Organic and organo-mineral fertilizers - Determination of the content of specific elements by ICP-AES after extraction by water

The document establishes the methodology for the determination of water-soluble content of P, K, Ca, Mg, Na, S, B, Co, Cu, Fe, Mn, Mo, Zn by ICP-AES.

Organische und organisch-mineralische Düngemittel - Bestimmung des Gehalts spezifischer Elemente mittels ICP-AES nach Extraktion mit Wasser

Dieses Dokument legt ein Verfahren zur Bestimmung von Bor (B), Kobalt (Co), Kupfer (Cu), Eisen (Fe), Mangan (Mn), Molybdän (Mo) und Zink (Zn) in Extrakten organischer Düngemittel und organisch-mineralischer Düngemittel mittels Atomemissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP AES) fest.
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.
Dieses Verfahren ist anwendbar auf Wasser-Extrakte, die nach CEN/TS 17766 hergestellt werden. Das Verfahren kann zur Bestimmung anderer Elemente angewendet werden, vorausgesetzt der Anwender hat die Anwendbarkeit überprüft.

Engrais organiques et organo-minéraux - Détermination de la teneur en éléments spécifiques par ICP-AES après extraction à l'eau

Le présent document spécifie une méthode pour le dosage du bore (B), du cobalt (Co), du cuivre (Cu), du fer (Fe), du manganèse (Mn), du molybdène (Mo) et du zinc (Zn) dans les extraits d’engrais organiques et organo-minéraux par spectrométrie d’émission atomique par plasma à couplage inductif (ICP-AES).
NOTE   La spectrométrie de masse par plasma à couplage inductif (ICP-MS) peut également être utilisée pour la mesure si l’utilisateur prouve que la méthode conduit aux mêmes résultats.
Cette méthode est applicable aux extraits aqueux préparés conformément à la CEN/TS 17766. La méthode peut également être utilisée pour le dosage d’autres éléments, à condition que l’utilisateur ait vérifié son applicabilité.

Organska in organsko-mineralna gnojila - Določanje vsebnosti specifičnih elementov z atomsko emisijsko spektrometrijo z induktivno sklopljeno plazmo (ICP-AES) po ekstrakciji z vodo

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

Buy Standard

Technical specification
SIST-TS CEN/TS 17774:2023
English language
12 pages
sale 10% off
Preview
sale 10% off
Preview
e-Library read for
1 day
Draft
kSIST-TS FprCEN/TS 17774:2021
English language
12 pages
sale 10% off
Preview
sale 10% off
Preview
e-Library read for
1 day

Standards Content (Sample)

SLOVENSKI STANDARD
SIST-TS CEN/TS 17774:2023
01-februar-2023
Organska in organsko-mineralna gnojila - Določanje vsebnosti specifičnih
elementov z atomsko emisijsko spektrometrijo z induktivno sklopljeno plazmo
(ICP-AES) po ekstrakciji z vodo

Organic and organo-mineral fertilizers - Determination of the content of specific elements

by ICP-AES after extraction by water
Organische und organisch-mineralische Düngemittel - Bestimmung des Gehalts
spezifischer Elemente mittels ICP-AES nach Extraktion mit Wasser
Engrais organiques et organo-minéraux - Détermination de la teneur en éléments
spécifiques par ICP-AES après extraction à l'eau
Ta slovenski standard je istoveten z: CEN/TS 17774:2022
ICS:
65.080 Gnojila Fertilizers
SIST-TS CEN/TS 17774:2023 en,fr,de

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

---------------------- Page: 1 ----------------------
SIST-TS CEN/TS 17774:2023
---------------------- Page: 2 ----------------------
SIST-TS CEN/TS 17774:2023
CEN/TS 17774
TECHNICAL SPECIFICATION
SPÉCIFICATION TECHNIQUE
April 2022
TECHNISCHE SPEZIFIKATION
ICS 65.080
English Version
Organic and organo-mineral fertilizers - Determination of
the content of specific elements by ICP-AES after
extraction by water

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

Détermination de la teneur en éléments spécifiques par Bestimmung des Gehalts spezifischer Elemente mittels

ICP-AES après extraction à l'eau ICP-AES nach Extraktion mit Wasser

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 17774:2022 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST-TS CEN/TS 17774:2023
CEN/TS 17774:2022 (E)
Contents Page

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

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

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

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

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

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

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

5.1 General ................................................................................................................................................................ 6

5.2 Spectral interferences ................................................................................................................................... 6

5.3 Transport interferences ............................................................................................................................... 6

5.4 Excitation interferences ............................................................................................................................... 6

5.5 Chemical interferences ................................................................................................................................. 6

5.6 Memory interferences ................................................................................................................................... 6

6 Reagents ............................................................................................................................................................. 7

7 Apparatus ........................................................................................................................................................... 7

8 Procedure........................................................................................................................................................... 8

8.1 Preparation of test and blank solution ................................................................................................... 8

8.2 Preparation of the calibration solutions ................................................................................................ 8

8.3 Measurement .................................................................................................................................................... 8

9 Calculation and expression of the results ........................................................................................... 11

10 Test report ...................................................................................................................................................... 11

Bibliography ................................................................................................................................................................. 12

---------------------- Page: 4 ----------------------
SIST-TS CEN/TS 17774:2023
CEN/TS 17774:2022 (E)
European foreword

This document (CEN/TS 17774:2022) 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 17774:2023
CEN/TS 17774:2022 (E)
Introduction

This document is part of a modular approach and concerns the analytical measurement step. “Modular”

means that a test standard concerns a specific step in assessing a property and not the whole chain of

measurements. Inductively coupled plasma atomic emission spectrometry (ICP-AES) is nowadays widely

used and a well-established method in many laboratories.
---------------------- Page: 6 ----------------------
SIST-TS CEN/TS 17774:2023
CEN/TS 17774:2022 (E)
1 Scope

This document specifies a method for the determination of boron (B), cobalt (Co), copper (Cu), iron (Fe),

manganese (Mn), molybdenum (Mo) and zinc (Zn) in organic fertilizers and organo-mineral fertilizers

extracts using inductively coupled plasma-atomic emission spectrometry (ICP-AES).

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.

This method is applicable to water extracts prepared according to CEN/TS 17766. The method can be

used for the determination of other elements, provided the user has verified the applicability.

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 17766, Organic and organo-mineral fertilizers — Extraction by water for subsequent

determination of elements

EN 12944-1, Fertilizers and liming materials — Vocabulary — Part 1: General terms

EN 12944-2, Fertilizers and liming materials — Vocabulary — Part 2: Terms relating to fertilizers

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 terms and definitions given in EN 12944-1 and EN 12944-2 apply.

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 method is based on the ICP-AES measurement of the concentration of boron (B), cobalt (Co), copper

(Cu), iron (Fe), manganese (Mn), molybdenum (Mo) and zinc (Zn) in fertilizer extracts prepared

according to CEN/TS 17766. The elements are determined after appropriate dilution of the extract. The

solution is dispersed by a nebulizer of the ICP-AES instrument and the resulting aerosol is transported

into the plasma. Element specific emission spectra are produced by a radio-frequency inductively coupled

argon plasma where atoms or ions are excited at high temperature. The emission spectra are dispersed

by a spectrometer, and the intensities of the emission lines are monitored by photosensitive devices.

Multi-element determinations using sequential or simultaneous optical systems and axial or radial

viewing of the plasma may be used.

The method may be used for the determination of other elements, provided the user has verified the

applicability.
---------------------- Page: 7 ----------------------
SIST-TS CEN/TS 17774:2023
CEN/TS 17774:2022 (E)
5 Interferences
5.1 General

Interferences and matrix effects shall be recognized and appropriate measures to minimize them shall be

made. There are several types of interferences – see 5.2 to 5.6.
5.2 Spectral interferences

Spectral interferences are due to incomplete isolation of the radiation emitted by the analyte from other

detected radiation sources. Spectral interferences are caused by background emission from continuous

or recombination phenomena, by stray light which causes background increase or overlap of a spectral

line from another element, or unresolved overlap of molecular band spectra. Background emission and

stray light can usually be compensated for by subtracting the background emission measured adjacent to

the analyte wavelength peak. To correct a sloping background shift two background correction points on

each side of the peak are used. Increase of background is more intensive with axial-view instruments.

Background correction is not required in cases of line broadening where a background correction

measurement would actually degrade the analytical result. A spectral line overlap usually leads to the

choice of an alternative line. If this is not possible, mathematical correction procedures (e.g. inter-element

correction technique, multi-component spectral fitting) can be used to compensate for the interference.

These correction procedures are usually a part of the instrument software.
5.3 Transport interferences

Transport interferences are caused by differences in the properties between the sample solutions and

the calibration solutions (viscosity, surface tension, density, dissolved solid content, type and

concentration of acids). As a consequence, the supply of solution to the nebuliser, the efficiency of

nebulisation and the droplet size distribution of the aerosol is altered, resulting in a change of sensitivity.

Errors due to these interferences can be overcome by dilution of the solutions, by matrix matching, by

standard addition or by internal standard.
5.4 Excitation interferences

Excitation interferences are attributed to a change in the excitation conditions in the plasma, especially

by the presence of easily ionisable elements. The interference depends on the operating conditions of the

plasma (e.g. power, sample introduction, gas flowrate or observation height) and differ from element to

element. Improvement of the plasma conditions can therefore reduce excitation interferences. Other

possibilities are dilution of the solutions, matrix matching or the standard addition technique.

5.5 Chemical interferences

Chemical interferences are not significant with the ICP-AES technique, but if observed,

...

SLOVENSKI STANDARD
kSIST-TS FprCEN/TS 17774:2021
01-december-2021
Organska in organsko-mineralna gnojila - Določevanje določenih elementov z
atomsko emisijsko spektrometrijo z induktivno sklopljeno plazmo (ICP/AES) po
ekstrakciji z vodo

Organic and organo-mineral fertilizers - Determination of the content of specific elements

by ICP-AES after extraction by water
Organische und organisch-mineralische Düngemittel - Bestimmung des Gehalts
spezifischer Elemente mittels ICP-AES nach Extraktion mit Wasser
Ta slovenski standard je istoveten z: FprCEN/TS 17774
ICS:
65.080 Gnojila Fertilizers
kSIST-TS FprCEN/TS 17774:2021 en,fr,de

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

---------------------- Page: 1 ----------------------
kSIST-TS FprCEN/TS 17774:2021
---------------------- Page: 2 ----------------------
kSIST-TS FprCEN/TS 17774:2021
FINAL DRAFT
TECHNICAL SPECIFICATION
FprCEN/TS 17774
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
November 2021
ICS 65.080
English Version
Organic and organo-mineral fertilizers - Determination of
the content of specific elements by ICP-AES after
extraction by water
Organische und organisch-mineralische Düngemittel -
Bestimmung des Gehalts spezifischer Elemente mittels
ICP-AES nach Extraktion mit Wasser

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 17774:2021 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
kSIST-TS FprCEN/TS 17774:2021
FprCEN/TS 17774:2021 (E)
Contents Page

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

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

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

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

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

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

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

5.1 General ................................................................................................................................................................ 6

5.2 Spectral interferences ................................................................................................................................... 6

5.3 Transport interferences ............................................................................................................................... 6

5.4 Excitation interferences ............................................................................................................................... 6

5.5 Chemical interferences ................................................................................................................................. 6

5.6 Memory interferences ................................................................................................................................... 6

6 Reagents ............................................................................................................................................................. 7

6.1 Water, grade 2 according to EN ISO 3696:1995 free from micronutrients. ............................... 7

6.2 Standard stock solutions, boron, cobalt, copper, iron, manganese, molybdenum and

zinc, mass concentration ρ = 1 000 mg/l for each element. ............................................................. 7

6.3 Standard solution, ρ = 100 mg/l of element. ......................................................................................... 7

6.4 Argon, purity 99,995 % or higher ............................................................................................................. 7

6.5 Nitric acid, substance concentration c(HNO3) ≈ 14,3 mol/l; ρ ≈ 1,4 g/ml. ................................. 7

7 Apparatus ........................................................................................................................................................... 7

7.1 Common laboratory glassware. ................................................................................................................. 7

7.2 Inductively coupled plasma atomic emission spectrometer. .......................................................... 7

8 Procedure........................................................................................................................................................... 8

8.1 Preparation of test and blank solution ................................................................................................... 8

8.2 Preparation of the calibration solutions ................................................................................................ 8

8.3 Measurement .................................................................................................................................................... 8

Table 1 — Example of instrument parameters (Radial instrument – Spectro Blue, Axial

instrument iCAP 6000)............................................................................................................................... 10

Table 2 — Recommended wavelengths.............................................................................................................. 10

9 Calculation and expression of the results ........................................................................................... 11

10 Test report ...................................................................................................................................................... 11

Bibliography ................................................................................................................................................................. 12

---------------------- Page: 4 ----------------------
kSIST-TS FprCEN/TS 17774:2021
FprCEN/TS 17774:2021 (E)
European foreword

This document (FprCEN/TS 17774:2021) 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 17774:2021
FprCEN/TS 17774:2021 (E)
Introduction

This document is part of a modular approach and concerns the analytical measurement step. “Modular”

means that a test standard concerns a specific step in assessing a property and not the whole chain of

measurements. Inductively coupled plasma atomic emission spectrometry (ICP-AES) is nowadays widely

used and a well-established method in many laboratories.
---------------------- Page: 6 ----------------------
kSIST-TS FprCEN/TS 17774:2021
FprCEN/TS 17774:2021 (E)
1 Scope

This document specifies a method for the determination of boron (B), cobalt (Co), copper (Cu), iron (Fe),

manganese (Mn), molybdenum (Mo) and zinc (Zn) in organic fertilizers and organo-mineral fertilizers

extracts using inductively coupled plasma-atomic emission spectrometry (ICP-AES).

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.

This method is applicable to water extracts prepared according to FprCEN/TS 17766. The method can be

used for the determination of other elements, provided the user has verified the applicability.

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 17766, Organic and organo-mineral fertilizers — Extraction by water for subsequent

determination of elements

EN 12944-1, Fertilizers and liming materials and soil improvers - Vocabulary - Part 1: General terms

EN 12944-2, Fertilizers and liming materials and soil improvers - Vocabulary - Part 2: Terms relating to

fertilizers

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 terms and definitions given in EN 12944-1 and EN 12944-2 apply.

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 method is based on the ICP-AES measurement of the concentration of boron (B), cobalt (Co), copper

(Cu), iron (Fe), manganese (Mn), molybdenum (Mo) and zinc (Zn) in fertilizer extracts prepared

according to FprCEN/TS 17766. The elements are determined after appropriate dilution of the extract.

The solution is dispersed by a nebulizer of the ICP-AES instrument and the resulting aerosol is

transported into the plasma. Element specific emission spectra are produced by a radio-frequency

inductively coupled argon plasma where atoms or ions are excited at high temperature. The emission

spectra are dispersed by a spectrometer, and the intensities of the emission lines are monitored by

photosensitive devices. Multi-element determinations using sequential or simultaneous optical systems

and axial or radial viewing of the plasma may be used.

The method may be used for the determination of other elements, provided the user has verified the

applicability.
---------------------- Page: 7 ----------------------
kSIST-TS FprCEN/TS 17774:2021
FprCEN/TS 17774:2021 (E)
5 Interferences
5.1 General

Interferences and matrix effects shall be recognized and appropriate measures to minimize them shall be

made. There are several types of interferences – see 5.2 to 5.6.
5.2 Spectral interferences

Spectral interferences are due to incomplete isolation of the radiation emitted by the analyte from other

detected radiation sources. Spectral interferences are caused by background emission from continuous

or recombination phenomena, by stray light which causes background increase or overlap of a spectral

line from another element, or unresolved overlap of molecular band spectra. Background emission and

stray light can usually be compensated for by subtracting the background emission measured adjacent to

the analyte wavelength peak. To correct a sloping background shift two background correction points on

each side of the peak are used. Increase of background is more intensive with axial-view instruments.

Background correction is not required in cases of line broadening where a background correction

measurement would actually degrade the analytical result. A spectral line overlap usually leads to the

choice of an alternative line. If this is not possible, mathematical correction procedures (e.g. inter-element

correction technique, multi-component spectral fitting) can be used to compensate for the interference.

These correction procedures are usually a part of the instrument software.
5.3 Transport interferences

Transport interferences are caused by differences in the properties between the sample solutions and

the calibration solutions (viscosity, surface tension, density, dissolved solid content, type and

concentration of acids). As a consequence, the supply of solution to the nebuliser, the efficiency of

nebulisation and the droplet size distribution of the aerosol is altered, resulting in a change of sensitivity.

Errors due to these interferences can be overcome by dilution of the solutions, by matrix matching, by

standard addition or by internal standard.
5.4 Excitation interferences

Excitation interferences are attributed to a change in the excitation conditions in the plasma, especially

by the presence of easily ionisable elements. The interference depends on the operating conditions of the

plasma (e.g. power, sample introduction, gas flowrate or observation height) and differ from element to

element. Improvement of the plasma conditions can therefore reduce excitation interferences. Other

possibilities are dilution of the solutions, matrix matching or the standard addition technique.

5.5 Chemical interferences
...

Questions, Comments and Discussion

Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.