Solid mineral fuels - Determination of total sulfur by Coulomb titration method

ISO 20336:2017 specifies an alternative method of determining the total sulfur content of coal and coke by high-temperature combustion ? Coulomb titration.

Combustibles minéraux solides — Détermination de la teneur totale en soufre par la méthode de titrage de Coulomb

General Information

Status
Published
Publication Date
12-Oct-2017
Current Stage
9599 - Withdrawal of International Standard
Start Date
10-Feb-2025
Completion Date
13-Dec-2025

Relations

Effective Date
27-May-2023

Overview

ISO 20336:2017 specifies a standardized laboratory method for determining the total sulfur content in solid mineral fuels (coal and coke) using high‑temperature combustion followed by Coulomb titration. The method uses automated instruments to combust a weighed test portion at controlled temperatures and to quantify sulfur oxides electrochemically. ISO 20336:2017 provides requirements for sample preparation, reagents, apparatus, calibration and routine operation to produce traceable sulfur results.

Key topics and technical requirements

  • Principle: Combustion of a weighed sample in purified air at high temperature converts sulfur to sulfur oxides which are absorbed in an electrolytic solution and titrated by iodine/bromine produced by electrolysis; the integrated electrical charge (Coulomb integrator) yields sulfur dioxide amount.
  • Temperature control: Combustion zone maintained at (1150 ± 10) °C with a preliminary decomposition zone around 500 °C.
  • Sample preparation: General analysis test sample ground to pass 212 µm (or 100 µm for samples with >5 % sulfur). Typical test portion: 0.05 ± 0.005 g (0.03 ± 0.005 g for >5 % sulfur).
  • Reagents: Electrolytic solution prepared from potassium iodide, potassium bromide and glacial acetic acid (5 g KI + 5 g KBr in 250–300 ml water + 10 ml acetic acid). Tungsten trioxide is used as catalyst.
  • Apparatus: Includes tube resistance furnace with silicon or corundum combustion tube, electrolytic cell (>400 ml) with platinum electrodes, magnetic stirrer, program controller, purified air supply and Coulomb integrator (integration linearity error < 0.1 % over 0–350 mA).
  • Calibration and quality control: Instrument calibration using certified reference materials (CRMs) by multi‑point or single‑point methods; regular calibration checks after 10–15 runs. Precision (repeatability and reproducibility) and test reporting requirements are addressed in the standard.
  • Safety and purity: Use analytical‑grade reagents and distilled or equivalent water; ensure gas‑tight connections and air purification (NaOH and silica gel) where required.

Applications and users

  • Laboratories performing routine sulfur determination in coal and coke for quality control, fuel specification and compliance testing.
  • Coal and coke producers, utilities and power plants monitoring fuel sulfur for combustion performance and emissions control.
  • Environmental and regulatory testing labs assessing sulfur content for reporting and permitting.
  • Instrument manufacturers and metrology labs implementing or validating automated Coulomb titration analyzers.

Related standards

  • ISO 687 - moisture determination for coke
  • ISO 5068-2 - moisture in brown coals and lignites
  • ISO 11722 - moisture in hard coal (drying in nitrogen)

Keywords: ISO 20336:2017, total sulfur, Coulomb titration, solid mineral fuels, coal and coke, high‑temperature combustion, sulfur determination, instrument calibration.

Standard

ISO 20336:2017 - Solid mineral fuels -- Determination of total sulfur by Coulomb titration method

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Frequently Asked Questions

ISO 20336:2017 is a standard published by the International Organization for Standardization (ISO). Its full title is "Solid mineral fuels - Determination of total sulfur by Coulomb titration method". This standard covers: ISO 20336:2017 specifies an alternative method of determining the total sulfur content of coal and coke by high-temperature combustion ? Coulomb titration.

ISO 20336:2017 specifies an alternative method of determining the total sulfur content of coal and coke by high-temperature combustion ? Coulomb titration.

ISO 20336:2017 is classified under the following ICS (International Classification for Standards) categories: 75.160.10 - Solid fuels. The ICS classification helps identify the subject area and facilitates finding related standards.

ISO 20336:2017 has the following relationships with other standards: It is inter standard links to ISO 20336:2025. Understanding these relationships helps ensure you are using the most current and applicable version of the standard.

ISO 20336:2017 is available in PDF format for immediate download after purchase. The document can be added to your cart and obtained through the secure checkout process. Digital delivery ensures instant access to the complete standard document.

Standards Content (Sample)


INTERNATIONAL ISO
STANDARD 20336
First edition
2017-10
Solid mineral fuels — Determination
of total sulfur by Coulomb titration
method
Combustibles minéraux solides — Détermination de la teneur totale
en soufre par la méthode de titrage de Coulomb
Reference number
©
ISO 2017
© ISO 2017, 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.
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Tel. +41 22 749 01 11
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ii © ISO 2017 – All rights reserved

Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Reagent and materials . 1
6 Apparatus . 2
7 Preparation of test sample . 3
8 Procedure. 4
8.1 Preparation of test . 4
8.2 Calibration . 4
8.3 Calibration procedure . 4
8.4 Procedure . 5
8.5 Calibration check . 5
9 Expression of result . 6
10 Precision . 6
10.1 Repeatability limit . 6
10.2 Reproducibility limit . 6
11 Test report . 6
Foreword
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different types of ISO documents should be noted. This document was drafted in accordance with the
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URL: www.iso.org/iso/foreword.html.
This document was prepared by Technical Committee ISO/TC 27, Solid mineral fuels, Subcommittee
SC 5, Methods of analysis.
iv © ISO 2017 – All rights reserved

Introduction
The objective of this document is to provide an alternative method for determining the total sulfur
content in solid mineral fuels with high-temperature combustion — Coulomb titration using automated
instruments.
INTERNATIONAL STANDARD ISO 20336:2017(E)
Solid mineral fuels — Determination of total sulfur by
Coulomb titration method
1 Scope
This document specifies an alternative method of determining the total sulfur content of coal and coke
by high-temperature combustion — Coulomb titration.
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 687, Solid mineral fuels — Coke — Determination of moisture in the general analysis test sample
ISO 5068-2, Brown coals and lignites — Determination of moisture content — Part 2: Indirect gravimetric
method for moisture in the analysis sample
ISO 11722, Solid mineral fuels — Hard coal — Determination of moisture in the general analysis test
sample by drying in nitrogen
3 Terms and definitions
No terms and definitions are listed in this document.
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 http://www.electropedia.org/
4 Principle
In the presence of the catalyst, a weighed sample is combusted at 1 150 °C in a stream of purified air.
The sulfur oxides are formed and dissolved in the electrolytic solution. The sulfur dioxides are titrated
by the iodine and bromine librated from the electrolysis of the potassium iodide and potassium
bromide solution. The quantity of the electricity consumed by electrolysis is integrated and used to
calculate the content of sulfur dioxides. The instrument is calibrated with certified reference materials.
The percentage of total sulfur in the sample is calculated according to the sulfur dioxides content and
the prior calibration.
5 Reagent and materials
During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only
distilled water or water of equivalent purity.
5.1 Potassium iodide.
5.2 Potassium bromide.
5.3 Glacial acetic acid.
5.4 Self-indicating silica gel, industrial grade.
5.5 Sodium hydroxide, chemical grade.
5.6 Electrolytic solution.
5 g of potassium iodide (5.1) and 5 g of potassium bromide (5.2) are dissolved in (250 to 300) ml of
water, then add 10 ml of glacial acetic acid.
5.7 Glass wool.
5.8 Aluminosilicate wool.
5.9 Catalyst, tungsten trioxide.
5.10 Certified reference materials (CRMs), coal or coke.
6 Apparatus
6.1 Instrument.
For determining sulfur by Coulomb titration, commercially available, consisting of the following
(
...

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