oSIST prEN 17505:2020

Soil and waste characterization - Temperature dependent differentiation of total carbon (TOC400, ROC, TIC900)

This European standard specifies a method for the differentiated determination of the organic carbon content (TOC400) which is released at temperatures up to 400 °C, the residual oxidizable carbon (ROC) (including e.g. lignite (brown coal), hard coal, charcoal, black carbon, soot) and the inorganic carbon (TIC900) which is released at temperatures up to 900 °C.
The basis is the dry combustion to CO2 in a in the presence of oxygen using using temperatures ranging from 150°C to 900 °C in dry solid samples of soil, soil with anthropogenic admixtures and solid waste (see Table 1) with carbon contents of more than 1 g per kg (0,1 % C) (per carbon type in the test portion).

Boden- und Abfallbeschaffenheit - Temperaturabhängige Unterscheidung von Gesamtkohlenstoff (TOC400, ROC, TIC900)

Diese Norm legt ein Verfahren zur differenzierten Bestimmung des Gehalts an organischem Kohlenstoff (TOC400), der bis 400 °C freigesetzt wird, restlichem oxidierbaren Kohlenstoff (ROC) (u. a. Braun-, Stein-, Holzkohle, schwarzer Kohlenstoff, Ruß) und anorganischem Kohlenstoff (TIC900), der bis 900 °C freigesetzt wird, fest.
Grundlage ist die trockene Verbrennung im Sauerstoffstrom zu CO2 mittels Temperaturgradienten von 150 °C bis 900 °C in trockenen Feststoffproben von Boden, Boden mit anthropogenen Beimengungen sowie festen Abfällen (siehe Tabelle 1) mit Gehalten von mehr als 1 g Kohlenstoff je kg (0,1 % C) (je Kohlenstoffart in der Messprobe).
Alternativ darf das Verfahren nach Anhang B verwendet werden.

Caractérisation des sols et des déchets - Différentiation en fonction de la température du carbone total (COT400, COR, CIT900)

Le présent document spécifie une méthode de détermination différenciée de la teneur en carbone organique (COT400) qui est libéré à des températures allant jusqu’à 400 °C, de la teneur en carbone oxydable résiduel (COR) (notamment du lignite (houille brune), de la houille, du charbon, du carbone suie, de la suie, par exemple) et de la teneur en carbone inorganique (CIT900) qui est libéré à des températures allant jusqu’à 900 °C.
La méthode repose sur la formation de CO2 par combustion sèche en présence d’oxygène à des températures allant de 150 °C à 900 °C d’échantillons solides anhydres de sol, de sol avec adjuvants anthropogènes et de déchets solides (voir Tableau 1) présentant des teneurs en carbone de plus de 1 g/kg (0,1 % C) (par type de carbone dans la prise d’essai).
La méthode spécifiée à l’Annexe B peut également être utilisée.

Karakterizacija tal in odpadkov - Diferenciacija celotnega ogljika (TOC400, ROC, TIC900) v odvisnosti od temperature

General Information

• Status: Not Published
• Public Enquiry End Date: 03-May-2020
• ICS: 13.030.10 - Solid wastes
• ICS: 13.080.10 - Chemical characteristics of soils
• Technical Committee: KAT - Soil quality
• Current Stage: 4020 - Public enquire (PE) (Adopted Project)
• Start Date: 28-Feb-2020
• Due Date: 17-Jul-2020
• Completion Date: 08-Jun-2020
• Ref Project: prEN 17505 - Soil and waste characterization — Temperature dependent differentiation of total carbon (TOC400, ROC, TIC900)

Standards Content (sample)

SLOVENSKI STANDARD
oSIST prEN 17505:2020
01-april-2020
Karakterizacija tal in odpadkov - Diferenciacija celotnega ogljika (TOC400, ROC,
TIC900) v odvisnosti od temperature

Soil and waste characterization - Temperature dependent differentiation of total carbon

(TOC400, ROC, TIC900)
Boden- und Abfallbeschaffenheit - Temperaturabhängige Unterscheidung von
Gesamtkohlenstoff (TOC400, ROC, TIC900)
Ta slovenski standard je istoveten z: prEN 17505
ICS:
13.030.10 Trdni odpadki Solid wastes
13.080.10 Kemijske značilnosti tal Chemical characteristics of
soils
oSIST prEN 17505:2020 en,fr,de

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

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oSIST prEN 17505:2020
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oSIST prEN 17505:2020
DRAFT
EUROPEAN STANDARD
prEN 17505
NORME EUROPÉENNE
EUROPÄISCHE NORM
April 2020
ICS 13.030.10; 13.080.10
English Version
Soil and waste characterization - Temperature dependent
differentiation of total carbon (TOC400, ROC, TIC900)
Boden- und Abfallbeschaffenheit -
Temperaturabhängige Unterscheidung von
Gesamtkohlenstoff (TOC400, ROC, TIC900)

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 17505:2020 E

worldwide for CEN national Members.
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Contents Page

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

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

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

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

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

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

5 Interferences .................................................................................................................................................... 6

5.1 Interference due to carbides ....................................................................................................................... 6

5.2 Interference due to sulfur and nitrogen compounds ......................................................................... 6

5.3 Interference due to carbonates .................................................................................................................. 6

5.4 Peak does not reach the baseline .............................................................................................................. 8

5.5 Difficulties in separating ROC peak and TIC peak .................................................................... 10

900

5.6 Interferences due to premature releases and deflagrations ....................................................... 10

6 Reagents .......................................................................................................................................................... 11

6.1 General ............................................................................................................................................................. 11

6.2 Oxygen, O , purity > 99,7 % (V/V) or synthetic air, purity > 99,7 %. ........................................ 11

6.3 Inert gas, e.g. nitrogen, N , (only for the alternative procedure specified in Annex B). .... 11

6.4 Calcium carbonate, CaCO . ....................................................................................................................... 11

6.5 Activated carbon........................................................................................................................................... 11

6.6 Microcrystalline cellulose ......................................................................................................................... 11

6.7 Aluminium oxide, Al O . ........................................................................................................................... 11

2 3

6.8 Standard for system control ..................................................................................................................... 11

7 Apparatus ........................................................................................................................................................ 11

7.1 Homogenization equipment, e.g. mixer, stirrer, grinders, mills. ................................................ 11

7.2 Analytical balance, (accurate to at least 0,5 % of the test portion weight). ............................ 11

7.3 Equipment for determining different carbon types in solids, which consists of: ................. 11

8 Procedure........................................................................................................................................................ 12

8.1 General ............................................................................................................................................................. 12

8.2 Sample preparation and processing ..................................................................................................... 12

8.3 Weighed portion ........................................................................................................................................... 12

8.4 Calibration ...................................................................................................................................................... 12

8.5 Measurement ................................................................................................................................................. 12

9 Evaluation ....................................................................................................................................................... 13

9.1 General ............................................................................................................................................................. 13

9.2 Control measurements ............................................................................................................................... 14

10 Expression of results ................................................................................................................................... 14

11 Test report ...................................................................................................................................................... 15

Annex A (informative) Performance characteristics ................................................................................... 16

Annex B (informative) Alternative carrier gases........................................................................................... 18

Bibliography ................................................................................................................................................................. 20

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European foreword

This document (prEN 17505:2020) has been prepared by Technical Committee CEN/TC 444 “Test

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

This document is currently submitted to the CEN Enquiry.
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Introduction

Carbon occurs in soils and materials similar to soil in a variety of compounds and forms. When

determining carbon in soils or soil-like materials, an overall determination of the different mass fractions

is most feasible. The summarized declaration of carbon is yet done by differentiating organic and

inorganic carbon (EN 15936, ISO 10694). In the proportion classified as “organic carbon”, a fraction of

very stable highly aromatic and highly condensed carbon compounds can be present, sometimes in

significant mass fractions. Since this black (pyrogenic) carbon is only very slowly decomposed and

released, its environmental relevance has to be differently evaluated than the proportions of organic

carbon which are faster chemical-biologically decomposed. The environmental relevance is estimated if

e.g. the suitability of soils and soil-like materials for disposal in landfill is assessed. For a differentiated

assessment, a separate declaration of the different mass fractions of organic, black (pyrogenic) and

inorganic carbon is necessary. Using the specified temperature-gradient method and utilizing the

combustion characteristic(s), the various bond types of carbon in soil and soil-like materials can be

differentiated.

In respect of the hazard potential, the content of solely organically bonded carbon in solids determined

with the described method can be important for disposal and/or recycling.

The method has been validated with the materials listed in Table 1, see also Annex A.

Table 1 — Materials used for validation
Material type Materials used for validation
soils from natural material mineral soils
soil with anthropogenic admixtures
tailing material (tailings) tailing material from coal mining
sludge dredged sludge
sediment sediment
waste waste incineration ash
foundry sands
recycling material
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1 Scope

This document specifies a method for the differentiated determination of the organic carbon content

(TOC ) which is released at temperatures up to 400 °C, the residual oxidizable carbon (ROC) (including

400

e.g. lignite (brown coal), hard coal, charcoal, black carbon, soot) and the inorganic carbon (TIC ) which

900
is released at temperatures up to 900 °C.

The basis is the dry combustion to CO in a in the presence of oxygen using temperatures ranging from

150 °C to 900 °C in dry solid samples of soil, soil with anthropogenic admixtures and solid waste (see

Table 1) with carbon contents of more than 1 g per kg (0,1 % C) (per carbon type in the test portion).

Alternatively, the method specified in Annex B may be applied.
2 Normative references
There are no normative references in this document.
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 http://www.iso.org/obp
— IEC Electropedia: available at http://www.electropedia.org/
3.1
total organic carbon which is released up to 400° C
TOC
400

carbon which is determined in the range between 150 °C to the 1st signal minimum at (400 ± 20) °C, in

the case of dry combustion in the presence of oxygen

Note 1 to entry: The TOC400 corresponds to the content of organically bonded carbon excluding ROC. This

carbon fraction is important regarding the hazard potential for disposal and/or recycling.

3.2
residual oxidizable carbon
ROC

carbon which is determined between the signal minima at (400 ± 20) °C and at (600 ± 20) °C, in the case

of dry combustion in the presence of oxygen

Note 1 to entry: When using the alternative normative method according to Annex B, then the ROC is defined as

the carbon determined during dry combustion in a current of oxygen after the TIC measurement at

900
(900 ± 20) °C.
Note 2 to entry: The black carbon is part of the ROC.
3.3
total inorganic carbon which is released up to 900° C
TIC
900

quantity of carbon present in the sample in the form of organic (TOC ), inorganic (TIC ) and black

400 900
carbon (ROC)
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3.4
total carbon

quantity of carbon present in the sample in the form of organic (TOC ), inorganic (TIC ) and black

400 900
carbon (ROC)
4 Principle

The determination of organic carbon (TOC ), residual oxidizable carbon (ROC) and inorganic carbon

400

(TIC ) in solid is effected by means of thermal oxidation or decomposition of the different bond types

900

of carbon at different temperatures to CO , if necessary, supported by changing between oxidizing and

non-oxidizing carrier gases.

The application of the gradient method with a suitable temperature program allows the determination of

organic carbon (TOC ), residual oxidizable carbon (ROC) and inorganic carbon (TIC ) and the

400 900
calculation of total carbon (TC) by totalling these contents.

The final analysis of CO can be performed with different methods, e.g. by means of infrared detection or

CO sensitive sensors.
5 Interferences
5.1 Interference due to carbides
Several carbides can interfere with this method.
5.2 Interference due to sulfur and nitrogen compounds

Depending on the measuring technique used, high contents of sulfur or nitrogen compounds can result

in overestimations or underestimations. This can be controlled by means of selected standard samples

(e.g. potassium sulfate, potassium nitrate). Furthermore, the information provided by the equipment

manufacturer shall be considered.
5.3 Interference due to carbonates

The thermal stability of carbonates exhibits a great bandwidth (for examples see Figures 1, 2 and 3).

Therefore, carbonates might be detected in both the TOC peak range and the ROC range. In the

400

presence of certain carbonates or carbonate mixtures which decompose at low temperature ranges, the

identification of the TIC peak is sometimes difficult or impossible. Alternatively, the impact of

900
carbonates on the TOC analysis can be determined by stripping with acid.
400

For samples containing the more thermally stable carbonates, e.g. barium carbonate, the liberation of

carbon dioxide can be improved by increasing temperature or using additives such as tungsten oxide.

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Key
X time
Y1 signal intensities
Y2 temperature in °C
Figure 1 — Example diagram FeCO
Key
X time
Y1 signal intensities
Y2 temperature in °C
Figure 2 — Example diagram MnCO ·fH O
3 2
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Key
X time
Y1 signal intensities
Y2 temperature in °C
Figure 3 — Example diagram PbCO
5.4 Peak does not reach the baseline
...