oSIST prEN ISO 13032:2023
(Main)Petroleum products - Determination of low concentration of sulfur in automotive fuels - Energy-dispersive X-ray fluorescence spectrometric method (ISO/DIS 13032:2023)
Petroleum products - Determination of low concentration of sulfur in automotive fuels - Energy-dispersive X-ray fluorescence spectrometric method (ISO/DIS 13032:2023)
This document is directed specifically at the lower end of the concentration range covered in ISO 20847. By selecting the instrument type, a better signal-to-background ratio for sulfur K L2,3 emission is assured. A knowledge of the general composition of the sample for analysis is advantageous in obtaining the best test result. Compared to the previous version new fuels have been added to the scope. In addition, the precision and bias statements as well as the concentration range were updated based on results of a new interlaboratory study. This has been done for gasoline and diesel type fuels including new fuels HVO and GTL as well as for FAME type samples.
Mineralölerzeugnisse - Bestimmung niedriger Schwefelgehalte in Kraftstoffen - Energiedispersives Röntgenfluoreszenzspektrometrieverfahren (ISO/DIS 13032:2023)
Produits pétroliers et connexes - Détermination de la teneur en soufre en faible concentration dans les carburants pour automobiles - Méthode spectrométrique de fluorescence de rayons X dispersive en énergie(ISO/DIS 13032:2023)
Naftni proizvodi - Določevanje nizke koncentracije žvepla v gorivih za motorna vozila - Metoda z energijsko-disperzivno rentgensko fluorescenčno spektrometrijo (ISO/DIS 13032:2023)
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
oSIST prEN ISO 13032:2023
01-julij-2023
Naftni proizvodi - Določevanje nizke koncentracije žvepla v gorivih za motorna
vozila - Metoda z energijsko-disperzivno rentgensko fluorescenčno spektrometrijo
(ISO/DIS 13032:2023)
Petroleum products - Determination of low concentration of sulfur in automotive fuels -
Energy-dispersive X-ray fluorescence spectrometric method (ISO/DIS 13032:2023)
Mineralölerzeugnisse - Bestimmung niedriger Schwefelgehalte in Kraftstoffen -
Energiedispersives Röntgenfluoreszenzspektrometrieverfahren (ISO/DIS 13032:2023)
Produits pétroliers et connexes - Détermination de la teneur en soufre en faible
concentration dans les carburants pour automobiles - Méthode spectrométrique de
fluorescence de rayons X dispersive en énergie(ISO/DIS 13032:2023)
Ta slovenski standard je istoveten z: prEN ISO 13032
ICS:
75.160.20 Tekoča goriva Liquid fuels
oSIST prEN ISO 13032:2023 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN ISO 13032:2023
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oSIST prEN ISO 13032:2023
DRAFT INTERNATIONAL STANDARD
ISO/DIS 13032
ISO/TC 28 Secretariat: NEN
Voting begins on: Voting terminates on:
2023-05-25 2023-08-17
Petroleum and related products — Determination of low
concentration of sulfur in automotive fuels — Energy-
dispersive X-ray fluorescence spectrometric method
ICS: 75.160.20
This document is circulated as received from the committee secretariat.
THIS DOCUMENT IS A DRAFT CIRCULATED
FOR COMMENT AND APPROVAL. IT IS
ISO/CEN PARALLEL PROCESSING
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NATIONAL REGULATIONS.
ISO/DIS 13032:2023(E)
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PROVIDE SUPPORTING DOCUMENTATION. © ISO 2023
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oSIST prEN ISO 13032:2023
DRAFT INTERNATIONAL STANDARD
ISO/DIS 13032
ISO/TC 28 Secretariat: NEN
Voting begins on: Voting terminates on:
Petroleum and related products — Determination of low
concentration of sulfur in automotive fuels — Energy-
dispersive X-ray fluorescence spectrometric method
ICS: 75.160.20
This document is circulated as received from the committee secretariat.
COPYRIGHT PROTECTED DOCUMENT
THIS DOCUMENT IS A DRAFT CIRCULATED
FOR COMMENT AND APPROVAL. IT IS
© ISO 2023
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THEREFORE SUBJECT TO CHANGE AND MAY
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Reference number
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NATIONAL REGULATIONS.
Website: www.iso.org ISO/DIS 13032:2023(E)
RECIPIENTS OF THIS DRAFT ARE INVITED
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ii
© ISO 2023 – All rights reserved
PROVIDE SUPPORTING DOCUMENTATION. © ISO 2023
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oSIST prEN ISO 13032:2023
ISO/DIS 13032:2023(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 2
5 Reagents and materials . 2
5.1 Diluent oil . 2
5.2 Sulfur compounds . 2
5.2.1 General . 2
5.3 Reference materials (CRMs) . 3
5.4 Quality control samples . 3
6 Apparatus . 3
6.1 Energy-dispersive X-ray fluorescence instrument . 3
7 Sampling and sample handling .4
8 Apparatus preparation .5
8.1 Analyser . 5
8.2 Sample cups . 5
9 Calibration .5
9.1 General . 5
9.2 Preparation of primary standards . 5
9.3 Calibration standards . 6
9.4 Calibration procedure . 7
10 Procedure .8
11 Calculation . 8
12 Expression of results .9
13 Precision . 9
13.1 General . 9
13.2 Repeatability, r. 9
13.3 Reproducibility, R . 9
14 Test report . 9
Annex A (informative) Matrix effects .11
Annex B (normative) Guidelines for measuring low sulfur concentrations .13
Bibliography .15
iii
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oSIST prEN ISO 13032:2023
ISO/DIS 13032:2023(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.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
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. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www.iso.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to
the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see
www.iso.org/iso/foreword.html.
This document was prepared by Technical Committee ISO/TC 28, Petroleum and related products, fuels
and lubricants from natural or synthetic sources, in collaboration with CEN/TC 19, Gaseous and liquid
fuels, lubricants and related products of petroleum, synthetic and biological origin.
This second edition cancels and replaces the first edition (ISO 13032:2012), which has been technically
revised.
The main changes compared to the previous edition are as follows:
— extension of the Scope to include hydrotreated vegetable oil (HVO), synthetic fuel Gas To Liquid
(GTL) and neat fatty acid methyl ester (FAME);
— update of the precision details.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www.iso.org/members.html.
iv
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oSIST prEN ISO 13032:2023
ISO/DIS 13032:2023(E)
Introduction
This document is directed specifically at the lower end of the concentration range covered in ISO 20847.
By selecting the instrument type, a better signal-to-background ratio for sulfur K L emission is
2,3
assured. A knowledge of the general composition of the sample for analysis is advantageous in obtaining
the best test result. Compared to the previous version new fuels have been added to the scope. In
addition, the precision and bias statements as well as the concentration range were updated based on
results of a new interlaboratory study. This has been done for gasoline and diesel type fuels as well as
for FAME type samples.
v
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oSIST prEN ISO 13032:2023
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oSIST prEN ISO 13032:2023
DRAFT INTERNATIONAL STANDARD ISO/DIS 13032:2023(E)
Petroleum and related products — Determination of low
concentration of sulfur in automotive fuels — Energy-
dispersive X-ray fluorescence spectrometric method
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 users of this document to take appropriate measures to
ensure the safety and health of personnel prior to application of the document, and fulfil other
applicable requirements for this purpose.
1 Scope
This document specifies an energy dispersive X-ray fluorescence (EDXRF) test method for the
determination of sulfur content in automotive gasoline containing up to 3,7 % oxygen by mass [including
those blended with ethanol up to 10 % by volume] having sulfur contents in the range of 6,9 mg/kg to
56,7 mg/kg., and in diesel fuels [including those containing up to about 30 % fatty acid methyl ester
(FAME) by volume], in synthetic fuels such as Hydrotreated Vegetable Oil (HVO), Gas To Liquid (GTL)
and neat FAME having sulfur contents in the range of 5,0 mg/kg to 60,2 mg/kg.
When analysing FAME, the corresponding procedures are followed (5.2.6, 9.1, and 9.4.5).
The sulfur content in other products can be determined according to this test method; however, no
precision data for products other than automotive fuels and for results outside the specified range have
been established for this document.
For reasons of spectral overlap, this document is not applicable to leaded automotive gasoline, gasoline
having a content of greater than 8 mg/kg lead or to product and feedstock containing lead, silicon,
phosphorus, calcium, potassium or halides at concentrations greater than one tenth of the concentration
of sulfur measured or more than 10 mg/kg, whichever is the greater.
NOTE 1 IUPAC X ray line notation (S K-L ) is used in this document; the corresponding Siegbahn X-ray line
2,3
notation (S Kα ορ Σ Κα ) is being phased out.
1,2
[3]
NOTE 2 This document is based on IP test method PM DU developed originally by the Energy Institute,
London, UK.
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.
ISO 3170, Petroleum liquids — Manual sampling
ISO 3171, Petroleum liquids — Automatic pipeline sampling
ISO 17034, General requirements for the competence of reference material producers
3 Terms and definitions
No terms and definitions are listed in this document.
1
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oSIST prEN ISO 13032:2023
ISO/DIS 13032:2023(E)
ISO and IEC maintain terminological 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/
4 Principle
The test portion, in a cup fitted with an X-ray transparent window, is placed in a beam of exciting
radiation from an X-ray tube. The intensity of the sulfur K-L characteristic X-radiation is measured
2,3
and the accumulated number of counts in a given time or a count rate is compared with a calibration
curve constructed from sulfur standards covering the range of sulfur contents under examination.
NOTE The excitation radiation can be either direct or indirect via a polarizing or secondary target.
5 Reagents and materials
5.1 Diluent oil
The reference diluent oil is white oil (light paraffin oil) of high purity grade, with a maximum sulfur
content of 0,5 mg/kg. However, if only one type of matrix is to be analysed (e.g. motor gasoline),
the accuracy of results may be improved by using a matrix-matched diluent. These should match,
approximately, the aromatic and oxygen contents of the material to be analysed and should consist of
high-purity components of less than 0,5 mg/kg sulfur content.
For the analysis of FAME an adjustment of the oxygen content to the sample matrix shall be done. The
use of a mixture of white oil with methyl oleate (see 5.2.6) or organic acid (see 5.2.7) is recommended
as diluent oil,
NOTE 1 Suitable components for the matched matrix diluent include n-heptane, 2,2,4-trimethylpentane,
toluene, xylenes, ethanol, methyl tertiary butyl ether (MTBE), ethyl tertiary butyl ether (ETBE) and tertiary
amyl methyl ether (TAME).
NOTE 2 For the analysis of diesel fuels containing FAME, the accuracy of results can be improved by use of a
matched matrix composed of a mixture of white oil and methyl oleate (see 5.2.6) or organic acid, to adjust the
oxygen content and the sample matrix.
5.2 Sulfur compounds
5.2.1 General
Sulfur compounds of known sulfur content shall be used for the preparation of the primary standards.
The compounds given in 5.2.2 to 5.2.5 are suitable and their nominal sulfur contents are given. Where
the purity of these compounds is less than 99 % by mass, either the concentrations and nature of all
impurities are to be known or certified reference materials (CRMs) (5.3) shall be used instead.
5.2.2 Dibenzothiophene (DBT), with a nominal sulfur content of 17,399 % by mass, or
5.2.3 Dibutylsulfide (DBS), with a nominal sulfur content of 21,915 % by mass, or
5.2.4 Thionaphthene (Benzothiophene) (TNA), with a nominal sulfur content of 23,890 % by mass,
or
5.2.5 Dibutyldisulfide (DBDS), with a nominal sulfur content of 35,950 % by mass.
5.2.6 Methyl oleate, for use as a blank solution with a sulfur content of less than 1 mg/kg when
FAME is analyzed. Check the blank solution prior to use with the spectrometer (6.1). A signal for sulfur
2
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oSIST prEN ISO 13032:2023
ISO/DIS 13032:2023(E)
shall not be detectable (i.e. the intensity shall be lower that the intensity equivalent to 1 mg/kg). Other
oxygen containing and sulfur-free blank solutions, such as octanol, may also be used. Methyl oleate may
also be used in combination with white oil to make a matrix-matched base for diesel fuels containing
FAME.
5.2.7 Organic acid, for use as a blank solution with a sulfur content of less than 1 mg/kg when FAME
is analyzed. Check the blank solution prior to use with the spectrometer (6.1). A signal for sulfur shall
not be detectable (i.e. the intensity shall be lower that the intensity equivalent to 1 mg/kg). Other
oxygen containing and sulfur-free blank solutions, such as octanol, may also be used. Organic acid can
also be used in combination with white oil to make a matrix-matched base for diesel fuels containing
FAME.
5.3 Reference materials (CRMs)
CRMs from suppliers complying with ISO 17034, containing a range of sulfur concentrations, are
suitable alternatives to the calibration standard solutions based on compounds listed in 5.2.2 to 5.2.5
for use as calibration standards.
5.4 Quality control samples
Stable samples representative of the materials being analysed, which have a sulfur content that
is known by this test method over a substantial period of time or are supplied commercially with a
certified value. Ensure, before use, that the material is within its shelf-life.
6 Apparatus
6.1 Energy-dispersive X-ray fluorescence instrument
6.1.1 Performance characteristics.
For a 10 mg/kg sulfur standard (see 8.3), the instrument shall be capable of meeting the performance
characteristics as described by Formula (1) and Formula (2):
RR− R ≥ 1,3 (1)
()
sb b
and
CR() < 5% (2)
V s
where
R is the gross count rate (counts per second) for the sulfur region of interest for a 10 mg/kg
s
sulfur standard;
R is the gross count rate (counts per second) for the same region of interest for a blank sample
b
[diluent oil (5.1, 5.2.6, 5.2.7 or a mixture of one of the last two mentioned with 5.1)];
1)
C is the coefficient of variation (relative standard deviation
V
The predecessor term "relative standard deviation" is deprecated by the term “coefficient
of variation”.
) based on 10 individual measurements of the calibration standard.
1) The predecessor term "relative standard deviation" is deprecated by the term “coefficient of variation”.
3
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oSIST prEN ISO 13032:2023
ISO/DIS 13032:2023(E)
The 10 mg/kg sulfur standard shall be a CRM (5.3) or shall be prepared from one of the compounds
given in 5.2.2 to 5.2.7 following the procedures described in Clause 9.
6.1.2 Source of X-ray excitation, with significant flux at X-ray energies above 2,5 keV.
For X-ray detectors with a resolution greater than 200 eV at 2,3 keV, all characteristic X-ray lines
originating from the X-ray tube anode shall have an energy above 3,3 keV to ensure minimal background
variation due to scatter from the X-ray tube anode lines.
6.1.3 Removable sample cup, providing a sample depth of at least 5 mm and equipped with
replaceable X-ray transparent thin film. It is important that samples, standards, quality control
standards and blanks are measured using the same batch of film to avoid bias.
6.1.4 X-ray transparent film, the thin film has to possess the necessary combination of consistency
and chemical and physical properties.
NOTE The thin film is typically made of polypropylene, polyester, polycarbonate or other materials with a
thickness between 2 µm and 6 µm. Beware that aromatics can dissolve polycarbonate or polypropylene films. It
is then preferable to choose films made of polyesters or other chemically resistant materials. Some types of film
may contain traces of silicon, calcium and sulfur. However, the effects are normally cancelled when samples and
standards are analysed with the same batch of film.
6.1.5 X-ray detector, with a resolution not exceeding 800 eV at 2,3 keV.
6.1.6 Means of discriminating between sulfur K-L characteristic X-radiation and other
2,3
X-rays of higher energy (if required, for example filters).
6.1.7 Signal conditioning and data-handling electronics, including the functions of pulse counting
and an energy region for the S peak as a minimum.
6.2 Analytical balance, capable of weighing to the nearest 0,1 mg.
6.3 Mixer, magnetic stirrer with PTFE-coated stirring rods.
6.4 Flasks, narrow-necked, conical and made of borosilicate glass. Seal and stopper that are
compatible with the matrix, sized so that the head space is minimal.
7 Sampling and sample handling
7.1 Unless otherwise specified, samples shall be taken in accordance with the procedures described
in ISO 3170 or ISO 3171.
7.2 Store samples which contain light fractions (e.g. motor gasoline and naphtha) in a refrigerator
(spark free).
7.3 Mix samples by means of gentle shaking by hand prior to the removal of the test portion.
7.4 Allow test portions to attain ambient temperature prior to analysis.
[4] [4]
NOTE Additional sample handling recommendations are given in IP 558 (ASTM D7343 ).
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oSIST prEN ISO 13032:2023
ISO/DIS 13032:2023(E)
8 Apparatus preparation
8.1 Analyser
8.1.1 Set up the analyser (6.1) in accordance with the manufacturer’s instructions. Wherever possible,
the instrument shall be continuously switched on to maintain optimum stability.
8.1.2 Purge the optical system with helium (minimum 99 % purity) following the manufacturer's
guidelines on flush time and flow rate to ensure stability of measurements.
8.2 Sample cups
It is recommended that disposable sample cups be used. If disposable cups are not used, thoroughly
clean the sample cups with an appropriate solvent and dry before use.
Do not re-use disposable cups.
Use the same batch of window material for each run of verification and sampling analysis (see 6.1.4).
Keep handling of window material to the absolute minimum. The guidelines described in Annex B shall
be followed.
NOTE Differences in window material thickness between batches or the presence of even partial finger
marks are sufficient to affect results.
9 Calibration
9.1 General
Use either CRMs (5.3) or primary standards prepared from the selected sulfur compound (5.2) dissolved
in diluent oil (5.1) as a basis for the preparation of the two primary standards. The user shall always
validate his/her calibration with CRMs whose matrices match his/her samples. If FAME is analysed, use
a diluent blank solution in accordance with 5.1 to minimize potential matrix effects.
NOTE 1 Recommendations on selection of diluent oil are provided in Annex A. Some instruments include the
capability for instrument-based matrix correction through which accuracy can be improved. Notes on the use of
this approach to compensate for matrix effects in the test sample are provided in A.3 for information. For this
method, see the manufacturer's recommended corrections.
NOTE 2 Where matrix matching is not used and where the C:H mass ratio of the test sample is known or can
be determined, accuracy can be improved by the use of Formula (A.1) (see A.2.3) to correct the result to the C:H
mass ratio of the calibration standards, i.e. the reference diluent oil (see 5.1).
9.2 Preparation of primary standards
9.2.1 Prepare two primary standards with sulfur contents of approximately 500 mg/kg and
1 000 mg/kg. Prepare the two primary standards independently.
9.2.2 Weigh, to the nearest 0,1 mg, the appropriate quantity of the selected sulfur compound (5.2) or
CRM (5.3) (see Table 1) into a flask (6.4) and add the appropriate quantity of diluent oil (5.1), weighed to
the nearest 0,1 mg.
Mix the contents of the flask thoroughly at room temperature using the mixer (6.3).
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oSIST prEN ISO 13032:2023
ISO/DIS 13032:2023(E)
Table 1 — Composition of primary standards based on nominal sulfur contents
a b c d
Approximate sulfur content Diluent blank DBT DBS TNA DBDS
mg/kg g g g g g
1 000 50,0 0,29 0,23 0,21 0,14
500 50,0 0,144 0,114 0,105 0,07
a
See 5.2.2.
b
See 5.2.3.
c
See 5.2.4.
d
See 5.2.5.
9.2.3 Calculate the sulfur content, S, in milligrams per kilogram, to one decimal place in each case,
from the amounts of diluent oil and sulfur compound used, as described in Formula (3):
()mc +mc
ss dd
S =×10 000 (3)
()mm+
sd
where
m is the mass of sulfur compound, expressed in grams (g);
s
c is the sulfur content of the sulfur compound, expressed as a mass percentage (%);
s
c is th
...
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