EN ISO 16994:2016

SLOVENSKI STANDARD
01-oktober-2016
1DGRPHãþD
SIST EN ISO 16994:2015
7UGQDELRJRULYD'RORþHYDQMHFHORWQHJDåYHSODLQNORUD,62
Solid biofuels - Determination of total content of sulfur and chlorine (ISO 16994:2016)
Biogene Festbrennstoffe - Bestimmung des Gesamtgehaltes an Schwefel und Chlor
(ISO 16994:2016)
Biocombustibles solides - Détermination de la teneur totale en soufre et en chlore (ISO
16994:2016)
Ta slovenski standard je istoveten z: EN ISO 16994:2016
ICS:
75.160.40 Biogoriva Biofuels
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EN ISO 16994
EUROPEAN STANDARD
NORME EUROPÉENNE
August 2016
EUROPÄISCHE NORM
ICS 75.160.10; 27.190 Supersedes EN ISO 16994:2015
English Version
Solid biofuels - Determination of total content of sulfur and
chlorine (ISO 16994:2016)
Biocombustibles solides - Détermination de la teneur Biogene Festbrennstoffe - Bestimmung des
totale en soufre et en chlore (ISO 16994:2016) Gesamtgehaltes an Schwefel und Chlor (ISO
16994:2016)
This European Standard was approved by CEN on 27 July 2016.

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-CENELEC 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-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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2016 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 16994:2016 E
worldwide for CEN national Members.

Contents Page
European foreword . 3

European foreword
This document (EN ISO 16994:2016) has been prepared by Technical Committee ISO/TC 238 "Solid
biofuels" in collaboration with Technical Committee CEN/TC 335 “Solid biofuels” the secretariat of
which is held by SIS.
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 February 2017, and conflicting national standards
shall be withdrawn at the latest by February 2017.
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.
This document supersedes EN ISO 16994:2015.
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, Former Yugoslav Republic of Macedonia,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,
Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.
Endorsement notice
The text of ISO 16994:2016 has been approved by CEN as EN ISO 16994:2016 without any modification.
INTERNATIONAL ISO
STANDARD 16994
Second edition
2016-07-01
Solid biofuels — Determination of
total content of sulfur and chlorine
Biocombustibles solides — Détermination de la teneur totale en
soufre et en chlore
Reference number
ISO 16994:2016(E)
©
ISO 2016
ISO 16994:2016(E)
© 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
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ii © ISO 2016 – All rights reserved

ISO 16994:2016(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 2
4.1 General . 2
4.2 Decomposition of the biofuel . 2
4.3 Determination of sulfate and chloride in the decomposition solution . 2
4.4 Automatic equipment. 2
5 Reagents . 3
6 Apparatus . 3
6.1 General . 3
6.2 Method A . 3
6.3 Method B . 4
7 Preparation of the test sample . 4
8 Procedure. 4
8.1 Decomposition . 4
8.1.1 Method A: Combustion in a closed combustion vessel . 4
8.1.2 Method B: Digestion in a closed vessel . 5
8.1.3 Blank test . 6
8.2 Detection methods . 6
8.2.1 Ion chromatography . 6
8.2.2 Other detection methods . 6
8.3 Calibration of the apparatus . 6
8.4 Analyses of the decomposition solutions . 6
9 Expression of results . 7
9.1 General . 7
9.2 Total chlorine . 7
9.3 Total sulfur . 7
10 Performance characteristics . 7
11 Test report . 8
Annex A (informative) Performance data . 9
Bibliography .11
ISO 16994:2016(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 238, Solid biofuels.
This second edition cancels and replaces the first edition (ISO 16994:2015), of which it constitutes a
minor revision.
iv © ISO 2016 – All rights reserved

ISO 16994:2016(E)
Introduction
Sulfur and chlorine are present in solid biofuels in varying concentrations. During the combustion
process, they are usually converted to sulfur-oxides and chlorides. The presence of these elements
and their reaction products can contribute significantly to corrosion and to environmentally harmful
emissions.
Chlorine can be present in different organic and inorganic compounds and is to exceed or equal the
water soluble amount that can be determined by ISO 16995.
Combustion in an oxygen atmosphere in a closed combustion vessel is the preferred method to digest
biomass samples for a determination of the total content of sulfur and chlorine. An advantage of the
method is that the digestion can be carried out in connection with the determination of the calorific
1)
value according to ISO 18125 . Decomposition in closed vessels is an appropriate alternative method.
Other analytical techniques (e.g. high-temperature combustion in a tube furnace and Eschka method)
may also be used. The determination of the resultant chlorine and sulfur compounds can be done by
different techniques, e.g. ion chromatography, ICP, titrimetry.
Automatic equipment and alternative methods may be used when these methods are validated with
biomass reference samples of an adequate type and also meet the requirements of Clause 10.
A list with typical sulfur and chlorine contents of solid biofuels can be found in ISO 17225-1:2014, Annex B.
1) To be published.
INTERNATIONAL STANDARD ISO 16994:2016(E)
Solid biofuels — Determination of total content of sulfur
and chlorine
1 Scope
This International Standard describes methods for the determination of the total sulfur and total
chlorine content in solid biofuels. This International Standard specifies two methods for decomposition
of the fuel and different analytical techniques for the quantification of the elements in the decomposition
solutions. The use of automatic equipment is also included in this International Standard, provided that
a validation is carried out as specified and that the performance characteristics are similar to those of
the method described in this International Standard.
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 10304-1, Water quality — Determination of dissolved anions by liquid chromatography of ions —
Part 1: Determination of bromide, chloride, fluoride, nitrate, nitrite, phosphate and sulfate
ISO 11885, Water quality — Determination of selected elements by inductively coupled plasma optical
emission spectrometry (ICP-OES)
2)
ISO 14780 , Solid biofuels — Sample preparation
ISO 16559, Solid biofuels — Terminology, definitions and descriptions
ISO 16967:2015, Solid biofuels — Determination of major elements — Al, Ca, Fe, Mg, P, K, Si, Na and Ti
2)
ISO 18125 , Solid biofuels — Determination of calorific value
ISO 18134-3, Solid biofuels — Determination of moisture content — Oven dry method — Part 3: Moisture
in general analysis sample
CEN Guide 13:2008, Validation of environmental test methods
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 16559 and the following apply.
3.1
reference material
RM
material or substance one or more of whose property values are sufficiently homogeneous and well-
established to be used for the calibration of an apparatus, the assessment of a measurement method, or
for assigning values to materials
2) To be published.
ISO 16994:2016(E)
3.2
certified reference material
CRM
reference material, accompanied by a certificate, one or more of whose property values are certified by
a procedure which establishes traceability to an accurate realization of the unit in which the property
values are expressed, and for which each certified value is accompanied by an uncertainty at a stated
level of confidence
3.3
NIST standard reference material
SRM
CRM issued by NIST that also meets additional NIST-specific certification criteria and is issued with
a certificate or certificate of analysis that reports the results of its characterisations and provides
information regarding the appropriate use(s) of the material
4 Principle
4.1 General
The determination of total sulfur and total chlorine content is performed in two steps (4.2 and 4.3) or
by using automatic equipment (see 4.4).
4.2 Decomposition of the biofuel
— Combustion in an oxygen atmosphere in a combustion vessel and absorption of the acidic gas
components in an absorption solution (method A).
— Digestion in closed vessels as described in ISO 16967:2015, Part A (method B).
4.3 Determination of sulfate and chloride in the decomposition solution
— Ion chromatography, in accordance with the principles of ISO 10304-1.
— ICP, in accordance with the principles of ISO 11885 (determination as sulfur and chlorine).
4.4 Automatic equipment
Automatic equipment may be used when the method is validated with biomass reference samples of
an adequate biomass type. If automatic equipment is used, sulfur and chlorine compounds may be
detected as gaseous components (e.g. by infrared methods). Examples for automatic analysers include
elemental analysers, AOX-analysers.
If automati
...