INTERNATIONAL ISO

STANDARD 21663

First edition
2020-11

Solid recovered fuels — Methods

for the determination of carbon (C),
hydrogen (H), nitrogen (N) and sulphur
(S) by the instrumental method
Combustibles solides de récupération — Méthodes de détermination
de la teneur en carbone (C), hydrogène (H), azote (N) et soufre (S) par
la méthode instrumentale
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ISO 21663:2020
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Reference number
ISO 21663:2020(E)

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Contents Page

Foreword......................................................................................................................................................................................................................................... iv
Introduction...................................................................................................................................................................................................................................v
1 Scope.................................................................................................................................................................................................................................. 1
2 Normative references....................................................................................................................................................................................... 1
3 Terms and definitions...................................................................................................................................................................................... 1
4 Safety remarks......................................................................................................................................................................................................... 3
5 Principle......................................................................................................................................................................................................................... 3
6 Reagents and calibration standards................................................................................................................................................. 3
7 Apparatus...................................................................................................................................................................................................................... 4
8 Procedure..................................................................................................................................................................................................................... 5
8.1 Sample conservation and pre-treatment.......................................................................................................................... 5
8.2 Sample preparation............................................................................................................................................................................. 5
8.3 Preparation of the test portion.................................................................................................................................................. 5
8.4 Calibration................................................................................................................................................................................................... 5
8.5 Analysis of samples.............................................................................................................................................................................. 6
9 Performance characteristics..................................................................................................................................................................... 6
10 Test report.................................................................................................................................................................................................................... 7
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Annex A (normative) Guidelines - Characteristics of the laboratory sample for chemical
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analysis of SRF.......................................................................................................................................................................................................... 8
Annex B (informative) Data on performance characteristics...................................................................................................... 9
ISO 21663:2020
Annex C (informative) Major results of robustness testing........................................................................................................11
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Bibliography.............................................................................................................................................................................................................................. 12

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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 of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to the
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World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www​.iso​.org/​
iso/​foreword​.html. (standards.iteh.ai)
This document was prepared by Technical Committee ISO/TC 300 Solid recovered fuels.
ISO 21663:2020
Any feedback or questions on this document should be directed to the user’s national standards body. A
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Introduction
The determination of total content of carbon, hydrogen, nitrogen and sulfur is usually performed
using instrumental methods. Depending on the amount of test portion used two different types of
instrumental methods can be used: micro methods require few milligrams of sample; macro methods
use grams of sample. Micro methods require a very careful preparation of the test sample for Solid
Recovered Fuel (SRF) analysis.

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INTERNATIONAL STANDARD ISO 21663:2020(E)

Solid recovered fuels — Methods for the determination of

carbon (C), hydrogen (H), nitrogen (N) and sulphur (S) by
the instrumental method

1 Scope
This document specifies the determination of total content of carbon, hydrogen, nitrogen and sulfur
in solid recovered fuels by instrumental method. Depending on the amount of test portion, micro or
macro instrumental apparatus are used.
This method is applicable for concentrations on dry matter basis of C > 0,1 %, N > 0,1 %, H > 0,1 % and
S > 0,05 %.

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.
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ISO 21637, Solid recovered fuels — Terminology, definitions and descriptions
ISO 21660-31) (standards.iteh.ai)
, Solid recovered fuels — Determination of moisture content using the oven dry method —
Part 3: Moisture in general analysis sample
ISO 21663:2020
ISO 216462), Solid recovered fuels — Sample preparation
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3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 21637 and the following apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https://​w ww​.iso​.org/​obp
— IEC Electropedia: available at http://​w ww​.electropedia​.org/​
3.1
coefficient of variation
estimate of the standard deviation of a population from a sample (3.10) of n results divided by the mean
of that sample
Note 1 to entry: Frequently stated as a percentage.

Note 2 to entry: Adapted from Eurachem/Citac Guide CG 4.

3.2
dry basis
calculation basis in which the material is considered free from moisture (3.6)
[SOURCE: ISO 21637, 3.20]

1) Under preparation. Stage at the time of publication ISO/FDIS 21660-3.

2) Under preparation. Stage at the time of publication ISO/DIS 21646.

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3.3
dry matter
material remaining after removal of moisture (3.6) under specific condition
[SOURCE: ISO 21637, 3.22]
3.4
general analysis sample
sub-sample of a laboratory sample having a nominal top size (3.7) of 1 mm or less and used for a number
of chemical and physical analyses
3.5
laboratory sample
combined sample received by the laboratory on which sample preparation procedures are undertaken
Note 1 to entry: When the laboratory sample is further prepared (reduced) by subdividing, mixing, grinding,
or by combinations of these operations, leading to a nominal top size ≤ 1mm, the result is the general analysis
sample. A test portion is removed from the general analysis sample for the performance of the test or for analysis.
When no preparation of the laboratory sample is required, the laboratory sample may become the test portion.

Note 2 to entry: The laboratory sample is the final sample from the point of view of sample collection, but it is the
initial sample from the point of view of the laboratory.

Note 3 to entry: Several laboratory samples are prepared and sent to different laboratories or to the same
laboratory for different purposes. When sent to the same laboratory, the set is generally considered as a single
laboratory sample and is documented as a single sample.

3.6
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moisture (standards.iteh.ai)
water removable under specific conditions
[SOURCE: ISO 21637, 3.46] ISO 21663:2020
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nominal top size
smallest aperture size of the sieve used for determining the particle size distribution of solid recovered
fuels through which at least 95 % by mass of the total material passes through the sieve
[SOURCE: ISO 21637, 3.48]
3.8
particle size
size of the fuel particles as determined in a solid fuel
Note 1 to entry: Different methods of determination can give different results.

3.9
precision
closeness of agreement between independent test/measurement results obtained under stipulated
conditions
[SOURCE: ISO 21637, 3.57]
3.10
sample
quantity of material, from a larger amount for which the quality is to be determined
Note 1 to entry: See also increment (3.39), stratified sample (3.78), stratified random sample (3.80), stratified
arbitrary sample (3.79), sub-sample (3.82) and test sample (3.84) in ISO 21637.

[SOURCE: ISO 21637, 3.63, modified — Notes 1 - 3 to entry were removed and new note 1 to entry
was added]

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3.11
test portion
sub-sample either of a laboratory sample or a test sample (3.12) required for the specific measurement
[SOURCE: ISO 21637, 3.83]
3.12
test sample
laboratory sample (3.5) after an appropriate preparation made by the laboratory
[SOURCE: ISO 21637, 3.84]

4 Safety remarks
The safety in handling of potentially hazardous materials is dealt with in relevant national and
European regulations, which every laboratory should refer to.
In addition, the following information is given:
— only experienced personnel, following the safety instructions of the manufacturer, shall use
instruments for carbon, hydrogen, nitrogen and sulfur determination.

5 Principle
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A known mass of sample is treated with oxygen, or in an oxygen/carrier gas mixture, under conditions
such that it is converted into gaseous products of combustion or decomposition. These consist mainly of
(standards.iteh.ai)
carbon dioxide, water vapour, elemental nitrogen and/or nitrogen oxides, oxyacids and oxides of sulfur
and hydrogen halides. The products are treated to ensure that any hydrogen associated with sulfur
or halides are converted, through a catalytic process, into water vapour. Nitrogen oxides are reduced
ISO 21663:2020
to nitrogen, and the products of combustion which can interfere with the subsequent gas-analysis
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procedures are properly removed. The carbon dioxide, water vapour and nitrogen mass fractions in the
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gas stream are then determined quantitatively by appropriate instrumental gas analysis procedures
after separation by trapping or suitable chromatographic column.
The samples are held in a suitable container (tin or other crucible) and then dropped inside the
quartz tube furnace at about 1 250 °C in an oxygen stream for complete oxidation in the presence of
a catalyst layer.

6 Reagents and calibration standards

All reagents shall be at least of analytical grade and suitable for their specific purposes.

6.1 Carrier gas: Helium, 99,99 % volume fraction or other gases as specified by the instrument
manufacturer.

6.2 Oxygen, free of combustion material, purity 99,95 % volume fraction, or as specified by the
instrument manufacturer.

6.3 Additional reagents: as specified by the instrument manufacturer.

6.4 Calibration standards

Examples of pure organic substances suitable for calibration are given in Table 1.
Examples of certified biomass sample with metrological traceability are given in Table 2.

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The two tables refer to different types of materials: Table 1 refers to pure substances to be used primary
calibration standards while Table 2 refers to biomass materials which can be used as controls since the
content depends on the batch.

Table 1 — Calibration standards

Name Formula C% H% N% S%
Acetanilide C8H9NO 71,1 6,7 10,4
Antipyrine C11H12N2O 70,19 6,43 14,88
Atropine C17H23NO3 70,6 8,0 4,8
Benzoic acid C7H6O2 68,8 5,0 0,0
Cystine C6H12N2O4S2 30,0 5,0 11,7 26,7
Diphenylamine C12H11N 85,2 6,5 8,3
EDTA C10H16N2O8 41,1 5,5 9,6
Phenylalanine C9H11NO2 65,4 6,7 8,5
Sulfanil amide C6H8N2O2S 41,8 4,7 16,3 18,6
Sulfanilic acid C6H7NO3S 41,6 4,1 8,1 18,5
Thiourea CH4N2S 15,78 5,3 36,8 42,12
TRIS C4H11NO3 39,7 9,1 11,6
2,5-Bis(5-tert-butyl-benzox-
C26H26N2O2S 72,5 6,0 6,5 7,4
azol-2-yl)thiophene (BBOT)
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Table 2 — Examples of certified biomass sample with metrological traceability
(standards.iteh.ai)
Name C% H% N% S%
Alfalfa 45,05 ISO 21663:2020 3,6 0,38
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Oat meal 45,8 6,7 2,8 0,25
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Rye Flour 45 6,4 1,7 0,14
Wheat Flour 45,3 6,4 2,7 0,19

NOTE Certified value for biomass samples is only indicative, depending on the batch.

7 Apparatus
Various instrumental configurations are available. The general requirements for a suitable apparatus are:
a) the combustion conditions shall be such that all carbon, hydrogen, nitrogen and sulfur are converted
to carbon dioxide, water vapour, nitrogen oxides or elemental nitrogen and sulfur oxides;
b) for the determination of sulfur, the instrumental configuration shall be able to reach adequate
conditions of temperature and combustion time to allow to convert all the chemical compounds
that can be present in the sample (e.g. metal sulphides require a temperature of 1 000 °C and
calcium sulfate a temperature > 1250 °C);
c) Tungsten wire may not be used for the determination of sulfur because it is a sulfur trap. For
instance, copper wire can be used as an alternative;
d) one or more separation steps are usually included to commercial devices, depending on the detector
used, to reduce or eliminate any possible interference during the subsequent determination;
e) nitrogen oxides shall be converted to the nitrogen before detection;
f) hydrogen associated with sulfur or halides are converted, through a catalytic process, into
water vapour

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g) the detection system shall provide response, that correlate directly with the concentrations of the
combustion gases, over the full range applicable and preferable in a linear manner;
h) if a nonlinear response is provided by a detection system, it shall include provisions for evaluating
that response in a manner which correlates accurately with the concentration of the combustion gas;
i) it shall include a means of displaying the detector responses or of calculating and presenting the
concentrations of carbon, hydrogen, nitrogen and sulfur in the sample following the input of other
appropriate data as necessary;
j) analytical balance, resolution of at least 1 part per thousand of the weighted amount.

8 Procedure

8.1 Sample conservation and pre-treatment

The laboratory samples shall be stored according to guidelines defined in Annex A.

8.2 Sample preparation

The test sample shall be prepared from the laboratory sample according to ISO 21646.
The nominal top size of the test sample shall be 1 mm or less. For some instruments it may be necessary
to prepare a test sample with a lower nominal top size than 1 mm in order to keep the desired precision.
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For “new products” an adequate particle size shall be determined by validation experiments.
The size of test portion depends(standards.iteh.ai)
on the particular instrument used.
For some types of instruments, it is necessary to carry out the determination of hydrogen on dried
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Whereas the determination is carried out on dry sample, the moisture content shall be determined
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according to ISO 21660-3.

8.3 Preparation of the test portion

Weigh the appropriate amount of test sample as recommended by the instrument manufacturer as
appropriate for the type of instrument and the expected content of carbon, hydrogen, nitrogen and sulfur.
The test portion shall be weighed directly into the sample capsule in the case of a micro- or semi-micro
analyser. Otherwise it may be weighed directly or transferred from a suitable weighing container.

8.4 Calibration
Set up the instrument following the manufacturer instructions.
Stabilize the furnace and analyser.
Select 3 to 5 calibration standards (6.4) with increasing concentration of nitrogen, hydrogen, carbon and
sulfur. Calibrate the instruments for nitrogen, hydrogen, carbon and sulfur determination following the
manufacturer instructions. Use the same procedure as for sample analysis (see below). Alternatively,
different amounts of the same substance may be used to prepare the calibration.
Verify the calibration by analysing as a test sample a portion of a suitable standard, preferably with a
different material than that used for the calibration.
Verification of the calibration is necessary if operating with pre-calibrated instruments.
Check the performance of the instrument using the accepted standard procedures like replicate
analysis, use of CRM and/or Standard Reference Material (SRM), control samples and create control

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