Organic and organo-mineral fertilizers - Digestion by aqua regia for subsequent determination of elements

The document establishes the methodology for the digestion by aqua regia of the different nutrients and trace elements (P, K, Ca, Mg, Na, S, B, Cu, Co, Fe, Mn, Mo, Zn, As, Cd, Cr, Hg, Ni, Pb) before the determination of their total content.

Organische und organisch-mineralische Düngemittel - Aufschluss durch Königswasser zur anschließenden Bestimmung der Elemente

Dieses Dokument legt das Verfahren für den Aufschluss verschiedener organischer Düngemittel und organisch-mineralischer Düngemittel mit Königswasser fest, um eine anschließende Bestimmung der Elemente zu ermöglichen.
Die Extrakte sind für die Analyse nach CEN/TS 17770 und CEN/TS 17769 geeignet.
ANMERKUNG   Alternativ kann die Massenspektrometrie mit induktiv gekoppeltem Plasma (ICP MS) für die Messung angewendet werden, sofern der Anwender nachweist, dass das Verfahren zu den gleichen Ergebnissen führt.

Engrais organiques et organo-minéraux - Digestion à l'eau régale pour le dosage ultérieur des éléments

Le présent document spécifie le mode opératoire de digestion de différents engrais organiques et organo-minéraux à l’eau régale pour permettre le dosage ultérieur des éléments.
Les extraits sont adaptés pour une analyse conformément à la CEN/TS 17770 et la CEN/TS 17769.
NOTE   Il est également possible d’utiliser la spectrométrie de masse couplée à un plasma inductif (ICP-MS) pour la mesure si l’utilisateur prouve que la méthode conduit aux mêmes résultats.

Organska in organsko-mineralna gnojila - Razklop z zlatotopko za določevanje elementov

General Information

Status
Published
Public Enquiry End Date
02-Jan-2022
Publication Date
09-Jan-2023
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
06-Jan-2023
Due Date
13-Mar-2023
Completion Date
10-Jan-2023

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SLOVENSKI STANDARD
SIST-TS CEN/TS 17768:2023
01-februar-2023
Organska in organsko-mineralna gnojila - Razklop z zlatotopko za določevanje
elementov
Organic and organo-mineral fertilizers - Digestion by aqua regia for subsequent
determination of elements

Organische und organisch-mineralische Düngemittel - Aufschluss durch Königswasser

zur anschließenden Bestimmung der Elemente
Engrais organiques et organo-minéraux - Digestion à l'eau régale pour le dosage
ultérieur des éléments
Ta slovenski standard je istoveten z: CEN/TS 17768:2022
ICS:
65.080 Gnojila Fertilizers
SIST-TS CEN/TS 17768:2023 en,fr,de

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

---------------------- Page: 1 ----------------------
SIST-TS CEN/TS 17768:2023
---------------------- Page: 2 ----------------------
SIST-TS CEN/TS 17768:2023
CEN/TS 17768
TECHNICAL SPECIFICATION
SPÉCIFICATION TECHNIQUE
April 2022
TECHNISCHE SPEZIFIKATION
ICS 65.080
English Version
Organic and organo-mineral fertilizers - Digestion by aqua
regia for subsequent determination of elements

Engrais organiques et organo-minéraux - Digestion à Organische und organisch-mineralische Düngemittel -

l'eau régale pour le dosage ultérieur des éléments Aufschluss durch Königswasser zur anschließenden

Bestimmung der Elemente

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 17768:2022 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST-TS CEN/TS 17768:2023
CEN/TS 17768:2022 (E)
Contents Page

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

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

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

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

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

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

5 Sampling and sample preparation ............................................................................................................ 5

6 Reagents ............................................................................................................................................................. 5

7 Apparatus ........................................................................................................................................................... 5

8 Procedure........................................................................................................................................................... 6

8.1 Sample digestion ............................................................................................................................................. 6

8.2 Sample pre-concentration ........................................................................................................................... 7

8.3 Blank .................................................................................................................................................................... 7

Annex A (informative) Adjustment to different digestion procedures and measurement

apparatuses ....................................................................................................................................................... 8

A.1 Adjustment of the procedure to different final volumes .................................................................. 8

A.2 Calculation of the sample mass .................................................................................................................. 8

A.2.1 General ................................................................................................................................................................ 8

A.2.2 Calculation of the mass of the sample – dry matter ............................................................................ 9

A.2.3 Calculation of the mass of the sample for analysis ............................................................................. 9

A.2.4 Example .............................................................................................................................................................. 9

Bibliography ................................................................................................................................................................. 10

---------------------- Page: 4 ----------------------
SIST-TS CEN/TS 17768:2023
CEN/TS 17768:2022 (E)
European foreword

This document (CEN/TS 17768:2022) 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 Standardization 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.
---------------------- Page: 5 ----------------------
SIST-TS CEN/TS 17768:2023
CEN/TS 17768:2022 (E)
Introduction

Aqua regia is applied to digest different matrices for the subsequent determination of many elements.

For example, a multi-matrix standard for aqua regia extraction of soils, sludges and biowaste was

prepared by CEN/TC 444 “Environmental characterization”. A similar procedure was applied for

determination of aqua regia extractable elements according to CEN/TS 17769 and CEN/TS 17770.

CEN/TC 223 “Soil improvers and growing media” published a standard for a similar procedure for soil

improvers and growing media. Wide use of the aqua regia digestion, availability of the instruments and

the possibility to merge the standards for different matrices in the future, were the main reasons for also

applying this method of digestion for organic and organo-mineral fertilizers.
---------------------- Page: 6 ----------------------
SIST-TS CEN/TS 17768:2023
CEN/TS 17768:2022 (E)
1 Scope

This document specifies the procedure for the digestion of different organic fertilizers and organo-

mineral fertilizers with aqua regia to enable a subsequent determination of elements.

The extracts are suitable for analysis using CEN/TS 17770 and CEN/TS 17769.

NOTE Alternatively, inductively coupled plasma mass spectrometry (ICP-MS) can be used for the measurement

if the user proves that the method gives the same results.
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:

— IEC Electropedia: available at https://www.electropedia.org/
— ISO Online browsing platform: available at https://www.iso.org/obp
4 Principle
The samples are digested by boiling in aqua regia.
5 Sampling and sample preparation

Sampling 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.

6 Reagents

All reagents should be of recognized analytical grade. The reagents and water used shall have negligible

concentrations of the elements to be determined if compared to the lowest concentrations of these

elements in the sample solution.
6.1 Hydrochloric acid 37 % HCl, c(HCl) ≈ 12 mol/l, ρ ≈ 1,18 g/ml.
6.2 Nitric acid 65 %, c(HNO ) ≈ 14,3 mol/l, ρ ≈ 1,4 g/ml.
6.3 Antifoaming agent, e.g. n-dodecane (C H ) or octanol (C H O) are suitabl
...

SLOVENSKI STANDARD
kSIST-TS FprCEN/TS 17768:2021
01-december-2021
Organska in organsko-mineralna gnojila - Razklop z zlatotopko za določevanje
elementov
Organic and organo-mineral fertilizers - Digestion by aqua regia for subsequent
determination of elements

Organische und organisch-mineralische Düngemittel - Aufschluss durch Königswasser

zur anschließenden Bestimmung der Elemente
Ta slovenski standard je istoveten z: FprCEN/TS 17768
ICS:
65.080 Gnojila Fertilizers
kSIST-TS FprCEN/TS 17768:2021 en,fr,de

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

---------------------- Page: 1 ----------------------
kSIST-TS FprCEN/TS 17768:2021
---------------------- Page: 2 ----------------------
kSIST-TS FprCEN/TS 17768:2021
FINAL DRAFT
TECHNICAL SPECIFICATION
FprCEN/TS 17768
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
November 2021
ICS 65.080
English Version
Organic and organo-mineral fertilizers - Digestion by aqua
regia for subsequent determination of elements
Organische und organisch-mineralische Düngemittel -
Aufschluss durch Königswasser zur anschließenden
Bestimmung der Elemente

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 17768:2021 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
kSIST-TS FprCEN/TS 17768:2021
FprCEN/TS 17768:2021 (E)
Contents Page

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

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

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

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

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

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

5 Sampling and sample preparation ............................................................................................................ 5

6 Reagents ............................................................................................................................................................. 5

6.1 Hydrochloric acid 37 % HCl, c(HCl) ≈ 12 mol/l, ρ ≈ 1,18 g/ml. ....................................................... 5

6.2 Nitric acid 65 %, c(HNO ) ≈ 14,3 mol/l, ρ ≈ 1,4 g/ml. ........................................................................ 5

6.3 Antifoaming agent, e.g. n-dodecane (C H ) or octanol (C H O) are suitable. ........................ 5

12 26 8 18

7 Apparatus ........................................................................................................................................................... 5

7.1 Common laboratory glassware .................................................................................................................. 5

7.2 Apparatus for thermal heating digestion, .............................................................................................. 5

7.3 Filter paper, ....................................................................................................................................................... 6

7.4 Analytical balance, capable of weighing to the nearest mg or better. ......................................... 6

8 Procedure........................................................................................................................................................... 6

8.1 Sample digestion ............................................................................................................................................. 6

8.2 Sample pre-concentration ........................................................................................................................... 6

8.3 Blank .................................................................................................................................................................... 7

Annex A (informative) Adjustment to different digestion procedures and measurement

apparatuses ....................................................................................................................................................... 8

A.1 Adjustment of the procedure to different final volumes .................................................................. 8

A.2 Calculation of the sample mass .................................................................................................................. 8

A.2.1 General ................................................................................................................................................................ 8

A.2.2 Calculation of the mass of the sample – dry matter ............................................................................ 9

A.2.3 Calculation of the mass of the sample for analysis ............................................................................. 9

A.2.4 Example .............................................................................................................................................................. 9

Bibliography ................................................................................................................................................................. 10

---------------------- Page: 4 ----------------------
kSIST-TS FprCEN/TS 17768:2021
FprCEN/TS 17768:2021 (E)
European foreword

This document (FprCEN/TS 17768:2021) 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 standardization request given to CEN by the European

Commission and the European Free Trade Association.
---------------------- Page: 5 ----------------------
kSIST-TS FprCEN/TS 17768:2021
FprCEN/TS 17768:2021 (E)
Introduction

Aqua regia is applied to digest different matrices for the subsequent determination of many elements.

For example, a multi-matrix standard for aqua regia extraction of soils, sludges and biowaste was

prepared by CEN/TC 444 “Environmental characterization”. A similar procedure was applied for

determination of aqua regia extractable elements according to FprCEN/TS 17769 and FprCEN/TS 17770.

CEN/TC 223 “Soil improvers and growing media” published a standard for a similar procedure for soil

improvers and growing media. Wide use of the aqua regia digestion, availability of the instruments and

the possibility to merge the standards for different matrices in the future, were the main reasons for also

applying this method of digestion for organic and organo-mineral fertilizers.
---------------------- Page: 6 ----------------------
kSIST-TS FprCEN/TS 17768:2021
FprCEN/TS 17768:2021 (E)
1 Scope

This document specifies the procedure for the digestion of different organic fertilizers and organo-

mineral fertilizers with aqua regia to enable a subsequent determination of elements.

The extracts are suitable for analysis using FprCEN/TS 17770 and FprCEN/TS 17769.

NOTE Alternatively, inductively coupled plasma mass spectrometry (ICP-MS) can be used for the measurement

if the user proves that the method gives the same results.
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:

• IEC Electropedia: available at https://www.electropedia.org/
• ISO Online browsing platform: available at https://www.iso.org/obp
4 Principle
The samples are digested by boiling in aqua regia.
5 Sampling and sample preparation

Sampling 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.

6 Reagents

All reagents should be of recognized analytical grade. The reagents and water used shall have negligible

concentrations of the elements to be determined if compared to the lowest concentrations of these

elements in the sample solution.
6.1 Hydrochloric acid 37 % HCl, c(HCl) ≈ 12 mol/l, ρ ≈ 1,18 g/ml.
6.2 Nitric acid 65 %, c(HNO ) ≈ 14,3 mol/l, ρ ≈ 1,4 g/ml.
6.3 Antifoaming agent, e.g. n-dodecane (C H ) or octanol (C H O) are suitable.
12 26 8 18
7 Apparatus
7.1
...

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