SIST EN ISO 3405:2019
(Main)Petroleum and related products from natural or synthetic sources - Determination of distillation characteristics at atmospheric pressure (ISO 3405:2019)
Petroleum and related products from natural or synthetic sources - Determination of distillation characteristics at atmospheric pressure (ISO 3405:2019)
This document specifies a laboratory method for the determination of the distillation characteristics
of light and middle distillates derived from petroleum and related products of synthetic or biological
origin 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 petrol, automotive
engine ethanol fuel blends with up to 85 % (V/V) ethanol, and aviation petrol. Middle distillates are
typically aviation turbine fuel, kerosene, diesel, diesel with up to 30 % (V/V) FAME, burner fuel, and
marine fuels that have no appreciable quantities of residua.
NOTE For the purposes of this document, the term “% (V/V)” is used to represent the volume fraction of a
material.
The distillation (volatility) characteristics of hydrocarbons and related products of synthetic or
biological origin 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
and liquid fuel 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).
Mineralölerzeugnisse und verwandte Produkte mit natürlichem oder synthetischem Ursprung - Bestimmung des Destillationsverlaufes bei Atmosphärendruck (ISO 3405:2019)
Dieses Dokument legt ein Laborprüfverfahren mittels manuellen als auch automatisierten Prüfgeräten zur Bestimmung des Destillationsverlaufes von aus Erdöl gewonnenen niedrig siedenden Fraktionen und Mitteldestillaten und verwandten synthetischen oder biologischen Produkten fest, die einen Destillationsbeginn über 0 °C und einen Destillationsendpunkt unter etwa 400 °C aufweisen. Niedrig siedende Fraktionen sind üblicherweise Ottokraftstoffe, Benzin Ethanol Gemische mit einem Ethanolgehalt von bis zu 85 % (V/V) und Flugzeugbenzine. Mitteldestillate sind üblicherweise Flugturbinenkraftstoffe, Kerosin, Diesel, Diesel mit Gehalten an Fettsäuremethylester (FAME) bis zu 30 % (V/V), Heizöl und Schifffahrtsbrennstoffe, die keine nennenswerten Rückstandsanteile aufweisen.
ANMERKUNG Für die Zwecke dieses Dokumentes wird zur Angabe des Volumenanteiles einer Substanz der Aus-druck „% (V/V)“ verwendet.
Der Destillationsverlauf (die Flüchtigkeit) von Kohlenwasserstoffen und verwandten Produkten mit natür-lichem oder synthetischem Ursprung hat eine große Bedeutung hinsichtlich der Sicherheit und Gebrauchs-fähigkeit, vor allem bei Kraftstoffen und Lösemitteln. Der Siedebereich gibt wichtige Informatio¬nen über die Zusammensetzung und das Verhalten bei Lagerung und Gebrauch, und die Verdampfungsrate ist ein wichtiger Faktor bei der Verwendung vieler Lösemittel. In den meisten Anforderungen für Destillate auf Mineralölbasis und flüssige Brennstoffe werden Grenzwerte für den Destillationsverlauf festgelegt, um die Endgebrauchsfähigkeit zu kontrollieren und die Bildung von Dämpfen zu begrenzen, die möglicherweise mit Luft explosionsfähige Gemische bilden oder auch als Emissionen (en: volatile organic compounds, VOC) in die Atmosphäre entweichen.
Produits pétroliers et connexes d'origine naturelle ou synthétique - Détermination des caractéristiques de distillation à pression atmosphérique (ISO 3405:2019)
Le présent document spécifie une méthode de laboratoire pour la détermination des caractéristiques de distillation des distillats pétroliers légers et moyens, ainsi que des produits connexes d'origine biologique ou synthétique, ayant un point initial de distillation supérieur à 0 °C et un point final inférieur à environ 400 °C, utilisant un équipement manuel ou automatisé. Les distillats légers habituels sont les essences pour moteur automobiles, les essences pour moteurs automobiles contenant jusqu'à 85 % (V/V) d'éthanol et l'essence aviation. Les distillats moyens habituels sont le carburéacteur, le kérosène, le gazole, le gazole contenant jusqu'à 30 % (V/V) d'EMAG, le combustible de chauffe et les combustibles pour la marine qui n'ont pas une quantité de résidus appréciable.
NOTE Pour les besoins du présent document, l'expression "% (V/V)" est utilisée pour désigner la fraction volumique des produits.
Les caractéristiques de distillation (volatilité) des hydrocarbures et des produits connexes d'origine synthétique ou biologique sont importantes en matière de sécurité et de performances, en particulier dans le cas des carburants et des solvants. L'intervalle de distillation donne des renseignements importants sur la composition et le comportement pendant le stockage et l'utilisation, et la vitesse d'évaporation est une caractéristique essentielle dans l'utilisation de nombreux solvants. La plupart des spécifications applicables aux distillats pétroliers et aux carburants liquides fixent des valeurs limites pour certaines caractéristiques de distillation, afin de mieux maîtriser les performances en utilisation et pour contrôler la formation de vapeurs qui pourraient devenir explosives en présence d'air ou s'échapper dans l'atmosphère (COV).
Naftni in sorodni proizvodi iz naravnih ali sintetičnih virov - Določevanje destilacijskih značilnosti pri atmosferskem tlaku (ISO 3405:2019)
Ta dokument določa laboratorijsko metodo za določanje destilacijskih značilnosti lahkih in srednjih destilatov iz naftnih in sorodnih proizvodov iz naravnih ali sintetičnih virov z začetnim vreliščem nad 0 °C in končno točko pod približno 400 °C pri uporabi ročne ali avtomatske opreme. Lahki destilati so običajno bencin za avtomobilski motor, mešanice z etanolom za avtomobilski motor z do 85-odstotno (V/V) vsebnostjo etanola in letalsko gorivo. Srednji destilati so običajno gorivo za letalske turbine, kerozin, dizel, dizel z do 30-odstotno (V/V) vsebnostjo metilnih estrov maščobnih kislin, kurilno olje in ladijska goriva, ki nimajo znatne količine ostankov.
OPOMBA: Za namene tega dokumenta se termin »% (V/V)« uporablja za prostorninski delež snovi.
Destilacijske značilnosti (hlapnost) ogljikovodikov in sorodnih proizvodov iz sintetičnih ali naravnih virov imajo pomemben učinek na njihovo varnost in lastnosti, predvsem v primeru goriv in topil. Območje vrelišča je pomembna informacija o sestavi in vedenju med skladiščenjem in uporabo, stopnja izhlapevanja pa je pomemben dejavnik pri uporabi številnih topil. Mejne vrednosti določenih destilacijskih značilnosti se uporabljajo za večino destiliranih naftnih proizvodov in specifikacij tekočih goriv, da bi nadzorovali končne lastnosti in nastajanje hlapov, ki lahko z zrakom tvorijo eksplozivne zmesi, ali kako drugače preidejo v atmosfero kot emisije (VOC).
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 3405:2019
01-julij-2019
Nadomešča:
SIST EN ISO 3405:2011
Naftni in sorodni proizvodi iz naravnih ali sintetičnih virov - Določevanje
destilacijskih značilnosti pri atmosferskem tlaku (ISO 3405:2019)
Petroleum and related products from natural or synthetic sources - Determination of
distillation characteristics at atmospheric pressure (ISO 3405:2019)
Mineralölerzeugnisse und verwandte Produkte mit natürlichem oder synthetischem
Ursprung - Bestimmung des Destillationsverlaufes bei Atmosphärendruck (ISO
3405:2019)
Produits pétroliers et connexes d'origine naturelle ou synthétique - Détermination des
caractéristiques de distillation à pression atmosphérique (ISO 3405:2019)
Ta slovenski standard je istoveten z: EN ISO 3405:2019
ICS:
75.080 Naftni proizvodi na splošno Petroleum products in
general
SIST EN ISO 3405:2019 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 3405:2019
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SIST EN ISO 3405:2019
EN ISO 3405
EUROPEAN STANDARD
NORME EUROPÉENNE
May 2019
EUROPÄISCHE NORM
ICS 75.080 Supersedes EN ISO 3405:2011
English Version
Petroleum and related products from natural or synthetic
sources - Determination of distillation characteristics at
atmospheric pressure (ISO 3405:2019)
Produits pétroliers et connexes d'origine naturelle ou Mineralölerzeugnisse und verwandte Produkte mit
synthétique - Détermination des caractéristiques de natürlichem oder synthetischem Ursprung -
distillation à pression atmosphérique (ISO 3405:2019) Bestimmung des Destillationsverlaufes bei
Atmosphärendruck (ISO 3405:2019)
This European Standard was approved by CEN on 7 March 2019.
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, Serbia, 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: Rue de la Science 23, B-1040 Brussels
© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 3405:2019 E
worldwide for CEN national Members.
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SIST EN ISO 3405:2019
EN ISO 3405:2019 (E)
Contents Page
European foreword . 3
2
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SIST EN ISO 3405:2019
EN ISO 3405:2019 (E)
European foreword
This document (EN ISO 3405:2019) has been prepared by Technical Committee ISO/TC 28 "Petroleum
and related products, fuels and lubricants from natural or synthetic sources" 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 November 2019, and conflicting national standards
shall be withdrawn at the latest by November 2019.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN ISO 3405:2011.
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, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.
Endorsement notice
The text of ISO 3405:2019 has been approved by CEN as EN ISO 3405:2019 without any modification.
3
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SIST EN ISO 3405:2019
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SIST EN ISO 3405:2019
INTERNATIONAL ISO
STANDARD 3405
Fifth edition
2019-03
Petroleum and related products
from natural or synthetic sources —
Determination of distillation
characteristics at atmospheric
pressure
Produits pétroliers et connexes d'origine naturelle ou synthétique —
Détermination des caractéristiques de distillation à pression
atmosphérique
Reference number
ISO 3405:2019(E)
©
ISO 2019
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SIST EN ISO 3405:2019
ISO 3405:2019(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2019
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting
on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address
below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2019 – All rights reserved
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SIST EN ISO 3405:2019
ISO 3405:2019(E)
Contents Page
Foreword .v
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) . 4
5.5 Heat source(s) . 8
5.6 Flask-support . 8
5.7 Graduated cylinders . 9
5.8 Temperature measurement system .10
5.9 Centring device .10
5.10 Barometer .10
6 Samples and sampling .12
6.1 Sample grouping .12
6.2 Sample maintenance prior to testing .12
6.2.1 General.12
6.2.2 Groups 1 and 2 .13
6.2.3 Groups 3 and 4 .13
6.3 Removing water from sample .13
6.3.1 General.13
6.3.2 Groups 1 and 2 .14
6.3.3 Groups 3 and 4 .14
7 Preparation of apparatus .14
8 Apparatus verification .16
8.1 Level follower .16
8.2 Electronic temperature-measurement devices .16
8.3 Electronic pressure measuring device .17
9 Procedure — Manual apparatus .17
10 Procedure — Automated apparatus .20
11 Calculations.21
12 Expression of results .24
13 Precision (Manual Apparatus) .25
13.1 General .25
13.2 Repeatability .26
13.3 Reproducibility .26
14 Precision (automated apparatus).27
14.1 General .27
14.2 Repeatability .27
14.3 Reproducibility .27
14.4 Bias .28
14.4.1 Bias .28
14.4.2 Relative bias .29
15 Test report .29
Annex A (normative) Thermometer specifications .30
© ISO 2019 – All rights reserved iii
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SIST EN ISO 3405:2019
ISO 3405:2019(E)
Annex B (normative) Determination of temperature-sensor lag times .31
Annex C (normative) Determination of specified distillation data .32
Annex D (informative) Examples of data calculations .34
Annex E (informative) Emulation of emergent-stem errors .37
Annex F (informative) Examples of a test report .38
Bibliography .40
iv © ISO 2019 – All rights reserved
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SIST EN ISO 3405:2019
ISO 3405:2019(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.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/directives).
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. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www .iso .org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to the
World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see www .iso
.org/iso/foreword .html.
This document was prepared by Technical Committee ISO/TC 28, Petroleum and related products, fuels
and lubricants from natural or synthetic sources.
This fifth edition cancels and replaces the fourth edition (ISO 3405:2011), which has been technically
revised. The main changes compared to the previous edition are as follows:
— extension of the scope to include synthetic and biological products in general and automotive petrol-
ethanol blends and to diesel with up to 30 % (V/V) FAME specifically;
[1]
— the procedure has been aligned with ASTM D86 and ASTM International has granted usage of its
precision data on 5 July 2017;
— update of the precision (for automated apparatus) for groups 1, 2, and 3, with the slope-based
[2]
precision obtained from a 2010 Interlaboratory Study ;
— for T95, group 4 now has a valid range of 260 °C to 360 °C and an updated precision, as a review of
a 2006 Interlaboratory Study revealed the absence of some group 4 samples having a final boiling
point near 360 °C, as well final boiling points above;
— the test report example in Annex F has been updated as group 0 is not addressed since the fourth
edition of this document;
— introduction of a solution for the replacement of mercury-in-glass thermometers.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www .iso .org/members .html.
© ISO 2019 – All rights reserved v
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SIST EN ISO 3405:2019
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SIST EN ISO 3405:2019
INTERNATIONAL STANDARD ISO 3405:2019(E)
Petroleum and related products from natural or synthetic
sources — Determination of distillation characteristics at
atmospheric pressure
WARNING — The use of this document can involve hazardous materials, operations and
equipment. This document does not purport to address all the safety problems associated with
its use. It is the responsibility of users of this document to take appropriate measures to ensure
the safety and health of personnel prior to the application of the standard, and to determine the
applicability of any other restrictions for this purpose.
1 Scope
This document specifies a laboratory method for the determination of the distillation characteristics
of light and middle distillates derived from petroleum and related products of synthetic or biological
origin 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 petrol, automotive
engine ethanol fuel blends with up to 85 % (V/V) ethanol, and aviation petrol. Middle distillates are
typically aviation turbine fuel, kerosene, diesel, diesel with up to 30 % (V/V) FAME, burner fuel, and
marine fuels that have no appreciable quantities of residua.
NOTE For the purposes of this document, the term “% (V/V)” is used to represent the volume fraction of a
material.
The distillation (volatility) characteristics of hydrocarbons and related products of synthetic or
biological origin 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
and liquid fuel 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 documents are referred to in the text in such a way that some or all of their content
constitutes requirements 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 4788, Laboratory glassware — Graduated measuring cylinders
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https: //www .iso .org/obp
© ISO 2019 – All rights reserved 1
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SIST EN ISO 3405:2019
ISO 3405:2019(E)
— IEC Electropedia: available at https: //www .electropedia .org/
3.1
decomposition point
thermometer reading (corrected) which coincides with the first indications of thermal decomposition
of the liquid in the flask
Note 1 to entry: 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
being disregarded
Note 1 to entry: 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 precision requirements given in Clauses 13 or 14.
3.3
final boiling point
end-point maximum thermometer reading (corrected) obtained during the test
Note 1 to entry: 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
calculated amount of uncondensed material
Note 1 to entry: 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 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 or 10.10
3.10
percent residue
volume of residue measured in accordance with 9.11 or 10.11, and expressed as a percentage of the
charge volume
2 © ISO 2019 – All rights reserved
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SIST EN ISO 3405:2019
ISO 3405:2019(E)
3.11
percent total recovery
combined percent recovery and residue in the flask, as determined in accordance with 11.1
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
standard 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 1 to entry: 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 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 from 1999 onwards shall be equipped with a device to
automatically shut down power to the unit and to spray an inert gas or vapour 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.
© ISO 2019 – All rights reserved 3
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SIST EN ISO 3405:2019
ISO 3405:2019(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.
For tests specifying the dry point, especially selected flasks with bottoms and walls of uniform
thickness are recommended.
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, and to satisfy the precision criteria given
in Clauses 13 or 14.
5.3.2 The condenser shall be made of seamless n
...
SLOVENSKI STANDARD
oSIST prEN ISO 3405:2018
01-januar-2018
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Petroleum and related products from natural or synthetic sources - Determination of
distillation characteristics at atmospheric pressure (ISO/DIS 3405:2017)
Mineralölerzeugnisse und verwandte Produkte mit natürlichem oder synthetischem
Ursprung - Bestimmung des Destillationsverlaufes bei Atmosphärendruck (ISO/DIS
3405:2017)
Pétrole et produits dérivés à partir de sources naturelle ou synthétique - Détermination
des caractéristiques de distillation à pression atmosphérique (ISO/DIS 3405:2017)
Ta slovenski standard je istoveten z: prEN ISO 3405
ICS:
75.080 Naftni proizvodi na splošno Petroleum products in
general
oSIST prEN ISO 3405:2018 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN ISO 3405:2018
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oSIST prEN ISO 3405:2018
DRAFT INTERNATIONAL STANDARD
ISO/DIS 3405
ISO/TC 28 Secretariat: NEN
Voting begins on: Voting terminates on:
2017-10-23 2018-01-15
Petroleum and related products from natural or synthetic
sources — Determination of distillation characteristics at
atmospheric pressure
Pétrole et produits dérivés à partir de sources naturelle ou synthétique — Détermination des
caractéristiques de distillation à pression atmosphérique
ICS: 75.080
THIS DOCUMENT IS A DRAFT CIRCULATED
This document is circulated as received from the committee secretariat.
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
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ISO/DIS 3405:2017(E)
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©
PROVIDE SUPPORTING DOCUMENTATION. ISO 2017
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ISO/DIS 3405:2017(E) ISO/DIS 3405:2017(E)
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
Bibliography . 37
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ii © ISO 2017 – All rights reserved
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oSIST prEN ISO 3405:2018
ISO/DIS 3405:2017(E)
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
Bibliography . 37
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ISO/DIS 3405:2017(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.
The procedures used to develop this document and those intended for its further maintenance are described
in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of
ISO documents should be noted. This document was drafted in accordance with the editorial rules of the
ISO/IEC Directives, Part 2 (see www.iso.org/directives).
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. Details of any patent
rights identified during the development of the document will be in the Introduction and/or on the ISO list of
patent declarations received (see www.iso.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment,
as well as information about ISO's adherence to the World Trade Organization (WTO) principles in the
Technical Barriers to Trade (TBT) see the following URL: www.iso.org/iso/foreword.html.
The committee responsible for this document is ISO/TC 28, Petroleum and related products, fuels and
lubricants from natural or synthetic sources. This International Standard includes content and data, with
[1]
permission of ASTM International, from ASTM D86 , copyright ASTM International.
This fifth edition cancels and replaces the fourth edition (ISO 3405:2010). The following updates have been
taken into account:
— extension of the scope to synthetic and biological products in general and to automotive petrol-ethanol
blends and to B30 biodiesel specifically;
— the procedure has been aligned with ASTM D86 [1] and ASTM International has granted usage of its
precision data on 5 July 2017;
— update of the precision (for automated apparatus) for Groups 1, 2, and 3, with the slope based precision
obtained from a 2010 Interlaboratory Study [2];
— for T95, Group 4 has a valid range now of 260 °C to 360 °C and an updated precision, as review of a
2006 Interlaboratory Study revealed the absence of some Group 4 samples having boiling point near
360 °C, as well final boiling points are above;
— introduction of a solution for the replacement of mercury-in-glass thermometers.
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oSIST prEN ISO 3405:2018
DRAFT INTERNATIONAL STANDARD ISO/DIS 3405:2017(E)
Petroleum and related products from natural or synthetic
sources — Determination of distillation characteristics at
atmospheric pressure
WARNING — The use of this Standard can involve hazardous materials, operations and equipment.
This Standard does not purport to address all of the safety problems associated with its use. It is the
responsibility of users of this standard to take appropriate measures to ensure the safety and health
of personnel prior to the application of the standard, and fulfil statutory and regulatory requirements
for this purpose.
1 Scope
This document specifies a laboratory method for the determination of the distillation characteristics of light and
middle distillates derived from petroleum and related products of synthetic or biological origin 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 petrol, automotive engine ethanol fuel blends with
up to 85 % (V/V) ethanol, and aviation petrol. Middle distillates are typically; aviation turbine fuel, kerosene,
diesel, diesel with up to 30 % (V/V) FAME, burner fuel, and marine fuels that have no appreciable quantities of
residua.
NOTE For the purposes of this document, the term “% (V/V)” is used to represent the volume fraction of a material.
The distillation (volatility) characteristics of hydrocarbons and related products of synthetic or biological origin
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 and liquid fuel 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, 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, 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 1 to entry: 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 1 to entry: 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 precision requirements given in Clause 13 or 14.
3.3
end-point
final boiling point
maximum thermometer reading (corrected) obtained during the test
NOTE 1 to entry: 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 1 to entry: 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 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 standard
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 1 to entry: 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 vapour 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.
For tests specifying the dry point, especially selected flasks with bottoms and walls of uniform thickness are
recommended.
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, 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 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° +/- 3° 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 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 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.
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 480 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).
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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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oSIST prEN ISO 3405:2018
ISO/DIS 3405:2017(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
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Dimensions in millimetres
Figure 3 — 125 ml flasks – Alternative neck designs
Dimensions in millimetres
Key
1 Total length 114 3
2 Linear part
Approx. 38
Figure 4 — Lower end of condenser tube
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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.
5.6.2 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 +/- 1.0ml 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. Receiving cylinders for use in automated units may
also have a metal base.
If required, the receiving 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.
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Dimensions in millimetres
Key
1 Fire polished
2 Wall thickness
3 Scale length
Figure 5 — 100 ml receiving cylinder (tolerance 1,0 ml)
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.
CAUT
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