Fertilizers - Determination of N-(n-Butyl)thiophosphoric acid triamide (NBPT) and N-(n-Propyl)thiophosphoric acid triamide (NPPT) - Method using high-performance liquid chromatography (HPLC)

This document specifies a method for the quantitative determination of the urease inhibitors N-(n-Butyl)thiophosphoric acid triamide (NBPT, CAS-No. 94317-64-3) and N-(n-Propyl)thiophosphoric acid triamide (NPPT, CAS-No. 916809-14-8) content in urea based fertilizers using high-performance liquid chromatography (HPLC).

Düngemittel - Bestimmung von N-(n-Butyl)thiophosphorsäuretriamid (NBPT) und N-(n-Propyl)thiophosphorsäuretriamid (NPPT) - Verfahren mit Hochleistungs-Flüssigchromatographie (HPLC)

Diese Europäische Norm legt ein Verfahren zur quantitativen Bestimmung des Gehalts der Ureasehemmstoffe N (n Butyl)thiophosphorsäuretriamid (NBPT, CAS-Nr. 94317 64 3) und N-(n-Propyl)thiophosphorsäuretriamid (NPPT, CAS-Nr. 916809 14 8) in harnstoffbasierten Düngemitteln mit Hochleistungs-Flüssigchromatographie (HPLC) fest.

Engrais - Dosage du acide triamide (NBPT) et de N-(n-propyl) triamide de l'acide thiophosphorique (NPPT) - Méthode par chromatographie liquide à haute performance (HPLC)

La présente norme européenne spécifie une méthode de détermination quantitative de la teneur en inhibiteurs d'uréase N-(n-butyl)triamide de l'acide thiophosphorique (NBPT, N° CAS 94317-64-3) et N-(n-propyl)triamide de l'acide thiophosphorique (NPPT, N° CAS 916809-14-8) dans les engrais à base d'urée, par chromatographie liquide à haute performance (HPLC).

Gnojila - Določevanje N-(n-butil)-triamida tiofosforne kisline (NBPT) in N-(n-propil)-triamida tiofosforne kisline (NPPT) - Metoda tekočinske kromatografije visoke ločljivosti (HPLC)

Ta dokument določa metodo kvantitativnega določanja vsebnosti inhibitorjev sečnine N-(n-butil)-triamida tiofosforne kisline (NBPT, št. CAS 94317-64-3) in N-(n-propil)-triamida tiofosforne kisline (NPPT št. CAS 916809-14-8) v gnojilih, ki temeljijo na sečnini, z metodo tekočinske kromatografije visoke ločljivosti (HPLC).

General Information

Status
Published
Public Enquiry End Date
03-Aug-2014
Publication Date
09-Aug-2015
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
08-Jul-2015
Due Date
12-Sep-2015
Completion Date
10-Aug-2015

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Düngemittel - Bestimmung von N-(n-Butyl)thiophosphorsäuretriamid (NBPT) und N-(n-Propyl)thiophosphorsäuretriamid (NPPT) - Verfahren mit Hochleistungs-Flüssigchromatographie (HPLC)Engrais - Dosage du acide triamide (NBPT) et de N-(n-propyl) triamide de l'acide thiophosphorique (NPPT) - Méthode par chromatographie liquide à haute performance (HPLC)Fertilizers - Determination of N-(n-Butyl)thiophosphoric acid triamide (NBPT) and N-(n-Propyl)thiophosphoric acid triamide (NPPT) - Method using high-performance liquid chromatography (HPLC)65.080GnojilaFertilizersICS:Ta slovenski standard je istoveten z:EN 16651:2015SIST EN 16651:2015en,fr,de01-september-2015SIST EN 16651:2015SLOVENSKI
STANDARD



SIST EN 16651:2015



EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16651
May 2015 ICS 65.080 English Version
Fertilizers - Determination of N-(n-Butyl)thiophosphoric acid triamide (NBPT) and N-(n-Propyl)thiophosphoric acid triamide (NPPT) - Method using high-performance liquid chromatography (HPLC)
Engrais - Dosage du N-(n-butyl)triamide de l'acide thiophosphorique (NBPT) et du N-(n-propyl)triamide de l'acide thiophosphorique (NPPT) - Méthode par chromatographie liquide à haute performance (HPLC)
Düngemittel - Bestimmung von N-(n-Butyl)thiophosphorsäuretriamid (NBPT) und N-(n-Propyl)thiophosphorsäuretriamid (NPPT) - Verfahren mit Hochleistungs-Flüssigchromatographie (HPLC) This European Standard was approved by CEN on 16 April 2015.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, 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:
Avenue Marnix 17,
B-1000 Brussels © 2015 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16651:2015 ESIST EN 16651:2015



EN 16651:2015 (E) 2 Contents Page Foreword .3 1 Scope .4 2 Normative references .4 3 Terms and definitions .4 4 Principle .4 5 Reagents .4 6 Apparatus .5 7 Sampling .6 8 Procedure .6 8.1 Preparation of the test solution .6 8.2 Calibration .6 8.3 Blank test .6 8.4 Calculation and expression of the results .6 8.4.1 Concentration of NBPT .6 8.4.2 Concentration of NPPT .7 8.4.3 External response factors .7 8.4.4 Calculation of the total content .8 8.5 Environmental aspects .8 9 Precision .8 9.1 Inter-laboratory test .8 9.2 Repeatability .8 9.3 Reproducibility .8 10 Test report .9 Annex A (informative)
Results of the inter-laboratory test . 10 Bibliography . 11
SIST EN 16651:2015



EN 16651:2015 (E) 3 Foreword This document (EN 16651:2015) has been prepared by Technical Committee CEN/TC 260 “Fertilizers and liming materials”, the secretariat of which is held by DIN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by November 2015, and conflicting national standards shall be withdrawn at the latest by November 2015. 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 organisations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. SIST EN 16651:2015



EN 16651:2015 (E) 4 1 Scope This European Standard specifies a method for the quantitative determination of the urease inhibitors N-(n-Butyl)thiophosphoric acid triamide (NBPT, CAS-No. 94317-64-3) and N-(n-Propyl)thiophosphoric acid triamide (NPPT, CAS-No. 916809-14-8) content in urea based fertilizers using high-performance liquid chromatography (HPLC). 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. 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 EN ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696) 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 The fertilizer sample is diluted in water, grade 1. The concentration of N-(n-Butyl)thiophosphoric acid triamide (NBPT) and N-(n-Propyl)thiophosphoric acid triamide (NPPT) is determined in diluted aqueous solution by high-performance liquid chromatography (HPLC) using an UV detector at 205 nm. 5 Reagents Use only reagents of recognized analytical grade. 5.1 Water, grade 1 according to EN ISO 3696. 5.2 Acetonitrile, HPLC grade. 5.3 Urea, analytical pure. 5.4 NBPT, N-(n-Butyl)thiophosphoric acid triamide, CAS-No. 94317-64-3, analytical pure. 5.5 NPPT, N-(n-Propyl)thiophosphoric acid triamide, CAS-No. 916809-14-8, analytical pure. 5.6 Eluent. Mix in a 1 000 ml volumetric flask (6.2), 750 ml of water (5.1) and 250 ml acetonitrile (5.2) and filter through a micro filter (6.3). 5.7 Stock solution, (NBPT) = 0,20 mg/ml and (NPPT) = 0,12 mg/ml. SIST EN 16651:2015



EN 16651:2015 (E) 5 Weigh in a 250 ml graduated flask (6.2), an amount of 50 mg NBPT and 30 mg NPPT. Add approximately 200 ml of water (5.1) and shake until NBPT and NPPT are diluted. Fill up to the mark with water (5.1) and shake. This stock solution may be used within 24 h. 5.8 Cal
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