prEN 17306
(Main)Liquid petroleum products - Determination of distillation characteristics at atmospheric pressure - Micro-distillation
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 unter
halb von etwa 400°C haben, unter Verwendung eines automatischen Mikrodestillationsgerätes fest.
Dieses Prüfverfahren ist anwendbar auf Produkte wie Leicht- und Mitteldestillate, Ottokraftstoffe, Ottokraft
stoffe 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. organi
sche 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.
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 geeig
nete 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 dar
zustellen.
Produits pétroliers liquides - Détermination des caractéristiques de distillation à la pression atmosphérique - Micro-distillation
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 diesel 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 de la présente Norme peut impliquer la mise en oeuvre 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 de la présente norme 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
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
oSIST prEN 17306:2022
01-januar-2022
Tekoči naftni proizvodi - Določanje destilacijskih značilnosti pri atmosferskem
tlaku - Mikrodestilacija
Liquid petroleum products - Determination of distillation characteristics at atmospheric
pressure - Micro-distillationFlüssige Mineralölerzeugnisse - Bestimmung der Destillationseigenschaften bei
atmosphärischem Druck - Mikrodestillation
Produits pétroliers liquides - Détermination des caractéristiques de distillation à la
pression atmosphérique - Micro-distillationTa slovenski standard je istoveten z: prEN 17306
ICS:
75.160.20 Tekoča goriva Liquid fuels
oSIST prEN 17306:2022 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------oSIST prEN 17306:2022
---------------------- Page: 2 ----------------------
oSIST prEN 17306:2022
DRAFT
EUROPEAN STANDARD
prEN 17306
NORME EUROPÉENNE
EUROPÄISCHE NORM
January 2022
ICS 75.160.20 Will supersede EN 17306:2019
English Version
Liquid petroleum products - Determination of distillation
characteristics at atmospheric pressure - Micro-distillation
Produits pétroliers liquides - Détermination des lüssige Mineralölerzeugnisse - Bestimmung der
caractéristiques de distillation à la pression Destillationseigenschaften bei atmosphärischem Druck
atmosphérique - Micro-distillation - MikrodestillationThis draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee
CEN/TC 19.If this draft becomes a European Standard, CEN members are bound to comply with the CEN/CENELEC Internal Regulations
which stipulate the conditions for giving this European Standard the status of a national standard without any alteration.
This draft European Standard was established by CEN in three official versions (English, French, German). A version in any other
language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-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.Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are
aware and to provide supporting documentation.Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without
notice and shall not be referred to as a European Standard.EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 17306:2022 E
worldwide for CEN national Members.---------------------- Page: 3 ----------------------
oSIST prEN 17306:2022
prEN 17306:2022 (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 .................................................................................................................................................................... 13
13.5 Relative bias ................................................................................................................................................... 15
13.6 Repeatability and reproducibility for FAME ...................................................................................... 16
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 ............................................................................................................................ 21
Annex C (informative) Typical samples ............................................................................................................ 22
Bibliography ................................................................................................................................................................. 23
---------------------- Page: 4 ----------------------oSIST prEN 17306:2022
prEN 17306:2022 (E)
European foreword
This document (prEN 17306:2022) 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 document is currently submitted to the CEN Enquiry.
This document will supersede EN 17306:2019.
In comparison with the previous edition, a bias correction explanation has been introduced, which has
no effect on the method precision.---------------------- Page: 5 ----------------------
oSIST prEN 17306:2022
prEN 17306:2022 (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].---------------------- Page: 6 ----------------------
oSIST prEN 17306:2022
prEN 17306:2022 (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.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 referencesThe 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 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---------------------- Page: 7 ----------------------
oSIST prEN 17306:2022
prEN 17306:2022 (E)
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 apparatusNote 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.
3.5initial boiling point
IBP
corrected temperature readings that corresponds to the instant of the flask internal pressure rise
observed3.6
liquid temperature
temperature of the liquid specimen in the distillation flask during the test obtained by a liquid
temperature measuring device of automatic apparatus3.7
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
3.8percent recovery
recovery predicted by the automatic apparatus and expressed as a percentage of the charge volume
3.9percent residue
volume of residue in the distillation flask expressed as a percentage of the charge volume
3.10reference method
test method or its analogues which is widely used for expression of the distillation characteristics of
petroleum products in industry---------------------- Page: 8 ----------------------
oSIST prEN 17306:2022
prEN 17306:2022 (E)
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 characteristics3.12
vapour temperature
temperature of the vapour in the distillation flask during the test obtained by a vapour temperature
measuring device of automatic apparatus4 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 % 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 Apparatus6.1 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 ----------------------
oSIST prEN 17306:2022
prEN 17306:2022 (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 deviceGlass or plastics syringe capacity (10 ± 0,3) ml or constant volume dispenser capacity (10 ± 0,3) ml.
6.4 Waste beakerGlass 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
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 ----------------------oSIST prEN 17306:2022
prEN 17306:2022 (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 systemAt 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 deviceAt 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 ----------------------oSIST prEN 17306:2022
prEN 17306:2022 (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.---------------------- Page: 12 ----------------------
oSIST prEN 17306:2022
prEN 17306:2022 (E)
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.
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
automatically controls all operations. The instrument applies heating to the specimen and regulates
automatically heating power during the distillation run using specimen liquid temperature data. The
distillation conditions, distillation flask internal pressure, specimen liquid temperature, an
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.