EUROPEAN COMMISSION ENTERPRISE AND INDUSTRY DIRECTORATE-GENERAL Chemicals, metals, mechanical, electrical and construction industries; Raw materials Chemicals - Classification & Labelling, Specific Products, Competitiveness Brussels, 29 May 2012 ENTR G2/KB D(2011) NOTE TO THE MEMBERS OF WORKING GROUP 4 (LABELLING, ENFORCEMENT AND CONTROL) Thought starter – Methods of analysis, tolerances and traceability requirements 1. INTRODUCTION WG 4 Members are invited to comment this thought starter document, which has been prepared in view of the next meeting. Please make use of the WG 4 CIRCA newsgroup for your suggestions. During your reflections, please bear in mind that analytical results aims at providing the necessary information to farmers to opt for the most suitable fertilization and helps the enforcement by Competent Authorities. This document might eventually serve as a basis for the preparation of a mandate to CEN for the development of analytical methods for the control of inorganic and organic fertilisers, soil improvers (SI)1 and growing media (GM). No method of analysis for the compliance check of plant biostimulants is described in this document as so far no specific quality parameters have been defined by WG 2. As this document refers to the various product categories, WG 4 members are invited to consult the thought starter for the WG 1 meeting of 13 June 2012 where definitions for those product categories are proposed. 2. MINIMUM NUTRIENT FERTILISERS CONTENT AND LABELLING REQUIREMENTS FOR The setting of minimum nutrient content criteria would be a proxy of the intrinsic agronomic value of the final fertilisers and would underpin the legal definition of fertilisers and related materials. WG 2 supports the setting of minimum nutrient content criteria for inorganic 1 This category includes liming materials, organic soil improvers and soil conditioner as defined in the though starter document for the meeting of WG 1 on 13 and 14 June 2012 Commission européenne, B-1049 Bruxelles / Europese Commissie, B-1049 Brussel - Belgium. Telephone: (32-2) 299 11 11. Office: BREY 11/254. Telephone: direct line (32-2) 299 48 60. Fax: (32-2) 295 02 81. E-mail: klaus.berend@ec.europa.eu fertilisers and organic fertilisers, in particular also to differentiate the latter from organic soil improvers. The provisional criteria discussed by WG 2 are the following: Inorganic fertiliser* Organic fertiliser* Organic soil improver Organic matter content on dry matter 0% No limit but the organic matter content must be declared Min. 15% or 20% Minimum nutrient content on dry matter (individual value qualifies the product as a … N total 2% P2O5 total 1.0% K2O total 1.5% N total 1.5% or 1% P2O5 total 0.5% K2O total 0.75% No minimum limit would be defined but the presence of nutrients shall be declared (*) in principle valid for fluid and solid fertilisers (to be confirmed) WG 4 should check whether the analytical methods proposed in the following sections are appropriate for the control of the abovementioned requirements in particular for the rather low nutrient content limits proposed by WG 2. 2.1. Declaration of nutrients in inorganic and organic fertilisers 2.1.1. Nitrogen in inorganic fertilisers During its first meeting, WG 4 agreed to simplify the forms of nitrogen to be declared for inorganic fertilisers compared to the current rules by proposing to declare the following forms: Forms of nitrogen in inorganic fertilisers if present (percentage on the product as received) Determination method Total nitrogen EN 157502 suitable for all forms of nitrogen including urea formaldehyde condensates but not for cyanamide nitrogen. EN 156043 covers all individual forms of nitrogen present in the fertiliser including cyanamide Nitric nitrogen Determined on the basis of the calculation [nitric and ammoniacal nitrogen according to Devarda (EN 15476)] 2 This European Standard specifies two different methods (Methods A and B) for the determination of the total nitrogen content in fertilizers. Method A specifies the titrimetric method after distillation according to ISO 5315:1984. Method B specifies a method by reduction of nitrate with iron and tin(II)-chloride. 3 this standard specifies a method for the determination of any of the nitrogen forms present. 2 minus ammoniacal nitrogen (EN 15475) Ammoniacal nitrogen EN 15475 Ureic nitrogen EN 15604 WG 4 should agree whether EN 15750 or EN 15604 should be used to determine the total nitrogen content in inorganic matrices. Are the methods listed above appropriate for any combination of inorganic fertilisers with other groups of products (organic fertilisers, liming materials, organic soil improvers, soil conditioners)? 2.1.2. Nitrogen in organic fertilisers WG 2 agreed that the following forms of nutrients shall be declared for organic fertilisers: Forms of nitrogen in organic fertilisers if present (percentage on the product as received) Determination method Total nitrogen [N total] = [Total Kjeldahl Nitrogen4 described in AOAC5 955.04] + [Nitric nitrogen] or Italian Norm UNI 10780 Organic nitrogen + the origin of [N Organic]=[Total Kjeldahl Nitrogen – Ammoniacal N the organic fraction6 – Ureic N] Ammoniacal nitrogen AOAC 920.03 (Magnesium Oxide method suggested by University of Bologna). Not applicable in presence of Urea Nitric nitrogen AOAC 930.01 Ureic nitrogen AOAC 2003.14 (HPLC method) According to some experts, the organic nitrogen content can only be determined on the basis of a calculation ([N total] – [N ammoniacal and ureic N]). However, as the organic nitrogen fraction would be partly soluble in water, the presence of other only partly water-soluble products such as urea formaldehyde condensates could interfere. 4 TKN AOAC stands for Association of Analytical Communities. More info on: http://www.aoac.org/about/History.htm 6 WG 2 also agreed that the origin of the organic nitrogen should be labelled, as for example nitrogen from animal blood is quickly released compared to nitrogen from other organic matter. 5 3 WG 4 is invited to confirm that the analytical methods proposed in the table above are appropriate for the compliance check of the various nitrogen forms in organic fertilisers. Are there possible interferences between nutrients and organic matter that could lead to an over- or underestimation of the nutrient content? WG 4 should give its opinion on whether the declaration of the origin of the organic nitrogen would be an alternative to the determination of the kinetics of nitrogen release or whether alternatively, a classification system for the kinetics of nitrogen release could be established (slow to rapid nitrogen release, as done in FR and PT). 2.1.3. Phosphorus in inorganic fertilisers WG 4 agreed to retain the following forms for the declaration of phosphorus where appropriate: Forms of phosphorus in Extraction method inorganic fertiliser (percentage on the product as received) Total phosphorus EN 15956 Water-soluble phosphorus EN 15958 Determination method EN 15959 P2O5 content soluble in weak EN 15919 acid (formic acid7) P2O5 content soluble in neutral EN 15957 ammonia citrate8 2.1.4. Phosphorus in organic fertilisers WG 4 could not yet find a consensus about the forms of phosphorus to be declared for organic fertilisers. Nevertheless, the following forms were discussed: Forms of phosphorus in Extraction method organic fertiliser matrices (percentage on the product as received) Total phosphorus Determination method EN 15956 EN 15959 Phosphorus content soluble in EN 15956 strong acid From an analytical point of view both forms are identical. WG 4 is invited to further reflect on whether other forms than total phosphorus should be declared on the label of organic fertilisers? 7 8 The solubility in formic acid was favoured by more participants as it will cover a broader range of products At the request of EU countries with alkaline soils 4 2.1.5. Declaration of potassium, calcium, magnesium, sodium and sulphur content in inorganic and organic fertilisers. At the last meeting, WG 4 agreed to the position of WG 2 to retain only the declaration of water-soluble forms of K, Ca, Mg, Na and S for inorganic fertilisers and that no difference should be made for organic fertilisers. Forms of K, Ca, Mg, Na and S in fertilisers (percentage on the product as received) Extraction method Determination method Water-soluble potassium EN 15477 EN 15477 Water-soluble magnesium EN 15961 Method 8.7 of Annex IV to Regulation (EC) No 2003/2003 Water-soluble sulphur EN 15961 EN 15749 Water-soluble sodium EN 15961 Method 8.10 of Annex IV to Regulation (EC) No 2003/2003 Water-soluble calcium EN 15961 Method 8.6 of Annex IV to Regulation (EC) No 2003/2003 WG 4 is asked to reflect whether the analytical methods mentioned above are appropriate for organic fertilisers? If these methods are not deemed appropriate, WG 4 is asked to identify specific national or international methods which are used by the Member States and/or industry. According to some experts, dolomite is often added to inorganic or organic fertilisers to maintain the soil magnesium content. The magnesium content from dolomite is not watersoluble and some experts suggested adding the declaration of the total magnesium content to the list above. However, the list of criteria for liming materials already foreseen the determination of the total magnesium content. WG 4 should reflect on whether it is necessary to add the total magnesium content in the list above when this requirement is already foreseen for liming fertilisers. 2.1.6. Declaration of micro-nutrients The declaration of the water-soluble content of micro-nutrients was largely supported by WG 4. The methods mentioned in the table below are the methods listed in Annex IV of Regulation (EC) No 2003/2003 for the determination of micro-nutrients. CEN is in the process of transforming the analytical methods that operate with modern instrumental methods into EN Standards. If deemed appropriate by CEN, some old chemical methods (highlighted in yellow in the table below) could also be transformed into EN Standards. Forms of micronutrients in inorganic Extraction method 5 Determination method and organic fertilisers (percentage on the product as received) Water-soluble B Water-soluble Co Water-soluble Cu Water-soluble Fe Water-soluble Mn Water-soluble Mo Water-soluble Zn Method 9.2 nutrient < 10% Method 9.4 or 9.5 Method 10.2 nutrient >10% Method 10.4 or 10.5 Method 9.2 nutrient < 10% Method 9.4 or 9.6 Method 10.2 nutrient >10% Method 10.4 or 10.6 Method 9.2 nutrient < 10% Method 9.4 or 9.7 Method 10.2 nutrient >10% Method 10.4 or 10.7 Method 9.2 nutrient < 10% Method 9.4 or 9.8 Method 10.2 nutrient >10% Method 10.4 or 10.8 Method 9.2 nutrient < 10% Method 9.4 or 9.9 Method 10.2 nutrient >10% Method 10.4 or 10.9 Method 9.2 nutrient < 10% Method 9.4 or 9.10 Method 10.2 nutrient >10% Method 10.4 or 10.10 Method 9.2 nutrient < 10% Method 9.4 or 9.11 Method 10.2 nutrient >10% Method 10.4 or 10.11 WG 4 should discuss whether the Atomic Absorption Spectroscopy method mentioned above under methods 9.4 and 10.4 could be used for the determination of micro-nutrients in organic fertilisers. Are there appropriate methods for the determination of micro-nutrient fertilisers in soil improvers and growing media? 2.1.7. Micro-nutrient chelates in inorganic and organic fertilisers At the first meeting, WG4 agreed to keep the existing rules for chelated micro-nutrients. However, the availability of CEN analytical methods seems to be problematic according to certain participants as the current EN standard titles are creating the belief that the determination of chelated forms of micronutrients is limited to iron. WG4 agreed also to keep the existing rules for complexed micro-nutrients. CEN is invited to check whether the analytical methods listed in Annex IV of the Fertilisers Regulation for chelated micro-nutrients are deemed to cover all the micronutrients or only iron chelates. A change in the titles of certain EN standards might consequently be required (EN 13368-1 and EN 13368-2). WG 4 is invited to propose appropriate analytical methods for the detection of micronutrient chelates in organic fertilisers, soil improvers and growing media if appropriate. 6 3. LABELLING REQUIREMENTS FOR ORGANIC SOIL IMPROVERS The analytical methods mentioned above do not have SI in their scopes. Therefore CEN TC/223 has developed specific methods for SI. WG 2 agreed that the following criteria shall be declared for organic soil improvers: Quality criteria for organic Determination method soil improvers (on the product as received) pH EN 13037 Organic matter content (%) EN 130399 Total nitrogen (%) EN 13654-110 or EN 13654-2 Total phosphorus (%) EN 13650 Total potassium (%) EN 13650 Dry matter content (%) EN 13040 Electric conductivity (optional) EN 13038 (mS/m) A separate description of the method of extraction is not required as the appropriate method is specified in the relevant determination standard. WG 4 should discuss whether the analytical methods mentioned above are appropriate. 4. LABELLING REQUIREMENTS FOR LIMING MATERIALS WG 2 agreed that the following criteria shall be declared: Quality criteria for liming materials (on the product as received) Determination method Comments Neutralising value EN 12945 Fineness EN 12948 A minimum neutralising value of 15% should be set For all natural limes and oxide and hydroxide lime of natural origin - optional Soil improvers and growing media – Determination of organic matter content and ash at 450 +/-25°C. Organic matter is determined by calculation: (100%-ash)=organic matter. 10 EN 13654-1 is the most commonly used for SI according to EPAGMA 9 7 Total calcium (% CaO) EN 13475 (Oxalate) EN 12946 (Complexometry) Total MgO) magnesium (% EN 12947 (AAS) EN 12946 (Complexometry) Reactivity (%) EN 16357 (in citric acid) For all natural limes – optional WG 4 should confirm that the standards listed above are appropriate for the control of the compliance of liming materials with the corresponding quality criteria. 5. LABELLING REQUIREMENTS FOR GROWING MEDIA (GM) WG 2 suggested that for growing media the following parameters be determined at the time of manufacturing as the stability of the end-product properties cannot be ensured over time. The technical Committee for soil improvers and growing media (CEN/ TC 223) has been working on an 'aerobic biological activity' test which might be appropriate to test the maturity of compost. Quality criteria for growing media (at the time of manufacturing) Determination method Comments Electric conductivity (mS/m) EN 13038 Measured at the time of manufacture. Tolerance : +/- 50% pH EN 13037 Tolerance : +/- 0.5 The tolerance mentioned in the table refer only to the analytical methods Quantity by volume (litres EN 12580 or m³) Tolerance : -5% for individual units within a batch at the time of manufacture and 0% for the whole batch at the time of manufacture Quantity (volume) EN 15238 determination of materials with particle size greater than 60 mm (for very coarse SI such as mulches (e.g. bark) Tolerance : -5% for individual units within a batch at the time of manufacture and 0% for the whole batch at the time of manufacture Quantity determination Tolerance : -5% for individual units within a (volume) EN 15761 of pre8 shaped GM (e.g. mineral wool slabs) batch at the time of manufacture and 0% for the whole batch at the time of manufacture Total nitrogen (mg/l) EN 13651 (Calcium Optional 11 Chloride/DTPA or CATmethod) or EN 13652 (watersoluble method) Total phosphorus (mg/l) EN 13651 or EN 13652 Optional Total potassium (mg/l) EN 13651 or EN 13652 Optional Total pore space (% by EN 13041 volume at a given pressure) Optional Water volume (% by EN 13041 volume at a given pressure) Optional Air volume (% by volume EN 13041 at a given pressure) Optional Shrinkage (% by volume) Optional EN 13041 WG 4 should confirm the scope of EN 13651 and EN 13652 as it seems that those methods are not appropriate for the determination for the total nutrient content. Would EN 13650 be more appropriate (extraction in strong acid) 6. Sampling methods SAMPLING METHODS Inorganic fertilisers Organic fertilisers and liming materials Soil improvers (including organic soil improvers and soil conditioners) and growing media EN 1482-1 EN 12579 ? Sampling of WI 00260140 static heaps (codification for a standard in development) 11 Diethylenetriaminepentaacetic acid 9 Sample preparation methods EN 1482- 2 ? EN 13040 WG 4 should confirm the sampling standards proposed for growing media and soil improvers (i.e. organic soil improvers and soil conditioners as defined in the thought starter document for WG 1). Can WG 4 confirm that the sampling methods for soil improvers and growing media can also apply to organic fertilisers or whether specific methods should be developed? 7. 7.1. MAXIMUM CONTAMINANT CONTENT Non-nutrient metals CEN has developed or is developing several analytical methods for the determination of non-nutrient metals for inorganic fertilisers, soil improvers and growing media. There is currently not yet full agreement on the acceptable maximum limits - the range of maximum limit values under discussion in WG 3 is indicated in the table below: Proposed Inorganic maximum limit fertilisers value (mg/kg d.m) Liming materials Organic fertilisers Soil improvers and growing media Arsenic 30 - 60 CEN/TS 16317 ? ? EN 13650 Cadmium 1.5 - 3 EN 14888 or ? CEN/TS 16319 ? EN 13650 CEN/TS 16318 ? n.a n.a12Cr (VI) is not relevant for organic fertilisers. Chromium 2 (VI) Lead 120 – 190 CEN/TS 16319 ? ? EN 13650 Mercury 1-2 CEN/TS 16320 ? ? EN 13650 Nickel 40 – 120 CEN/TS 16319 ? ? EN 13650 12 Cr (VI) is not relevant for organic based fertilisers as Cr 6+ is reduced to Cr3+ in the presence of fresh organic matter. 10 Liming materials have a high pH value. Therefore the extraction method for the determination of heavy metals in lime should ensure that total extraction is achieved. WG 4 and or CEN should confirm that the detection limits of the standards listed are compatible with the maximum limit values discussed by WG 3. Can WG 4 suggest methods for organic fertilisers? Which method could be recommended for mixtures of fertilisers? WG 4 should decide whether extraction in aqua regia is appropriate for liming materials. 7.2. Micro-nutrient metals WG 3 considered that maximum limit values should be set only for products in which copper, zinc and selenium are not intentionally added. Therefore the determination of traces of copper, zinc and selenium should be limited to straight liming materials, organic fertilisers, soil improvers and growing media Proposed maximum limit values (EoW criteria JRC-Ispra mg/kg d.m) Liming Organic fertilisers materials from by-products of the steel industry Organic soil improvers and growing media Copper 100 ICP-OES. VDLUFA method II.10 – 8.10 micronutrients ? EN 13650 Zinc 400 ICP-OES. VDLUFA method II.10 – 8.10 micronutrients ? EN 13650 Hybrid AAS. VDLUFA method 2.1.1.2 ? ISO N 373 ? Selenium 15 (Finland) Can WG 4 suggest or confirm standards for the determination of Cu and Zn as contaminants in the product categories mentioned in the table above? WG 4 is also invited to discuss whether the appropriate analytical methods for Se are appropriate. 7.3. Organic contaminants WG 3 suggested the following range of maximum limit values for the organic pollutants listed below. 11 Proposed maximum Organic limit values fertilisers Organic soil improvers and growing media (depending on the source of the input materials) PCBs 0.1 – 0.2 mg/kg d.m ? (sum of 6 congeners – 28,52,101,138,153,180) Fpr EN 16167determination of PCBs by gas chromatography PCDD/Fs 20 – 30 ng WHO - ? TE/kg d.m toxicity equivalent of 2-,3-,7-,8TCDD Fpr EN 16190 – determination of dioxins and furans and dioxin-like polychlorinated biphenyl by gas chromatography PAHs 6 mg/kg d.m (sum of 6 ? congeners13) Fpr EN 16181determination of polycyclic aromatic carbons by gas chromatography Or VDLUFA VII 3.3.3 (16 congeners including the congeners mentioned in footnote 13) WG 4 is invited to suggest standards for the determination of PCBs, PCDD/Fs and PAHs in the categories of products listed in the table above or whether the suggested methods are appropriate? Inorganic fertilisers are in principle not concerned. However, WG 4 should reflect on whether Thomas slag (inorganic fertiliser as by-product of the steel industry) should also be tested for the presence of PCBs, PCDD/Fs or PAHs as mentioned during the last meeting of WG 2. How many congeners should be determined for PCDD/Fs? 13 Benzo(a)pyrene, benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(g,h,i) perylen, fluoranthene, indeno(1,2,3-c,d)pyrene. 12 Can WG 4 also suggest relevant analytical methods for the identification of possible marker(s) (e.g. benzo(a) pyrene for PAHs) for the categories of products listed in the table above? 7.4. Pathogens WG 3 agreed that microbiological standards for microbial pathogens should be set for organic fertilisers, soil improvers and growing media. Proposed maximum Organic fertilisers limit values Soil improvers growing media Salmonella Absence sample ISO 6579 E.Coli 1000 CFU/g ISO 11866-2 ISO 11866-2 Enterococcae 1000 CFU/g EN ISO 7899-1 EN ISO 7899-114 in 25 g ISO 6579 and WG 4 is invited to confirm that the methods mentioned above are appropriate for organic fertilisers, soil improvers and growing media? 7.5. Plant propagules The EoW criteria for biowaste suggest a limit value of 2 viable weed seeds/liter of organic soil improver. TC 223 needs to work on revising the horizontal standard mentioned below. Proposed maximum Organic fertilisers limit values Plant propagules 2 viable weed seeds FprCEN /TS 1620115 Soil improvers growing media and FprCEN /TS 16201 WG 4 should consider whether FprCEN/TS 16201 is appropriate for the determination of viable plant seeds in soil improvers, growing media and organic fertilisers. 7.6. Inert materials and impurities At the last meeting of WG 3, FEAD proposed the determination of physical impurities Proposed maximum Organic fertilisers limit values Soil improvers growing media Glass > 2mm 14 15 Enterococceae are not routinely analysed in growing media. E.Coli is standard Sludge, treated biowaste and soil – determination of viable plant seeds and propagules 13 and Stone Metal residues 2mm > All kind of plastic residues > 5mm This requirement is awaiting the results of the discussions on the End of Waste criteria, which are under development by the Commission (DG JRC). If only certain source-separate waste streams will become eligible to limit the number of contaminants, a requirement for inert materials might become obsolete. 8. RECORD KEEPING 8.1. Verification of compliance after the placing on the market Article 29 of Regulation (EC) No 2003/2003 specifies that compliance with the provisions of the Regulation may be verified only by means of sampling and analysis methods established in accordance with Annex III and IV and taking into account the tolerances of Annex II. However, the provisions of the current Regulation are less prescriptive as regards the type of records to be maintained by producers to allow verification of the compliance of products by market surveillance authorities. The frequency with which tests need to be repeated, as well as measures that are designed to ensure that the fertiliser put on the market is identical with the fertiliser tested are not detailed. As a remedy to this loophole, the future legislation could describe the frequency of controls in relation to the volume of material produced and the type of analysis as described in the table below as an example for soil improvers: Type of analysis Tonnage band for organic soil improvers 0 to 350 t/year 350 to 3500 t/year 3500 to 7000t/year Above 7000 t/year 2/year 3/year 4/year 4/year 1/year 2/year 3/year 4/year Declared nutrients Heavy metals Organic contaminants 1/year Pathogens 1/year Inert and impurities 1/year (Source French norm NF U 44-051) 1/year 2/year 2/year 1/year 3/year 2/year 2/year 4/year 3/year Which type of records (e.g. registration of input materials, full traceability during the production process of the ingredients used, frequency of controls by the operators…) should be kept by manufacturers/ importers for inspection? 14 Are the proposed frequencies of testing proposed in the table above appropriate for soil improvers? Should these measures apply in a similar way across the various product categories (not only for SI)? Do we need to be more or less strict in the frequency of controls for other categories? 8.2. Report for products presenting serious risks – safeguard clause In 2004, the RAPEX system for information about dangerous products was created when the revised General Product Safety Directive came into force. This system has proved its effectiveness and efficiency in the field of consumer product safety. The new framework for market surveillance established by Regulation (EC) No 765/2008 foresees in its Article 22 the establishment of a rapid exchange information system about products presenting serious risks and makes a direct reference to the RAPEX system. However, the Regulation specifies that the system should be extended to: – all products covered by EU laws whether they are consumer products or products intended for professional uses. – Risks to public interests covered by any relevant EU legislation (e.g. the environment, the security at the workplace, the consumption of energy etc.). Therefore, the new GRAS-RAPEX system will include those changes and the future legislation on fertilisers could refer to this platform for information exchange about products posing serious risks. Article 15 (safeguard clause) of Regulation (EC) No 2003/2003 obliges Member States to inform the Commission about any restrictive measure they intend to take for fertilisers that although complying with the provisions of the current legislation, present serious risks. In order to ensure that the Member States are informed of the real emergency situation for the safety of products, the new GRAS-RAPEX could be an appropriate tool for Member States notifications in relation with the safeguard clause. 8.3. Report for non-complying products that do not present serious risks and/or non-performing products Article 23 of Regulation (EC) No 765/2008 requires the Commission to develop and maintain an IT tool for the purposes of the general exchange of information between Member States and the Commission relating to market surveillance activities. The ICSMS16 database should contain information on the controls performed by the Member States to verify the compliance of the fertilisers placed on the market. Nonconformities should be reported in this database. For non-performing products (namely products that although complying with the quality criteria mentioned above may be regarded as ineffective), the ICSMS platform could also be an appropriate tool for the exchange of information between Member States. 16 The internet-supported information and communication system for the pan-European market surveillance. 15