65.080 - Fertilizers

This document specifies general requirements for the testing, sampling and preparation of test samples and the marking, labelling, packaging, transport and storage of compound fertilizers. This document is applicable to inorganic solid compound fertilizers. This document is not applicable to controlled-release compound fertilizers.

When handling fertilizer grains, dust is at every moment generated on the surface. The fertilizer thus contains more or less free dust, and has a potential for generating more dust (abrasion dust) when subject to subsequent handling. In all existing gravitational test methods dust will be generated during the testing time, and the two types of dust will be measured simultaneously.

This CEN report gives the results of inter-laboratory testing to compare the accuracy and convenience of the official EC method for porosity measurement (given as Annex B) with two non-standardized alternative methods (given as Annexes C and D) already used in some participating laboratories.

This Technical Report is applicable to crushing strength measurement as applied to grains of fertilizers obtained in prilling or wet-granulation process. Compacted or crystalline materials were not considered.

This document specifies a method for the determination of total nitrogen content in all nitrogen containing fertilizers by combustion method. NOTEÂ 1Â Â The presence of non-nutritive sources of nitrogen (e.g. chelating agents) causes positive bias to samples being analysed for nutritive nitrogen content. The non-nutritive nitrogen content is subtracted from the total nitrogen value to determine the nutritive nitrogen content. NOTEÂ 2Â Â Common internationally traded fertilizers were evaluated for total nitrogen by combustion analysis in the ring-study in this document. While the fertilizers analysed in this international ring study were mineral fertilizers, previous studies have shown that total nitrogen by combustion is suitable for use with many non-mineral, nitrogen-containing fertilizers.

This document specifies the method for the determination of the EDTA soluble phosphorus content of inorganic fertilizers. The method is applicable for fertilizers composed of or blended from multiple sources such as superphosphate, ammonium phosphate, triple superphosphate, and/or nitrophosphate. It is not suitable for fertilizers containing calcium magnesium phosphates.

This document specifies a method for the determination of the cold and hot water insoluble nitrogen content in solid urea formaldehyde and methylene urea slow-release fertilizers and for the determination of the hot water soluble nitrogen content in nutrient polymers (see Component Material Category CMC 9 as specified in the Regulation (EC) No xxxx/2019 on Fertilizing Products [1]).

This document establishes an overview of the relevant methods for the determination of calcium and magnesium as defined in ISO 8157. This document is applicable to any mineral soil amendment, neutral, basic or acid containing calcium and/or magnesium.

This document specifies a method for the determination of traces of perchlorate with liquid chromatography and tandem mass spectrometry detection (LC‐MS/MS). The method is applicable to mineral fertilizers.

This document specifies a method to measure the total sulfur content in fertilizer and soil conditioner materials. This method is applicable for measuring total sulfur concentration in solid and liquid fertilizers and its raw inputs in the range of 0,1 % to 97 %.

This document is applicable to the sampling of mineral fertilizers and liming materials supplied or ready for supply to third parties, as a lot or in smaller lots, where such supply or readiness for supply is subject to legal requirements. This document specifies plans and methods of sampling of a lot of solid fertilizer or liming material, if sampling in motion is not possible, to obtain samples from bulk static heaps in order to ascertain compliance with legal requirements, in particular in relation to the accuracy of compulsory or permitted statutory declarations. The methods specified in this document are not applicable to obtain samples for physical size analysis or for chemical analysis which may be altered by particle granulometric segregation. This document is applicable to single nutrient fertilizers, to uniform complex fertilizers and to milled or granulated fertilizers and liming materials. The methods described in this document are not suitable for sampling other types of fertilizer, for example blended fertilizers. NOTE The term 'fertilizer' is used throughout the body of this document and includes liming materials unless otherwise indicated.

This document establishes a method for the determination of monosilicic acid concentrations in nonliquid fertilizer materials. Monosilicic acid is reported as silicon (Si). This extraction method is applicable to the detection of monosilicic acid in nonliquid fertilizer products, blended products, and beneficial substances at silicon (Si) concentrations of 2 to 84 g/kg, with a limit of detection (LOD) of 0,6 g/kg Si, and a limit of quantification (LOQ) of 2 g/kg correlating well with plant uptake. This method is not applicable to liquid silicon fertilizer sources due to an expected low bias of Si recovery and low correlation with plant uptake.

This document specifies a method for the determination of the speed and effectiveness of the neutralizing potential of calcium carbonate, calcium magnesium carbonate and calcium magnesium silicate liming materials by potentiometric titration with hydrochloric acid.
For liming materials coarser than 1 mm, it is essential to prepare the sample of a liming material by following exactly the description of Annex A.
This method is applicable only to liming materials with a maximum particle size of 6,3 mm.
The type of liming material can be identified according to EN 14069 and the particle size can be determined according to EN 12948.

This document specifies the test procedure for the determination of the salt out temperature (SOT), also known as the crystallization temperature (CT) of liquid (fluid) fertilizers, using an inexpensive and simple technique. This method might not be applicable to the binary and ternary fertilizers, especially with regards to the last crystal to disappear (LCTD). Some of these exceptions are discussed in the procedure (Clause 8).

This document specifies two methods for the determination of the neutralizing value (NV) of liming materials. Method A is applicable to all liming materials except silicate liming materials. NOTE 1 Examples of hard liming materials are limestone and dolomite. Examples of soft liming materials are chalk, marl and burnt lime. Method B is applicable to all liming materials. Neither method correctly takes into account the potential neutralizing value of material containing more than 3 % P2O5. For a more accurate agronomic assessment of products containing more than 3 % P2O5, EN 14984[8] is used to determine the liming efficiency. NOTE 2 The methods described in ISO 6598 and ISO 7497 can be used for the determination of P2O5 content. Further information on P analyses is given in References [5] and [6]. NOTE 3 Carbonate consumes H+ and removes acidity in solution with subsequent dissociation to H2O and CO2. Forms of orthophosphate can consume H+ but are not dissociated to molecular forms that remove acidity. The acidity is back titrated with alkali causing an underestimation of NV.

This European Standard describes a method to determine the aerobic biological activity of growing media and soil improvers or constituents thereof by measuring the oxygen uptake rate (OUR). The oxygen uptake rate is an indicator of the extent to which biodegradable organic matter is being broken down within a specified time period. The method is not suitable for material with a content of particle sizes > 10 mm exceeding 20 %.

This document describes a method to determine the aerobic biological activity of growing media and soil improvers or constituents thereof by measuring the oxygen uptake rate (OUR). The oxygen uptake rate is an indicator of the extent to which biodegradable organic matter is being broken down within a specified time period. The method is not suitable for material with a content of particle sizes > 10 mm exceeding 20 %.

This document specifies a method for the extraction of water soluble phosphorus. The method is applicable to all fertilizers, including compound fertilizers, where water soluble phosphorus is to be determined.

This document specifies a method for the determination of traces of perchlorate in mineral fertilizers by ion chromatography and conductivity detection (IC-CD).

This document specifies a method for the determination of traces of perchlorate in mineral fertilizers by ion chromatography and conductivity detection (IC-CD).

This European Standard defines terms relating to liming materials.
An index of all terms defined in this part of EN 12944, with their French and German equivalents is given in Annex A.
A general index of all terms defined in all three parts of EN 12944, with their French and German equivalents, is given in Annex B.

This European Technical Specification specifies a method for the determination of the lime requirement of acid soils to target pH levels at requested time of maintenance as determined by reaction with 0,1 mol/l ammonium acetate pH 5,5.
Due to general soil buffering systems, the method is applicable to all soils which are acid enough to dissociate hydrogen ions from the soil colloid system to depress the pH of the buffer solution.

This European Standard defines terms relating to liming materials.
An index of all terms defined in this part of EN 12944, with their French and German equivalents; is given in Annex A.
A general index of all terms defined in all three parts of EN 12944, with their French and German equivalents, is given in Annex B.

This document specifies a method for the determination of the lime requirement of acid soils to target pH levels at requested time of maintenance as determined by reaction with 0,1 mol/l ammonium acetate pH 5,5.
Due to general soil buffering systems, the method is applicable to all soils which are acid enough to dissociate hydrogen ions from the soil colloid system to depress the pH of the buffer solution.
NOTE 1   The method originates from research in Canada and Norway, see [1] and [2].
NOTE 2   Annex A gives regression equations to predict the maintenance of a range of pH levels at different times after liming in mineral and organic soils in Europe.

This method specifies a method for the determination of the nitrification inhibitor 2-(3,4-dimethyl-pyrazol-1-yl-succinic acid (DMPSA) using high-performance liquid chromatography (HPLC). The method is applicable to all mineral fertilizers.

This document specifies two methods for the determination of the particle size distribution of liming materials. Method A (the dry sieving method) is applicable to all liming materials except wet and paste-like products. Method A is not applicable if blinding, caking, electrostatic charges or agglomeration occur after drying. Method B (the wet sieving method) is applicable to products which are susceptible to blinding, caking, electrostatic charges or agglomeration after drying. Method B can be used to determine the primary particle size distribution of granulated products. Method B is not applicable to burnt lime and liming materials containing water-soluble constituents.

This document specifies a method for determining the reactivity of calcium carbonate and calcium magnesium carbonate liming materials. It assesses the speed and effectiveness of their neutralising potential by automatic titration with citric acid. This method is applicable only to liming materials with a maximum particle size of 6,3 mm determined in accordance with ISO 20977. NOTE For marble dolomite (BET procedure as defined in ISO 9277 below 500 m2/kg), see EN 14984.

This document specifies a method for the determination of nitrification inhibitor 2-(3,4-dimethyl-pyrazol-1-yl)-succinic acid (DMPSA) using high-performance liquid chromatography (HPLC), which is applicable to all mineral fertilizers.

This document specifies the procedure for the analysis of humic acids and hydrophobic fulvic acids which is applicable to dry and liquid materials used as ingredients in commercial fertilizers, soil amendments, and geological deposits.

This document specifies the procedure for determination of total and water extractable molybdenum in fertilizers containing less than or equal to 10 % molybdenum. The extraction methods are specified in EN 260172 and/or EN 260176.

This European Standard specifies a method for the determination of total and water extractable boron in mineral fertilizers containing more than 10 % boron.
This method is applicable to water and aqua regia fertilizer extracts obtained according to prEN 16962 and/or prEN 16964.
NOTE    A method used for determination of boron in mineral fertilizers containing less than 10 % of boron (spectrophotometric determination by azomethine-H) can be also used for the scope of this method after appropriate dilution of the extracts.

This document specifies the procedure for determination of total and water extractable boron in mineral fertilizers containing less than or equal to 10 % boron using spectrometry with azomethine-H. The method is not suitable for fertilizers with Fe concentrations more than twenty times higher than the concentration of boron.

This European Standard specifies a method for the determination of total and water extractable boron in mineral fertilizers containing less than or equal to 10 % boron. The method is not suitable for fertilizers with Fe concentrations more than twenty times higher than the concentration of boron.
This method is applicable to water and aqua regia fertilizer extracts obtained according to EN 16962 and/or EN 16964.
The method can also be used for the determination of boron in mineral fertilizers containing more than 10 % boron after appropriate dilution of the extracts.

This European Standard specifies a method for determination of total and water extractable molybdenum in mineral fertilizers containing less than or equal to 10 % molybdenum.
This method is applicable to water and aqua regia fertilizer extracts obtained according to EN 16962 and/or EN 16964.

This European Standard specifies a method for the determination of total and water extractable boron in mineral fertilizers containing more than 10 % boron.
This method is applicable to water and aqua regia fertilizer extracts obtained according to EN 16962 and/or EN 16964.
NOTE   A method used for the determination of boron in mineral fertilizers containing less than or equal to 10 % of boron (spectrophotometric determination by azomethine-H) can be also used for the scope of this method after appropriate dilution of the extracts.

The document specifies a method for the chromatographic determination of the chelating agent [S,S]-EDDS in fertilizers. The method allows the identification and the determination of the total concentration of the water soluble fraction of this chelating agent. It does not allow to distinguish between the free form and the metal bound form of the chelating agent. This method is applicable to EC-fertilizers containing chelates of one or more of the following micro-nutrients: cobalt, copper, iron, manganese and zinc covered by Regulation (EC) No 2003/2003. It is applicable to a mass fraction of the metal chelated of at least 0,35 %.

This European Standard specifies the procedure for extracting water soluble forms of boron, cobalt, copper, iron, manganese, molybdenum and zinc from mineral fertilizers containing one or more micro-nutrients and the procedure for removal of organic compounds from the water extracts.
The extracts can be analysed according to WI 00260173, prEN 16963, prEN 16965, WI 00260179, WI 00260180 and WI 00260182.

This European Standard specifies a method for the determination of cobalt, copper, iron, manganese and zinc in fertilizer extracts using flame atomic absorption spectrometry (FAAS).
This method is applicable to water and aqua regia fertilizer extracts obtained according to prEN 16962 and/or prEN 16964.
NOTE   In most cases, the presence of small quantities of organic matter will not affect determinations by FAAS and it is not necessary to apply organic matter removal.

This European Standard specifies a method for the determination of boron, cobalt, copper, iron, manganese, molybdenum and zinc in fertilizer extracts using inductively coupled plasma-atomic emission spectrometry (ICP-AES).
This method is applicable to water and aqua regia fertilizer extracts prepared according to prEN 16962 and/or prEN 16964.
NOTE   In most cases, the presence of small quantities of organic matter will not affect determinations by ICP-AES and it is not necessary to apply organic matter removal.

This European Standard specifies the procedure for total extraction of boron, cobalt, copper, iron, manganese, molybdenum and zinc with aqua regia from mineral fertilizers containing one or more micro-nutrients.
The extracts can be analysed according to WI 00260173, prEN 16963, prEN 16965, WI 00260179, WI 00260180 and WI 00260182.
NOTE   This method is also suitable for the extraction of cadmium, chromium, nickel and lead to be determined according to EN 16319; the extraction of mercury to be determined according to EN 16320 and the extraction of arsenic to be determined according to EN 16317.

ISO 7409:2018 specifies the procedure for marking containers or labels for fertilizers. ISO 7409:2018 is applicable to all fertilizers in containers or bulk.

This European Standard specifies a method for the extraction of water soluble forms of boron, cobalt, copper, iron, manganese, molybdenum and zinc from mineral fertilizers containing one or more micro-nutrients and the procedure for removal of organic compounds from the water extracts.
The extracts can be analysed according to EN 16963, EN 16965, prEN 17041, prEN 17042, prEN 17043 and CEN/TS 17060.

This European Standard specifies a method for the determination of boron, cobalt, copper, iron, manganese, molybdenum and zinc in fertilizer extracts using inductively coupled plasma-atomic emission spectrometry (ICP-AES).
This method is applicable to water and aqua regia fertilizer extracts prepared according to EN 16962 and/or EN 16964.
NOTE   In most cases, the presence of small quantities of organic matter will not affect determinations by ICP-AES and it is not necessary to apply organic matter removal.

This European Standard specifies a method for the total extraction of boron, cobalt, copper, iron, manganese, molybdenum and zinc with aqua regia from mineral fertilizers containing one or more micro-nutrients.
The extracts can be analysed according to EN 16963, EN 16965, prEN 17041, prEN 17042 and prEN 17043.
This method is also suitable for the extraction of cadmium, chromium, nickel and lead to be determined according to EN 16319; the extraction of mercury to be determined according to EN 16320 and the extraction of arsenic to be determined according to EN 16317.

This European Standard specifies a method for the determination of cobalt, copper, iron, manganese and zinc in fertilizer extracts using flame atomic absorption spectrometry (FAAS).
This method is applicable to water and aqua regia fertilizer extracts obtained according to EN 16962 and/or EN 16964.
NOTE   In most cases, the presence of small quantities of organic matter will not affect determinations by FAAS and it is not necessary to apply organic matter removal.

ISO 21263:2017 specifies a method for the determination of the slow release properties of nutrients from coated fertilizers. pH-dependent hydrolysis and degradation by biological or microbial mechanisms are excluded. The specified method is only applicable to products releasing any nutrients by means of a non-biological process (i.e. those where the nutrients are released by a physical mechanism). Microbial attack on the coating (e.g. sulfur coated fertilizers) and the consequences thereof are not measurable by the technique described. This method involves a lengthy process which may not be appropriate for day to day testing purposes. Accelerated methods can be used provided they are correlated with this document. An example of such an accelerated method is described in Annex B. Regression analysis can also be used for this purpose.

This European Standard specifies a method for the chromatographic determination of the chelating agent [S,S]-EDDS in fertilizers. The method allows the identification and the determination of the total concentration of the water-soluble fraction of this chelating agent. It does not allow distinguishing between the free form and the metal bound form of the chelating agent.
This method is applicable to EC fertilizers containing chelates of one or more of the following micro-nutrients: cobalt, copper, iron, manganese and zinc, covered by Regulation (EC) No 2003/2003 [4]. It is applicable to a mass fraction of the metal chelated of at least 0,35 %.
NOTE 1   The substance EDDS (ethylenediamine-N,N'-disuccinic acid) exists as several different stereo isomeric forms. [S,S] (with CAS Number 20846–91–7), [R,R] and [R,S] optical isomers are possible. [S,S] and [R,R] are mirror images with equal chemical characteristics. However only the [S,S] isomer is biodegradable. When both are present, they form the racemic mixture. The [R,S] isomer (the meso isomer) is only slowly biodegradable.
Only the [S,S]-EDDS isomer is allowed by the Regulation (EC) No 2003/2003. Since the Cu chelate of the [R,R]-EDDS isomer presents the same stability than the [S,S]-EDDS, both should coelute. The absence of [R,S]-EDDS indicates that only a pure isomer ([S,S] or [R,R]) exist. An additional test based on polarimetry can be used to ascertain the isomeric characteristic of the sample, or the standard.

This European Standard specifies a method for the chromatographic determination of the iron chelated by each individual ortho(hydroxy)-ortho(hydroxy) isomer of the chelating agents [o,o] EDDHA, [o,o] EDDHMA and by HBED in fertilizers containing one or more of these substances, except for [o,o] EDDHMA and HBED mixes. The method allows the identification and the determination of the total concentration of water soluble iron chelates of these chelating agents. Also, after derivatization with Fe, the soluble amount of the chelating agents may be determined when other micro-nutrients, beside Fe are present in fertilizers containing [o,o] EDDHA, [o,o] EDDHMA or HBED.
This method is applicable to EC fertilizers covered by Regulation (EC) No 2003/2003 [4]. It is applicable to a mass fraction of the metal chelated of at least 0,625 %.
NOTE 1   The substances EDDHA (ethylenediamine-N,N'-di[(hydroxyphenyl)acetic acid] and EDDHMA (ethylenediamine-N,N'-di[(hydroxymethylphenyl)acetic acid] exist as several different isomeric forms. Positional isomers for the hydroxyl or methyl groups (in ortho, meta, and para positions) as well as stereo isomers (meso and dl-racemic forms) are known. Both meso and dl-racemic forms of the [ortho,ortho] EDDHA and [ortho,ortho] EDDHMA are positional isomers for the hydroxyl groups allowed by the Regulation (EC) No 2003/2003. Since para, meta and ortho methyl positional isomers of the EDDHMA present quite similar stability, they could be grouped: in the method here described the para, meta and ortho methyl positional isomers of the [o,o] EDDHMA are considered together. HBED (N,N'-bis(2-hydroxybenzyl)-ethylenediamine-N,N'-diacetic acid) does not present isomeric forms.
NOTE 2   At present, analytically pure standards only exist for [ortho,ortho] EDDHA, [ortho,ortho] EDDHMA and HBED. All other substances being unavailable as a standard, the influence of their eventual presence in the samples (with respect to the sensitivity and the selectivity of this method) has not been studied.
NOTE 3   The meso and the dl-racemic forms of [o,o] EDDHA and [o,o] EDDHMA can be determined separately by this method.

This document describes and specifies the basic and premium requirements of products of natural origin and products from industrial processes to be used as liming materials in agriculture for raising the pH of soil (and water).

ISO 20702:2017 specifies the ion chromatography method for the determination of microamounts of water soluble inorganic anions, such as fluoride (F−), chloride (Cl−), bromide (Br−), iodide (I−), nitrite (NO2−) and thiocyanate (SCN−), in fertilizers.