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IP 440/14 BS EN 12662 : 2014

BS 2000-440 : 2014
BS EN 12662:2014
EUROPEAN STANDARD EN 12662

NORME EUROPÉENNE
EUROPÄISCHE NORM February 2014
ICS 75.160.20 Supersedes EN 12662:2008
English Version
Liquid petroleum products - Determination of total contamination

in middle distillates, diesel fuels and fatty acid methyl esters
Produits pétroliers liquides - Détermination de la Flüssige Mineralölerzeugnisse - Bestimmung der

contamination totale des distillats moyens, des gazoles et Gesamtverschmutzung in Mitteldestillaten, Dieselkraftstoff
des esters méthyliques d'acides gras und Fettsäure-Methylestern
This European Standard was approved by CEN on 13 December 2013.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European
Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national
standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by translation
under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same
status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United
Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION

COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2014 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 12662:2014 E
worldwide for CEN national Members.
440.1
DETERMINATION OF TOTAL CONTAMINATION IN MIDDLE DISTILLATES, DIESEL FUELS AND FATTY ACID METHYL ESTERS, IP 440
Contents Page
Foreword................................................................................................................................. 3
1 Scope............................................................................................................................ 4
2 Normative references...................................................................................................... 4
3 Terms and definitions...................................................................................................... 4
4 Principle......................................................................................................................... 4
5 Reagents and materials.................................................................................................... 4
6 Equipment...................................................................................................................... 5
7 Cleansing of sample containers and filtration apparatus....................................................... 6
8 Sampling....................................................................................................................... 6
9 Preparation of the test portion.......................................................................................... 7
10 Preparation of the equipment............................................................................................ 8
11 Procedure...................................................................................................................... 8
12 Calculation..................................................................................................................... 9
13 Expression of results....................................................................................................... 9
14 Precision........................................................................................................................ 9
15 Test report................................................................................................................... 10
Bibliography.............................................................................................................................11
440.2
Foreword
This document (EN 12662:2014) has been prepared by Technical Committee CEN/TC 19 'Gaseous and
liquid fuels, lubricants and related products of petroleum, synthetic and biological origin', the secretariat
of which is held by NEN.
This European Standard shall be given the status of a national standard, either by publication of an
identical text or by endorsement, at the latest by August 2014, and conflicting national standards shall
be withdrawn at the latest by August 2014.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent
rights.
This document supersedes EN 12662:2008.
The significant technical changes between this European Standard and the previous edition are:
— extension of the scope to middle distillates, diesel fuels containing up to 30 % (V/V) fatty
acid methyl ester (FAME) and neat FAME;
— update of the working range and precision statement based on interlaboratory study with
field samples carried out in 2011 within CEN/TC 19;
— inclusion of a dilution procedure for the determination of total contamination of neat
FAME;
— improved description of the filtration procedure and equipment.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus,
Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany,
Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United
Kingdom.
440.3
1 Scope EN ISO 3170, Petroleum liquids — Manual

sampling (ISO 3170)
This European Standard specifies a method for
the determination of the content of undissolved EN ISO 3171, Petroleum liquids — Automatic
substances, referred to as total contamination, pipeline sampling (ISO 3171)
in middle distillates, in diesel fuels containing up
to 30 % (V/V) fatty acid methyl esters (FAME), ISO 3819, Laboratory glassware — Beakers
and in neat FAME. The working range is from
12 mg/kg to 30 mg/kg and it was established in
3 Terms and definitions
an interlaboratory study by applying EN ISO 4259
[1].
For the purposes of this document, the following
terms and definitions apply.
This European Standard in general applies
to products having a kinematic viscosity not
exceeding 8 mm2/s at 20 °C, or 5 mm2/s at 3.1
40 °C, e.g. diesel fuel as specified in EN 590 [2] total contamination
and FAME as in EN 14214 [3]. undissolved substances retained on a filter after
filtration under test conditions
This test method may be used for diesel fuels
containing more than 30 % (V/V) FAME and for 3.2
petroleum products having a kinematic viscosity absolute pressure
exceeding 8 mm2/s at 20 °C, or 5 mm2/s at pressure measured relative to zero pressure or a
40 °C, however, in such cases the precision of total vacuum
the test method has not been defined.
4 Principle
NOTE 1 Excessive contamination in a fuel system
can give rise to premature blocking of filters and/or A sample portion is weighed and filtered under
hardware failure, and is therefore undesirable. vacuum through a pre-weighed filter. In the case of
neat FAME and liquid petroleum products having a
NOTE 2 For the purposes of this European Standard, kinematic viscosity exceeding 8 mm2/s at 20 °C,
the term '% (V/V)' is used to represent the volume or 5 mm2/s at 40 °C, the weighed sample portion
fraction, φ, of a material. is diluted with a solvent before filtration. The filter
with the residue is washed, dried and weighed.
WARNING — Use of this standard may involve Contamination is calculated from the difference
hazardous materials, operations and equipment. in mass of the filter and expressed relative to the
This standard does not purport to address all of sample mass as mg/kg.
the safety problems associated with its use. It is
the responsibility of the user of this standard to 5 Reagents and materials
establish appropriate safety and health practices
and to determine the applicability of regulatory
5.1 Heptane, with a purity no less than 99,0 %
limitations prior to use.
(V/V), filtered using a membrane filter (6.18).
2 Normative references NOTE Heptane used as a reference fuel in EN ISO 5164

[4] is suitable.
The following documents, in whole or in part,
are normatively referenced in this document 5.2 Xylene, analytical grade, filtered using a
and are indispensable for its application. For membrane filter (6.18).
dated references, only the edition cited applies.
For undated references, the latest edition of the 5.3 Propan-2-ol, with a purity no less than
referenced document (including any amendments) 99,0 % (V/V).
applies.
NOTE Propan-2-ol is used to dry glassware and the
EN 14275, Automotive fuels — Assessment sample container after rinsing with water.
of petrol and diesel fuel quality — Sampling
from retail site pumps and commercial site fuel 5.4 Solvent, add 750 ml heptane (5.1) and
dispensers 250 ml xylene (5.2) to a 1 l glass bottle (6.5) and
mix thoroughly.
440.4
6 Equipment 6.8 Glass Petri dishes with covers, greater

than 50 mm in diameter.
All glassware and sample containers shall be
carefully cleaned as described in Clause 7. 6.9 Analytical balance, capable of weighing to
the nearest 0,1 mg.
Usual laboratory apparatus and glassware,
together with the following: 6.10 Forceps, with round shaped tips for
transferring the filter from the filter holder to the
6.1 Filtration apparatus, suitable for a filter Petri dish and from the latter on to the dish of the
(6.2), as shown in Figure 1. analytical balance.
A different filtration apparatus may be used if it is 6.11 Water bath or oven, capable of maintaining
suitable to take the filters given in 6.2. the following temperatures: (40 ± 1) °C and (60
± 1) °C.
6.2 Filters, of high retention glass fibre type,
47 mm in diameter and with a 0,7 μm mean pore 6.12 Wash bottle, fitted with spray nozzle,
size. suitable for use with heptane (5.1).
NOTE Glass fibre filters Whatman GF-F type have been 6.13 Top load balance, capable of weighing
found suitable for total contamination measurements. 1 500 g to the nearest 0,1 g.
This information is given for the convenience of users
of this European Standard and does not constitute an 6.14 Vacuum source, capable of maintaining
endorsement by CEN of this product.
an absolute pressure of 2 kPa to 5 kPa inside the
filtration apparatus (see Figure 1).
6.3 Beakers, tall form 0,5 l and 1 l, conforming
with ISO 3819 or an equivalent national standard. NOTE The vacuum range excludes the use of a water
vacuum pump.
6.4 Cylinders, 500 ml and 1 000 ml graduated
cylinders. 6.15 Suitable clean sample containers.
6.5 Glass bottles, 0,5 l and 1 l, with screw 6.16 Stopwatch, capable of measuring 30 min
caps. ± 1 min.
6.6 Oven, of the static type (without fan 6.17 Clean plastic film or aluminium foil.
assisted circulation), explosion-proof, capable of
heating to (110 ± 5) °C. 6.18 Filter, membrane with a mean pore size of
0,45 μm.
6.7 Desiccator, containing freshly activated
silica gel (or equivalent desiccant) with a moisture
content indicator.
440.5
Key
1 wire to ground 4 filter holder 7 safety flask

2 clamp 5 receiving flask 8 vacuometer
3 funnel 6 vacuum tubing 9 to vacuum pump
Figure 1 Filtration apparatus for determining contamination
7 Cleansing of sample containers 7.7 Cover the top of the sample container
and filtration apparatus and the funnel opening of the assembled filtration
apparatus (6.1) with clean plastic film or aluminium
foil (6.17) previously rinsed with heptane (5.1)
IMPORTANT — Due to the extremely low levels
and air-dried.
of material being measured, it is essential that
this testing is performed in a clean environment
to minimize the possibility of contamination. 8 Sampling
7.1 Clean strictly, in the manner described in 8.1 Unless otherwise specified, obtain
7.2 to 7.7, all the surfaces of all components of samples in accordance with the requirements of
the sample containers and parts of the apparatus EN ISO 3170, EN ISO 3171, EN 14275, or an
that are: equivalent national standard.
a) likely to come into contact with the sample 8.2 The preferred procedure is to take samples
or heptane (5.1), or dynamically from a sampling loop in a distribution
b) capable of transferring extraneous matter line or from the flushing line of an automatic
to the filter. pipeline sampling device in accordance with the
principles specified in EN ISO 3171. Ensure that
7.2 Wash with warm tap water containing the line to sampler is flushed with fuel before
water soluble detergent taking the sample.
7.3 Rinse thoroughly with warm tap water 8.3 If samples are taken manually the samples
shall be taken directly into the sample container
7.4 Rinse thoroughly with water, handling (6.15).
container caps externally only with clean
laboratory tongs or gloves during this and 8.4 Where it is only possible to obtain samples
subsequent washings. from static storage follow the procedures given in
EN ISO 3170, ensuring that the final sample has
7.5 Rinse thoroughly with propan-2-ol (5.3). not passed through intermediate containers prior
to placement in the prepared container.
7.6 Rinse thoroughly with heptane (5.1).
440.6
8.5 Glass containers shall be used to take container walls, repeat shaking procedure. The
and store the samples. These containers should use of a mixer is not allowed.
be cleaned according to Clause 7. Glass is used
in order to facilitate the visual surveillance of 9.2.5 Weigh into the beaker a test portion
the sample homogenisation before subsequent equivalent to approximately 300 ml. The sample
analysis. Ensure that the samples receive the shall be poured very quickly into the beaker,
minimum exposure to light. Use either brown without trying to get a volume as close as possible
glass containers or shield the samples from light to 300 ml. Record the mass of the test portion mE
during transportation and storage. To facilitate to the nearest 0,1 g.
sampling from refuelling nozzles, wide necked
bottles should be used. 9.3 Neat FAME
8.6 Fill the sample container to between 80 % 9.3.1 Loosen the sample container closure and
and 85 % of its capacity. place the container and its content in a water bath
or oven (6.11) at 60 °C for at least 2 h to 2,5 h to
8.7 The collected sample shall be homogenised ensure that any components that have separated
according to the procedure given in 9.2.4 before out have dissolved again.
any other analytical measurements are carried
out, to avoid non-representative sampling when 9.3.2 Remove the sample container from the
this method is performed. water bath or oven and tighten the container
closure. Let it cool down to room temperature.
9 Preparation of the test portion Wash the outside of the container with propan-2-ol.
9.1 General 9.3.3 Place the 1 l bottle (6.5) onto the balance
(6.13) and tare.
Make sure that the sample container (6.15) is
free of adhering particles which can distort the 9.3.4 Shake the sample container for at least
analysis. In case of doubt, rinse the outside of the 10 s, one-to-two strokes per second, using
container and its closure with water and propan- 10 cm to 25 cm strokes. Invert the container
2-ol (5.3), as described in 7.2 to 7.5, to remove and continue to shake for at least a further
any adhering particles and avoid introducing 10 s, then re-invert and shake for at least a further
undesirable contamination in the test sample. 10 s. If there are any visible signs of contaminant
adhering to the container walls, repeat shaking
procedure. The use of a mixer is not allowed.
9.2 Middle distillates and diesel fuels
9.3.5 Weigh into the bottle a test portion

9.2.1 Loosen the sample container closure and
equivalent to approximately 300 ml. The sample
place the container and its content in a water bath
shall be poured very quickly into the bottle, without
or oven (6.11) at 40 °C for 30 min to 60 min to
trying to get a volume as close as possible to
ensure that any components that have separated
300 ml. Record the mass of the test portion mE to
out have dissolved again.
the nearest 0,1 g.
9.2.2 Remove the sample container from the
9.3.6 Add 300 ml of the solvent (5.4) by
water bath or oven and tighten the container
means of a 500 ml graduated cylinder (6.4). Mix
closure. Let it cool down to room temperature.
thoroughly and leave at ambient temperature for
Wash the outside of the container with propan-2-
2 h before filtration.
ol.
9.4 Liquid petroleum products with a kinematic

9.2.3 Place the beaker (6.3) onto the balance
viscosity exceeding 8 mm2/s at 20 °C, or 5 mm2/s
(6.13) and tare.
at 40 °C
9.2.4 Shake the sample container for at least
9.4.1 Loosen the sample container closure and
10 s, one-to-two strokes per second, using 10 cm to
place the container and its content in a water bath
25 cm strokes. Invert the container and continue
or oven (6.11) at 40 °C for 30 min to 60 min to
to shake for at least a further 10 s, then re-invert
ensure that any components that have separated
and shake for at least a further 10 s. If there are
out have dissolved again.
any visible signs of contaminant adhering to the
440.7
9.4.2 Remove the sample container from the vacuum. Release the vacuum slowly and then
water bath or oven and tighten the container remove carefully the filter from the filter holder by
closure. Let it cool down to room temperature. means of the forceps (6.10), place it on the Petri
Wash the outside of the container with propan-2- dish (6.8) and place in the oven (6.6) at 110 °C
ol. ± 5 °C for at least 45 min. Use the cover during
transport to the oven, remove the cover when the
9.4.3 Place the 1 l bottle (6.5) onto the balance Petri dish is placed in the oven. Check carefully
(6.13) and tare. that the filter is centred on the filter holder. The
filter shall not be damaged by the filter holder
9.4.4 Shake the sample container for at least equipment. Damaged filters affect the mass of the
10 s, one-to-two strokes per second, using filter and lead to erroneous results.
10 cm to 25 cm strokes. Invert the container and
continue to shake for at least a further 10 s, then re- 10.2.3 Remove the Petri dish (6.8) and filter from
invert and shake for at least a further 10 s. If there the oven (6.6), apply the cover and cool in the
are any visible signs of contaminant adhering to desiccator (6.7), located near to the analytical
the container walls, repeat shaking procedure. balance (6.9), for approximately 45 min.
The use of a mixer is not allowed.
10.2.4 Immediately before the determination,
9.4.5 Weigh into the bottle a test portion remove the filter (6.2) from the Petri dish (6.8)
equivalent to approximately 300 ml. The sample and using the analytical balance (6.9) weigh the
shall be poured very quickly into the bottle, filter to the nearest 0,1 mg. Record this mass m1.
without trying to get a volume as close as possible
to 300 ml. Record the mass of the test portion mE 10.2.5 Place the filter (6.2) directly on to the
to the nearest 0,1 g. filter holder of the pre-cleaned apparatus and fix
the funnel with the clamp. Rinse the filter with
9.4.6 Dilute the weighed sample portion (mE) heptane (5.1). Ensure that the filter is free from
with heptane (5.1) to a kinematic viscosity not bubbles and is firmly fixed between the round
exceeding 8 mm2/s at 20 °C, or 5 mm2/s at surfaces of the filter apparatus.
40 °C. Mix thoroughly.
11 Procedure
10 Preparation of the equipment
WARNING — Electrostatic charges can be
generated during the filtration of petroleum
10.1 Preparation of the filtration apparatus
products; therefore the filter apparatus shall be
earthed.
10.1.1 Visually check that the filtration apparatus
(6.1) is clean both internally and externally. If not
11.1 Filter the test sample (9.2.5, 9.3.6 or
clean, repeat in accordance with Clause 7.
9.4.6) using the filter after its preparation (10.2)
applying suction or vacuum as necessary to reach
10.1.2 Follow all existing safety precautions and an absolute pressure of 2 kPa to 5 kPa (6.14)
earth the apparatus to avoid electrostatic build-up inside. The sample shall be transferred into the
and discharge. filtration apparatus (6.1) in small portions. Be
careful not to let the filter assembly dry during
10.1.3 Assemble the filtration apparatus (6.1) this transfer.
without the filter (6.2) and wash the inside with
heptane (5.1). Ensure seal between filter holder If foaming is observed in the receiving flask, check
and receiving flask, and between tube, hose and the vacuum pressure. A pressure lower than that
wire and safety flask with appropriate sealant. mentioned above may lead to foaming.
10.2 Preparation of the filter If the filtration of the sample is not completed after
30 min, turn off the vacuum system and record
10.2.1 For all operations handle the filter (6.2) by the volume filtered. A correction on the mass of
the edge using forceps (6.10). the sample test portion, mE, may be applied.
10.2.2 Place the filter (6.2) properly centred on 11.2 Using the wash bottle (6.12) wash the
to the filter holder of the pre-cleaned apparatus. sediment from the beaker (6.3) or the glass bottle
Rinse the filter (6.2) with heptane (5.1) and apply (6.5) onto the filter (6.2) with heptane (5.1).
440.8
Carefully rinse the inside wall and base of the mE is the mass of the sample test portion in
beaker (6.3) and filter the rinsings. Repeat the grams (9.2.5, 9.3.5 or 9.4.5).
washing operation twice more.
13 Expression of results
11.3 Using the wash bottle (6.12) wash the
inside wall of the funnel of the filtration apparatus Express the total contamination as a mass
(6.1) and filter (6.2) with heptane (5.1) and dry fraction, μ, rounded to the nearest 0,5 mg/kg,
under suction. The funnel should be washed with or report as incomplete filtration and indicate the
a gentle stream and circumferential movement. volume filtered (see 11.1).
Repeat the washing operation two more times.
11.4 Carefully remove the funnel and with the

14 Precision
vacuum applied, wash the filter (6.2) from the
periphery inwards by directing a gentle stream 14.1 General
of heptane (5.1). Take care not to wash any of
the particulate from the surface of the filter (6.2). The precision given in 14.2 and 14.3 was
Maintain the vacuum after the final washing for determined by statistical examination of
approximately 10 s to 15 s or until all excess interlaboratory test results in accordance with EN
heptane is removed from the filter. ISO 4259 [1].
11.5 Release the vacuum slowly and then 14.2 Repeatability

remove carefully the filter (6.2) from the filter
holder by means of the forceps (6.10), place it The difference between two successive test
on the Petri dish (6.8) (see 10.2) and apply cover. results obtained by the same operator with
Place the Petri dish (6.8), including the filter (6.2), the same apparatus under constant operating
into the oven (6.6), remove the cover and dry at conditions on identical test material would, in the
110 °C ± 5 °C for 45 min. Allow to cool down normal and correct operation of the test method,
to room temperature for approximately 45 min in exceed the values calculated from the following
the desiccator (6.7) located close to the analytical formula only in one case in twenty:
balance using the Petri dish cover.
r = 0,064 4 X + 1,609 9 (2)
11.6 Using the analytical balance (6.9), weigh
the filter (6.2) without the Petri dish (6.8) to the where
nearest 0,1 mg. Record this mass m2. The filter
shall be weighed to a constant value. Temperature X is the average of the two results being
and time given in 11.5 are adequate to remove compared, in milligrams per kilogram (mg/
the washing medium. However, it is necessary to kg).
verify that the filter has reached a constant mass.
If not, the filter is further dried according to 11.5. 14.3 Reproducibility
12 Calculation The difference between two single and independent

results obtained by different operators working
Calculate the total contamination as a mass in different laboratories on nominally identical
fraction μ in mg/kg, using the following formula: test material would, in the normal and correct
operation of the test method, exceed the values
calculated from the following equation only in one
1000( m2 − m1 )
μm = case in twenty:
mE
(1)
R = 0,164 4 X + 4,111 0 (3)
where
where
m1 is the mass of the filter, in milligrams (see
10.2.4); X is the average of the two results being
compared, in milligrams per kilogram (mg/
kg).
m2 is the mass of the filter with the
contaminant in milligrams (see 11.6);
440.9
15 Test report c) sampling procedure used (see Clause 8);

d) result of the test (see Clause 13);
The test report shall contain at least the following e) when applicable, the notification
information: 'incomplete filtration' plus test volume
filtered, in ml, after 30 min (see 11.1);
f) any deviation, by agreement or otherwise,
a) type and identification of the product
from the procedure described;
under test;
g) date of the test.
b) reference to this European standard;
440.10
Bibliography
[1] EN ISO 4259, Petroleum products - Determination and application of precision data in relation to
methods of test (ISO 4259)
[2] EN 590, Automotive fuels - Diesel - Requirements and test methods
[3] EN 14214, Liquid petroleum products — Fatty acid methyl esters (FAME) for use in diesel engines
and heating applications — Requirements and test methods
[4] EN ISO 5164, Petroleum products - Determination of knock characteristics of motor fuels -
Research method (ISO 5164)
440.11

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COPYRIGHT NOTICE & TERMS OF USE

SAI GLOBAL, Index House, Ascot, Berks, SL5 7EU, UK

SAI GLOBAL, 286 Sussex Street, Sydney NSW 2000, Australia

IP 440/14 BS EN 12662 : 2014

EUROPEAN STANDARD EN 12662

ICS 75.160.20 Supersedes EN 12662:2008

Liquid petroleum products - Determination of total contamination

Produits pétroliers liquides - Détermination de la Flüssige Mineralölerzeugnisse - Bestimmung der

This European Standard was approved by CEN on 13 December 2013.

EUROPEAN COMMITTEE FOR STANDARDIZATION

CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels

This document supersedes EN 12662:2008.

1 Scope EN ISO 3170, Petroleum liquids — Manual

2 Normative references NOTE Heptane used as a reference fuel in EN ISO 5164

6 Equipment 6.8 Glass Petri dishes with covers, greater

1 wire to ground 4 filter holder 7 safety flask

Figure 1 Filtration apparatus for determining contamination

9.3.5 Weigh into the bottle a test portion

9.4 Liquid petroleum products with a kinematic

11.4 Carefully remove the funnel and with the

11.5 Release the vacuum slowly and then 14.2 Repeatability

12 Calculation The difference between two single and independent

15 Test report c) sampling procedure used (see Clause 8);

[2] EN 590, Automotive fuels - Diesel - Requirements and test methods

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