SIST EN ISO 3405:2011
(Main)Petroleum products - Determination of distillation characteristics at atmospheric pressure (ISO 3405:2011)
Petroleum products - Determination of distillation characteristics at atmospheric pressure (ISO 3405:2011)
This International Standard specifies a laboratory method for the determination of the distillation characteristics of light and middle distillates derived from petroleum with initial boiling points above 0 °C and end-points below approximately 400 °C, utilizing either manual or automated equipment. Light distillates are typically; automotive engine petrols, automotive engine petrols with up to 10% (V/V) ethanol, and aviation petrols. Middle distillates are typically; aviation turbine fuels, kerosines, diesel, diesel with up to 20% (V/V) FAME, burner fuels, and marine fuels that have no appreciable quantities of residua.
Mineralölerzeugnisse - Bestimmung des Destillationsverlaufes bei Atmosphärendruck (ISO 3405:2011)
Diese Internationale Norm legt ein Laborprüfverfahren zur Bestimmung des Destillationsverlaufes von aus
Erdöl gewonnenen niedrig siedenden Fraktionen und Mitteldestillaten mit einem Destillationsbeginn über 0 °C
und einem Destillationsendpunkt unter etwa 400 °C mittels manuellen als auch automatischen Prüfgeräten
fest.
Niedrig siedende Fraktionen sind üblicherweise Kraftstoffe, Kraftstoffe mit einem Ethanolgehalt von bis zu
10 % (V/V), sowie Flugzeugbenzine. Mitteldestillate sind üblicherweise Flugturbinenkraftstoffe, Kerosin, Diesel
mit Gehalten an Fettsäuremethylester (FAME) bis zu 20 % (V/V), Brennstoffe und Schifffahrtsbrennstoffe, die
keine bedeutenden Rückstandsanteile aufweisen.
ANMERKUNG Für die Zwecke dieser internationalen Norm wird der Ausdruck „% (V/V)“ verwendet, um den
Volumenanteil in Prozent eines Erzeugnisses auszudrücken.
Produits pétroliers - Détermination des caractéristiques de distillation à pression atmosphérique (ISO 3405:2011)
L'ISO 3405:21011 spécifie une méthode d'essai de laboratoire, utilisant des appareils manuels ou automatisés, pour la détermination des caractéristiques de distillation des distillats pétroliers légers et moyens ayant un point initial de distillation supérieur à 0 °C et un point final inférieur à environ 400 °C.
Les distillats légers habituels sont les essences pour moteur automobiles, les essences pour moteurs automobiles contenant jusqu'à 10 % (V/V) d'éthanol et les essences d'aviation. Les distillats moyens sont les carburéacteurs, les kérosènes, les gazoles, les gazoles contenant jusqu'à 20 % (V/V) d'EMAG (esters méthyliques d'acide gras), les combustibles de chauffe et les combustibles pour la marine qui n'ont pas une quantité appréciable de résidus.
Naftni proizvodi - Določevanje destilacijskih značilnosti pri atmosferskem tlaku (ISO 3405:2011)
Ta mednarodni standard določa laboratorijsko metodo za določevanje destilacijskih značilnosti lahkih in srednjih destilatov, pridobljenih iz nafte z začetno točko vretja nad 0 °C in končno točko pod približno 400 °C, z uporabo ročne ali avtomatske opreme. Lahki destilati so običajno: avtomobilska maziva motorja, avtomobilska maziva motorja z do 10 % (V/V) etanola, letalska maziva. Srednji destilati so običajno: letalske turbine, goriva, kerozini, dizel, dizel z do 20 % (V/V) FAME, goriva za gorilce in pomorska goriva, ki nimajo občutnih količin ostankov.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 3405:2011
01-marec-2011
1DGRPHãþD
SIST EN ISO 3405:2000
1DIWQLSURL]YRGL'RORþHYDQMHGHVWLODFLMVNLK]QDþLOQRVWLSULDWPRVIHUVNHPWODNX
,62
Petroleum products - Determination of distillation characteristics at atmospheric pressure
(ISO 3405:2011)
Mineralölerzeugnisse - Bestimmung des Destillationsverlaufes bei Atmosphärendruck
(ISO 3405:2011)
Produits pétroliers - Détermination des caractéristiques de distillation à pression
atmosphérique (ISO 3405:2011)
Ta slovenski standard je istoveten z: EN ISO 3405:2011
ICS:
75.080 Naftni proizvodi na splošno Petroleum products in
general
SIST EN ISO 3405:2011 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 3405:2011
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SIST EN ISO 3405:2011
EUROPEAN STANDARD
EN ISO 3405
NORME EUROPÉENNE
EUROPÄISCHE NORM
January 2011
ICS 75.080 Supersedes EN ISO 3405:2000
English Version
Petroleum products - Determination of distillation characteristics
at atmospheric pressure (ISO 3405:2011)
Produits pétroliers - Détermination des caractéristiques de Mineralölerzeugnisse - Bestimmung des
distillation à pression atmosphérique (ISO 3405:2011) Destillationsverlaufes bei Atmosphärendruck (ISO
3405:2011)
This European Standard was approved by CEN on 31 December 2010.
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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,
Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2011 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 3405:2011: E
worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST EN ISO 3405:2011
EN ISO 3405:2011 (E)
Contents Page
Foreword .3
2
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SIST EN ISO 3405:2011
EN ISO 3405:2011 (E)
Foreword
This document (EN ISO 3405:2011) has been prepared by Technical Committee ISO/TC 28 "Petroleum
products and lubricants" in collaboration with 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 July 2011, and conflicting national standards shall be withdrawn at the
latest by July 2011.
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 ISO 3405:2000.
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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia,
Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain,
Sweden, Switzerland and the United Kingdom.
Endorsement notice
The text of ISO 3405:2011 has been approved by CEN as a EN ISO 3405:2011 without any modification.
3
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SIST EN ISO 3405:2011
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SIST EN ISO 3405:2011
INTERNATIONAL ISO
STANDARD 3405
Fourth edition
2011-01-15
Petroleum products — Determination of
distillation characteristics at atmospheric
pressure
Produits pétroliers — Détermination des caractéristiques de distillation à
pression atmosphérique
Reference number
ISO 3405:2011(E)
©
ISO 2011
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SIST EN ISO 3405:2011
ISO 3405:2011(E)
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© ISO 2011
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,
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Published in Switzerland
ii © ISO 2011 – All rights reserved
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SIST EN ISO 3405:2011
ISO 3405:2011(E)
Contents Page
Foreword .v
Introduction.vi
1 Scope.1
2 Normative references.1
3 Terms and definitions .1
4 Principle .3
5 Apparatus.3
5.1 General .3
5.2 Distillation flasks.4
5.3 Condenser tube and cooling bath .4
5.4 Metal shield or enclosure for flask (manual apparatus only) .8
5.5 Heat source .8
5.6 Flask support .8
5.7 Graduated cylinders.8
5.8 Temperature measurement system.9
5.9 Centring device.10
5.10 Barometer.10
6 Samples and sampling.11
6.1 Sample grouping .11
6.2 Sample maintenance prior to testing .12
6.3 Removing water from sample .13
7 Preparation of apparatus.13
8 Apparatus verification.15
8.1 Level follower.15
8.2 Electronic temperature-measurement devices .15
8.3 Electronic pressure-measuring device .16
9 Procedure — Manual apparatus .16
10 Procedure — Automated apparatus.18
11 Calculations .20
12 Expression of results.22
13 Precision — Manual apparatus .23
13.1 General .23
13.2 Repeatability .24
13.3 Reproducibility .24
14 Precision — Automated apparatus.25
14.1 General .25
14.2 Repeatability .25
14.3 Reproducibility .25
14.4 Bias .26
15 Test report.26
Annex A (normative) Thermometer specifications .27
Annex B (normative) Determination of temperature-sensor lag times .28
Annex C (normative) Determination of specified distillation data.29
© ISO 2011 – All rights reserved iii
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SIST EN ISO 3405:2011
ISO 3405:2011(E)
Annex D (informative) Examples of data calculations. 31
Annex E (informative) Emulation of emergent-stem errors . 34
Annex F (informative) Examples of test reports . 35
iv © ISO 2011 – All rights reserved
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SIST EN ISO 3405:2011
ISO 3405:2011(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. Each 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.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 3405 was prepared by Technical Committee ISO/TC 28, Petroleum products and lubricants.
This fourth edition cancels and replaces the third edition (ISO 3405:2000), which has been technically revised.
1)
It has been aligned with ASTM D86 .
1) ASTM D86, Standard Method for Distillation of Petroleum Products at Atmospheric Pressure.
© ISO 2011 – All rights reserved v
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SIST EN ISO 3405:2011
ISO 3405:2011(E)
Introduction
The distillation (volatility) characteristics of hydrocarbons have an important effect on their safety and
performance, especially in the case of fuels and solvents. The boiling range gives important information on
composition and behaviour during storage and use, and the rate of evaporation is an important factor in the
application of many solvents. Limiting values to specified distillation characteristics are applied to most
distillate petroleum product specifications in order to control end-use performance and to regulate the
formation of vapours which may form explosive mixtures with air or otherwise escape into the atmosphere as
emissions (volatile organic compounds or VOCs).
vi © ISO 2011 – All rights reserved
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SIST EN ISO 3405:2011
INTERNATIONAL STANDARD ISO 3405:2011(E)
Petroleum products — Determination of distillation
characteristics at atmospheric pressure
WARNING — The use of this International Standard may involve hazardous materials, operations and
equipment. This International Standard does not purport to address all of the safety problems
associated with its use. It is the responsibility of the user of this International Standard to establish
appropriate safety and health practices and to determine the applicability of regulatory limitations
prior to use.
1 Scope
This International Standard specifies a laboratory test method, utilizing either manual or automated equipment,
for determining the distillation characteristics of light and middle distillates derived from petroleum and having
initial boiling points above 0 °C and end points below approximately 400 °C.
Light distillates are typically automotive engine petrols, automotive engine petrols with up to 10 % (V/V)
ethanol and aviation petrols. Middle distillates are aviation turbine fuels, kerosenes, diesel, diesel with up to
20 % (V/V) FAME (fatty acid methylesters), burner fuels and marine fuels that have no appreciable quantities
of residua.
NOTE For the purposes of this International Standard, “% (V/V)” is used to represent the volume fraction of a material.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated
references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.
ISO 918, Volatile organic liquids for industrial use — Determination of distillation characteristics
ISO 3170, Petroleum liquids — Manual sampling
ISO 3171, Petroleum liquids — Automatic pipeline sampling
ISO 4259, Petroleum products — Determination and application of precision data in relation to methods of test
ISO 4788:2005, Laboratory glassware — Graduated measuring cylinders
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
decomposition point
thermometer reading (corrected) which coincides with the first indications of thermal decomposition of the
liquid in the flask
NOTE Characteristic indications of thermal decomposition are an evolution of fumes and erratic thermometer
readings which usually show a decided decrease after any attempt has been made to adjust the heat.
© ISO 2011 – All rights reserved 1
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SIST EN ISO 3405:2011
ISO 3405:2011(E)
3.2
dry point
thermometer reading (corrected) that is observed at the instant the last drop of liquid evaporates from the
lowest point in the flask, any drops or film of liquid on the side of the flask or on the thermometer being
disregarded
NOTE The end point (final boiling point), rather than the dry point, is intended for general use. The dry point can be
reported in connection with special purpose naphthas, such as those used in the paint industry. It is substituted for the
end point (final boiling point) whenever the sample is of such a nature that the precision of the end point cannot
consistently meet the precision requirements given in Clause 13 or 14.
3.3
end point
final boiling point
maximum thermometer reading (corrected) obtained during the test
NOTE This usually occurs after evaporation of all liquid from the bottom of the flask.
3.4
initial boiling point
thermometer reading (corrected) that is observed at the instant the first drop of condensate falls from the
lower end of the condenser tube
3.5
percent evaporated
sum of the percent recovered and the percent loss
3.6
percent loss
front-end loss
amount of uncondensed material lost in the initial stages of the distillation, equal to 100 % minus the total
recovery
3.7
corrected loss
percent loss corrected for barometric pressure
3.8
percent recovered
volume of condensate observed in the receiving cylinder at any point in the distillation in connection with a
simultaneous temperature reading
NOTE It is expressed as a percentage of the charge volume.
3.9
percent recovery
maximum percent recovered, as observed in accordance with this International Standard
NOTE See 9.10.
3.10
percent residue
volume of residue measured in accordance with this International Standard
NOTE 1 See 9.11.
NOTE 2 It is expressed as a percentage of the charge volume.
2 © ISO 2011 – All rights reserved
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SIST EN ISO 3405:2011
ISO 3405:2011(E)
3.11
percent total recovery
combined percent recovery and residue in the flask, as determined in accordance with this International
Standard
NOTE See 10.1.
3.12
thermometer reading
temperature recorded by the sensor of the saturated vapour, measured in the neck of the flask below the
vapour tube and under the specified conditions of this test
3.13
temperature reading
thermometer reading or other temperature measurement device reading which is corrected to 101,3 kPa
barometric pressure
3.14
emergent-stem effect
offset in temperature reading caused by the use of a total immersion mercury-in-glass thermometer in the
partial immersion mode
NOTE The emergent part of the mercury column is at a lower temperature than the immersed portion, resulting in a
lower temperature reading than that obtained with the thermometer completely immersed for calibration.
3.15
temperature lag
offset in temperature reading between a mercury-in-glass thermometer and an electronic temperature-
measurement device, caused by the different response times of the systems involved
4 Principle
The sample is assigned to one of four groups, based on its composition and expected volatility characteristics,
with each group defining the apparatus arrangement, condenser temperature and operational variables. A
100 ml test portion is distilled under the specified conditions appropriate to the group into which the sample
falls, and systematic observations of thermometer readings and volumes of condensate recovered are made.
The volume of the residue in the flask is measured, and the loss on distillation recorded. The thermometer
readings are corrected for barometric pressure and the data are then used for calculations appropriate to the
nature of the sample and the specification requirements.
5 Apparatus
5.1 General
Typical assemblies of the manual apparatus are shown in Figures 1 and 2. In addition to the basic
components described in this clause, automated apparatus also are equipped with a system for measuring
and automatically recording the vapour temperature and the associated recovered volume in the receiving
cylinder.
Automated equipment manufactured in or after the year 1999 shall be equipped with a device for
automatically shutting down power to the unit and for spraying an inert gas or vapour in the chamber where
the distillation flask is mounted in the event of fire.
NOTE Some causes of fire are breakage of the distillation flask, electrical shorts, and foaming and spilling of liquid
sample through the top opening of the flask.
© ISO 2011 – All rights reserved 3
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SIST EN ISO 3405:2011
ISO 3405:2011(E)
5.2 Distillation flasks
The distillation flasks shall have a capacity of 125 ml and be constructed of heat-resistant glass, according to
the dimensions and tolerances shown in Figure 3.
NOTE For tests specifying the dry point, specially selected flasks with bottoms and walls of uniform thickness are
desirable.
5.3 Condenser tube and cooling bath
5.3.1 Typical types of condenser and cooling bath are illustrated in Figures 1 and 2. Other types of
apparatus may be used, provided that the test results obtained by their use are such as to correlate with the
results obtained with those illustrated in Figures 1 and 2 and to satisfy the precision criteria given in Clause 13
or 14.
5.3.2 The condenser shall be made of seamless non-corrosive metal tubing, 560 mm ± 5 mm in length, with
an outside diameter of 14 mm and a wall thickness of 0,8 mm to 0,9 mm.
NOTE Brass or stainless steel are suitable materials.
5.3.3 The condenser shall be set so that a length of 393 mm ± 3 mm of the tube is in contact with the
cooling medium, with 50 mm ± 3 mm outside the cooling bath at the upper end, and 114 mm ± 3 mm outside
at the lower end. The portion of tube projecting at the upper end shall be set at an angle of 75° to the vertical.
The portion of the tube inside the cooling bath shall be either straight or bent in any suitable continuous
smooth curve. The average gradient shall be 15° ± 1° with respect to the horizontal, and no 100 mm section
shall have a gradient outside the range of 15° ± 3°. The projecting lower portion of the condenser tube shall
be curved downward for a length of 76 mm and the lower end cut off at an acute angle. Provisions shall be
made to enable the flow of distillate to run down the side of the receiving cylinder. Figure 4 gives an illustration
of the lower end of the condenser tube.
The flow of distillate down the side of the graduated cylinder may be accomplished either by using a drip
deflector inserted in the receiver, or by having the downward length of the condenser tube curve slightly
backwards so as to ensure contact with the wall of the receiving cylinder at a point 25 mm to 32 mm below the
top of the receiving cylinder when it is in position to receive distillate.
5.3.4 The volume and design of the cooling bath will depend on the cooling medium employed. The cooling
capacity of the bath shall be adequate to maintain the required temperature for the desired condenser
performance. A single cooling bath may be used for several condenser tubes.
4 © ISO 2011 – All rights reserved
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SIST EN ISO 3405:2011
ISO 3405:2011(E)
Key
1 cooling bath
2 air vents
3 burner
4 shield
5 heat-resistant boards
6 distillation flask
7 thermometer
8 bath cover
9 blotting paper
10 support
11 graduated cylinder
12 gas line
Figure 1 — Apparatus assembly using a gas burner
© ISO 2011 – All rights reserved 5
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SIST EN ISO 3405:2011
ISO 3405:2011(E)
Key
1 receiving cylinder
2 blotting paper
3 thermometer
4 distillation flask
5 flask-support board
6 electric heating element
7 flask-support platform
8 flask-adjusting knob
9 indicating dial
10 switch
11 open-bottom shield
12 cooling bath
13 condenser tube
14 shield
Figure 2 — Apparatus assembly using an electric heater
6 © ISO 2011 – All rights reserved
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SIST EN ISO 3405:2011
ISO 3405:2011(E)
Dimensions in millimetres
Key
1 19/22 or 19/26
a
Reinforcing bead.
b
Fire-polished.
Figure 3 — 125 ml flasks — Alternative neck designs
Dimensions in millimetres
Figure 4 — Lower end of condenser tube
© ISO 2011 – All rights reserved 7
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SIST EN ISO 3405:2011
ISO 3405:2011(E)
5.4 Metal shield or enclosure for flask (manual apparatus only)
Shields shall be provided to protect the operator from damage to the unit during operation, and to protect the
distillation flask from draughts. These shall allow easy access to the distillation setup during operation, and be
provided with at least one window for observing the dry point at the end of the distillation.
NOTE 1 A typical shield for a unit fitted with a gas burner would be 400 mm high, 280 mm long and 200 mm wide,
made of sheet metal approximately 0,8 mm in thickness (see Figure 1).
NOTE 2 A typical shield for a unit fitted with an electric heater would be 440 mm high, 200 mm long and 200 mm wide,
made of sheet metal approximately 0,8 mm in thickness (see Figure 2).
5.5 Heat source
5.5.1 Gas burner (see Figure 1), capable of bringing over the first drop from a cold start within the time
specified, and continuing the distillation at the specified rate. A sensitive regulating valve and gas pressure
governor to give complete control of heating shall be provided.
5.5.2 Electric heater (see Figure 2), of low heat retention and adjustable from 0 W to 1 000 W.
5.6 Flask support
5.6.1 Type 1, for use with gas burner (see Figure 1). Either a ring support of the ordinary laboratory type,
100 mm or larger in diameter, supported on a stand inside the shield, or a platform adjustable from the outside
of the shield shall be used.
The flask support board shall be constructed of ceramic or other heat-resistant material, 3 mm to 6 mm in
thickness, and shall have a central opening conforming to the dimensions given in Table 2. The flask support
board shall be of sufficient dimension to ensure that thermal heat to the flask only comes from the central
opening and that extraneous heat to the flask other than through the central opening is minimized. The flask-
support board may be moved slightly in accordance with the directions for positioning the distillation flask so
that direct heat is applied to the flask only through the opening in this board. The position of the flask is set by
adjusting the length of the side arm inserted into the condenser.
5
...
SLOVENSKI STANDARD
oSIST prEN ISO 3405:2009
01-november-2009
1DIWQLSURL]YRGL'RORþHYDQMHGHVWLODFLMVNLK]QDþLOQRVWLSULDWPRVIHUVNHPWODNX
,62',6
Petroleum products - Determination of distillation characteristics at atmospheric pressure
(ISO/DIS 3405:2009)
Mineralölerzeugnisse - Bestimmung des Destillationsverlaufes bei Atmosphärendruck
(ISO/DIS 3405:2009)
Produits pétroliers - Détermination des caractéristiques de distillation à pression
atmosphérique (ISO/DIS 3405:2009)
Ta slovenski standard je istoveten z: prEN ISO 3405
ICS:
75.080 Naftni proizvodi na splošno Petroleum products in
general
oSIST prEN ISO 3405:2009 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN ISO 3405:2009
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oSIST prEN ISO 3405:2009
EUROPEAN STANDARD
DRAFT
prEN ISO 3405
NORME EUROPÉENNE
EUROPÄISCHE NORM
September 2009
ICS 75.160.20 Will supersede EN ISO 3405:2000
English Version
Petroleum products - Determination of distillation characteristics
at atmospheric pressure (ISO/DIS 3405:2009)
Produits pétroliers - Détermination des caractéristiques de Mineralölerzeugnisse - Bestimmung des
distillation à pression atmosphérique (ISO/DIS 3405:2009) Destillationsverlaufes bei Atmosphärendruck (ISO/DIS
3405:2009)
This draft European Standard is submitted to CEN members for parallel enquiry. It has been drawn up by the Technical Committee
CEN/TC 19.
If this draft becomes a European Standard, 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.
This draft European Standard was established by CEN 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 Management Centre has the
same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,
Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are aware and to
provide supporting documentation.
Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without notice and
shall not be referred to as a European Standard.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2009 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN ISO 3405:2009: E
worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
oSIST prEN ISO 3405:2009
prEN ISO 3405:2009 (E)
Contents Page
Foreword .3
2
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oSIST prEN ISO 3405:2009
prEN ISO 3405:2009 (E)
Foreword
This document (prEN ISO 3405:2009) has been prepared by Technical Committee ISO/TC 28 "Petroleum
products and lubricants" in collaboration with 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 document is currently submitted to the parallel Enquiry.
This document will supersede EN ISO 3405:2000.
Endorsement notice
The text of ISO/DIS 3405:2009 has been approved by CEN as a prEN ISO 3405:2009 without any
modification.
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oSIST prEN ISO 3405:2009
DRAFT INTERNATIONAL STANDARD ISO/DIS 3405
ISO/TC 28 Secretariat: ANSI
Voting begins on: Voting terminates on:
2009-09-17 2010-02-17
INTERNATIONAL ORGANIZATION FOR STANDARDIZATION • МЕЖДУНАРОДНАЯ ОРГАНИЗАЦИЯ ПО СТАНДАРТИЗАЦИИ • ORGANISATION INTERNATIONALE DE NORMALISATION
Petroleum products — Determination of distillation
characteristics at atmospheric pressure
Produits pétroliers — Détermination des caractéristiques de distillation à pression atmosphérique
[Revision of third edition (ISO 3405:2000)]
ICS 75.080
ISO/CEN PARALLEL PROCESSING
This draft has been developed within the International Organization for Standardization (ISO), and
processed under the ISO-lead mode of collaboration as defined in the Vienna Agreement.
This draft is hereby submitted to the ISO member bodies and to the CEN member bodies for a parallel
five-month enquiry.
Should this draft be accepted, a final draft, established on the basis of comments received, will be
submitted to a parallel two-month approval vote in ISO and formal vote in CEN.
To expedite distribution, this document is circulated as received from the committee secretariat.
ISO Central Secretariat work of editing and text composition will be undertaken at publication
stage.
Pour accélérer la distribution, le présent document est distribué tel qu'il est parvenu du
secrétariat du comité. Le travail de rédaction et de composition de texte sera effectué au
Secrétariat central de l'ISO au stade de publication.
THIS DOCUMENT IS A DRAFT CIRCULATED FOR COMMENT AND APPROVAL. IT IS THEREFORE SUBJECT TO CHANGE AND MAY NOT BE
REFERRED TO AS AN INTERNATIONAL STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS BEING ACCEPTABLE FOR INDUSTRIAL, TECHNOLOGICAL, COMMERCIAL AND USER PURPOSES, DRAFT
INTERNATIONAL STANDARDS MAY ON OCCASION HAVE TO BE CONSIDERED IN THE LIGHT OF THEIR POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN NATIONAL REGULATIONS.
RECIPIENTS OF THIS DRAFT ARE INVITED TO SUBMIT, WITH THEIR COMMENTS, NOTIFICATION OF ANY RELEVANT PATENT RIGHTS OF WHICH
THEY ARE AWARE AND TO PROVIDE SUPPORTING DOCUMENTATION.
©
International Organization for Standardization, 2009
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ISO/DIS 3405
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Contents Page
Foreword. iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions. 2
4 Principle . 3
5 Apparatus . 3
6 Samples and sampling . 11
7 Preparation of apparatus . 13
8 Apparatus verification . 15
9 Procedure – Manual Apparatus. 16
10 Procedure – Automated Apparatus. 18
11 Calculations. 19
12 Expression of results . 22
13 Precision (Manual Apparatus) . 22
14 Precision (Automated Apparatus). 24
15 Test report . 26
Annex A (normative) Thermometer specifications . 27
Annex B (normative) Determination of temperature-sensor lag times. 28
Annex C (normative) Determination of specified distillation data . 29
Annex D (informative) Examples of data calculations. 31
Annex E (informative) Emulation of emergent-stem errors . 34
Annex F (informative) Examples of Test Report . 35
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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. Each 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.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 3405 was prepared by Technical Committee ISO/TC 28, Petroleum products and lubricants.
This fourth edition cancels and replaces the third edition (ISO 3405:2000), of which has been technically
revised.
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oSIST prEN ISO 3405:2009
DRAFT INTERNATIONAL STANDARD ISO/DIS 3405
Petroleum products — Determination of distillation
characteristics at atmospheric pressure
WARNING — The use of this International Standard may involve hazardous materials, operations and
equipment. This International Standard does not purport to address all of the safety problems
associated with its use. It is the responsibility of the user of this International Standard to establish
appropriate safety and health practices and to determine the applicability of regulatory limitations
prior to use.
1 Scope
This International Standard specifies a laboratory method for the determination of the distillation
characteristics of light and middle distillates derived from petroleum with initial boiling points above 0 °C and
end-points below approximately 400 °C, utilizing either manual or automated equipment. Light distillates are
typically; automotive engine petrols, automotive engine petrols with up to 10% (V/V) ethanol, and aviation
petrols. Middle distillates are typically; aviation turbine fuels, kerosines, diesel, diesel with up to 20% (V/V)
FAME, burner fuels, and marine fuels that have no appreciable quantities of residua.
NOTE 1 For the purposes of this International Standard, the term “% (V/V)” is used to represent the volume fraction of
a material.
NOTE 2 The method is applicable to petroleum products incorporating a minor constitution of components from non-
petroleum origin, but the precision data may not apply in all cases.
The distillation (volatility) characteristics of hydrocarbons have an important effect on their safety and
performance, especially in the case of fuels and solvents. The boiling range gives important information on
composition and behaviour during storage and use, and the rate of evaporation is an important factor in the
application of many solvents. Limiting values to specified distillation characteristics are applied to most
distillate petroleum product specifications in order to control end-use performance and to regulate the
formation of vapours which may form explosive mixtures with air, or otherwise escape into the atmosphere as
emissions (VOC).
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated
references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.
ISO 918:1983, Volatile organic liquids for industrial use — Determination of distillation characteristics
ISO 3170:2004, Petroleum liquids — Manual sampling
ISO 3171:1988, Petroleum liquids — Automatic pipeline sampling
ISO 4259:2006, Petroleum products — Determination and application of precision data in relation to methods
of test
ISO 4788:2005, Laboratory glassware — Graduated measuring cylinders
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3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
decomposition point
thermometer reading (corrected) which coincides with the first indications of thermal decomposition of the
liquid in the flask
NOTE Characteristic indications of thermal decomposition are an evolution of fumes and erratic thermometer
readings which usually show a decided decrease after any attempt has been made to adjust the heat.
3.2
dry point
thermometer reading (corrected) that is observed at the instant the last drop of liquid evaporates from the
lowest point in the flask; any drops or film of liquid on the side of the flask or on the thermometer are
disregarded
NOTE The end-point (final boiling point), rather than the dry point is intended for general use. The dry point can be
reported in connection with special purpose naphthas, such as those used in the paint industry. Also, it is substituted for
the end-point (final boiling point) whenever the sample is of such a nature that the precision of the end-point cannot
consistently meet the requirements given in Clause 12.
3.3
end-point
final boiling point
maximum thermometer reading (corrected) obtained during the test
NOTE This usually occurs after evaporation of all liquid from the bottom of the flask.
3.4
initial boiling point
thermometer reading (corrected) that is observed at the instant that the first drop of condensate falls from the
lower end of the condenser tube
3.5
percent evaporated
sum of the percent recovered and the percent loss
3.6
percent loss
100 minus the total recovery
NOTE Sometimes called “front-end loss”; this is the amount of uncondensed material lost in the initial stages of the
distillation.
3.7
corrected loss
percent loss corrected for barometric pressure
3.8
percent recovered
volume of condensate observed in the receiving graduated cylinder at any point in the distillation, expressed
as a percentage of the charge volume, in connection with a simultaneous temperature reading
3.9
percent recovery
maximum percent recovered, as observed in accordance with 9.10
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3.10
percent residue
volume of residue measured in accordance with 9.11, and expressed as a percentage of the charge volume
3.11
percent total recovery
combined percent recovery and residue in the flask, as determined in accordance with 10.1
3.12
thermometer reading
temperature recorded by the sensor of the saturated vapour measured in the neck of the flask below the
vapour tube, under the specified conditions of this test
3.13
temperature reading
thermometer or temperature-measurement device reading (3.12) which is corrected to 101,3 kPa barometric
pressure
3.14
emergent stem effect
offset in temperature reading caused by the use of a total immersion mercury-in-glass thermometer in the
partial immersion mode
NOTE The emergent part of the mercury column is at a lower temperature than the immersed portion, resulting in a
lower temperature reading than that obtained when the thermometer was completely immersed for calibration.
3.15
temperature lag
offset in temperature reading between a mercury-in-glass thermometer and an electronic temperature-
measurement device, caused by the different response time of the systems involved
4 Principle
The sample is assigned into one of four groups based on its composition and expected volatility
characteristics, each group defining the apparatus arrangement, condenser temperature and operational
variables. A 100 ml test portion is distilled under the specified conditions appropriate to the group into which
the sample falls, and systematic observations of thermometer readings and volumes of condensate recovered
are made. The volume of the residue in the flask is measured, and the loss on distillation recorded. The
thermometer readings are corrected for barometric pressure, and the data are then used for calculations
appropriate to the nature of the sample and the specification requirements.
5 Apparatus
5.1 General
Typical assemblies of the manual apparatus are shown in Figures 1 and 2. In addition to the basic
components described in Clause 5, automated apparatus also are equipped with a system to measure and
automatically record the vapour temperature and the associated recovered volume in the receiving cylinder.
Automated equipment manufactured in 1999 and later shall be equipped with a device to automatically shut
down power to the unit and to spray an inert gas or vapor in the chamber where the distillation flask is
mounted in the event of fire.
NOTE Some causes of fires are breakage of the distillation flask, electrical shorts, and foaming and spilling of liquid
sample through the top opening of the flask.
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5.2 Distillation flasks
The distillation flasks shall have a capacity of 125 ml and be constructed of heat-resistant glass, according to
the dimensions and tolerances shown in Figure 3.
NOTE For tests specifying the dry point, especially selected flasks with bottoms and walls of uniform thickness are
desirable.
5.3 Condenser tube and cooling bath
Typical types of condenser and cooling bath are illustrated in Figures 1 and 2.
NOTE Other types of apparatus may be used, provided that the test results obtained by their use are such as to
correlate with the results obtained with those illustrated, and to satisfy the precision criteria given in Clause 12.
5.3.1 The condenser shall be made of seamless non-corrosive metal tubing, 560 mm ± 5 mm in length, with
an outside diameter of 14 mm and a wall thickness of 0,8 mm to 0,9 mm.
NOTE Brass or stainless steel are suitable materials.
5.3.2 The condenser shall be set so that 393 mm ± 3 mm of the tube is in contact with the cooling medium,
with 50 mm ± 3 mm outside the cooling bath at the upper end, and 114 mm ± 3 mm outside at the lower end.
The portion of tube projecting at the upper end shall be set at an angle of 75 ° to the vertical. The portion of
the tube inside the cooling bath shall be either straight or bent in any suitable continuous smooth curve. The
average gradient shall be 15° ± 1° with respect to the horizontal, and no 100 mm section shall have a gradient
outside a 15° ± 3° range. The projecting lower portion of the condenser tube shall be curved downward for a
length of 76 mm and the lower end cut off at an acute angle. Provisions shall be made to enable the flow of
distillate to run down the side of the receiving graduated cylinder. Figure 4 gives an illustration of the lower
end of the condenser tube.
The flow of distillate down the side of the graduated cylinder may be accomplished either by using a drip-
deflector which is inserted in the receiver, or by having the downward length of the condenser tube curve
slightly backwards so as to ensure contact with the wall of the graduated cylinder at a point 25 mm to 32 mm
below the top of the graduated cylinder when it is in position to receive distillate.
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Key
1 Cooling bath
2 Air vents
3 Burner
4 Shield
5 Heat-resistant boards
6 Distillation flask
7 Thermometer
8 Bath cover
9 Blotting paper
10 Support
11 Graduated cylinder
12 Gas line
Figure 1 — Apparatus assembly using a gas burner
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Key
1 Graduated cylinder
2 Blotting paper
3 Thermometer
4 Distillation flask
5 Flask-support board
6 Electric heating
element
7 Flask-support
platform
8 Flask-adjusting knob
9 Indicating dial
10 Switch
11 Open bottom shield
12 Cooling bath
13 Condenser tube
14 Shield
Figure 2 — Apparatus assembly using an electric heater
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Dimensions in millimetres
Figure 3 — 125 ml flasks – Alternative neck designs
Dimensions in millimetres
Key
1 Total length 114 ± 2
2 Linear part
Approx. 38
Figure 4 — Lower end of condenser tube
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5.3.3 The volume and design of the cooling bath will depend on the cooling medium employed. The cooling
capacity of the bath shall be adequate to maintain the required temperature for the desired condenser
performance. A single cooling bath may be used for several condenser tubes.
5.4 Metal shield or enclosure for flask (manual apparatus only)
Shields shall be provided to protect the operator from damage from the unit during operation, and to protect
the distillation flask from draughts. They shall allow easy access to the distillation during operation, and be
provided with at least one window to observe the dry point at the end of the distillation.
NOTE 1 A typical shield for a unit fitted with a gas burner would be 400 mm high, 280 mm long and 200 mm wide,
made of sheet metal approximately 0,8 mm in thickness (see Figure 1).
NOTE 2 A typical shield for a unit fitted with an electric heater would be 440 mm high, 200 mm long and 200 mm wide,
made of sheet metal approximately 0,8 mm in thickness (see Figure 2).
5.5 Heat source
5.5.1 Gas burner (see Figure 1), capable of bringing over the first drop from a cold start within the time
specified, and continuing the distillation at the specified rate. A sensitive regulating valve and gas pressure
governor to give complete control of heating shall be provided.
5.5.2 Electric heater (see Figure 2), of low heat retention and adjustable from 0 W to 1 000 W.
5.6 Flask-support
5.6.1 Type 1 for use with gas burner (see Figure 1). Either a ring support of the ordinary laboratory type,
100 mm or larger in diameter, supported on a stand inside the shield, or a platform adjustable from the outside
of the shield shall be used.
The flask support board shall be constructed of ceramic or other heat-resistant material, 3 to 6 mm in
thickness and shall have a central opening conforming to the dimensions given in Table 2. The flask support
board shall be of sufficient dimension to ensure that thermal heat to the flask only comes from the central
opening and that extraneous heat to the flask other than through the central opening is minimized. The flask-
support board may be moved slightly in accordance with the directions for positioning the distillation flask so
that direct heat is applied to the flask only through the opening in this board. The position of the flask is set by
adjusting the length of the side-arm inserted into the condenser.
5.6.2 Type 2 for use with an electric heater (see Figure 2). The flask-support is a platform on top of the
electric heater and adjustable from the outside of the shield. The flask support board described in 5.6.1 is
mounted on this support. Provision shall be made for moving the upper (flask-support) board slightly in the
horizontal plane to ensure that direct heat is applied only through the specified opening in this board. The
flask-support assembly shall be able to move vertically to ensure contact of the flask-support board with the
bottom of the distillation flask during the distillation, and to allow for easy mounting and removal of the
distillation flask from the unit.
5.7 Graduated cylinders
5.7.1 Receiving cylinder, of 100 ml capacity, generally in accordance with ISO 4788. It shall be graduated at
intervals of 1 ml beginning at least at the 5 ml mark and have a graduation at the 100 ml mark. The shape of
the base shall be such that the receiver does not topple when placed empty on a surface inclined at an angle
of 13° to the horizontal. Construction details and tolerances for the graduated cylinder are shown in Figure 5.
For automated apparatus, the cylinder shall conform to the physical specifications described in this subclause,
with the exception of all graduations but that at 100 ml. Graduated cylinders for use in automated units may
also have a metal base.
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Dimensions in millimetres
Key
1 Fire polished
2 Wall thickness
3 Scale length
Figure 5 — 100 ml graduated cylinder (tolerance ± 1,0 ml)
If required, the graduated cylinder shall be immersed up to above the 100 ml graduation line in a cooling
liquid contained in a cooling bath, such as a tall-form beaker of clear glass or transparent plastic, or placed in
a thermostatically controlled air-circulation chamber.
5.7.2 Residue cylinder, of 5 ml capacity, generally in accordance with ISO 4788.
5.8 Temperature measurement system
5.8.1 Thermometers, if used, shall be of the mercury-in-glass type, nitrogen filled, graduated on the stem
and enamel backed, and shall conform to the specifications given in annex A.
CAUTIONARY NOTE — Under certain test conditions, the bulb of the thermometer can be 28 °C above
the temperature indicated, and at an indicated temperature of 371 °C, the temperat
...
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