Petroleum products - Determination of boiling range distribution by gas chromatography method - Part 2: Heavy distillates and residual fuels

This document specifies a method for the determination of the boiling range distribution of petroleum products by capillary gas chromatography using flame ionization detection. The document is applicable to materials having a vapour pressure low enough to permit sampling at ambient temperature, and which have a boiling range of at least 100 °C. The document is applicable to materials with initial boiling points (IBP) above 100 °C and final boiling points (FBP) above 750 °C, for example, heavy distillate fuels and residuals. The method is not applicable to bituminous samples.
The test method is not applicable for the analysis of petroleum or petroleum products containing low molecular weight components (for example naphthas, reformates, gasolines) or middle distillates like Diesel and Jet fuel.
Petroleum or petroleum products containing blending components, which contain hetero atoms (for example alcohols, ethers, acids, or esters) or residue, are not to be analysed by this test method.
NOTE   For the purposes of this document, the terms “% (m/m)” and “% (V/V)” are used to represent respectively the mass fraction and the volume fraction.
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 the user of this standard to establish appropriate safety and health practices and to determine the applicability of regulatory limitations prior to use.

Mineralölerzeugnisse - Gaschromatographische Bestimmung des Siedeverlaufes - Teil 2: Schweröle und Rückstandsöle

Produits pétroliers - Détermination de la répartition dans l'intervalle de distillation par méthode de chromatographie en phase gazeuse - Partie 2 : Fiouls lourds et fiouls résiduels

Naftni proizvodi - Določanje porazdelitve območja vrelišč z metodo plinske kromatografije - 2. del: Težki destilati in goriva iz destilacijskih ostankov

General Information

Status
Not Published
Public Enquiry End Date
01-Mar-2026
Current Stage
4020 - Public enquire (PE) (Adopted Project)
Start Date
05-Jan-2026
Due Date
25-May-2026

Relations

Effective Date
01-Feb-2026

Overview

The oSIST prEN 15199-2:2026:2026 standard, developed by the European Committee for Standardization (CEN), specifies a precise method for determining the boiling range distribution of heavy petroleum products and residual fuels via capillary gas chromatography with flame ionization detection (GC-FID). This methodology is applicable for materials with low vapor pressure that can be sampled at ambient temperature, having initial boiling points (IBP) above 100 °C and final boiling points (FBP) exceeding 750 °C. It primarily targets heavy distillate fuels and residuals and excludes bituminous samples, light molecular weight products, and blends with heteroatoms such as alcohols or esters.

This standard supersedes the previous EN 15199-2:2020 and introduces flexibility in the usage of carrier gases, improving the analytical scope for heavy petroleum fractions. It forms part of the broader EN 15199 series addressing various petroleum product distillation ranges using gas chromatography.

Key Topics

  • Scope and Applicability: Focus on heavy distillates and residual fuels with vapor pressures low enough for ambient temperature sampling, IBP >100 °C and FBP >750 °C.
  • Exclusions: Not suitable for bituminous materials, light molecular weight fuels (naphthas, reformates, gasoline), middle distillates (diesel, jet fuel), or heteroatom-containing blends.
  • Method Principle: Separation of hydrocarbons is achieved through gas chromatography via programmed temperature ramping. The boiling point correlates with retention times calibrated using a standard n-alkane mixture.
  • Reagents and Materials:
    • Carrier gases such as helium, nitrogen, or hydrogen with 99.999% purity.
    • Calibration mixtures containing n-alkanes (C5-C28) for system calibration.
    • Polyethylene wax solutions and solvents like carbon disulfide (CS2) or cyclohexane.
  • Apparatus:
    • Gas chromatograph equipped with a flame ionization detector operating continuously at high temperature.
    • Temperature programmable column for linear heating.
  • Performance Checks & Calibration:
    • Use of reference materials (e.g., Reference Material 5010) to verify boiling range distribution accuracy and recovery.
    • Calibration curves developed from known n-alkanes to assign boiling points to chromatographic data.
  • Safety Considerations: Handling of hazardous chemicals like carbon disulfide and flammable gases like hydrogen requires stringent safety measures.

Applications

The oSIST prEN 15199-2:2026 standard is critical for industries involved in petroleum refining, fuel production, and quality control of heavy distillate and residual fuel products. Its applications include:

  • Fuel Quality Characterization: Accurate boiling range profiles help define combustion properties and ensure specification compliance of heavy distillates and residual fuels.
  • Product Development: Assessment of boiling range distributions aids in formulation adjustments for optimized fuel performance or meeting environmental regulations.
  • Refinery Process Monitoring: Real-time boiling range data assists in controlling distillation units and blending processes.
  • Regulatory Compliance: Authentic and traceable boiling point data support conformity to EU and international petroleum product standards.
  • Research & Analysis: The method underpins studies of petroleum fractions’ chemical and thermal behavior, providing valuable insight into fuel chemistry.

Related Standards

The oSIST prEN 15199-2:2026 standard complements other parts of the EN 15199 series and related international standards:

  • EN 15199-1 - For middle distillates and lubricating base oils with IBP above 100 °C but FBP below 750 °C.
  • EN 15199-3 - Covers crude oils characterization from IBP below 100 °C to FBP over 750 °C.
  • EN 15199-4 - Focuses on light fractions of crude oil, including hydrocarbons up to n-nonane.
  • EN ISO 3924 - General method for boiling range distribution by gas chromatography, limited to a range below 538 °C.
  • EN ISO 3170 & EN ISO 3171 - Standards for manual and automatic sampling of hydrocarbon liquids relevant to sample collection protocols.
  • ASTM D7169 and related ASTM methods - Provide comparable approaches to boiling range analysis for fuels, sharing common principles and safety requirements.

Keywords: oSIST prEN 15199-2:2026, boiling range distribution, heavy distillates, residual fuels, gas chromatography, GC-FID method, petroleum product analysis, capillary gas chromatography, heavy fuel oils, residual fuel analysis, European standard petroleum, chromatographic boiling point, petroleum quality control, reference materials petroleum.

Draft

oSIST prEN 15199-2:2026

English language
29 pages
Preview
Preview
e-Library read for
1 day

Frequently Asked Questions

oSIST prEN 15199-2:2026 is a draft published by the Slovenian Institute for Standardization (SIST). Its full title is "Petroleum products - Determination of boiling range distribution by gas chromatography method - Part 2: Heavy distillates and residual fuels". This standard covers: This document specifies a method for the determination of the boiling range distribution of petroleum products by capillary gas chromatography using flame ionization detection. The document is applicable to materials having a vapour pressure low enough to permit sampling at ambient temperature, and which have a boiling range of at least 100 °C. The document is applicable to materials with initial boiling points (IBP) above 100 °C and final boiling points (FBP) above 750 °C, for example, heavy distillate fuels and residuals. The method is not applicable to bituminous samples. The test method is not applicable for the analysis of petroleum or petroleum products containing low molecular weight components (for example naphthas, reformates, gasolines) or middle distillates like Diesel and Jet fuel. Petroleum or petroleum products containing blending components, which contain hetero atoms (for example alcohols, ethers, acids, or esters) or residue, are not to be analysed by this test method. NOTE For the purposes of this document, the terms “% (m/m)” and “% (V/V)” are used to represent respectively the mass fraction and the volume fraction. 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 the user of this standard to establish appropriate safety and health practices and to determine the applicability of regulatory limitations prior to use.

This document specifies a method for the determination of the boiling range distribution of petroleum products by capillary gas chromatography using flame ionization detection. The document is applicable to materials having a vapour pressure low enough to permit sampling at ambient temperature, and which have a boiling range of at least 100 °C. The document is applicable to materials with initial boiling points (IBP) above 100 °C and final boiling points (FBP) above 750 °C, for example, heavy distillate fuels and residuals. The method is not applicable to bituminous samples. The test method is not applicable for the analysis of petroleum or petroleum products containing low molecular weight components (for example naphthas, reformates, gasolines) or middle distillates like Diesel and Jet fuel. Petroleum or petroleum products containing blending components, which contain hetero atoms (for example alcohols, ethers, acids, or esters) or residue, are not to be analysed by this test method. NOTE For the purposes of this document, the terms “% (m/m)” and “% (V/V)” are used to represent respectively the mass fraction and the volume fraction. 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 the user of this standard to establish appropriate safety and health practices and to determine the applicability of regulatory limitations prior to use.

oSIST prEN 15199-2:2026 is classified under the following ICS (International Classification for Standards) categories: 75.080 - Petroleum products in general; 75.160.01 - Fuels in general. The ICS classification helps identify the subject area and facilitates finding related standards.

oSIST prEN 15199-2:2026 has the following relationships with other standards: It is inter standard links to SIST EN 15199-2:2021. Understanding these relationships helps ensure you are using the most current and applicable version of the standard.

You can purchase oSIST prEN 15199-2:2026 directly from iTeh Standards. The document is available in PDF format and is delivered instantly after payment. Add the standard to your cart and complete the secure checkout process. iTeh Standards is an authorized distributor of SIST standards.

Standards Content (Sample)


SLOVENSKI STANDARD
01-februar-2026
Naftni proizvodi - Določanje porazdelitve območja vrelišč z metodo plinske
kromatografije - 2. del: Težki destilati in goriva iz destilacijskih ostankov
Petroleum products - Determination of boiling range distribution by gas chromatography
method - Part 2: Heavy distillates and residual fuels
Mineralölerzeugnisse - Gaschromatographische Bestimmung des Siedeverlaufes - Teil
2: Schweröle und Rückstandsöle
Produits pétroliers - Détermination de la répartition dans l'intervalle de distillation par
méthode de chromatographie en phase gazeuse - Partie 2 : Fiouls lourds et fiouls
résiduels
Ta slovenski standard je istoveten z: prEN 15199-2
ICS:
75.080 Naftni proizvodi na splošno Petroleum products in
general
75.160.01 Goriva na splošno Fuels in general
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

DRAFT
EUROPEAN STANDARD
NORME EUROPÉENNE
EUROPÄISCHE NORM
February 2026
ICS 75.080 Will supersede EN 15199-2:2020
English Version
Petroleum products - Determination of boiling range
distribution by gas chromatography method - Part 2:
Heavy distillates and residual fuels
Produits pétroliers - Détermination de la répartition Mineralölerzeugnisse - Gaschromatographische
dans l'intervalle de distillation par méthode de Bestimmung des Siedeverlaufes - Teil 2: Schweröle und
chromatographie en phase gazeuse - Partie 2 : Distillats Rückstandsöle
sévères et residuals
This 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, Türkiye 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
© 2026 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 15199-2:2026 E
worldwide for CEN national Members.

Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Principle . 6
5 Reagents and materials . 6
6 Apparatus . 9
7 Sampling . 11
8 Preparation of the apparatus . 11
8.1 Gas chromatograph preparation . 11
8.2 System performance check . 11
9 Sample and reference material preparation . 11
10 Calibration . 12
11 Procedure . 13
12 Visual inspection of the chromatograms . 14
13 Calculation . 15
14 Expression of results . 15
15 Precision . 15
15.1 General . 15
15.2 Repeatability . 15
15.3 Reproducibility . 15
16 Test report . 16
Annex A (normative) Calculation procedure . 18

Annex B (normative) System performance check. 21
Annex C (normative) Boiling points of n-alkanes . 23
Annex D (informative) Additional guidance for the calculation algorithm . 25
Bibliography . 29
European foreword
This document (prEN 15199-2:2026) 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 15199-2:2020.
The main change in this edition is the allowance of alternative carrier gasses.
EN 15199 consists of the following parts, under the general title Petroleum products — Determination of
boiling range distribution by gas chromatography method:
— Part 1: Middle distillates and lubricating base oils;
— Part 2: Heavy distillates and residual fuels;
— Part 3: Crude oil;
— Part 4: Light fractions of crude oil.
This document specifies the determination of boiling range distribution of materials with initial boiling
points (IBP) above 100 °C and final boiling points (FBP) above 750 °C. For testing materials with initial
boiling points (IBP) above 100 °C and final boiling point (FBP) below 750 °C, Part 1 of the standard can be
used. For testing materials with initial boiling points (IBP) below 100 °C and final boiling points (FBP)
above 750 °C, such as crude oils, Part 3 is applicable. Part 4 describes the determination of boiling range
distribution of hydrocarbons up to n-nonane in crude oil.
This document is a joint development between the EI [5], ASTM [4] and CEN.

1 Scope
This document specifies a method for the determination of the boiling range distribution of petroleum
products by capillary gas chromatography using flame ionization detection. The document is applicable
to materials having a vapour pressure low enough to permit sampling at ambient temperature, and which
have a boiling range of at least 100 °C. The document is applicable to materials with initial boiling points
(IBP) above 100 °C and final boiling points (FBP) above 750 °C, for example, heavy distillate fuels and
residuals. The method is not applicable to bituminous samples.
The test method is not applicable for the analysis of petroleum or petroleum products containing low
molecular weight components (for example naphthas, reformates, gasolines) or middle distillates like
Diesel and Jet fuel.
Petroleum or petroleum products containing blending components, which contain hetero atoms (for
example alcohols, ethers, acids, or esters) or residue, are not to be analysed by this test method.
NOTE For the purposes of this document, the terms “% (m/m)” and “% (V/V)” are used to represent respectively
the mass fraction and the volume fraction.
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 the user of this standard to establish appropriate safety and health practices and to
determine the applicability of regulatory limitations prior to use.
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, Hydrocarbon Liquids — Manual Sampling (ISO 3170)
EN ISO 3171, Petroleum liquids — Automatic pipeline sampling (ISO 3171)
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https://www.iso.org/obp
— IEC Electropedia: available at https://www.electropedia.org/
3.1
initial boiling point
IBP
temperature corresponding to the retention time at which a net area (3.7) counts equal to 0,5 % of the
total sample area (3.6) under the chromatogram is obtained (see Figure 1)
3.2
final boiling point
FBP
temperature corresponding to the retention time at which a net area (3.7) counts equal to 99,5 % of the
total sample area (3.6) under the chromatogram is obtained (see Figure 1)
Key
1 start of elution 4 end of elution
2 IBP (3.1) X retention time (minutes)
3 FBP (3.2) Y response (pA)
Figure 1 — Typical chromatogram
3.3
area slice
area resulting from the integration of the chromatographic detector signal within a specified retention
time interval
Note 1 to entry: In area slice mode peak detection parameters are bypassed and the detector signal integral is
recorded as area slices of consecutive, fixed duration time interval.
3.4
corrected area slice
area slice (3.3) corrected for baseline offset by subtraction of the exactly corresponding area slice (3.3) in
a previously recorded blank (non-sample) analysis
3.5
cumulative corrected area
accumulated sum of corrected area slices (3.4) from the beginning of the analysis through a given
retention time, ignoring any non-sample area for example of solvent
3.6
total sample area
cumulative corrected area (3.5), from the initial area point to the final area point, where the
chromatographic signal has returned to baseline after complete sample elution
3.7
net area
cumulative area counts for the sample minus the cumulative area count for the blank
3.8
recovery
ratio of the cumulative area count of the sample to that of the reference material (external standard)
corrected for dilution and material weights combined with the percentage of light ends, if applicable
4 Principle
A test portion is introduced into a gas chromatographic column, which separates hydrocarbons in the
order of increasing boiling point. The column temperature is raised at a linear reproducible rate and the
area under the chromatogram is recorded throughout the analysis. Boiling points are assigned to the time-
axis from a calibration curve, which is obtained by running a mixture of known n-alkanes covering the test
portion boiling range, under the same conditions. From these data, the boiling range distribution is
obtained. The recovery (3.8) at a specified temperature is determined by comparing the area under the
chromatogram with that of a reference standard which has been completely eluted. The temperature at
which the recovery was measured is recorded. If the found recovery is less than 100 %, the final boiling
point (3.2) is reported as 720 °C or 750 °C at that recovery.
Several SIMDIS methods are standardized test methods and each one is dedicated to a certain boiling point
range or product.
EN ISO 3924 [2] is limited to products having an initial boiling point greater than 55 °C, a final boiling
point lower than 538 °C and having a vapour pressure sufficiently low to permit sampling at ambient
temperature.
EN 15199-1 [1] is applicable to materials having a boiling range of at least 100 °C, an initial boiling points
(IBP) above 100 °C and final boiling points (FBP) below 750 °C, for example, middle distillates and
lubricating base stocks.
EN 15199-3 is applicable to crude oils. The boiling range distribution and recovery up to C or C can
100 120
be determined.
5 Reagents and materials
Unless otherwise stated, only chemicals of recognized analytical quality shall be used.
5.1 Carrier gas, helium, nitrogen or hydrogen, of at least 99,999 % (V/V) purity. Any oxygen present is
removed by a chemical resin filter.
WARNING — Follow the safety instructions from the filter supplier.
CAUTION — Helium and nitrogen are compressed gases under high pressure. Hydrogen is an extremely
flammable gas under high pressure.
5.2 Hydrogen, grade suitable for flame ionization detectors.
5.3 Compressed air, suitable for flame ionization detectors.
5.4 Alkanes, n-alkanes of at least 98 % (m/m) purity from C to C , C , C , C , C , C , C and C .
5 10 12 14 16 18 20 24 28
NOTE The calibration mixture from EN ISO 3924 [2] is also suitable.
5.5 Polyethylene wax solution .
5.6 Carbon disulfide (CS ), with a minimum purity of 99,7 % (V/V).
WARNING — Extremely flammable and toxic.
CAUTION — It is recommended that all work with CS is carried out in an explosion protected fume
cupboard.
Cyclohexane (C H )—(>99 % pure) may be used in place of CS for the preparation of the calibration
6 12 2
mixture. However, the precision of this method is based on calibration mixtures, reference material and
samples prepared with CS only.
5.7 Calibration mixture
Dissolve 0,1 g of Polyethylene wax solution (5.5) in 7 ml CS2 (5.6), warming gently if necessary. Prepare
an equal volume mixture of alkanes (5.4) and add 10 µl to the Polyethylene wax solution.
NOTE 1 Commercially available alkane standards are suitable for column performance checks.
NOTE 2 The calibration mix is used to determine the column resolution, skewness of the C peak, and retention
time versus boiling point calibration curve.
5.8 Reference materials
5.8.1 A reference material has two functions:
— External Standard: to determine the recovery (3.8) of samples by comparing the total sample area
(3.6) of the reference material with the total sample area (3.6) of the unknown sample.
— Boiling Point Distribution Standard: to check the proper functioning of the system by comparing the
results with a known boiling point distribution on a routine basis. Typical example is given in (5.8.2).
5.8.2 Reference Material 5010, a reference sample that has been analysed by laboratories
participating in the test method cooperative study. Consensus values for the boiling range distribution of
this sample are given in Table 1.
5.8.3 Binary gravimetric blend, a binary distillate mixture with boiling points ranges that gives a
baseline at the start, a baseline between the two peaks and an end time that is as close to the end of the
chromatogram as possible (see Figure 2 and Clause B.3). This mixture is used to check the relative
response of the two distillates and to check the baselines at the start, middle and end of the chromatogram.

Polywax is the tradename of fully saturated homopolymers of ethylene supplied by Baker Hughes Holdings LLC.
This information is given for the convenience of users of this document and does not constitute an endorsement by
CEN of this (these) product(s).
Table 1 — Reference material 5010
Accepted
% Maximum allowable range
reference
recovered 95,5 % confidence interval
value
°C °C
IBP 428 9
5 477 3
10 493 3
15 502 3
20 510 3
25 518 4
30 524 4
35 531 4
40 537 4
45 543 4
50 548 5
55 554 4
60 560 4
65 566 4
70 572 4
75 578 5
80 585 4
85 593 4
90 602 4
95 616 4
FBP 655 18
Key
Y response (pA)
X retention time (minutes)
Figure 2 — Typical chromatogram of binary gravimetric blend distillate
6 Apparatus
6.1 Gas chromatograph, with the following performance characteristics.
6.1.1 Flame ionization detector, connected to the column so as to avoid any cold spots. The detector
shall be capable of operating at a temperature at least equivalent to the maximum column temperature
employed in the method.
6.1.2 Column temperature programmer, capable of linear programmed temperature operation over
a range of 10 °C above ambient to 450 °C.
6.1.3 Sample inlet system, consisting of a programmable temperature vaporizer (PTV) or cold on-
column (COC) injection port. The maximum temperature of the injection device shall be equal to, or higher
than, the final oven temperature. The minimum temperature shall be low enough to prevent sample or
solvent flashback, but high enough to allow sample focusing at the front of the column. Table 2 contains
the typical operating conditions.
6.2 Column
6.2.1 The capillary column should sit just below the flame tip and it is recommended that the orifice of
the jet should be 0,6 mm minimum to prevent frequent blocking with silicones.
6.2.2 Use a metal column with 0,53 mm internal diameter and coated with methyl silicone. Commercially
available columns with film thickness (d ) = 0,09 µm (for analysis up to C ) and (d ) = 0,17 µm (for
f 120 f
analysis up to C ) have been found to be satisfactory.
The column resolution, R, shall be at least 2 and not more than 4 (see Clause B.2).
6.2.3 Use some form of column bleed compensation to obtain a stable baseline. This may be carried out
by subtraction of a column bleed profile previously obtained using exactly the same conditions as used for
the sample analysis, by injecting the same volume, using solvent for the blank run and sample dilution
from one batch taken at the same time, to avoid differences due to contamination.
Table 2 — Typical operating conditions for gas chromatograph
Unit Specification
Column length m 5
Column internal diameter mm 0,53
Column material — Ultimetal
Stationary phase — Methyl silicone
Film thickness µm 0,09 or 0,17
Initial column temperature °C 35
Final column temperature °C 430
Program rate °C/min 10
Injector initial temperature °C 100
Injector final temperature °C 430
Program rate °C/min 15
Hold time min 5
Detector temperature °C 450
Detector hydrogen flow rate (5.2) ml/min 35
Detector air flow rate (5.3) ml/min 350
Carrier gas — Helium
a
Carrier gas flow rate ml/min 19
Sample size µl 1,0
Sample concentration % (m/m) 2
Injector — PTV or COC
a
A carrier gas flow rate up to 25 ml/min maybe used to ensure all material elutes before the end of the
temperature program.
6.3 Carrier gas control
The chromatograph shall be able to deliver a constant carrier gas flow over the whole temperature range
of the analysis.
6.4 Micro-syringe, of appropriate volume, e.g. 10 µl, for introduction of 1 µl of the calibration mixture
and test portions. Plunger in needle syringes are not recommended due to excessive carry over of heavy
ends to the following analysis.
6.5 Volumetric flask, 10 ml capacity.
6.6 Refrigerator, shall be of an explosion-protected design.
6.7 Analytical balance, capable of weighing to the nearest 0,1 mg.
7 Sampling
Samples shall be taken as specified in EN ISO 3170 or EN ISO 3171 (see the requirements of national
standards or regulations for the sampling of petroleum products for further information).
Store samples in either glass or metal containers. Plastic containers for sample storage shall not be used
as prolonged contact with the sample can cause contamination of the sample due to possible leaching of
the plasticizer.
8 Preparation of the apparatus
8.1 Gas chromatograph preparation
8.1.1 Set up and operate the gas chromatograph (6.1) in accordance with the manufacturer’s
instructions.
Typical operating conditions are shown in Table 2.
8.1.2 Deposits can form on the jet from combustion of decomposition products from the liquid
stationary phase. These will affect the characteristics of the detector and shall be removed.
The following parameters are affected by deposits on the jet: increase in inlet pressure; FID difficult to
light; increase in the CS response and an off specification reference material. To clean the jet, an
ultrasonic cleaner with a suitable solvent, and a cleaning wire may be used.
8.2 System performance check
Check the system performance at the intervals given and by the procedures specified in Annex B.
9 Sample and reference material preparation
9.1 Mix the sample by shaking, warming prior to shaking where necessary.
9.2 Weigh approximately 0,1 g to 0,3 g of the sample to the nearest 0,1 mg, into a clean 10 ml volumetric
flask (6.5) and add 5 ml to 7 ml CS (5.6).
Shake the mixture to completely dissolve the test portion and then add CS (5.6) to the mark. Immediately
transfer the solution to auto test portion vials, seal, and store in a refrigerator until ready for use.
If the density of the sample is known, the test portion may be prepared on a mass/mass basis, and the
following correction applied:
100m

m
% = (1)

V  
mm

+
 
σσ
 
where
m is the mass of the test portion, in g;
m is the mass of CS (5.6), in g;
2 2
σ is the density of the test portion at 20 °C, in kg/l;
σ is the density of CS (5.6) at 20 °C, in kg/m ; (= 1,26).
2 2
The density is quoted at 20 °C as a temperature approximately ambient in most laboratories. Appropriate
adjustments should be made if the laboratory temperature is outside (20 ± 5) °C.
9.3 Sample preparation is important to calculate the recovery (3.8) of the sample. The sample may be
prepared by weighing the sample in a 10 ml flask as specified. Using this procedure, it is not required to
know or measure the density of the sample. Due to the low boiling point and the health restrictions of CS
it is preferred to prepare the sample by weight and correct for the density.
9.4 When the density is unknown and therefore no correction can be applied, the error in the recovery
calculation is minor. Not correcting for density can result in a deviation of at most 1 % on the recovery
3 3
(3.8) for the density range 700 kg/m to 1 000 kg/m .
10 Calibration
10.1 It is highly recommended to carry out the steps given in 10.2 to 10.4 each day before sample analysis.
The first run of the day shall not be a blank, a reference material or a sample, due to the possible elution
of extraneous components, which have built up in the injector, but it may be the calibration mixture (5.7).
10.2 Run the calibration mixture (5.7) as specified in Clause 11.
Take care to ensure the test portion volume chosen does not allow any peak to exceed the linear range of
the detector, or overload the column. Determine the skewness according to Annex B System Performance
(B4). A skew of > 3 indicates the sample is too concentrated and a skew of < 1 indicates an old column or
dirty liner. As a guide, 1 µl of the calibration mixture (5.7) has been found to be suitable for columns with
film thickness less than 0,17 µm.
10.3 Record the retention time of each component and plot the retent
...

Questions, Comments and Discussion

Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.

Loading comments...