SAMPLING METHODS

OILS, FATS, TECHNICAL TALLOWS, GREASES AND ACID OILS

Sampling ISO 5555:2001

Preparation of laboratory samples ISO 5555:2001 Section 6.9

Labelling of laboratory samples ISO 5555:2001 Section 7.2

Preparation of test sample ISO 661:2003

Packaging and storage of oils and fats samples FOSFA International Official Method

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 FOSFA INTERNATIONAL OFFICIAL METHOD
PACKAGING AND STORAGE OF OILS AND FATS SAMPLES

1 Scope
This FOSFA method for the labelling, packaging, transport and storage of samples is applicable to all
samples drawn under the terms of FOSFA International contracts for analysis, arbitration or standards
purposes.

2 Label design
2.1 Labels must comply with ISO 5555:2001 Section 7.2.

2.2 Labels should be completed in legible handwriting, preferably in capital letters, or typed. Labels
should be securely attached to the samples they represent.

3 Sample labelling, sealing and distribution

The label is to be affixed to the sample bottle and sealed to the bottle (jointly where appropriate) and
to clearly indicate the appropriate FOSFA International contract number.

Sealing wax, if used, should not contain copper. If a sealing wax does contain copper or the
composition is unknown, the sample container shall be placed in a tight-fitting plastic bag and labelled
and sealed therein.

Samples shall be distributed in accordance with the relevant FOSFA International contract
requirements.

4 Packaging of oils and fats samples for analysis

The samples shall be packed in accordance with ISO 5555:2001. For contractual analysis a sample
of 250 ml is sufficient. Where special analyses are needed, a sample of 500 ml or more will be
required.

5 Storage of samples after analysis

Samples should be clearly marked and stored with an in-house reference number in cool, dry
conditions, away from strong light. The sample area should be insect and rodent free and hygienic. In
normal circumstances, it has been the experience that contractual samples should be stored for a
minimum of three months and longer if circumstances so dictate.

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 FULL ANALYST MEMBERS

Mandatory Contractual Analysis Methods: Oils, Fats, Technical Tallows and

Greases (except Acid Oils, Palm and Palm Kernel Oil Products traded on FOSFA Contract No 81)
The tests shown below are mandatory for all Full Analyst Members in the Oils and Fats Section.

TEST METHOD OF
DETERMINATION
NO ANALYSIS

1 Determination of Lovibond colour ISO 15305:1998

2 Flashpoint limit test using Pensky-Martens closed cup flash tester ISO 15267:1998

3 Determination of free fatty acid content ISO 660:2009

4 Determination of insoluble impurities content ISO 663:2007

5 Determination of iodine value ISO 3961:2009

6 Determination of conventional mass per volume (litre weight in air) ISO 6883:2007

7 Determination of melting point in open capillary tubes (slip point) ISO 6321:2002

8 Determination of moisture and volatile matter content ISO 662:1998

9 Determination of peroxide value ─ Iodometric (visual) endpoint ISO 3960:2007

determination

10 Determination of acid value and acidity ISO 660:2009

11 Determination of ash ISO 6884:2008

12 Determination of carotene in vegetable oils BS 684-2.20:1977

13 Cold Test AOCS Cc 11-53

2009
14 Determination of sea water contamination in oils FOSFA
Method:2010
15 Determination of copper. Colorimetric method (Reference method) BS 684-2.16:1976

16 Determination of erucic acid content (Total C22 monoenes) ISO 5508:1990

17 Determination of visible foots in crude fats and oils ISO 19219:2002

18 Preparation of methyl esters of fatty acids ISO 5509:2000

19 Analysis by gas chromatography of methyl esters of fatty acids ISO 5508:1990

20 Determination of iron. Colorimetric method (Reference method) BS 684-2.17:1976

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 21 Determination of Chlorophyll Pigments in Crude Vegetable Oils AOCS Cc 13i-96
2009
22 Determination of phosphorus content ─ Part 1: Colorimetric method ISO 10540-1:2003
(Reference method)

23 Determination of refractive index ISO 6320:2000/

Cor 1:2006
24 Determination of saponification value ISO 3657:2002

25 Determination of alkalinity ISO 10539:2002

26 Determination of ultraviolet absorbance expressed as specific UV ISO 3656:2002

extinction

27 Calculation of total fatty matter BS 684-2.4:1976

28 Determination of unsaponifiable matter ─ Method using diethyl ether ISO 3596:2000

extraction (Reference method)

29 Determination of water content ─ Entrainment method ISO 934:1980

30 Determination of water content ─ Karl Fischer method (pyridine free) ISO 8534:2008

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 FULL ANALYST MEMBERS

Optional Contractual Analysis Methods: Oils, Fats, Technical Tallows and

Greases (except Acid Oils, Palm and Palm Kernel Oil Products traded on FOSFA Contract No 81)
The tests shown below are optional for all Full Analyst Members in the Oils and Fats Section.

TEST METHOD OF
DETERMINATION
NO ANALYSIS

31 Determination of bleachability a. General Case BS 684-2.27:1987

32 Determination of bleachability b. Bleach Test for Palm Oil BS 684-2.27:1987

33 Determination of cadmium content by direct graphite furnace atomic ISO 15774:2000

absorption spectrometry

34 Determination of cloud point BS 684-1.5:1987/

Amd:1989
35 Color - FAC Standard Color AOCS Cc 13a-43 2009

36 Color - Wesson Method Using Color Glasses Calibrated in AOCS Cc 13b-45 2009
Accordance with the AOCS-Tintometer Color Scale

37 Color - Gardner 1963 (Glass Standards) AOCS Td 1a-64 2009

38 Determination of copper, iron and nickel contents ─ Graphite ISO 8294:1994

furnace atomic absorption method

39 Evaluation of technical tallows and animal greases BS 3919:1987/

Amd:1989
40 Determination of oxidized fatty acids BS 684-2.12:1984

41 Determination of oxidative stability (accelerated oxidation test) ISO 6886:2006

Rancimat or equivalent

42 Determination of phosphorus content ─ Part 2: Method using ISO 10540-2:2003

graphite furnace atomic absorption spectrometry

43 Determination of phosphorus content ─ Part 3: Method using ISO 10540-3:2002

inductively coupled plasma (ICP) optical emission spectroscopy

44 Determination of content of polar compounds ISO 8420:2002/

Cor 1:2004
45 Phosphoric acid test ISO 150:2006

46 Determination of polyethylene-type polymers ISO 6656:2002

47 Refined and Bleached Colour AOCS Cc 8d-55 2009

48 Determination of smoke point BS 684-1.8:1976

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 49 Determination of solid fat content by pulsed NMR ─ Part 1: Direct ISO 8292-1:2008
method

50 Determination of solid fat content by pulsed NMR ─ Part 2: Indirect ISO 8292-2:2008
method

51 Determination of individual and total sterols contents ─ Gas ISO 12228:1999

chromatographic method

52 Determination of titre ISO 935:1988

53 Determination of lead by direct graphite furnace atomic absorption ISO 12193:2004

spectroscopy

54 Determination of unsaponifiable matter ─ Method using hexane ISO 18609:2000

extraction (for Sheanut Oil only)

55 Determination of sediment in crude fats and oils ─ Centrifuge ISO 15301:2001/

method Cor 1:2007

56 Determination of benzo[a]pyrene ─ Reverse-phase high ISO 15302:2007

performance liquid chromatography method

57 Determination of the deterioration of bleachability index (DOBI) ISO 17932:2005

58 Determination of anisidine value ISO 6885:2006

59 Determination of the composition of fatty acids in the 2-position of ISO 6800:1997

the triglyceride molecules

60 Determination of residual technical hexane content ISO 9832:2002

61 Determination of mineral acidity BS 684-2.48:1998

62 Determination of water-insoluble solvents BS 684-1.9:1976

63 Detection and identification of a volatile organic contaminant by ISO 15303:2001

GC/MS

64 Determination of stigmastadienes in vegetable oils ─ Part 1: Method ISO 15788-1:1999

using capillary-column gas chromatography (Reference method)

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 ASSOCIATE ANALYST MEMBERS

Mandatory Contractual Analysis Methods: Oils, Fats, Technical Tallows and

Greases (except Acid Oils, Palm and Palm Kernel Oil Products traded on FOSFA Contract No 81)
The tests shown below are mandatory for all Associate Analyst Members in the Oils and Fats Section.

TEST METHOD OF
DETERMINATION
NO ANALYSIS

1 Determination of Lovibond colour ISO 15305:1998

2 Flashpoint limit test using Pensky-Martens closed cup flash tester ISO 15267:1998

3 Determination of free fatty acid content ISO 660:2009

4 Determination of insoluble impurities content ISO 663:2007

5 Determination of iodine value ISO 3961:2009

6 Determination of conventional mass per volume (litre weight in air) ISO 6883:2007

7 Determination of melting point in open capillary tubes (slip point) ISO 6321:2002

8 Determination of moisture and volatile matter content ISO 662:1998

9 Determination of peroxide value ─ Iodometric (visual) endpoint ISO 3960:2007

determination

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 ANALYSIS METHODS

ACID OILS

TEST
DETERMINATION METHOD OF ANALYSIS
NO

1 Determination of ash ISO 6884:2008

2 Determination of insoluble impurities content ISO 663:2007

3 Determination of iodine value ISO 3961:2009

4 Determination of mineral acidity BS 684-2.48:1998

5 Determination of soap content FOSFA Method:2010

6 Determination of unsaponifiable matter ─ Method ISO 3596:2000

using diethyl ether extraction (Reference method)

7 Determination of water content ─ Entrainment method ISO 934:1980

8 Determination of water content ─ Karl Fischer method ISO 8534:2008

(pyridine free)

9 Determination of free fatty acid content ISO 660:2009

10 Total saponifiable matter shall be equivalent to: Determined by the Standard

Contractual Methods as per this List
100 – (W + I + U + S)

where:

W is water content
I is insoluble impurities
U is unsaponifiable matter
S = soap content

11 Total fatty matter shall be equivalent to: Determined by the Standard

Contractual Methods as per this List
100 – (W + A + I)

where:

W is water content
A is ash
I is insoluble impurities

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 FOSFA INTERNATIONAL/PORAM STANDARD
CONTRACTUAL METHODS LIST

PALM OIL AND PALM KERNEL OIL PRODUCTS IN BULK CIF

FOR USE WITH FOSFA INTERNATIONAL CONTRACT NO 81

DETERMINATION METHODS OF ANALYSIS

FFA % (as Palmitic for palm oil products and as Lauric for palm ISO 660:2009
kernel oil products) AOCS Ca 5a-40 2009
MPOB Method p2.5:2004

Moisture and Volatile Matter ISO 662:1998

(Palm Oil/Palm Stearin/Palm Olein) AOCS Ca 2c-25 2009
MPOB Method p2.1:2004

Moisture and Volatile Matter ISO 662:1998

(Processed Palm Kernel Oil products) AOCS Ca 2c-25 2009
MPOB Method k1.4:2004

Iodine Value (Wijs) ISO 3961:2009

AOCS Cd 1d-92 2009
MPOB Method p3.2:2004

Insoluble Impurities ISO 663:2007

(Warm solvent may be used)
AOCS Ca 3a-46 2009
MPOB Method p2.2:2004

Colour ISO 15305:1998

AOCS Cc 13e-92 2009
(Without the use of black
sheath)
MPOB Method p4.1:2004

Melting Point (Slip Point) ISO 6321:2002

AOCS Cc 3-25 2009
MPOB Method p4.2:2004

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 FOSFA INTERNATIONAL/PORAM STANDARD
CONTRACTUAL METHODS LIST

PALM ACID OIL/PFAD/FLAKED STEARIC ACID

DETERMINATION METHODS OF ANALYSIS

Free Fatty Acid (FFA) (as Palmitic) AOCS Ca 5a-40 2009

MPOB Method p2.5:2004

Saponification Value AOCS Cd 3-25 2009

Moisture and Volatile Matter AOCS Ca 2b-38 2009

AOCS Ca 2c-25 2009
MPOB Method p2.1:2004

Unsaponifiable Matter AOCS Ca 6a-40 2009

Total Fatty Matter 100 - (M + I ) *

Saponifiable Matter 100 - (M + I + U) *

Soap FOSFA Method 2010

Impurities ISO 663:2007

MPOB Method p2.2:2004

*Where:

M is Moisture as per AOCS Ca 2b-38 2009

I is Impurities as per ISO 663:2007/MPOB Method p2.2:2004

U is Unsaponifiable Matter as per AOCS Ca 6a-40 2009

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 FOSFA INTERNATIONAL OFFICIAL METHOD
DETERMINATION OF SEA WATER CONTAMINATION IN OILS

1 Scope
The method is applicable to all oils, with the exception of those (such as acid oils) which are known to
have been treated with hydrochloric acid.

2 Principle
The oil is examined for the presence of chloride ions in the aqueous contaminant. If chloride ions are
detected and the amount of aqueous phase permits, quantitative determinations of chloride and other
ions may be carried out.

3 References
3.1 Official, Standardised and Recommended Methods of Analysis. The Society for Analytical
Chemistry, London, 1973.

3.2 Analysis of Raw, Potable and Waste Waters. HMSO, 1972.

3.3 Methods for the examination of Water and Associated Materials. The National Water Council,
Department of the Environment.

3.4 Official Methods of Analysis of the Association of Official Analytical Chemists. 13th edition,
Washington, 1980.

4 Reagents
4.1 Silver nitrate solution, approximately 0.1 M.

4.2 Nitric acid, concentrated, AR.

5 Procedure
5.1 Sample preparation

5.1.1 If the nature of the sample permits, separate the aqueous and oil components by
centrifugation, or by allowing the sample to stand. Determine the volume of aqueous contaminant in
the oil.

5.1.2 If the amount of the contaminant is small, extract it by shaking the oil with water. Dilution of the
oil with petroleum ether may assist the separation of the aqueous layer. If this procedure is
unsatisfactory the oil should ashed at a temperature of not more than 450C and the tests carried out
on an aqueous solution of the ash.

5.2 Qualitative test

Acidify a portion of the aqueous phase with a few drops of concentrated nitric acid, and add a few
drops of silver nitrate solution. A white precipitate which darkens upon exposure to light, especially
sunlight, (or turbidity if the sample solution is very dilute) indicates the presence of chloride and
suggests that the sample may have been contaminated with sea water.

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6 Further examination
If a more detailed examination of the aqueous contaminant is required, quantitative determination of
chloride and sodium should first be carried out. Determinations of other major constituents of sea
water, such as sulphate, magnesium, potassium and calcium may then be carried out as further
confirmatory tests.

The principal inorganic constituents of typical sea water are:

% m/m
Chloride 1.90
Sodium (as Na) 1.06
Sulphate 0.26
Magnesium (as Mg) 0.13
Calcium (as Ca) 0.04
Potassium (as K) 0.01
Bicarbonate 0.01
Bromide 0.007

The methods of analysis will depend on the quantity of the aqueous contaminant available. Some
sources of suitable analytical methods are given in Section 3 (References).

7 Test report
The Analyst's report shall indicate the method(s) of analysis employed.

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 FOSFA INTERNATIONAL OFFICIAL METHOD
DETERMINATION OF SOAP IN ACID OILS

1 Scope
A non-aqueous titration method is described for the determination of soap in all types of acid oils.

2 Definition
The soap content is expressed as sodium oleate as a percentage by mass calculated from the total
alkalinity of the oil.

3 Principle
The total alkalinity is determined by titration in neutral solvent solution of the oil using standard
ethanolic hydrochloric acid and bromophenol blue indicator solution. For dark coloured and/or very
low expected soap contents (less than 0.01 % by mass) the end-point is measured electrometrically.

4 Reagents
Use only reagents of recognised analytical quality.

4.1 Ethanolic hydrochloric acid solution 0.01N and/or 0.1N accurately standardised.

4.2 Bromophenol blue indicator. Solution of 49 g per litre of 95 % (m/m) ethanol.

4.3 Solvent mixture. 1 volume ethanol/2 volumes acetone neutralised by adding a few drops of
indicator solution (4.2) and titrating with hydrochloric acid solution (4.1) or with ethanolic potassium
hydroxide solution until just yellow.

5 Apparatus
Use laboratory apparatus and in particular the following.

5.1 Burette 10 ml graduated in 0.02 ml.

5.2 pH meter fitted with automatic temperature compensation and equipped with a suitable electrode
system. The electrode assembly should be washed with neutral solvent (4.3) before use.

NOTE It is essential that the pH equipment be very carefully checked for both repeatability and
reproducibility at the required operational temperatures. Some equipment has been found to give
variations in excess of 0.6 pH units in day-to-say measurements on the same solvent mixture and to
require several minutes to give a constant reading after agitation has ceased.

5.3 pH electrode suitable for work in non-aqueous solvent mixture is recommended.

5.4 Suitable means of heating the solvent mixture and oil solution such as a water bath
thermostatically controlled at about 46C.

5.5 Conical Erlenmeyer flasks (250 ml) having no alkaline reaction.

6 Preparation of sample
Melt the oil sample and mix thoroughly.

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7 Procedure
7.1 Oils which yield a clear colourless solution in the solvent mixture (4.3)

7.1.1 Test solution

Accurately weigh a suitable mass of sample (6) directly into a 250 ml conical (Erlenmeyer) flask then
add 100 ml of solvent mixture (4.3) and dissolve at 40C to 45C.

7.1.2 Titration

Add a few drops of indicator solution (4.2). The formation of a green colour indicates the presence of
soap. Titrate the test solution (7.1.1) with ethanolic hydrochloric acid (4.1) until the solution is just
yellow at its initial temperature (40C to 45C). Allow adequate time (5 min) for reaction of calcium
soaps etc.

7.2 Oils which yield a dark solution in the solvent mixture (4.3) and/or are expected to have a
very low (less than 0.01 % by mass) soap content

7.2.1 pH of solvent mixture

Warm 100 ml solvent mixture (4.3) to 40C to 45C, Measure the temperature accurately and adjust
the pH meter (5.2) for operation at this temperature and measure the pH. Determine end-point by
reference to a calibration curve.

NOTE Choose the vessel to contain the solvent mixture which will subsequently permit the insertion
of the pH electrodes (5), such as a beaker or wide-necked conical flask.

8 Expression of results
8.1 Method of calculation

Calculate the soap content, expressed as a percentage (mass/mass) of sodium oleate in the original
sample (6) from the formula.

% Soap content = V x N x 30.4

(as sodium oleate) W

Where:

V is volume in ml of ethanolic hydrochloric acid used (7.1.2 or 7.2.2) to reach equivalence

N is normality of ethanolic hydrochloric acid (4.1)
W is mass of sample used to prepare test solution (7.1.1 or 7.2.2)

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 DETERMINATION OF SOAP IN ACID OILS

Figure 1: Curve of change in scale reading per unit volume of acid added against volume of acid
added and from this measure the equivalence volume corresponding to the curve maximum.

700

600

500

400

300

200

100

0
0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 1.9 1.95 2.0 2.1 2.4 2.6 2.8 3.1 3.2

Volume of HCL (ml)

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