SIST-TS CEN/TS 17768:2023

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

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.

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

Dokument vzpostavlja metodologijo za razklop z zlatotopko za določevanje različnih hranil in elementov v sledovih (P, K, Ca, Mg, Na, S, B, Cu, Co, Fe, Mn, Mo, Zn, As, Cd, Cr, Hg, Ni, Pb) pred določitvijo njihove skupne vsebnosti.

General Information

• Status: Published
• Public Enquiry End Date: 02-Jan-2022
• Publication Date: 09-Jan-2023
• ICS: 65.080 - Fertilizers
• Technical Committee: KAT - Soil quality
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 06-Jan-2023
• Due Date: 13-Mar-2023
• Completion Date: 10-Jan-2023
• Directive: 2019/1009 - Regulation (EU) 2019/1009 of the European Parliament and of the Council of 5 June 2019 laying down rules on the making available on the market of EU fertilising products and amending Regulations (EC) No 1069/2009 and (EC) No 1107/2009 and repealing Regulation (EC) No 2003/2003
• Mandate: M/564 - Fertilising products in support of Regulation (EU) 2019/1009
• Ref Project: CEN/TS 17768:2022 - Organic and organo-mineral fertilizers - Digestion by aqua regia for subsequent determination of elements

Overview

CEN/TS 17768:2022 specifies an aqua regia digestion procedure for organic and organo‑mineral fertilizers to produce extracts suitable for subsequent element determination. The Technical Specification defines sample masses, reagent volumes, digestion conditions, pre‑concentration for low‑dry‑matter liquids, blank handling and storage of extracts. Extracts generated by this method are intended for analysis with CEN/TS 17770 and CEN/TS 17769 (e.g., ICP‑AES); ICP‑MS may be used as an alternative if equivalence is demonstrated.

Key topics and technical requirements

• Scope: digestion of organic and organo‑mineral fertilizers to enable multi‑element analysis (aqua regia soluble fraction).
• Sample mass:
  • Solids: weigh 2.5–5.0 g sample (≈1.5–3.0 g dry matter) for standard 150 ml final volume.
  • Liquids with low dry matter: pre‑concentration recommended (see below).
• Reagents (analytical grade): HCl 37% (≈12 mol/L), HNO3 65% (≈14.3 mol/L); antifoaming agents such as n‑dodecane or octanol.
• Typical digestion for 150 ml final volume:
  • Add 21 ml HCl and 7 ml HNO3 to sample (moisten solids with water first).
  • Reflux with condenser, maintain reflux for 2 hours (condensation zone < 1/3 height).
  • Cool, rinse condenser with ~10 ml water, transfer to 150 ml volumetric flask and dilute to mark.
• Alternative final volumes and recalculated reagent/sample parameters are provided (100 ml and 50 ml options).
• Pre‑concentration for liquids: weigh 10–50 g (to represent 1–3 g dry matter), evaporate to ≈5 ml at ~75 °C, then digest.
• Quality control: prepare blank using same procedure; filter/centrifuge if needed using ash‑free filter paper; store extracts in closed vessels for up to 15 days.
• Safety: perform digestion in a well‑ventilated fume hood and take precautions against acid fumes.
• Calculation of sample mass when LOQ/legislative limits require it:
  • m = LOQ × VF / LL
  • SW = m × 100 / DM (formulas and examples are given in Annex A).

Applications and users

• Laboratories performing regulatory compliance testing for EU fertilising products (Regulation (EU) 2019/1009).
• Quality control teams at fertilizer manufacturers and processors of organic or organo‑mineral products.
• Environmental and agricultural testing labs determining aqua‑regia‑extractable metals (Cd, Pb, As, Ni, etc.).
• Research groups comparing extraction methodologies or validating ICP‑AES / ICP‑MS measurement workflows.

Related standards

• CEN/TS 17769, CEN/TS 17770 (analytical measurement of extracts)
• CEN/TS 17773 (dry matter determination)
• EN 1482 (sampling and sample preparation)
• EN 13650 / EN 16174 (aqua regia extraction for other matrices)

Keywords: CEN/TS 17768:2022, aqua regia digestion, organic fertilizers, organo‑mineral fertilizers, element determination, ICP‑AES, ICP‑MS, sample pre‑concentration, EU fertilising products.

Standards Content (Sample)

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

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.

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

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.
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.
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
...