ISO 3890-2:2009
Milk and milk products — Determination of residues of organochlorine compounds (pesticides) — Part 2: Test methods for crude extract purification and confirmation
ISO 3890-2|IDF 75-2:2009 specifies test methods for the purification of the crude extracts obtained by the general methods given in ISO 3890-1|IDF 75-1. It also gives recommended methods for the determination of the residues of organochlorine compounds in milk and milk products, together with confirmatory tests and clean-up procedures.
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Scope
Normative references
Method A: Liquid-liquid partitioning with
Principle
Reagents
Apparatus
Procedure
Extraction of fat and organochlorine compounds.
General methods.
Special method for cheese
Liquid-liquid partitioning
Clean-up on Florisil1)
Gas chromatography
Method B: Liquid-liquid partitioning with dimethylformamide
Principle
Reagents
Apparatus
Procedure
Extraction of fat and organochlorine compounds
General methods
Special methods
Milk
Butter
DMF-partitioning of fat and organochlorine compounds
Clean-up on aluminium oxide with n-hexane
Gas chromatography
Method C: Liquid-liquid partitioning with
Principle
Reagents
Apparatus
Procedure
Extraction of fat and organochlorine compounds
DMF-partitioning of fat and pesticides
Clean-up on Florisil1) with light petroleum
Gas chromatography
Method D: Column chromatography on aluminium oxide of precis
Principle
Reagents
Apparatus
Procedure
General methods
Test portion
Extraction of fat and organochlorine compounds
Determination of extracted fat
Clean-up
Gas chromatography
Method E: Column chromatography on alumina column
Principle
Reagents
Apparatus
Procedure
Extraction of fat and organochlorine compounds
General methods
Special methods
Anhydrous butterfat
Milk
Cheese
Column chromatography
Gas chromatography
Method F: Column chromatography on partia
Principle
Reagents
Apparatus
Procedure
Extraction of fat and organochlorine compounds
General methods
Special methods
Milk and unsweetened condensed milk
Sweetened condensed milk
Clean-up on Florisil1)
Gas chromatography
Method G: Column chromatography on partially deactivated sil
Principle
Reagents
Apparatus
Procedure
Extraction of fat and organochlorine compounds
Clean-up
Fat and organochlorine compounds
Short procedure for milk, evaporated milk, dried milk and ch
Gas chromatography
Method H: Gel-permeation chromatography
Principle
Reagents
Apparatus
Procedure
Extraction of fat and organochlorine compounds
Clean-up by gel-permeation chromatography
Gas chromatography
Confirmatory tests and additional clean-up procedure
Confirmatory test A: Determination of organochlorine compoun
Principle
Apparatus
Injection technique
Splitless injector
All-glass solid injector
Testing the whole system
Application and analysis of samples
Confirmatory test B: Thin-layer chromatography of organochlo
Principle
Reagents
Apparatus
Procedure
Evaluation of the chromatogram
Confirmatory test C: Chemical modifications
General
Derivative formation in solid matrix
Reagents
Procedure
Confirmation of DDT, TDE, methoxychlor, -chlordane, heptach
Confirmation of endrin residues
Confirmation of endosulfan residues
Confirmation of dieldrin residues
Confirmation of the identity of hexachlorobenzene (HCB) resi
Reagents
Procedure
Confirmatory test D: Photochemical modifications
General
Apparatus
Procedure
Additional clean-up procedure
Principle
Reagents
Apparatus
Procedure
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Scope
Normative references
Method A: Liquid-liquid partitioning with
Principle
Reagents
Apparatus
Procedure
Extraction of fat and organochlorine compounds.
General methods.
Special method for cheese
Liquid-liquid partitioning
Clean-up on Florisil1)
Gas chromatography
Method B: Liquid-liquid partitioning with dimethylformamide
Principle
Reagents
Apparatus
Procedure
Extraction of fat and organochlorine compounds
General methods
Special methods
Milk
Butter
DMF-partitioning of fat and organochlorine compounds
Clean-up on aluminium oxide with n-hexane
Gas chromatography
Method C: Liquid-liquid partitioning with
Principle
Reagents
Apparatus
Procedure
Extraction of fat and organochlorine compounds
DMF-partitioning of fat and pesticides
Clean-up on Florisil1) with light petroleum
Gas chromatography
Method D: Column chromatography on aluminium oxide of precis
Principle
Reagents
Apparatus
Procedure
General methods
Test portion
Extraction of fat and organochlorine compounds
Determination of extracted fat
Clean-up
Gas chromatography
Method E: Column chromatography on alumina column
Principle
Reagents
Apparatus
Procedure
Extraction of fat and organochlorine compounds
General methods
Special methods
Anhydrous butterfat
Milk
Cheese
Column chromatography
Gas chromatography
Method F: Column chromatography on partia
Principle
Reagents
Apparatus
Procedure
Extraction of fat and organochlorine compounds
General methods
Special methods
Milk and unsweetened condensed milk
Sweetened condensed milk
Clean-up on Florisil1)
Gas chromatography
Method G: Column chromatography on partially deactivated sil
Principle
Reagents
Apparatus
Procedure
Extraction of fat and organochlorine compounds
Clean-up
Fat and organochlorine compounds
Short procedure for milk, evaporated milk, dried milk and ch
Gas chromatography
Method H: Gel-permeation chromatography
Principle
Reagents
Apparatus
Procedure
Extraction of fat and organochlorine compounds
Clean-up by gel-permeation chromatography
Gas chromatography
Confirmatory tests and additional clean-up procedure
Confirmatory test A: Determination of organochlorine compoun
Principle
Apparatus
Injection technique
Splitless injector
All-glass solid injector
Testing the whole system
Application and analysis of samples
Confirmatory test B: Thin-layer chromatography of organochlo
Principle
Reagents
Apparatus
Procedure
Evaluation of the chromatogram
Confirmatory test C: Chemical modifications
General
Derivative formation in solid matrix
Reagents
Procedure
Confirmation of DDT, TDE, methoxychlor, -chlordane, heptach
Confirmation of endrin residues
Confirmation of endosulfan residues
Confirmation of dieldrin residues
Confirmation of the identity of hexachlorobenzene (HCB) resi
Reagents
Procedure
Confirmatory test D: Photochemical modifications
General
Apparatus
Procedure
Additional clean-up procedure
Principle
Reagents
Apparatus
Procedure