Petroleum products - Determination of boiling range distribution - Gas chromatography method (ISO 3924:2010)

This International Standard specifies a method for the determination of the boiling-range distribution of petroleum products. The method is applicable to petroleum products and fractions with a final boiling point of 538 °C or lower at atmospheric pressure as determined by this International Standard. This International Standard is not applicable to gasoline samples or gasoline components. The method is limited to products having a boiling range greater than 55 °C and having a vapour pressure sufficiently low to permit sampling at ambient temperature. The method has successfully been applied to samples containing biodiesel up to 10 %.

Mineralölerzeugnisse - Bestimmung der Siedebereichsverteilung - Gaschromatographisches Verfahren (ISO 3924:2010)

Diese Internationale Norm legt ein Verfahren zur Bestimmung des Siedeverlaufes von Mineralölerzeugnissen
fest. Das Verfahren ist anwendbar auf Mineralölprodukte und Fraktionen mit einem Siedeendpunkt von 538 °C
oder niedriger bei Atmosphärendruck, wie nach dieser Internationalen Norm bestimmt. Diese Internationale
Norm ist nicht anwendbar auf Ottokraftstoff oder dessen Komponenten. Das Verfahren ist beschränkt auf
Produkte mit einem Siedebereich größer als 55 °C und mit einem Dampfdruck, der niedrig genug ist, um eine
Probenahme bei Umgebungstemperatur zu erlauben.
Dieses Verfahren wurde bereits erfolgreich auf Proben mit Gehalten an Biodiesel bis zu 10 % (V/V) angewandt.
ANMERKUNG Für die Zwecke dieses Dokuments wird zur Angabe des Massenanteils einer Substanz der Ausdruck
% (m/m)“ und für den Volumenanteil einer Substanz der Ausdruck % (V/V) verwendet.

Produits pétroliers - Détermination de la répartition dans l'intervalle de distillation - Méthode par chromatographie en phase gazeuse (ISO 3924:2010)

L'ISO 3924:2010 spécifie une méthode pour déterminer la répartition dans l'intervalle de distillation des produits pétroliers. La méthode est applicable aux produits pétroliers et aux fractions pétrolières dont le point final de distillation est inférieur ou égal à 538 °C à la pression atmosphérique quand il est déterminé selon l'ISO 3924:2010. L'ISO 3924:2010 n'est pas applicable aux échantillons d'essences ou aux composés à base d'essences. La méthode est limitée aux produits dont l'intervalle de distillation est supérieur à 55 °C et dont la pression de vapeur est suffisamment basse pour permettre un échantillonnage à la température ambiante.
L'ISO 3924:2010 a été appliquée avec succès à des échantillons contenant du biodiesel jusqu'à 10 %.

Naftni proizvodi - Določevanje destilacijskega območja - Metoda plinske kromatografije (ISO 3924:2010)

Ta mednarodni standard opredeljuje metodo za določevanje destilacijskega območja naftnih proizvodov. Metoda se uporablja za naftne proizvode in frakcije s končnim vreliščem 538°C ali nižjim pri atmosferskem tlaku, kot določa ta mednarodni standard. Ta mednarodni standard se ne uporablja za vzorce goriva ali sestavine goriva. Metoda je omejena na proizvode, ki imajo vrelišče višje od 55°C in imajo dovolj nizek parni tlak, da omogoča vzorčenje pri temperaturi prostora. Metoda je bila uspešno uporabljena za vzorce, ki vsebujejo biodizel do 10 %.

General Information

Status
Withdrawn
Public Enquiry End Date
30-Sep-2008
Publication Date
08-Mar-2010
Withdrawal Date
19-Oct-2016
Current Stage
9900 - Withdrawal (Adopted Project)
Start Date
20-Oct-2016
Due Date
12-Nov-2016
Completion Date
20-Oct-2016

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SLOVENSKI STANDARD
SIST EN ISO 3924:2010
01-april-2010
1DIWQLSURL]YRGL'RORþHYDQMHGHVWLODFLMVNHJDREPRþMD0HWRGDSOLQVNH
NURPDWRJUDILMH ,62
Petroleum products - Determination of boiling range distribution - Gas chromatography
method (ISO 3924:2010)
Mineralölerzeugnisse - Bestimmung der Siedebereichsverteilung -
Gaschromatographisches Verfahren (ISO 3924:2010)
Produits pétroliers - Détermination de la répartition dans l'intervalle de distillation -
Méthode par chromatographie en phase gazeuse (ISO 3924:2010)
Ta slovenski standard je istoveten z: EN ISO 3924:2010
ICS:
75.080 Naftni proizvodi na splošno Petroleum products in
general
SIST EN ISO 3924:2010 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 3924:2010

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SIST EN ISO 3924:2010


EUROPEAN STANDARD
EN ISO 3924

NORME EUROPÉENNE

EUROPÄISCHE NORM
February 2010
ICS 75.080
English Version
Petroleum products - Determination of boiling range distribution -
Gas chromatography method (ISO 3924:2010)
Produits pétroliers - Détermination de la répartition dans Mineralölerzeugnisse - Bestimmung der
l'intervalle de distillation - Méthode par chromatographie en Siedebereichsverteilung - Gaschromatographisches
phase gazeuse (ISO 3924:2010) Verfahren (ISO 3924:2010)
This European Standard was approved by CEN on 13 February 2010.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European
Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national
standards may be obtained on application to the CEN 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 Management Centre has the same status as the
official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,
Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.






EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2010 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 3924:2010: E
worldwide for CEN national Members.

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SIST EN ISO 3924:2010
EN ISO 3924:2010 (E)
Contents Page
Foreword .3
2

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SIST EN ISO 3924:2010
EN ISO 3924:2010 (E)
Foreword
This document (EN ISO 3924:2010) 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, in collaboration with Technical Committee ISO/TC 28 "Petroleum products and
lubricants".
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 August 2010, and conflicting national standards shall be withdrawn at
the latest by August 2010.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech
Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia,
Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain,
Sweden, Switzerland and the United Kingdom.
3

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SIST EN ISO 3924:2010

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SIST EN ISO 3924:2010

INTERNATIONAL ISO
STANDARD 3924
Third edition
2010-02-15

Petroleum products — Determination of
boiling range distribution — Gas
chromatography method
Produits pétroliers — Détermination de la répartition dans l'intervalle de
distillation — Méthode par chromatographie en phase gazeuse




Reference number
ISO 3924:2010(E)
©
ISO 2010

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SIST EN ISO 3924:2010
ISO 3924:2010(E)
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All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,
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Published in Switzerland

ii © ISO 2010 – All rights reserved

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SIST EN ISO 3924:2010
ISO 3924:2010(E)
Contents Page
Foreword .iv
1 Scope.1
2 Normative references.1
3 Terms and definitions .1
4 Principle.2
5 Reagents and materials .2
6 Apparatus.4
7 Sampling.6
8 Preparation of apparatus.6
9 Calibration.9
10 Procedure.12
11 Calculation .13
12 Expression of results.13
13 Precision.14
14 Test report.15
Annex A (informative) Calculation of ISO 3405-equivalent data .16
Annex B (informative) Accelerated analysis .18
Annex C (informative) Boiling points of non-normal alkane hydrocarbons .20
Bibliography.24

© ISO 2010 – All rights reserved iii

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SIST EN ISO 3924:2010
ISO 3924:2010(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies
(ISO member bodies). The work of preparing International Standards is normally carried out through ISO
technical committees. Each member body interested in a subject for which a technical committee has been
established has the right to be represented on that committee. International organizations, governmental and
non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the
International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 3924 was prepared by the European Committee for Standardization (CEN) Technical Committee
CEN/TC 19, Gaseous and liquid fuels, lubricants and related products of petroleum, synthetic and biological
origin, in collaboration with Technical Committee ISO/TC 28, Petroleum products and lubricants, in
accordance with the Agreement on technical cooperation between ISO and CEN (Vienna Agreement).
[3] [4]
This method is harmonized with the analogous IP 406 and ASTM D2887 methods.
This third edition cancels and replaces the second edition (ISO 3924:1999), to which two additional
informative annexes, Annexes A and B, have been added and some updating on definitions has been
incorporated. (The Annex A in ISO 3924:1999 has become Annex C in this revised edition.) Annex A basically
contains a table for a correlation of certain data with those obtained using the ISO 3405 method and some
extra wording to the basic procedure, without changing the scope. With this information, the revised ISO 3924
becomes an updated document, describing the method actually in practice without changing the basic
procedure. The data presented in Annex A allow a reference in modern, global specifications, such as for
aviation fuels. This underlines the fact that availability of these chemical data in an ISO method supports their
use in these specific fields.
Also, because ISO 3924 is extensively used and referenced in many fuel specifications and there is a
requirement for a faster method, Annex B describes a method that, without any instrumental adaptation,
reduces the analysis time by a factor 5.

iv © ISO 2010 – All rights reserved

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SIST EN ISO 3924:2010
INTERNATIONAL STANDARD ISO 3924:2010(E)

Petroleum products — Determination of boiling range
distribution — Gas chromatography method
WARNING — The use of this International Standard may involve hazardous materials, operations and
equipment. This International Standard does not purport to address all of the safety problems
associated with its use. It is the responsibility of the user of this International Standard to establish
appropriate safety and health practices and determine the applicability of regulatory limitations prior
to use.
1 Scope
This International Standard specifies a method for the determination of the boiling-range distribution of
petroleum products. The method is applicable to petroleum products and fractions with a final boiling point of
538 °C or lower at atmospheric pressure as determined by this International Standard. This International
Standard is not applicable to gasoline samples or gasoline components. The method is limited to products
having a boiling range greater than 55 °C and having a vapour pressure sufficiently low to permit sampling at
ambient temperature.
The method has successfully been applied to samples containing biodiesel up to 10 %.
NOTE For the purposes of this International Standard, the term “% (m/m)” is used to represent the mass fraction of a
material.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated
references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.
ISO 3170:2004, Petroleum liquids — Manual sampling
ISO 3171:1988, Petroleum liquids — Automatic pipeline sampling
ISO 3405:2000, Petroleum products — Determination of distillation characteristics at atmospheric pressure
ISO 4259:2006, Petroleum products — Determination and application of precision data in relation to methods
of test
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
initial boiling point
IBP
temperature corresponding to the retention time at which a net area count equal to 0,5 % of the total sample
area under the chromatogram is obtained
© ISO 2010 – All rights reserved 1

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SIST EN ISO 3924:2010
ISO 3924:2010(E)
3.2
final boiling point
FBP
temperature corresponding to the retention time at which a net area count equal to 99,5 % of the total sample
area under the chromatogram is obtained
3.3
slice rate
number of data slices acquired per unit of time used to integrate the continuous (analogue) chromatographic
detector response during an analysis
NOTE The slice rate is expressed in hertz (for example slices per second).
4 Principle
A sample is introduced into a gas chromatographic column, which separates hydrocarbons in the order of
increasing boiling point. The column temperature is raised at a reproducible rate and the area under the
chromatogram is recorded throughout the analysis. Boiling temperatures are assigned to the time axis from a
calibration curve, obtained under the same conditions by running a known mixture of hydrocarbons covering
the boiling range expected in the sample. From these data, the boiling range distribution is obtained.
[6]
Annex A presents a correlation model for the calculation of physical distillation (ISO 3405-, IP 123 - or
[5]
ASTM D86 -equivalent data) from boiling-range distribution analysis by gas chromatography determined
following this International Standard.
Annex B describes an alternative, accelerated analysis.
5 Reagents and materials
5.1 Stationary phase for columns, non-polar, that elutes hydrocarbons in boiling-point order.
NOTE The following materials have been used successfully as liquid phases:
a) for packed columns:
⎯ silicone gum rubber UC-W98,
⎯ silicone gum rubber GE-SE-30,
⎯ silicone gum rubber OV-1,
⎯ silicone gum rubber OV-101;
b) for capillary columns:
⎯ polydimethylsiloxane.
5.2 Solid support for packed columns, usually consisting of crushed fire brick or chromatographic
diatomaceous earth.
The particle size and support loading shall be such as to give optimum resolution and analysis time.
NOTE In general, support loadings of 3 % to 10 % have been found most satisfactory.
5.3 Carrier gas, consisting of helium or hydrogen for use with thermal conductivity detectors, or nitrogen,
helium or argon for use with flame ionization detectors.
5.4 Calibration mixture, consisting of an accurately weighed mixture of hydrocarbons covering the range
from C to C and dissolved in carbon disulfide (5.6).
5 44
2 © ISO 2010 – All rights reserved

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SIST EN ISO 3924:2010
ISO 3924:2010(E)
The following mixture of n-alkanes has been found to be satisfactory for most samples: C , C , C , C , C ,
5 6 7 8 9
C , C , C , C , C , C , C , C , C , C , C , C . At least one component of the mixture shall have a
10 12 14 16 18 20 24 28 32 36 40 44
boiling point lower than the initial boiling point of the sample and at least one component shall have a boiling
point higher than the final boiling point of the sample. The boiling points of alkanes are listed in Table 1.
Table 1 — Boiling points of normal alkanes
Carbon number Boiling point Carbon number Boiling point
°C °C
2 −89 24 391
3 25 402
−42
4 0 26 412
5 36 27 422
6 69 28 431
7 98 29 440
8 126 30 449
9 151 31 458
10 174 32 466
11 196 33 474
12 216 34 481
13 235 35 489
14 254 36 496
15 271 37 503
16 287 38 509
17 302 39 516
18 316 40 522
19 330 41 528
20 344 42 534
21 356 43 540
22 369 44 545
23 380
[1]
NOTE It is believed that API Project 44 provided the original normal paraffin boiling point data that were listed in the first and
second editions of this International Standard. However, over the years some of the data contained in both API Project 44
(Thermodynamics Research Center Hydrocarbon Project) and the test methods have changed, and they are no longer equivalent. This
table represents the current normal paraffin boiling point values accepted by ISO, ASTM and the Energy Institute.
NOTE It is recommended that the final concentration for packed columns be approximately 10 parts by volume of the
hydrocarbon mixture to 100 parts by volume of carbon disulfide and for capillary columns, approximately 1 part by volume
of the hydrocarbon mixture to 100 parts by volume of carbon disulfide.
If the test sample contains significant quantities of n-alkanes that can be identified on the chromatogram,
these peaks may be used as internal boiling-point calibration points. However, it is advisable to use the
calibration mixture to verify peak identifications.
© ISO 2010 – All rights reserved 3

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SIST EN ISO 3924:2010
ISO 3924:2010(E)
Propane and butane can be added non-quantitatively to the calibration mixture, if necessary, to comply with
5.4. This may be done by bubbling a small amount of the gaseous hydrocarbon into a septum-sealed vial of
the calibration mixture using a gas syringe.
If stationary phases other than those listed in 5.1, Note, are used, the retention times of a few alkylbenzenes,
such as o-xylene, n-butylbenzene, 1,3,5-tri-isopropylbenzene, n-decylbenzene and n-tetradecylbenzene,
across the boiling range shall also be checked to confirm that the column is separating according to the boiling
point order (see Annex C).
5.5 Primary reference material, which shall be the ASTM reference gas-oil No. 1.
5.6 Carbon disulfide, reagent grade.
6 Apparatus
6.1 Chromatograph
Any gas chromatograph that has the following performance characteristics may be used.
6.1.1 Detector, of either the flame-ionization or thermal-conductivity type.
The detector shall have sufficient sensitivity to detect a mass fraction of 1,0 % (m/m) of dodecane with a peak
height of at least 10 % of full scale on the recorder under the conditions specified in this International Standard,
and without loss of resolution as defined in 8.3. When operating at this sensitivity level, the detector stability
shall be such that a baseline drift of not more than 1 % of full scale per hour is obtained. The detector shall be
capable of operating continuously at a temperature equivalent to the maximum column temperature employed.
The detector shall be connected to the column in such a way that cold spots between the detector and the
column are avoided.
NOTE It is not desirable to operate thermal conductivity detectors at a temperature higher than the maximum column
temperature employed. Operation at higher temperatures only serves to shorten the useful life of the detector and
generally contributes to higher noise levels and greater drift.
6.1.2 Column temperature programmer, capable of programmed temperature operation over a range
sufficient to establish a retention time of at least 1 min for the initial boiling point and to elute the entire sample
within the temperature ramp.
The programming rate shall be sufficiently reproducible to obtain retention time repeatability of 6 s for each
component in the calibration mixture (5.4).
If the initial boiling point is less than approximately 93 °C, an initial column temperature below ambient can be
required. However, excessively low initial column temperatures shall be avoided to ensure that the stationary
phase remains liquid. The initial temperature of the column shall be only low enough to obtain a calibration
curve meeting the requirements of this International Standard.
6.1.3 Sample inlet system, either be capable of operating continuously at a temperature equivalent to the
maximum column temperature employed or provide on-column injection with some means of programming the
entire column, including the point of sample introduction, up to the maximum temperature required.
The sample inlet system shall be connected to the chromatographic column in such a way that cold spots
between the inlet system and the column are avoided.
6.2 Column
Any column and conditions may be used, provided that, under the conditions of the test, separations are in the
order of boiling points as given in Table 1, and that the column resolution, R, is at least 3. Typical column
operating conditions are given in Tables 2 and 3.
4 © ISO 2010 – All rights reserved

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SIST EN ISO 3924:2010
ISO 3924:2010(E)
Table 2 — Typical operating conditions for packed columns
Packed columns 1 2
Column length, metres 0,7 0,5
Column outside diameter, millimetres 3,2 3,2
Stationary phase OV-101 UC-W98
Percent stationary phase 5 10
a b
Support material
G P
Support mesh size, micrometres 80/100 80/100
Initial column temperature, degrees Celsius -40 -30
Final column temperature, degrees Celsius 350 360
Programming rate, degrees Celsius per minute 10 10
Carrier gas Helium Nitrogen
Carrier gas flow, millilitres per minute 30 25
Detector FID FID
Detector temperature, degrees Celsius 370 360
Injection-port temperature, degrees Celsius 370 350
Sample size, microlitres 0,5 1
a 1)
Chromosorb® G (AW-DMS) .
b 1)
Chromosorb® P (AW) .
6.3 Recorder/plotter
This apparatus is used for plotting the chromatogram. This may be accomplished using a 0 mV to 1 mV
recording potentiometer having a full-scale response time of 2 s or less and a minimum chart width of
approximately 120 mm. Alternatively, a computer or other device may be used, provided it is capable of a
graphics presentation of the same or better quality as a potentiometric recorder.
6.4 Integrator/computer
This apparatus is used for determining the accumulated area under the chromatogram. This may be achieved
by using a computer-based chromatography data system or an electronic integrator. The integrator/computer
system shall have normal chromatographic software for measuring the retention times and areas of eluting
peaks. In addition, the system shall be capable of converting the continuously integrated detector signal into
area slices of fixed duration. These contiguous area slices, collected for the entire analysis, shall be stored for
later processing. The electronic range of the integrator/computer (e.g. 1 V) shall be within the linear range of
the detector/electrometer system used. The system shall be capable of subtracting the area slice of a blank
run from the corresponding area slice of a sample run.
Some gas chromatographs have an algorithm built into their operating software that allows storing a
mathematical model of the baseline profile in the memory. This profile may be automatically subtracted from
the detector signal on subsequent sample analyses to compensate for any baseline offset. Some integration
systems can also store and automatically subtract a blank analysis from subsequent sample analysis.

1) Chromosorb® G and Chromosorb® P are examples of suitable products available commercially. This information is
given for the convenience of users of this International Standard and does not constitute an endorsement by ISO of this
product.
© ISO 2010 – All rights reserved 5

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SIST EN ISO 3924:2010
ISO 3924:2010(E)
6.5 Flow/pressure controllers
6.5.1 If a packed column is used, the chromatograph shall be equipped with constant-flow controllers
capable of maintaining the carrier gas flow constant to ±1 % over the full operating temperature range.
6.5.2 If a wide-bore capillary column is used, the chromatograph shall be equipped with a controller of
carrier gas flow or pressure appropriate for the inlet used.
6.6 Micro-syringe
This apparatus is used to introduce the sample into the chromatograph.
Sample injection may be either manual or automatic. Automatic sample injection is preferred because it gives
better retention time precision.
7 Sampling
Unless otherwise specified, samples shall be taken by the procedures in accordance with ISO 3170 or
ISO 3171.
8 Preparation of apparatus
8.1 Column preparation
8.1.1 General
Any satisfactory method that produces a column meeting the requirements of 6.2 may be used. The column
shall be conditioned at the maximum operating temperature to reduce baseline shifts due to bleeding of the
column substrate.
8.1.2 Packed columns
An acceptable method of column conditioning that has been found effective for columns with an initial loading of
10 % liquid phase consists of purging the column with carrier gas at the normal flow rate while holding the
column at the maximum operating temperature for 12 h to 16 h.
8.1.3 Capillary columns
Capillary columns may be conditioned using the following procedure.
a) Install the column following the manufacturer's instructions. Set the column and detector gas flows.
Ensure that the system is leak-free.
b) Allow the system to purge with carrier gas at ambient temperature for at least 30 min. Then increase the
oven temperature by approximately 5 °C/min to 10 °C/min to the final operating temperature and hold for
approximately 30 min.
c) Cycle the chromatograph through its temperature programme several times until a stable baseline is
obtained.
NOTE Capillary columns with cross-linked and bonded phases are available from many manufacturers and are
usually preconditioned. These columns have much lower column bleed than packed columns.
8.2 Chromatograph
Place the chromatograph in service in accordance with the manufacturer's instructions. Typical operating
conditions are shown in Tables 2 and 3.
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SIST EN ISO 3924:2010
ISO 3924:2010(E)
If a flame ionization detector is used, the deposits formed in the detector from combustion of the silicone
decomposition products shall be removed regularly, as they change the response characteristics of the
detector.
NOTE Without any instrumental adaptation, it is possible to decrease analysis time, as described in Annex B.
Table 3 — Typical operating conditions for capillary columns
Capillary columns 3 4 5
Column length, metres 7,5 5 10
Column inner diameter, millimetres 0,53 0,53 0,53
Stationary phase DB-1 HP-1 HP-1
Stationary phase thickness, micrometres 1,5 0,88 2,65
Carrier gas Nitrogen Helium Helium
Carrier gas flow rate, millilitres per minute 30 12 20
Initial column temperature, degrees Celsius 40 35 40
Final column temperature, degrees Celsius 340 350 350
Programming rate, degrees Celsius per minute 10 10 15
Detector FID FID FID
Detector temperature, degrees Celsius 350 380 350
Injector temperature, degrees Celsius 340 Cool on-column type Programmed
temperature
vaporization type
Sample size, microlitres 0,5 1 0,2
Sample concentration, % (m/m) 25 10 Neat
8.3 Column resolution
Analyse the calibration mixture under the same conditions as those used for the samples. Using the procedure
illustrated in Figure 1, calculate the resolution, R, from the time between the C and C
...

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