Sludge, treated biowaste, soil and waste - Determination of loss on ignition

This European Standard specifies a method for the determination of the loss on ignition (LOI) of dry matter at 550 °C. The dry matter is determined according to EN 15934.
This method applies to the determination of loss on ignition of sludge, treated biowaste, soil and waste. The LOI of sediments can also be determined with this method.
The loss on ignition is often used as an estimate for the content of organic matter in the sample. Inorganic substances or decomposition products (e. g. H2O, CO2, SO2, O2) are released or absorbed and some inorganic substances are volatile under the reaction conditions.

Schlamm, behandelter Bioabfall, Boden und Abfall - Bestimmung des Glühverlusts

Dieses Dokument legt ein Verfahren zur Bestimmung des Glühverlusts (LOI) bei 550 °C fest. Die Trockenmasse wird mit dem Verfahren nach EN 15934 bestimmt.
Dieses Verfahren zur Bestimmung des Glühverlusts ist anwendbar für Sediment, Schlamm, behandelten Bioabfall, Boden und Abfall.
ANMERKUNG   Der Glühverlust dient oft als Schätzwert für den Gehalt an organischen Bestandteilen in der Probe. Anorganische Stoffe oder Zersetzungsprodukte (z. B. H2O, CO2, SO2, O2) werden freigesetzt oder absorbiert und einige anorganische Stoffe sind unter den Reaktionsbedingungen flüchtig.

Boue, biodéchet traité, sol et déchets - Détermination de la perte au feu

Le présent document spécifie une méthode de détermination de la perte au feu (LOI) à 550 °C. La teneur en matière sèche est déterminée conformément à l’EN 15934.
Cette méthode s’applique à la détermination de la perte au feu des sédiments, des boues, des biodéchets traités, des sols et des déchets.
NOTE   La perte au feu est souvent utilisée comme une estimation de la teneur en matière organique dans l'échantillon. Des substances inorganiques ou des produits de décomposition (par exemple, H2O, CO2, SO2, O2) sont libérés ou absorbés et certaines substances inorganiques sont volatiles dans les conditions opératoires.

Blato, obdelani biološki odpadki, tla in odpadki - Določevanje žarilne izgube

General Information

Status
Published
Public Enquiry End Date
03-May-2020
Publication Date
10-Oct-2021
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
19-Aug-2021
Due Date
24-Oct-2021
Completion Date
11-Oct-2021

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SLOVENSKI STANDARD
SIST EN 15935:2021
01-november-2021
Nadomešča:
SIST EN 15169:2007
SIST EN 15935:2012
Blato, obdelani biološki odpadki, tla in odpadki - Določevanje žarilne izgube
Sludge, treated biowaste, soil and waste - Determination of loss on ignition
Schlamm, behandelter Bioabfall, Boden und Abfall - Bestimmung des Glühverlusts
Boue, biodéchet traité, sol et déchets - Détermination de la perte au feu
Ta slovenski standard je istoveten z: EN 15935:2021
ICS:
13.030.20 Tekoči odpadki. Blato Liquid wastes. Sludge
SIST EN 15935:2021 en,fr,de

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

---------------------- Page: 1 ----------------------
SIST EN 15935:2021
---------------------- Page: 2 ----------------------
SIST EN 15935:2021
EN 15935
EUROPEAN STANDARD
NORME EUROPÉENNE
August 2021
EUROPÄISCHE NORM
ICS 13.030.01 Supersedes EN 15169:2007, EN 15935:2012
English Version
Soil, waste, treated biowaste and sludge - Determination of
loss on ignition

Sols, déchets, biodéchets traités et boues - Boden, Abfall, behandelter Bioabfall und Schlamm -

Détermination de la perte au feu Bestimmung des Glühverlusts
This European Standard was approved by CEN on 4 July 2021.

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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,

Poland, Portugal, Republic of North Macedonia, Romania, Serbia, 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: Rue de la Science 23, B-1040 Brussels

© 2021 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 15935:2021 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST EN 15935:2021
EN 15935:2021 (E)
Contents Page

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

Introduction .......................................................................................................................................................... 4

1 Scope .......................................................................................................................................................... 5

2 Normative references .......................................................................................................................... 5

3 Terms and definitions ......................................................................................................................... 5

4 Principle ................................................................................................................................................... 5

5 Interferences and sources of errors............................................................................................... 6

6 Apparatus ................................................................................................................................................ 6

7 Procedure ................................................................................................................................................ 6

7.1 Preservation ........................................................................................................................................... 6

7.2 Pretreatment .......................................................................................................................................... 6

7.3 Determination ........................................................................................................................................ 7

7.4 Samples containing a high content of volatile or organic substances or undried

samples ..................................................................................................................................................... 7

8 Calculation and expression of results ........................................................................................... 8

8.1 Loss on ignition, based on dry mass according to EN 15934 (7.3) ...................................... 8

8.2 Loss on ignition, based on undried sample (7.4) ...................................................................... 9

8.3 Residue on ignition .............................................................................................................................. 9

9 Performance characteristics............................................................................................................. 9

10 Test report ............................................................................................................................................... 9

Annex A (informative) Performance characteristics ............................................................................ 10

Bibliography ....................................................................................................................................................... 12

---------------------- Page: 4 ----------------------
SIST EN 15935:2021
EN 15935:2021 (E)
European foreword

This document (EN 15935:2021) has been prepared by Technical Committee CEN/TC 444

“Environmental characterization of solid matrices”, the secretariat of which is held by NEN.

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 2022, and conflicting national standards shall

be withdrawn at the latest by February 2022.

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. CEN shall not be held responsible for identifying any or all such patent rights.

This document supersedes EN 15169:2007 and EN 15935:2012.
The following technical modifications have been made:
— two existing standards have been combined;
— the scope defines more sample types;
— the criteria for the heating time are specified.

This document specifies a method for the determination of the loss on ignition (LOI) at 550 °C of

sediment, sludge, treated biowaste, soil and waste and combines the methods previously described in

EN 15935:2012 and EN 15169.

Any feedback and questions on this document should be directed to the users’ national standards body.

A complete listing of these bodies can be found on the CEN website.

According to the CEN-CENELEC Internal Regulations, the national standards organisations of the

following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia,

Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland,

Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of North

Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United

Kingdom.
---------------------- Page: 5 ----------------------
SIST EN 15935:2021
EN 15935:2021 (E)
Introduction

The method described in this document has been developed from EN 15169 (derived from EN 12879),

which was prepared by CEN/TC 292 “Characterization of waste” and from EN 15935:2012, which was

prepared by CEN/TC 400 “Horizontal standards in the field of sludge, biowaste and soil”.

This document specifies a method for the determination of the loss on ignition (LOI) at 550 °C of

sediment, sludge, treated biowaste, soil and waste and combines the methods previously described in

EN 15935:2012 and EN 15169. Both dried and undried samples which are pretreated prior to

determination can be used. The determination is ended after a predefined timeframe or when constant

mass is reached.

This document is applicable and validated for several types of matrices as indicated in Table 1 (see also

Annex A for the results of the validation).
Table 1 — Matrices for which this document is applicable and validated
Matrix Materials used for validation
Sludge Municipal sludge
Biowaste Compost,
Fresh Compost
Soil Sludge amended soil,
Agricultural soil
Waste Contaminated soil,
Dredged sludge (sediment),
Nickel sludge
---------------------- Page: 6 ----------------------
SIST EN 15935:2021
EN 15935:2021 (E)
1 Scope

This document specifies a method for the determination of the loss on ignition (LOI) at 550 °C. The dry

matter is determined according to EN 15934.

This method applies to the determination of loss on ignition of sediment, sludge, treated biowaste, soil

and waste.

NOTE The loss on ignition is often used as an estimate for the content of organic matter in the sample. Inorganic

substances or decomposition products (e.g. H O, CO , SO , O ) are released or absorbed and some inorganic

2 2 2 2
substances are volatile under the reaction conditions.
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.

EN 15934, Sludge, treated biowaste, soil and waste - Calculation of dry matter fraction after determination

of dry residue or water content
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— IEC Electropedia: available at https://www.electropedia.org/
— ISO Online browsing platform: available at https://www.iso.org/obp
3.1
loss on ignition
LOI

mass fraction lost by incineration of a dried sample to constant mass (3.3) at a specified temperature

3.2
residue on ignition

mass fraction remaining after incineration of a dried sample to constant mass (3.3) at a specified

temperature
3.3
constant mass

mass obtained when the change in mass during a further period of heating of 1 h is within 0,5 % (m/m)

or 2 mg, whatever is greater
4 Principle

A weighed test portion is incinerated in a furnace to constant mass at (550 ± 25) °C. The difference in

mass before and after the ignition process is used to calculate the loss on ignition.

The determination is performed on a dried sample or directly on the undried sample including a drying

step or by referring to the dry matter.
---------------------- Page: 7 ----------------------
SIST EN 15935:2021
EN 15935:2021 (E)
5 Interferences and sources of errors

LOI is an empirical parameter, thus in principle there is no interference connected to the determination.

However, for some purposes the determination of LOI is used for the assessment of the content of organic

matter in the sample. It should be noted that elemental carbon in the sample will be included in the loss

on ignition value. Furthermore, any volatilisation or chemical reactions of inorganic compounds will also

be included in the loss on ignition value.

Chemically bound water could be released during heating, thereby contributing to the loss on ignition.

Samples containing iron or other metals in low bonding state or in metallic state can be oxidized during

heating, thereby contributing to the loss on ignition with a negative amount.

Sulphides present in the sample could be oxidized to sulphate during heating, thereby contributing to the

loss on ignition with a negative amount.

Explosive ignition is likely to result in loss of residue from the crucible, thereby contributing to the loss

on ignition with a positive amount. If such loss of residue is observed during the removal of the crucible

from the furnace, the test shall be discharged and repeated taken the necessary precautions, e.g. using a

smaller test portion.

Calcium hydroxide or calcium oxide present in large amounts (e.g. sludge conditioned with lime) can

combine with sulphuric oxides liberated during ignition or with carbon dioxide formed during ignition

resulting in a too low content of the loss on ignition. Such reactions can be avoided using the stepwise

heating procedure stated in 7.4 combined with a sufficient ventilation rate in the furnace

...

SLOVENSKI STANDARD
oSIST prEN 15935:2020
01-april-2020
Blato, obdelani biološki odpadki, tla in odpadki - Določevanje žarilne izgube
Sludge, treated biowaste, soil and waste - Determination of loss on ignition
Schlamm, behandelter Bioabfall, Boden und Abfall - Bestimmung des Glühverlusts
Boue, biodéchet traité, sol et déchets - Détermination de la perte au feu
Ta slovenski standard je istoveten z: prEN 15935
ICS:
13.030.20 Tekoči odpadki. Blato Liquid wastes. Sludge
oSIST prEN 15935:2020 en,fr,de

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

---------------------- Page: 1 ----------------------
oSIST prEN 15935:2020
---------------------- Page: 2 ----------------------
oSIST prEN 15935:2020
DRAFT
EUROPEAN STANDARD
prEN 15935
NORME EUROPÉENNE
EUROPÄISCHE NORM
March 2020
ICS Will supersede EN 15169:2007, EN 15935:2012
English Version
Sludge, treated biowaste, soil and waste - Determination of
loss on ignition
Schlamm, behandelter Bioabfall, Boden und Abfall -
Bestimmung des Glühverlusts

This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee

CEN/TC 444.

If this draft becomes a European Standard, 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.

This draft European Standard was established by CEN 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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,

Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and

United Kingdom.

Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are

aware and to provide supporting documentation.

Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without

notice and shall not be referred to as a European Standard.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 15935:2020 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
oSIST prEN 15935:2020
prEN 15935:2020 (E)
Contents Page

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

Introduction .................................................................................................................................................................... 4

1 Scope .................................................................................................................................................................... 5

2 Normative references .................................................................................................................................... 5

3 Terms and definitions ................................................................................................................................... 5

4 Principle ............................................................................................................................................................. 5

5 Interferences and sources of errors ......................................................................................................... 5

6 Apparatus ........................................................................................................................................................... 6

6.1 Crucible, preferably flat bottom type and typically 50 mm to 70 mm in diameter,

suitable for ignition at 550 °C, e.g. made of nickel, platinum, porcelain, or silica. .................. 6

6.2 Furnace, capable of maintaining a temperature of (550 ± 25) °C .................................................. 6

6.3 Metal plate, or comparable plate, suitable for the initial cooling of crucibles ......................... 6

6.4 Desiccator, with an active drying agent, such as silica gel ............................................................... 6

6.5 Balance, with an accuracy of at least 1 mg ............................................................................................. 6

7 Procedure........................................................................................................................................................... 6

7.1 Preservation...................................................................................................................................................... 6

7.2 Pretreatment .................................................................................................................................................... 6

7.3 Determination .................................................................................................................................................. 6

7.4 Samples containing volatile substances ................................................................................................. 7

8 Calculation and expression of results ...................................................................................................... 8

9 Performance characteristics ....................................................................................................................... 8

10 Test report ......................................................................................................................................................... 8

Annex A (informative) Performance characteristics ...................................................................................... 9

A.1 Materials used in the interlaboratory comparison study ................................................................ 9

A.2 Interlaboratory comparison results ..................................................................................................... 10

Bibliography ................................................................................................................................................................. 11

---------------------- Page: 4 ----------------------
oSIST prEN 15935:2020
prEN 15935:2020 (E)
European foreword

This document (prEN 15935:2020) has been prepared by Technical Committee CEN/TC 444 “Test

methods for environmental characterization of solid matrices”, the secretariat of which is held by NEN.

This document is currently submitted to the CEN Enquiry.
This document will supersede EN 15169:2007and EN 15936:2012.
---------------------- Page: 5 ----------------------
oSIST prEN 15935:2020
prEN 15935:2020 (E)
Introduction

The method described in this document has been developed from EN 15169 (derived from EN 12879)

which was prepared by CEN/TC 292 and from EN 15935:2012 which was prepared by CEN/TC 400.

This European Standard is applicable and validated for several types of matrices as indicated in Table 1

(see also Annex A for the results of the validation).
Table 1 — Matrices for which this European Standard is applicable and validated
Matrix Materials used for validation
Sludge Municipal sludge
Biowaste Compost,
Fresh Compost
Soil Sludge amended soil,
Agricultural soil
Waste Contaminated soil,
Dredged sludge (sediment),
Nickel sludge
---------------------- Page: 6 ----------------------
oSIST prEN 15935:2020
prEN 15935:2020 (E)
1 Scope

This document specifies a method for the determination of the loss on ignition (LOI) of dry matter at

550 °C. The dry matter is determined according to EN 15934.

This method applies to the determination of loss on ignition of sediment, sludge, treated biowaste, soil

and waste.

NOTE The loss on ignition is often used as an estimate for the content of organic matter in the sample. Inorganic

substances or decomposition products (e.g. H O, CO , SO , O ) are released or absorbed and some inorganic

2 2 2 2
substances are volatile under the reaction conditions.
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.

EN 15934, Sludge, treated biowaste, soil and waste - Calculation of dry matter fraction after determination

of dry residue or water content
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— IEC Electropedia: available at http://www.electropedia.org/
— ISO Online browsing platform: available at http://www.iso.org/obp
3.1
loss on ignition
LOI

mass fraction lost by incineration of a dried sample to constant mass at a specified temperature

3.2
residue on ignition

mass fraction remaining after incineration of a dried sample to constant mass at a specified temperature

4 Principle

A weighed test portion is incinerated in a furnace to constant mass at (550 ± 25) °C. The difference in

mass before and after the ignition process is used to calculate the loss on ignition.

The determination is performed on a dried sample or directly on the undried sample including a drying

step or by referring to the dry matter.
5 Interferences and sources of errors

LOI is an empirical parameter, thus in principle there is no interference connected to the determination.

However, for some purposes the determination of LOI is used for the assessment of the content of organic

matter in the sample. It should be noted that elemental carbon in the sample will be included in the loss

on ignition value. Furthermore, any volatilisation or chemical reactions of inorganic compounds will also

be included in the loss on ignition value.

Chemically bound water could be released during heating, thereby contributing to the loss on ignition.

---------------------- Page: 7 ----------------------
oSIST prEN 15935:2020
prEN 15935:2020 (E)

Samples containing iron or other metals in low bonding state or in metallic state could be oxidized during

heating, thereby contributing to the loss on ignition with a negative amount.

Sulfides present in the sample could be oxidized to sulfate during heating, thereby contributing to the

loss on ignition with a negative amount.

Explosive ignition is likely to result in loss of residue from the crucible, thereby contributing to the loss

on ignition.
Calcium hydrox
...

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