ISO/TS 18806:2014
(Main)Solid mineral fuels — Determination of Chlorine content
Solid mineral fuels — Determination of Chlorine content
ISO/TS 18806:2014 specifies two methods (high temperature combustion and bomb combustion) for the determination of chlorine in solid mineral fuels. It is applicable to hard coals, brown coals, coke, and tailings. The chlorine in the digestion solution can be determined using different methods, e.g. an ion-selective electrode, coulometric or potentiometric titration, spectrophotometry, or ion chromatography. In this Technical Specification, the ion chromatographic separation with conductivity detection is described. The method is applicable to determine the chlorine content higher than 0,005 per cent mass fraction.
Combustibles minéraux solides — Dosage de la teneur en chlore
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Standards Content (Sample)
TECHNICAL ISO/TS
SPECIFICATION 18806
First edition
2014-12-15
Solid mineral fuels — Determination
of Chlorine content
Combustibles minéraux solides — Dosage de la teneur en chlore
Reference number
ISO/TS 18806:2014(E)
©
ISO 2014
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ISO/TS 18806:2014(E)
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ii © ISO 2014 – All rights reserved
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ISO/TS 18806:2014(E)
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
4.1 Method A — High temperature combustion in oxygen . 1
4.2 Method B — Bomb combustion . 1
5 Reagent . 2
5.1 Method A . 2
5.2 Method B . 2
6 Apparatus . 2
6.1 Method A . 2
6.2 Method B . 4
7 Preparation of sample . 4
8 Procedure. 5
8.1 Blank Value Determination . 5
8.2 Method A . 5
8.3 Method B — Bomb Combustion. 5
9 Determination of dissolved chloride . 6
9.1 General . 6
9.2 Determination by ion chromatography . 6
10 Calculation and expression of results . 7
11 Test report . 7
Annex A (normative) Quality control . 8
Annex B (Informative)Results of the German Interlaboratory comparison 2009 for
DIN 51727:2011 “Solid fuels-Determination of the chlorine content” .9
Bibliography .11
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ISO/TS 18806:2014(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
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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 27, Solid mineral fuels, Subcommittee SC 5,
Methods of Analysis.
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TECHNICAL SPECIFICATION ISO/TS 18806:2014(E)
Solid mineral fuels — Determination of Chlorine content
1 Scope
This Technical Specification specifies two methods (high temperature combustion and bomb
combustion) for the determination of chlorine in solid mineral fuels. It is applicable to hard coals, brown
coals, coke, and tailings.
The chlorine in the digestion solution can be determined using different methods, e.g. an ion-selective
electrode, coulometric or potentiometric titration, spectrophotometry, or ion chromatography. In this
Technical Specification, the ion chromatographic separation with conductivity detection is described.
The method is applicable to determine the chlorine content higher than 0,005 per cent mass fraction.
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 687, Solid mineral fuels — Coke — Determination of moisture in the general analysis test sample
ISO 1170, Coal and coke — Calculation of analyses to different bases
ISO 1213-2, Solid mineral fuels — Vocabulary — Part 2: Terms relating to sampling, testing and analysis
ISO 5068-2, Brown coals and lignites — Determination of moisture content — Part 2: Indirect gravimetric
method for moisture in the analysis sample
ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results — Part 2: Basic method
for the determination of repeatability and reproducibility of a standard measurement method
ISO 11722, Solid mineral fuels — Hard coal — Determination of moisture in the general analysis test sample
by drying in nitrogen
EN 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
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 1213-2 apply.
4 Principle
4.1 Method A — High temperature combustion in oxygen
The sample is combusted at high temperature in an oxygen atmosphere. The gaseous combustion products
including the formed chloride are collected in a trap filled with water, in which they are dissolved.
4.2 Method B — Bomb combustion
The sample is combusted in a high pressure bomb in an oxygen atmosphere. The formed chloride is
collected in an absorption solution inside the bomb.
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ISO/TS 18806:2014(E)
5 Reagent
5.1 Method A
5.1.1 Oxygen, pure, with an assay of at least 99,5 % volume fraction.
5.1.2 Combustion aid (optional), spectroscopic carbon or iron phosphate (FePO ).
4
5.2 Method B
5.2.1 Oxygen, pure, with an assay of at least 99,5 % volume fraction.
5.2.2 Combustion aid (optional), paraffin, benzoic acid, polyethylene combustion bags, acetobutyrate
capsules, or other suitable materials.
5.2.3 Fuse, ignition wire (e.g. platinum) and cotton fuse (optional).
Note A possible contribution of the cotton fuse to the chlorine content should be considered.
5.2.4 Absorption solution, either eluent used for ion chromatographic determination, or alkaline
solution (e.g. 0,2 mol/l KOH or 0,1 mol/l NaOH), or deionised water.
6 Apparatus
6.1 Method A
6.1.1 Fused silica combustion tube, absorber, and headpiece, the sintered glass discs in the absorber
and the headpiece shall have a pore size of 90 µm to 150 µm (see Figure 1).
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ISO/TS 18806:2014(E)
Ø34
1
2
102
154
3
12
820
25
Ø22
10 6
Ø55
428
4
Ø39
5
124
6
7
84
8
Key
1 headpiece
2 sintered glass disc
3 V45/50 conical ground joint (ISO 383)
4 combustion tube
5 VS 13 spherical joint (ISO 641)
6 oxygen inlet
7 absorber
8 sintered glass disc
Figure 1 — Apparatus for Method A
6.1.2 Porcelain combustion boat, with handle, e.g. 70 mm long, 10 mm wide, and 7 mm deep.
6.1.3 Silica pusher, with iron inlay (see Figure 2).
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ISO/TS 18806:2014(E)
1 2
Ø5 Ø15
25
275
Key
1 silica pusher
2 iron inlay
Figure 2 — Silica pusher
6.1.4 Magnet.
6.1.5 Electrical tube furnace, about 300 mm long, capable of being heated to at least 1 300 °C and
maintained at (1 250 ± 25) °C.
6.1.6 Flow meter.
6.1.7 Oxygen inlet, consisting of a pierced silicon stopper with a glass tube.
6.2 Method B
6.2.1 Digestion unit
6.2.1.1 Digestion bomb, with inner surface that is resistant to corrosion by acidic gases formed or
emitted during combustion.
6.2.1.2 Pressure regulator, to control the filling of the b
...
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