Commission Implementing Regulation (EU) 2023/383 of 16 February 2023 amending Regulation (EC) No 2870/2000 laying down Community reference methods for the analysis of spirit drinks, and repealing Regulation (EEC) No 2009/92 determining Community analysis methods for ethyl alcohol of agricultural origin in the preparation of spirit drinks, aromatized wines, aromatized wine-based drinks and aromatized wine-product cocktails

THE EUROPEAN COMMISSION,

Having regard to the Treaty on the Functioning of the European Union,

Having regard to Regulation (EU) 2019/787 of the European Parliament and of the Council of 17 April 2019 on the definition, description, presentation and labelling of spirit drinks, the use of the names of spirit drinks in the presentation and labelling of other foodstuffs, the protection of geographical indications for spirit drinks, the use of ethyl alcohol and distillates of agricultural origin in alcoholic beverages, and repealing Regulation (EC) No 110/2008 ¹, and in particular Article 20, first paragraph, point (d), thereof,

Whereas:

• (1) The definition and requirements for ethyl alcohol of agricultural origin laid down in Article 5 of Regulation (EU) 2019/787 have been amended by Commission Delegated Regulation (EU) 2022/1303 ² among others to bring the maximum level of certain residues in line with the technical parameters currently used by the industry and by most laboratories of analysis.

• (2) In that context, it is deemed necessary to amend Commission Regulation (EC) No 2870/2000 ³ to extend the reference methods set out in the Annex thereto to the analysis of ethyl alcohol of agricultural origin.

• (3) The alcoholic strength by volume of ethyl alcohol of agricultural origin should be established on the basis of the reference method set out in Chapter I of the Annex to Regulation (EC) No 2870/2000 as that is the established method currently used for the analysis of spirit drinks. For that purpose, it is appropriate to establish that ethyl alcohol of agricultural origin should be considered as a distillate whose alcoholic strength by volume is to be measured directly and not after distillation. Nonetheless, since automatic densimeters provide an erratic number when the injected alcohol is not clear, it is appropriate to provide that the sample should be distilled in that case.

• (4) In view of determining the origin of ethyl alcohol, notably that it has been obtained from products listed in Annex I to the Treaty, it is appropriate to resume method 13 set out in Commission Regulation (EC) No 625/2003 ⁴, which is now obsolete, aimed at determining the ¹⁴C content in ethanol permitting a distinction between synthetic alcohol and fermentation alcohol.

• (5) The measurement of ethyl acetate, acetaldehyde, higher alcohols and methanol in ethyl alcohol of agricultural origin should be based on the reference methods set out in point III.2 of Chapter III of the Annex to Regulation (EC) No 2870/2000 as those are established methods currently used for the analysis of a number of spirit drinks.

• (6) Concerning furfural, the reference method for its measurement should be based on the established method provided for the analysis of furfural in spirit drinks, which is the liquid chromatography method for wood compounds set out in Chapter X of the Annex to Regulation (EC) No 2870/2000.

• (7) As there is a difference in alcoholic strength between ethyl alcohol of agricultural origin and the spirit drinks for which there are reference methods of analysis set out in the Annex to Regulation (EC) No 2870/2000, and taking into account that concentrations of volatile substances (esters, aldehydes, higher alcohols) expected for ethyl alcohol of agricultural origin are considerably at lower limits than for some spirit drinks, it is appropriate to determine minor adaptations to those methods to accommodate those differences.

• (8) Regulation (EC) No 2870/2000 should therefore be amended accordingly.

• (9) Commission Regulation (EEC) No 2009/92 ⁵ relates to the analysis of ethyl alcohol of agricultural origin. Since its adoption, the rules concerning these methods of analysis have evolved with the repeal of Commission Regulation (EEC) No 1238/92 ⁶, concerning the analysis of neutral alcohol, by Commission Regulation (EC) No 1623/2000 ⁷, as well as the adoption of a definition and requirements for ethyl alcohol of agricultural origin in Article 5 of Regulation (EU) 2019/787. Regulation (EEC) No 2009/92 is therefore becoming obsolete.

• (10) In the interest of clarity and legal certainty, Regulation (EEC) No 2009/92 should be repealed.

• (11) The measures provided for in this Regulation are in accordance with the opinion of the Committee for Spirit Drinks,

HAS ADOPTED THIS REGULATION:

Article 1

Amendments to Regulation (EC) No 2870/2000

Regulation (EC) No 2870/2000 is amended as follows:

• (1) the following Article 1a is inserted:

‘Article 1a

1. This Regulation applies to ethyl alcohol of agricultural origin as defined by Article 5 of Regulation (EU) 2019/787 of the European Parliament and of the Council[^ntr*1-L_2023053EN.01000301-E0008].

1. The Union reference methods of analysis for ethyl alcohol of agricultural origin shall be those set out in the Annex to this Regulation.

1. For the purposes of this Regulation, ethyl alcohol of agricultural origin shall be considered as a distillate whose alcoholic strength by volume shall be measured directly as set out in Appendix II of Chapter I of the Annex.

However, where the alcohol sample is not clear or suspended particles are visible, the sample shall be distilled.

1. For the determination of volatile substances the calibration with the standard solution C prepared in absolute ethanol shall be required to achieve appropriate matrix matching between samples and standard solutions detailed in Chapter III.2 of the Annex.

1. For the determination of furfural, as detailed in Chapter X of the Annex, ethyl alcohol of agricultural origin shall be diluted by two through the addition of water so as to double its initial volume and reach an alcoholic strength by volume compatible with the calibration solutions. Results for the analysis of furfural shall be converted to grams per hectolitre of 100 % vol. alcohol in accordance with the equation ‘Concentration of furfural in grams per hectolitre of 100 % vol. alcohol = Concentration of furfural in mg/l x 10/alcoholic strength by volume (% vol)’, where alcoholic strength by volume (% vol) is the alcoholic strength of the measured sample as determined in Chapter I of the Annex.

1. For the determination of ¹⁴C content in ethanol, the method set out in Chapter XI of the Annex shall be used.

[^ntr*1-L_2023053EN.01000301-E0008]: Regulation (EU) 2019/787 of the European Parliament and of the Council of 17 April 2019 on the definition, description, presentation and labelling of spirit drinks, the use of the names of spirit drinks in the presentation and labelling of other foodstuffs, the protection of geographical indications for spirit drinks, the use of ethyl alcohol and distillates of agricultural origin in alcoholic beverages, and repealing Regulation (EC) No 110/2008 (OJ L 130, 17.5.2019, p. 1).’;"

• (2) the Annex is amended in accordance with the Annex to this Regulation.

Article 2

Repeal of Regulation (EEC) No 2009/92

Regulation (EEC) No 2009/92 is repealed.

Article 3

Entry into force

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

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

Done at Brussels, 16 February 2023.

For the Commission

The President

Ursula VON DER LEYEN

ANNEX

The Annex to Regulation (EC) No 2870/2000 is amended as follows:

• (1) in the table of contents, the following point is added:

• ‘XI. Determination of ¹⁴C content in ethanol’;

• (2) in point 5 (Reagents and Materials) of part III.2 (Gas chromatographic determination of volatile congeners: aldehydes, higher alcohols, ethyl acetate and methanol) of Chapter III, the following points are inserted:

• ‘5.13a For ethyl alcohol of agricultural origin only, ethanol absolute (CAS 64-17-5).’;

• ‘5.14.1a For ethyl alcohol of agricultural origin only, standard solution A shall be prepared pipetting the reagents with reduced volumes of higher alcohols with the purpose of having standard solutions with concentrations close to the legal limits for ethyl alcohol of agricultural origin.’;

• ‘5.14.2a For ethyl alcohol of agricultural origin only, standard solution B shall be prepared pipetting a suitable internal standard with the reduced volumes with the purpose of having standard solutions with concentrations close to the legal limits for ethyl alcohol of agricultural origin.’;

• (3) the following Chapter XI is added:

‘XI.   DETERMINATION OF ¹⁴C CONTENT IN ETHANOL

1. Introduction

Determination of the ¹⁴C content in ethanol permits a distinction to be made between alcohol from fossil fuels (synthesis alcohol) and alcohol from recent raw materials (fermentation alcohol).

1. Definition

The ¹⁴C content of ethanol shall be considered as the ¹⁴C content determined using the method described here or the method described in standard EN 16640 Method C.

The natural ¹⁴C content in the atmosphere (the reference value), which is absorbed by living vegetation by assimilation, is not a constant value. The reference value is therefore determined on ethanol from raw materials of the most recent vegetation period. This annual reference value is determined according to standard EN 16640. However, another reference value can be accepted where it is certified by an accredited body.

1. Principle

The ¹⁴C content of samples containing alcohol with at least 85 % mass ethanol is determined directly by liquid scintillation count.

1. Reagents

4.1.   Toluene scintillator

5,0 g 2,5-diphenyloxazole (PPO)

0,5 g p-bis-[4-methyl-5-phenyloxazolyl(2)]-benzene (dimethyl-POPOP) in 1 litre analytical grade toluene.

Commercial, ready-to-use toluene scintillators of this composition may also be used.

4.2.   ¹⁴C standard

n-Hexadecane ¹⁴C with an activity of about 1 × 10⁶ dpm/g (approximately 1,67 × 10⁶ cBq/g) and a guaranteed accuracy of determined activity of ± 2 % rel.

4.3.   ¹⁴C-free ethanol

Synthesis alcohol from raw materials of fossil origin with at least 85 % mass ethanol, to determine the background.

	4.4.	Alcohol from recent raw materials of the most recent vegetation period with at least 85 % mass ethanol as reference material.

1. Apparatus

	5.1.	Multi-channel liquid scintillation spectrometer with processor and automatic external standardisation and display of the external standard/channel ratio (usual design: three meter channels and two external standard channels).

	5.2.	Low-potassium counter tubes suitable for the spectrometer, with dark screw-tops containing a polyethylene insert.

	5.3.	Volumetric pipettes, 10 ml.

	5.4.	Automatic dosing device 10 ml.

	5.5.	250 ml round-bottom flask with ground-glass stopper.

	5.6.	Alcohol distillation apparatus with heating mantle, e.g. type Micko.

	5.7.	Microliter syringe 50 μl.

	5.8.	Pycnometer funnel, pycnometers, 25 ml and 50 ml. As an alternative, equivalent equipment, such as electronic densimetry, should be allowed.

	5.9.	Thermostat with a temperature stability of ± 0,01 °C.

1. Procedure

6.1.   Adjusting the equipment

The equipment shall be adjusted according to the manufacturer’s instructions. Measuring conditions are optimal when the value E2/B, the quality index, is at its maximum.

E = efficiency

B = background

Only two meter channels are optimised. The third is left fully open for control purposes.

6.2.   Selection of counter tubes

A larger number of counter tubes than will later be needed are each filled with 10 ml of ¹⁴C-free synthesis ethanol and 10 ml toluene scintillator. Each is measured for at least 4 cycles × 100 minutes. Tubes whose backgrounds vary by more than ± 1 % rel. from the mean are discarded. Only tubes new from the factory and from the same batch may be used.

6.3.   Determination of the external standard/channel ratio (ESCR).

During the process of setting the channels (point 6.1) the ESCR is determined using the appropriate computer program when the efficiency is determined. The external standard used is ¹³⁷caesium, which is already built-in by the manufacturer.

6.4.   Preparation of sample

Samples having an ethanol content of at least 85 % mass and free from impurities, which absorb at wavelengths below 450 nm may be measured. The low residue of esters and aldehydes has no disruptive effect. The alcohol content of the sample is previously determined with an approximation of 0,1 %.

1. Measurement of samples using external standard

	7.1.	The low absorbance samples as described in point 6.4 with an ESCR value of approximately 1,8 may be measured through the ESCR, which provides a measure of the efficiency ratio.

7.2.   Measurement

10 ml each of the samples prepared according to point 6.4 is pipettes into a selected counter tube checked for background and 10 ml of toluene scintillator is added via an automatic dosing device. The samples in the tubes are homogenised by suitable rotary movements; the liquid shall not be allowed to wet the polyethylene insert in the screw-top. A tube containing ¹⁴C-free fossil ethanol is prepared in the same way to measure the background. To check the relevant annual ¹⁴C value a duplicate of recent ethanol from the latest vegetation period is prepared, a tube being mixed with internal standard, see point 8.

The control and background samples are placed at the beginning of the measurement series, which shall contain no more than 10 samples for analysis. Total measuring time per sample is at least 2 × 100 minutes, with the individual samples being measured in part stages of 100 minutes so that any equipment drift or other defect can be detected. (One cycle therefore corresponds to a measuring interval of 100 minutes per sample).

Background and control samples shall be freshly prepared every four weeks.

In the case of slightly extinguished samples (ESCR circa 1,8) the efficiency is only negligibly affected by the change in this value. If the change is within ± 5 % rel. the same efficiency can be expected. For more greatly extinguished samples, such as denatured alcohols, the efficiency may be established via the extinction correction graph. If an appropriate computer program is not available the internal standard shall be used, and this gives an unambiguous result.

1. Measuring samples using internal standard hexadecane¹⁴C

8.1.   Procedure

Control and background samples (recent and fossil ethanol) and the unknown material are each measured as duplicates. One sample of the duplicate is prepared in a non-selected tube and an accurately dosed quantity (30 μl) of hexadecane¹⁴C is added as internal standard (added activity around 26 269 dpm/gC approximately 43 782 cBq/gC). For the sample preparation and measuring time of the other samples see point 7.2, but the measuring time for the samples with the internal standard may be reduced to about five minutes by presetting at 10⁵ pulses. One duplicate each of background and control samples is used per measuring series; these are placed at the beginning of the measuring series.

8.2.   Handling the internal standard and counter tubes

To prevent contamination when measuring with the internal standard these shall be stored and handled well away from the area where the samples for analysis are prepared and measured. After measurement the tubes checked for background may be re-used. The screw-tops and tubes containing the internal standard shall be disposed of.

1. Expression of the results

9.1.   The unit of activity of a radio-active substance is the becquerel; 1 Bq = 1 decay/sec.

Indication of specific radio-activity is expressed as becquerels relative to one gram carbon = Bq/gC.

To obtain more practical results, these shall be expressed in centi-bequerels = cBq/gC.

The descriptions and formulae used in the literature, based on dpm, may also be used. To obtain corresponding figures in cBq merely multiply the dpm figure by 100/60.

9.2.   Expression of results with external standard

Image omitted; see official source

9.3.   Expression of results with internal standard

Image omitted; see official source

9.4.   Abbreviations

cpmpr	=	the mean sample count rate over the total measuring time.
cpmNE	=	the mean background pulse rate calculated in the same way.
cpmIS	=	count rate of samples, with an internal standard.
dpmIS	=	the quantity of internal standard added (calibration radioactivity dpm).
V	=	the volume of the samples used in ml.
F	=	the content in grammes pure alcohol per ml corresponding to its concentration.
Z	=	the efficiency corresponding to the ESCR value.
1,918	=	the number of grammes alcohol per gramme carbon.

1. Reliability of the method

10.1.   Repeatability (r)

r = 0,632 cBq/g C; S(r) = ± 0,223 cBq/g C

10.2.   Reproducibility (R)

R = 0,821 cBq/g C; S(R) = ± 0,290 cBq/g C.’