SIST-TS CEN/TS 15959:2010
(Main)Fertilizers - Determination of extracted phosphorus (Method 3.2)
Fertilizers - Determination of extracted phosphorus (Method 3.2)
This document specifies a method for the determination of phosphorus in fertilizer extracts. The method is applicable to all extracts of fertilizers for the determination of the different forms of phosphorus as phosphorus soluble in mineral acids, water soluble phosphorus, phosphorus soluble in solutions of ammonium citrate, phosphorus soluble in 2 % citric acid and phosphorus soluble in 2 % formic acid.
Düngemittel - Bestimmung von Phosphor in den Extrakten
Das vorliegende Dokument legt ein Verfahren zur Bestimmung von Phosphor in Düngemittelextrakten fest.
Das Verfahren ist auf alle Düngemittelextrakte anwendbar, die zur Bestimmung von Phosphor in seinen
verschiedenen Formen dienen, wie z. B. in Mineralsäuren löslicher Phosphor, wasserlöslicher Phosphor,
Phosphor löslich in Ammoniumcitratlösungen verschiedener Konzentration, löslich in 2%iger Citronensäure
und löslich in 2%iger Ameisensäure.
Engrais - Dosage du phosphore extrait
Le présent document spécifie une méthode de dosage du phosphore dans des extraits d’engrais.
La méthode est applicable à tous les extraits d'engrais pour le dosage des différentes formes de phosphore
telles que le phosphore soluble dans les acides minéraux, dans l’eau, dans des solutions de citrate
d’ammonium, dans l’acide citrique à 2 % et le phosphore soluble dans l’acide formique à 2 %.
Gnojila - Določevanje ekstrahiranega fosforja (metoda 3.2)
Ta tehnična specifikacija opredeljuje metodo določanja fosforja v ekstraktih gnojilih. Ta metoda velja za vse ekstrakte gnojil za določanje različnih oblik fosforja kot topnega v mineralnih kislinah, v vodi topnega fosforja, fosforja, topnega v raztopini amonijevega citrata, fosforja, topnega v 2 % citronski kislini, in fosforja, topnega v 2 % mravljični kislini.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST-TS CEN/TS 15959:2010
01-februar-2010
*QRMLOD'RORþHYDQMHHNVWUDKLUDQHJDIRVIRUMD PHWRGD
Fertilizers - Determination of extracted phosphorus (Method 3.2)
Düngemittel - Bestimmung von Phosphor in den Extrakten
Engrais - Dosage du phosphore extrait
Ta slovenski standard je istoveten z: CEN/TS 15959:2009
ICS:
65.080 Gnojila Fertilizers
SIST-TS CEN/TS 15959:2010 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST-TS CEN/TS 15959:2010
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SIST-TS CEN/TS 15959:2010
TECHNICAL SPECIFICATION
CEN/TS 15959
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
December 2009
ICS 65.080
English Version
Fertilizers - Determination of extracted phosphorus
Engrais - Dosage du phosphore extrait Düngemittel - Bestimmung von Phosphor in den Extrakten
This Technical Specification (CEN/TS) was approved by CEN on 19 October 2009 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, 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
© 2009 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 15959:2009: E
worldwide for CEN national Members.
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SIST-TS CEN/TS 15959:2010
CEN/TS 15959:2009 (E)
Contents Page
Foreword .3
1 Scope .4
2 Normative references .4
3 Terms and definitions .4
4 Principle .4
5 Sampling and sample preparation .4
6 Reagents .5
7 Apparatus .5
8 Procedure .6
9 Calculation and expression of the result .7
10 Precision .8
11 Test report .9
Annex A (informative) Statistical results of the inter-laboratory test . 10
Bibliography . 12
2
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SIST-TS CEN/TS 15959:2010
CEN/TS 15959:2009 (E)
Foreword
This document (CEN/TS 15959:2009) 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, 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 15959:2010
CEN/TS 15959:2009 (E)
1 Scope
This Technical Specification specifies a method for the determination of phosphorus in fertilizer extracts.
The method is applicable to all extracts of fertilizers for the determination of the different forms of phosphorus
as phosphorus soluble in mineral acids, water soluble phosphorus, phosphorus soluble in solutions of
ammonium citrate, phosphorus soluble in 2 % citric acid and phosphorus soluble in 2 % formic acid.
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
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
After possible hydrolysis, phosphorus is precipitated in an acid media in the form of quinoline
phosphomolybdate.
After filtering and washing, the precipitate is dried at 250 °C and weighed.
In the above mentioned conditions no interfering action is exerted by the compounds likely to be found in the
solution (mineral and organic acids, ammonium ions, soluble silicates, etc.) if a reagent based on sodium
molybdate or ammonium molybdate is used in the precipitation.
5 Sampling and sample preparation
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.
4
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SIST-TS CEN/TS 15959:2010
CEN/TS 15959:2009 (E)
6 Reagents
6.1 Water, distilled or demineralized.
6.2 Concentrated nitric acid, ρ = 1,40 g/ml.
6.3 Preparation of reagents
6.3.1 Preparation of the reagent based on sodium molybdate
Solution A: Dissolve 70 g of sodium molybdate dihydrate in 100 ml of distilled water.
Solution B: Dissolve 60 g of citric acid monohydrate in 100 ml of distilled water and add 85 ml concentrated
nitric acid (6.2).
Solution C: Stir solution A into solution B to obtain solution C.
Solution D: To 50 ml of distilled water, add 35 ml of concentrated nitric acid (6.2), then 5 ml of freshly distilled
quinoline. Add this solution to solution C, mix thoroughly and leave standing overnight in the dark. After this
make up to 500 ml with distilled water, mix again, and filter through a sintered glass funnel (7.7).
6.3.2 Preparation of the reagent based on ammonium molybdate
Solution A: In 300 ml of distilled water, dissolve 100 g of ammonium molybdate while heating gently and
stirring from time to time.
Solution B: Dissolve 120 g of citric acid monohydrate in 200 ml of distilled water, add 170 ml of concentrated
nitric acid (6.2).
Solution C: Add 10 ml of freshly distilled quinoline to 70 ml of concentrated nitric acid (6.2).
Solution D: Slowly pour, stirring well, solution A into solution B. After thoroughly mixing add solution C to this
mixture and make up to 1 l. Leave standing for two days in a dark place and filter through a sintered glass
funnel (7.7).
The reagents 6.3.1 and 6.3.2 may be used in the same way; both shall be kept in the dark in stoppered
polyethylene bottles.
7 Apparatus
7.1 Standard laboratory equipment.
7.2 500 ml Erlenmeyer flask, with a wide neck.
7.3 Graduated pipettes, of 10 ml, 25 ml and 50 ml.
7.4 Filter crucible, with porosity of 5 µm to 20 µm.
7.5 Buchner flask.
7.6 Drying oven, regulated at (250 ± 10) °C.
7.7 Sintered glass funnel, with porosity of 5 µm to 20 µm.
5
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SIST-TS CEN/TS 15959:2010
CEN/TS 15959:2009 (E)
8 Procedure
8.1 Treatment of the solution
With a pipette (7.3), take an aliquot part of fertilizer extract (see Table 1) containing about 0,01 g of P O and
2 5
place it in the Erlenmeyer flask (7.2). Add 15 ml of concentrated nitric acid (6.2) and dilute with water to about
100 ml. When the solution to be precipitated contains more than 15 ml of citrate solution (neutral citrate,
Petermann or Joulie alkaline
...
SLOVENSKI STANDARD
kSIST-TS FprCEN/TS 15959:2009
01-julij-2009
*QRMLOD'RORþHYDQMHHNVWUDKLUDQHJDIRVIRUMD PHWRGD
Fertilizers - Determination of extracted phosphorus (Method 3.2)
Düngemittel - Bestimmung von Phosphor in den Extrakten
Engrais - Dosage du phosphore extrait
Ta slovenski standard je istoveten z: FprCEN/TS 15959
ICS:
65.080 Gnojila Fertilizers
kSIST-TS FprCEN/TS 15959:2009 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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kSIST-TS FprCEN/TS 15959:2009
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kSIST-TS FprCEN/TS 15959:2009
TECHNICAL SPECIFICATION
FINAL DRAFT
FprCEN/TS 15959
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
June 2009
ICS 65.080
English Version
Fertilizers - Determination of extracted phosphorus (Method 3.2)
Engrais - Dosage du phosphore extrait Düngemittel - Bestimmung von Phosphor in den Extrakten
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, 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
© 2009 CEN All rights of exploitation in any form and by any means reserved Ref. No. FprCEN/TS 15959:2009: E
worldwide for CEN national Members.
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kSIST-TS FprCEN/TS 15959:2009
FprCEN/TS 15959:2009 (E)
Contents Page
Foreword .3
1 Scope .4
2 Normative references .4
3 Terms and definitions .4
4 Principle .4
5 Sampling and sample preparation .4
6 Reagents .5
7 Apparatus .6
8 Procedure .6
9 Calculation and expression of the result .7
10 Precision .8
11 Test report .9
Annex A (informative) Statistical results of the inter-laboratory test . 10
Bibliography . 12
2
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kSIST-TS FprCEN/TS 15959:2009
FprCEN/TS 15959:2009 (E)
Foreword
This document (FprCEN/TS 15959:2009) 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
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kSIST-TS FprCEN/TS 15959:2009
FprCEN/TS 15959:2009 (E)
1 Scope
This document specifies a method for the determination of phosphorus in fertilizer extracts.
The method is applicable to all extracts of fertilizers for the determination of the different forms of phosphorus
as phosphorus soluble in mineral acids, water soluble phosphorus, phosphorus soluble in solutions of
ammonium citrate, phosphorus soluble in 2 % citric acid and phosphorus soluble in 2 % formic acid.
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
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
After possible hydrolysis, phosphorus is precipitated in an acid media in the form of quinoline
phosphomolybdate.
After filtering and washing, the precipitate is dried at 250 °C and weighed.
In the above mentioned conditions no interfering action is exerted by the compounds likely to be found in the
solution (mineral and organic acids, ammonium ions, soluble silicates, etc.) if a reagent based on sodium
molybdate or ammonium molybdate is used in the precipitation.
5 Sampling and sample preparation
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.
4
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kSIST-TS FprCEN/TS 15959:2009
FprCEN/TS 15959:2009 (E)
6 Reagents
6.1 Water, distilled or demineralized.
6.2 Concentrated nitric acid, ρ = 1,40 g/ml.
6.3 Preparation of reagents
6.3.1 Preparation of the reagent based on sodium molybdate
Solution A: Dissolve 70 g of sodium molybdate dihydrate in 100 ml of distilled water.
Solution B: Dissolve 60 g of citric acid monohydrate in 100 ml of distilled water and add 85 ml concentrated
nitric acid (6.2).
Solution C: Stir solution A into solution B to obtain solution C.
Solution D: To 50 ml of distilled water, add 35 ml of concentrated nitric acid (6.2), then 5 ml of freshly distilled
quinoline. Add this solution to solution C, mix thoroughly and leave standing overnight in the dark. After this
make up to 500 ml with distilled water, mix again, and filter through a sintered glass funnel (7.7).
6.3.2 Preparation of the reagent based on ammonium molybdate
Solution A: In 300 ml of distilled water, dissolve 100 g of ammonium molybdate while heating gently and
stirring from time to time.
Solution B: Dissolve 120 g of citric acid monohydrate in 200 ml of distilled water, add 170 ml of concentrated
nitric acid (6.2).
Solution C: Add 10 ml of freshly distilled quinoline to 70 ml of concentrated nitric acid (6.2).
Solution D: Slowly pour, stirring well, solution A into solution B. After thoroughly mixing add solution C to this
mixture and make up to 1 l. Leave standing for two days in a dark place and filter through a sintered glass
funnel (7.7).
The reagents 6.3.1 and 6.3.2 may be used in the same way; both shall be kept in the dark in stoppered
polyethylene bottles.
5
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kSIST-TS FprCEN/TS 15959:2009
FprCEN/TS 15959:2009 (E)
7 Apparatus
7.1 Standard laboratory equipment.
7.2 500 ml Erlenmeyer flask, with a wide neck.
7.3 Graduated pipettes, of 10 ml, 25 ml and 50 ml.
7.4 Filter crucible, with porosity of 5 µm to 20 µm.
7.5 Buchner flask.
7.6 Drying oven, regulated at (250 ± 10) °C.
7.7 Sintered glass funnel, with porosity of 5 µm to 20 µm.
8 Procedure
8.1 Treatment of the solution
With a pipette (7.3), take an aliquot part of fertilizer extract (see Table 1) containing about 0,01 g of P O and
2 5
1
place it in the Erlenmeyer flask (7.2). Add 15 ml of concentrated nitric acid (6.2) and dilute with water to about
100 ml.
Table 1 — Determination of the aliquot parts of the phosphate solutions
Quinoline Quinoline
Sample Sample
phospho- phospho-
% P O % P
2 5
for Dilution Sample Dilution to be
molybdate molybdate
in the in the
analysis precipitated
conversion conversion
to ml ml to ml
fertilizer fertilizer
factor (F), factor (F’),
g ml
in % P O in % P
2 5
2,2 to 4,4
1 500 - - 50 32,074 13,984
5 to 10
5 500 - - 10 32,074 13,984
{
4,4 to
1 500 - - 25 64,148 27,968
10 to 25
5 500 50 500 50 64,148 27,968
11,0 {
1 500 - - 10 160,370 69,921
> 25
> 11 {
5
...
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