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Commission Regulation (EC) No 1882/2006 of 19 December 2006 laying down methods of sampling and analysis for the official control of the levels of nitrates in certain foodstuffs (Text with EEA relevance)
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For the purposes of this Annex, the following definitions shall apply:
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Repeatability, the value below which the absolute difference between two single test results obtained under repeatability conditions, namely same sample, same operator, same apparatus, same laboratory, and short interval of time may be expected to lie within a specific probability (typically 95 %) and hence r = 2,8 × sr.
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Standard deviation, calculated from results generated under repeatability conditions.
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Relative standard deviation, calculated from results generated under repeatability conditions ((sr /) × 100).
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Reproducibility, the value below which the absolute difference between single test results obtained under reproducibility conditions, namely on identical material obtained by operators in different laboratories, using the standardised test method may be expected to lie within a certain probability (typically 95 %); R = 2,8 × sR.
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Standard deviation, calculated from results under reproducibility conditions.
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Relative standard deviation calculated from results generated under reproducibility conditions ((sR /) × 100).
Methods of analysis used for food control purposes must comply with the provisions of items 1 and 2 of Annex III to Regulation (EC) No 882/2004.
Particular attention must be paid to the extraction procedure applied. Several extraction procedures have proven to guarantee an effective extraction of the nitrate, such as hot water or methanol/water (30/70) extraction method. Cold water extraction may only be used if the analytical sample has been frozen prior to sample extraction.
The specific criteria for methods of analysis used in the monitoring of nitrate levels shall be:
Precision RSDr may be calculated as 0,66 times Precision RSDR at the concentration of interest. | |||
Criterion | Concentration range | Recommended value | Maximum permitted value |
---|---|---|---|
Recovery | < 500 mg/kg | 60-120 % | |
≥ 500 mg/kg | 90-110 % | ||
Precision RSDR | All | As derived from Horwitz Equation | 2 × value derived from Horwitz Equation |
Concentration ranges are not stated, as the precision values are calculated at the concentrations of interest,
the precision values are calculated from the Horwitz equation, i.e.:
RSDR = 2(1-0,5logC)
where:
The analytical result must be reported corrected or uncorrected for recovery. The manner of reporting and the level of recovery must be reported. The analytical result corrected for recovery shall be used for checking compliance.
The analytical result must be reported as × +/–- U whereby × is the analytical result and U is the expanded measurement uncertainty.
U is the expanded measurement uncertainty, using a coverage factor of 2 which gives a level of confidence of approximately 95 %.
The present interpretation rules of the analytical result in view of acceptance or rejection of the lot apply for the analytical result obtained on the sample for official control. In case of analysis for defence or referee purposes, the national rules apply.
Laboratory must comply with the provisions of Article 12 of Regulation (EC) No 882/2004.
More details on procedures for the estimation of measurement uncertainty and on procedures for assessing recovery can be found in the report ‘Report on the relationship between analytical results, measurement uncertainty, recovery factors and the provisions of EU food and feed legislation’ — http://ec.europa.eu/food/food/chemicalsafety/contaminants/report-sampling_analysis_2004_en.pdf
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