prEN 15936

Soil, waste, treated biowaste and sludge - Determination of total organic carbon (TOC) by dry combustion

This document specifies two methods for the determination of total organic carbon (TOC) in sludge, treated biowaste, soil, waste and sediment samples containing more than 1 g carbon per kg of dry matter (0,1 %).

Schlamm, behandelter Bioabfall, Boden und Abfall - Bestimmung des gesamten organischen Kohlenstoffs (TOC) mittels trockener Verbrennung

Dieses Dokument legt zwei Verfahren zur Bestimmung des gesamten organischen Kohlenstoffs (TOC) in Schlamm, behandeltem Bioabfall, Boden, Abfall und Sedimentproben fest, die mehr als 1 g Kohlenstoff je Kilogramm Trockenmasse (0,1 %) enthalten.

Boues, biodéchets traités, sols et déchets - Dosage du carbone organique total (COT) par combustion sèche

Le présent document spécifie deux méthodes de dosage du carbone organique total (COT) dans des échantillons de boues, de biodéchets traités, de sols et de sédiments contenant plus de 1 g de carbone par kg de matière sèche (0,1 %).

Blato, obdelani biološki odpadki, tla in odpadki - Določevanje celotnega organskega ogljika (TOC) s suhim sežigom

General Information

• Status: Not Published
• ICS: 13.030.01 - Wastes in general
• ICS: 13.080.10 - Chemical characteristics of soils
• Technical Committee: CEN/TC 444 - Environmental characterization
• Drafting Committee: CEN/TC 444/WG 3 - Inorganic analysis
• Current Stage: 4599 - Dispatch of FV draft to CMC - Finalization for Vote
• Due Date: 23-Jun-2021
• Completion Date: 23-Jun-2021
• Directive: 86/278/EEC - Protection of the environment, and in particular of the soil, when sewage sludge is used in agriculture
• Mandate: M/330 - Mandate given to CEN for the development of horizontal standards in the fields of sludge, biowaste and soil.
• Ref Project: oSIST prEN 15936:2020 - Sludge, treated biowaste, soil and waste - Determination of total organic carbon (TOC) by dry combustion

RELATIONS

• Revised: EN 15936:2012 - Sludge, treated biowaste, soil and waste - Determination of total organic carbon (TOC) by dry combustion
• Effective Date: 07-Aug-2019

Standards Content (sample)

SLOVENSKI STANDARD
oSIST prEN 15936:2020
01-julij-2020
Blato, obdelani biološki odpadki, tla in odpadki - Določevanje celotnega
organskega ogljika (TOC) s suhim sežigom

Sludge, treated biowaste, soil and waste - Determination of total organic carbon (TOC)

by dry combustion
Schlamm, behandelter Bioabfall, Boden und Abfall - Bestimmung des gesamten
organischen Kohlenstoffs (TOC) mittels trockener Verbrennung

Boues, bio-déchets traités, sols et déchets - Détermination de la teneur en carbone

organique total (COT) par combustion sèche
Ta slovenski standard je istoveten z: prEN 15936
ICS:
13.030.20 Tekoči odpadki. Blato Liquid wastes. Sludge
13.080.10 Kemijske značilnosti tal Chemical characteristics of
soils
oSIST prEN 15936:2020 en,fr,de

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

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oSIST prEN 15936:2020
DRAFT
EUROPEAN STANDARD
prEN 15936
NORME EUROPÉENNE
EUROPÄISCHE NORM
June 2020
ICS 13.030.01; 13.080.10 Will supersede EN 15936:2012
English Version
Sludge, treated biowaste, soil and waste - Determination of
total organic carbon (TOC) by dry combustion

Boues, bio-déchets traités, sols et déchets - Schlamm, behandelter Bioabfall, Boden und Abfall -

Détermination de la teneur en carbone organique total Bestimmung des gesamten organischen Kohlenstoffs

(COT) par combustion sèche (TOC) mittels trockener Verbrennung

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 15936:2020 E

worldwide for CEN national Members.
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Contents Page

European foreword ....................................................................................................................................................... 4

Introduction .................................................................................................................................................................... 5

1 Scope .................................................................................................................................................................... 6

2 Normative references .................................................................................................................................... 6

3 Terms and definitions ................................................................................................................................... 6

4 Principle ............................................................................................................................................................. 6

4.1 Method A (indirect procedure) .................................................................................................................. 6

4.2 Method B (direct procedure) ...................................................................................................................... 7

4.3 Applicability of Methods A or B .................................................................................................................. 7

5 Interferences .................................................................................................................................................... 7

6 Reagents ............................................................................................................................................................. 8

6.2 Sodium carbonate, Na2CO3, anhydrous. .................................................................................................. 8

-EDTA ∙ 4 H O
6.3 Tetrasodium ethylenediamine tetraacetate-tetra-hydrate, Na4 2

(C H N O Na ∙ 4 H O), heated at 80 °C for 2 h. .................................................................................. 8

10 12 2 8 4 2

6.4 Potassium hydrogen phthalate, C H O K. ............................................................................................... 8

8 5 4

6.5 Acetanilide, C H NO. ....................................................................................................................................... 8

8 9

6.6 Atropine, C H NO . ....................................................................................................................................... 8

17 23 3

6.7 Spectrographic graphite powder, C. ......................................................................................................... 8

6.8 Sodium salicylate, C H O Na........................................................................................................................ 8

7 5 3

6.9 Aluminium oxide, Al O , neutral, granular size < 200 µm, annealed at 600 °C. ....................... 8

2 3

6.10 Control mixture A, prepared from sodium carbonate (6.2), Na -EDTA ∙ 4 H O (6.3)

4 2

and aluminium oxide (6.9) in a mass ratio of 2,34 : 1,00 : 7,28. ..................................................... 8

6.11 Control mixture B, prepared from sodium salicylate (6.8), calcium carbonate (6.1),

Na4-EDTA · 4 H O (6.3) and aluminium oxide (6.9) in a mass ratio of

1,00 : 4,36 : 1,97 : 8,40. .................................................................................................................................. 8

6.12 Non-oxidizing mineral acid, used for carbon dioxide expulsion, e.g. phosphoric acid

H PO (w = 85 %). .......................................................................................................................................... 8

3 4

6.13 Carrier gas, e.g. synthetic air, nitrogen, oxygen or argon, free of carbon dioxide and

organic impurities in accordance with the manufacturer's instructions. .................................. 8

7 Apparatus ........................................................................................................................................................... 9

7.1 Precision balance, accurate to at least 0,5 % of test portion weight. ........................................... 9

7.2 Equipment for determination of carbon in solids, with relevant accessories. ......................... 9

7.3 Purging unit for TIC determination, for Method A only. ................................................................... 9

7.4 Vessels, made of e.g. ceramic, silica, quartz, silver or platinum..................................................... 9

8 Sample pre-treatment ................................................................................................................................... 9

9 Procedure – Method A (indirect method) .............................................................................................. 9

9.1 Determination .................................................................................................................................................. 9

9.1.1 General ................................................................................................................................................................ 9

9.1.2 Determination of the TC ............................................................................................................................... 9

9.1.3 Determination of the TIC ........................................................................................................................... 10

9.2 Calibration ...................................................................................................................................................... 10

9.3 Control measurements ............................................................................................................................... 11

9.4 Calculation and expression of results ................................................................................................... 11

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10 Procedure Method B (direct method) ................................................................................................... 12

10.1 Determination................................................................................................................................................ 12

10.1.1 General ............................................................................................................................................................. 12

10.1.2 Removal of the inorganic carbon and determination of the TOC ................................................ 13

10.2 Calibration ....................................................................................................................................................... 13

10.3 Control measurements ............................................................................................................................... 13

10.4 Calculation and expression of results ................................................................................................... 14

11 Performance data ......................................................................................................................................... 14

12 Expression of results ................................................................................................................................... 15

13 Test report ...................................................................................................................................................... 15

Annex A (informative) Repeatability and reproducibility data ................................................................ 16

A.1 Materials used in the interlaboratory comparison study .............................................................. 16

A.2 Interlaboratory results ............................................................................................................................... 17

Annex B (informative) Factors influencing dry combustion methods ................................................... 19

B.1 Influence of temperature and modifiers on the decomposition of barium carbonate

as an example for a refractory compound ........................................................................................... 19

B.2 Recovery of the control mixture A .......................................................................................................... 19

B.3 Influence of aluminium oxide or sodium sulfate used for sample preparation for the

recovery of TOC ............................................................................................................................................. 20

B.4 Influence of TIC:TOC ratio on the recovery and the coefficient of variation ........................... 21

B.5 Method B: Influence of the temperature during the removal of inorganic carbon on

the recovery of TOC ...................................................................................................................................... 22

Bibliography ................................................................................................................................................................. 23

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European foreword

This document (prEN 15936:2020) has been prepared by Technical Committee CEN/TC 444

“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 15936:2012.
This document combines methods from EN 15936:2012 and EN 13137:2001.
The main changes compared to the previous edition are as follows:

— New composition of the substances in control mixture A [6.10] was defined and the recovery

requirement [9.3] was adapted to the results of a lab trial.

— Annex C – “Determination of total organic carbon (TOC) in solid samples using the suspension

method” was skipped.
— The text was editorially revised.
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Introduction

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 Filter cake,
Bottom ash,
Electro-plating sludge,
Dredged sludge,
Rubble

WARNING — Persons using this document should be familiar with usual laboratory practice. This

document does not purport to address all of the safety problems, if any, associated with its use. It is the

responsibility of the user to establish appropriate safety and health practices and to ensure compliance

with any national regulatory conditions.

IMPORTANT — It is absolutely essential that tests conducted according to this document be carried

out by suitably trained staff.
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1 Scope

This document specifies two methods for the determination of total organic carbon (TOC) in sludge,

treated biowaste, soil, waste and sediment samples containing more than 1 g carbon per kg of dry

matter (0,1 %).
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 15002, Characterization of waste - Preparation of test portions from the laboratory sample

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

determination of dry residue or water content
EN 16179, Sludge, treated biowaste and soil - Guidance for sample pretreatment
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:

— ISO Online browsing platform: available at https://www.iso.org/obp/ui
— IEC Electropedia: available at http://www.electropedia.org/
3.1
total carbon

quantity of carbon present in the sample in the form of organic, inorganic and elemental carbon

3.2
total inorganic carbon
TIC

quantity of carbon that is liberated as carbon dioxide by acid treatment. Typically, the TIC represents

the carbonates present in a sample
3.3
total organic carbon
TOC

quantity of carbon that is converted into carbon dioxide by combustion and which is not liberated as

carbon dioxide by acid treatment
4 Principle
4.1 Method A (indirect procedure)

In this procedure, the TOC is obtained by the difference between the results of the measurements of TC

and TIC.

The total carbon (TC) present in the sample is converted into carbon dioxide by combustion in an

oxygen-containing gas flow free of carbon dioxide. To ensure complete combustion, catalysts and/or

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modifiers can be used. The released amount of carbon dioxide is measured e.g. by infrared

spectrometry, thermal conductivity detection, or other suitable techniques.

The TIC is determined separately from another sub-sample by means of acidification and purging of the

released carbon dioxide. The carbon dioxide shall be measured by one of the techniques mentioned

above.

NOTE Alternatively, for soil, the carbon present as carbonate (TIC) can be determined according to e.g.

ISO 10693 (volumetric method).
4.2 Method B (direct procedure)

In this procedure, the TIC present in the sample are previously removed by treating the sample with

acid. The carbon dioxide released by the following combustion step is measured by one of the

techniques mentioned in 4.1 and indicates the TOC directly.
4.3 Applicability of Methods A or B

Methods A and B have the same applicability for the determination of TOC and/or the determination of

the TIC to TOC ratio. In samples with relatively high TIC contents method B should be applied.

Method B can lead to incorrect results in the following cases:

— the sample contains volatile substances that evaporate during the acidification (e.g. volatile

hydrocarbons from sludge of oil separators);

— side reactions between the sample and the acid take place (e.g. decarboxylation, volatile reaction

products).

NOTE The quality of results of Method B is dependent on experience and practice, especially regarding the

steps before the determination of TOC. Use of automatic dispensing units regarding removal of TIC prior to

determination of TOC can improve the performance of Method B.
5 Interferences

Volatile organic substances can be lost during sample preparation. If necessary, the carbon content

resulting from volatile organic substances shall be determined separately.

Depending on the laboratory experience with samples containing high amounts of TIC, the procedures

can lead to unreliable TOC results if the TIC to TOC ratio is very high (e.g. ≥ 10).

Depending on the detection method used, different interferences can occur, for instance:

— the presence of cyanide can interfere with the coulometric detection of TIC by modifying the pH

value (dissolution of HCN);

— high content of halogenated compounds can lead to an overestimation of TOC when coulometric

detection is used; in some cases the classical silver or copper trap can be insufficient to absorb all

halides.

When present, elemental carbon, carbides, cyanides, cyanates, isocyanates, isothiocyanates and

thiocyanates are determined as organic carbon using the methods described in this document. An

interpretation of the measured value can therefore be problematic in cases where the sample contains

relevant levels of the above-mentioned components. If needed, these components shall be determined

separately by means of a suitable validated method and be recorded in the test report.

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6 Reagents
Use only reagents of recognized analytical grade, unless otherwise specified.
Hygroscopic substances shall be stored in a desiccator.
6.1 Calcium carbonate, CaCO .
6.2 Sodium carbonate, Na CO , anhydrous.
2 3
6.3 Tetrasodium ethylenediamine tetraacetate-tetra-hydrate, Na4-EDTA ∙ 4 H2O
(C H N O Na ∙ 4 H O), heated at 80 °C for 2 h.
10 12 2 8 4 2

Other forms of Na -EDTA hydrates may be used if the water content is exactly known. In these cases,

the composition of the control mixtures shall be recalculated accordingly (see also 6.10 and 6.11).

6.4 Potassium hydrogen phthalate, C H O K.
8 5 4
6.5 Acetanilide, C8H9NO.
6.6 Atropine, C H NO .
17 23 3
6.7 Spectrographic graphite powder, C.
6.8 Sodium salicylate, C7H5O3Na.
6.9 Aluminium oxide, Al2O3, neutral, granular size < 200 µm, annealed at 600 °C.

6.10 Control mixture A, prepared from sodium carbonate (6.2), Na -EDTA ∙ 4 H O (6.3)

4 2
and aluminium oxide (6.9) in a mass ratio of 2,34 : 1,00 : 7,28.

The mixture shall be homogenized. It should contain 25,00 g/kg TIC and 25,00 g/kg TOC (e.g. 22,06 g of

sodium carbonate, 9,41 g Na -EDTA ∙ 4 H O, 68,53 g of aluminium oxide).
4 2

6.11 Control mixture B, prepared from sodium salicylate (6.8), calcium carbonate (6.1), Na4-

EDTA · 4 H2O (6.3) and aluminium oxide (6.9) in a mass ratio of 1,00 : 4,36 : 1,97 : 8,40.

The mixture shall be homogenized. It should contain 33,3 g/kg TIC and 66,6 g/kg TOC (e.g. 6,36 g of

sodium salicylate, 27,78 g of calcium carbonate, 12,50 g of Na -EDTA · 4 H O, 53,36 g of aluminium

4 2
oxide).

6.12 Non-oxidizing mineral acid, used for carbon dioxide expulsion, e.g. phosphoric acid

H PO (w = 85 %).
3 4

NOTE Due to potential corrosion by hydrochloric acid, phosphoric acid is preferred for TIC determination in

Method A (9.1.3). Due to potential formation of P O during combustion, hydrochloric acid is preferred for

4 10
removal of inorganic carbon in Method B (10.1.2).

6.13 Carrier gas, e.g. synthetic air, nitrogen, oxygen or argon, free of carbon dioxide and

organic impurities in accordance with the manufacturer's instructions.
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7 Apparatus
7.1 Precision balance, accurate to at least 0,5 % of test portion weight.
7.2 Equipment for determination of carbon in solids, with relevant accessories.
7.3 Purging unit for TIC determination, for Method A only.
7.4 Vessels, made of e.g. ceramic, silica, quartz, silver or platinum.

NOTE Tin and nickel vessels are not acid-resistant. Tin vessels are suitable only for Method A.

8 Sample pre-treatment

Pre-treat the sample according to EN 16179 or EN 15002, if not otherwise specified.

For solid materials, dried samples shall be used.
NOTE 1 The drying method can affect the result.

Moist or paste-like waste samples may be mixed with aluminium oxide (6.9) until granular material is

obtained and then be comminuted. In this case, the ratio of aluminium oxide to sample shall be

considered in the calculation of TOC (according to 9.4 or 10.4).

If samples contain – depending on the accuracy of the method – negligible amounts of volatile

compounds except water, the samples may be dried.

NOTE 2 For waste samples, the homogeneity is important and often the aluminium oxide step is helpful. More

information is given in Annex B.
9 Procedure – Method A (indirect method)
9.1 Determination
9.1.1 General

The mass of the test portion should be as large as possible and shall be chosen so that the liberated

quantity of carbon dioxide lies within the working range of the equipment/calibration.

9.1.2 Determination of the TC

The sample prepared according to Clause 8 is weighed into a suitable vessel (7.4). To minimize carbon

blank values the vessel may be pre-treated by heating (in a muffle furnace or the TC apparatus itself).

The sample is combusted or decomposed in a flow of carrier gas containing oxygen (6.13).

The combustion temperature should be high enough to convert all carbon completely to carbon dioxide.

NOTE For samples containing carbonates, which are difficult to decompose, e.g. barium carbonate, the

release of the carbon dioxide can be improved by increasing the temperature or by the use of modifiers, e.g. tin,

copper (see B.1)

The temperature range of commercially available instruments is between 900 °C and 1500 °C.

During the combustion of reactive samples, explosion or fuming can be prevented by covering the

sample with inert material e.g. silica sand.

The amount of carbon dioxide released during the combustion is measured e.g. by infrared

spectrometry, thermal conductivity detection, or other suitable techniques, and is expressed as total

carbon (TC).
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9.1.3 Determination of the TIC

The sample prepared according to Clause 8 is weighed into the purging unit (7.3) or in the sample

vessel (7.4).

The system is closed gas-tight and flushed with carrier gas until no more carbon dioxide from ambient

air is present. Then acid (6.12) is added and the carbon dioxide is stripped by purging or stirring and/or

heating. The released carbon dioxide is transferred to the detector by the carrier gas.

The addition of wetting agents, e.g. surfactants, can improve wetting of the surface of the sample.

The addition of anti-foaming agents, e.g. silicone oil, can be helpful in the case of strongly foaming

samples.

The amount of carbon dioxide released during the gas evolution is measured e.g. by infrared

spectrometry, thermal conductivity detection, or other suitable techniques and is expressed as total

inorganic carbon (TIC).
NOTE TIC can alternatively be determined according to e.g. ISO 10693.

Samples containing persistent carbonates (e.g. concrete, cement) require treatment with hot acid for

complete release of carbon dioxide according to manufacturers' instructions.
9.2 Calibration

If a relative method is used for detection, e.g. infrared detection, calibration is necessary.

Calibration is to be performed according to the manufacturer's instruction.

Examples of calibration substances suitable for TC are calcium carbonate (6.1), potassium hydrogen

phthalate (6.4), acetanilide (6.5), atropine (6.6), spectrographic graphite powder (6.7).

The following procedure should be applied for calibration:
— Establish the preliminary working range.

— Measure a minimum of five standard samples. Typically, different sample weights of one calibration

substance are used to cover the calibration range. The absolute amount of carbon of these standard

samples shall be distributed evenly over the working range.

— Carry out a linear regression analysis and test the linearity of the calibration function (see also

ISO 8466-1).

— Use the calibration function for calculating the mean values of the recovery of each standard

sample.

The function shall be linear. Otherwise, the working range shall be restricted to the linear range.

If an absolute method is used for detection, e.g. coulometry, only control measurements according to 9.3

shall be carried out.

This calibration should be carried out for initial validation purposes or after major changes of the

equipment.
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9.3 Control measurements

Control measurements should be carried out using control mixture A (6.10) for the procedures

according to 9.1.2 (TC) and 9.1.3 (TIC). Analysis of one concentration from the middle of the respective

working range, possibly repeated two or three times, is sufficient. For the TC and TIC the mean recovery

shall be between 80 % and 120 % with a coefficient of variation ≤ 5 %.
Blank values shall be taken into account, if necessary.

If the required recoveries are not achieved, the following measures can be helpful.

For TC analysis:
— checking the homogeneity of the control mixture;
— checking the calibration;
— increasing the temperature during release of carbon dioxide;
— reducing the flow of the carrier gas;
— encouraging a turbulent flow in the combustion tube;
— use of modifiers;
— use of catalysts for post-oxidation of combustion gases.
For TIC analysis:
— optimizing the stirring speed and/or the gas flow in the purging vessel;
— improving the gas exchange in the purging vessel;
— avoiding condensation in the system.
9.4 Calculation and expression of results
The TC and TIC mass contents are calculated from
— calibration function and sample mass if relative detection methods are used,
— specific constants and sample mass if absolute detection methods are used.

The calculation of TOC is achieved from the difference of the mean values of TC and TIC according to

Formula (1):
m Fm− m (1)
( )
TOC TC TIC
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In case of mixing the sample with aluminium oxide (see Clause 8) a dilution factor following

Formula (2) shall be used:
m + m
F= (2)
where

is the TOC content as carbon in the sample expressed in grams per kilogram (g/kg);

TOC

is the mean value of the TC content as carbon in the sample, prepared according to Clause 8

expressed in grams per kilogram (g/kg);

is the mean value of the TIC content as carbon in the sample prepared according to Clause 8

TIC
expressed in grams per kilogram (g/kg);

is the dilution factor resulting from the sample preparation of the sample according to

Clause 8;
is the mass of the sample expressed in grams (g);
is the mass of aluminium oxide expressed in grams (g).
The TOC value resulting from Formula (1) is calculate
...