ISO/TS 17307:2016

Petroleum products - Biodiesel - Determination of total esters content by gas chromatography

ISO/TS 17307:2016 establishes a method for determining the total methyl ester content in fatty acid methyl ester (FAME) by gas chromatography and using an external standard. The method is suitable for biodiesel which contains esters between C6 and C26. This method allows verifying that the total ester content is greater than 96,5 % (m/m). NOTE 1 The method also allows determination of the total ethyl ester content in FAEE, but precision for this has not been established. This Technical Specification does not determine the linolenic nor the poly-unsaturated alkyl ester content. Alternative techniques, such as EN 14103[1] and EN 15779[2], respectively, are available for this. NOTE 2 For the purposes of this Technical Specification, the term "% (m/m)" is used to represent the mass fraction, µ.

Produits pétroliers — Biodiesel — Dosage de la teneur en esters totale par chromatographie en phase gazeuse

General Information

• Status: Published
• Publication Date: 18-Jan-2016
• ICS: 75.160.20 - Liquid fuels
• ICS: 75.160.40 - Biofuels
• Technical Committee: ISO/TC 28/SC 7 - Liquid Biofuels
• Drafting Committee: ISO/TC 28/SC 7 - Liquid Biofuels
• Current Stage: 9060 - Close of review
• Completion Date: 04-Mar-2029

Overview

ISO/TS 17307:2016 specifies a gas chromatography (GC) procedure for determining the total ester content of biodiesel (FAME - fatty acid methyl esters) using an external standard. The method is applicable to biodiesel esters in the carbon range C6–C26 and is intended to verify that total esters exceed 96.5 % (m/m). The procedure uses GC with a flame ionization detector (GC‑FID) and provides instructions for calibration, sample preparation, analysis and result expression.

Key topics and technical requirements

• Analyte scope: Total methyl esters (FAME); method can also quantify ethyl esters (FAEE) though precision for FAEE is not established.
• Range covered: Esters from C6 to C26. The method does NOT determine linolenic or other specific poly‑unsaturated alkyl ester contents (see Related standards).
• Instrumentation: GC with FID, on‑column injector (or equivalent), temperature‑programmed oven; typical detector temperature up to 380 °C.
• Column: Fused silica capillary, 30 m × 0.32 mm × 0.1 μm, stationary phase ~95% dimethylpolysiloxane / 5% phenyl‑methylpolysiloxane (high‑temperature capable).
• Calibration: External calibration using methyl (or ethyl) octadecanoate for most samples; when short‑chain esters (< C14) are present, a second calibration with methyl (or ethyl) dodecanoate is required. A minimum of six calibration points is recommended; acceptable regression coefficient > 0.999.
• Sample prep & injection: Typical sample mass ~0.1 g diluted in 26.8 g n‑heptane; injection volume 0.5 µL; integrate peaks from C6 to C26.
• Result expression: Total ester % (m/m) calculated from summed peak areas and calibration slope/intercept; reported to nearest 0.1 % (m/m).
• Precision & quality: Precision statistics and repeatability/reproducibility guidance are provided (interlaboratory assessment per ISO 4259). Normative sampling references: ISO 3170, ISO 3171.

Applications and users

• Quality control laboratories processing biodiesel batch release and conformity testing.
• Biodiesel producers verifying product ester content and feedstock independence.
• Regulatory and certification bodies assessing compliance with biodiesel specifications.
• R&D and analytical laboratories comparing feedstocks or optimizing production processes.

Practical benefits include a standardized GC‑FID workflow for confirming high ester purity, detecting incomplete transesterification or residual glycerides, and supporting product specification and trade.

Related standards

• EN 14103 - alternative technique for quantifying ester content (and specific unsaturates).
• EN 15779 - methods for poly‑unsaturated alkyl ester content.
• ISO 3170 / ISO 3171 - sampling of petroleum liquids.
• ISO 4259 - precision data and interlaboratory evaluation.

Note: Users must follow appropriate laboratory safety and regulatory practices when handling chemicals and high‑temperature GC equipment.

Standards Content (Sample)

TECHNICAL ISO/TS
SPECIFICATION 17307
First edition
Petroleum products — Biodiesel —
Determination of total esters content
by gas chromatography
Produits pétroliers — Biodiesel — Dosage de la teneur en esters
totale par chromatographie en phase gazeuse
PROOF/ÉPREUVE
Reference number
ISO/TS 17307:2015(E)
©
ISO 2015
ISO/TS 17307:2015(E)
© ISO 2015, Published in Switzerland
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior
written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of
the requester.
ISO copyright office
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. [phone]
Fax [phone]
[e-mail]
www.iso.org
ii © ISO 2015 – All rights reserved

ISO/TS 17307:2015(E)
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Apparatus . 2
6 Reagents and materials . 2
7 Sampling . 3
8 Procedure. 3
8.1 Preparation of the apparatus . 3
8.2 Preparation of the calibration curve . 4
8.3 Sample preparation . 4
8.4 Procedure . 4
9 Expression of results . 5
10 Precision . 5
10.1 General . 5
10.2 Repeatability, r .5
10.3 Reproducibility, R .5
11 Test report . 6
Annex A (informative) Examples of chromatograms . 7
Annex B (informative) Preparation of standard solutions .10
Bibliography .11
ISO/TS 17307:2015(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 on the meaning of ISO specific terms and expressions related to conformity
assessment, as well as information about ISO’s adherence to the WTO principles in the Technical
Barriers to Trade (TBT) see the following URL: Foreword - Supplementary information
The committee responsible for this document is ISO/TC 28, Petroleum products and related products of
synthetic or biological origin, Subcommittee SC 7, Liquid biofuels.
iv PROOF/ÉPREUVE © ISO 2015 – All rights reserved

TECHNICAL SPECIFICATION ISO/TS 17307:2015(E)
Petroleum products — Biodiesel — Determination of total
esters content by gas chromatography
WARNING — The use of this Technical Specification might involve the usage of dangerous
materials and equipment. It is the responsibility of the user to establish the appropriate security,
health and environmental practices, and to determine the applicability of regulatory limitations
before their use.
1 Scope
This Technical Specification establishes a method for determining the total methyl ester content in
fatty acid methyl ester (FAME) by gas chromatography and using an external standard. The method is
suitable for biodiesel which contains esters between C6 and C26. This method allows verifying that the
total ester content is greater than 96,5 % (m/m).
NOTE 1 The method also allows determination of the total ethyl ester content in FAEE, but precision for this
has not been established.
This Technical Specification does not determine the linolenic nor the poly-unsaturated alkyl ester
[1] [2]
content. Alternative techniques, such as EN 14103 and EN 15779 , respectively, are available for this.
NOTE 2 For the purposes of this Technical Specification, the term “% (m/m)” is used to represent the mass
fraction, µ.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. 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 4259, 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
biodiesel
fuel comprised of monoalkyl esters of fatty acids, derived from vegetable oils or animal fat
3.2
total esters
sum of concentration of all esters (C6 – C26)
4 Principle
A sample is analysed by gas chromatography using an external calibration method to quantify the
esters present in biodiesel regardless of the raw material used in its production.
ISO/TS 17307:2015(E)
The quantification of biodiesel samples with C18 carbon chains is performed using an analytical curve
prepared with methyl or ethyl octadecanoate. If there is presence of esters with carbon chain shorter
than C , in addition m
...

TECHNICAL ISO/TS
SPECIFICATION 17307
First edition
2016-02-01
Petroleum products — Biodiesel —
Determination of total esters content
by gas chromatography
Produits pétroliers — Biodiesel — Dosage de la teneur en esters
totale par chromatographie en phase gazeuse
Reference number
©
ISO 2016
© ISO 2016, Published in Switzerland
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior
written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of
the requester.
ISO copyright office
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. [phone]
Fax [phone]
[e-mail]
www.iso.org
ii © ISO 2016 – All rights reserved

Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Apparatus . 2
6 Reagents and materials . 2
7 Sampling . 3
8 Procedure. 3
8.1 Preparation of the apparatus . 3
8.2 Preparation of the calibration curve . 4
8.3 Sample preparation . 4
8.4 Procedure . 4
9 Expression of results . 5
10 Precision . 5
10.1 General . 5
10.2 Repeatability, r .5
10.3 Reproducibility, R .5
11 Test report . 6
Annex A (informative) Examples of chromatograms . 7
Annex B (informative) Preparation of standard solutions .10
Bibliography .11
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 on the meaning of ISO specific terms and expressions related to conformity
assessment, as well as information about ISO’s adherence to the WTO principles in the Technical
Barriers to Trade (TBT) see the following URL: Foreword - Supplementary information
The committee responsible for this document is ISO/TC 28, Petroleum products and related products of
synthetic or biological origin, Subcommittee SC 7, Liquid biofuels.
iv © ISO 2016 – All rights reserved

TECHNICAL SPECIFICATION ISO/TS 17307:2016(E)
Petroleum products — Biodiesel — Determination of total
esters content by gas chromatography
WARNING — The use of this Technical Specification might involve the usage of dangerous
materials and equipment. It is the responsibility of the user to establish the appropriate security,
health and environmental practices, and to determine the applicability of regulatory limitations
before their use.
1 Scope
This Technical Specification establishes a method for determining the total methyl ester content in
fatty acid methyl ester (FAME) by gas chromatography and using an external standard. The method is
suitable for biodiesel which contains esters between C6 and C26. This method allows verifying that the
total ester content is greater than 96,5 % (m/m).
NOTE 1 The method also allows determination of the total ethyl ester content in FAEE, but precision for this
has not been established.
This Technical Specification does not determine the linolenic nor the poly-unsaturated alkyl ester
[1] [2]
content. Alternative techniques, such as EN 14103 and EN 15779 , respectively, are available for this.
NOTE 2 For the purposes of this Technical Specification, the term “% (m/m)” is used to represent the mass
fraction, µ.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. 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 4259, 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
biodiesel
fuel comprised of monoalkyl esters of fatty acids, derived from vegetable oils or animal fat
3.2
total esters
sum of concentration of all esters (C6 – C26)
4 Principle
A sample is analysed by gas chromatography using an external calibration method to quantify the
esters present in biodiesel regardless of the raw material used in its production.
The quantification of biodiesel samples with C18 carbon chains is performed using an analytical curve
prepared with methyl or ethyl octadecanoate. If there is presence of ester
...