
Article 1 
The quality criteria for validated analytical methods for sampling, identification and characterisation of primary smoke products, as referred to in point 4 of Annex II to Regulation (EC) No 2065/2003, shall be as set out in the Annex to this Regulation.
Article 2 
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, 21 April 2006.
For the Commission
Markos KYPRIANOU
Member of the Commission
ANNEX
1. 
The basic requirement is to obtain a representative and homogeneous laboratory sample.

The analyst shall ensure that samples do not become contaminated during sample preparation. Containers have to be rinsed with high purity acetone or hexane (p.A., HLPC grade or equivalent) before use to minimise the risk of contamination. Wherever possible, apparatus coming into contact with the sample shall be made of inert materials e.g. glass or polished stainless steel. Plastics such as polypropylene are to be avoided, because the analyte can adsorb onto these materials.

All of the sample material received by the laboratory is to be used for the preparation of test material. Only very finely homogenised samples give reproducible results.

There are many satisfactory specific sample preparation procedures which may be used.

2.  2.1. 
For the purpose of this Annex the following definitions shall apply:

Solvent free massThe mass of the material after abstraction of the solvent, which normally is water.Volatile fractionThe part of the solvent free mass, which is volatile and analysable by gas chromatography.Identification of a primary productResults of a descriptive analysis, which identifies substances present in the primary product.Characterisation of a primary productIdentification of the major physical-chemical fractions and quantification and identification of the chemical constituents.

LOQLimit of QuantificationLODLimit of DetectionSiThe single-laboratory standard deviation, calculated from results generated under repeatability conditions as defined in ISO standard 5725-1 (= repeatability standard deviation estimated in a single laboratory approach according to the Harmonized Guidelines for Single-Laboratory Validation of Methods of Analysis).SrThe average within laboratory standard deviation, calculated from results generated under repeatability conditions as defined in ISO standard 5725-1 in a collaborative trial with a minimum of eight laboratories conducted according to the Protocol for the Design, Conduct and Interpretation of Method-Performance Studies.SRThe between laboratory standard deviation, calculated from results under reproducibility conditions as defined in ISO standard 5725-1 and according to the Protocol for the Design, Conduct and Interpretation of Method-Performance Studies.RSDiRelative single-laboratory repeatability standard deviation (Si expressed in percent of the measured value),RSDrRelative average repeatability standard deviation (Sr expressed in percent of the measured value),RSDRRelative reproducibility standard deviation (SR expressed in percent of the measured value).
 2.2. 
Without prejudice to Article 11 of Regulation (EC) No 882/2004, the validated method for identification and characterisation to be selected by the laboratory shall comply with the quality criteria indicated in Tables 1 and 2.


Parameter Value/Comment
Solvent free mass At least 50 % by mass shall be identified and quantified
Volatile fraction At least 80 % by mass shall be identified and quantified


Analyte(s) PAH RSDi RSDr RSDR LOD LOQ Analytical range Recovery
 % % % μg/kg μg/kg μg/kg %
benzo[a]pyrene 20 20 40 1,5 5,0 5,0-15 75-110
benzo[a]anthracene 20 20 40 3,0 10 10-30 75-110
cyclopenta[cd]pyrenedibenzo[a,e]pyrenedibenzo[a,i]pyrenedibenzo[a,h]pyrene 35 35 70 5,0 15 15-45 50-110
chrysene5-methylchrysenebenzo[b]fluoranthenebenzo[j]fluoranthenebenzo[k]fluorantheneindeno[123-cd]pyrenedibenzo[a,h]anthracenebenzo[ghi]perylenedibenzo[a,l]pyrene 25 25 50 5,0 15 10-30 60-110



