Fertilizers - Determination of magnesium by atomic absorption spectrometry

This Technical Specification specifies a method for the determination of the magnesium content in fertilizer extracts using atomic absorption spectrometry (AAS).
This method is applicable to EC fertilizer extracts obtained according to CEN/TS 15960 and CEN/TS 15961, for which a declaration of the total magnesium and/or water soluble magnesium content is required, with the exceptions of the following fertilizers according to [1] Annex I D relating to secondary nutrients:
-   type 4 (kieserite);
-   type 5 (magnesium sulfate) and type 5.1 (magnesium sulfate solution);
-   type 7 (kieserite with potassium sulfate)
to which [1], method 8.8, applies.
NOTE   Method 8.8 is covered by prCEN/TS 16198 (see Bibliography).
The method applies to all fertilizer extracts containing elements in quantities that might interfere with the complexometric determination of magnesium.

Düngemittel - Bestimmung von Magnesium mit Atomabsorptionsspektrometrie

Diese Technische Spezifikation legt ein Verfahren zur Bestimmung des Magnesiumgehalts in Düngemittelextrakten mit Atomabsorptionsspektrometrie (AAS) fest.
Dieses Verfahren gilt für nach CEN/TS 15960 und CEN/TS 15961 hergestellte EG-Düngemittelextrakte, für die die Angabe des Gesamtmagnesiums und/oder des wasserlöslichen Magnesiumgehalts vorgeschrieben ist, mit Ausnahme der folgenden Düngemittel nach Anhang I D [1], der sich auf mineralische Sekundär-nährstoffdünger bezieht:
-   Typ 4 (Kieserit);
-   Typ 5 (Magnesiumsulfat) und Typ 5.1 (Magnesiumsulfatlösung);
-   Typ 7 (Kieserit mit Kaliumsulfat).
Für diese Düngemittel gilt [1], Methode 8.8.
ANMERKUNG   Methode 8.8 ist durch prCEN/TS 16198 (siehe Literaturhinweise) abgedeckt.
Das Verfahren gilt für alle Düngemittelextrakte, die Elemente in einer Menge enthalten, die eine komplexometrische Bestimmung von Magnesium stören könnten.

Engrais - Dosage du magnésium par spectrométrie d'absorption atomique

La présente Spécification technique spécifie une méthode de dosage du magnésium dans des extraits
d'échantillons d’engrais par spectrométrie d’absorption atomique (SAA).
Cette méthode est applicable aux extraits d'échantillons d’engrais CE obtenus conformément à la
CEN/TS 15960 et à la CEN/TS 15961, pour lesquels une déclaration de la teneur en magnésium total et/ou
hydrosoluble est requise, à l’exception des engrais suivants, selon l’Annexe I D de la référence
bibliographique [4] relative aux éléments nutritifs secondaires :
- type 4 (kiésérite) ;
- type 5 (sulfate de magnésium) et type 5.1 (solution de sulfate de magnésium) ;
- type 7 (kiésérite avec sulfate de potassium)
pour lesquels la méthode 8.8 de la référence bibliographique [4] s’applique.
NOTE La méthode 8.8 est abordée par la prCEN/TS 16198 (voir la Bibliographie).
La méthode s’applique à tous les extraits d'échantillons d’engrais contenant des éléments dans des quantités
susceptibles d’interférer avec le dosage complexométrique du magnésium.

Gnojila - Določevanje magnezija z atomsko absorpcijsko spektrometrijo

Ta tehnična specifikacija opredeljuje metodo določevanja vsebnosti magnezija v ekstraktih gnojil z uporabo atomske absorpcijske spektrometrije (AAS). Ta metoda velja za ekstrakte gnojil ES, pridobljene v skladu s CEN/TS 15960 in CEN/TS 15961, za katere je potrebna deklaracija o celotni vsebnosti magnezija in/ali vsebnosti v vodi topnega magnezija, razen naslednjih gnojil v skladu z dodatkom I D, ki se nanaša na sekundarna hranila: tip 4 (kiezerit); tip 5 (magnezijev sulfat) in tip 5.1 (raztopina magnezijevega sulfata); tip 7 (kiezerit s kalijevim sulfatom), za katerega se uporablja metoda 8.8.

General Information

Status
Withdrawn
Public Enquiry End Date
31-Jan-2011
Publication Date
14-Sep-2011
Withdrawal Date
21-Apr-2013
Technical Committee
Current Stage
9900 - Withdrawal (Adopted Project)
Start Date
04-Apr-2013
Due Date
27-Apr-2013
Completion Date
22-Apr-2013

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SLOVENSKI STANDARD
SIST-TS CEN/TS 16197:2011
01-oktober-2011
*QRMLOD'RORþHYDQMHPDJQH]LMD]DWRPVNRDEVRUSFLMVNRVSHNWURPHWULMR
Fertilizers - Determination of magnesium by atomic absorption spectrometry
Düngemittel - Bestimmung von Magnesium mit Atomabsorptionsspektrometrie
Engrais - Dosage du magnésium par spectrométrie d'absorption atomique
Ta slovenski standard je istoveten z: CEN/TS 16197:2011
ICS:
65.080 Gnojila Fertilizers
SIST-TS CEN/TS 16197:2011 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------

SIST-TS CEN/TS 16197:2011

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SIST-TS CEN/TS 16197:2011


TECHNICAL SPECIFICATION
CEN/TS 16197

SPÉCIFICATION TECHNIQUE

TECHNISCHE SPEZIFIKATION
June 2011
ICS 65.080
English Version
Fertilizers - Determination of magnesium by atomic absorption
spectrometry
Engrais - Dosage du magnésium par spectrométrie Düngemittel - Bestimmung von Magnesium mit
d'absorption atomique Atomabsorptionsspektrometrie
This Technical Specification (CEN/TS) was approved by CEN on 5 March 2011 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, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.





EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2011 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 16197:2011: E
worldwide for CEN national Members.

---------------------- Page: 3 ----------------------

SIST-TS CEN/TS 16197:2011
CEN/TS 16197:2011 (E)
Contents Page
Foreword .3
1 Scope .4
2 Normative references .4
3 Terms and definitions .4
4 Principle .4
5 Sampling .5
6 Reagents .5
7 Apparatus .5
8 Preparation of the extraction solution .5
9 Procedure .6
9.1 Preparation of the test solution .6
9.2 Preparation of the blank solution .6
9.3 Preparation of the calibration solutions .6
9.4 Measurement .6
10 Calculation and expression of the result .6
11 Precision .7
11.1 Inter-laboratory test .7
11.2 Repeatability .7
11.3 Reproducibility .7
12 Test report .8
Annex A (informative) Statistical results of the inter-laboratory test .9
Bibliography . 11

2

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SIST-TS CEN/TS 16197:2011
CEN/TS 16197:2011 (E)
Foreword
This document (CEN/TS 16197:2011) 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 [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.
This document has been prepared under a mandate given to CEN by the European Commission and the
European Free Trade Association.
According to the CEN/CENELEC Internal Regulations, the national standards organizations 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, Romania, Slovakia, Slovenia,
Spain, Sweden, Switzerland and the United Kingdom.
3

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SIST-TS CEN/TS 16197:2011
CEN/TS 16197:2011 (E)
1 Scope
This Technical Specification specifies a method for the determination of the magnesium content in fertilizer
extracts using atomic absorption spectrometry (AAS).
This method is applicable to EC fertilizer extracts obtained according to CEN/TS 15960 and CEN/TS 15961,
for which a declaration of the total magnesium and/or water soluble magnesium content is required, with the
exceptions of the following fertilizers according to [4], Annex I D relating to secondary nutrients:
 type 4 (kieserite);
 type 5 (magnesium sulfate) and type 5.1 (magnesium sulfate solution);
 type 7 (kieserite with potassium sulfate)
to which [4], method 8.8, applies.
NOTE Method 8.8 is covered by CEN/TS 16198 (see Bibliography).
The method applies to all fertilizer extracts containing elements in quantities that might interfere with the
complexometric determination of magnesium.
2 Normative references
The following referenced documents are indispensable for the application 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.
EN 1482-2, Fertilizers and liming materials — Sampling and sample preparation — Part 2: Sample
preparation
EN 12944-1:1999, Fertilizers and liming materials and soil improvers — Vocabulary — Part 1: General terms
EN 12944-2:1999, Fertilizers and liming materials and soil improvers — Vocabulary — Part 2: Terms relating
to fertilizers
CEN/TS 15960, Fertilizers — Extraction of total calcium, total magnesium, total sodium and total sulfur in the
forms of sulfates
CEN/TS 15961, Fertilizers — Extraction of water soluble calcium, magnesium, sodium and sulfur in the form
of sulfates
3 Terms and definitions
For the purposes of this document, the terms and definitions given in EN 12944-1:1999 and EN 12944-2:1999
apply.
4 Principle
Determination of magnesium by atomic absorption spectrometry (AAS) after appropriate dilution of the extract.
4

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SIST-TS CEN/TS 16197:2011
CEN/TS 16197:2011 (E)
5 Sampling
Sampling is not part of the method specified in this document. A recommended sampling method is given in
EN 1482-1.
Sample preparation shall be carried out in accordance with EN 1482-2. Grinding of the laboratory sample is
recommended for homogeneity reasons.
6 Reagents
6.1 Hydrochloric acid solution, c = 1 mol/l.
6.2 Hydrochloric acid solution, c = 0,5 mol/l.
6.3 Standard solution of magnesium, ρ = 1,00 mg/ml.
6.3.1 Preferably use a commercially available certified stock solution of magnesium.
6.3.2 Dissolve 1,013 g of magnesium sulfate (MgSO , 7H O) in hydrochloric acid solution (6.2), transfer
4 2
quantitatively into a graduated flask (7.3) and make up the volume with the same acid and mix.
6.3.3 Weigh 1,658 g of m
...

SLOVENSKI STANDARD
kSIST-TS FprCEN/TS 16197:2011
01-januar-2011
*QRMLOD'RORþHYDQMHPDJQH]LMD]DWRPVNRDEVRUSFLMVNRVSHNWURPHWULMR
Fertilizers - Determination of magnesium by atomic absorption spectrometry
Düngemittel - Bestimmung von Magnesium mit Atomabsorptionsspektrometrie
Engrais - Dosage du magnésium par spectrométrie d'absorption atomique
Ta slovenski standard je istoveten z: FprCEN/TS 16197
ICS:
65.080 Gnojila Fertilizers
kSIST-TS FprCEN/TS 16197:2011 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------

kSIST-TS FprCEN/TS 16197:2011

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kSIST-TS FprCEN/TS 16197:2011


TECHNICAL SPECIFICATION
FINAL DRAFT
FprCEN/TS 16197
SPÉCIFICATION TECHNIQUE

TECHNISCHE SPEZIFIKATION

November 2010
ICS
English Version
Fertilizers - Determination of magnesium by atomic absorption
spectrometry
Engrais - Dosage du magnésium par spectrométrie Düngemittel - Bestimmung von Magnesium mit
d'absorption atomique Atomabsorptionsspektrometrie


This draft Technical Specification is submitted to CEN members for formal 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, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.



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

Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2010 CEN All rights of exploitation in any form and by any means reserved Ref. No. FprCEN/TS 16197:2010: E
worldwide for CEN national Members.

---------------------- Page: 3 ----------------------

kSIST-TS FprCEN/TS 16197:2011
FprCEN/TS 16197:2010 (E)
Contents Page
Foreword .3
1 Scope .4
2 Normative references .4
3 Terms and definitions .4
4 Principle .4
5 Sampling .5
6 Reagents .5
7 Apparatus .5
8 Preparation of the extraction solution .5
9 Procedure .6
10 Calculation and expression of the result .6
11 Precision .7
12 Test report .8
Annex A (informative) Statistical results of the inter-laboratory test .9
Bibliography . 11

2

---------------------- Page: 4 ----------------------

kSIST-TS FprCEN/TS 16197:2011
FprCEN/TS 16197:2010 (E)
Foreword
This document (FprCEN/TS 16197:2010) 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 Formal Vote.
This document has been prepared under a mandate given to CEN by the European Commission and the
European Free Trade Association.
3

---------------------- Page: 5 ----------------------

kSIST-TS FprCEN/TS 16197:2011
FprCEN/TS 16197:2010 (E)
1 Scope
This Technical Specification specifies a method for the determination of the magnesium content in fertilizer
extracts using atomic absorption spectrometry (AAS).
This method is applicable to EC fertilizer extracts obtained according to CEN/TS 15960 and CEN/TS 15961,
for which a declaration of the total magnesium and/or water soluble magnesium content is required, with the
exceptions of the following fertilizers according to [1] Annex I D relating to secondary nutrients:
 type 4 (kieserite);
 type 5 (magnesium sulfate) and type 5.1 (magnesium sulfate solution);
 type 7 (kieserite with potassium sulfate)
to which [1], method 8.8, applies.
NOTE Method 8.8 is covered by prCEN/TS 16198 (see Bibliography).
The method applies to all fertilizer extracts containing elements in quantities that might interfere with the
complexometric determination of magnesium.
2 Normative references
The following referenced documents are indispensable for the application 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.
EN 1482-2, Fertilizers and liming materials — Sampling and sample preparation — Part 2: Sample
preparation
EN 12944-1:1999, Fertilizers and liming materials and soil improvers — Vocabulary — Part 1: General terms
EN 12944-2:1999, Fertilizers and liming materials and soil improvers — Vocabulary — Part 2: Terms relating
to fertilizers
CEN/TS 15960, Fertilizers — Extraction of total calcium, total magnesium, total sodium and total sulfur in the
forms of sulfates
CEN/TS 15961, Fertilizers — Extraction of water soluble calcium, magnesium, sodium and sulfur in the form
of sulfates
3 Terms and definitions
For the purposes of this document, the terms and definitions given in EN 12944-1:1999 and EN 12944-2:1999
apply.
4 Principle
Determination of magnesium by atomic absorption spectrometry (AAS) after appropriate dilution of the extract.
4

---------------------- Page: 6 ----------------------

kSIST-TS FprCEN/TS 16197:2011
FprCEN/TS 16197:2010 (E)
5 Sampling
Sampling is not part of the method specified in this document. A recommended sampling method is given in
EN 1482-1.
Sample preparation shall be carried out in accordance with EN 1482-2. Grinding of the laboratory sample is
recommended for homogeneity reasons.
6 Reagents
6.1 Hydrochloric acid solution, c = 1 mol/l.
6.2 Hydrochloric acid solution, c = 0,5 mol/l.
6.3 Standard solution of magnesium, ρ = 1,00 mg/ml.
6.3.1 Dissolve 1,013 g of magnesium sulfate (MgSO , 7H O) in hydrochloric acid solution (6.2).
4 2
6.3.2 Weigh 1,658 g of magnesium oxide (MgO), previously calcined to remove all traces of carbonation.
Place in a beaker with 100 ml of water and 120 ml of hydrochloric acid (6.1). When it has dissolved, decant
quantitatively into a graduated flask (7.5). Make up the volume by adding and mix, or take a commercial
standard solution.
The laboratory is responsible for testing such solutions.
6.4 Strontium chloride solution.
Dissolve 75 g of strontium chloride (SrCl 6H O) in a hydrochloric acid solution (6.2) and make up to 500 ml
2 2
with the same acid solution.
7 Apparatus
7.1 Spectrometer, fitted for atomic absorption, with a magnesium lamp, set at 285,2 nm.
7.2 Air-acetylene flame.
7.3 100 ml graduated flask.
7.4 200 ml graduated flask.
7.5 1 000 ml graduated flask.
8 Preparation of the extraction solution
The extraction solutions shall be prepared according to CEN/TS 15960 or CEN/TS 15961.
5

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kSIST-TS FprCEN/TS 16197:2011
FprCEN/TS 16197:2010 (E)
9 Procedure
9.1 Preparation of the test solution
9.1.1 If the fertilizer has a declared magnesium (Mg) content of mo
...

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