Decree No. 309 / 2021 Coll.
Ordinance on collection and chemical and biological analysis of fertiliser samples
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Order
Effective from 01.10.2021
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01.10.2021
27.08.2021
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309
DECLARATION
of 19 August 2021
on collection and chemical and biological analyses of fertiliser samples
The Ministry of Agriculture shall determine, pursuant to Article 4 (9) of Act No. 156 / 1998 Coll., on fertilisers, soil aids, plant biostimulants and substrates, and on agrochemical testing of agricultural soils (Fertilizer Act), as amended by Act No. 9 / 2009 Coll., Act No. 61 / 2017 Coll. and Act No. 299 / 2021 Coll.:
Sampling of fertilisers, soil aids, plant biostimulants and substrates
For the purposes of this decree:
(a) lots of such quantities of fertilisers, soil improvers, plant biostimulants, substrates (hereinafter referred to as "products"), which constitute a single whole with their characteristics, labelling and spatial layout;
(b) a partial sample of the quantity of the product obtained by a single sample of the lot;
(c) by aggregate sample, a set of individual incremental samples taken from the lot;
(d) by a reduced aggregate sample, a subquantity of the aggregate sample with the same composition as the aggregate sample; and
(e) by the final sample, the incremental quantity of the aggregate or reduced aggregate sample required for the test.
The sampling of products shall include the taking of incremental samples, the creation of aggregate and final samples, the storage and labelling of final samples.
(1) Sampling aids are used which are meant in the case of:
(a) the rigid products, the mechanical devices of the manufacturer, directly intended to be used for the sampling of products in motion or moving during sampling, as well as samples, in particular tubular, flat blades and spiral samples, suitable for the size of the lot and the product particles; and
(b) liquid products of the sampling pump, the lower-end sampling tube and the sampling vessel.
(2) A divider is used to divide the sample and, exceptionally, the sample is divided by quarts.
(3) The sampling aids and working areas must be clean and dry. They may not be of material that affects the quality of the product sample.
(1) If the lot is so large or stored that it is not possible to take individual incremental samples from it, only the part thereof shall be considered a lot which allows the incremental samples to be taken.
(2) In the case of products intended solely for consumer use (1), the contents of a single original package, which at the same time constitutes an aggregate sample, are considered a lot. Where the weight of the contents of the package is insufficient, the number of packages shall be taken to meet the requirement of weight of the final sample.
(1) The weight of the incremental sample taken from bulk products, packaged products with a weight of more than 50 kg or more than 50 l shall be at least 0,2 kg except for the incremental sample taken by mechanical equipment from the moving product.
(2) The minimum number of incremental samples by product type and batch size is given in Annex 1 to this Regulation.
(3) One aggregate sample shall be produced from incremental samples taken from one lot. In the same way, 2 aggregate samples shall be produced if, for products which consist of more than 1 type-determining component and which have a tendency to break the mixture, a tube sampling device is used for sampling.
(4) The aggregate sample shall be reduced to a final maximum weight of 4 kg. The aggregate sample of one-component ammonium nitrate products with a nitrate nitrogen content of more than 28% for which the explosive tests are carried out at the same time shall not exceed 75 kg.
(1) A minimum of 3 final samples shall be produced from each aggregate sample or from each reduced aggregate sample.
(2) The weight of the final sample of solid products is at least 1 kg, liquid products at least 0,5 kg.
(3) The weight of the final sample of solid organic fertilisers and substrates is at least 2 kg.
(4) The final sample of liquid organic fertilisers and liquid fertilisers must contain at least 0,1 kg dry matter.
(5) The weight of the final sample of consumer packages is at least 0,25 kg.
(6) For packages of up to 1 kg, the contents of the package or their set shall be the final sample.
(7) The weight of the final sample of single-component ammonium nitrate products with a nitrate nitrogen content of more than 28% for which explosive tests are carried out at the same time is not more than 25 kg.
(1) Partial samples shall be taken at random from the whole lot. The mass or volume of incremental samples taken shall be the same.
(2
(3) A partial sample shall be taken from the packaging of a solid product of 50 kg or less by means of a tube sampling device or by repeatedly dividing the whole contents of the package into dividers.
(4) A partial sample shall be taken from the liquid product after mixing, emulsions, suspensions and cashew mixtures only from the stream of the flowing product.
(5) If it contains an aggregate sample of clumps, they shall be crushed separately and reassembled with the aggregate sample. The original aggregate sample shall be used to determine the particle size.
(6) When sampling for the determination of microbiological parameters, five samples weighing between 0,1 and 0,2 kg randomly distributed over the sampled unit shall be taken. Each sample so collected for microbiological analysis shall be the final sample. Individual final samples shall not be mixed.
(7) The final sample shall be kept for a period of 12 months from the completion of the sampling protocol in clean, dry, moisture-free, airtight and closed packages made of materials which do not affect their quality. In the case of a final sample for microbiological analysis, the closing packaging with the final sample immediately after closure shall be inserted into the refrigerating liners thermoxes. Final samples of consumer fertilisers weighing up to 3 kg shall be kept in the original package. The label shall be firmly affixed to the packaging of the final sample with the following particulars:
(a) the name of the product;
(b) the name and surname of the inspector;
(c) date and
(d) the protocol number.
(8) The final sample shall be kept by the Central Audit and Examination Institute of the Agricultural Institute (hereinafter referred to as the Institute). The Institute shall draw up a sampling report for each final sample containing the following information:
(a) the name and address of the Institute, the inspection department;
(b) the name and surname of the inspector;
(c) identification details of the manufacturer, importer or supplier;
(d) name of product,
(e) forms of nutrients and their solubility;
(f) size, type of lot and batch number,
(g) the arrangements for putting the product into circulation;
(h) type of packaging;
(i) the method of storage of the product;
(j) the place, address and date of sampling;
(k) the relevant facts found during sampling;
(l) identification of documents and other materials; and
(m) the protocol number.
(9) The Institute shall publish on its website details of the sampling and storage methods.
Chemical analyses and biological tests
Chemical analyses of the products shall be carried out using the procedures set out in Annex 2 to this Decree.
(1) Biological testing shall be carried out by the Institute in the field, greenhouse, growing hall or laboratory.
(2) Biological tests shall be carried out as follows:
(a) the product shall be verified on the crops and at the doses for which it is intended;
(b) the nature and the declared use of the product derive from the selection of the type of test and the site, the length of the verification, the variants of the test and the parameters evaluated;
(c) at least one comparative control option shall be included in the biological tests;
(d) in biological tests, the certified variants shall be repeated at least four times.
(3) Biological tests in the form of microbiological tests shall be carried out in accordance with the principles set out in Annex 2 to this Decree, point 1 (c).
(4) Biological tests in the form of ecotoxicological tests shall be carried out as follows:
(a) the product shall be verified using standardised tests with micro-organisms, invertebrates and plants in order to affect more food chain levels;
(b) the product is tested at different concentration levels based on the highest recommended dose specified by the manufacturer;
(c) at least 1 control comparative variant shall be included in ecotoxicological tests; and
(d) in ecotoxicological tests, each concentration level shall include at least 3 repetitions.
Transitional provision
Chemical and biological testing of products started before the date of entry into force of this Order shall be completed in accordance with Decree No. 273 / 1998 Coll., as effective before the date of entry into force of this Order.
Repeal
They shall be deleted:
1. Decree of the Ministry of Agriculture No. 273 / 1998 Coll., on collection and chemical analysis of fertiliser samples.
2. Decree of the Ministry of Agriculture No. 475 / 2000 Coll., amending Decree of the Ministry of Agriculture No. 273 / 1998 Coll., on collection and chemical analysis of fertiliser samples.
Efficacy
This Decree shall take effect on 1 October 2021.
Minister:
Ing. Toman, CSc., v. r.
Příloha č. 1
Annex No. 1 to Decree No. 309 / 2021 Coll.
Minimum number of incremental samples by product type and batch size
| druh výrobku a velikosti | minimální počet |
| TUHÉ VÝROBKY | |
|---|---|
| volně ložené tuhé výrobky a v obalech nad 50 kg | |
| počet vzorků | |
| 7 | |
| druhá odmocnina z dvacetinásobku hmotnosti | |
| 40 | |
| balené tuhé výrobky v obalech do obsahu 50 kg | |
| balení s obsahem větším než 1 kg | počet balení |
| do 4 kusů | všechna |
| 5 až 16 kusů | 4 |
| 17 až 400 kusů | druhá odmocnina z počtu balení, zaokrouhleno na celá čísla |
| nad 400 kusů | 20 |
| balení s obsahem do 1 kg | 3 |
| KAPALNÉ VÝROBKY | |
| volně ložené kapalné výrobky a v obalech nad 50 kg | |
| počet vzorků | |
| 7 | |
| druhá odmocnina z dvacetinásobku hmotnosti | |
| 40 | |
| balené kapalné výrobky v obalech do obsahu 50 kg | |
| balení s obsahem větším než 1 kg | počet balení |
| do 4 kusů | všechny |
| 5 až 16 kusů | 4 |
| 17 až 400 kusů | druhá odmocnina z počtu balení, zaokrouhleno na celá čísla |
| nad 400 kusů | 20 |
| balení s obsahem do 1 kg | 3 |
Příloha č. 2
Annex No 2 to Decree No. 309 / 2021 Coll.
Chemical analysis procedures
1. Preparation of samples for analysis
Modification of the final sample delivered to the laboratory shall be a sequence of operations, in particular sifting, dilution and homogenisation, carried out in such a way that:
(a) even the smallest of the samples envisaged by the analytical methods are representative of the final sample;
(b) the grain size of the fertiliser has not been changed in such a way that the solubility in the various leaching agents is significantly affected;
(c) the microbiological tests comply with the principles set out in AHEM 7 / 2001 (Acta hygienica, epidemiologica et microbiologica) and AHEM 1 / 2008 (Acta hygienica, epidemiologica et microbiologica).
2. Nitrogen
2.1 Determination of ammonium nitrogen
2.1.1 Determination of ammonium nitrogen by distillation method
Ammonia is removed by excess of sodium hydroxide, distilled, collected in an appropriate intake solution and subsequently determined in titration.
2.1.2 Determination of ammonium nitrogen by formaldehyde method
Ammonium ions in an aqueous solution are converted by reaction with formaldehyde to hexamethylenetetramine, releasing equivalent amounts of oxonium ions. These are determined directly by titrated sodium hydroxide solution to phenolphthalein.
2.1.3 Determination of ammonium nitrogen by spectrophotometric method
The nitrogen in the ammonium form contained in the sample reacts with hypochlorite and salicylate to create a blue colour (indophenol salicylate analogue). The colour intensity shall be measured spectrophotometric at 660 nm.
2.2 Determination of ammonium and nitrate nitrogen according to Devard
Nitrates and possibly present nitrites in a highly alkaline environment are reduced by hydrogen in the state of birth, resulting in a reaction of Devard's sodium hydroxide alloy. Ammonia produced, together with the sodium hydroxide surplus initially present, is distilled, collected in a suitable intake solution and subsequently determined by titration.
2.3 Determination of total nitrogen (sum of inorganic and organically bonded nitrogen)
2.3.1 Determination of total nitrogen in nitrate-free nitrogen lime
The sample shall be broken down by the Kjeldahl method by boiling with sulphuric acid in the presence of a copper catalyst. Ammonium sulphate produced is extracted with sodium hydroxide, distilled, collected in an appropriate intake solution and subsequently titrated in it.
2.3.2 Determination of total nitrogen in nitrogen lime with nitrate
First, nitrates shall be reduced to ammonia by powder iron and tin chloride and the sample shall be further distributed using the Kjeldahl method as in paragraph 2.3.1.
2.3.3 Determination of total nitrogen in urea
The urea nitrogen is converted by boiling the sample with sulphuric acid into ammonium sulphate. Ammonia is distilled from the alkaline environment, collected in an appropriate intake solution and subsequently determined in titration.
2.3.4 Determination of total nitrogen by Jodlbauer
Nitrates in the sulphuric acid environment reduce phenol to p-nitrophenol, which is then reduced by zinc to p-aminophenol. This, together with the organic component of the sample, is decomposed by boiling sulphuric acid in the presence of a catalyst, whereby organically bound nitrogen is zineralised. The produced ammonium nitrogen is distilled together with the originally present ammonium nitrogen after alkalisation, collected in an appropriate intake solution and subsequently determined by titration.
2.3.5 Determination of total nitrogen by Dumas (elementary analysis)
The samples are burned in a high temperature oxygen stream. The resulting mixture of gases is separated from nitrogen, carbon and sulphur and catalytic converted into N2, CO2 and SO2 forms which are appropriately detected.
2.4 Determination of cyanamide nitrogen
Cyanamide is precipitated from the solution as a silver salt which is decomposed by the Kjeldahl method and the nitrogen is determined as in paragraph 2.3.1.
2.5 Determination of biurete in urea
2.5.1 Determination of biurete in urea spectrophotometric
Biuret forms a blue-violet water-soluble complex in an alkaline environment in the presence of sodium potassium tartrate with bivalent copper, whose absorbance is measured at a wavelength of 546 nm.
2.5.2 The determination of biurete in urea by high performance liquid chromatography (HPLC) Biuret is determined in an aqueous solution using HPLC with detection at 195 nm wavelength.
2.6 Determination of different forms of nitrogen side by side
Determination of different forms of nitrogen side by side in fertilisers with ammonium, nitrate, urea and cyanamide nitrogen
2.6.1 Determination of soluble and insoluble nitrogen (sum). Determination shall be made only if cyanamide nitrogen is also present from the above forms of nitrogen.
2.6.1.1. In the absence of nitrates, the sample is mineralised directly by Kjeldahl as in paragraph 2.3.1.
2.6.1.2. In the presence of nitrates, the sample shall be mineralized by the Kjeldahl method (paragraph 2.3.1) until reduced by powdered iron and tin chloride.
Note: Ammonium, nitrate and urea nitrogen (including biureth) are excreted from fertilizers at laboratory temperature, calcium cyanide is hydrolysed (on Ca (HCN2) 2) and urea-aldehyde condensates remain undissolved. If the insoluble nitrogen content is found to be more than 0,5%, the presence of urea-aldehyde condensates or other forms of insoluble nitrogen may be considered. In this case, the analytical procedure described is inappropriate without modification.
2.6.2 Determination of soluble forms of nitrogen in different proportions of a single sample solution:
2.6.2.1 Solvent total nitrogen
2.6.2.1.1 in the absence of nitrates, by direct degradation using the Kjeldahl method, as in paragraph 2.3.1.
2.6.2.1.2 in the presence of nitrates by decomposing the aliquot of the sample solution by the Jodlbauer method, paragraph 2.3.4.
In both cases, the ammonia produced shall be determined by the distillation method described in paragraph 2.1.1.
2.6.2.2 Nitrate nitrogen
2.6.2.2.1 of the difference: in the absence of calcium cyanide
Difference between 2.6.2.1.2 and the sum of ammonium and urea nitrogen (2.6.2.3.2 or 2.6.2.3.3 + 2.6.2.4).
2.6.2.2.2. Difference: in the presence of calcium cyanide
Difference between 2.6.2.1.2 and the sum (2.6.2.3.2 or 2.6.2.3.3 + 2.6.2.4 + 2.6.2.5).
2.6.2.2.3 Direct determination: Nitrate nitrogen determination by spectrophotometric method Nitrates absorb in the ultraviolet spectrum area at 210 nm wavelength. After the nitrate reduction in the nitrate leaching to nitrite, a second measurement at 210 nm shall be made and the nitrogen content expressed as nitrate nitrogen (N-NO3) shall be calculated from the difference of the measured values.
2.6.2.3 Ammonium nitrogen
2.6.2.3.1 in the presence of ammonium or ammonium and nitrate nitrogen alone, using the distillation method described in paragraph 2.1.1.
2.6.2.3.2 in the presence of Urea or Cyanamide Nitrogen by gasification of ammonia by cooling from a weak alkaline environment through air. The ammonia is bound in a known volume of a volumetric sulphuric acid solution and determined as in the distillation method according to paragraph 2.1.1.
2.6.2.3.3 Direct determination: The determination of ammonium nitrogen by the spectrophotometric method Nitrogen in the ammonium form contained in the sample reacts with hypochlorite and salicylate to create a blue colour (salicylate analogue of indophenol). The colour intensity shall be measured spectrophotometric at 660 nm.
2.6.2.4. Urea nitrogen
2.6.2.4.1. Transformation of urea by urease into ammonia, to be determined by procedure 2.6.3.3.1. At the same time, the content of free ammonia present without the addition of urease according to paragraph 2.6.3.3.1 shall be determined in the sample. Urea nitrogen content 2.6.2.4 is calculated from the difference (2.6.2.4.1 - 2.6.3.3.1)
2.6.2.4.2 Determination of urea (amidic) nitrogen using high performance liquid chromatography (HPLC).
Urea nitrogen is determined in HPLC extract using detection at 195 nm wavelength.
2.6.2.4.3. Calculation of differences by table
| Případ | N-NO3- | N-NH4+ | N-CN22- | N-CO(NH2)2 |
|---|---|---|---|---|
| 1 | přítomen | přítomen | přítomen | 2.6.2.1.2 nebo 2.3.5 – (2.6.2.3.2 nebo 2.6.2.3.3 + 2.6.3.2.2 + 2.6.2.5) |
| 2 | nepřítomen | přítomen | přítomen | 2.6.2.1.1 – (2.6.2.3.2 nebo 2.6.2.3.3 + 2.6.2.5) |
| 3 | nepřítomen | přítomen | nepřítomen | 2.6.2.1.1 – (2.6.2.3.2 nebo 2.6.2.3.3) |
| 4 | přítomen | přítomen | nepřítomen | 2.6.2.1.2 – (2.6.2.3.2 nebo 2.6.2.3.3 + 2.6.3.2.2) |
2.6.2.5.4 Determination of nitrogen forms by direct methods
2.6.2.5. Cyanamide nitrogen by precipitating as silver salt and determining nitrogen in the precipitate according to the Kjeldahl method. The cyanamide nitrogen is transferred to the diluted acetic acid solution, then precipitated from the ammonia environment as a silver salt and in the precipitate determined by the Kjeldahl method as in paragraph 2.3.1.
2.6.3 Determination of different forms of nitrogen side by side in ammonium, nitrate and urea nitrogen fertilisers in different proportions of a single sample solution:
2.6.3.1 Total nitrogen
2.6.3.1.1 in the absence of nitrates by direct degradation according to the Kjeldahl method, as in paragraph 2.3.1.
2.6.3.1.2 in the presence of nitrates after decomposition of the aliquot of the sample solution by the Jodlbauer method, according to paragraph 2.3.4.
In both cases, the ammonia produced shall be determined by the distillation method described in paragraph 2.1.1.
2.6.3.2 Nitrate nitrogen
2.6.3.2.1 of the difference between 2.6.3.1.2 and the sum of soluble ammonium and urea nitrogen (2.6.3.3 + 2.6.3.4).
2.6.3.2.2 Direct determination: Determination of nitrate nitrogen by spectrophotometric method
Nitrates absorb the UV spectrum at a wavelength of 210 nm. After the nitrate reduction in the nitrate leaching to nitrite, a second measurement at 210 nm shall be made and the nitrogen content expressed as nitrate nitrogen (N-NO3) shall be calculated from the difference of the measured values.
2.6.3.3 Ammonium nitrogen
2.6.3.3.1 by sealing ammonia for cold from a weak alkaline environment by pushing air. The ammonia is bound in a known volume of the volumetric sulphuric acid solution and determined as in the distillation method in paragraph 2.1.1.
2.6.3.3.2 Direct determination: Determination of ammonium nitrogen by spectrophotometric method
The nitrogen in the ammonium form contained in the sample reacts with hypochlorite and salicylate to create a blue colour (indophenol salicylate analogue). The colour intensity shall be measured spectrophotometric at 660 nm.
2.6.3.4. Urea nitrogen
2.6.3.4.1 by converting urea by means of urease into ammonia, which is titrated with a graduated hydrochloric acid solution.
2.6.3.4.2 Determination of urea (amidic) nitrogen using high performance liquid chromatography (HPLC)
Urea nitrogen is determined in HPLC extract with a wave detection of 195 nm.
2.6.3.4.3. Calculation of differences by table
2.7 Determination of urea (amidical) nitrogen
2.7.1 Determination of urea (amidic) nitrogen by spectrophotometric method
Urea reacts in an acidic environment with 4-dimethylaminobenzaldehyde to produce a yellow coloured condensation product whose absorbance is measured at a wavelength of 420 nm. The method is intended for selective determination of urea (amidic) nitrogen in both single and compound fertilisers. It cannot be used for fertilisers containing or releasing substances that also form colour compounds with 4-dimethylaminobenzaldehyde, such as cyanamide, thiourea, primary and secondary aromatic amines, hydrazine and derivatives with one free amino group, semicarbazides.
2.7.2 Determination of urea (amidic) nitrogen using high performance liquid chromatoqraphy (HPLC)
The urea nitrogen is determined in an aqueous solution using HPLC reverse phase using detection at a wavelength of 200 nm.
2.8 Determination of urea-aldehyde condensates
Note: Urea-aldehydic condensates are nitrogen-soluble in water. Their different solubility in cold and hot water is used to determine them. The water is replaced by dampening solutions which prevent hydrolysis of condensates to urea and aldehyde while ensuring stable solubility conditions during leaching.
2.8.1 Determination of total urea-aldehyde condensates by subtracting individual forms of nitrogen from total nitrogen
2.8.2 Determination of urea-aldehyde condensates soluble in cold water (RSV)
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Regulation Information
| Citation | Decree No. 309 / 2021 Coll., on collection and chemical and biological analyses of fertiliser samples |
|---|---|
| Regulation Type | Order |
| Author | - |
| Collection | Code of Laws |
| Date of Promulgation | 27.08.2021 |
|---|---|
| Effective from | 01.10.2021 |
| Effective until | - |
| Status | Valid |
Legal Areas:
Administrative law
Agriculture
The regulation text is for informational purposes only.
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