obtained by blending or coupage only where the constituents of that blending or coupage possess the required characteristics for obtaining wine and comply with Regulation (EC) No 479/2008 and this Regulation.

Coupage of a non-PDO/PGI white wine with a non-PDO/PGI red wine cannot produce a rosé wine.

However, the second subparagraph does not exclude coupage of the type referred to therein where the final product is intended for the preparation of a cuvée as defined in Annex I to Regulation (EC) No 479/2008 or intended for the production of semi-sparkling wines.

2.  Coupage of a grape must or a wine which has undergone the oenological practice referred to in paragraph 14 of Annex I A to this Regulation with a grape must or a wine which has not undergone that practice shall be prohibited.

Article 9

The purity and identification specifications of substances used in oenological practices

1.  Where they are not laid down by Commission Directive 2008/84/EC ( 5 ), the purity and identification specifications of substances used in the oenological practices referred to in point (e) of the second paragraph of Article 32 of Regulation (EC) No 479/2008 shall be those laid down and published in the International Oenological Codex of the International Organisation of Vine and Wine.

Where necessary, those purity criteria shall be supplemented by the specific requirements provided for in Annex I A hereto.

2.  The enzymes and enzymatic preparations used in the authorised oenological practices and processes listed in Annex I A shall meet the requirements of Regulation (EC) No 1332/2008 of the European Parliament and of the Council of 16 December 2008 on food enzymes ( 6 ).

Article 10

Conditions governing the holding, circulation and use of products not complying with Chapter II of Title III of Regulation (EC) No 479/2008 or this Regulation

1.  Products not complying with Chapter II of Title III of Regulation (EC) No 479/2008 or this Regulation shall be destroyed. However, Member States may authorise the use of certain products, the characteristics of which they shall determine, by distilleries or vinegar factories or for industrial purposes.

2.  Such products may not be held without legitimate cause by producers or traders and they may be moved only to distilleries, vinegar factories, or establishments using them for industrial purposes or products or elimination plants.

3.  Member States may have denaturing agents or indicators added to wines as referred to in paragraph 1 in order to make them more easily identifiable. Where justified, they may also prohibit the uses provided for in paragraph 1 and have the products disposed of.

4.  Wine produced before 1 August 2009 may be offered or supplied for direct human consumption provided that it complies with the Community or national rules in force prior to that date.

Article 11

General rules applicable to the enrichment, acidification and deacidification of products other than wine

The processes referred to in paragraph 1 of point D of Annex V to Regulation (EC) No 479/2008 must be carried out in a single operation. However, Member States may permit some of these processes to be carried out in more than one operation where this improves the vinification of the products concerned. In such cases, the limits laid down in Annex V to Regulation (EC) No 479/2008 shall apply to the whole operation concerned.

Article 12

Administrative rules applicable to enrichment

1.  Notifications as referred to in paragraph 4 of point D of Annex V to Regulation (EC) No 479/2008 relating to operations to increase alcoholic strength shall be made by the natural or legal persons carrying out the operations concerned and in compliance with suitable time limits and control conditions set by the competent authority of the Member State on whose territory the operation takes place.

2.  Notifications as referred to in paragraph 1 shall be made in writing and shall include the following information:

3.  Member States may allow prior notifications covering several operations or a specified period to be sent to the competent authorities. Such notifications shall be accepted only if the person making the notification keeps a written record of each enrichment operation as provided for in paragraph 6 and of the information required by paragraph 2.

4.  Where the person concerned is prevented by reasons of force majeure from carrying out the notified operation in due time, Member States shall specify the conditions under which that person is to submit a new notification to the competent authority so that the necessary checks can be carried out.

5.  The notification referred to in paragraph 1 shall not be required in Member States in which the competent inspection authorities carry out systematic analytical checks of all batches of products turned into wine.

6.  The particulars relating to operations to increase alcoholic strength shall be entered in the registers referred to in Article 112(2) of Regulation (EC) No 479/2008 immediately after the operation is completed.

In cases where prior notifications covering several operations do not indicate the date and time when the operations are to commence, an entry must also be made in those registers before each operation commences.

Article 13

Administrative rules applicable to acidification and deacidification

1.  In the case of acidification and deacidification, operators shall make notifications as referred to in paragraph 4 of point D of Annex V to Regulation (EC) No 479/2008 not later than the second day following the first operation carried out in any wine year. Such notifications shall be valid for all operations in that wine year.

2.  Notifications as referred to in paragraph 1 shall be made in writing and shall include the following information:

3.  The particulars relating to each acidification and deacidification operation shall be entered in the registers referred to in Article 112(2) of Regulation (EC) No 479/2008.

Article 14

Pouring of wine or grape must to lees or grape marc or pressed ‘aszú’/‘výber’ pulp

The pouring of wine or grape must to lees or grape marc or pressed ‘aszú’/‘výber’ pulp, provided for in paragraph 2 of point D of Annex VI to Regulation (EC) No 479/2008, shall be carried out as follows, in accordance with the national provisions in force on 1 May 2004:

The products concerned must be from the same harvest year.

Article 15

Applicable Community analysis methods

1.  The analysis methods referred to in the second paragraph of Article 31 of Regulation (EC) No 479/2008 applicable for the verification of certain wine products and certain limits laid down at Community level are set out in Annex IV hereto.

2.  The Commission shall publish in the C Series of the Official Journal of the European Union the list and description of the analysis methods referred to the first paragraph of Article 31 of Regulation (EC) No 479/2008 and described in the Compendium of International Methods of Analysis of Wines and Musts of the International Organisation of Vine and Wine and applicable for verification of the limits and requirements laid down by Community rules for the production of wine products.

Article 16

Repeal

Regulations (EEC) No 2676/90 and (EC) No 423/2008 are repealed.

References to the repealed Regulations and to Regulation (EC) No 1493/1999 shall be construed as references to this Regulation and shall be read in accordance with the correlation table in Annex V.

Article 17

This Regulation shall enter into force on the seventh day following its publication in the Official Journal of the European Union.

It shall apply from 1 August 2009.

This Regulation shall be binding in its entirety and directly applicable in all Member States.

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ANNEX I A

AUTHORISED OENOLOGICAL PRACTICES AND PROCESSES.

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Appendix 1

Requirements for beta-glucanase

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Appendix 2

L(+) tartaric acid

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Appendix 3

Aleppo pine resin

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Appendix 4

Ion exchange resins

The ion exchange resins which may be used accordance with paragraph 20 of Annex I A are styrene and divinylbenzene copolymers containing sulphonic acid or ammonium groups. They must comply with the requirements laid down in Regulation (EC) No 1935/2004 of the European Parliament and of the Council ( 7 ) and Community and national provisions adopted in implementation thereof. In addition, when tested by the analysis method laid down in paragraph 2, they must not lose more than 1 mg/l of organic matter into any of the solvents listed. They must be regenerated with substances permitted for use in the preparation of foodstuffs.

These resins may be used only under the supervision of an oenologist or technician and in installations approved by the authorities of the Member States on whose territory they are used. Such authorities shall lay down the duties and responsibility incumbent on approved oenologists and technicians.

Analysis method for determining the loss of organic matter from ion exchange resins:

1.   SCOPE AND AREA OF APPLICATION

The method determines the loss of organic matter from ion exchange resins.

2.   DEFINITION

The loss of organic matter from ion exchange resins. The loss of organic matter is determined by the method specified.

3.   PRINCIPLE

Extracting solvents are passed through prepared resins and the weight of organic matter extracted is determined gravimetrically.

4.   REAGENTS

All reagents shall be of analytical quality.

Extracting solvents.

4.1.	Distilled water or deionised water of equivalent purity.

4.2.	Ethanol, 15 % v/v. Prepare by mixing 15 parts of absolute ethanol with 85 parts of water (paragraph 4.1).

4.3.	Acetic acid, 5 % m/m. Prepare by mixing 5 parts of glacial acetic acid with 95 parts of water (paragraph 4.1).

5.   APPARATUS

5.1.	Ion exchange chromatography columns.

5.2.	Measuring cylinders, capacity 2 l.

5.3.	Evaporating dishes capable of withstanding a muffle furnace at 850 °C.

5.4.	Drying oven, thermostatically controlled at 105 ± 2 °C.

5.5.	Muffle furnace, thermostatically controlled at 850 ± 25 °C.

5.6.	Analytical balance, accurate to 0.1 mg.

5.7.	Evaporator, hot plate or infra-red evaporator.

6.   PROCEDURE

6.1.	Add to each of three separate ion exchange chromatography columns (paragraph 5.1) 50 ml of the ion exchange resin to be tested, washed and treated in accordance with the manufacturer’s directions for preparing resins for use with food.

6.2.

For the anionic resins, pass the three extracting solvents (paragraphs 4.1, 4.2 and 4.3) separately through the prepared columns (paragraph 6.1) at a flow rate of 350 to 450 ml/h. Discard the first litre of eluate in each case and collect the next two litres in measuring cylinders (paragraph 5.2). For the cationic resins, pass only solvents referred to in paragraphs 4.1 and 4.2 through the columns prepared for this purpose.

6.3.	Evaporate the three eluates over a hotplate or with an infrared evaporator (paragraph 5.7) in separate evaporating dishes (paragraph 5.3) which have been previously cleaned and weighed (m0). Place the dishes in an oven (paragraph 5.4) and dry to constant weight (m1).

6.4.	After recording the constant weight (paragraph 6.3), place the evaporating dish in the muffle furnace (paragraph 5.5) and ash to constant weight (m2).

6.5.

Calculate the organic matter extracted (paragraph 7.1). If the result is greater than 1 mg/l, carry out a blank test on the reagents and recalculate the weight of organic matter extracted. The blank test shall be carried out by repeating the operations referred to in paragraphs 6.3 and 6.4 but using two litres of the extracting solvent, to give weights m3 and m4 in paragraphs 6.3 and 6.4 respectively.

7.   EXPRESSION OF THE RESULTS

7.1.

Formula and calculation of results The organic matter extracted from ion exchange resins, in mg/l, is given by: 500 (m1 – m2) where m1 and m2 are expressed in grams. The corrected weight (mg/l) of the organic matter extracted from ion exchange resins is given by: 500 (m1 – m2 – m3 + m4) where m1, m2, m3 and m4 are expressed in grams.

7.2.	The difference in the results between two parallel determinations carried out on the same sample must not exceed 0,2 mg/l.

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Appendix 5

Potassium ferrocyanide

Calcium phytate

DL tartaric acid

Potassium ferrocyanide or calcium phytate, the use of which is provided for in paragraph 26 of Annex I A, or DL tartaric acid, the use of which is provided for in paragraph 29 of Annex I A, may be used only under the supervision of an oenologist or technician officially approved by the authorities of the Member State in whose territory the process is carried out, the extent of whose responsibility shall be fixed, if necessary, by the Member State concerned.

After treatment with potassium ferrocyanide or calcium phytate, the wine must contain traces of iron.

Supervision of the use of the product referred to in the first paragraph shall be governed by the provisions adopted by the Member States.

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Appendix 6

Requirements for dimethyldicarbonate

AREA OF APPLICATION

Dimethyldicarbonate may be added to wine for the following purpose: microbiological stabilisation of bottled wine containing fermentable sugar.

REQUIREMENTS

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Appendix 7

Requirements for electrodialysis treatment

The purpose is to obtain tartaric stability of the wine with regard to potassium hydrogen tartrate and calcium tartrate (and other calcium salts) by extraction of ions in supersaturation in the wine under the action of an electrical field and using membranes that are either anion-permeable or cation-permeable.

1.   MEMBRANE REQUIREMENTS

1.1.	The membranes are to be arranged alternately in a ‘filter-press’ type system or any other appropriate system separating the treatment (wine) and concentration (waste water) compartments.

1.2.	The cation-permeable membranes must be designed to extract cations only, in particular K+, Ca++.

1.3.	The anion-permeable membranes must be designed to extract anions only, in particular tartrate anions.

1.4.

The membranes must not excessively modify the physico-chemical composition and sensory characteristics of the wine. They must meet the following requirements: — they must be manufactured according to good manufacturing practice from substances authorised for the manufacture of plastic materials intended to come into contact with foodstuffs as listed in Annex II to Commission Directive 2002/72/EC ( 8 ), — the user of the electrodialysis equipment must show that the membranes used meet the above requirements and that any replacements have been carried out by specialised personnel, — they must not release any substance in quantities endangering human health or affecting the taste or smell of foodstuffs and must meet the criteria laid down in Directive 2002/72/EC, — their use must not trigger interactions between their constituents and the wine liable to result in the formation of new compounds that may be toxic in the treated product. The stability of fresh electrodialysis membranes is to be determined using a simulant reproducing the physico-chemical composition of the wine for investigation of possible migration of certain substances from them. The experimental method recommended is as follows: The simulant is a water-alcohol solution buffered to the pH and conductivity of the wine. Its composition is as follows: — absolute ethanol: 11 l, — potassium hydrogen tartrate: 380 g, — potassium chloride: 60 g, — concentrated sulphuric acid: 5 ml, — distilled water: to make up 100 litres, This solution is used for closed circuit migration tests on an electrodialysis stack under tension (1 volt/cell), on the basis of 50 l/m2 of anionic and cationic membranes, until 50 % demineralisation of the solution. The effluent circuit is initiated by a 5 g/l potassium chloride solution. Migrating substances are tested for in both the simulant and the effluent. Organic molecules entering into the membrane composition that are liable to migrate into the treated solution will be determined. A specific determination will be carried out for each of these constituents by an approved laboratory. ►M1  The content in the simulant of all the determined compounds must be less than 50 μg/l. ◄ The general rules on controls of materials in contact with foodstuffs must be applied to these membranes.

2.   MEMBRANE UTILISATION REQUIREMENTS

The membrane pair is formulated so that the following conditions are met:

The treatment is to be recorded in the register referred to in Article 112(2) of Regulation (EC) No 479/2008.

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Appendix 8

Requirements for urease

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Appendix 9

Requirements for pieces of oak wood

PURPOSE, ORIGIN AND AREA OF APPLICATION

Pieces of oak wood are used in winemaking and ageing, including in the fermentation of fresh grapes and grape must, to pass on certain characteristics of oak wood to wine.

The pieces of oak wood must come exclusively from the Quercus genus.

They may be left in their natural state, or heated to a low, medium or high temperature, but they may not have undergone combustion, including surface combustion, nor be carbonaceous or friable to the touch. They may not have undergone any chemical, enzymatic or physical processes other than heating. No product may be added for the purpose of increasing their natural flavour or the amount of their extractible phenolic compounds.

LABELLING

The label must mention the origin of the botanical species of oak and the intensity of any heating, the storage conditions and safety precautions.

DIMENSIONS

The dimensions of the particles of wood must be such that at least 95 % in weight are retained by a 2 mm mesh filter (9 mesh).

PURITY

The pieces of oak wood may not release any substances in concentrations which may be harmful to health.

This treatment is to be recorded in the register referred to in Article 112(2) of Regulation (EC) No 479/2008.

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Appendix 10

Requirements for the partial dealcoholisation of wine

The aim of this treatment is to produce a partially dealcoholised wine, by eliminating some of the alcohol (ethanol) in it using physical separation techniques.

Requirements

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Appendix 11

Requirements for treatment with PVI/PVP copolymers

The purpose of this treatment is to reduce excessively high concentrations of metals and to prevent defects caused by this excessively high content, such as ferric casse, through the addition of copolymers that adsorb these metals.

Requirements

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Appendix 12

Requirements for treatment with cation exchangers to ensure the tartaric stabilisation of the wine

The purpose is to obtain tartaric stability of the wine with regard to potassium hydrogen tartrate and calcium tartrate (and other calcium salts).

Requirements

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ANNEX I B

THE MAXIMUM SULPHUR DIOXIDE CONTENT OF WINES

A.   THE SULPHUR DIOXIDE CONTENT OF WINES

B.   THE SULPHUR DIOXIDE CONTENT OF LIQUEUR WINES

The total sulphur dioxide content of liqueur wines, on their release to the market for direct human consumption, may not exceed:

150 mg/l where the sugar content is less than 5 g/l;

200 mg/l where the sugar content is not less than 5 g/l.

C.   THE SULPHUR DIOXIDE CONTENT OF SPARKLING WINES

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Appendix 1

Increase in the maximum total sulphur dioxide content where the climate conditions make this necessary

(Annex I B to this Regulation)

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ANNEX I C

THE MAXIMUM VOLATILE ACID CONTENT OF WINES

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ANNEX I D

LIMITS AND CONDITIONS FOR THE SWEETENING OF WINES

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ANNEX II

AUTHORISED OENOLOGICAL PRACTICES AND RESTRICTIONS APPLICABLE TO SPARKLING WINES, QUALITY SPARKLING WINES AND QUALITY AROMATIC SPARKLING WINES

A.   Sparkling wine

B.   Quality sparkling wine

C.   Sparkling wines and quality sparkling wines with a protected designation of origin

▼M1

▼B

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Appendix 1

List of vine varieties grapes of which may be used to constitute the cuvée for preparing quality aromatic sparkling wines and quality sparkling wines with a protected designation of origin

▼M1

▼B

▼M1 —————

▼B

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ANNEX III

AUTHORISED OENOLOGICAL PRACTICES AND RESTRICTIONS APPLICABLE TO LIQUEUR WINES AND LIQUEUR WINES WITH A PROTECTED DESIGNATION OF ORIGIN OR PROTECTED GEOGRAPHICAL INDICATION

A.   Liqueur wines

B.   Liqueur wines with a protected designation of origin (provisions other than those laid down in point A of this Annex and concerning specifically liqueur wines with a protected designation of origin)

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Appendix 1

The list of liqueur wines with a protected designation of origin whose production involves special rules

A.   LIST OF LIQUEUR WINES WITH A PROTECTED DESIGNATION OF ORIGIN WHOSE PRODUCTION INVOLVES THE USE OF GRAPE MUST OR A MIXTURE THEREOF WITH WINE

(Paragraph B 1 of this Annex)

GREECE

Σάμος (Samos), Μοσχάτος Πατρών (Patras Muscatel), Μοσχάτος Ρίου Πατρών (Rio Patron Muscatel), Μοσχάτος Κεφαλληνίας (Kefallonia Muscatel), Μοσχάτος Ρόδου (Rhodes Muscatel), Μοσχάτος Λήμνου (Lemnos Muscatel), Σητεία (Sitia), Νεμέα (Nemea), Σαντορίνη (Santorini), Δαφνές (Dafnes), Μαυροδάφνη Κεφαλληνίας (Mavrodafne of Kefallonia), Μαυροδάφνη Πατρών (Mavrodafne of Patras)

SPAIN

ITALY

Cannonau di Sardegna, Giró di Cagliari, Malvasia di Bosa, Malvasia di Cagliari, Marsala, Monica di Cagliari, Moscato di Cagliari, Moscato di Sorso-Sennori, Moscato di Trani, Masco di Cagliari, Oltrepó Pavese Moscato, San Martino della Battaglia, Trentino, Vesuvio Lacrima Christi.

B.   LIST OF LIQUEUR WINES WITH A PROTECTED DESIGNATION OF ORIGIN WHOSE PRODUCTION INVOLVES THE ADDITION OF THE PRODUCTS REFERRED TO IN PARAGRAPH 3(f) OF ANNEX IV TO REGULATION (EC) No 479/2008

(Paragraph 2 of point B of this Annex)

1.   List of liqueur wines with a protected designation of origin whose production involves the addition of wine alcohol or dried-grape alcohol with an actual alcoholic strength of not less than 95 % vol. and not more than 96 % vol.

(First indent of paragraph 3(f)(ii) of Annex IV to Regulation (EC) No 479/2008)

GREECE

Σάμος (Samos), Μοσχάτος Πατρών (Patras Muscatel), Μοσχάτος Ρίου Πατρών (Rio Patron Muscatel), Μοσχάτος Κεφαλληνίας (Kefallonia Muscatel), Μοσχάτος Ρόδου (Rhodes Muscatel), Μοσχάτος Λήμνου (Lemnos Muscatel), Σητεία (Sitia), Σαντορίνη (Santorini), Δαφνές (Dafnes), Μαυροδάφνη Πατρών (Mavrodafne of Patras), Μαυροδάφνη Κεφαλληνίας (Mavrodafne of Kefallonia).

SPAIN

Condado de Huelva, Jerez-Xérès-Sherry, Manzanilla-Sanlúcar de Barrameda, Málaga, Montilla-Moriles, Rueda, Terra Alta.

CYPRUS

Κουμανδαρία (Commandaria).

2.   List of liqueur wines with a protected designation of origin whose production involves the addition of spirits distilled from wine or grape marc with an actual alcoholic strength of not less than 52 % vol. and not more than 86 % vol.

(Second indent of paragraph 3(f)(ii) of Annex IV to Regulation (EC) No 479/2008)

GREECE

Μαυροδάφνη Πατρών (Mavrodafne of Patras), Μαυροδάφνη Κεφαλληνίας (Mavrodafne of Kefallonia), Σητεία (Sitia), Σαντορίνη (Santorini), Δαφνές (Dafnes), Νεμέα (Nemea).

FRANCE

Pineau des Charentes or Pineau charentais, Floc de Gascogne, Macvin du Jura.

CYPRUS

Κουμανδαρία (Commandaria).

3.   List of liqueur wines with a protected designation of origin whose production involves the addition of spirits distilled from dried grapes with an alcoholic strength of not less than 52 % vol. but less than 94,5 % vol.

(Third indent of paragraph 3(f)(ii) of Annex IV to Regulation (EC) No 479/2008)

GREECE

Μαυροδάφνη Πατρών (Mavrodafne of Patras), Μαυροδάφνη Κεφαλληνίας (Mavrodafne of Kefallonia).

4.   List of liqueur wines with a protected designation of origin whose production involves the addition of partially fermented grape must obtained from raisined grapes

(First indent of paragraph 3(f)(iii) of Annex IV to Regulation (EC) No 479/2008)

SPAIN

ITALY

Aleatico di Gradoli, Giró di Cagliari, Malvasia delle Lipari, Malvasia di Cagliari, Moscato passito di Pantelleria

CYPRUS

Κουμανδαρία (Commandaria).

5.   List of liqueur wines with a protected designation of origin whose production involves the addition of concentrated grape must obtained by the action of direct heat, complying, with the exception of this operation, with the definition of concentrated grape must.

(Second indent of paragraph 3(f)(iii) of Annex IV to Regulation (EC) No 479/2008)

SPAIN

ITALY

Marsala

6.   List of liqueur wines with a protected designation of origin whose production involves the addition of concentrated grape must

(Third indent of paragraph 3(f)(iii) of Annex IV to Regulation (EC) No 479/2008)

SPAIN

ITALY

Oltrepó Pavese Moscato, Marsala, Moscato di Trani.

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Appendix 2

A.   Lists referred to in paragraph 5(a) of Annex III B

1.   List of liqueur wines with a protected designation of origin produced from grape must with a natural alcoholic strength by volume of not less than 10 % vol. obtained by the addition of spirit obtained from wine or grape marc with a registered designation of origin, possibly from the same holding.

FRANCE

Pineau des Charentes or Pineau charentais, Floc de Gascogne, Macvin du Jura.

2.   List of liqueur wines with a protected designation of origin produced from fermenting grape must with an initial natural alcoholic strength by volume of not less than 11 % vol. obtained by the addition of neutral alcohol or of a distillate of wine with a an actual alcoholic strength by volume of not less than 70 % vol., or of spirit of vinous origin.

PORTUGAL

ITALY

3.   List of liqueur wines with a protected designation of origin produced from wine with an initial natural alcoholic strength by volume of not less than 10,5 % vol.

SPAIN

4.   List of liqueur wines with a protected designation of origin obtained from fermenting grape must with an initial natural alcoholic strength by volume of not less than 9 % vol.

PORTUGAL

Madeira.

B.   List referred to in paragraph 5(b) of Annex III B

List of liqueur wines with a protected designation of origin with a total alcoholic strength by volume of less than 17,5 % vol. but not less than 15 % vol., where national laws applicable thereto before 1 January 1985 expressly so provided

(Paragraph 3(b) of Annex IV to Regulation (EC) No 479/2008)

SPAIN

ITALY

Trentino

PORTUGAL

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Appendix 3

List of varieties that may be used to produce liqueur wines with a protected designation of origin that bear the specific, traditional terms ‘vino dulce natural’, ‘vino dolce naturale’, ‘vinho doce natural’ and ‘οινος γλυκυς φυσικος’

Muscats — Grenache — Garnacha Blanca — Garnacha Peluda — Listán Blanco — Listán Negro-Negramoll — Maccabéo — Malvoisies — Mavrodaphne — Assirtiko — Liatiko — Garnacha tintorera — Monastrell — Palomino — Pedro Ximénez — Albarola — Aleatico — Bosco — Cannonau — Corinto nero — Giró — Monica — Nasco — Primitivo — Vermentino — Zibibbo.

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ANNEX IV

SPECIAL COMMUNITY ANALYSIS METHODS

A.   ALLYL ISOTHIOCYANATE

1.   Principle of the method

Any allyl isothiocyanate present in the wine is collected by distillation and identified by gas chromatography.

2.   Reagents

2.1.	Ethanol, absolute.

2.2.	Standard solution: solution of allyl isothiocyanate in absolute alcohol containing 15 mg of allyl isothiocyanate per litre.

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

3.   Apparatus

3.1.	Distillation apparatus as shown in the figure. A stream of nitrogen is passed continuously through the apparatus.

3.2.	Heating mantle, thermostatically controlled.

3.3.	Flowmeter.

3.4.	Gas chromatograph fitted with a flame spectrophotometer detector equipped with a selective filter for sulphur compounds (wavelength = 394 nm) or any other suitable detector.

3.5.	Stainless steel chromatograph column of internal diameter 3 mm and length 3 m filled with Carbowax 20M at 10 % on Chromosorb WHP, 80 to 100 mesh.

3.6.	Microsyringe, 10μl.

4.   Procedure

Put two litres of wine into the distillation flask, introduce a few millilitres of ethanol (paragraph 2.1) into the two collecting tubes so that the porous parts of the gas dispersion rods are completely immersed. Cool the two tubes externally with the freezing mixture. Connect the flask to the collecting tubes and begin to flush the apparatus with nitrogen at a rate of three litres per hour. Heat the wine to 80 °C with the heating mantle, distil and collect 45 to 50 ml of the distillate.

Stabilize the chromatograph. It is recommended that the following conditions are used:

With the microsyringe, introduce a volume of the standard solution such that the peak corresponding to the allyl isothiocyanate can easily be identified on the gas chromatogram.

Similarly introduce an aliquot of the distillate into the chromatograph. Check that the retention time of the peak obtained corresponds with that of the peak of allyl isothiocyanate.

Under the conditions described above, compounds naturally present in the wine will not produce interfering peaks on the chromatogram of the sample solution.

Apparatus for distillation under a current of nitrogen

B.   SPECIAL ANALYSIS METHODS FOR RECTIFIED CONCENTRATED GRAPE MUST

(a)   Total cations

1.   Principle

The test sample is treated by a strongly acid cation exchanger. The cations are exchanged with H+. Total cations are expressed by the difference between the total acidity of the effluent and that of the test sample.

2.   Apparatus

2.1.	Glass column of internal diameter 10 to 11 mm and length approximately 300 mm, fitted with a drain tap.

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

2.3.	Electrodes: — glass electrode, kept in distilled water, — calomel/saturated potassium chloride reference electrode, kept in a saturated solution of potassium chloride, or — a combined electrode, kept in distilled water,

3.   Reagents

3.1.	Strongly acid cation exchange resin in H + form pre-swollen by soaking in water overnight.

3.2.	Sodium hydroxide solution, 0,1 M.

3.3.	Paper pH indicator.

4.   Procedure

4.1.   Preparation of sample

Use the solution obtained by diluting the rectified concentrated must to 40 % (m/v): introduce 200 g of accurately weighed rectified concentrated must into a 500 ml volumetric flask. Make up to the mark with water and homogenise.

4.2.   Preparation of the ion exchange column

Introduce into the column approximately 10 ml pre-swollen ion exchanger in H + form. Rinse the column with distilled water until all acidity has been removed, using the paper indicator to monitor this.

4.3.   Ion exchange

Pass 100 ml of the rectified concentrated must solution prepared as in paragraph 4.1 through the column at the rate of one drop every second. Collect the effluent in a beaker. Rinse the column with 50 ml of distilled water. Titrate the acidity in the effluent (including the rinse water) with the 0,1 M sodium hydroxide solution until the pH is 7 at 20 °C. The alkaline solution should be added slowly and the solution continuously shaken. Let n ml be the volume of 0,1 M sodium hydroxide solution used.

5.   Expression of the results

The total cations are expressed in milliequivalents per kilogram of total sugar to one decimal place.

5.1.   Calculations

(b)   Conductivity

1.   Principle

The electrical conductivity of a column of liquid defined by two parallel platinum electrodes at its ends is measured by incorporating it in one arm of a Wheatstone bridge.

The conductivity varies with temperature and it is therefore expressed at 20 °C.

2.   Apparatus

2.1.	Conductivity meter enabling measurements of conductivity to be made over a range from 1 to 1 000 microsiemens per cm (μS cm–1).

2.2.	Waterbath for bringing the temperature of samples to be analysed to approximately 20 °C (20 ± 2 °C).

3.   Reagents

3.1.	Demineralised water with specific conductivity below 2 μS cm–1 at 20 °C.

3.2.

Reference solution of potassium chloride Dissolve 0,581 g of potassium chloride, KCl, previously dried to constant mass at a temperature of 105 °C, in demineralised water (paragraph 3.1). Make up to one litre with demineralised water (paragraph 3.1). This solution has a conductivity of 1 000 μS cm–1 at 20 °C. It should not be kept for more than three months.

4.   Procedure

4.1.   Preparation of the sample to be analysed

Use the solution with a total sugar concentration of 25 % (m/m) (25° Brix): weigh a mass equal to 2 500/P and make up to 100 g with water (paragraph 3.1), where P = percentage (m/m) concentration of total sugars in the rectified concentrated must.

4.2.   Determination of conductivity

Bring the sample to be analysed to 20 °C by immersion in a waterbath. Maintain the temperature to within ± 0,1 °C.

Rinse the conductivity cell twice with the solution to be examined.

Measure the conductivity and express the result in μS cm–1.

5.   Expression of the results

The result is expressed in microsiemens per cm (μScm–1) at 20 °C to the nearest whole number for the 25 % (m/m) (25° Brix) solution of rectified concentrated must.

5.1.   Calculations

If the apparatus does not have temperature compensation, correct the measured conductivity using Table I. If the temperature is below 20 °C, add the correction; if the temperature is above 20 °C, subtract the correction.

(c)   Hydroxymethylfurfural (HMF)

1.   Principle of the methods

1.1.   Colorimetric method

Aldehydes derived from furan, the main one being hydroxymethylfurfural, react with barbituric acid and paratoluidine to give a red compound which is determined by colorimetry at 550 nm.

1.2.   High-performance liquid chromatography (HPLC)

Separation through a column by reversed-phase chromatography and determination at 280 nm.

2.   Colorimetric method

2.1.   Apparatus

2.1.1.

Spectrophotometer for making measurements between 300 and 700 nm.

2.1.2.

Glass cells with optical paths of 1 cm.

2.2.   Reagents

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

Dissolve 500 mg of barbituric acid, C4O3N2H4, in distilled water and heat slightly over a waterbath at 100 °C. Make up to 100 ml with distilled water. The solution keeps for about a week.

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

Place 10 g of paratoluidine, C6H4(CH3) NH2, in a 100 ml volumetric flask; add 50 ml of isopropanol, CH3CH(OH)CH3, and 10 ml of glacial acetic acid, CH3COOH (ρ20 = 1,05 g/ml). Make up to 100 ml with isopropanol. This solution should be renewed daily.

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

Prepare just before use.

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

Prepare successive dilutions containing 5, 10, 20, 30 and 40 mg/l. The 1 g/l and the diluted solutions must be freshly prepared.

2.3.   Procedure

2.3.1.   Preparation of sample

Use the solution obtained by diluting the rectified concentrated must to 40 % (m/v): introduce 200 g of accurately weighed rectified concentrated must into a 500 ml volumetric flask. Make up to the mark with water and homogenise. Carry out the determination on 2 ml of this solution.

2.3.2.   Colorimetric determination

Into each of two 25 ml flasks a and b fitted with ground glass stoppers place 2 ml of the sample prepared as in paragraph 2.3.1. Place in each flask 5 ml of paratoluidine solution (paragraph 2.2.2); mix. Add 1 ml of distilled water to flask b (control) and 1 ml barbituric acid solution (paragraph 2.2.1) to flask a. Shake to homogenize. Transfer the contents of the flasks into spectrophotometer cells with optical paths of 1 cm. Zero the absorbence scale using the contents of flask b for a wavelength of 550 nm. Follow the variation in the absorbence of the contents of flask a; record the maximum value A, which is reached after two to five minutes.

Samples with hydroxymethylfurfural concentrations above 30 mg/l must be diluted before the analysis.

2.3.3.   Preparation of the calibration curve

Place 2 ml of each of the hydroxymethylfurfural solutions with 5, 10, 20, 30 and 40 mg/l (paragraph 2.2.4) into two sets of 25 ml flasks a and b and treat them as described in paragraph 2.3.2.

The graph representing the variation of absorbence with the hydroxymethylfurfural concentration in mg/l is a straight line passing through the origin.

2.4.   Expression of results

The hydroxymethylfurfural concentration in rectified concentrated musts is expressed in milligrams per kilogram of total sugars.

2.4.1.   Method of calculation

The hydroxymethylfurfural concentration C mg/l in the sample to be analysed is that concentration on the calibration curve corresponding to the absorbence A measured on the sample.

The hydroxymethylfurfural concentration in milligrams per kilogram of total sugars is given by:

250 × ((C)/(P))

P = percentage (m/m) concentration of total sugars in the rectified concentrated must.

3.   High-performance liquid chromatography

3.1.   Apparatus

3.1.1.

High-performance liquid chromatograph equipped with: — a loop injector, 5 or 10 μl, — spectrophotometer detector for making measurements at 280 nm, — column of octadecyl-bonded silica (e.g.: Bondapak C18 — Corasil, Waters Ass.), — a recorder and, if required, an integrator, Flow rate of mobile phase: 1,5 ml/minute.

3.1.2.

Membrane filtration apparatus, pore diameter 0,45 μm.

3.2.   Reagents

3.2.1.

Doubly distilled water.

3.2.2.

Methanol, CH3OH, distilled or HPLC quality.

3.2.3.

Acetic acid, CH3COOH, (ρ20 = 1,05 g/ml).

3.2.4.

Mobile phase: water-methanol (paragraph 3.2.2)-acetic acid (paragraph 3.2.3) previously filtered through a membrane filter (0,45 μm), (40:9:1 v/v). This mobile phase must be prepared daily and outgassed before use.

3.2.5.

Reference solution of hydroxymethylfurfural, 25 mg/l (v/v). Into a 100 ml volumetric flask, place 25 mg of hydroxymethylfurfural, C6H3O6, accurately weighed, and make up to the mark with methanol (paragraph 3.2.2). Dilute this solution 1/10e with methanol (paragraph 3.2.2) and filter through a membrane filter (0,45 μm). If kept in a hermetically sealed brown glass bottle in a refrigerator, this solution will keep for two to three months.

3.3.   Procedure

3.3.1.   Preparation of sample

Use the solution obtained by diluting the rectified concentrated must to 40 % (m/v) (introduce 200 g of accurately weighed rectified concentrated must into a 500 ml volumetric flask. Make up to the mark with water and homogenise) and filter it through a membrane filter (0,45 μm).

3.3.2.   Chromatographic determination

Inject 5 (or 10) μl of the sample prepared as described in paragraph 3.3.1. and 5 (or 10) μl of the reference hydroxymethylfurfural solution (paragraph 3.2.5) into the chromatograph. Record the chromatogram.

The retention time of hydroxymethylfurfural is approximately six to seven minutes.

3.4.   Expression of results

The hydroxymethylfurfural concentration in rectified concentrated musts is expressed in milligrams per kilogram of total sugars.

3.4.1.   Method of calculation

Let the hydroxymethylfurfural concentration in the 40 % (m/v) solution of the rectified concentrated must be C mg/l.

The hydroxymethylfurfural concentration in milligrams per kilogram of total sugars is given by:

250 × ((C)/(P))

P = percentage (m/m) concentration of total sugars in the rectified concentrated must.

(d)   Heavy metals

1.   Principle

I.   Rapid method for evaluation of heavy metals

Heavy metals are revealed in the suitably diluted rectified concentrated must by the coloration produced by the formation of sulphides. They are assessed by comparison with a standard lead solution corresponding to the maximum admissible concentration.

II.   Determination of lead content by atomic absorption spectrophotometry

The chelate given by lead with ammonium pyrrolidinedithiocarbamate is extracted with methylisobutylketone and the absorbence measured at 283,3 nm. The lead content is determined by using known additional amounts of lead in a set of reference solutions.

2.   Rapid method for evaluation of heavy metals

2.1.   Reagents

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

Take 70 g of hydrochloric acid, HCl (ρ20 = 1,16 to 1,19 g/ml), and make up to 100 ml with water.

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

Take 20 g of hydrochloric acid, HCl (ρ20 = 1,16 to 1,19 g/ml), and make up to 100 ml with water.

2.1.3.   Dilute ammonia.

Take 14 g of ammonia, NH3 (ρ20 = 0,931 to 0,934 g/ml) and make up to 100 ml with water.

2.1.4.   pH 3,5 buffer solution.

Dissolve 25 g of ammonium acetate (CH3COONH4), in 25 ml of water and add 38 ml of dilute hydrochloric acid (paragraph 2.1.1). Adjust the pH if necessary with the dilute hydrochloric acid (paragraph 2.1.2) or the dilute ammonia (paragraph 2.1.3) and make up to 100 ml with water.

2.1.5.

Thioacetamide solution, (C2H5NS), 4 % (m/v).

2.1.6.

Glycerol solution, (C3H8O3, 85 % (m/v) (nD 20 °C = 1,449 to 1,455).

2.1.7.

Thioacetamide reagent. To 0,2 ml of thioacetamide solution (paragraph 2.1.5) add 1 ml of a mixture of 5 ml of water, 15 ml of 1 M sodium hydroxide solution and 20 ml of glycerol (paragraph 2.1.6). Heat over a waterbath at 100 °C for 20 seconds. Prepare just before use.

2.1.8.

Solution containing 0,002 g/l of lead. Prepare a 1 g/l lead solution by dissolving 0,400 g of lead nitrate, Pb (NO3)2, in water and making up to 250 ml with water. At the time of use, dilute this solution with water to two parts in 1 000 (v/v) in order to obtain a 0,002 g/l solution.

2.2.   Procedure

Dissolve a test sample of 10 g of the rectified concentrated must in 10 ml of water. Add 2 ml of the pH 3,5 buffer solution (paragraph 2.1.4); mix. Add 1,2 ml of the thioacetamide reagent (paragraph 2.1.7). Mix at once. Prepare the control under the same conditions by using 10 ml of the 0,002 g/l lead solution (paragraph 2.1.8).

After two minutes, any brown coloration of the rectified concentrated must solution should not be more intense than that of the control.

2.3.   Calculations

Under the conditions of the above procedure, the control sample corresponds to a maximum admissible heavy metal concentration expressed as lead of 2 mg/kg of rectified concentrated must.

3.   Determination of lead content by atomic absorption spectrophotometry

3.1.   Apparatus

3.1.1.

Atomic absorption spectrophotometer equipped with an air-acetylene burner.

3.1.2.

Lead hollow cathode lamp.

3.2.   Reagents

3.2.1.

Dilute acetic acid. Take 12 g of glacial acetic acid (ρ20 = 1,05 g/ml) and make up to 100 ml with water.

3.2.2.

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

3.2.3.

Methylisobutylketone, (CH3)2 CHCH2COCH3.

3.2.4.

Solution containing 0,010 g/l of lead. Dilute the 1 g/l lead solution (paragraph 2.1.8) to 1 % (v/v).

3.3.   Procedure

3.3.1.   Preparation of solution to be examined

Dissolve 10 g of rectified concentrated must in a mixture of equal volumes of dilute acetic acid (paragraph 3.2.1) and water, and make up to 100 ml with this mixture.

Add 2 ml of ammonium pyrrolidinedithiocarbamate solution (paragraph 3.2.2) and 10 ml of methylisobutylketone (paragraph 3.2.3). Shake for 30 seconds while protected from bright light. Leave the two layers to separate. Use the methylisobutylketone layer.

3.3.2.   Preparation of reference solutions

Prepare three reference solutions containing, in addition to 10 g of rectified concentrated must, 1, 2 and 3 ml respectively of the solution containing 0,010 g/l of lead (paragraph 3.2.4). Treat these in the same way as the solution to be examined.

3.3.3.   Control

Prepare a control by proceeding under the same conditions as in paragraph 3.3.1, but without the addition of the rectified concentrated must.

3.3.4.   Determination

Set the wavelength to 283,3 nm.

Atomise the methylisobutylketone from the control sample in the flame and zero the absorbence scale.

By operating with their respective solvent extracts, determine the absorbences of the solution to be examined and the reference solutions.

3.4.   Expression of results

Express the lead content in milligrams per kilogram of rectified concentrated must to one decimal place.

3.4.1.   Calculations

Plot the curve giving the variation in absorbence as a function of the lead concentration added to the reference solutions, zero concentration corresponding to the solution to be examined.

Extrapolate the straight line joining the points until it cuts the negative part of the concentration axis. The distance of the point of intersection from the origin gives the lead concentration in the solution to be examined.

(e)   Chemical determination of ethanol

This method is used for the determination of the alcoholic strength of low-alcohol liquids such as musts, concentrated musts and rectified concentrated musts.

1.   Principle

Simple distillation of the liquid. Oxidation of the ethanol in the distillate by potassium dichromate. Titration of the excess dichromate with an iron (II) solution.

2.   Apparatus

2.1.    Distillation apparatus used to measure the alcoholic strength

3.   Reagents

3.1.   Potassium dichromate solution.

Dissolve 33,600 g of potassium dichromate, (K2Cr2O7), in sufficient quantity of water to make one litre of solution at 20 °C.

One millilitre of this solution oxidizes 7,8924 mg of alcohol.

3.2.   Iron (II) ammonium sulphate solution.

Dissolve 135 g of iron (II) ammonium sulphate, Fe SO4, (NH4)2SO4, 6 H2O in sufficient quantity of water to make one litre of solution and add 20 ml of concentrated sulphuric acid, (H2SO4), (ρ20 = 1,84 g/ml). This solution more or less corresponds to half its volume of dichromate solution when just prepared. Subsequently, it oxidizes slowly.

3.3.   Potassium permanganate solution.

Dissolve 1,088 g of potassium permanganate, KMnO4, in a sufficient quantity of water to make one litre of solution.

3.4.   Sulphuric acid, diluted 1:2 (v/v).

A little at a time and stirring continuously, add 500 ml of sulphuric acid, (H2SO4) (ρ20 = 1,84 g/ml) to 500 ml of water.

3.5.   Ferrous orthophenanthroline reagent.

Dissolve 0,695 g of ferrous sulphate, FeSO4, 7 H2O, in 100 ml of water, and add 1,485 g of orthophenanthroline monohydrate, C12H8N2, H2O. Heat to help the dissolution. This bright red solution keeps well.

4.   Procedure

4.1.   Distillation

Place 100 g of rectified concentrated must and 100 ml of water in the distillation flask. Collect the distillate in a 100 ml volumetric flask and make up to the mark with water.

4.2.   Oxidation

Take a 300 ml flask with a ground glass stopper and with a widened neck enabling the neck to be rinsed without loss. In the flask, place 20 ml of the titrant potassium dichromate solution (paragraph 3.1) and 20 ml of the 1:2 (v/v) dilute sulphuric acid (paragraph 3.4) and shake. Add 20 ml of the distillate. Stopper the flask, shake, and wait at least 30 minutes, shaking occasionally. (This is the ‘measurement’ flask.)

Carry out the titration of the iron (II) ammonium sulphate solution (paragraph 3.2) with respect to the potassium dichromate solution by placing in an identical flask the same quantities of reagents but replacing the 20 ml of distillate by 20 ml of distilled water. (This is the ‘control’ flask.)

4.3.   Titration

Add four drops of the orthophenanthroline reagent (paragraph 3.5) to the contents of the ‘measurement’ flask. Titrate the excess dichromate by adding to it the iron (II) ammonium sulphate solution (paragraph 3.2). Stop adding the ferrous solution when the mixture changes from green-blue to brown.

To judge the end-point more precisely, change the colour of the mixture back from brown to green-blue with the potassium permanganate solution (paragraph 3.3). Subtract a tenth of the volume of this solution used from the volume of the iron (II) solution added. Let the difference be n ml.

Proceed in the same way with the ‘control’ flask. Let n′ ml be the difference here.

5.   Expression of the results

The ethanol is expressed in grams per kilogram of total sugars and is quoted to one decimal place.

5.1.   Method of calculation

n′ ml of ferrous solution reduces 20 ml of dichromate solution which oxidizes 157,85 mg of pure ethanol.

One millilitre of iron (II) solution has the same reducing power as:

((157,85)/(n)) mg of ethanol

n-n′ ml of iron (II) solution have the same reducing power as:

157,85 × ((n′ — n)/(n)) mg of ethanol.

Ethanol concentration in g/kg of rectified concentrated must is given by:

7,892 × ((n′ — n)/(n))

Ethanol concentration in g/kg of total sugars is given by:

789,2 × ((n′ — n)/(n′ × P))

P = percentage (m/m) concentration of total sugars in the rectified concentrated must.

(f)   Meso-inositol, scyllo-inositol and sucrose

1.   Principle

Gas chromatography of silylated derivatives.

2.   Reagents

2.1.	Internal standard: xylitol (aqueous solution of about 10 g/l to which a spatula tip of sodium azide is added)

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

2.3.	Trimethylchlorosilane (C3H9ClSi)

2.4.	Pyridine p.A. (C5H5N)

2.5.	Meso-inositol (C6H12O6)

3.   Apparatus

3.1.	Gas chromatograph equipped with:

3.2.

Capillary column (e.g. in fused silica, coated with OV 1, film thickness of 0,15 μ, length 25 m and internal diameter of 0,3 mm). Operating conditions: carrier gas: hydrogen or helium — carrier gas flow rate: about 2 ml/minute, — injector and detector temperature: 300 °C, — programming of temperature: 1 minute at 160 °C, 4 °C per minute to 260 °C, constant temperature of 260 °C for 15 minutes, — splitter ratio: about 1:20.

3.3.	Integrator.

3.4.	Microsyringe, 10 μl.

3.5.	Micropipettes, 50, 100 and 200 μl.

3.6.	2 ml flasks with Teflon stopper.

3.7.

Oven.

4.   Procedure

An accurately weighed sample of about 5 g of rectified concentrated must is placed in a 50 ml flask. 1 ml of standard solution of xylitol (paragraph 2.1) is added and water added to capacity. After mixing, 100 μl of solution is taken and placed in a flask (point 3.6) where it is dried under a gentle stream of air. 100 μl of absolute ethyl alcohol may be added if necessary to facilitate evaporation.

The residue is carefully dissolved in 100 μl of pyridine (paragraph 2.4) and 100 μl of bis(trimethylsilyl)trifluoroacetamide (paragraph 2.2) and 10 μl of trimethylchlorosilane (paragraph 2.3) are added. The flask is closed with the Teflon stopper and heated at 60 °C for one hour.

Draw off 0,5 μl of clear fluid and inject using a heated hollow needle in accordance with the stated splitter ratio.

5.   Calculation of results

5.1.

A solution is prepared containing: 60 g/l of glucose, 60 g/l of fructose, 1 g/l of meso-inositol and 1 g/l of sucrose. 5 g of the solution is weighed and the procedure at paragraph 4 followed. The results for meso-inositol and sucrose with respect to xylitol are calculated from the chromatogram. In the case of scyllo-inositol, which is not commercially available and has a retention time lying between the last peak of the anomeric form of glucose and the peak for meso-inositol (see diagram), the same result as for meso-inositol is taken.

6.   Expression of the results

6.1.	Meso-inositol and scyllo-inositol are expressed in milligrams per kilogram of total sugars. Sucrose is expressed in grams per kilogram of must.

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ANNEX V

CORRELATION TABLE REFERRED TO IN THE SECOND PARAGRAPH OF ARTICLE 16

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( 1 ) OJ L 148, 6.6.2008, p. 1.

( 2 ) OJ L 179, 14.7.1999, p. 1.

( 3 ) OJ L 272, 3.10.1990, p. 1.

( 4 ) OJ L 127, 15.5.2008, p. 13.

( 5 ) OJ L 253, 20.9.2008, p. 1.

( 6 ) OJ L 354, 31.12.2008, p. 7.

( 7 ) OJ L 338, 13.11.2004, p. 4.

( 8 ) OJ L 220, 15.8.2002, p. 18.

( 9 ) Treatment with PVI/PVP copolymers can only occur after the purity and identification specifications for authorised copolymers have been laid down and published in the OIV’s International Oenological Codex.

( 10 ) OJ L 338, 13.11.2004, p. 4.