EN 17306:2023

Liquid petroleum products - Determination of distillation characteristics at atmospheric pressure - Micro-distillation

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 20 °C and end-points below approximately 400 °C, at atmospheric pressure utilizing an automatic micro distillation apparatus.
This test method is applicable to such products as light and middle distillates, automotive spark-ignition engine fuels, automotive spark-ignition engine fuels containing up to 20 % (V/V) ethanol, aviation gasolines, aviation turbine fuels, (paraffinic) diesel fuels, FAME (B100), diesel blends up to 30 % (V/V) fatty acid methyl esters (FAME), special petroleum spirits, naphtha’s, white spirits, kerosene’s, burner fuels, and marine fuels.
The test method is also applicable to hydrocarbons with a narrow boiling range, like organic solvents or oxygenated compounds.
The test method is designed for the analysis of distillate products; it is not applicable to products containing appreciable quantities of residual material.
WARNING - The use of this document can involve hazardous materials, operations and equipment. This document does not purport to address all of the safety problems associated with its use. It is the responsibility of user of this document to take appropriate measures to ensure the safety and health of personnel prior to application of the document, and to fulfil statutory and regulatory requirements for this purpose.
NOTE   For the purpose of this document, the expression "% (V/V)" is used to represent the volume fraction.

Flüssige Mineralölerzeugnisse - Bestimmung der Destillationseigenschaften bei atmosphärischem Druck - Mikrodestillation

Dieses Dokument legt ein Laboratoriumsverfahren zur Bestimmung der Destillationseigenschaften von Leicht- und Mitteldestillaten aus Mineralöl und verwandten Produkten mit synthetischem oder biologischem Ursprung, die bei atmosphärischem Druck einen Destillationsbeginn oberhalb von 20 °C und Destillationsendpunkte unterhalb von etwa 400 °C haben, unter Verwendung eines automatischen Mikrodestillationsgeräts fest.
Dieses Prüfverfahren ist anwendbar auf Produkte wie Leicht- und Mitteldestillate, Ottokraftstoffe, Ottokraftstoffe mit einem Ethanolgehalt von bis zu 20 % (V/V), Flugbenzine, Flugturbinenkraftstoffe, (paraffinische) Dieselkraftstoffe, FAME (B100), Dieselkraftstoffmischungen mit bis zu 30 % (V/V) Fettsäuremethylester (FAME), spezielle Petroleumbenzine, Naphthas (Rohbenzine), Testbenzine, Kerosin, Brennstoffe für Brenner und Schifffahrtsbrennstoffe.
Das Prüfverfahren ist auch auf Kohlenwasserstoffe mit einem engen Siedebereich anwendbar, wie z. B. organische Lösemittel oder sauerstoffhaltige Verbindungen.
Das Prüfverfahren ist für die Analyse von Destillatprodukten ausgelegt; es ist nicht auf Produkte anwendbar, die beträchtliche Mengen an Rückstandsmaterial enthalten.
WARNUNG — Die Anwendung dieses Dokuments kann die Anwendung gefährlicher Stoffe, Arbeitsgänge und Geräte mit sich bringen. Dieses Dokument beansprucht nicht, alle damit verbundenen Sicherheitsprobleme zu behandeln. Es liegt in der Verantwortung des Anwenders dieses Dokuments, vor dessen Anwendung geeignete Maßnahmen für die Sicherheit und den Gesundheitsschutz des Personals zu ergreifen, und dafür Sorge zu tragen, dass behördliche und gesetzliche Maßnahmen eingehalten werden.
ANMERKUNG   Für den Zweck dieses Dokuments wird der Ausdruck „% (V/V)“ verwendet, um den Volumenanteil darzustellen.

Produits pétroliers liquides - Détermination des caractéristiques de distillation à la pression atmosphérique - Microdistillation

Le présent document spécifie une méthode de laboratoire pour la détermination des caractéristiques de distillation des distillats légers et moyens dérivés du pétrole et des produits connexes d'origine synthétique ou biologique dont le point d’ébullition initial est supérieur à 20 °C et le point final inférieur à environ 400 °C, à la pression atmosphérique, à l'aide d'un appareil de microdistillation automatique.
Cette méthode d'essai est applicable à des produits tels que les distillats légers et moyens, les carburants pour moteurs à allumage commandé, les carburants pour moteurs à allumage commandé contenant jusqu'à 20 % (V/V) d'éthanol, les essences aviation, les carburants pour turbines aviation, les carburants diesel (paraffiniques), les mélanges gazoles contenant jusqu'à 30 % (V/V) d'esters méthyliques d'acides gras (EMAG), les EMAG (B100), les essences spéciales, le naphta, le white spirit, le kérosène, les combustibles pour brûleurs et les carburants marins.
Cette méthode d'essai s'applique également aux hydrocarbures présentant un intervalle de distillation étroit, tels que les solvants organiques ou les composés oxygénés.
La méthode d'essai est conçue pour l'analyse des produits de distillation ; elle ne s'applique pas aux produits qui contiennent des quantités appréciables de matières résiduelles.
AVERTISSEMENT — L'utilisation du présent document peut impliquer la mise en œuvre de produits, d'opérations et d'équipements à caractère dangereux. La présente norme ne prétend pas aborder tous les problèmes de sécurité associés à son utilisation. Il incombe aux utilisateurs du présent document de prendre les mesures appropriées pour assurer la sécurité et préserver la santé du personnel avant son application, et de satisfaire aux exigences légales et réglementaires applicables à cet effet.
NOTE: Pour les besoins de ce document, l'expression "% (V/V)" est utilisée pour représenter la fraction volumique.

Tekoči naftni proizvodi - Določanje destilacijskih značilnosti pri atmosferskem tlaku - Mikrodestilacija

Ta dokument določa laboratorijsko metodo za določanje destilacijskih značilnosti lahkih in srednjih destilatov iz naftnih ter sorodnih proizvodov iz naravnih ali sintetičnih virov, ki imajo začetno vrelišče nad 20 °C in končno točko pod približno 400 °C, pri atmosferskem tlaku z avtomatsko aparaturo za mikrodestilacijo.
Ta preskusna metoda se uporablja za proizvode, kot so lahki in srednji destilati, gorivo za motorna vozila z motorjem z vžigom na iskro, gorivo za motorna vozila z motorjem z vžigom na iskro, ki vsebuje do 20 % etanola, letalski bencin, gorivo za letalske turbine, (parafinsko) dizelsko gorivo, metilni estri maščobnih kislin (FAME) – B100, mešanice dizla, ki vsebujejo do 30 % metilnih estrov maščobnih kislin, specialni bencin, nafta, beli špirit, kerozin, kurilno olje in ladijsko gorivo.
Uporablja se tudi za ogljikovodike z majhnim območjem vrelišča, kot so organska topila ali kisikove spojine.
Ta preskusna metoda je zasnovana za analizo destilacijskih proizvodov in se ne uporablja za proizvode, ki vsebujejo znatne količine ostankov materiala.

General Information

• Status: Published
• Publication Date: 31-Oct-2023
• ICS: 75.160.20 - Liquid fuels
• Technical Committee: CEN/TC 19 - Petroleum products, lubricants and related products
• Drafting Committee: CEN/TC 19/WG 40 - Distillation characteristics
• Current Stage: 6060 - Definitive text made available (DAV) - Publishing
• Start Date: 01-Nov-2023
• Due Date: 16-Mar-2023
• Completion Date: 01-Nov-2023
• Ref Project: SIST EN 17306:2024 - Liquid petroleum products - Determination of distillation characteristics at atmospheric pressure - Micro-distillation

Relations

• Replaces: EN 17306:2019 - Liquid petroleum products - Determination of distillation characteristics at atmospheric pressure - Micro-distillation
• Effective Date: 19-Jan-2023

Standards Content (Sample)

SLOVENSKI STANDARD
01-januar-2024
Nadomešča:
SIST EN 17306:2019
Tekoči naftni proizvodi - Določanje destilacijskih značilnosti pri atmosferskem
tlaku - Mikrodestilacija
Liquid petroleum products - Determination of distillation characteristics at atmospheric
pressure - Micro-distillation
Flüssige Mineralölerzeugnisse - Bestimmung der Destillationseigenschaften bei
atmosphärischem Druck - Mikrodestillation
Produits pétroliers liquides - Détermination des caractéristiques de distillation à la
pression atmosphérique - Micro-distillation
Ta slovenski standard je istoveten z: EN 17306:2023
ICS:
75.160.20 Tekoča goriva Liquid fuels
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EN 17306
EUROPEAN STANDARD
NORME EUROPÉENNE
November 2023
EUROPÄISCHE NORM
ICS 75.160.20 Supersedes EN 17306:2019
English Version
Liquid petroleum products - Determination of distillation
characteristics at atmospheric pressure - Micro-distillation
Produits pétroliers liquides - Détermination des Flüssige Mineralölerzeugnisse - Bestimmung der
caractéristiques de distillation à la pression Destillationseigenschaften bei atmosphärischem Druck
atmosphérique - Microdistillation - Mikrodestillation
This European Standard was approved by CEN on 18 September 2023.

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, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye 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
© 2023 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 17306:2023 E
worldwide for CEN national Members.

Contents Page
European foreword . 4
Introduction . 5
1 Scope . 6
2 Normative references . 6
3 Terms and definitions. 6
4 Principle . 8
5 Reagents and materials . 8
6 Apparatus . 9
6.1 Micro distillation unit . 9
6.2 Barometer for calibration . 9
6.3 Sampling device . 9
6.4 Waste beaker . 9
7 Sampling . 9
8 Apparatus preparation . 10
9 Calibration, verification and quality control . 10
9.1 General . 10
9.2 Calibration . 10
9.2.1 General . 10
9.2.2 Temperature measurement system . 10
9.2.3 Ambient pressure measuring device . 11
9.2.4 Differential pressure measuring device . 11
9.3 Instrument verification . 11
10 Procedure . 11
11 Calculation . 12
12 Expression of results . 13
13 Precision . 13
13.1 General . 13
13.2 Repeatability, r . 13
13.3 Reproducibility, R . 15
13.4 Bias . 16
13.5 Relative bias . 16
13.6 Repeatability and reproducibility for FAME. 17
13.7 Relative bias for FAME . 17
14 Test report . 18
Annex A (normative) Micro distillation apparatus . 19
A.1 Detailed description of apparatus . 19
Annex B (normative) Precision of the volume percent evaporated or recovered at a prescribed
temperature . 23
Annex C (informative) Typical samples. 24
Bibliography . 25

European foreword
This document (EN 17306:2023) has been prepared by Technical Committee CEN/TC 19
“Gaseous and liquid fuels, lubricants and related products of petroleum, synthetic and
biological origin”, the secretariat of which is held by NEN.
This European Standard shall be given the status of a national standard, either by publication of
an identical text or by endorsement, at the latest by May 2024, and conflicting national standards
shall be withdrawn at the latest by May 2024.
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 17306:2019.
In comparison with the previous edition, a bias correction explanation has been introduced,
which has no effect on the method precision.
Any feedback and questions on this document should be directed to the users’ national standards
body. A complete listing of these bodies can be found on the CEN website.
According to the CEN-CENELEC Internal Regulations, the national standards organisations 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, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden,
Switzerland, Türkiye and the United Kingdom.

Introduction
The distillation (volatility) characteristics of hydrocarbons and other liquids have an important
effect on their safety and performance, especially in the case of fuels and solvents. The boiling
range gives information on the composition, the properties, and the behaviour of the fuel during
storage and use. Volatility is the major determinant of the tendency of a hydrocarbon mixture to
produce potentially explosive vapours.
The distillation characteristics are critically important for both automotive and aviation
gasolines, affecting starting, warm-up and tendency to vapour lock at high operating temperature
or at high altitude, or both. The presence of high boiling point components in these and other fuels
can significantly affect the degree of formation of solid combustion deposits.
Distillation limits are often included in petroleum product specifications, in commercial contract
agreements, process refinery/control applications, and for compliance to regulatory rules.
This test method can be applied to contaminated products or hydrocarbon mixtures. This is
valuable for fast product quality screening, refining process monitoring, fuel adulteration control,
or other purposes including use as a portable apparatus for field testing.
This document is at of the time of publication technically equivalent to ASTM D7345 [1], on which
it is based.
This test method uses an automatic micro distillation apparatus, provides fast results using small
sample volume, and eliminates much of the operator time and subjectivity in comparison to
EN ISO 3405 or ASTM D1160 [2].

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 20 °C and end-points below
approximately 400 °C, at atmospheric pressure utilizing an automatic micro distillation
apparatus.
This test method is applicable to such products as light and middle distillates, automotive spark-
ignition engine fuels, automotive spark-ignition engine fuels containing up to 20 % (V/V) ethanol,
aviation gasolines, aviation turbine fuels, (paraffinic) diesel fuels, FAME (B100), diesel blends up
to 30 % (V/V) fatty acid methyl esters (FAME), special petroleum spirits, naphtha’s, white spirits,
kerosene’s, burner fuels, and marine fuels.
The test method is also applicable to hydrocarbons with a narrow boiling range, like organic
solvents or oxygenated compounds.
The test method is designed for the analysis of distillate products; it is not applicable to products
containing appreciable quantities of residual material.
WARNING — The use of this document can involve hazardous materials, operations and
equipment. This document does not purport to address all of the safety problems
associated with its use. It is the responsibility of user of this document to take appropriate
measures to ensure the safety and health of personnel prior to application of the
document, and to fulfil statutory and regulatory requirements for this purpose.
NOTE For the purpose of this document, the expression “% (V/V)” is used to represent the volume
fraction.
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.
EN ISO 3170, Petroleum liquids — Manual sampling (ISO 3170)
EN ISO 3171, Petroleum liquids — Automatic pipeline sampling (ISO 3171)
EN ISO 3405, Petroleum and related products from natural or synthetic sources — Determination
of distillation characteristics at atmospheric pressure (ISO 3405)
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:
— IEC Electropedia: available at https://www.electropedia.org/
— ISO Online browsing platform: available at https://www.iso.org/obp
3.1
automatic apparatus
microprocessor-controlled unit that performs the procedures of automatically controlling the
evaporation of a liquid specimen under specific conditions of this test method, collecting
measurement data and converting this data by patented algorithm in order to predict distillation
results in correlation with industry recognized reference method
3.2
corrected temperature reading
temperature readings, corrected to 101,3 kPa barometric pressure
3.3
end point
final boiling point FBP
maximum thermometer reading (corrected) obtained during the test
Note 1 to entry: This usually occurs after the evaporation of all liquid from the bottom of the distillation
flask.
Note 2 to entry: The term maximum temperature is a frequently used synonym.
3.4
flask internal pressure
pressure within the distillation flask obtained during the test by a differential pressure sensor of
automatic apparatus
Note 1 to entry: The flask internal pressure data recorded during the test is automatically converted to the
volume percent recovered or evaporated data by patented algorithm employed by automatic apparatus.
3.5
initial boiling point IBP
corrected temperature readings that corresponds to the instant of the flask internal pressure rise
observed
3.6
liquid temperature
temperature of the liquid specimen in the distillation flask during the test obtained by a liquid
temperature measuring device of automatic apparatus
3.7
percent recovered
volume of condensate observed by the automatic apparatus at any point in the distillation,
expressed as a percentage of the charge volume, in connection with a simultaneous temperature
reading
3.8
percent recovery
recovery predicted by the automatic apparatus and expressed as a percentage of the charge
volume
3.9
percent residue
volume of residue in the distillation flask expressed as a percentage of the charge volume
3.10
reference method
test method or its analogues which is widely used for expression of the distillation characteristics
of petroleum products in industry
3.11
temperature reading
adjusted vapour and liquid temperature by using an algorithm of the automatic apparatus to
mimic the same temperature lag and emergent stem effects as would be seen when using a liquid-
in-glass thermometer to determine the distillation characteristics
3.12
vapour temperature
temperature of the vapour in the distillation flask during the test obtained by a vapour
temperature measuring device of automatic apparatus
4 Principle
A sample is transferred into the distillation flask, the distillation flask is placed into position on
the automatic apparatus, and heat is applied to the bottom of the distillation flask.
The automatic apparatus measures and records sample vapour and liquid temperatures, and
pressure in the distillation flask as the sample gradually distils under atmospheric pressure
conditions. Automatic recordings are made throughout the distillation and the data stored into
the apparatus memory.
At the conclusion of the distillation, the collected data are treated by the data processing system,
converted to distillation characteristics and corrected for barometric pressure.
Test results are commonly expressed as percent recovered or evaporated versus corresponding
temperature in compliance with industry recognized standard form and reference method either
in a table or graphically, as a plot of the distillation curve.
5 Reagents and materials
5.1 Cleaning solvents, suitable for cleaning and drying the test flask such as; petroleum
naphtha and acetone.
5.2 Toluene, 99,5 % (V/V) purity.
5.3 n-Hexadecane, 99 % (V/V) purity.
5.4 Chemicals of at least 99 % purity shall be used in the calibration procedure (see 9.3).
5.5 Granular pumice stones, clean and dry fine grade pumice stones of diameter 0,8 mm to
3,0 mm, approximately 10 grains are necessary for each test.
5.6 Sample drying agent, Anhydrous sodium sulphate has been found to be suitable.
5.7 Verification fluids
5.7.1 Certified Reference Material (CRM), CRM is a stable mixture of hydrocarbon or other
stable petroleum product with a method-specific distillation characteristic established by a
method-specific interlaboratory study produced in accordance with the principles of
ISO 17034 [11] or ISO Guide 35 [3] or equivalent standards. The method-specific distillation
characteristic for each material of the current production batch is provided on the certificate of
the CRM.
5.7.2 Secondary Working Standard (SWS), a stable mixture of pure hydrocarbons, or other
petroleum product whose composition is known to remain appreciably stable. Establish the mean
value of control points and the statistical control limits for the SWS using standard statistical
techniques.
6 Apparatus
6.1 Micro distillation unit
The basic components of the micro distillation unit are the distillation flask, a condensate
recovery area with waste beaker, an enclosure for the distillation flask with the heat source and
flask support, the specimen liquid temperature measuring device, the specimen vapour
temperature measuring device, the distillation flask internal pressure measuring device, the
ambient pressure measuring device, the control systems for regulating the distillation process,
and the data processing system for converting recorded information into typical industry
recognized standard report form.
A detailed description of the apparatus is given in Annex A.
6.2 Barometer for calibration
A pressure measuring device capable of measuring local station pressure with an accuracy of
0,1 kPa (or better, at the same elevation relative to sea level where the apparatus is located.
WARNING — The barometer is only required for periodic calibration of the ambient
pressure measuring devices. Do not take readings from ordinary aneroid barometers, such
as those used at weather stations and airports, since these are pre-corrected to give sea
level readings.
6.3 Sampling device
Glass or plastics syringe capacity (10 ± 0,3) ml or constant volume dispenser capacity (10 ± 0,3)
ml.
6.4 Waste beaker
Glass approximately 200 ml capacity, outside diameter approximately 70 mm and height
approximately 130 mm fitted with a cover to reduce evaporation. The cover design shall allow
the beaker to remain open to atmospheric pressure.
7 Sampling
7.1 Unless otherwise specified, samples shall be taken as described in EN ISO 3170 or
EN ISO 3171, whereas requirements of national regulations for the sampling of the product under
test should be taken into account. At least 50 ml of sample is recommended.
7.2 The extreme sensitivity of volatility measurements to losses through evaporation and the
resulting change in composition is such as to require the utmost precaution in the drawing and
handling of volatile product samples.
7.3 Sample shall be free from any suspended solids or other insoluble contaminations. Obtain
another sample or remove solid particle by filtration. During filtration operation take care to
minimize any loss of light ends.
7.4 All samples shall be stored in a tightly closed and leak-free container away from direct
sunlight or sources of direct heat.
Protect samples containing light materials having expected initial boiling point lower than 100 °C
from excessive temperatures prior to testing. This should be accomplished by storage of the
sample container in an appropriate ice bath or refrigerator at a temperature below 10 °C. Other
samples may be stored at ambient or lower temperature.
7.5 If the sample has partially or completely solidified during storage, it shall be carefully
heated to a temperature when it is completely fluid. It shall be vigorously shaken after melting,
prior to opening the sample container, to ensure homogeneity.
7.6 Wet samples of materials that visibly contain water are not suitable for testing by this test
method. If the sample is not dry, obtain another sample that is free from suspended water.
If such a sample cannot be obtained, remove any free water by placing approximately 30 ml of
the sample to be tested in a glass conical flask containing approximately 10 g of the drying agent.
Stopper and shake gently. Allow the mixture to settle for approximately 15 min. Once the sample
shows no visible signs of water, use a decanted portion of the sample for the analysis. It is
recommended to filter the test portion from the residual or suspended drying agent. During this
drying and filtration operations take care to minimize any loss of light ends. Report that the
sample has been dried by the addition of a drying agent.
8 Apparatus preparation
Install the analyser for operation in accordance with the manufacturer’s instructions.
This instrument shall be located away from direct sunlight, sources of direct heat or air draft.
Turn on the main power switch of the analyser.
9 Calibration, verification and quality control
9.1 General
Calibrate and verify the apparatus at each of the following occasions:
— after it is installed and commissioned;
— after replacement of critical parts or components;
— whenever QC sample d
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