Fertilizers - Manganimetric determination of extracted calcium following precipitation in the form of oxalate

This Technical Specification specifies a manganimetric method for the determination of the calcium content in fertilizer extracts.
This method is applicable to EC fertilizers for which a declaration of the total and/or water-soluble calcium content is provided for in Regulation (EC) 2003/2003, Annex I [1].

Düngemittel - Manganometrische Bestimmung von Calcium nach Oxalatfällung

Diese Technische Spezifikation legt ein Verfahren zur Bestimmung des Calciumgehalts in Dünge-mittelextrakten fest.
Dieses Verfahren gilt für EG-Düngemittel, für die die Verordnung (EG) Nr. 2003/2003, Anhang I [1] die Angabe des gesamten und/oder des wasserlöslichen Calciumgehalts vorschreibt.

Engrais - Dosage manganimétrique du calcium extrait après précipitation sous forme d'oxalate

La présente Spécification technique spécifie une méthode de dosage manganimétrique du calcium dans des solutions d’extraction d’engrais.
Cette méthode est applicable aux engrais CE pour lesquels une déclaration de la teneur en calcium total et/ou hydrosoluble est prévue dans le Règlement (CE) n° 2003/2003, Annexe I [1].

Gnojila - Manganometrijsko določevanje ekstrahiranega kalcija po obarjanju v obliki oksalata

Ta tehnična specifikacija opredeljuje manganometrijsko metodo določevanja vsebnosti kalcija v ekstraktih gnojilih. Ta metoda se uporablja za gnojila ES, za katera je zagotovljena deklaracija o celotni vsebnosti kalcija in/ali vsebnosti v vodi topnega kalcija v Uredbi (ES) št. 2003/2003, Priloga I [3].

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Withdrawn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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Standards Content (Sample)

SLOVENSKI STANDARD
SIST-TS CEN/TS 16196:2011
01-oktober-2011
*QRMLOD0DQJDQRPHWULMVNRGRORþHYDQMHHNVWUDKLUDQHJDNDOFLMDSRREDUMDQMXY
REOLNLRNVDODWD
Fertilizers - Manganimetric determination of extracted calcium following precipitation in
the form of oxalate
Düngemittel - Manganometrische Bestimmung von Calcium nach Oxalatfällung
Engrais - Dosage manganimétrique du calcium extrait après précipitation sous forme
d'oxalate
Ta slovenski standard je istoveten z: CEN/TS 16196:2011
ICS:
65.080 Gnojila Fertilizers
SIST-TS CEN/TS 16196:2011 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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

SIST-TS CEN/TS 16196:2011

---------------------- Page: 2 ----------------------

SIST-TS CEN/TS 16196:2011


TECHNICAL SPECIFICATION
CEN/TS 16196

SPÉCIFICATION TECHNIQUE

TECHNISCHE SPEZIFIKATION
June 2011
ICS 65.080
English Version
Fertilizers - Manganimetric determination of extracted calcium
following precipitation in the form of oxalate
Engrais - Dosage manganimétrique du calcium extrait Düngemittel - Manganometrische Bestimmung von Calcium
après précipitation sous forme d'oxalate nach Oxalatfällung
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 16196:2011: E
worldwide for CEN national Members.

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

SIST-TS CEN/TS 16196:2011
CEN/TS 16196:2011 (E)
Contents Page
Foreword .3
1 Scope .4
2 Normative references .4
3 Terms and definitions .4
4 Sampling .4
5 Principle .4
6 Reagents .4
7 Apparatus .5
8 Preparation of the test portion .5
9 Procedure .5
9.1 Preparation of the calcium oxalate .5
9.2 Titration of the oxalate precipitate .5
10 Calculation and expression of the result .6
11 Precision .6
11.1 Inter-laboratory test .6
11.2 Repeatability .6
11.3 Reproducibility .6
12 Test report .7
Annex A (informative) Statistical results of the inter-laboratory tests .8
Bibliography . 10

2

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SIST-TS CEN/TS 16196:2011
CEN/TS 16196:2011 (E)
Foreword
This document (CEN/TS 16196:2011) 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

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

SIST-TS CEN/TS 16196:2011
CEN/TS 16196:2011 (E)
1 Scope
This Technical Specification specifies a manganimetric method for the determination of the calcium content in
fertilizer extracts.
This method is applicable to EC fertilizers for which a declaration of the total and/or water-soluble calcium
content is provided for in Regulation (EC) 2003/2003, Annex I [3].
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 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.
5 Principle
Precipitation of the calcium contained in an aliquot of the extraction solution in the form of an oxalate, which is
determined by titration using potassium permanganate.
6 Reagents
6.1 Diluted hydrochloric acid, one volume of hydrochloric acid, ρ = 1,18g/ml, and one volume of water.
4

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

SIST-TS CEN/TS
...

SLOVENSKI STANDARD
kSIST-TS FprCEN/TS 16196:2011
01-januar-2011
*QRMLOD0DQJDQRPHWULMVNRGRORþHYDQMHHNVWUDKLUDQHJDNDOFLMDSRREDUMDQMXY
REOLNLRNVDODWD
Fertilizers - Manganimetric determination of extracted calcium following precipitation in
the form of oxalate
Düngemittel - Manganometrische Bestimmung von Calcium nach Oxalatfällung
Engrais - Dosage manganimétrique du calcium extrait après précipitation sous forme
d'oxalate
Ta slovenski standard je istoveten z: FprCEN/TS 16196
ICS:
65.080 Gnojila Fertilizers
kSIST-TS FprCEN/TS 16196:2011 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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

kSIST-TS FprCEN/TS 16196:2011

---------------------- Page: 2 ----------------------

kSIST-TS FprCEN/TS 16196:2011


TECHNICAL SPECIFICATION
FINAL DRAFT
FprCEN/TS 16196
SPÉCIFICATION TECHNIQUE

TECHNISCHE SPEZIFIKATION

November 2010
ICS
English Version
Fertilizers - Manganimetric determination of extracted calcium
following precipitation in the form of oxalate
Engrais - Dosage manganimétrique du calcium extrait Düngemittel - Manganometrische Bestimmung von Calcium
après précipitation sous forme d'oxalate nach Oxalatfällung


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 16196:2010: E
worldwide for CEN national Members.

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

kSIST-TS FprCEN/TS 16196:2011
FprCEN/TS 16196:2010 (E)
Contents Page
Foreword .3
1 Scope .4
2 Normative references .4
3 Terms and definitions .4
4 Sampling .4
5 Principle .4
6 Reagents .5
7 Apparatus .5
8 Preparation of the test portion .5
9 Procedure .5
10 Calculation and expression of the result .6
11 Precision .6
12 Test report .7
Annex A (informative) Statistical results of the inter-laboratory tests .8
Bibliography . 10

2

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

kSIST-TS FprCEN/TS 16196:2011
FprCEN/TS 16196:2010 (E)
Foreword
This document (FprCEN/TS 16196:2010) 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 16196:2011
FprCEN/TS 16196:2010 (E)
1 Scope
This Technical Specification specifies a manganimetric method for the determination of the calcium content in
fertilizer extracts.
This method is applicable to EC fertilizers for which a declaration of the total and/or water-soluble calcium
content is provided for in Regulation (EC) 2003/2003, Annex I [1].
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 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.
5 Principle
Precipitation of the calcium contained in an aliquot of the extraction solution in the form of an oxalate, which is
determined by titration using potassium permanganate.
4

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

kSIST-TS FprCEN/TS 16196:2011
FprCEN/TS 16196:2010 (E)
6 Reagents
6.1 Diluted hydrochloric acid, one volume of hydrochloric acid, ρ = 1,18g/ml, and one volume of water.
6.2 Sulfuric acid, 1:10 diluted, one volume of sulfuric acid, ρ = 1,84 g/ml, in ten volumes of water.
6.3 Ammonia solution, 1:1 diluted, one volume of ammonia, ρ = 0,88 g/ml, and one volume of water.
6.4 Ammonia oxalate, [(NH ) C O H O], saturated solution at ambient temperature, approximately
4 2 2 4 2
ρ = 40 g/l.
6.5 Citric acid solution, 30 % (mass concentration).
6.6 Ammonium chloride solution, 5 % (mass concentration).
6.7 Solution of bromothymol blue in ethanol, at 95 %, 0,1 % (mass concentration).
6.8 Solution of bromocresol green in ethanol, at 95 %, 0,04 % (mass concentration).
6.9 Standard solution of potassium permanganate, c = 0,02 mol/l.
7 Apparatus
7.1 Filter crucible, with 5 µm to 20 µm porosity sintered glass.
7.2 Hot water bath.
7.3 400 ml beaker.
8 Preparation of the test portion
Using a pipette, ta
...

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