Commission Regulation (EC) No 627/2006 of 21 April 2006 implementing Regulation (EC) No 2065/2003 of the European Parliament and of the Council as regards quality criteria for validated analytical methods for sampling, identification and characterisation of primary smoke products

• CELEX: Regulation (EC) No 627/2006
• Articles: 3

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 .

Schedules & Appendices

ANNEX

ANNEX

Quality criteria for validated analytical methods for sampling, identification and characterisation of primary smoke products

1.   Sampling

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.   Identification and characterisation

2.1.   Definitions

For the purpose of this Annex the following definitions shall apply:

Solvent free mass

:

The mass of the material after abstraction of the solvent, which normally is water.

Volatile fraction

:

The part of the solvent free mass, which is volatile and analysable by gas chromatography.

Identification of a primary product

:

Results of a descriptive analysis, which identifies substances present in the primary product.

Characterisation of a primary product

:

Identification of the major physical-chemical fractions and quantification and identification of the chemical constituents.

LOQ

:

Limit of Quantification

LOD

:

Limit of Detection

S i

:

The single-laboratory standard deviation, calculated from results generated under repeatability conditions as defined in ISO standard 5725-1  ( 1 ) (= repeatability standard deviation estimated in a single laboratory approach according to the Harmonized Guidelines for Single-Laboratory Validation of Methods of Analysis  ( 2 ) ).

S r

:

The average within laboratory standard deviation, calculated from results generated under repeatability conditions as defined in ISO standard 5725-1  ( 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  ( 3 ) .

S R

:

The between laboratory standard deviation, calculated from results under reproducibility conditions as defined in ISO standard 5725-1  ( 1 ) and according to the Protocol for the Design, Conduct and Interpretation of Method-Performance Studies  ( 3 ) .

RSD i

:

Relative single-laboratory repeatability standard deviation (S i expressed in percent of the measured value),

RSD r

:

Relative average repeatability standard deviation (S r expressed in percent of the measured value),

RSD R

:

Relative reproducibility standard deviation (S R expressed in percent of the measured value).

2.2.   Requirements

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.

Table 1

Quality criteria for methods for identification and quantification of chemical constituents in the solvent free mass and the volatile fraction of primary products

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

Table 2

Minimum method quality criteria for analysing Polycyclic Aromatic Hydrocarbons (PAHs)

Analyte(s) PAH

RSD i

( *1 )

RSD r

( *1 )

RSD R

( *1 )

LOD  ( *3 )

LOQ  ( *3 )

Analytical range  ( *3 )

Recovery  ( *1 )

%

%

%

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 ]pyrene  ( *2 )

dibenzo[ a,e ]pyrene  ( *2 )

dibenzo[ a,i ]pyrene  ( *2 )

dibenzo[ a,h ]pyrene  ( *2 )

35

35

70

5,0

15

15-45

50-110

chrysene

5-methylchrysene

benzo[ b ]fluoranthene

benzo[ j ]fluoranthene

benzo[ k ]fluoranthene

indeno[123- cd ]pyrene

dibenzo[ a,h ]anthracene

benzo[ ghi ]perylene

dibenzo[ a,l ]pyrene

25

25

50

5,0

15

10-30

60-110

( 1 )   ISO 5725-1: Accuracy (trueness and precision) of measurement methods and results — Part 1: General principles and definitions. Geneva, 1994.

( 2 )   Thompson, M., S.L.R. Ellison, and R. Wood, Harmonized Guidelines for Single-Laboratory Validation of Methods of Analysis. Pure and Applied Chemistry, 2002. 74 (5): pp. 835-855.

( 3 )   Horwitz, W., Protocol for the design, conduct and interpretation of method-performance studies. Pure and Applied Chemistry, 1995. 67 (2): pp. 331-343.

( *1 )   Over the whole analytical range.

( *2 )   The RSD i , RSD r and RSD R values are relatively high due to the low stability of the analytes in primary smoke condensate.

( *3 )   Corrected for recovery.