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BS EN 16215:2020 Animal feeding stuffs: Methods of sampling and analysis. Determination of dioxins and dioxin-like PCBs by GC/HRMS and of indicator PCBs by GC/HRMS, 2020
- undefined
- 1 Scope
- 2 Normative references
- 3 Terms and definitions
- 4 Principle
- 5 Reagents [Go to Page]
- 5.1 General
- 5.2 Dioxins, furans, non-ortho PCBs, mono-ortho PCBs and non-dioxin-like PCBs and their labelled analogues
- 6 Apparatus
- 7 Sampling
- 8 Preparation of test sample
- 9 Procedure [Go to Page]
- 9.1 General
- 9.2 Animal feed stuff sample and oil/fat sample [Go to Page]
- 9.2.1 10 g animal feed stuff sample (12 % moisture content)
- 9.2.2 2,5 g oil/fat sample
- 10 Extraction [Go to Page]
- 10.1 General
- 10.2 Module BI Extraction using automated Pressurized Fluid Extraction (PFE) system
- 10.3 Module BII: Manual extraction procedure
- 11 Clean-up [Go to Page]
- 11.1 General
- 11.2 Module CI: Automated clean-up
- 11.3 Module CII: Manual sample clean-up, removal of fat and group separation
- 11.4 Additional clean-up-steps for fraction A and fraction B of module CII
- 11.5 Module CIII: Removal of matrix, manual sample clean-up and group separation
- 12 Module D: Gas chromatograph-high resolution mass spectrometer (GC-HRMS) [Go to Page]
- 12.1 General [Go to Page]
- 12.2 Reagents and materials
- 12.3 Procedure
- 13 Calculation and expression of results [Go to Page]
- 13.1 General
- 13.2 Calibration by Isotope Dilution
- 13.3 Linearity
- 13.4 Calibration criteria
- 13.5 Identification and confirmation
- 13.6 Calculation
- 13.7 Toxic Equivalent (TEQ) values
- 13.8 Recovery
- 14 Precision
- 15 Test report
- Annex A (informative)Description of PTV injection system [Go to Page]
- A.1 Large volume injection (100 µl) – GC-HRMS Calibration mixtures dioxins and non-ortho PCBs
- A.2 Sample preparation procedure
- A.3 PTV injection conditions using 100 µl injection
- Annex B (informative)Description of standards and concentration of the standard solutions [Go to Page]
- B.1 CAS Registry numbers for dioxins, furans, non-ortho PCBs, mono-ortho PCBs and non-dioxin-like PCBs and their labelled analogues
- B.2 Standard solutions [Go to Page]
- B.2.1 13C-1,2,3,4-TCDD (50 µg/ml)
- B.2.2 13C-1,2,3,6,7,8-HxCDF (50 µg/ml)
- B.2.3 37Cl4-2,3,7,8 TCDD (50 µg/ml)
- B.2.4 Mixture 13C-PCDD (1 µg/ml)
- B.2.5 Mixture 13C-PCDF (1 µg/ml)
- B.2.6 Mixture TCDD-HpCDD (5 µg/ml)
- B.2.7 Mixture TCDF-HpCDF (5 µg/ml)
- B.2.8 OCDD (10 µg/ml)
- B.2.9 OCDF (50 µg/ml)
- B.2.10 OCDF standard (5 µg/ml)
- B.2.11 Mixture 13C-non-ortho PCBs (1 µg/ml)
- B.2.12 Mixture 13C-mono-ortho PCBs (1 µg/ml)
- B.2.13 Mixture 13C-non-dioxin-like PCBs (5 µg/ml)
- B.2.14 Mixture non-ortho PCBs (10 µg/ml)
- B.2.15 Mixture mono-ortho PCBs (10 µg/ml)
- B.2.16 Commercially available mixture non-dioxin-like PCBs (10 µg/ml)
- B.2.17 Recovery standard DIOX-RS-100 (100 pg/µl 13C-1,2,3,4-TCDD and 100 pg/µl 13C-1,2,3,6,7,8-HxCDF in toluene)
- B.2.18 Recovery standard DIOX-RS-1 (1,0 pg/µl 13C-1,2,3,4-TCDD, 1,0 pg/µl 13C-1,2,3,6,7,8-HxCDF in toluene)
- B.2.19 Recovery standard TCDD-RS-III (100 pg/µl 13C-1,2,3,4-TCDD in iso-octane)
- B.2.20 Recovery standard TCDD-RS-VI (25 pg/µl 13C-1,2,3,4-TCDD in iso-octane)
- B.2.21 Clean-up standard CS-50 (50 pg/µl 37Cl4-2,3,7,8-TCDD in toluene)
- B.2.22 Clean-up standard CS-1 (1,0 pg/µl 37Cl4-2,3,7,8-TCDD in toluene)
- B.2.23 Mixture non-ortho PCBs (NOP-500) (500 pg/µl in toluene)
- B.2.24 Mixture PCDD/F and non-ortho PCBs (DIOXNOP) (20 pg/µl in toluene)
- B.2.25 Mixture PCDD/F and non-ortho PCBs (DIOXNOP-1) (2,0 pg/µl in toluene)
- B.2.26 Mixture mono-ortho PCBs and indicator PCBs (MOPIP-500) (500 pg/µl in iso-octane)
- B.2.27 Mixture mono-ortho PCBs and indicator PCBs (MOPIP-25) (25 pg/µl in iso-octane)
- B.2.28 Mixture mono-ortho PCBs and indicator PCBs (MOPIP-2,5) (2,5 pg/µl in iso-octane)
- B.2.29 Mixture mono-ortho PCBs and indicator PCBs (MOPIP-,.25) (0,25 pg/µl in iso-octane)
- B.2.30 Mixture 13C-PCDD/F and 13C-non-ortho PCBs (13C-DIOXNOP) (50 pg/µl in toluene)
- B.2.31 Mixture 13C-PCDD/F and 13C-non-ortho PCBs (13C-DIOXNOP-2) (0,10 pg/µl in toluene)
- B.2.32 Mixture 13C-mono-ortho PCBs and 13C-indicator PCBs (13C-MOPIP-1) (50 pg/µl in iso-octane)
- B.2.33 Mixture 13C-mono-ortho PCBs and 13C-indicator PCBs (13C-MOPIP-2) (2,0 pg/µl in iso-octane)
- B.3 GC-standard solutions [Go to Page]
- B.3.1 Standard dioxins and non-ortho PCBs mixtures
- B.3.2 Preparation mono-ortho PCBs standard mixtures.
- Annex C (informative)Example of automated procedure
- Annex D (informative)Mass spectrometer (MS)
- Annex E (informative)Use of additional clean-up after fractionation using a small multi-layer silica column [Go to Page]
- E.1 Preparation of the silica mixtures
- E.2 Preparation of the small multi-layer column [Go to Page]