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
ICS
65.080 - Fertilizers
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
28-Jan-2026
Directive
2003/2003 - Regulation (EC) N° 2003/2003 of the European Parlament and of the council of 13 October 2003 relating to fertilisers
2019/1009 - Regulation (EU) 2019/1009 of the European Parliament and of the Council of 5 June 2019 laying down rules on the making available on the market of EU fertilising products and amending Regulations (EC) No 1069/2009 and (EC) No 1107/2009 and repealing Regulation (EC) No 2003/2003
Mandate
M/418 - Standardization mandate M/335 assigned to CEN concerning the modernisation of the methods of analysis of fertilizers
Ref Project
SIST EN 16328:2013 - Fertilizers - Determination of 3,4-dimethyl-1H-pyrazole phosphate (DMPP) - Method using high-performance liquid chromatography (HPLC)

Relations

Refers
EN 12944-2:1999 - Fertilizers and liming materials and soil improvers - Vocabulary - Part 2: Terms relating to fertilizers
Effective Date
28-Jan-2026
Refers
EN 1482-2:2024 - Fertilizers, liming materials and inhibitors - Sampling and sample preparation - Part 2: General sample preparation provisions
Effective Date
28-Jan-2026
Refers
EN 12944-1:1999 - Fertilizers and liming materials and soil improvers - Vocabulary - Part 1: General terms
Effective Date
28-Jan-2026
Referred By
EN 15207:2006 - Tanks for transport of dangerous goods - Plug/socket connection and supply characteristics for service equipment in hazardous areas with 24 V nominal supply voltage
Effective Date
28-Jan-2026
Referred By
CEN/TS 17752:2022 - Inorganic fertilizers - Determination of specific inhibitors
Effective Date
28-Jan-2026

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.

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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 has the following relationships with other standards: It is inter standard links to EN 12944-2:1999, EN 1482-2:2024, EN 12944-1:1999, EN 15207:2006, CEN/TS 17752:2022. Understanding these relationships helps ensure you are using the most current and applicable version of the standard.

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.

EN 16328:2012 is available in PDF format for immediate download after purchase. The document can be added to your cart and obtained through the secure checkout process. Digital delivery ensures instant access to the complete standard document.

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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