laboratories - mvo · • contractual methods of analysis • method development by iso ... •...

LABORATORIES Mar Verhoeff Dr. A. Verwey / Agrolab Rotterdam MVO course April 2014

1

Agenda

• Role of an independent laboratory • Contract organizations • Contractual methods of analysis • Method development by ISO • Laboratory certification • Tankcleaning

3

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

4

Good analysis, good sample first

Contract organisations

• FOSFA, London • NOFOTA, Rotterdam • GAFTA, London • PORAM, Malaysia

6

Contractual methods of analyses

• FOSFA – ISO methods (if available), BS, AOCS

• NOFOTA - follows FOSFA, NEN (exceptional)

• GAFTA - own methods, originating from EU

7

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)

8

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

9

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

10

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

11

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)

12

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

13

Free Fatty Acids

14

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

15

Pesticide residues

16

Question

• Sample CPO from an incoming seagoing vessel arrives in the lab, without instructions

• Which analyses would you perform?

17

Answer

• Free Fatty Acids • Moisture and volatile matter • Impurities • Lauric acid (C12) • DOBI • Hydrocarbons

18

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

19

Question 2

• Sample of Ukrainian Sunflowerseed oil arrives without instructions

• Which analyses would you perform?

20

Answer 2

• Free Fatty Acids • Moisture and volatile matter • Insoluble impurities • Hydrocarbons • Linoleic / oleic acid ?

21

How about Argentinian Sunflower Seed Oil?

22

Acceptable results 2

• Hydrocarbons (mineral) (C10 - C56) max 50 mg/kg

23

Acceptable results

• Hydrocarbons (mineral) (C10-C40) max 300 mg/kg

24

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

25

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

32

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

33

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

34

35

Thanks for

your attention

36