BCR Approach to Certification

Inteilaboratory study (30 lata) Analysis of test mixtures and/or matrices of known content of the analytes to be certified  

Certification of the reference material (RM - CRM) by 10 labs using at least two different analytical techniques, e g. 

BCR Analytical Approach for the Certification of PAHs in Natural Matrix CRMs Prior to the certification analyses for the CRM, each participating laboratory has to prepare standard solutions of the analytes to be determined from certified reference compounds (purity 99.0 %) to calibrate their instruments for response and response linearity (multiple point calibration), detection limit, and reproducibility. In the case of PAH measurements, reference compounds of certified purity are used as internal standards, which are not present at a detectable concentration in the matrix to be analyzed (e.g. indeno[i,2,3-cd]fluoranthene (CRM 267), 5-methylchrysene (CRM 081R), benzo[f ]chry-sene (CRM 046), picene (CRM 168), and/or phenanthrene-dio). 

The analytical procedure is checked by analyses of method blanlcs to assure that secondary contamination by the analytes to be determined is avoided or minimized. Because the water content of the CRM matrix to be analyzed may vary from one laboratory to another (dependent on the local humidity and temperature), the water content has to be determined. Accordingly, at least three independent samples are kept at I05°C for 2 h, then allowed to cool to ambient temperature in a desiccator and the water loss is determined. The certified values are generally reported on a dry mass basis. 

The first step for the determination of PAHs is removal from the matrix by solvent extraction, which preferably is performed with boiling toluene or benzene (hot solvent extraction by refluxing see Jacob and Grimmer 1994), although other solvents (e.g. tol-uene/acetone, acetone, and dichloromethane) and other extraction procedures (ultrasonic treatment, Soxhlet extraction, and accelerated solvent extraction) can also be applied. 

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