Solid biofuels - Determination of total content of sulfur and chlorine (ISO 16994:2016)

ISO 16994:2016 describes methods for the determination of the total sulfur and total chlorine content in solid biofuels. It 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 ISO 16994:2016, provided that a validation is carried out as specified and that the performance characteristics are similar to those of the method described in ISO 16994:2016.

Biogene Festbrennstoffe - Bestimmung des Gesamtgehaltes an Schwefel und Chlor (ISO 16994:2016)

Diese Internationale Norm beschreibt Verfahren zur Bestimmung des Gesamtgehaltes an Schwefel und an Chlor in biogenen Festbrennstoffen. Diese Internationale Norm legt zwei Verfahren für den Aufschluss des Brennstoffs und verschiedene Analysenverfahren für die quantitative Bestimmung der Elemente in den Aufschlusslösungen fest. Der Einsatz automatischer Geräte ist in dieser Internationalen Norm ebenfalls enthalten, sofern eine Validierung, wie im Dokument festgelegt, durchgeführt wird, und die Leistungsdaten denen des in dieser Internationalen Norm beschriebenen Verfahrens ähnlich sind.

Biocombustibles solides - Détermination de la teneur totale en soufre et en chlore (ISO 16994:2016)

L'ISO 16994 :2016 décrit des méthodes de détermination de la teneur totale en soufre et en chlore des biocombustibles solides. Elle spécifie deux méthodes de décomposition du combustible et différentes techniques d'analyse pour la quantification des éléments présents dans les solutions de décomposition. Elle englobe également l'utilisation d'équipements automatiques sous réserve que la validation soit effectuée conformément aux spécifications et que les caractéristiques de performance soient similaires à celles de la méthode décrite dans l'ISO 16994 :2016.

Trdna biogoriva - Določevanje celotnega žvepla in klora (ISO 16994:2016)

Ta mednarodni standard opisuje metode za določevanje celotnega žvepla in klora v trdnih biogorivih. Ta mednarodni standard določa dve metodi za razkrajanje
goriva in različne analizne tehnike za kvantifikacijo elementov v
rešitvah razkrajanja. V tem mednarodnem standardu je vključena tudi uporaba avtomatske opreme pod pogojem, da je potrjevanje izvedeno, kot je opredeljeno, in da so lastnosti podobne lastnostim metode, opisane v tem mednarodnem standardu.

General Information

Status
Published
Publication Date
02-Aug-2016
Technical Committee
Drafting Committee
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Due Date
03-Aug-2016
Completion Date
03-Aug-2016

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SLOVENSKI STANDARD
SIST EN ISO 16994:2016
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
SIST EN ISO 16994:2016 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 16994:2016
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SIST EN ISO 16994:2016
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.
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SIST EN ISO 16994:2016
EN ISO 16994:2016 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

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SIST EN ISO 16994:2016
EN ISO 16994:2016 (E)
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.

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SIST EN ISO 16994:2016
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SIST EN ISO 16994:2016
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
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SIST EN ISO 16994:2016
ISO 16994:2016(E)
COPYRIGHT PROTECTED DOCUMENT
© 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. +41 22 749 01 11
Fax +41 22 749 09 47
copyright@iso.org
www.iso.org
ii © ISO 2016 – All rights reserved
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SIST EN ISO 16994:2016
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 2016 – All rights reserved iii
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SIST EN ISO 16994:2016
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
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SIST EN ISO 16994:2016
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

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.
© ISO 2016 – All rights reserved v
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SIST EN ISO 16994:2016
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SIST EN ISO 16994:2016
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)
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

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

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 2016 – All rights reserved 1
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SIST EN ISO 16994:2016
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
...

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