EN 16328:2012
(Main)Fertilizers - Determination of 3,4-dimethyl-1H-pyrazole phosphate (DMPP) - Method using high-performance liquid chromatography (HPLC)
Fertilizers - Determination of 3,4-dimethyl-1H-pyrazole phosphate (DMPP) - Method using high-performance liquid chromatography (HPLC)
This European Standard specifies a method for the determination of 3,4-dimethyl-1H-pyrazole phosphate (DMPP, CAS-No: 202842-98-6) in mineral N containing fertilizers using high-performance liquid chromatography (HPLC).
Düngemittel - Bestimmung von 3,4-Dimethyl-1H-pyrazolphosphat (DMPP) - Verfahren mit Hochleistungs-Flüssigchromatographie (HPLC)
Dieses Dokument legt ein Verfahren zur Bestimmung von 3,4-Dimethyl-1H-pyrazolphosphat (DMPP, CAS-No: 202842-98-6) in mineralischen stickstoffhaltigen Düngemitteln mit Hochleistungs-Flüssigchromato-graphie (HPLC) fest.
Engrais - Dosage du 3,4-diméthyl-1H-pyrazole phosphate (DMPP) - Méthode par chromatographie liquide à haute performance (HPLC)
La présente Norme européenne spécifie une méthode de dosage du 3,4-diméthyl-1H-pyrazole phosphate (DMPP, n° CAS : 202842-98-6) dans les engrais minéraux contenant de l'azote par la méthode de chromatographie liquide à haute performance (HPLC).
Gnojila - Določevanje 3,4-dimetil-1H-pirazol fosfata (DMPP) - Metoda tekočinske kromatografije visoke ločljivosti (HPLC)
Ta evropski standard določa metodo za določevanje 3,4-dimetil-1H-pirazol fosfata (DMPP, številka CAS: 202842-98-6) v mineralnem dušiku, ki vsebuje gnojila, z metodo tekočinske kromatografije visoke ločljivosti (HPLC).
General Information
- Status
- Published
- Publication Date
- 11-Dec-2012
- Withdrawal Date
- 29-Jun-2013
- Technical Committee
- CEN/TC 260 - Fertilizers and liming materials
- Drafting Committee
- CEN/TC 260/WG 7 - Chemical analysis
- Current Stage
- 9093 - Decision to confirm - Review Enquiry
- Start Date
- 04-Jun-2024
- Completion Date
- 14-Apr-2025
Overview
EN 16328:2012 (CEN) specifies an HPLC method for the determination of 3,4-dimethyl-1H-pyrazole phosphate (DMPP) in mineral nitrogen-containing fertilizers. The standard defines sample preparation, HPLC conditions, calibration, calculation of results and precision criteria (repeatability and reproducibility). It is intended for analytical laboratories, fertilizer manufacturers and regulatory bodies requiring consistent, traceable DMPP analysis across Europe.
Key topics and technical requirements
- Scope: Determination of DMPP (CAS 202842-98-6) in mineral N fertilizers using reversed-phase HPLC.
- Sample preparation: Dissolve 30.000 g sample in 1 000 mL de‑ionized water (ultrasonic bath ~15 min), filter (0.45 µm) and, if necessary, dilute to calibration range.
- Calibration: Prepare at least four calibration concentrations (recommended range 3–100 mg/L) from weighed stock solutions of DMPP; inject each calibration level three times.
- HPLC conditions (typical settings provided):
- Reversed-phase column (e.g. C18, 5 µm, 150 × 4.6 mm)
- Mobile phase: NaH2PO4 solution in water with acetonitrile (recipe given)
- Flow rate: 1.5 mL/min; injection volume: 10 µL; detection wavelength: 224 nm
- Typical DMPP retention time ≈ 5.3 min
- Quantification: Use least-squares calibration curve (correlation coefficient p ≥ 0.99) and calculate DMPP content from peak area/height with the provided formula and dilution factor.
- Precision: Results from an inter-laboratory study (2010) are reported. Example precision limits:
- Mean values around 706–1 700 mg/kg depending on matrix
- Repeatability limits (r) e.g. 56–90 mg/kg
- Reproducibility limits (R) e.g. 170–410 mg/kg
- Safety and reagents: Use analytical grade solvents (HPLC acetonitrile, de‑ionized water) and follow laboratory safety for hazardous materials.
Applications and users
- Fertilizer manufacturers: Quality control of N fertilizer products containing DMPP to verify label claims and product consistency.
- Independent testing laboratories: Routine and regulatory testing for compliance with EU fertilizer regulations.
- Regulatory authorities: Verification of product conformity and enforcement of limits for nitrification inhibitors.
- Research labs: Methodology for studies on DMPP behavior, degradation and efficacy in fertilizer matrices.
Related standards
- EN 1482-1 / EN 1482-2 - sampling and sample preparation for fertilizers (referenced for sampling and preparation).
- ISO 5725 series - precision and accuracy methods used for inter-laboratory statistics.
Keywords: EN 16328:2012, DMPP analysis, HPLC method, fertilizer testing, 3,4-dimethyl-1H-pyrazole phosphate, CEN, mineral N fertilizers, analytical method.
Frequently Asked Questions
EN 16328:2012 is a standard published by the European Committee for Standardization (CEN). Its full title is "Fertilizers - Determination of 3,4-dimethyl-1H-pyrazole phosphate (DMPP) - Method using high-performance liquid chromatography (HPLC)". This standard covers: This European Standard specifies a method for the determination of 3,4-dimethyl-1H-pyrazole phosphate (DMPP, CAS-No: 202842-98-6) in mineral N containing fertilizers using high-performance liquid chromatography (HPLC).
This European Standard specifies a method for the determination of 3,4-dimethyl-1H-pyrazole phosphate (DMPP, CAS-No: 202842-98-6) in mineral N containing fertilizers using high-performance liquid chromatography (HPLC).
EN 16328:2012 is classified under the following ICS (International Classification for Standards) categories: 65.080 - Fertilizers. The ICS classification helps identify the subject area and facilitates finding related standards.
EN 16328:2012 is associated with the following European legislation: EU Directives/Regulations: 2003/2003, 2019/1009; Standardization Mandates: M/418. When a standard is cited in the Official Journal of the European Union, products manufactured in conformity with it benefit from a presumption of conformity with the essential requirements of the corresponding EU directive or regulation.
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Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Düngemittel - Bestimmung von 3,4-dimethyl-1H-pyrazolphosphat (DMPP) - Verfahren mit Hochleistungs-Flüssigchromatographie (HPLC)Engrais - Dosage de la 3,4-diméthyle-1H-pyrazole phosphate (DMPP) - Méthode par chromatographie liquide à haute performance (CLHP)Fertilizers - Determination of 3,4-dimethyl-1H-pyrazole phosphate (DMPP) - Method using high-performance liquid chromatography (HPLC)65.080GnojilaFertilizersICS:Ta slovenski standard je istoveten z:EN 16328:2012SIST EN 16328:2013en,fr,de01-maj-2013SIST EN 16328:2013SLOVENSKI
STANDARD
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16328
December 2012 ICS 65.080 English Version
Fertilizers - Determination of 3,4-dimethyl-1H-pyrazole phosphate (DMPP) - Method using high-performance liquid chromatography (HPLC)
Engrais - Dosage du 3,4-diméthyl-1H-pyrazole phosphate (DMPP) - Méthode par chromatographie liquide à haute performance (HPLC)
Düngemittel - Bestimmung von 3,4-Dimethyl-1H-pyrazolphosphat (DMPP) - Verfahren mit Hochleistungs-Flüssigchromatographie (HPLC) This European Standard was approved by CEN on 27 October 2012.
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
Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16328:2012: ESIST EN 16328:2013
Results of the inter-laboratory test .8A.1 Inter-laboratory tests .8A.2 Statistical results .8Bibliography .9 SIST EN 16328:2013
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