The Fertilisers (Sampling and Analysis) Regulations 1996

1Title, commencement and interpretation

2Prescribed amount for the purposes of the definition of sampled portion

3Manner of taking, marking, sealing and fastening up of samples

4Methods of sending part of a sample

5Qualifications of agricultural analysts and deputy agricultural analysts

6Application of the methods of analysis

7Form of certificate of analysis

8Modification of the Agriculture Act 1970

SCHEDULE 1MANNER OF TAKING, MARKING, SEALING AND FASTENING UP OF SAMPLES

PART IDEFINITIONS

PART IIGENERAL INSTRUCTIONS FOR THE TAKING OF SAMPLES

1In the case of fertiliser in containers, only unopened containers...

2The sample shall be taken and prepared as quickly as...

3No sample shall be drawn from any part of the...

4When stones are naturally present in a fertiliser, they shall,...

5An inspector who intends to take a sample in accordance...

6The sampling apparatus shall be made of materials which cannot...

7In the case of a sampling spear its dimensions shall...

8Notwithstanding the provisions of these Regulations, a sampling spear shall...

9Mechanical apparatus may be used for the sampling of moving...

10Apparatus designed to divide the sample into approximately equal parts...

11A sample taken in accordance with the methods described below...

PART IIIQUANTITATIVE REQUIREMENTS

1Sampled portion

2Incremental sample

3Aggregate sample

PART IVTAKING AND PREPARATION OF SAMPLES

1Incremental samples

2Aggregate sample

3Reduced sample

PART VMARKING, SEALING AND FASTENING UP OF THE FINAL SAMPLE

1Each container of a final sample shall be so secured...

2A label shall be attached to the container or receptacle...

3The container or receptacle may also be sealed, or the...

PART VISAMPLING TABLES

SCHEDULE 2METHODS OF ANALYSIS

5Methods of Analysis

1.PREPARATION OF THE SAMPLE FOR ANALYSIS

2.1Solid fertilisers: the preparation of a final sample received at...

2.2Fluid fertilisers: the final sample is mixed by shaking to...

3.1Sample divider (optional).

3.2Sieves with apertures of 0.2 mm and 0.5 mm.

3.3250 ml flasks, stoppered.

3.4Porcelain pestle and mortar or grinder.

4CHOICE OF TREATMENT TO BE USED

4Final samples which must not be ground

4.2Finals samples which must be divided and part of which must be ground

4.3Final samples in respect of which all determinations are carried out on a grounded product

7FLUID FERTILISERS

2.DETERMINATION OF AMMONIACAL NITROGEN

2FIELD OF APPLICATION

4.1Hydrochloric acid solution, 50% (V/V): dilute an appropriate volume of...

4.8Sodium hydroxide solution, 30 g per 100 ml, ammonia free...

4.9Indicator solutions: Mixed indicator: (4.9.1) Solution A: dissolve 1 g...

5.1Distillation apparatus consisting of a round-bottomed flask of suitable capacity...

5.2Rotary shaker, 35 to 40 turns per minute.

6PREPARATION OF SAMPLE

7.2Determination

7.4Control test

8EXPRESSION OF RESULT

TABLE FOR METHOD 2

3a.DETERMINATION OF NITRIC AND AMMONIACAL NITROGEN — ULSCH METHOD

2FIELD OF APPLICATION

6PREPARATION OF SAMPLE

7.1Preparation of the solution

7.2Determination

7.4Control test

8EXPRESSION OF RESULTS

3b.DETERMINATION OF NITRIC AND AMMONIACAL NITROGEN — ARND METHOD

2FIELD OF APPLICATION

6PREPARATION OF SAMPLE

7.1Preparation of the solution for analysis

7.2Determination

7.4Control test

8EXPRESSION OF RESULTS

3c.DETERMINATION OF NITRIC AND AMMONIACAL NITROGEN — DEVARDA METHOD

2FIELD OF APPLICATION

5.1Distillation apparatus consisting of a round bottomed flask of suitable...

6PREPARATION OF THE SAMPLE

7.1Preparation of the solution for analysis

7.2Determination

7.4Control test

8EXPRESSION OF RESULTS

4a.DETERMINATION OF TOTAL NITROGEN IN CALCIUM CYANAMIDE — IN THE ABSENCE OF NITRATE

2FIELD OF APPLICATION

5.1Distillation apparatus. See Method 2.

6PREPARATION OF SAMPLE

7.1Preparation of the solution

7.2Determination

7.4Control test

8EXPRESSION OF RESULT

4b.DETERMINATION OF TOTAL NITROGEN IN CALCIUM CYANAMIDE — IN THE PRESENCE OF NITRATE

2FIELD OF APPLICATION

6PREPARATION OF THE SAMPLE

7.1Preparation of the solution

7.2Determination

7.4Control test

8EXPRESSION OF RESULT

5.DETERMINATION OF TOTAL NITROGEN IN UREA

2FIELD OF APPLICATION

5.1Distillation apparatus. See Method 2.

6PREPARATION OF THE SAMPLE

7.1Preparation of the solution

7.2Determination

7.4Control test

8EXPRESSION OF RESULT

6.DETERMINATION OF CYANAMIDE NITROGEN

2FIELD OF APPLICATION

5.1Distillation apparatus. See Method 2.

5.2500 ml graduated flask (e.g. Stohmann).

5.3Rotary shaker, 35 – 40 turns per minute.

6PREPARATION OF THE SAMPLE

7.1Preparation of the solution for analysis

7.2Determination

7.4Control test

8EXPRESSION OF RESULT

7.DETERMINATION OF BIURET IN UREA

2FIELD OF APPLICATION

5.1Spectrophotometer.

6PREPARATION OF SAMPLE

7.1Preparation of the standard curve

7.2Preparation of solution for analysis

7.3Determination

8EXPRESSION OF RESULTS

8a.DETERMINATION OF DIFFERENT FORMS OF NITROGEN IN THE SAME SAMPLE — IN THE PRESENCE OF CYANAMIDE NITROGEN

2FIELD OF APPLICATION

3.1Total soluble and insoluble nitrogen

3.2Forms of soluble nitrogen

4.1Potassium sulfate.

4.2Iron powder, reduced with hydrogen (the prescribed quantity of iron...

4.3Potassium thiocyanate.

4.4Potassium nitrate.

4.5Ammonium sulfate.

4.7Sulfuric acid solution: dilute an appropriate volume of sulfuric acid...

4.8Sulfuric acid, 0.1 M solution.

4.9Sodium hydroxide solution, 30 g per 100 ml, ammonia free....

4.10Sodium or potassium hydroxide, 0.2 M solution, free from carbonates....

4.11Stannous chloride solution: Dissolve 120 g of stannous chloride (SnCl2.2H2O)...

4.12Sulfuric acid, concentrated (p=1.84 g/ml).

4.13Hydrochloric acid solution: dilute an appropriate volume of hydrochloric acid...

4.14Glacial acetic acids.

4.15Sulfuric acid solution, approximately 30% (W/V) H2SO4.

4.16Ferrous sulfate, crystalline, FeSO4.7H2O

4.17Sulfuric acid, 0.05 M solution.

4.18Octan-1-ol.

4.19Potassium carbonate, saturated solution.

4.20Sodium or potassium hydroxide, 0.1 M solution, free from carbonate....

4.21Barium hydroxide, saturated solution.

4.22Sodium carbonate solution, 10 g per 100 ml.

4.23Hydrochloric acid, 2 M solution.

4.24Hydrochloric acid, 0.1 M solution.

4.25Urease solution: Suspend 0.5 g of active urease in 100...

4.26Xanthydrol solution, 5 g per 100 ml in ethanol or...

4.27Copper oxide (CuO): 0.3 to 0.4 g per determination or...

4.28Anti-bump granules washed in hydrochloric acid and ignited.

4.29Indicator solutions: (4.29.1) Mixed indicator solution: Solution A: dissolve 1...

4.30Indicator papers: Litmus, bromothymol blue (or other papers sensitive in...

4.31Ethanol or methanol: solution 95%.

5.1Distillation apparatus. See Method 2.

5.2Apparatus for the determination of ammoniacal nitrogen 7.2.5.3. An example...

5.3Apparatus for the estimation of urea nitrogen (7.2.6.1). It consists...

5.4Rotary shaker, 35 – 40 turns per minute.

5.6Laboratory oven.

5.7Sintered glass crucibles, diameter of pores 5 to 15 microns....

6PREPARATION OF THE SAMPLE

7.1Total soluble and insoluble nitrogen

7.2Forms of soluble nitrogen

8VERIFICATION OF RESULTS

8.1In certain cases, a difference may be found between the...

8.2Before each analysis, check that the apparatus is working properly...

8b.DETERMINATION OF DIFFERENT FORMS OF NITROGEN IN THE SAME SAMPLE — IN THE ABSENCE OF CYANAMIDE NITROGEN

2FIELD OF APPLICATION

3.1Total soluble nitrogen

3.2Total soluble nitrogen except nitric nitrogen, by Kjeldahl digestion after...

3.3Nitric nitrogen, by difference: between 3.1.2 and 3.2 and/or between...

3.4Ammoniacal nitrogen, by cold distillation of a weak alkaline solution;...

3.5Ureic nitrogen, either: (3.5.1) By conversion using urease, into ammonia,...

4.1Potassium sulfate.

4.2Iron powder, reduced with hydrogen (the prescribed quantity of iron...

4.3Potassium nitrate.

4.4Ammonium sulfate.

4.6Sulfuric acid, 0.1 M solution.

4.7Sodium hydroxide solution 30 g per 100 ml, ammonia free....

4.8Sodium or potassium hydroxide, 0.2 M solution, free of carbonates....

4.9Sulfuric acid (p=1.84 g/ml).

4.10Hydrochloric acid solution: dilute an appropriate volume of hydrochloric acid...

4.11Glacial acetic acid.

4.12Sulfuric acid solution, approximately 30% (W/V) H2SO4.

4.13Ferrous sulfate, crystalline FeSO4.7H2O.

4.14Sulfuric acid, 0.05 M solution.

4.15Octan-1-ol.

4.16Potassium carbonate, saturated solution.

4.17Sodium or potassium hydroxide, 0.1 M solution.

4.18Barium hydroxide, saturated solution.

4.19Sodium carbonate solution, 10 g per 100 ml.

4.20Hydrochloric acid, 2 M solution.

4.21Hydrochloric acid, 0.1 M solution.

4.22Urease solution: suspend 0.5 g active urease in 100 ml...

4.23Xanthydrol solution, 5 g per 100 ml in ethanol or...

4.24Catalyst: copper oxide (CuO), 0.3 to 0.4 g per determination,...

4.25Anti-bump granules of pumice stone washed with hydrochloric acid and...

4.26Indicator solutions: (4.26.1) Mixed indicator: Solution A: dissolve 1 g...

4.27Indicator papers: litmus, bromothymol blue (or other papers sensitive in...

4.28Ethanol or methanol, 95% (V/V).

5.1Distillation apparatus. See Method 2.

5.2Apparatus for determination of ammoniacal nitrogen. An example of the...

5.3Apparatus for determination of ureic nitrogen by the urease method...

5.4Rotary shaker: 35 – 40 turns per minute.

5.6Sintered glass crucibles, diameter of pores 5 to 15 microns....

6PREPARATION OF SAMPLE

7.1Preparation of solution for analysis

7.2Total nitrogen

7.3Total nitrogen excluding nitric nitrogen

7.4Nitric nitrogen is obtained: by difference between

7.5Ammoniacal nitrogen

7.6Ureic nitrogen

8VERIFICATION OF RESULTS

8.1Before each analysis, check the functioning of the apparatus and...

9a.EXTRACTION OF TOTAL PHOSPHORUS BY MINERAL ACIDS

2FIELD OF APPLICATION

4.1Sulfuric acid (p=1.84 g/ml).

4.2Nitric acid (p=1.40 g/ml).

5.1A Kjeldahl flask, with a capacity of at least 500...

6PREPARATION OF THE SAMPLE

7.2Determination

9b.EXTRACTION OF PHOSPHORUS BY 2% FORMIC ACID

2FIELD OF APPLICATION

4.1Formic acid, 2% (20 g per litre): dilute 82 ml...

5.1500 ml graduated flask with a wide neck (eg Stohmann)....

5.2Rotary shaker, 35 – 40 turns per minute.

6PREPARATION OF THE SAMPLE

7.1Extraction Weigh to the nearest 0.001 g, 5 g of...

7.2Determination Determine the phosphorus using Method 10 on an aliquot...

9c.EXTRACTION OF PHOSPHORUS BY 2% CITRIC ACID

2FIELD OF APPLICATION

4.12% citric acid solution (20 g per litre), prepared from...

5.1Rotary shaker: 35 – 40 turns per minute.

6PREPARATION OF THE SAMPLE

7.2Determination

9d.EXTRACTION OF PHOSPHORUS BY NEUTRAL AMMONIUM CITRATE

2FIELD OF APPLICATION

4.1Neutral ammonium citrate solution (pH=7.0). This solution must contain 185...

5.2Water bath which can be set thermostatically at 65°C, equipped...

6PREPARATION OF THE SAMPLE

7.2Determination

9e.EXTRACTION OF PHOSPHORUS BY ALKALINE AMMONIUM CITRATE (PETERMANN'S METHOD) AT 65°C

2FIELD OF APPLICATION

4.1Petermann’s solution

5.1Water bath which can be maintained at a temperature of...

5.2500 ml graduated flask with a wide neck (eg Stohmann)....

6PREPARATION OF SAMPLE

7.1Extraction Weigh to the nearest 0.001g, 1 g of the...

7.2Determination Determine the phosphorus using Method 10 on an aliquot...

9f.EXTRACTION OF PHOSPHORUS BY ALKALINE AMMONIUM CITRATE (PETERMANN'S) METHOD AT AMBIENT TEMPERATURE

2FIELD OF APPLICATION

5.1250 ml graduated flask with a wide neck (eg Stohmann)....

5.2Rotary shaker, 35 – 40 turns per minute.

6PREPARATION OF THE SAMPLE

7.2Determination

9g.EXTRACTION OF PHOSPHORUS BY ALKALINE AMMONIUM CITRATE (JOULIE'S METHOD)

2FIELD OF APPLICATION

4.1Joulie’s alkaline solution of ammonium citrate: This solution contains 400...

4.28-Hydroxyquinoline (oxine), powdered.

5.1Rotary shaker, 35 – 40 turns per minute.

5.2500 ml graduated flask with a wide neck (Stohmann).

6PREPARATION OF THE SAMPLE

7.2Determination

9h.EXTRACTION OF PHOSPHORUS BY WATER

2FIELD OF APPLICATION

4.1500 ml graduated flask with a wide neck (eg Stohmann)....

4.2Rotary shaker, 35 – 40 turns per minute.

5PREPARATION OF THE SAMPLE

6.2Determination

10.DETERMINATION OF EXTRACTED PHOSPHORUS (Gravimetric method using quinoline phosphomolybdate)

2FIELD OF APPLICATION

4.1Concentrated nitric acid (p = 1.40 g/ml).

4.2Molybdate reagent: (4.2.1) Preparation of the reagent based on sodium...

5.1Filter crucible with porosity of 5 to 20 microns.

5.2Drying oven regulated at 250°C+10°C.

5.3Sintered glass funnel with porosity of 5 to 20 microns....

6.1Treatment of the solution

6.3Weighing the crucible

6.4Precipitation

6.5Filtering and Washing

6.6Drying and weighing

6.8Control test

7EXPRESSION OF RESULTS

11.DETERMINATION OF WATER-SOLUBLE POTASSIUM

2FIELD OF APPLICATION

4.1Formaldehyde, 25 – 35% solution, filter if necessary before use....

4.2Potassium chloride.

4.3Sodium hydroxide, 10 M solution. Care should be taken to...

4.4Indicator solution: dissolve 0.5 g phenolphthalein in 100 ml 90%...

4.5EDTA solution: 4 g of the dihydrated disodium salt of...

4.6STPB solution: dissolve 32.5 g sodium tetraphenylborate in 480 ml...

4.7Wash liquid: dilute 20 ml of the STPB solution (4.6)...

4.8Bromine water: saturated bromine solution in water.

5.1Filter crucibles with a porosity of 5 to 20 microns....

5.2Oven regulated at 120° + 10° C.

6PREPARATION OF THE SAMPLE

7.2Determination

7.3Weighing the crucible

7.4Precipitation

7.5Filtering and washing

7.6Drying and weighing

7.8Control test

8EXPRESSION OF RESULTS

8.1Method of calculation and formulae

12.DETERMINATION OF CHLORIDES IN THE ABSENCE OF ORGANIC MATERIAL

2FIELD OF APPLICATION

4.1Nitrobenzene or diethyl ether.

4.2Nitric acid, 10 M solution.

4.3Indicator solution: dissolve 40 g of ferric ammonium sulfate [Fe2(SO4)3.(NH4)2SO4.24H2O]...

4.4Silver nitrate, 0.1 M solution.

4.5Ammonium thiocyanate, 0.1 M solution. Preparation: since this salt is...

4.6Potassium Chloride solution: Dissolve 2.103g of potassium chloride, previously dried...

5.1Rotary shaker, 35 – 40 turns per minute.

6PREPARATION OF SAMPLE

7.2Determination

7.4Control test

8EXPRESSION OF RESULT

13a.DETERMINATION OF FINENESS OF GRINDING — DRY METHOD

2FIELD OF APPLICATION

4.1Mechanical sieve shaker.

4.2Sieves with apertures of 0.160 mm and 0.630 mm respectively...

6EXPRESSION OF RESULTS

13b.DETERMINATION OF FINENESS OF GRINDING OF SOFT NATURAL PHOSPHATES

2FIELD OF APPLICATION

4REAGENTS Sodium hexametaphosphate solution, 1 g per 100 ml.

5.1Sieves with apertures of 0.063 mm and 0.125 mm respectively...

5.2Glass funnel of 20 cm diameter mounted on a stand....

5.3Laboratory oven.

7EXPRESSION OF RESULTS

14.METHODS OF ANALYSIS AND TEST PROCEDURES FOR AMMONIUM NITRATE FERTILISERS CONTAINING MORE THAN 28% NITROGEN BY WEIGHT

14a.METHOD FOR THE APPLICATION OF THERMAL CYCLES

2FIELD OF APPLICATION

3PRINCIPLE AND DEFINITION

4.1Water baths thermostated at 25 (+1) and 50 (+1)° C...

4.2Erlenmeyer flasks with an individual capacity of 150 ml.

14b.DETERMINATION OF THE OIL RETENTION VALUE

1SCOPE AND FIELD OF APPLICATION

5.1Balance, capable of weighing to the nearest 0.01 gram.

5.2Beakers, of capacity 500 ml.

5.3Funnel, plastic, preferably with a cylindrical wall at the upper...

5.4Test sieve, aperture 0.5 mm, fitting into the funnel (5.3)....

5.5Filter paper, rapid filtering grade, creped, soft, weight 150 g/m2....

5.6Absorbent tissue (laboratory grade).

6.1Carry out two individual determinations in quick succession on separate...

6.2Remove particles smaller than 0.5 mm using the test sieve...

6.3Filter the entire contents of the beaker through the funnel...

6.4Lay two sheets of filter paper (5.5) (about 500 ×...

6.5Repeating the rolling procedure and reweighing.

7EXPRESSION OF RESULTS

7.1Method of calculation and formula

14c.DETERMINATION OF COMBUSTIBLE INGREDIENTS

1SCOPE AND FIELD OF APPLICATION

3.1Analytical-grade chromium VI oxide; CrVlO3.

3.2Sulfuric acid diluted to 60% by volume: pour 360 ml...

3.3Silver nitrate: 0.1 M solution.

3.4Barium hydroxide: weigh out 15 grams of barium hydroxide (Ba(OH)2.8H2O),...

3.5Hydrochloric acid: 0.1 M standard solution.

3.6Sodium hydroxide: 0.1 M standard solution.

3.7Bromophenol blue: solution of 0.4 grams per litre in water....

3.8Phenolphthalein: solution of 2 grams per litre in 60% by...

3.9Soda lime: particle dimensions, about 1.0 to 1.6 mm.

3.10Demineralised water, freshly boiled to remove carbon dioxide.

4.1filter crucible with a plate of sintered glass and a...

4.2Compressed nitrogen supply.

4.3Apparatus made up of the following parts and assembled, if...

5.1Sample for analysis

5.2Removal of carbonates

5.3Oxidation and absorption

5.4Measurement of the carbonates originating from organic material

7EXPRESSION OF RESULTS

14d.DETERMINATION OF THE pH VALUE

1SCOPE AND FIELD OF APPLICATION

3.1Buffer solution, pH 6.88 at 20° C

3.2Buffer solution, pH 4.00 at 20° C

3.3Commercially available pH standard solutions may be used.

5.1Calibration of the pH meter Calibrate the pH meter (4)...

5.2Determination

6EXPRESSION OF RESULTS

14e.DETERMINATION OF THE PARTICLE SIZE

1SCOPE AND FIELD OF APPLICATION

3.1200 mm diameter woven-wire test sieves to BS 410 (1986)...

3.2Balance to weigh to 0.1 gram.

3.3Mechanical sieve shaker (if available) capable of imparting both vertical...

4.1The sample is divided representatively into portions of approximately 100...

4.2Weigh one of these portions to the nearest 0.1 gram....

4.3Arrange the nest of sieves in ascending order (receiver, 0.5...

4.4Shake by hand or machine, imparting both a vertical and...

4.5Remove the sieves from the nest in turn and collect...

4.6Weigh the material retained on each sieve and that collected...

5EVALUATION OF RESULTS

5.1Convert the fraction masses to a percentage of the total...

5.2At least two separate analyses should be carried out and...

6EXPRESSION OF RESULTS

14f.DETERMINATION OF THE CHLORINE CONTENT (AS CHLORIDE ION)

1SCOPE AND FIELD OF APPLICATION

3.2Concentrated nitric acid (density at 20°C p=1.40 g/ml).

3.3Silver nitrate 0.1 M standard solution. Store this solution in...

3.4Silver nitrate 0.004 M standard solution — prepare this solution...

3.5Potassium chloride 0.1 M standard reference solution. Weigh, to the...

3.6Potassium chloride 0.004 M standard reference solution — prepare this...

4.1Potentiometer with silver indicating electrode and calomel reference electrode, sensitivity...

4.2Bridge, containing a saturated potassium nitrate solution, connected to the...

4.3etic stirrer, with a Teflon-coated rod.

4.4Microburette with fine-pointed tip, graduated in 0.01 ml divisions.

5.1Standardisation of the silver nitrate solution

5.4Determination Take a portion of sample in the range of...

6EXPRESSION OF RESULTS

14g.DETERMINATION OF COPPER

1SCOPE AND FIELD OF APPLICATION

3.1Hydrochloric acid (density at 20° C ρ = 1.18 g/ml)....

3.2Hydrochloric acid, 6 M solution.

3.3Hydrochloric acid, 0.5 M solution.

3.4Ammonium nitrate.

3.5Hydrogen peroxide, 30%.

3.6Copper solution (stock): weigh, to the nearest 0.001 gram, 1...

5.1Preparation of the solution for analysis

5.2Blank solution

5.3Determination

6EXPRESSION OF RESULTS

15.EXTRACTION OF TOTAL CALCIUM, TOTAL MAGNESIUM, TOTAL SODIUM AND TOTAL SULFUR IN THE FORM OF SULFATES

2FIELD OF APPLICATION

4.1Diluted hydrochloric acid; One volume of hydrochloric acid (p =...

6PREPARATION OF THE SAMPLE

7.1Test sample. Calcium, magnesium, sodium and sulfur in the form...

7.2Preparation of the solution. Add approximately 400 ml of water...

16.EXTRACTION OF TOTAL SULFUR

2FIELD OF APPLICATION

4.1Diluted hydrochloric acid: One volume of hydrochloric acid (p =...

4.2Sodium hydroxide solution, NaOH, 30% minimum (p = 1.33)

4.3Hydrogen peroxide solution, 30% w/w.

4.4Aqueous solution of barium chloride BaCl2.2H2O, 122 gram per litre....

6PREPARATION OF THE SAMPLE

7.1Test sample. Weigh out to within 1 mg a quantity...

7.2Oxidation. Add 20 ml of sodium hydroxide solution (4.2) and...

7.3Preparation of the solution to be analysed. Add approximately 50...

17.EXTRACTION OF WATER-SOLUBLE CALCIUM, MAGNESIUM, SODIUM AND SULFUR (IN THE FORM OF SULFATES)

2FIELD OF APPLICATION

6PREPARATION OF THE SAMPLE

7.1Test sample. (a) Where fertilisers contain no sulfur or where...

7.2Preparation of the solution. Add approximately 400 ml of water...

18.EXTRACTION OF WATER — SOLUBLE SULFUR

2FIELD OF APPLICATION

4.1Diluted hydrochloric acid: One volume of hydrochloric acid (p =...

5.1500 ml graduated Stohmann flask.

5.2Rotary shaker, 30 to 40 turns per minute.

5.3Electric hot plate with adjustable temperature.

6PREPARATION OF THE SAMPLE

7.1Test sample. (a) Where fertilisers contain a maximum of 3%...

7.2Preparation of the solution. Add approximately 400 ml of water....

7.3Oxidation of the aliquot portion to be analysed. Take an...

19.EXTRACTION AND DETERMINATION OF ELEMENTAL SULFUR

2FIELD OF APPLICATION

5.1100 ml extraction flask with ground glass stopper.

5.2Soxhlet apparatus.

5.3Vacuum rotary evaporator.

5.4Electric oven, fan assisted, set at 90+2° C.

5.5Petri dishes, five to seven centimetres in diameter, not exceeding...

5.6Electric hot plate with adjustable temperature.

6PREPARATION OF THE SAMPLE

7.1Test sample. Weigh out 5 – 10 g of the...

7.2Extraction of the sulfur. Wash thoroughly the contents of the...

7.3Determination of the purity of the elemental sulfur. Certain substances...

8EXPRESSION OF RESULTS

20.MANGANIMETRIC DETERMINATION OF EXTRACTED CALCIUM FOLLOWING PRECIPITATION IN THE FORM OF OXALATE

2FIELD OF APPLICATION

4.1Diluted hydrochloric acid: One volume of hydrochloric acid (ρ =...

4.21:10 dilute sulfuric acid: One volume of sulfuric acid (ρ...

4.31:1 dilute ammonia solution: One volume of ammonia (ρ =...

4.4Saturated solution of ammonium oxalate [(NH4)2C2O4.H2O] at ambient temperature (approximately...

4.5Citric acid solution, 30% (m/v).

4.6Ammonium chloride solution, 5% (m/v).

4.7Solution of bromothymol blue in 95% ethanol, 0.1% (m/v).

4.8Solution of bromocresol green in 95% ethanol, 0.04% (m/v).

4.9Standard solution of potassium permanganate, 0.02 M.

5.1Filter crucible with 5 to 20μ porosity sintered glass.

5.2Hot water bath.

6PREPARATION OF THE ALIQUOT PORTION TO BE ANALYSED

7PRECIPITATION OF THE CALCIUM OXALATE

8TITRATION OF THE OXALATE PRECIPITATE

9EXPRESSION OF RESULTS

21.DETERMINATION OF MAGNESIUM BY ATOMIC ABSORPTION SPECTROMETRY

2FIELD OF APPLICATION

4.1Hydrochloric acid, 1 M solution.

4.2Hydrochloric acid, 0.5 M solution.

4.3Standard solution of magnesium, 1.00 mg per ml.

4.4Strontium chloride solution. Dissolve 75 g of strontium chloride (SrCl2.6H2O)...

5.1Spectrometer fitted for atomic absorption, with a magnesium lamp, set...

5.2Air-acetylene flame.

6PREPARATION OF THE SOLUTION TO BE ANALYSED

7.1If the fertiliser has a declared magnesium (Mg) content of...

7.2Using a pipette, take 10 ml of the extraction solution...

7.3Dilute this solution (7.2) with the 0.5 M hydrochloric acid...

7.4Preparation of blank solution. Prepare a blank solution by repeating...

7.5Preparation of calibration solutions. By diluting the standard solution (4.3)...

7.6Measurement. Set up the spectrometer (5.1) at a wavelength of...

8EXPRESSION OF RESULTS

22.DETERMINATION OF MAGNESIUM BY COMPLEXOMETRY

2FIELD OF APPLICATION

4.1Standard 0.05 M solution of magnesium: (4.1.1) Dissolve 1.232 g...

4.20.05 M solution of EDTA. Weigh out 18.61 g of...

4.30.05 molar standard solution of calcium. Weigh out 5.004 g...

4.4Calcein indicator. Carefully mix in a mortar one gram of...

4.5Calcon carbonic acid indicator. Dissolve 400 mg of calcon carbonic...

4.6Eriochrome black — T indicator. Dissolve 300 mg of Eriochrome...

4.7Potassium cyanide solution. Aqueous solution of KCN at 2%. (CAUTION:...

4.8Solution of potassium hydroxide and potassium cyanide. Dissolve 280 g...

4.9Buffer solution, pH 10.5. In a 500 ml graduated flask,...

4.10Diluted hydrochloric acid: One volume of hydrochloric acid (ρ =...

4.11Hydrochloric acid solution approximately 0.5 M.

4.12Hydrochloric acid solution approximately 1 M.

4.13Sodium hydroxide solution 5 M.

5.1Magnetic or mechanical stirrer.

7PREPARATION OF THE SOLUTION TO BE ANALYSED

8.1Aliquot portions to be taken. Take aliquot portions of the...

8.2Titration in the presence of Eriochrome black-T. Pipette an aliquot...

8.3Titration in the presence of calcein or of calcon carbonic...

9EXPRESSION OF RESULTS

10.1The stoichiometric EDTA-metal ratio in the complexometric analyses is always...

10.2Complexometric indicators are often sensitive to air. The solution may...

10.3The metal-indicator complexes are often relatively stable and it may...

10.4The colour change of the indicator must not be observed...

10.5This analysis requires a certain amount of experience. The task...

10.6If an EDTA solution of guaranteed strength is used (Titrisol,...

10.7The solutions containing potassium cyanide must not be poured down...

23.DETERMINATION OF SULFATES

2FIELD OF APPLICATION

4.1Diluted hydrochloric acid: One volume of hydrochloric acid (ρ =...

4.2Barium chloride solution BaCl2.2H2O:122 grams per litre.

4.3Silver nitrate solution: 5 grams per litre.

5.2Hot water bath.

5.3Drying oven set at 105° C ± 1° C.

5.4Electric furnace set at 800° C ± 50° C.

6.1Sampling of the solution. Pipette an aliquot portion of one...

6.2Preparation of the precipitate. Bring the solution to the boil....

6.3Incineration and weighing of the precipitate. Place the filter paper...

7EXPRESSION OF RESULTS

24.DETERMINATION OF THE SODIUM EXTRACTED

2FIELD OF APPLICATION

4.1Diluted hydrochloric acid: One volume of hydrochloric acid (ρ =...

4.2Aluminium nitrate Al(NO3)3.9H2O.

4.3Caesium chloride, CsCl.

4.4Anhydrous sodium chloride, NaCl.

4.5Caesium chloride and aluminium nitrate solution. Dissolve in water 50...

4.6Standard sodium solution of 1 mg/ml of Na. Dissolve in...

6CALIBRATION SOLUTIONS

6.1Pipette 10 ml of standard solution (4.6) into a 250...

6.2Using a burette place 0, 5, 10, 15, 20, 25...

7PREPARATION OF SOLUTIONS TO BE MEASURED

9CALCULATION OF RESULTS

25.TRACE ELEMENTS AT A CONCENTRATION LESS THAN 10%

25a.EXTRACTION OF TOTAL TRACE ELEMENTS

2FIELD OF APPLICATION

4.1Dilute hydrochloric acid (HCI) solution, about 6 M: Mix 1...

4.2Concentrated ammonia solution (NH4OH, p = 0.9g/ml)

6PREPARATION OF THE SAMPLE

7.1Test sample Take a quantity of fertiliser weighing between 2...

7.2Preparation of the solution If necessary moisten the sample with...

25b.EXTRACTION OF WATER-SOLUBLE TRACE ELEMENTS

2FIELD OF APPLICATION

4.1Dilute hydrochloric acid (HCI) solution, above 6 M: Mix 1...

5.1Rotary shaker set at about 35 to 40 rpm.

5.2pH-meter. (Note) Where the boron content of the extract is...

6PREPARATION OF THE SAMPLE

7.1Test sample Take a quantity of fertiliser weighing between 2...

7.2Preparation of the solution Add about 200 ml of water...

7.3Preparation of the test solution Filter immediately into a clean,...

25c.REMOVAL OF ORGANIC COMPOUNDS FROM FERTILISER EXTRACTS

2FIELD OF APPLICATION

4.1Dilute hydrochloric acid (HCI) solution, about 0.5 M: Mix 1...

4.2Hydrogen peroxide solution (30% H2O2 ρ = 1.11 g/ml), free...

25d.DETERMINATION OF TRACE ELEMENTS IN FERTILISER EXTRACTS BY ATOMIC ABSORPTION SPECTROMETRY (GENERAL PROCEDURE)

2FIELD OF APPLICATION

4.1Dilute hydrochloric acid solution (HCI), about 6 M: Mix one...

4.2Dilute hydrochloric acid solution (HCI), about 0.5 M: Mix one...

4.3Lanthanum salt solutions (10 g of La per litre). This...

4.4Calibration solutions For the preparation of these, see the individual...

6PREPARATION OF THE SOLUTION TO BE ANALYSED

6.1Preparation of extract solutions of the trace elements to be...

6.2Treatment of the test solution Dilute an aliquot portion of...

7.1Preparation of a blank solution Prepare a blank solution by...

7.2Preparation of calibration solutions From the working calibration solution prepared...

7.3Determination Prepare the spectrometer (5) for the determination and adjust...

8EXPRESSION OF RESULTS

25e.DETERMINATION OF BORON IN FERTILISER EXTRACTS BY MEANS OF SPECTROMETRY WITH AZOMETHINE-H

2FIELD OF APPLICATION

4.1EDTA buffer solution Place in a 500 ml volumetric flask...

4.2Azomethine-H solution Place in a 200 ml volumetric flask —...

4.3Boron calibration solutions (4.3.1) Boron stock solution (100 μg/ml) Dissolve...

6PREPARATION OF THE SOLUTION TO BE ANALYSED

6.1Preparation of the boron solution See Methods 25a and/or 25b...

6.2Preparation of the test solution Dilute an aliquot portion of...

6.3Preparation of the correction solution. If the test solution (6.2)...

7.1Preparation of the blank solution Prepare a blank solution by...

7.2Preparation of the calibration solutions Transfer 0, 5, 10, 15,...

7.3Colour development Transfer 5 ml of the calibration solutions (7.2),...

7.4Determination Measure the absorbance of the solutions obtained at 7.3...

8EXPRESSION OF RESULTS

25f.DETERMINATION OF COBALT IN FERTILISER EXTRACTS BY ATOMIC ABSORPTION SPECTROMETRY

2FIELD OF APPLICATION

4.1Hydrochloric acid solution, about 6 M. See Method 25d (4.1)....

4.2Hydrochloric acid solution, about 0.5 M. See Method 25d (4.2)....

4.3Lanthanum salt solutions (10 g of La per litre) See...

4.4Cobalt calibration solutions. (4.4.1) Cobalt stock solution (1,000 μg/ml) In...

6PREPARATION OF THE SOLUTION TO BE ANALYSED

6.1Cobalt extract solution See Methods 25a and/or 25b and, if...

6.2Preparation of the test solution See Methods 25d (6.2). The...

7.1Preparation of blank solution See Method 25d (7.1). The blank...

7.2Preparation of calibration solutions See Method 25d (7.2). For an...

7.3Determination See Method 25d (7.3). Prepare the spectrometer (5) for...

8EXPRESSION OF RESULTS

25g.DETERMINATION OF COPPER IN FERTILISER EXTRACTS BY ATOMIC ABSORPTION SPECTROMETRY

2FIELD OF APPLICATION

4.1Hydrochloric acid solution, about 6 M See Method 25d (4.1)....

4.2Hydrochloric acid solution, about 0.5 M See Method 25d (4.2)....

4.3Hydrogen peroxide solution (30% H2O, p = 1.11 g/ml), free...

4.4Copper calibration solutions (4.4.1) Copper stock solution (1,000 μg/ml) In...

6PREPARATION FOR THE SOLUTION TO BE ANALYSED

6.1Copper extract solution See Methods 25a and/or 25b and, if...

6.2Preparation of the test solution See Method 25d (6.2).

7.1Preparation of blank solution See Method 25d (7.1).

7.2Preparation of calibration solutions See Method 25d (7.2). For an...

7.3Determination See Method 25d (7.3). Prepare the spectrometer (5) for...

8EXPRESSION OF RESULTS

25h.DETERMINATION OF IRON IN FERTILISER EXTRACTS BY ATOMIC ABSORPTION SPECTROMETRY

2FIELD OF APPLICATION

4.1Hydrochloric acid solution, about 6M. See Method 25d (4.1).

4.2Hydrochloric acid solution, about 0.5 M See Method 25d (4.2)....

4.3Hydrogen peroxide solution (30% H2O2 p = 1.11 g/ml) free...

4.4Lanthanum salt solutions (10 g of La per litre) See...

4.5Iron calibration solutions (4.5.1) Iron stock solution (1,000 μg/ml) In...

6PREPARATION FOR THE SOLUTION TO BE ANALYSED

6.1Iron extract solution See Methods 25a and/or 25b and, if...

6.2Preparation of the test solution See Method 25d (6.2). The...

7.1Preparation of blank solution See Method 25d (7.1). The test...

7.2Preparation of calibration solutions See Method 25d (7.2). For an...

7.3Determination See Method 25d (7.3). Prepare the spectrometer (5) for...

8EXPRESSION OF RESULTS

25i DETERMINATION OF MANGANESE IN FERTILISER EXTRACTS BY ATOMIC ABSORPTION SPECTROMETRY

2FIELD OF APPLICATION

4.1Hydrochloric acid solution, about 6 M See Method 25d (4.1)....

4.2Hydrochloric acid solution, about 0.5 M See Method 25d (4.2)....

4.3Lanthanum salt solutions (10 g of La per litre) See...

4.4Manganese calibration solutions (4.4.1) Manganese stock solution (1,000 μg/ml) In...

6PREPARATION OF THE SOLUTION TO BE ANALYSED

6.1Manganese extract solution See Methods 25a and/or 25b and, if...

6.2Preparation of the test solution See Method 25d (6.2). The...

7.1Preparation of the blank solution See Method 25d (7.1). The...

7.2Preparation of the calibration solutions See Method 25d (7.2). For...

7.3Determination See Method 25d (7.3). Prepare the spectrometer (5) for...

8EXPRESSION OF RESULTS

25j.DETERMINATION OF MOLYBDENUM IN FERTILISER EXTRACTS BY SPECTROMETRY OF A COMPLEX WITH AMMONIUM THIOCYANATE

2FIELD OF APPLICATION

4.1Dilute hydrochloric acid solution (HCI), about 6 M See method...

4.2Copper solution (70 mg/l) in 1.5 M hydrochloric acid Dissolve...

4.3Ascorbic acid solution (50 g/l) Dissolve 50 g of ascorbic...

4.4n-butyl acetate

4.5Ammonium thiocyanate solution, 0.2 M Dissolve 15.224 g of NH4SCN...

4.6Stannous chloride solution (50 g/l) in 2 M hydrochloric acid...

4.7Molybdenum calibration solutions (4.7.1) Molybdenum stock solution (500 μg/ml) Dissolve...

5.1Spectrometer fitted for molecular absorption with cells having a 20...

5.2200 or 250 ml separating funnels.

6PREPARATION OF THE SOLUTION TO BE ANALYSED

6.1Molybdenum extract solution See Methods 25a and/or 25b and, if...

6.2Preparation of the test solution Dilute an aliquot portion of...

7.1Preparation of the blank solution Prepare a blank solution by...

7.2Preparation of the series of calibration solutions Prepare a series...

7.3Development and separation of the complex To each separating funnel...

7.4Determination Measure the absorbencies of the solutions obtained at 7.3...

8EXPRESSION OF RESULTS

25k.DETERMINATION OF ZINC IN FERTILISER EXTRACTS BY ATOMIC ABSORPTION SPECTROMETRY

2FIELD OF APPLICATION

4.1Hydrochloric acid solution, about 6 M See Method 25d (4.1)....

4.2Hydrochloric acid solution, about 0.5 M See Method 25d (4.2)....

4.3Lanthanum salt solutions (10 g of La per litre) See...

4.4Zinc calibration solutions (4.4.1) Zinc stock solution (1,000 μg/ml) In...

6PREPARATION OF THE SOLUTION TO BE ANALYSED

6.1Zinc extract solution See Methods 25a and/or 25b and, if...

6.2Preparation of the test solution See Method 25d (6.2). The...

7.1Preparation of the blank solution See Method 25d (7.1). The...

7.2Preparation of the calibration solutions See Method 25d (7.2). For...

7.3Determination See Method 25d (7.3). Prepare the spectrometer (5) for...

8EXPRESSION OF RESULTS

26.TRACE ELEMENTS AT A CONCENTRATION GREATER THAN 10%

26a.EXTRACTION OF TOTAL TRACE ELEMENTS

2FIELD OF APPLICATION

4.1Diluted hydrochloric acid (HCI) solution, about 6M Mix 1 volume...

4.2Concentrated ammonia solution (NH4OH, p = 0.9 g/ml)

5.1Electric hotplate with variable temperature control.

5.2pH meter (Note) Where the boron content of an extract...

6PREPARATION OF THE SAMPLE

7.1Test sample Take a quantity of fertiliser weighing 1 or...

7.2Preparation of the solution If necessary moisten the sample with...

26b.EXTRACTION OF WATER — SOLUBLE TRACE ELEMENTS

2FIELD OF APPLICATION

4.1Diluted hydrochloric acid (HCI) solution, about 6 M Mix 1...

5.1Rotary shaker set at about 35 to 40 rpm.

6PREPARATION OF THE SAMPLE

7.1Test sample Take a quantity of fertiliser weighing 1 or...

7.2Preparation of the solution Add about 400 ml of water....

7.3Preparation of the test solution Filter immediately into a clean,...

26c.REMOVAL OF ORGANIC COMPOUNDS FROM FERTILISER EXTRACTS

2FIELD OF APPLICATION

4.1Diluted hydrochloric acid solution, about 0.5 M Mix 1 volume...

4.2Hydrogen peroxide solution (30% H2O2, p = 1.11 g/ml), free...

26d.DETERMINATION OF TRACE ELEMENTS IN FERTILISER EXTRACTS BY ATOMIC ABSORPTION SPECTROMETRY

(GENERAL PROCEDURE)

2FIELD OF APPLICATION

4.1Diluted hydrochloric acid solution (HCI), about 6 M Mix one...

4.2Diluted hydrochloric acid solution (HCI), about 0.5 M Mix one...

4.3Lanthanum salt solutions (10 g of La per litre) This...

4.4Calibration solutions For the preparation of these, see the individual...

6PREPARATION OF THE SOLUTION TO BE ANALYSED

6.1Preparation of extract solutions containing the elements to be determined....

6.2Treatment of the test solution Dilute an aliquot portion of...

7.1Preparation of a blank solution. Prepare a blank solution by...

7.2Preparation of calibration solutions From the working calibration solution prepared...

7.3Determination Prepare the spectrometer (5) for the determination and adjust...

8EXPRESSION OF RESULTS

26e.DETERMINATION OF BORON IN FERTILISER EXTRACTS BY MEANS OF ACIDIMETRIC TITRATION

2FIELD OF APPLICATION

4.1Methyl red indicator solution Dissolve 0.1 g of methyl red...

4.2Diluted hydrochloric acid solution, about 0.5 M Mix 1 volume...

4.3Sodium hydroxide solution, about 0.5 M Must be free of...

4.4Standard sodium hydroxide solution, about 0.025 M Must be free...

4.5Boron calibration solution (100 μg/ml B) Dissolve 0.5719 g of...

4.6D-mannitol (C6H14O6) powder.

4.7Sodium chloride (NaCl).

5.1pH meter with glass electrode

5.2Magnetic stirrer

5.3400 ml beaker with teflon rod

6PREPARATION OF THE SOLUTION TO BE ANALYSED

6.1Preparation of the boron solution See Methods 26a, 26b and,...

7.1Determination Place in a 400 ml beaker (5.3) an aliquot...

8BLANK SOLUTION

9BORON (B) VALUE OF THE SODIUM HYDROXIDE SOLUTION (4.4)

10EXPRESSION OF RESULTS

26f.DETERMINATION OF COBALT IN FERTILISER EXTRACTS BY THE GRAVIMETRIC METHOD WITH 1-NITROSO-2-NAPHTHOL

2FIELD OF APPLICATION

4.1Hydrogen peroxide solution (H2O2 ρ = 1.11 g/ml) 30%

4.2Sodium hydroxide solution, about 2 M Dissolve 8 g of...

4.3Diluted hydrochloric acid solution, about 6 M Mix one volume...

4.4Acetic acid (99.7% CH3COOH) (ρ = l.05 g/ml).

4.5Acetic acid solution (1:2), about 6 M Mix one volume...

4.6Solution of l-nitroso-2-naphthol in 100 ml of acetic acid (4.4)....

5.1Filter crucible P 16/ISO 4793, porosity 4, capacity 30 or...

5.2Drying oven at 130 2° C

6PREPARATION OF THE SOLUTION TO BE ANALYSED

6.1Preparation of the cobalt solution See Methods 26a or 26b....

6.2Preparation of the solution to be analysed Place the aliquot...

8EXPRESSION OF RESULTS

26g.DETERMINATION OF COPPER IN FERTILISER EXTRACTS BY THE TITRIMETRIC METHOD

2FIELD OF APPLICATION

4.1Nitric acid (HNO3, ρ = 1.40 g/ml).

4.2Urea [(NH2)2 C O].

4.3Ammonium bifluoride (NH4HF2) solution (10 % w/v) Keep the solution...

4.4Ammonium hydroxide solution (1 + 1) Mix 1 volume of...

4.5Sodium thiosulfate standard solution Dissolve 7.812 g of sodium thiosulfate...

4.6Potassium iodide (KI).

4.7Potassium thiocyanate (KSCN) solution (25 % w/v) Keep this solution...

4.8Starch solution (about 0.5 %) Place 2.5 g of starch...

5PREPARATION OF THE SOLUTION TO BE ANALYSED

6.1Preparation of the solution for titration Place an aliquot portion...

6.2Titration of the solution Place the Erlenmeyer flask on a...

7EXPRESSION OF RESULTS

26h.DETERMINATION OF IRON IN FERTILISER EXTRACTS BY ATOMIC ABSORPTION SPECTROMETRY

2FIELD OF APPLICATION

4.1Hydrochloric acid solution, about 6 M See Method 26d, (4.1)....

4.2Hydrochloric acid solution, about 0.5 M See Method 26d, (4.2)....

4.3Hydrogen peroxide solution (30% H2O2 p = 1.11 g/ml) free...

4.4Lanthanum salt solutions (10 g of La per litre) See...

4.5Iron calibration solution (4.5.1) Iron stock solution (1,000 μg/ml) In...

6PREPARATION OF THE SOLUTION TO BE ANALYSED

6.1Iron extract solution See Methods 26a and/or 26b and, if...

6.2Preparation of the test solution See Method 26d, (6.2). The...

7.1Preparation of the blank solution See Method 26d (7.1). The...

7.2Preparation of calibration solutions See Method 26d, (7.2). For an...

7.3Determination See Method 26d, (7.3). Prepare the spectrometer (5) for...

8EXPRESSION OF RESULTS

26i.DETERMINATION OF MANGANESE IN FERTILISER EXTRACTS BY TITRATION

2FIELD OF APPLICATION

4.1Concentrated sulfuric acid (H2SO4, ρ = 1.84 g/ml).

4.2Sulfuric acid, about 9 M Carefully mix 1 volume of...

4.3Nitric acid, 6 M Mix 3 volumes of nitric acid...

4.4Nitric acid, 0.3 M Mix 1 volume of 6 M...

4.5Sodium bismuthate (NaBiO3) (85 %).

4.7Orthophosphoric acid, 15 M (H3PO4, ρ = 1.71 g/ml).

4.8Ferrous sulfate solution, 0.15 M Dissolve 41.6 g of ferrous...

4.9Potassium permanganate solution, 0.02 M Weigh out 3.160 g of...

5.1Filter crucible P16/ISO 4793, porosity 4, capacity 50 ml, mounted...

5.2Magnetic stirrer.

6PREPARATION OF THE SOLUTION TO BE ANALYSED

6.1Manganese extract solution See Methods 26a and 26b. If it...

6.2In the absence of chloride ions, place an aliquot portion...

6.3If chloride ions are present, it is necessary to remove...

8EXPRESSION OF RESULTS

26j.DETERMINATION OF MOLYBDENUM IN FERTILISER EXTRACTS BY THE GRAVIMETRIC METHOD WITH 8-HYDROXYQUINOLINE

2FIELD OF APPLICATION

4.1Sulfuric acid solution, approximately 1 M Carefully pour 55 ml...

4.2Diluted ammonia solution (1:3) Mix 1 volume of concentrated ammonia...

4.3Diluted acetic acid solution (1:3) Mix 1 volume of concentrated...

4.4Solution of disodium salt of ethylene diamine tetraacetic acid (EDTA)...

4.5Buffer solution In a 100 ml volumetric flask, dissolve 15...

4.68-hydroxyquinoline (oxine) solution In a 100 ml volumetric flask dissolve...

5.1Filter crucible P16/ISO 4793, porosity 4, capacity 30 ml.

5.2pH meter with glass electrode.

5.3Drying oven at 130 to 135°C.

6PREPARATION OF THE SOLUTION TO BE ANALYSED

6.1Preparation of the molybdenum solution. See Methods 26a and 26b....

7.1Preparation of the test solution Place an aliquot portion containing...

7.2Obtaining and washing the precipitate Obtaining the precipitate Heat the...

7.3Weighing the precipitate Dry the precipitate at 130 to 135°C...

8EXPRESSION OF RESULTS

26k.DETERMINATION OF ZINC IN FERTILISER EXTRACTS BY ATOMIC ABSORPTION SPECTROMETRY

2FIELD OF APPLICATION

4.1Hydrochloric acid solution, about 6 M See Method 26d (4.1)....

4.2Hydrochloric acid solution, about 0.5 M See Method 26d (4.2)....

4.3Lanthanum salt solutions (10 g of La per litre) See...

4.4Zinc calibration solutions (4.4.1) Zinc stock solution (1000 μg/ml) In...

6PREPARATION OF THE SOLUTION TO BE ANALYSED

6.1Zinc extract solution See Methods 25a and/or 26b.

6.2Preparation of the test solution See Method 26d, (6.2). The...

7.1Preparation of the blank solution. See Method 26d. (7.1). The...

7.2Preparation of the calibration solutions See Method 26d (7.2). For...

7.3Determination See Method 26d (7.3). Prepare the spectrometer (5) for...

8EXPRESSION OF RESULTS

5Methods of Analysis

1Preparation of the sample for analysis

2Determination of moisture

3Determination of total nitrogen — chromium powder reduction method

4Determination of urea

5Determination of potassium — gravimetric method

6Determination of the neutralising value in liming materials

7Determination of fineness of products other than potassic basic slag...

8Determination of fineness of potassic basic slag

9Determination of fineness of certain lime products by wet sieving....

1.PREPARATION OF THE SAMPLE FOR ANALYSIS

2SCOPE AND FIELD OF APPLICATION

3.1Solid fertilisers:

3.2Fluid fertilisers:

4.1Sample grinder capable of grinding the fertiliser to pass the...

4.2Mortar and pestle of suitable material and size.

4.3Sieves having square apertures of 0.18 mm, 0.5 mm and...

4.4Sample containers of non-corrodible materials, with air-tight closures.

5.2Place the prepared sample in a clean container (4.4) and...

5.3Before taking each test portion for analysis, the whole sample...

5.4If the sample contains foreign matter which cannot be ground...

6.1Samples not to be ground

6.2Products which may be difficult to grind mechanically, including products with abnormal moisture or products which become doughy through grinding

6.3Organic materials

6.4Fertilisers comprising several different materials

7FLUID FERTILISERS

2.DETERMINATION OF MOISTURE

1SCOPE AND FIELD OF APPLICATION

3.1Suitable containers with lids ensuring air-tight closure; the dimensions should...

3.2Electrically heated oven, suitably ventilated and capable of being maintained...

4PREPARATION OF SAMPLE

6EXPRESSION OF RESULT

3.DETERMINATION OF TOTAL NITROGEN CHROMIUM POWDER REDUCTION METHOD

1SCOPE AND FIELD OF APPLICATION

3.1Sodium hydroxide solution: 40 g per 100 ml, ammonia free....

3.2Sulfuric acid, 0.05 M solution.

3.3Sulfuric acid, 0.1 M solution.

3.4Sulfuric acid, 0.25 M solution.

3.5Sodium hydroxide, 0.2 M solution, carbonate free.

3.6Chromium metal powder, 100 mesh, low nitrogen content.

3.7Anti-bump granules of pumice stone, washed in hydrochloric acid and...

3.8Anti-foaming agent, paraffin wax.

3.9Sulfuric acid (ρ = 1.84 g/ml).

3.10Hydrochloric acid (ρ = 1.18 g/ml).

3.11Catalyst mixture: 1,000 g potassium sulfate and 50 g copper...

3.12Indicator solutions: (3.12.1) Mixed indicator: mix 50 ml of 2...

3.13pH indicator paper, wide range.

5PREPARATION OF SAMPLE

6.2Hydrolysis, when the fertiliser is known not to contain organic matter

6.3Digestion, when the fertiliser is known to contain organic matter

6.4Distillation

7EXPRESSION OF RESULTS

4.DETERMINATION OF UREA

1SCOPE AND FIELD OF APPLICATION

3.1Activated charcoal.

3.2Carrez solution I: dissolve 21.9 g zinc acetate dihydrate in...

3.3Carrez solution II: 10.6 g potassium ferrocyanide per 100 ml....

3.4Hydrochloric acid solution, 0.02 M.

3.5Sodium acetate solution: 136 g sodium acetate trihydrate per litre....

3.64-dimethylaminobenzaldehyde solution: dissolve 1.6 g of 4-dimethylaminobenzaldehyde (4-DMAB) in 100...

3.7Urea standard solution: 1.0 g per 100 ml (1 ml...

4.1Mechanical shaker.

4.2Spectrometer with 10 mm cells.

5PREPARATION OF SAMPLE

6.1Preparation of the solution for analysis

6.2Determination

6.3Calibration curve

7EXPRESSION OF RESULTS

5.DETERMINATION OF POTASSIUM — GRAVIMETRIC METHOD

1SCOPE AND FIELD OF APPLICATION

3<1 Formaldehyde, 25 – 35% solution, filtered if necessary before use.

3.2Potassium chloride.

3.3Sodium hydroxide, 10 M solution. Care should be taken to...

3.4Indicator solution: dissolve 0.5 g phenolphthalein in 100 ml 90%...

3.5EDTA solution: 4 g of the dihydrated disodium salt of...

3.6STPB solution: dissolve 32.5 g sodium tetraphenylborate in 480 ml...

3.7Liquid for washing: dilute 20 ml of the STPB solution...

3.8Hydrochloric acid (ρ =1.18 g/ml).

4.1Filter crucibles with a porosity of 5 to 20 microns....

4.2Oven regulated to 120°C10°C.

5PREPARATION OF SAMPLE

6.1Preparation of the solution for analysis

6.2Determination

6.3Weighing the crucible

6.4Precipitation

6.5Filtering and washing

6.6Drying and weighing

6.8Control test

7EXPRESSION OF RESULTS

6.DETERMINATION OF THE NEUTRALISING VALUE IN LIMING MATERIALS

1SCOPE AND FIELD OF APPLICATION

3.1Hydrochloric acid, 0.5 M solution.

3.2Sodium hydroxide, 0.5 M solution (carbonate free).

3.3Phenolphthalein indicator solution: dissolve 0.25 g phenolphthalein in 150 ml...

4PREPARATION OF SAMPLE

5.1Determination

6EXPRESSION OF RESULTS

7.DETERMINATION OF FINENESS OF PRODUCTS OTHER THAN POTASSIC BASIC SLAG

1SCOPE AND FIELD OF APPLICATION

4.1For sieving through 3.5 mm, 1.0 mm and 150 micron sieves

4.2For sieving through 6.7 mm, 6.3 mm and 5 mm sieves

4.3For sieving through a 45 mm sieve

5EXPRESSION OF RESULTS

8.DETERMINATION OF FINENESS OF POTASSIC BASIC SLAG

1SCOPE AND FIELD OF APPLICATION

4.1Preparation of the sample

5EXPRESSION OF RESULTS

9.DETERMINATION OF FINENESS OF CERTAIN LIME PRODUCTS BY WET SIEVING

3.1Balance, capable of weighing to the nearest 0.01 g

3.2Stainless steel woven wire test sieves 100 mm diameter, complying...

3.3Stainless steel woven wire test sieves complying with ISO 3310...

3.4Oven capable of being controlled at 105°C2

3.5Rotating end over end shaker: 35 – 40 turns per...

4.1Procedure for samples with dry matter content <60% Pass the...

4.2Procedure for samples with dry matter content<60% which cannot be...

6DRY MATTER CONTENT

7EXPRESSION OF RESULTS

7.1Original dry mass Calculate the original dry mass (Md) of...

7.2Sieve fraction Calculate the percentage of material retained on each...

APPENDIX TO SCHEDULE 2

1996 No. 1342

AGRICULTURE

The Fertilisers (Sampling and Analysis) Regulations 1996

Made25th May 1996

Laid before Parliament31st May 1996

Coming into force21st June 1996

The Minister of Agriculture, Fisheries and Food, the Secretary of State for Scotland and the Secretary of State for Wales, acting jointly, in exercise of the powers conferred by sections 66(1), 67(5), 74A, 75(1), 76(1), 77, 78(2), (4) and (6), 79(1), (2) and (9) and 84 of the Agriculture Act 19701 and of all other powers enabling them in that behalf, after consultation as required by section 84(1) of the said Act with such persons or organisations as appear to them to represent the interests concerned, hereby make the following Regulations: —