INTERNATIONAL ISO

STANDARD 12205
First edition
1995-02-01

Petroleum products - Determination of

the Oxidation stability of middle-distillate
fuels
iTeh STANDARD PREVIEW
(standards.iteh.ai)
Produits pktroliers - Dktermina tion de Ia stabilite a Ioxyda tion des
dis tilla ts moyens de p6 trole
ISO 12205:1995
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564b3686d720/iso-12205-1995

Reference number
ISO 12205:1995(E)
 ISO 12205:1995(E)

Foreword
ISO (the International Organization for Standardization) is a worldwide
federation of national Standards bodies (ISO member bodies). The work
of preparing International Standards is normally carried out through ISO
technical committees. Esch member body interested in a subject for
which a technical committee has been established has the right to be
represented on that committee. International organizations, governmental
and non-governmental, in liaison with ISO, also take part in the work. ISO
collaborates closely with the International Electrotechnical Commission
(IEC) on all matters of electrotechnical standardization.

Draft International Standards adopted by the technical committees are

circulated to the member bodies for voting. Publication as an International
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Standard requires approval by at least 75 % of the member bodies casting
a vote.

International Standard ISO

(standards.iteh.ai)
12205 was prepared by Technical Committee
lSO/TC 28, Petroleum products and lubricants.
ISO 12205:1995
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Annex A of this International Standard is for information only.
564b3686d720/iso-12205-1995

0 ISO 1995
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced
or utilized in any form or by any means, electronie or mechan ical, including photocopying and
microfilm, witho ut Permission in writing from the Pu blisher.
Internationa I Organization for Standardization
Case Pastal e 56 l CH-121 1 Geneve 20 l Switz erland
Printed in Switzerland

ii
INTERNATIONAL STANDARD 0 ISO ISO 12205:1995(E)

Petroleum products - Determination of the Oxidation

stability of middle-distillate fuels

WARNING - The use of this International Standard may involve hazardous materials, operations
and equipment. This Standard does not purport to address all of the safety Problems associated
with its use. lt is the responsibility of the User of this Standard to establish appropriate safety and
health practices and determine the applicability of regulatory limitations Prior to use.

1 Scope are subject to revision, and Parties to agreements

based on this International Standard are encouraged
iTeh STANDARD PREVIEW
This International Standard describes a procedure for to investigate the possibility of applying the most re-
cent editions of the Standards indicated below.
the measurement of inherent stability of middle-
(standards.iteh.ai)
distillate Petroleum fuels under accelerated oxidizing Members of IEC and ISO maintain registers of cur-
rently valid International Standards.
conditions. lt is not applicable to fuels containing re-
sidual components, or any significant component
ISO 12205:1995
from a non-Petroleum Source. ISO 3170:1988, Petroleum
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sampling.
564b3686d720/iso-12205-1995
The method provides a basis for the estimation of the
storage stability, under the conditions of this test, of ISO 3171 :1988, Petroleum liquids - Automatic pipe-
middle-distillate fuels with an initial boiling Point above line sampling.
approximately 175 “C and a 90% (WV) recovery Point
below 370 “C. ISO 3696: 1987, Wa ter for analytical laboratory use -
Specification and test methods.
The method may not provide a prediction of the
quantity of insolubles that will form in field storage ISO 6246: -‘1, Petroleum products - Gum content
over any given period of time. The amount of such of light and middle distillate fuels - Jet evaporation
insolubles is subject to the specific conditions, which me thod.
are too variable for this test method to predict accu-
rately. ISO 6353-2:1983 and Addendum 2:1986, Reagents
for Chemical analysis - Part 2: Specifica tions - First
NOTE 1 Oxidation is a Chemical process causing adher- series.
ent and filterable insolubles to form. Any substance such
as topper or chromium that catalyses Oxidation reactions
will Cause greater quantities of insolubles to form. 3 Definitions
For the purposes of this International Standard, the
2 Normative references following definitions apply.

The following Standards contain provisions which, 3.1 adherent insolubles: Material, produced in the
through reference in this text, constitute provisions course of stressing middle-distillate fuel under the
of this International Standard. At the time sf publi- conditions of this test, that adheres to the glassware
cation, the editions indicated were valid. All Standards after the fuel has been flushed from the System.

1) To be published. (Revision of ISO 6246:1981)

 ISO 12205:1995(E) 0 ISO

3.2 filterable insolubles: Material, produced in the 5.5 2,2,4=trimethylpentane (iso-octane),

course of stressing middle-distillate fuel under the CH,C(CH,),CH,CH(CH,)CH,, of minimum purity
conditions of this test, that is capable of being re- 99,5 %.
moved from the fuel by filtration. This includes both
material suspended in the fuel and material removed 5.6 Oxygen, minimum purity 99,5 %.
easily from the Oxidation cell and Oxygen delivery tube
with hydrocarbon solvent. When Oxygen is delivered through a plant System of
piping, a filter shall be provided adjacent to the heat-
3.3 inherent stability: Resistance to Change when ing bath (6.2). Control the Oxygen supply by an ap-
exposed to air, but in the absence of other environ- propriate regulation System.
mental factors such as water, or reactive metallic
surfaces or dir-t. 6 Apparatus
3.4 total insolubles: Sum of adherent and filterable All measuring apparatus shall be calibrated, verified
insolubles. and periodically monitored for Performance, as appro-
priate and according to manufacturer’s instructions, to
3.5 zero time: Time at which the first Oxidation cell assure consistency of results.
is placed in the heating bath.
6.1 Oxidation cell, of borosilicate glass as shown in
4 Principle figure 1, consisting of a test tube, condenser and
Oxygen delivery tube.
A test Portion of filtered middle-distillate fuel is aged
at 95 “C for 16 h while bubbling Oxygen through the Since the apparatus used in this test tan also be used
Sample. After ageing, the Sample is cooled to ap- in ISO 4263 (see annex A), where coils of topper and
proximately room temperature iTeh STANDARD PREVIEW
before filtering to ob- steel are used, ensure that any residue that could
tain the quantity of filterable insolubles. Adherent contain these metals is eliminated from the apparatus
(standards.iteh.ai)
insolubles are then removed from the Oxidation cell by thorough cleaning Prior to use.
and associated glassware with trisolvent. The
To preclude the presence of chromium ions, as well
trisolvent is evaporated to obtain the quantity of ad-ISO 12205:1995
as to protect laboratory personnel from potential
herent insolubles. The sum ofhttps://standards.iteh.ai/catalog/standards/sist/f8898a24-6ac1-4108-a3e7-
the filterable and ad-
harm, chromosulfuric acid shall not be used for
herent insolubles is reported as total insolubles. 564b3686d720/iso-12205-1995
cleaning glassware in the practice of this method.

5 Reagents and materials 6.2 Heating bath, containing a liquid medium

whose temperature is thermostatically controlled to
Reagent grade solvents, conforming to the require- maintain the fuel in the Oxidation cells at a temper-
ments of ISO 6353 or better, shall be used for the ature of 95,0 “C -+ 0,2 “C (see note 4).
preparation of the trisolvent (TAM). Water shall con-
form to grade 3 of ISO 3696. lt shall be fitted with a suitable stirring device to pro-
vide a uniform temperature throughout the bath, and
NOTE 2 It has been found that commercial grades of large enough to hold the desired number of Oxidation
solvents, if used for the procedures of this International
cells immersed to a depth of approximately 350 mm.
Standard, tan have levels of impurities that will affect the
result.
Further, the bath construction shall shield the fuel
samples from light while they are undergoing
Oxidation. A minimum liquid capacity of 6 I per
5.1 Acetone, CHsCOCH,.
Oxidation cell shall be provided.

5.2 Toluene, C,H,CH,. NOTES

5.3 Methanol, CH,OH. 3 lt has been found that a bath temperature in the range
of 95,5 “C to 95,8 “C is necessary to maintain the fuel
temperature in the specified range.
5.4 Trisolvent (TAM), comprising a Solution of
equal volumes of acetone (5.1), toluene (5.2) and 4 A metal block bath, conforming to the same capacity and
methanol (5.3). control requirements, is also suitable.
 ISO 12205:1995(E)

Dimensions in millimetres

Glass condenser
/-

Oxygen delivery tube

43 7 mm borosilicate
glass tubing

iTeh STANDARD PREVIEW

@ 6 mm bo rosilicate
(standards.iteh.ai)
CJl ass rod

ISO 12205:1995

r
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564b3686d720/iso-12205-1995

k (Bext.45 = /

rrgure 1 - Oxidation cell

6.3 Flowmeters, capable of measuring 3,0 I/h 6.7 Filter media, 47 mm diameter, of nylon mem-
+ 0,3 I/h of Oxygen flow. One flowmeter shall be brane with a nominal pore diameter of 0,8 Pm.
irovided for each Oxidation cell.
Use Single filters for prefiltration, and matched pairs
for the determination of filterable insolubles.
6.4 Filter drying oven, capable of safely evaporat-
ing the solvent at 80 “C $I 2 “C for the dtying of filter NOTE 5 Whilst the use of nylon membrane filters is pre-
ferred, as they have advantages with regard to handling,
materials.
cellulose ester membrane filters may also be used.

6.5 Glassware drying oven, capable of drying

glassware at 105 “C *- 5 “C.
6.8 Evaporating vessels, comprising tall form
beakers of borosilicate glass, of capacity either
6.6 Filter assembly, capable of holding the filter 200 ml or 100 ml depending on the technique, for
media (6.7), as illustrated in figure 2. determining adherent insolubles (10.5).
ISO 12205:1995(E) 0 ISO

7.3 Preparation of evaporating beakers

rv Filter funnel Dry the cleaned evaporating vessels (6.8) for 60 min
in the oven (6.5). Place the beakers in the desiccator
(6.9), and allow to cool for 60 min. Weigh the beakers
to the nearest 0,l mg.

8 Sampling

8.1 Samples shall be taken by the procedure de-

scribed in ISO 3170, ISO 3171 or an equivalent na-
tional Standard.
Membra ,ne filter support

8.2 Test pot-tions from the samples shall be drawn

after thorough mixing and subdivision away from di-
rect sunlight, and in an area that would be compatible
with other laboratory operations. Storage before
stress, the stress period and cool-down after stress-
ing shall occur in the dark.
Figure 2 - Filter assembly

8.3 Containers for samples shall be of metal lined

with epoxy resin or similar material, previously rinsed
6.9 General apparatus iTeh STANDARD PREVIEW twice with the material to be sampled, or borosilicate
glass, if they are wrapped or boxed to exclude light.
(standards.iteh.ai)
A balance capable of weighing to 0,l mg, a hotplate
capable of heating the liquid in the evaporating ves-
DO not use soft (Soda) glass Containers, or plastic
Containers (due to the potential for leaching of
sels (6.8) to 135 “C, a desiccator (without desiccant), plasticizers).
ISO 12205:1995
spade-ended forceps for handling the filter media, and
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a suitable. timing device.
564b3686d720/iso-12205-1995
8.4 Analyse fuel samples as soon as possible after
receipt.

7 Apparatus preparation NOTE 6 If a fuel cannot be tested within one day, it

should be blanketed with an inert gas such as Oxygen-free
nitrogen, argon or helium, and stored at a temperature no
higher than 10 “C, but not lower than its cloud Point.
7.1 Preparation of glassware other than
Oxidation cells
9 Sample preparation
Rinse all glassware thoroughly with trisolvent (5.4)
followed by water, then wash with a mildly alkaline 9.1 If the received Sample is in a tank, drum or
or neutral laboratory detergent. Rinse three times with Container exceeding 19 I capacity, use the subdivision
grade 3 water (5) followed by acetone (5.1) to remove procedures described in 8.2.
water, and allow to dry.

9.2 Thoroughly mix smaller samples by shaking,

7.2 Preparation of Oxidation cells and rolling or other techniques before taking a laboratory
Sample by pouring, pipetting or other means.
accessories

After completion of 7.1, fill Oxidation cells with Iab- 9.3 Clean any tube, thief, pipette, beaker or other
oratory detergent in grade 3 water (5). Place the oxy- apparatus or equipment that is to come into contact
gen delivery tube in the Oxidation cell, place the with the received Sample, with trisolvent (5.4) fol-
condenser over the Oxygen delivery tube, and allow lowed by a Portion of the Sample Prior to use. Allow
to soak for at least 2 h. Wash, drain, then rinse five samples that have been stored at temperatures sig-
times with tap water followed by three rinses with nificantly below 10 “C to warm to room temperature,
grade 3 water (5). Rinse with acetone (5.1), drain, and and examine for the absence of any undissolved wax
allow the Oxidation cell and delivery tube to dry. Prior to mixing thoroughly and taking an aliquot.

4
0 ISO ISO 12205:1995(E)

NOTE 7 Warming allows any separated wax to redis- or plastic to prevent entrance of dirt or dust. Record
solve, and the viscosity to decrease to a Point at which the time of removal as an interval from zero time.
mixing is effective. Agitation during the warming period as- Place the cell(s) in a dark ventilated site at room tem-
sists the redissolution of the wax. perature, which shall be above the cloud Point of the
fuel. Leave the samples until they have attained room
10 Procedure temperature, but for no longer than 4 h.

10.1 Sample filtration 10.4 Determining filterable insolubles

Place a Single filter membrane (6.7) on the filter sup- Assemble the filter apparatus as illustrated in
Port, and clamp the filter funnel to the support as figure2, using one pair of matched mass filters (6.7).
shown in figure2. Apply suction of approximately Apply suction (approximately 80 kPa), and pour the
80 kPa (an absolute pressure of approximately cooled Sample through the filter. Pull all the fuel
20 kPa in the flask). Pour 400 ml of the fuel through through the filter before completely rinsing the
the filter (6.7) into a clean (7.1) 500 ml glass suction Oxidation cell and Oxygen delivery tube with three
flask. After filtration is complete, discard the filter separate 50 ml + 5 ml volumes of 2,2,4-tri-
medium. Repeat preparation for each Sample to be methylpentane (5.5). Pass all rinsings through the fil-
run. ter assembly. After filtration is complete, disconnect
the top part of the filter assembly and wash down the
Never use the same filters for a second increment of rim of the filter-media-adjacent Parts of the filter
fuel, because any material deposited on the filters by assembly with a further 50 ml + 5 ml of
a previous increment of fuel tan result in a greater 2,2,4-trimethylpentane. Discard the filtrate. Dry the
removal of solids from the next increment. two filter media at 80 “C for 30 min, cool them for
30 min, and weigh the upper (Sample) and lower
10.2 Assembling iTeh STANDARD
the Oxidation apparatus PREVIEW (blank) filters separately to the nearest 0,l mg.

Place a clean Oxygen (standards.iteh.ai)

delivery tube into a clean NOTE 8 Using matched mass filters assumes no col-
Oxidation cell (7.2), and pour 350 ml -+ 5 ml of the fil- lection of Sediment on the lower filter medium that has
ISO 12205:1995passed through the upper medium, and that the blank cor-
tered fuel into the cell. As soon thereafter as possible,
rection is for sample/solvent absorption. Occasionally, ma-
but never more than 60https://standards.iteh.ai/catalog/standards/sist/f8898a24-6ac1-4108-a3e7-
min after measuring the fuel,
immerse the test cell in the heating bath (6.2) such terial is retained on the lower filter after having passed
564b3686d720/iso-12205-1995through the upper medium. If there is a visible deposit, or
that the level of fuel in the Oxidation cell shall be be-
if the mass gain of the lower filter exceeds 10 mg, the sum
low the level of the liquid medium in the heating bath. of the mass gains should be used for the calculations.
During any interim period, store the cell in the dark.
If severe filter plugging occurs, and filtration cannot
Place a condenser over the Oxygen delivery tube and
be completed within 120 min, filter the remaining fuel
Oxidation cell; connect the condenser to the cooling
through a separate set of weighed filters, using a fur-
water. Connect the Oxygen delivery tube to the oxy-
ther 50 ml -+ 5 ml Portion of 2,2,4-trimethylpentane to
gen supply through the flowmeter, and adjust the
wash down the filter media and filter assembly.
Oxygen flow to 3,0 I/h + 0,3 I/h. Ensure samples are
protected from light.
10.5 Determining adherent insolubles
Record the time the first Oxidation cell is placed in the
bath as zero time, and allow the cell to remain in the After completing the rinsing of the Oxidation cell and
bath for 16,00 h k 0,25 h. Note the sequence of Oxygen delivery tube as described in 10.4, dissolve
placement of Oxidation cells in the bath. the adherent insolubles from them using three equal
rinses of trisolvent (5.4) totalling 75 ml +- 5 ml. The
When the number of test cells is less than the ca- Oxidation cell and Oxygen delivery tube shall be ex-
pacity of the heating bath, the bath shall be filled with amined for evidente of stain or colour, indicating in-
Oxidation cells containing 350 ml of a stable liquid. No complete removal. If such stain or colour is noted,
Oxygen delivery tube or condenser is required for rinse with a fourth 25 ml volume of trisolvent.
these “dummy” tubes.
Either collect the rinsings in one or more tared
10.3 Cooling the Sample 100 ml beakers (6.8) as specified in ISO 6246 and
evaporate the trisolvent mixture at 160 “C by the air
Remove the Sample(s) from the heating bath in the jet procedure described in ISO 6246, or alternatively,
Same sequence as they were placed therein, cover collect the rinsings in a tared 200 ml beaker (6.8) and
the opening of each cell with a piece of aluminium foil evaporate the trisolvent mixture with extreme caution

5
ISO 12205:1995(E) 0 ISO

(especially if carrying out the procedure on more than NOTE 9 Some specifications may still use the historical
one beaker at a time) by placing on the 135 “C units of milligrams per 100 ml. In this instance, the results
hotplate (6.9) located under a hood. above should be divided by 10; or 3,5 should be used as the
divisor in the equations in 11 .l and 11.2.
When all the solvent has been evaporated, place the
tared beaker(s) containing adherent insolubles in the
desiccator (6.9) to cool for 60 min. An adherent insol- 12 Expression of results
ubles blank, to correct for the presence of impurities
in the solvents, shall be run on a volume of trisolvent
12.1 Report the total insolubles (C) to the nearest
(5.4) equal to that used in the test. When dry and cool,
1 g/m3, and the number of filters used (10.4).
weigh the beakers to the nearest 0,l mg.
Optionally, also report the filterable insolubles (A) and
the adherent insolubles (B), to the nearest 1 g/m3.
11 Calculation

12.2 Report the time that the Oxidation cell was in

11.1 Filterable insolubles
the heating bath, if other than 16 h +- 025 h.
Calculate the filterable insolubles, A, in grams per cu-
hic metre, using the following equation:
13 Precision
A= m2 - m1
0,35 Some examples of calculated precision values at
several levels of total insolubles are given in table 1.
where
NOTE 10 The same precision values apply if either of the
iTeh STANDARD
is the mass of the blank (bottom)
filter, in
PREVIEW
two optional methods are used for the determination of
milligrams; (standards.iteh.ai)
adherent insolubles.

9 is the mass of the Sample (top) filter, in

milligrams. 13.1 Repeatability,
ISO 12205:1995 r
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The differente
564b3686d720/iso-12205-1995 between successive
test results ob-
11.2 Adherent insolubles tained by the same Operator with the Same apparatus
under constant operating conditions on identical test
Calculate the adherent insolub les , B, in grams per cu- material would, in the normal and correct Operation
hic metre , usi ng the following eq uation of the test method, exceed the value below only in
one case in 20:
m4> - (mg-4
B = b-6 - 0,25
0,35

where
where C is the average value of the total insolubles
is the tare of the blank beaker, in
being compared, in grams per cubic metre.
milligrams;

is the tare mass of the Sample beaker, in 13.2 Reproducibility, R

milligrams;

is the final mass of the blank beaker, in The differente between two test results indepen-
*5
milligrams; dently obtained by different Operators operating in
different laboratories on nominally identical test ma-
is the final mass of the Sample beaker, in terial would, in the normal and correct Operation of the
m6
milligrams. test method, exceed the value below only in one case
in 20:
0,25
11.3 Total insolubles

Calculate the total insolubles, C, in grams per cubic

metre, using the following equation: where C is the average value of the total insolubles
being compared, in grams per cubic metre.
C=A+B
 ISO 12205:1995(E)

14 Test report
Table 1 - Calculated precision data
The test report shall contain at least the following in-
formation:

a) sufficient details for complete identification of the

product tested;

b) a reference to this International Standard;

c) the results of the test (see clause 12);

d) any deviation, by agreement or otherwise, fror-n

the procedure specified;

e) the date of the test.

iTeh STANDARD PREVIEW

(standards.iteh.ai)
ISO 12205:1995
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