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LABORATORIES Mar Verhoeff Dr. A. Verwey / Agrolab Rotterdam MVO course April 2014
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Agenda
• Role of an independent laboratory • Contract organizations • Contractual methods of analysis • Method development by ISO • Laboratory certification • Tankcleaning
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Role of an independent laboratory
• To determine the quality / quantity of the commodity
• The price of the goods is based on the quality / quantity
• Also the processing (refining & bleaching) is depending on the quality of the crude oils/fats
• All based on independent analyses, using contractual methods
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Good analysis, good sample first
Contract organisations
• FOSFA, London • NOFOTA, Rotterdam • GAFTA, London • PORAM, Malaysia
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Contractual methods of analyses
• FOSFA – ISO methods (if available), BS, AOCS
• NOFOTA - follows FOSFA, NEN (exceptional)
• GAFTA - own methods, originating from EU
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International Standardisation Organisation (ISO) based Geneva
• Member states (not complete list):
– The Netherlands (NEN) – United Kingdom (BSI) – France (AFNOR) – Germany (DGF) – Argentina (IRAM) – Spain (AENOR) – USA (AOCS) – Australia (Standards Australia)
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Birth of an ISO-method • A member state proposes a method (New
Work Item Proposal) • This is balloted with the members for adding
to the work programme and for comments • These comments are evaluated and the
method is amended • An international ring test is organised • The ring test results are evaluated to see if
they meet the ISO statistical requirements
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Birth of an ISO-method 2
• Additional comments (if any) are taken into account for the next version of the method
• Voting is performed • Method is accepted if the members agree • In general this procedure takes about 3
years • The methods are reviewed after 3/5 years
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Laboratory certification
• The laboratory must be recognised by the contract organisations and others e.g. FEDIOL, VERNOF, GMP, QS
• By means of: – participation in ring trials, questionaires
and audits • Accreditation according to ISO 17025 is
recommended and appreciated
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ISO 17025 accreditation
• Management and documentation quality system in compliance with ISO 9001
• Suitable, qualified employees • Using validated methods • Using calibration standards and equipment
that can be traced back to national standards • Yearly participation in proficiency tests • Yearly audit by Council for Accreditation
(RVA)
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Price of laboratory equipment
• Free Fatty Acids – EUR 100
• Pesticide residues (GC/LC-MS-MS ) – EUR 250.000 (each)
• Dioxins (HRGC-MS/MS) – EUR 500.000
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Free Fatty Acids
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Free Fatty Acids, calculation
ml NaOH x concentration x mol.weight (282) ----------------------------------------------------------- x 100% weight of oil (mg)
• mol. weight, palm oil (palmitic) = 256 • mol. weight, coconut-/palmkernel oil (lauric) = 200
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Pesticide residues
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Question
• Sample CPO from an incoming seagoing vessel arrives in the lab, without instructions
• Which analyses would you perform?
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Answer
• Free Fatty Acids • Moisture and volatile matter • Impurities • Lauric acid (C12) • DOBI • Hydrocarbons
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Generally acceptable results
• DOBI min 1,5 • C12 (lauric acid) max 0,25 % • Hydrocarbons (C10 - C56) max 300 mg/kg • Hydrocarbons (C10 - C24) max 25 mg/kg
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Question 2
• Sample of Ukrainian Sunflowerseed oil arrives without instructions
• Which analyses would you perform?
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Answer 2
• Free Fatty Acids • Moisture and volatile matter • Insoluble impurities • Hydrocarbons • Linoleic / oleic acid ?
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How about Argentinian Sunflower Seed Oil?
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Acceptable results 2
• Hydrocarbons (mineral) (C10 - C56) max 50 mg/kg
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Acceptable results
• Hydrocarbons (mineral) (C10-C40) max 300 mg/kg
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Tank Cleaning
• Deep sea tanker vessels arrive in Rotterdam from the Far East, carrying vegetable oils/fats.
• Cannot return empty (too expensive) • Tank cleaning has to be performed • Vessels return to the Far East after cleaning
and after loading petrochemicals
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Problems that may occur after discharge / prior to cleaning
Cleaning of Cargo Lines • Clean tanks is not enough • All parts in contact with cargo must
be cleaned • Difficult to give specific instructions • Standard recommendations are
given
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Tank cleaning procedure
• Butterworthing with fixed / transportable machines
• Depending on the melting point of the cargo, this must be done with cold / warm or hot seawater
• Followed by many cleaning cycles with (alkaline !!) detergents
• Afterwards the tank is rinsed with fresh water
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Tank Cleaning final
• Inspection of the tank; visually and by means of wall wash tests
• Analyses of these wall washes on the spot or in the laboratory
• Calculation of the risk in case of any doubt
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Thanks for
your attention
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