Oilseeds — Determination of hexane extract (or light petroleum extract), called "oil content"

Graines oléagineuses — Détermination de l'extrait à l'hexane (ou à l'éther de pétrole), dit "teneur en huile"

General Information

Status
Withdrawn
Publication Date
31-Jul-1979
Withdrawal Date
31-Jul-1979
Current Stage
9599 - Withdrawal of International Standard
Completion Date
01-Feb-1988
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ISO 659:1979 - Oilseeds -- Determination of hexane extract (or light petroleum extract), called "oil content"
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International Standard 659
INTERNATIONAL ORGANIZATION FOR STANDARDlZATION*MEXLIYHAPOLIHAR OPrAHMBAUHR no CTAHLIAPTH3AUHH.OAGANlSATlON INTERNATIONALE DE NORMALISATION
Oilseeds - Determination of hexane extract (or light
petroleum extract), called "oil content"
L
Graines oléagineuses - Détermination de l'extrait a I'hexane iou a I'ether de pétrole), dit ((teneur en huile))
First edition - 1979-08-15
-.-
- UDC 665.3: 620.1 Ref. No. IS0 669-1979 (E)
e
Descriptors : oilseeds, chemical analysis, determination of content, oils, extraction analysis.
E
$!
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E Price based on 5 pages

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Foreword
IS0 (the International Organization for standardization) is a worldwide federation of
national standards institutes (IS0 member bodies). The work of developing Inter-
national Standards is carried out through IS0 technical committees. Every member
body interested in a subject for which a technical committee has been set up has the
right to be represented on that committee. International organizations, governmental
and non-governmental, in liaison with EO, also take part in the work.
Draft International Standards adopted by the technical committees are circulated to
the member bodies for approval before their acceptance as International Standards by
the IS0 Council.
International Standard IS0 659 was developed by Technical Committee ISO/TC 34,
Agricultural foodproducts, and was circulated to the member bodies in October 1977.
It has been approved by the member bodies of the following countries :
Australia India Portugal
Canada Iran Romania
South Africa, Rep. of
Chile Israel
Czechoslovakia Korea, Rep. of Thailand
Turkey
Egypt, Arab Rep. of Malaysia
Ethiopia Mexico United Kingdom
France Netherlands USSR
New Zealand Yugoslavia
Germany, F. R.
Hungary Poland
The member body of the following country expressed disapproval of the document on
technical grounds :
USA
This International Standard cancels and replaces IS0 Recommendation R 659-1968 of
which it constitutes a technical revision.
O International Organization for Standardization, 1979 O
Printed in Switzerland

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INTERNATIONAL STANDARD IS0 659-1979 (E)
Oilseeds - Determination of hexane extract (or light
petroleum extract), called "oil content"
1 Scope and field of application 5.2 Hydrochloric acid, concentrated, ez0 1,19 giml (only in
the case of cottonseed with adherent linters - see 8.1.4).
This International Standard specifies a reference method for
the determination of the hexane extract (or light petroleum ex-
tract), called "oil content", of oilseeds used as industrial raw
6 Apparatus
materials.
Usual laboratory apparatus and in particular
NOTE - If required, the following may be analysed separately
~
the pure seeds and the impurities (see 10.2);
6.1 Analytical balance.
~
in the case of groundnuts, the pure seeds, the total fines, the
non-oleaginous impurities and the oleaginous impurities.
6.2 Mechanical mill, easy to clean, appropriate to the
nature of the oilseeds and allowing the oilseeds to be ground
without heating or appreciable change in moisture, volatile
2 References
matter or oil content.
ISOi R 542, Oilseeds - Sampling.
Mechanical grater or, failing this, hand grater (only in
6.3
the case of copra - see 8.1.2).
IS0 664, Oilseeds - Reduction of contract samp._s to ana., sis
samples.
6.4 Mechanical micro-grinder (see 10.1). capable of pro-
IS0 665, Oilseeds - Determination of moisture and volatile
ducing a fineness of grinding of oilseeds of less than 160 pm,
matter content.
with the exception of the "shell", particles of which may reach
400 pm.
.- 3 Definition
6.5 Extraction thimble and cotton wool, free from matter
soluble in hexane or light petroleum.
hexane extract, called "oil content" : The whole of the
substances extracted under the operating conditions specified
below, and expressed as a percentage by mass of the product
6.6 Suitable extraction apparatus (fitted with a flask of
as received. On request, it may be expressed relative to the dry
capacity 200 to 250 ml).
matter.
NOTE - Several flasks are necessary (see 8.4)
4 Principle
Pumice stone, in small particles, previously dried in an
6.7
oven at 130 f 2 OC and cooled in a desiccator.
Extraction of a test portion in a suitable apparatus, with
technical hexane or, failing this, light petroleum. Elimination of
Electric heating bath (sand bath, water bath, etc.) or
the solvent and weighing of the extract obtained. 6.8
hot-plate.
5 Reagents
6.9 Electrically heated oven, with thermostatic control,
permitting ventilation or obtaining reduced pressure.
5.1 Technical n-hexane, or, failing this, light petroleum,
essentially composed of hydrocarbons with 6 carbon atoms, of
6.10 Desiccator, containing an efficient desiccant
which less than 5 YO distils below 50 OC and more than 95 YO
distils between 50 and 70 OC and which has a bromine value
less than 1. For either solvent, the residue on complete
6.11 In the case of cottonseed with adherent linters, the
evaporation shall not exceed 2 mg per 100 ml.
following are also required.
1

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IS0 659-1979 (E)
6.11.1 Electrically heated oven, capable of being main-
8.1.4 Cottonseed with adherent linters
tained at 130 f 2 OC.
Weigh, to the nearest 1 mg in the tared metal dish (6.11.3),
about 60 g of the analysis sample as received. Place the dish
6.11.2 Fumigation oven, with thermostatic control capable
and seeds in the oven (6.11.1 ), previously heated to 130 OC,
of heating a sample to 115 OC in 30 min.
and leave to dry for 2 h at 130 f 2 OC; then remove the dish
from the oven and allow to cool in air for about 30 min.
6.11.3 Metal dish, flat-bottomed, diameter 100 mm, height
Transfer the dried seeds to the porous ceramic vessel (6.1 1.4),
about 40 mm.
the inside walls and the base of which have been previously
moistened with 1,5 ml of the hydrochloric acid (5.2) by means
of the pipette (6.11.61, taking care that the acid is completely
6.11.4 Porous vessel, of ceramic material, cylindrical, inter-
absorbed without forming adherent drops. Cover the vessel
nal diameter 68 mm, external diameter 80 mm, height 85 mm,
with the watch glass (6.11.5) and place it in the fumigation
thickness of walls and base 6 mm.
oven (6.11.2). Heat so as to reach 115 OC in 30 min; do not heat
beyond this temperature and maintain it for another 30 min.
6.11.5 Watch glass, diameter 80 to 90 mm
Remove the vessel from the oven, allow to cool for 1 h in air,
6.11.6 Pipette, 2 ml, graduated in 0.1 ml.
reweigh the treated seeds to the nearest 1 mg, then grind the
seeds in the mechanical mill (6.2) and proceed as specified in
8.1.3.
8.1.5 Small seeds (linseed, colza, etc.)
7 Sampling
Carefully mix the analysis sample without previous mechanical
See ISO/R 542.
grinding.
8 Procedure
8.2 Test portion
8.1 Preparation of the test sample
8.2.1 The test portion shall be representative of the analysis
sample.
8.1.1 Reduction of sample
8.2.2 Weigh, to the nearest 1 mg, about 10 g of the test sam-
Take an analysis sample obtained in accordance with IS0 664.
p!" (see 8.1.2, 8.1.3, 8.1.4 or 8.1.5, as appropriate).
If large non-oleaginous foreign bodies have been separated
before the reduction of the laboratory sample, make allowance
NOTE - In the case of groundnuts, the test portion may comprise the
for this in the calculation (see 9.3.3). According to the re-
separated fractions of pure seeds, non-oleaginous and oleaginous im-
quirements of the contract, use an analysis sample as received
purities, and the total fines in quantities proportional to those of the dif-
or after separation of the impurities.
ferent constituents in the analysis sample itself.
8.1.2 Copra
8.2.3 In the case of copra and medium-sized seeds, including
cottonseed with adherent linters, transfer the test portion to
Grate the product by hand or, preferably, using a mechanical
the thimble (6.5) and plug the latter with a wad of cotton wool
grater (6.3) which allows the whole sample to be treated. When
(6.5).
grating by hand (a process which does not allow all the analysis
sample to be grated), endeavour to obtain a test sample which
8.2.4 In the case of small seeds, grind the test portion in the
is as representative as possible and, to this end, take account of
micro-grinder (6.4) or in the mill (6.21, taking care not to leave
the size and colour of different fragments.
any seeds intact. Transfer the ground seeds, without loss, to
the thimble (6.5), using a spatula. Wipe the bowl of the micro-
The length of the particles shall be close to 2 mm but shall not
grinder or mill and the spatula with a wad of cotton wool (6.5)
be greater than 5 mm. Mix the particles carefully and carry out
soaked with solvent (5.1), and plug the thimble with this wad.
the determination without delay.
8.1.3 Seeds of medium-size (sunflower, groundnut, soya,
etc.)
8.3 Predrying
Except in the case of cottonseed with adherent linters, grind
the analysis sample in the mechanical mill (6.2), which has If the test portion is very moist [moisture and volatile matter
content above 10 YO (rn/rn)l, leave the filled thimble for some
previously been well cleaned, until the major dimension of the
particles obtained is not greater than 2 mm. Reject the first par- time in an oven, maintained at a temperature not higher than
80 OC, to reduce the moisture and volatile matter content to
ticles (about one-twentieth of the sample), collect the rest, mix
carefully and carry out the determination without delay. less than 10 % (m/rn).
2

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IS0 659-1979 (E)
8.4 Determination If the mass of extract in flask B does not exceed 10 mg, the ex-
traction is completed. Otherwise, carry out a fresh extraction
...

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