SIST-TS CEN/TS 17776:2023
(Main)Organic and organo-mineral fertilizers - Determination of the total organic carbon (TOC) content by dry combustion
Organic and organo-mineral fertilizers - Determination of the total organic carbon (TOC) content by dry combustion
This document specifies a method for the determination of the organic carbon content in organic and organo-mineral fertilizers.
Organische und organisch-mineralische Düngemittel - Bestimmung des Gehalts an gesamtem organischem Kohlenstoff (TOC) durch trockene Verbrennung
Dieses Dokument ist für Düngeprodukte anzuwenden, die den Kategorien PFC 1(A) und PFC 1(B) zugeordnet oder als Komponente der Kategorien PFC 1(A) und PFC 1(B) in PFC 7 der Verordnung (EU) 2019/1009 [5] eingestuft sind. Das vorliegende Verfahren wurde jedoch nicht für Mischungen validiert.
In diesem Dokument wird ein Verfahren zur Bestimmung des gesamten organischen Kohlenstoffes (TOC, en: total organic carbon) durch Elementaranalyse mit Trockenverbrennung angegeben. Das Verfahren ist anzuwenden für organische und organisch-mineralische Düngemittel mit einem Kohlenstoffgehalt von mehr als 1 g je kg Trockenmasse (0,1 %), ausgenommen organisch-mineralische Düngemittel, die Harnstoff-Formaldehyd-Polymere enthalten, solange kein Verfahren zur Beurteilung von Kohlenstoff in Harnstoff-Formaldehyd-Polymeren zur Verfügung steht.
Engrais organiques et organo-minéraux - Détermination de la teneur en carbone organique total (COT) par combustion sèche
Le présent document est applicable aux fertilisants qui sont classés dans les catégories PFC 1(A) et PFC 1(B) ou comme composants de PFC 1(A) et de PFC 1(B) dans la catégorie PFC 7 du Règlement (UE) 2019/1009 [5]. Toutefois, la présente méthode n’a pas été validée pour les mélanges.
Le présent document spécifie une méthode pour la détermination de la teneur en carbone organique total (COT) par une analyse élémentaire ayant recours à une combustion sèche. La méthode est applicable aux engrais organiques et organo-minéraux contenant plus de 1 g de carbone par kg de matière sèche (0,1 %), à l’exclusion des engrais organo-minéraux contenant des polymères urée-formaldéhyde tant qu’il n’existe pas de méthode disponible pour évaluer la teneur en carbone dans les polymères urée-formaldéhyde.
Organska in organsko-mineralna gnojila - Določevanje celotnega organskega ogljika (TOC) s suhim sežigom
Ta dokument določa metodo za določevanje organskega ogljika v organskih in organsko-mineralnih gnojilih.
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
SIST-TS CEN/TS 17776:2023
01-februar-2023
Organska in organsko-mineralna gnojila - Določevanje celotnega organskega
ogljika (TOC) s suhim sežigom
Organic and organo-mineral fertilizers - Determination of the total organic carbon (TOC)
content by dry combustion
Organische und organisch-mineralische Düngemittel - Bestimmung des Gehalts an
gesamtem organischem Kohlenstoff (TOC) durch trockene Verbrennung
Engrais organiques et organo-minéraux - Détermination de la teneur en carbone
organique total (COT) par combustion sèche
Ta slovenski standard je istoveten z: CEN/TS 17776:2022
ICS:
65.080 Gnojila Fertilizers
SIST-TS CEN/TS 17776:2023 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST-TS CEN/TS 17776:2023
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SIST-TS CEN/TS 17776:2023
CEN/TS 17776
TECHNICAL SPECIFICATION
SPÉCIFICATION TECHNIQUE
April 2022
TECHNISCHE SPEZIFIKATION
ICS 65.080
English Version
Organic and organo-mineral fertilizers - Determination of
the total organic carbon (TOC) content by dry combustion
Engrais organiques et organo-minéraux - Organische und organisch-mineralische Düngemittel -
Détermination de la teneur en carbone organique Bestimmung des Gehalts an organischem Kohlenstoff
(TOC) durch trockene Verbrennung
This Technical Specification (CEN/TS) was approved by CEN on 13 March 2022 for provisional application.
The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to
submit their comments, particularly on the question whether the CEN/TS can be converted into a European Standard.
CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS
available promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in
parallel to the CEN/TS) until the final decision about the possible conversion of the CEN/TS into an EN is reached.
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
© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 17776:2022 E
worldwide for CEN national Members.
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SIST-TS CEN/TS 17776:2023
CEN/TS 17776:2022 (E)
Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Process . 5
4.1 Principle . 5
4.2 Applicability . 5
4.3 Interferences . 5
5 Reagents . 5
6 Apparatus . 6
7 Procedure . 6
7.1 Sampling and sample preparation . 6
7.2 Determination . 7
7.3 Calibration . 8
7.4 Control measurements . 9
8 Calculation and expression of results . 9
9 Test report . 10
Annex A (informative) Example of operational information . 12
Bibliography . 14
2
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SIST-TS CEN/TS 17776:2023
CEN/TS 17776:2022 (E)
European foreword
This document (CEN/TS 17776:2022) has been prepared by Technical Committee CEN/TC 260
“Fertilizers and liming materials”, the secretariat of which is held by DIN.
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 has been prepared under a standardisation request given to CEN by the European
Commission and the European Free Trade Association.
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 announce this Technical Specification: 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.
3
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SIST-TS CEN/TS 17776:2023
CEN/TS 17776:2022 (E)
1 Scope
This document is applicable to fertilizing products, which are classified as PFC 1(A) and PFC 1(B) or the
PFC 1(A) and PFC 1(B) component in PFC 7 of Regulation (EU) 2019/1009 [5]. However, the present
method was not validated for blends.
This document specifies a method for the determination of total organic carbon (TOC) by elemental
analysis using dry combustion. The method is applicable to organic and organo-mineral fertilizers
containing more than 1 g carbon per kg of dry matter (0,1 %), with the exclusion of organo-mineral
fertilizers containing urea-formaldehyde polymers as long as there is no method available to assess
carbon in urea-formaldehyde polymers.
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.
CEN/TS 17771, Organic and organo-mineral fertilizers — Determination of the nitrogen content
CEN/TS 17773, Organic and organo-mineral fertilizers — Determination of the dry matter content
EN 15705, Fertilizers — Determination of urea condensates using high-performance liquid
chromatography (HPLC) — Isobutylidenediurea and crotonylidenediurea (method A) and methylen-urea
oligomers (method B)
EN ISO 3696:1995, Water for analytical laboratory use — Specification and test methods (ISO 3696: 1987)
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
• IEC Electropedia: available at https://www.electropedia.org/
3.1
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
Note 1 to entry: In agreement with Regulation (EU) 2019/1009 [5], carbon derived from urea and polymers
containing urea are not considered as organic in this document.
4
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SIST-TS CEN/TS 17776:2023
CEN/TS 17776:2022 (E)
4 Process
4.1 Principle
The carbon dioxide released by the following combustion in an oxygen containing gas flow free of carbon
dioxide, is measured by infrared spectrometry, thermal conductivity detection, or by the detector
provided by the equipment used. To ensure complete combustion, catalysts and/or modifiers can be
used. The released amount of carbon dioxide indicates the TOC.
The carbonates present in the sample shall be previously removed by treating the sample with acid.
4.2 Applicability
The method is applicable to organic and organo-mineral fertilizers both solid and liquid.
The present method is not selective, because combustion occurs for both organic and inorganic carbon.
4.3 Interferences
In the case of experience with samples containing high amounts of carbonates (e.g. carbonates to TOC
ratio higher than 10) the operator shall take care to correctly eliminate all the carbonates to make sure
to produce reliable TOC results.
When present, carbon from urea and urea-condensates carbides is determined as organic carbon using
the method described in this document. An interpretation of the measured value may 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.
Carbon from urea and urea-condensates (crotonyliden diurea, CDU and isobutyliden diurea, IBDU),
determined separately using CEN/TS 17771 and EN 15705 may be subtracted if required for the sample.
If this is done this shall be reported by the laboratory.
5 Reagents
All water used shall be grade 3 according to EN ISO 3696:1995. All reagents shall be of recognized
analytical grade.
5.1 Potassium hydrogen phthalate, C H O K.
8 5 4
5.2 Acetanilide, C H NO.
8 9
5.3 Atropine, C H NO .
17 23 3
5.4 Sodium salicylate, C H O Na.
7 5 3
5.5 Tetrasodium ethylenediamine tetraacetate-tetra-hydrate, Na -EDTA ⋅ 4H O
4 2
(C H N O Na ⋅ 4H 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
4
composition of the control mixtures shall be recalculated accordingly (see also 5.8).
5.6 Aluminum oxide, Al O , neutral, granular size < 200 µm, annealed at 600 °C.
2 3
5.7 Calcium carbonate, CaCO .
3
5
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SIST-TS CEN/TS 17776:2023
CEN/TS 17776:2022 (E)
5.8 Control mixture
Control mixture prepared from sodium salicylate (5.4), calcium carbonate (5.7), Na -EDTA ⋅ 4H O (5.5)
4 2
and aluminum oxide (5.6) in a mass ratio of 1,00 : 4,36 : 1,97 : 8,40.
The mixture shall be homogenised. It should contain 33,3 g/kg total inorganic carbon 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 ⋅ 4H O, 53,36 g of
4 2
aluminum oxide).
®1
5.9 Chromosorb (inert absorbent material for determination on fluid samples).
5.10 Non-oxidizing mineral acid used for carbon dioxide expulsion, e.g. phosphoric acid H PO
3 4
(w = 85 %).
NOTE Due to possible corrosion by hydrochloric acid, phosphoric acid is preferred.
5.11 Carrier gas, e.g. helium, oxygen or argon, free of carbon dioxide and organic impurities in
accordance with the manufacturer's instructions.
6 Apparatus
6.1 Precision balance, capable of weighing to the nearest 0,5 % of test portion mass.
6.2 Equipment for determination of carbon in solids, with accessories.
6.3 Crucibles, capsules or boats, made of e.g. silver, tin, ceramics or platinum.
Tin and nickel crucibles are not acid-resistant. In case of the necessity to remove inorganic carbon (see
7.2.4), silver or ceramics vessels shall be used.
6.4 Pasteur pipettes.
6.5 Drying system, thermostatically controlled and capable of maintaining temperature of
(105 ± 2) °C.
6.6 Desiccator, with an active drying agent such as silica gel.
6.7 Evaporating dish or crucible, temperature tolerant laboratory vessel with a temperature
resistance of at least 110 °C. Suitable materials are metallic, ceramic, borosilicate glass or quartz,
porcelain, etc.
7 Procedure
7.1 Sampling and sample preparation
Sampling and sample preparation should be performed carefully, following the principles described in
EN 1482 (all parts) with appropriate adaptations, required to ac
...
SLOVENSKI STANDARD
kSIST-TS FprCEN/TS 17776:2021
01-december-2021
Organska in organsko-mineralna gnojila - Določevanje organskega ogljika
Organic and organo-mineral fertilizers - Determination of the organic carbon content
Organische und organisch-mineralische Düngemittel - Bestimmung des Gehalts an
organischem Kohlenstoff
Engrais organiques et organo-minéraux - Détermination de la teneur en carbone
organique
Ta slovenski standard je istoveten z: FprCEN/TS 17776
ICS:
65.080 Gnojila Fertilizers
kSIST-TS FprCEN/TS 17776:2021 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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kSIST-TS FprCEN/TS 17776:2021
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kSIST-TS FprCEN/TS 17776:2021
FINAL DRAFT
TECHNICAL SPECIFICATION
FprCEN/TS 17776
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
November 2021
ICS 65.080
English Version
Organic and organo-mineral fertilizers - Determination of
the organic carbon content
Organische und organisch-mineralische Düngemittel -
Bestimmung des Gehalts an organischem Kohlenstoff
This draft Technical Specification is submitted to CEN members for Vote. It has been drawn up by the Technical Committee
CEN/TC 260.
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 Technical Specification. It is distributed for review and comments. It is subject to change
without notice and shall not be referred to as a Technical Specification.
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. FprCEN/TS 17776:2021 E
worldwide for CEN national Members.
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kSIST-TS FprCEN/TS 17776:2021
FprCEN/TS 17776:2021 (E)
Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Process . 5
4.1 Principle . 5
4.2 Applicability . 5
4.3 Interferences . 5
5 Reagents . 5
6 Apparatus . 6
7 Procedure . 6
7.1 Sampling and sample preparation . 6
7.2 Determination . 7
7.2.1 General. 7
7.2.2 Preparation of solid samples . 7
7.2.3 Preparation of liquid samples . 7
7.2.4 Removal of inorganic carbon and determination of the TOC . 7
7.3 Calibration . 8
7.4 Control measurements . 9
8 Calculation and expression of results . 9
9 Test report . 10
Annex A (informative) Example of operational information . 12
Bibliography . 14
2
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kSIST-TS FprCEN/TS 17776:2021
FprCEN/TS 17776:2021 (E)
European foreword
This document (FprCEN/TS 17776:2021) has been prepared by Technical Committee CEN/TC 260
“Fertilizers and liming materials”, the secretariat of which is held by DIN.
This document is currently submitted to the Vote on TS.
This document has been prepared under a standardisation request given to CEN by the European
Commission and the European Free Trade Association.
3
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kSIST-TS FprCEN/TS 17776:2021
FprCEN/TS 00260239:2021 (E)
1 Scope
This document is applicable to fertilizing products, which are classified as PFC 1(A) and PFC 1(B) or the
PFC 1(A) and PFC 1(B) component in PFC 7 of Regulation (EU) 2019/1009 [5]. However, the present
method was not validated for blends.
This document specifies a method for the determination of total organic carbon (TOC) by elemental
analysis using dry combustion. The method is applicable to organic and organo-mineral fertilizers
containing more than 1 g carbon per kg of dry matter (0,1 %), with the exclusion of organo-mineral
fertilizers containing urea-formaldehyde polymers as long as there is no method available to assess
carbon in urea-formaldehyde polymers.
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.
FprCEN/TS 17771, Organic and organo-mineral fertilizers — Determination of the nitrogen content
FprCEN/TS 17773, Organic and organo-mineral fertilizers — Determination of the dry matter content
EN 15705, Fertilizers — Determination of urea condensates using high-performance liquid
chromatography (HPLC) — Isobutylidenediurea and crotonylidenediurea (method A) and methylen-urea
oligomers (method B)
EN ISO 3696:1995, Water for analytical laboratory use — Specification and test methods (ISO 3696: 1987)
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
• IEC Electropedia: available at https://www.electropedia.org/
3.1
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
Note 1 to entry: In agreement with Regulation (EU) 2019/1009 [5], carbon derived from urea and polymers
containing urea are not considered as organic in this document.
4
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kSIST-TS FprCEN/TS 17776:2021
FprCEN/TS 17776:2021 (E)
4 Process
4.1 Principle
The carbon dioxide released by the following combustion in an oxygen containing gas flow free of carbon
dioxide, is measured by infrared spectrometry, thermal conductivity detection, or by the detector
provided by the equipment used. To ensure complete combustion, catalysts and/or modifiers can be
used. The released amount of carbon dioxide indicates the TOC.
The carbonates present in the sample shall be previously removed by treating the sample with acid.
4.2 Applicability
The method is applicable to organic and organo-mineral fertilizers both solid and liquid.
The present method is not selective, because combustion occurs for both organic and inorganic carbon.
4.3 Interferences
In the case of experience with samples containing high amounts of carbonates (e.g. carbonates to TOC
ratio higher than 10) the operator shall take care to correctly eliminate all the carbonates to make sure
to produce reliable TOC results.
When present, carbon from urea and urea-condensates carbides is determined as organic carbon using
the method described in this document. An interpretation of the measured value may 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.
Carbon from urea and urea-condensates (crotonyliden diurea, CDU and isobutyliden diurea, IBDU),
determined separately using FprCEN/TS 17771 and EN 15705 may be subtracted if required for the
sample. If this is done this shall be reported by the laboratory.
5 Reagents
All water used shall be grade 3 according to EN ISO 3696:1995. All reagents shall be of recognized
analytical grade.
5.1 Potassium hydrogen phthalate, C H O K.
8 5 4
5.2 Acetanilide, C H NO.
8 9
5.3 Atropine, C H NO .
17 23 3
5.4 Sodium salicylate, C H O Na.
7 5 3
5.5 Tetrasodium ethylenediamine tetraacetate-tetra-hydrate, Na -EDTA ⋅ 4H O (C H N O Na ⋅
4 2 10 12 2 8 4
4H O), heated at 80 °C for 2 h.
2
Other forms of Na -EDTA hydrates may be used if the water content is exactly known. In these cases, the
4
composition of the control mixtures shall be recalculated accordingly (see also 5.8).
5.6 Aluminum oxide, Al O , neutral, granular size < 200 µm, annealed at 600 °C.
2 3
5.7 Calcium carbonate, CaCO .
3
5
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kSIST-TS FprCEN/TS 17776:2021
FprCEN/TS 00260239:2021 (E)
5.8 Control mixture
Control mixture prepared from sodium salicylate (5.4), calcium carbonate (5.7), Na -EDTA ⋅ 4H O (5.5)
4 2
and aluminum oxide (5.6) in a mass ratio of 1,00 : 4,36 : 1,97 : 8,40.
The mixture shall be homogenised. It should contain 33,3 g/kg total inorganic carbon 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 ⋅ 4H O, 53,36 g of
4 2
aluminum oxide).
®1
5.9 Chromosorb (inert absorbent material for determination on fluid samples).
5.10 Non-oxidizing mineral acid used for carbon dioxide expulsion, e.g. phosphoric acid H PO
3 4
(w = 85 %).
NOTE Due to possible corrosion by hydrochloric acid, phosphoric acid is preferred.
5.11 Carrier gas, e.g. helium, oxygen or argon, free of carbon dioxide and organic impurities in
accordance with the manufacturer's instructions.
6 Apparatus
6.1 Precision balance, capable of weighing to the nearest 0,5 % of test portion mass.
6.2 Equipment for determination of carbon in solids, with accessories.
6.3 Crucibles, capsules or boats, made of e.g. silver, tin, ceramics or platinum.
Tin and nickel crucibles are not acid-resistant. In case of the necessity to remove inorganic carbon (see
7.2.4), silver or ceramics vessels shall be used.
6.4 Pasteur pipettes.
6.5 Drying system, thermostatically controlled and capable of maintaining temperature of
(105 ± 2) °C.
6.6 Desiccator, with an active drying agent such as silica gel.
6.7 Evaporating dish or crucible, temperature tolerant laboratory vessel with a temperature
resistance of at least 110 °C. Suitable materials are metallic, ceramic, borosilicate glass or quartz,
porcelain, etc.
7 Procedure
7.1 Sampling and sample preparation
Sampling and sample preparation should be performed carefully, following the principles described in
EN 1482 (all parts) with appropriate adaptations, required to account for specificities of organic and
organo-mineral fertilizers. Grinding of the laboratory sample is recommended for homogeneity reasons.
The sample shall then pass through a sieve of 0,5 mm.
1 ®
Chromosorb is the trade name of a product. This information is given for the convenience of users of this
document and do
...
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