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I NT ERN AT I ON AL
O RG A N lZATl ON FOR STAND AR D I2 AT1 O N
IS0 RECOMMENDATION
R 150
RAW, REFINED AND BOlLED LINSEED OIL
1st EDITION
COPYRIGHT RESERVED
The copyright of IS0 Recommendations and IS0 Standards
belongs to IS0 Member Bodies. Reproduction of these
documents, in any country, may be authorized therefore only
by the national standards organization of that country, being
a member of ISO.
For each individual country the only valid standard is the national standard of that country.
Printed in Switzerland
Also issued in French and Russian. Copies to be obtained through the national standards organizations.
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BRIEF HISTORY
The IS0 Recommendation R 150, Raw, Rejined and Boiled Linseed Oil, was drawn up
by Technical Committee ISO/TC 35, Paints, Varnishes and Related Products and their Raw
Materials, the Secretariat of which is held by the Nederlands Normalisatie-instituut ("1).
Work on this question by the Technical Committee began in 1950 and led, in 1958, to
the adoption of a Draft IS0 Recommendation.
In June 1958, this Draft IS0 Recommendation (No. 158) was circulated to all the IS0
Member Bodies for enquiry. It was approved, subject to a few modifications of an editorial
nature, by the following Member Bodies:
Austria Ireland Portugal
Burma Israel Republic of
South Africa
Chile Italy
Czechoslovakia Japan Romania
Denmark Mexico Spain
Sweden
Germany Net herlands
New Zealand U.S.A.
Greece
India Poland U.S.S.R.
Four Member Bodies opposed the approval of the Draft:
Belgium
Canada
France
United Kingdom
The Draft IS0 Recommendation was then submitted by correspondence to the IS0
Council, which decided, in February 1960, to accept it as an IS0 RECOMMENDATION.
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lSO/ R 150 - 1880 (E)
I SO Recom men dation R 150 February 1960
RAW, REFINED AND BOILED LINSEED OIL
1. SCOPE
This IS0 Recommendation establishes the more important requirements for raw, refined and
of test for these requirements.
boiled linseed oils and the methods
2. DEFINITIONS
O
2.1 Raw linseed oil. The oil obtained solely from mature seeds of linseed (Linum usitatissimum L.).
2.2 Refined linseed oil. The oil obtained by refining raw linseed oil as defined in clause 2.1.
2.3 Boiled linseed oil, The oil obtained from raw or refined linseed oil as defined in clause 2.1 or
2.2, by the incorporation of driers and by heating with or without blowing with air or
oxygen.
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ISO/ R 150 - I960 (E)
3. REQUIRED CHARACTERISTICS AND THEIR TOLERANCES
The raw, refined and boiled linseed oils should have the following characteristics :
Clause
describinl
Property Raw linseed oil
Re~ed linseed oil Boiled linseed oil
test
memod
0.926 to 0.933
0.926 to 0.933
0.928 to 0.950
5.,
(0.912 to 0.919)
(0.912 to 0.919) (0.914 to 0.936)
To be agreed To be agreed
Not darker than
Colour
/between purchaser between purchaser 5.2
test solution
and vendor and vendor
-
Clarity No sediment (a)
No sediment (2) 1 5.3
Refractive index (8) I-
1.4790 to 1.4840 1.4785 to 1.4825
nz
(1.4720 to 1.4770)
(1.4715 to 1.4755)
(n4,o)
Volatile matter,
0.20
0.10 0.20 1 5.5
max. %
Ash, max.
0.15 0.02 (4)
%
acid refined
Acid value, max. 4
8 (4) 1 5.7
g (6)
Saponification value 188 to 195 188 to 195 185 to 200 5.8
Unsaponifiable matter,
1.8 :l.5 2.0 5.9
max. %
I-
Iodine value, min.
175 175 - 5.10
(Wijs method) (7)
1 .O nil - 5.11
Foots, max. %
24 h at
15 to 20 "C
-
Drying time, max. or 5.12
18 h at
25 to 30 "C
Colophony negative test negative test 5.13
negative test
negative text I 5.14
Fish oil negative test negative test
Mineral acid - 1 5.15
negative test
(l) The figures between brackets are for use in countries with a tropical climate.
As factor of variation per degree C, O.OO0 68 is used.
(*) Stricter requirements may be agreed between purchaser and vendor. See also " Foots " and 5.11.
(*) The figures between brackets are for use in countries with a tropical climate.
As factor of variation per degree C, 0.000 35 is used.
Or to be agreed between purchaser and vendor.
(a) It is recommended that requirements for the ash content be agreed between purchaser and vendor.
The ash may contain metallic oxides.
(O) The value for alkali refined linseed oil to be agreed between purchaser and vendor.
(') Raw or refined linseed oil with an iodine value of over 190 should be designated " high iodine value linseed oil ".
If the Hanus method is used, it should be taken into account that this method can give different values from
those obtained by the Wijs method.
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lSO/ R 150 - I960 (E)
4. SAMPLING
See IS0 Recommendation R . , ., Sampling Raw Materials for Paints and Varnishes *.
5. TEST METHODS
5.1 Density
Refer to the Annex A, subject to the provision that IS0 recommends that densities, like
refractive indices, be quoted at 20 "C (and if necessary at 40 "C in countries with a tropical
climate).
5.2 Colour
Prepare a solution of 0.08 g of iodine and 0.8 g of pure potassium iodide (free from iodate)
in 100 ml of water. Compare the iodine solution with the oil in identical glass tubes, 1 cm
in diameter and about 10 cm long, by viewing them transversely by transmitted light.
5.3 Clarity
O
The oil is kept at a temperature of 15 to 20 "C for a period of 24 hours and then examined
for the presence of sediment and for other insoluble matter. See also 5.11, Foots.
5.4 Refractive index
Refer to the Annex A, subject to the provision that IS0 recommends taking the reading at
20 "C (and if necessary at 40 "C in countries with a tropical climate).
5.5 Volatile matter
Weigh about 10 g of oil (m g) with an accuracy of 1 mg into a 200 ml conical flask (diameter
of the bottom 73 mm, height 125 mm). Heat the flask for 30 min in an oil bath of 105 to
110 OC, drawing a dry inert gas over the surface of the oil at a rate of 10 litres per hour.
Remove the inert gas before weighing. (Loss of mass m, g.)
Calculate the percentage of volatile matter (V) with the formula :
v=- ml x 100
m
in which
O
m = mass, in grammes, of the sample
m, = loss of mass, in grammes.
5.6 Asb
5.7 Acid value Refer to the Annex A.
5.8 Saponification value
5 .!I Unsaponifiable matter
Refer to the Annex A.
The solvent to be used should be agreed upon between purchaser and vendor.
5.10 10- value
Refer to the Annex A.
* At present Second Draft IS0 Recommendation No. 731.
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lSO/ R 150 - 1980 (E)
5.11 Foots
5.11.1 Apparatus. The test is carried out in a cone-shaped or a pear-shaped sediment tube
(see Fig. 1 and 2 below).
5.11.2 Procedure. Place 100 ml of the oil in the tu6e and allow it to stand there in a vertical
position for 4 days (96 hours) at a temperature between 15 and 20 OC. During this
4 days (96 hours), read the
time, the tube should remain undisturbed. At the end of the
volume of sediments or foots at the bottom of the tube. Report that value as the per-
centage of foots, by volume.
Dimensions in millimetres
1
al/ 1.5.20
c
-m,,-
- 100-
0 39.5 max.
-
75
-50
- 25
a
- 20
8
I
-
15
\ q
-A
y
-2
O 9,640 int.
FIG. 2.- Cone-shaped sediment tube
FIG. 1 .- Pear-shaped sediment tube
5.12 Drying time
Spread two drops of oil (about 75 mg) with the finger evenly over the whole surface of a
glass panel, dimensions 9 cm x 12 cm.
Place the panel in diffuse daylight in a room at a temperature between 15 and 20 "C and at
a relative humidity between 60 and 70%.
The end of the drying time is when clean sand, graded so as to pass a sieve with a width of
aperture of 0.315 mm, but to be retained on a sieve with a width of aperture of 0.160 mm,
placed on the surface of the panel and allowed to remain there for a minute, can be removed
by means of a camel-hair brush without injury to the oil film.
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ISO/ R 150 - 1960 (E)
5.13 Liebermam-Storch-Morawski test for presence of colophony
Mix 3 to 5 drops of the oil with 3 ml of acetic anhydride. Add 1 drop of sulphuric acid
(d = 1.54). The reaction for colophony is positive if a fugitive violet colour appears which,
at the moment of its maximum intensity, is stronger than the colour of potassium per-
manganate solution 0.001 N.
5 14 Test for presence of fish oil
5.14.1 Reagents
5.14.1.1 Acetic acid, glacial.
5.14.1.2 Nitric acid 4 N.
5.14.1.3 Hydrochloric acid 1 N.
5.14.1.4 Ethanolic potassium hydroxide solution 1 N.
5.14.1.5 Mixture of equal volumes of acetic acid and chloroform.
5.14.1.6 Bromine, analytical grade.
5.14.1.7 Chloroform.
5.14.1.8 Light petroleum (boiling range 40 to 60 OC).
5.14.1.9 Diethyl ether, d = 0.712 to 0.716, the residue of non-volatile matter at 80 OC not
exceeding 0.001 %.
5.14.2 Procedure
Saponify 5 g of linseed oil, as in the determination of unsaponifiable matter (see clause
5.9), using 50 ml of the ethanolic potassium hydroxide solution and boiling under reflux
for one hour, with swirling at intervals.
Remove the flask from the condenser and evaporate the contents to a syrupy paste on
a water or steam bath.
To ensure removal of ethanol, add 10 ml of water and again evaporate, almost to
dryness.
Dissolve the soap in about 100 ml of boiling distilled water and transfer to a separating
funnel. Add an excess of hydrochloric acid and shake vigorously to decompose the soap.
Cool and add about 200 ml of light petroleum. Shake well and allow to stand for several
hours. Run off the acid layer. Filter the light petroleum layer through a fast-filtering,
fat-free paper, pouring the liquid from the top of the separating funnel. Wash the filtered
solution with 10 ml of nitric acid. Allow to settle, run off the acid layer and wash several
times with distilled water. Repeat the acid and subsequent water washes until no trace
of metal is present. Evaporate the light petroleum and carefully dry the residual fatty
acids.
Take 1.5 ml of the residual fatty acids and dissolve in 40 ml of diethyl ether and 5 ml
of glacial acetic acid in a 25 mm x 150 mm test tube. Cool the solution in an ice-
water bath to O OC.
Add bromine drop by drop, keeping the temperature at O OC, until an excess, as indicated
by the colour, is present. Allow to stand at O OC, preferably overnight. Decant the
supernatant diethyl ether-bromine mixture and wash the precipitated polybromides
until they are free from bromine into a filter paper with diethyl ether previously cooled
to about O "C. Allow the ether to evaporate from the bromides.
Take 0.1 to 0.2 g of the dry bromides thus prepared and add acetic acid-chloroform
mixture in the proportion of 1.5 ml of mixture to 0.1 g of bromides and boil.
Vegetable oils give a clear solution. When 1 % of fish or marine animal oil is present,
the solution does not become bright; when 5 % is present, the mixture is quite cloudy.
5.15 Test for presence of mineral acid
Shake 10 nll of refined linseed oil with 25 ml of distilled water. Take off the aqueous layer
and add a few drops of litmus solution.
In the presence of mineral acid the colour turns to red.
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I
lSO/ R 150 - I960 (E)
ANNEX A
ANNEX A
(prepared in 1966)
Extracts from the publications of the
INTERNATIONAL UNION OF PURE AND APPLIED CHEMISTRY
(IUPAC)
Standard methods of the
O
OILS AND FATS SECTION (OFS)
and
ORGANIC COATJNGS SECTION (OCS)
A.l Density (from OFS, 4th edition) . page 10
A. 2 Refractive index (from OFS, 5th edition) . page 11
A.3 Ash content (from OFS, 5th edition) . page 12
A.4 Acid value (from OCS, 1st edition) . page 13
A.5 Saponification value (from OCS, 1st edition) . page 14
A.6 Unsaponifiable matter (from OCS, 1st edition) . page 15
O
A.7 Iodine value (Wijs) (from OCS, 1st edition) . page 18
is expressly forbidden unless explicit reference to the origin is stated.
Reproduction of these texts
Reproduction authorized by the IUPAC.
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ISO/ R 150 - 1960 (E)
ANNEX A
A. 1 DENSITY
A. 1.1 General
In view of the confusion which may be caused by the terms density and specific mass in the dif-
ferent countries, and sometimes even in one country, the term density at t OC is defined as the
absolute density, that is to say, the mass of unit volume, expressed in grammes per millilitre at the
temperature indicated t. This quantity is indicated by the symbol pt.
To within 0.000 027, that is to say, within a degree of approximation closer than that obtained in
ordinarily accurate measurements, this quantity will correspond with the density in relation to
water at 4 OC: pp.
The exact determination of the temperature t is of considerable importance since the density of
the fat varies by about 0.000 68 per degree C.
Densities, like refractive indices, shall be determined on the dried and filtered fat and shall be
quoted at 20 OC (and if necessary at 40 OC, 60 OC, or other temperatures, if the substance does not
have a well defined state at 20 OC).
The observations may be made at a temperature il, approximating to the standard temperature t,
and be corrected to the latter temperature by means of the equation:
pt=ph+(tl-t) X O.OO0 68
A. 1.2 Procedure
The density bottle, having reached the constant temperature of the surrounding medium, is filled
to the upper edge of the capillary tube. After the thermometer has been inserted, the density bottle
is weighed, the temperature being noted.
The density at t "C (pt) is then calculated by the following formula:
c-a
pt = --
A
b-a
in which a = weight of empty density bottle,
b = weight of density bottle plus water at t OC,
c = weight of density bottle plus oil at t "C,
d = density of water at t "C (to be ascertained from tables).
air
The approximat value of pt determined as above may now be corrected for the effect of th
pressure by means of the following formula :
if
(pt) is the corrected value and 0.0012 the density of air
then (pt) = pt + 0.0012 (1 - pt).
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lSO/ R 150 - I960 (E)
ANNEX A
A.2 REFRACTIVE INDEX
A.2.1 Foreword
The refractive index of a medium is the ratio of the speed of light in vacuo to its speed in the
medium. It is measured by the ratio of the sine of the angle of incidence to the sine of the angle
of refraction when a ray of light passes from air into the oil or fat. In general, the refractive index
of a given substance varies with the wave length of the refracted light and with the temperature.
Unless otherwise specified, the refractive index is reported for the mean wave length of the
D lines of sodium.
The notation nt always denotes the index relative to the D line at t OC.
For a light of wave length x at t OC, the notation is n:.
In the case of refractometers in common use, the observation is made in white light but is cor-
rected to sodium light by a compensating device in the instrument.
In general, the refractive index is given
O
at t = 20 OC for fats which are liquid at this temperature;
at t = 40 OC, 60 OC, 80 OC or above for fats which are solid at a temperature of 20 OC.
The temperature of observation tl must be accurately known and should not differ from the
selected temperature by more than f 2 OC.
A.2.2 Apparatus
A precision refractometer having a prism heated by means of a thermostatically controlled
circulating liquid. An instrument reading only in arbitrary units is not regarded as suitable.
A.2.3 Measurement
The space between the two prisms must be completely filled with the fat.
5 minutes.
The reading is taken after the temperature has remained constant for not less than
Note the temperature, say tp
O
A.2.4 Calculation
If t, is different from t, the correction factor Fis a function of the temperature:
F = O.OO0 35 for temperatures around 20 OC.
F = 0.000 36 for a temperature of 40 OC and above.
We have then
nt = ne1 + (t, - t)F when tl > t
nt = nt1 - (t - t3P when tl < t
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BO/ R 110 - I960 (E)
ANNEX A
A.3 ASH CONTENT
A.3.1 Foreword
The ash content is the percentage of mineral matter found in oils and fats which have been
filtered.
In order to avoid the inclusion of certain elements twice the ash content should not be added to
that of the impurities insoluble in a solvent.
On the other hand, the ash can be determined on the purified matter when the determination is
being made after that of the impurities.
A.3.2 Apparatus
A 50 ml crucible.
A. 3.3 Procedure
O
Weigh about 10 g of the fatty material to within 0.01 g in the previously tared crucible.
Heat gently to point of ignition and allow to burn spontaneously. Ignite until a carbon residue is
obtained which no longer emits a vapour.
Take up the residue with distilled water. Filter through an ashless filter paper. Keep the filtrate.
Ignite the filter completely, if necessary with the help of a gentle stream of oxygen or a few drops
of hydrogen peroxide.
Allow the crucible to cool.
Pour the filtrate quantitatively into it. Evaporate to dryness over a water-bath. Then ignite for a
few moments at about 400 OC.
Finally recarbonate the ash with ammonium carbonate or water saturated with carbon dioxide.
A.3.4 Calculation
lOOa
Ash content = -- per cent
O
P
a = weight of ash in grammes
where
p = weight of sample in grammes.
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ISO/ R 150 - I960 (E)
ANNEX A
A.4 ACID VALUE *
A. 4.1 Definition
The acid value is defined as the number of milligrammes of potassium hydroxide required -J
neutralize 1 g of the sample under the conditions specified below.
A.4.2 Reagents required
Standard potassium hydroxide solution (0.1 N) in ethanol (95% v/v). This solution must be
colourless or not darker than straw yellow. Methanol may be used instead of ethanol (95 % v/v).
1 % v/v of phenolphthalein in ethanol (95% v/v). Other indicators with a
...