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(1) These Regulations may be cited as the Fertilisers (Sampling and Analysis) (Amendment) Regulations 1994 and shall come into force on 17th February 1994.
(2) In these Regulations, “the principal Regulations ” means the Fertilisers (Sampling and Analysis) Regulations 1991 .
The principal Regulations are hereby further amended in accordance with regulations 3 and 4 below.
In paragraph (2) of regulation 6, after the words “Groups 1(a), 1(b) and 2 of Section C”, there shall be added the words “Section D”.
In Part I of Schedule 2—
(1) in paragraph 3, after item 26 there shall be added the provisions set out in Schedule 1 to these Regulations;
(2) in paragraph 7 of method 10, (“DETERMINATION OF EXTRACTED PHOSPHORUS”), for the figure “0.03074” there shall be substituted the figure “0.032074”;
(3) after the provisions relating to method 26, (“DETERMINATION OF THE SODIUM EXTRACTED”), there shall be added the provisions set out in Schedule 2 of these Regulations.
(a) Extraction of total trace elements
(b) Extraction of water-soluble trace elements
(c) Removal of organic compounds from fertiliser extracts
(d) Determination of trace elements in fertiliser extracts by atomic absorption spectrophometry (general procedure)
(e) Determination of boron in fertiliser extracts by means of spectrophotometry with azomethine-h
(f) Determination of cobalt in fertiliser extracts by atomic absorption spectrophotometry
(g) Determination of copper in fertiliser extracts by atomic absorption spectrophotometry
(h) Determination of iron in fertiliser extracts by atomic absorption spectrophotometry
(i) Determination of manganese in fertiliser extracts by atomic absorption spectrophotometry
(j) Determination of molybdenum in fertiliser extracts by spectrophotometry of a complex with ammonium thiocyanate
(k) Determination of zinc in fertiliser extracts by atomic absorption spectrophotometry
This method defines the procedure for extracting the following trace elements: total boron, total cobalt, total copper, total iron, total manganese, total molybdenum and total zinc.The aim is to carry out the minimum number of extractions, making use wherever possible of the same extract to determine the total level of each of the trace elements listed above.
This method defines the procedure for extracting water-soluble forms of the following trace elements: boron, cobalt, copper, iron, manganese, molybdenum and zinc.The aim is to carry out the minimum number of extractions, making use wherever possible of the same extract to determine the level of each of the trace elements listed above.
This method defines a procedure for removing organic compounds from fertiliser extracts.
This method defines a general procedure for determining the levels of certain trace elements in fertiliser extracts by atomic absorption spectrophotometry.
This method describes a procedure for determining boron in fertiliser extracts.
This method describes a procedure for determining cobalt in fertiliser extracts.
This method describes a procedure for determining copper in fertiliser extracts.
This method describes a procedure for determining iron in fertiliser extracts.
This method describes a procedure for determining manganese in fertiliser extracts.
This method describes a procedure for determining molybdenum in fertiliser extracts.
This method describes a procedure for determining zinc in fertiliser extracts.
This procedure is applicable to all fertilisers in Groups 1(a), 2(a) and 3(a) of Section A, Groups 1 to 4 of Section B, Groups 1(a) and 2 of Section C, Section D, and Section E, of the table in Schedule 1 of the Fertilisers Regulations 1991 , containing one or more of the following trace elements: boron, cobalt, copper, iron, manganese, molybdenum and zinc.It is applicable to each trace element, the declared content of which is less than or equal to 10%.
This procedure is applicable to all fertilisers contained in Groups 1(a), 2(a) and 3(a) of Section A, Groups 1 to 4 of Section B, Groups 1(a) and 2 of Section C, Section D, and Section E of the Table in Schedule 1 of the Fertilisers Regulations 1991, containing one or more of the following trace elements: boron, cobalt, copper, iron, manganese, molybdenum and zinc.It is applicable to each trace element, the declared content of which is less than or equal to 10%.
This procedure is applicable to analysing samples of all fertilisers extracted by Methods 27a and 27b for which a declaration of the total and/or water-soluble element is required.
Note: The presence of small quantities of organic matter usually does not affect determinations by means of atomic absorption spectrophotometry.
This procedure is applicable to analysing samples of all fertilisers extracted by Methods 27a and 27b for which a declaration of the total and/or water-soluble element is required.
Adaptations of this procedure for the various trace elements are detailed in the methods defined specifically for each element.
Note: In most cases the presence of small quantities of organic matter will not affect determinations by atomic absorption spectrophotometry.
This procedure is applicable to analysing samples of all fertilisers extracted by Methods 27a and 27b for which a declaration of the total and/or water-soluble boron is required.
This procedure is applicable to analysing samples of all fertilisers extracted by Methods 27a and 27b for which a declaration of the total and/or water-soluble cobalt is required.
This procedure is applicable to analysing samples of all fertilisers extracted by Methods 27a and 27b for which a declaration of the total and/or water-soluble copper is required.
This procedure is applicable to analysing samples of all fertilisers extracted by Methods 27a and 27b for which a declaration of the total and/or water-soluble iron is required.
This procedure is applicable to analysing samples of all fertilisers extracted by Methods 27a and 27b for which a declaration of the total and/or water-soluble manganese is required.
This procedure is applicable to analysing samples of all fertilisers extracted by Methods 27a and 27b for which a declaration of the total and/or water-soluble molybdenum is required.
This procedure is applicable to analysing samples of all fertilisers extracted by Methods 27a and 27b for which a declaration of the total and/or water-soluble zinc is required.
Dissolution in boiling diluted hydrochloric acid.
Note: The extraction is empirical and may not be quantitative depending on the product or the other constituents of the fertiliser.In particular, in the case of certain manganese oxides, the quantity extracted may be substantially smaller than the total quantity of manganese which the product contains.It is the responsibility of fertiliser manufacturers to ensure that the declared content actually corresponds to the quantity extracted under the conditions pertaining to the method.
The trace elements are extracted by shaking the fertiliser in water at 20°C ± 2°C.
Note: The extraction is empirical and may or may not be quantitative.
The organic compounds in an aliquot portion of the extract are oxidized with hydrogen peroxide.
After the extract has been treated where necessary to reduce or eliminate interfering chemical species, the extract is diluted so that its concentration is in the optimum range of the spectrophotometer set to a wave-length suitable for the trace element to be determined.
In an azomethine-H solution, borate irons form a yellow complex, the concentration of which is determined by molecular absorption spectrophotometry at 410 nm.Interfering ions are masked with EDTA.
After suitable treatment and dilution of the extracts, the cobalt content is determined by atomic absorption spectrophotometry.
After suitable treatment and dilution of the extracts, the copper content is determined by atomic absorption spectrophotometry.
After suitable treatment and dilution of the extract, the iron content is determined by atomic absorption spectrophotometry.
After suitable treatment and dilution of the extracts, the manganese content is determined by atomic absorption spectrophotometry.
Molybdenum( V ) forms a complex [MoO(SCN) 5 ] −− in an acid medium with SCN − ions.The complex is extracted with n-butyl acetate. Interfering ions such as those of iron remain in the aqueous phase. The yellow-orange colour is determined by molecular absorption spectrophotometry at 470 nm.
After suitable treatment and dilution of the extracts, the zinc level is determined by atomic absorption spectrophotometry.
(4.1) Diluted hydrochloric acid ( HCl ) solution, approximately 6 m:
Mix 1 volume of hydrochloric acid (ρ = 1.18 g/ml) with 1 volume of water.
(4.2) Concentrated ammonia solution ( NH 4 OH, ρ = 0.88 g/ml).
(4.1) Diluted hydrochloric acid (HCl) solution, approximately 6 M:
Mix 1 volume of hydrochloric acid (ρ = 1.18 g/ml) with 1 volume of water.
(4.1) Diluted hydrochloric acid (HCl) solution, approximately 0.5 M:
Mix 1 volume of hydrochloric acid (ρ = 1.18 g/m) with 20 volumes of water.
(4.2) Hydrogen peroxide solution (30% H 2 O 2 (100 volumes), ρ = 1.11 g/ml), free from trace elements.
(4.1) Diluted hydrochloric acid solution (HCl), approximately 6 M:
Mix one volume of hydrochloric acid (ρ = 1.18 g/ml) with 1 volume of water.
(4.2) Diluted hydrochloric acid solution (HCl), approximately 0.5 M:
Mix one volume of hydrochloric acid (ρ = 1.18 g/ml) with 20 volumes of water.
(4.3) Lanthanum salt solutions (10 g of La per litre).
This reagent is used in the determinations of cobalt, iron, manganese and zinc.It can be prepared either:
(a) with lanthanum oxide dissolved in hydrochloric acid (4.1). Place 11.73 g of lanthanum oxide (La 2 O 3 ) in 150 ml of water in a 1 litre volumetric flask and add 120 ml of 6 m hydrochloric acid (4.1).Allow to dissolve and then make up to 1 litre with water and mix thoroughly.This solution is approximately 0.5 M in hydrochloric acid; or
(b) with solutions of lanthanum chloride, sulphate or nitrate. Dissolve 26.7 g of lanthanum chloride heptahydrate (LaCl 3 . 7H 2 O) or 31.2 g of lanthanum nitrate hexahydrate [La(NO 3 ) 3 .6H 2 O] or 26.2 g of lanthanum sulphate nonahydrate [La 2 (SO 4 ) 3 .9H 2 O] in 150 ml of water, then add 85 ml of 6 mhydrochloric acid (4.1).Allow to dissolve and then make up to 1 litre with water.Mix thoroughly. This solution is approximately 0.5 M in hydrochloric acid.
(4.4) Calibration solutions
For the preparation of these, see the individual method of determination for each trace element.
(4.1) EDTA buffer solution
Place in a 500 ml volumetric flask containing 300 ml of water:
75 g of ammonium acetate (NH 4 OOCCH 3 );
10 g of disodium salt of ethylene diamine tetraacetic acid (Na 2 EDTA);
40 ml of acetic acid (CH 3 COOH, ρ = 1.05 g/ml).
Make up to volume with water and mix thoroughly.The pH of the solution, checked by means of a glass electrode, must be 4.8 ± 0.1.
(4.2) Azomethine-H solution
Place in a 200 ml volumetric flask
10 ml of the buffer solution (4.1);
400 mg of azomethine-H (C 17 H 12 NNaO 8 S 2 );
2 g of ascorbic acid (C 6 H 8 O 6 ).
Make up to volume and mix thoroughly.Do not prepare large quantities of this reagent as it is stable for only a few days.
(4.3) Boron calibration solutions
(4.3.1) Boron stock solution (100 μg/ml)
Dissolve 0.5719 g of boric acid (H 3 BO 3 ) in water in a 1000 ml volumetric flask.Make up to volume with water and mix thoroughly. Transfer to a plastic bottle for storage in a refrigerator.
(4.3.2) Boron working solution (10 μg/ml)
Place 50 ml of stock solution (4.3.1) in a 500 ml volumetric flask. Make up to volume with water and mix thoroughly.
(4.1) Hydrochloric acid solution, approximately 6 M.
See Method 27d (4.1).
(4.2) Hydrochloric acid solution, approximately 0.5 M.
See Method 27d (4.2).
(4.3) Lathanum salt solutions (10 g of La per litre)
See Method 27d (4.3).
(4.4) Cobalt calibration solutions.
(4.4.1) Cobalt stock solution (1,000 μg/ml)
In a 250 ml beaker, weigh to the nearest 0.1 mg, 1 g of cobalt, add 25 ml of 6 M hydrochloric acid (4.1) and heat on a hotplate until the cobalt is completely dissolved.When cool, transfer quantitatively to a 1,000 ml volumetric flask.Make up to volume with water and mix thoroughly.
(4.4.2) Cobalt working solution (100 μg/ml) Place 10 ml of the stock solution (4.4.1) in a 100 ml volumetric flask.Make up to volume with 0.5 M hydrochloric acid solution (4.2) and mix thoroughly.
(4.1) Hydrochloric acid solution, approximately 6 M
See Method 27d (4.1).
(4.2) Hydrochloric acid solution, approximately 0.5 M
See Method 27d (4.2).
(4.3) Hydrogen peroxide solution (30% H 2 O 2 (100 Volumes), ρ = 1.11 g/ml), free from trace elements.
(4.4) Lanthanum salt solutions (10 g of La per litre)
See Method 27d (4.3).
(4.5) Iron calibration solutions.
(4.5.1) Iron stock solution (1,000 μg/ml
In a 500 ml beaker, weigh to the nearest 0.1 mg, 1 g of pure iron wire, add 200 ml of 6 M hydrochloric acid (4.1) and 15 ml of hydrogen peroxide solution (4.3). Heat on a hotplate until the iron is completely dissolved.When cool, transfer quantitatively to a 1,000 ml volumetric flask.Make up to volume with water and mix thoroughly.
(4.5.2) Iron working solution (100 μg/ml)
Place 20 ml of the stock solution (4.5.1) in a 200 ml volumetric flask.Make up to volume with the 0.5 M hydrochloric acid solution (4.2) and mix thoroughly.
(4.1) Hydrochloric acid solution, approximately 6 M
See Method 27d (4.1).
(4.2) Hydrochloric acid solution, approximately 0.5 M
See Method 27d (4.2).
(4.3) Lanthanum salt solutions (10 g of La per litre)
See Method 27d (4.3).
(4.4) Manganese calibration solutions.
(4.4.1) Manganese stock solution (1,000 μg/ml)
In a 250 ml beaker, weigh to the nearest 0.1 mg, 1 g of manganese, add 25 ml of 6 M hydrochloric acid solution (4.1).Heat on a hotplate until the manganese is completely dissolved.When cool, transfer quantitatively to a 1,000 ml volumetric flask.Make up to volume with water and mix thoroughly.
(4.4.2) Manganese working solution (100 μg/ml)
Dilute 20 ml of the stock solution (4.4.1) in the 0.5 M hydrochloric acid solution (4.2) in a 200 ml volumetric flask.Make up to volume with the 0.5 M hydrochloric acid solution (4.2) and mix thoroughly.
(4.1) Diluted hydrochloric acid solution (HCl), about 6 M
See Method 27d (4.1).
(4.2) Copper solution (70 mg/l) in 1.5 M hydrochloric acid
Dissolve 275 mg of copper sulphate (CuSO 4 .5H 2 O) weighed to within 0.1 mg in 250 ml of the 6 M hydrochloric acid solution (4.1) in a 1,000 ml volumetric flask.Make up to volume with water and mix thoroughly.
(4.3) Ascorbic acid solution (50 g/l)
Dissolve 50 g of ascorbic acid (C 6 H 8 O 6 ) in water in a 1,000 ml volumetric flask.Make up to volume with water, mix thoroughly and keep in a refrigerator.
(4.4) n-butyl acetate
(4.5) Ammonium thiocyanate solution, 0.2 M
Dissolve 15.224 g of NH 4 SCN in water in a 1,000 ml volumetric flask. Make up to volume with water; mix thoroughly and store in a dark-coloured bottle.
(4.6) Stannous chloride solution (50 g/l) in 2 m hydrochloric acid
Note: This solution must be perfectly clear and prepared immediately before use.Very pure stannous chloride must be used otherwise the solution will not be clear.
To prepare 100 ml of solution, dissolve 5 g of (SnCl 2 .2H 2 O) in 35 ml of 6 M HCl solution (4.1).Add 10 ml of the copper solution (4.2). Make up to volume with water and mix thoroughly.
(4.7) Molybdenum calibration solutions.
(4.7.1) Molybdenum stock solution (500 μg/ml)
Dissolve 0.920 g of ammonium molybdate [(NH 4 ) 6 Mo 7 O 24 .4H 2 O] weighed to within 0.1 mg in the 6 M hydrochloric acid (4.1) in a 1,000 ml volumetric flask.Make up to volume with 6 M hydrochloric acid and mix thoroughly.
(4.7.2) Molybdenum intermediate solution (25 μg/ml)
Place 25 ml of the stock solution (4.7.1) in a 500 ml volumetric flask.Make up to volume with 6 M hydrochloric acid (4.1) and mix thoroughly.
(4.7.3) Molybdenum working solution (2.5 μg/ml)
Place 10 ml of the intermediate solution (4.7.2) in a 100 ml volumetric flask.Make up to volume with 6 M hydrochloric acid (4.1) and mix thoroughly.
(4.1) Hydrochloric acid solution, approximately 6 M
See Method 27d (4.1).
(4.2) Hydrochloric acid solution, approximately 0.5 M
See Method 27d (4.2).
(4.3) Lanthanum salt solutions (10 g of La per litre)
(4.4) See Method 27d (4.3).
Zinc calibration solutions
(4.4.1) Zinc stock solution (1,000 μg/ml)
In a 1,000 ml volumetric flask dissolve 1 g of zinc powder or flakes weighed to within 0.1 mg in 25 ml of 6 M hydrochloric acid (4.1). When completely dissolved make up to volume with water and mix thoroughly.
(4.4.2) Zinc working solution (100 μg/ml)
In a 200 ml volumetric flask, dilute 20 ml of the stock solution (4.4.1) in 0.5 M hydrochloric acid solution (4.2).Make up to volume with the 0.5 M hydrochloric acid solution and mix thoroughly.
Electric hot plate with variable temperature control.
Note: Where the boron content of an extract is to be determined, do not use borosilicate glassware.As the method involves boiling, teflon or silica is preferable.Rinse the glassware thoroughly if it has been washed in detergents containing borates.
(5.1) Rotary shaker set at between 35 to 40 rpm.
(5.2) pH-meter.
Note: Where the boron content of the extract is to be determined, do not use borosilicate glassware.Teflon or silica is preferable for this extraction.Rinse the glassware thoroughly if it has been washed in detergents containing borates.
The Fertilisers (Sampling and Analysis) (Amendment) Regulations 1994 (legislation.gov.uk, OGL v3.0). Retrieved via LawPlayer, https://lawplayer.com/uk/act/uksi-1994-129
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