EN 17306:2019

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 % ethanol, aviation gasolines, aviation turbine fuels, (paraffinic) diesel fuels, FAME (B100), diesel blends up to 30 % 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.

Flüssige Mineralölerzeugnisse - Bestimmung der Destillationseigenschaften bei atmosphärischem Druck - Mikrodestillation

Dieses Dokument legt ein Laborverfahren zur Bestimmung der Destillationseigenschaften von leichten und mittleren Destillaten aus Erdöl und verwandten Produkten mit biologischem oder synthetischem Ursprung, die bei atmosphärischem Druck einen Destillationsbeginn oberhalb von 20 °C und Destillationsendpunkte unterhalb von etwa 400 °C haben, unter Verwendung eines automatischen Mikrodestillationsgerätes 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) Fettsäure-methylester (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 Destillaten ausgelegt; es ist nicht auf Produkte anwendbar, die beträchtliche Mengen an Rückstandsmaterial enthalten.
ANMERKUNG   Für den Zweck dieser Norm wird der Ausdruck „% (V/V)“ verwendet, um den Volumenanteil darzustellen.

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

Le présent document spécifie une méthode de laboratoire pour l'identification 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 20 °C et un point final inférieur à environ 400 °C, à la pression atmosphérique en utilisant un appareillage de micro-distillation automatique.
Cette méthode d'essai s'applique aux produits tels que les distillats légers et moyens, les carburants automobiles pour moteurs à allumage par étincelle, les carburants automobiles pour moteurs à allumage par étincelle contenant jusqu'à 20 % (V/V) d'éthanol, les essences aéronautiques, les carburéacteurs, les carburants diesel (paraffiniques), les EMAG (B100), les mélanges de diesel contenant jusqu'à 30 % (V/V) d'esters méthyliques d'acides gras (EMAG), les essences pétrolières spéciales, le naphta, le white-spirit, le kérosène, les combustibles de chauffe et les combustibles pour la marine.
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.
NOTE   Pour les besoins de la présente norme, le terme «% (V/V)» est utilisé pour représenter la fraction volumique.

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

Ta dokument zajema postopek za določevanje destilacijskih značilnosti naftnih proizvodov, ki imajo pri atmosferskem tlaku območje vrelišča med 20 °C in 400 °C, z avtomatsko aparaturo za mikrodestilacijo. Preskusna metoda se uporablja za proizvode, kot so lahki in srednji destilati, gorivo za motorna vozila z motorjem z vžiganjem na iskro, gorivo za motorna vozila z motorjem z vžiganjem na iskro, ki vsebuje do 10 % (vol.) etanola, letalski bencin, gorivo za letalske turbine, dizelsko gorivo z običajno in nizko vsebnostjo žvepla, mešanice biodizla z do 30 % (vol.) biodizla, specialni petroleter, nafta, beli špirit, kerozin, kurilna olja in ladijska goriva. Uporablja se tudi za ogljikovodike z majhnim območjem vrelišča, kot so organska topila ali kisikove spojine.

General Information

• Status: Published
• Publication Date: 30-Dec-2019
• Withdrawal Date: 30-Mar-2020
• 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: 18-Sep-2019
• Due Date: 17-Mar-2020
• Completion Date: 18-Sep-2019
• Ref Project: SIST EN 17306:2019 - Liquid petroleum products - Determination of distillation characteristics at atmospheric pressure - Micro-distillation

Relations

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

Standards Content (Sample)

SLOVENSKI STANDARD
SIST EN 17306:2019
01-november-2019

Tekoči naftni proizvodi - Določevanje 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 - Distillation des produits pétroliers et de combustibles liquides à la

pression atmosphérique - Méthode Micro Distillation
Ta slovenski standard je istoveten z: EN 17306:2019
ICS:
75.160.20 Tekoča goriva Liquid fuels
SIST EN 17306:2019 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
SIST EN 17306:2019
---------------------- Page: 2 ----------------------
SIST EN 17306:2019
EN 17306
EUROPEAN STANDARD
NORME EUROPÉENNE
September 2019
EUROPÄISCHE NORM
ICS 75.160.20
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 - Micro-distillation - Mikrodestillation
This European Standard was approved by CEN on 21 June 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, 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, 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 17306:2019 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST EN 17306:2019
EN 17306:2019 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

Introduction .................................................................................................................................................................... 4

1 Scope .................................................................................................................................................................... 5

2 Normative references .................................................................................................................................... 5

3 Terms and definitions ................................................................................................................................... 5

4 Principle ............................................................................................................................................................. 7

5 Reagents and materials ................................................................................................................................. 7

6 Apparatus ........................................................................................................................................................... 7

6.1 Micro distillation unit .................................................................................................................................... 7

6.2 Barometer for calibration ............................................................................................................................ 8

6.3 Sampling device ............................................................................................................................................... 8

6.4 Waste beaker .................................................................................................................................................... 8

7 Sampling ............................................................................................................................................................. 8

8 Apparatus preparation ................................................................................................................................. 9

9 Calibration, verification and quality control......................................................................................... 9

9.1 General ................................................................................................................................................................ 9

9.2 Calibration ......................................................................................................................................................... 9

9.3 Instrument verification ................................................................................................................................. 9

9.4 Quality control .............................................................................................................................................. 10

10 Procedure........................................................................................................................................................ 10

11 Calculation ...................................................................................................................................................... 11

12 Expression of results ................................................................................................................................... 11

13 Precision .......................................................................................................................................................... 11

13.1 General ............................................................................................................................................................. 11

13.2 Repeatability, r .............................................................................................................................................. 12

13.3 Reproducibility, R ........................................................................................................................................ 13

13.4 Bias .................................................................................................................................................................... 15

13.5 Relative bias ................................................................................................................................................... 15

13.6 Repeatability and reproducibility for FAME ...................................................................................... 15

13.7 Relative bias for FAME ................................................................................................................................ 16

14 Test report ...................................................................................................................................................... 17

Annex A (normative) Micro distillation apparatus ....................................................................................... 18

A.1 Detailed description of apparatus ......................................................................................................... 18

Annex B (normative) Precision of the volume percent evaporated or recovered at a

prescribed temperature ............................................................................................................................ 22

Annex C (informative) Typical samples and group classification ........................................................... 23

Bibliography ................................................................................................................................................................. 24

---------------------- Page: 4 ----------------------
SIST EN 17306:2019
EN 17306:2019 (E)
European foreword

This document (EN 17306:2019) 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 March 2020, and conflicting national standards shall be

withdrawn at the latest by March 2020.

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. CEN not be held responsible for identifying any or all such patent rights.

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, Republic of North

Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United

Kingdom.
---------------------- Page: 5 ----------------------
SIST EN 17306:2019
EN 17306:2019 (E)
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 as 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].

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 application of the standard, and fulfil statutory and regulatory requirements for this

purpose.
---------------------- Page: 6 ----------------------
SIST EN 17306:2019
EN 17306:2019 (E)
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.

NOTE For the purpose of this standard, 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)

EN ISO 4259-1, Petroleum and related products - Precision of measurement methods and results - Part 1:

Determination of precision data in relation to methods of test (ISO 4259-1)
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 http://www.electropedia.org/
— ISO Online browsing platform: available at http://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
---------------------- Page: 7 ----------------------
SIST EN 17306:2019
EN 17306:2019 (E)
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
---------------------- Page: 8 ----------------------
SIST EN 17306:2019
EN 17306:2019 (E)
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 is 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 % purity.
5.3 n-Hexadecane, 99 % 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.

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.
---------------------- Page: 9 ----------------------
SIST EN 17306:2019
EN 17306:2019 (E)
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

and/or in accordance with the requirements of national standards or regulations for the sampling of the

product under test. At least 50 ml of sample is recommended.

7.2 The extreme sensitivity of volatility measurements to losses through evaporation and the resulting

changes 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 can be accomplished by storage of the sample container in

an appropriate ice bath or refrigerator at a temperature below 10 °C. Other samples can 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.

---------------------- Page: 10 ----------------------
SIST EN 17306:2019
EN 17306:2019 (E)
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 determinations are not in statistical control, and the reasons for QC non-

compliance have been suitably addressed.
9.2 Calibration

9.2.1 Follow the manufacturer’s instructions for verifying the correct operation of the apparatus.

9.2.2 Temperature measurement system

At intervals of not more than six months or after the system has been replaced or repaired, or both,

following the apparatus instruction manual, check the calibration of the liquid and vapour temperature

measuring sensors by distilling of pure compounds, like toluene and n-hexadecane. If the sample is solid,

heat it to about 25 °C and wait until all the material is liquid before starting the test.

NOTE The melting point of n-hexadecane is 18 °C.
9.2.3 Ambient pressure measuring device

At intervals of not more than six months, or after the system has been replaced or repaired, or both, the

ambient pressure measuring device reading of the apparatus shall be verified against a barometer (6.3).

9.2.4 Differential pressure measuring device

At intervals of not more than six months, or after the system has been replaced or repaired, or both, the

differential pressure measuring device reading of the apparatus shall be verified in accordance with the

manufacturer’s instructions.
9.3 Instrument verification

9.3.1 To verify the temperature measurement system, distil high purity toluene in accordance with this

test method and comparing the temperature reading at 50 % distilled. If the temperature reading differs

more than 0,5 °C from the expected temperature of 109,3 °C (see 9.2.2), then check the instrument

calibration (see 9.2).

9.3.2 To verify the temperature measurement system at elevated temperatures, use n-hexadecane and

record the temperature at 50 % distilled. If the temperature reading differs more than 1,0 °C from the

expected temperature of 278,6 °C (see 9.2.2), then check the instrument calibration (see 9.2).

---------------------- Page: 11 ----------------------
SIST EN 17306:2019
EN 17306:2019 (E)

NOTE The temperatures are those that would be obtained if the toluene and hexadecane were distilled using

EN ISO 3405 and are not the figures that are given as the boiling points of these materials in literature.

9.3.3 Verification of apparatus performance under dynamic conditions and wide temperature range

can be done by distillation of a Certified Reference Material (CRM, 9.4.1) or Secondary Working Standard

(SWS, 9.4.2).
9.4 Quality control
9.4.1 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 following

EN ISO 4259-1, or alternatively Guide 35 [3]. Suppliers of CRMs will provide certificates stating the

method-specific distillation characteristic for each material of the current production batch.

9.4.2 Secondary Working Standard (SWS)

SWS is 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.
10 Procedure

10.1 Material with an Initial Boiling Point of 100 °C and below — Bring the temperature of the sample

and container to a temperature at least 10 °C below the expected initial boiling point of the material

before opening the sample container.

10.2 Material with a Boiling Point above 100 °C — Bring the sample and its container to ambient

temperature. If the sample has partially or completely solidified during storage warm until fluid, then mix

by gentle shaking.

10.3 Not respecting the requirements given in 10.1 can lead to improper IBP detection on samples

containing volatile materials. If expected initial boiling point of the sample to be tested is unknown, it is

advised to make a test at ambient conditions. If the distillation result shows that the requirements of 10.1

were not respected, discard the result and repeat the test strictly respecting the conditions.

10.4 Ensure that the distillation measuring head of automatic apparatus has been allowed to reach

ambient temperature and that any residual condensate has been removed.
10.5 Check that the distillation flask is clean and dry.

10.6 Place at least 10 grains of clean and dry granular pumice stones into the distillation flask. Some

apparatus supplies a suitable boiling stone dispenser. When the sample is FAME (B100), do not use any

pumice stones.

10.7 Measure (10 ± 0,3) ml test portion using the sampling device (see 6.4). When the sample is FAME

(B100), measure (5 ± 0,3) ml test portion. Check for the presence of any bubbles and if present discard

the test portion and refill with bubble free material. Transfer the bubble free test portion to the prepared

distillation flask, taking care that none of the liquid flows into the vapour tube.

Use new disposable syringe or disposable dispenser tip for each new sampling to avoid any products

cross contamination which can cause erroneous distillation results.

10.8 Fit the distillation measurement head into its position on the distillation flask securely in

accordance with the manufacturer’s instructions.

10.9 Place the distillation flask into the heating enclosure and insert the sidearm of the distillation

flask into the sealing of the condenser tube, while also attaching the measurement head holder.

---------------------- Page: 12 ----------------------
SIST EN 17306:2019
EN 17306:2019 (E)

10.10 Position the heating source or flask support around the lower section of the distillation flask.

10.11 Close heating enclosure by positioning the protection shield to its position.

10.12 Check that a waste collection beaker is placed under the projecting lower end of the condenser

tube. Ensure that the waste collection beaker remains open to atmospheric pressure.

Monitor that the liquid level in the waste beaker does not exceed two thirds of its total capacity and drain

it on periodic intervals.

10.13 Without delay initiate the distillation process according to the apparatus manufacturer’s

instructions. From this point up to and including the termination of the measurement, the apparatus

...