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The Fertilisers (Sampling and Analysis) Regulations (Northern Ireland) 1991

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  1. Introductory Text

  2. 1.Title, commencement and interpretation

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

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

  5. 4.Methods of sending part of a sample

  6. 5.Application of the methods of analysis

  7. 6.Form of certificate of analysis

  8. 7.Modification of the Agriculture Act 1970

  9. 8.Revocations

  10. Signature

    1. SCHEDULE 1

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

      1. PART I DEFINITIONS

      2. PART II GENERAL INSTRUCTIONS FOR THE TAKING OF SAMPLES

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

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

        3. 3.A sample shall not be drawn from any part of...

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

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

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

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

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

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

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

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

      3. PART III QUANTITATIVE REQUIREMENTS

        1. 1.Sampled portion

        2. 2.Incremental sample

        3. 3.Aggregate sample

        4. 4.Final sample

      4. PART IV TAKING AND PREPARATION OF SAMPLES

        1. 1.Incremental samples

        2. 2.Aggregate sample

        3. 3.Reduced sample

        4. 4.Final samples

      5. PART V MARKING, SEALING AND FASTENING UP OF .I-HE FINAL SAMPLE

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

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

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

      6. PART VI SAMPLING TABLES

    2. SCHEDULE 2

      METHODS OF ANALYSIS

      1. PART I

        1. 1.General

        2. 2.Reagents and Apparatus

        3. 3.Methods of Analysis

        4. 1.Preparation of the sample for analysis

        5. 2.Determination of ammoniacal nitrogen

        6. 3.(a) Determination of nitrate and ammoniacal nitrogen-Ulsch method

        7. 4.(a) Determination of nitrogen in calcium cyanamide-in the absence of...

        8. 5.Determination of total nitrogen in urea

        9. 6.Determination of cyanamide nitrogen

        10. 7.Determination of biuret in urea

        11. 8.(a) Determination of different forms of nitrogen-in the presence of...

        12. 9.(a) Extraction of total phosphorus-by mineral acids

        13. 10.Determination of extracted phosphorus

        14. 11.Determination of water-soluble potassium

        15. 12.(a) Determination of water-soluble magnesium-atomic absorption spectro-photometric method

        16. 13.(a) Determination of total magnesium-atomic absorption spectrophoto-metric method

        17. 14.Determination of chlorides, in the absence of organic matter

        18. 15.(a) Determination of fineness of grinding—dry method

        19. 16.Methods of analysis and test procedures for ammonium nitrate fertiliser...

        20. A.Methods for the application of thermal cycles

        21. B.Determination of oil retention

        22. C.Determination of the combustible ingredients

        23. D.Determination of the pH value

        24. E.Determination of particle size

        25. F.Determination of the chloride content (as chloride ion)

        26. G.Determination of copper

      2. 1. PREPARATION OF THE SAMPLE FOR ANALYSIS

        1. 1.SCOPE

        2. 2.PRINCIPLE

        3. 2.1.Solid fertilisers: the preparation of a final sample received at...

        4. 2.2.Fluid fertilisers: the final sample is mixed by shaking to...

        5. 3.APPARATUS

        6. 3.1.Sample divider (optional).

        7. 3.2.Sieves with apertures of 0.2 mm and 0.5 mm.

        8. 3.3.250 ml flasks, stoppered.

        9. 3.4.Porcelain pestle and mortar or grinder.

        10. 4.CHOICE OF TREATMENT TO BE USED

        11. 4.1.Final samples which must not be ground

        12. 4.2.Final samples which must be divided and part of which must be ground

        13. 4.3.Final samples in respect of which all determinations are carried out on a ground product

        14. 5.METHOD

        15. 6.SPECIAL CASES

        16. 7.FLUID FERTILISERS

      3. 2. DETERMINATION OF AMMONIACAL NITROGEN

        1. 1.SCOPE

        2. 2.FIELD OF APPLICATION

        3. 3.PRINCIPLE

        4. 4.REAGENTS

        5. 4.1.Hydrochloric acid solution, 50% (V/V): dilute an appropriate volume of...

        6. 4.8.Sodium hydroxide solution, 30 g per 100 ml ammonia free....

        7. 4.9.Indicator solutions: Mixed indicator: (4.9.1) Solution A: dissolve 1 g...

        8. 4.10.Anti-bump granules of pumice stone, washed in hydrochloric acid and...

        9. 4.11.Ammonium sulphate.

        10. 5.APPARATUS

        11. 5.1.Distillation apparatus consisting of a round-bottomed flask of suitable capacity...

        12. 5.2.Rotary shaker, 35 to 40 turns per minute.

        13. 6.PREPARATION OF SAMPLE

        14. 7.PROCEDURE

        15. 7.2.Determination

        16. Note:

        17. 7.3.Blank

        18. 7.4.Control test

        19. 8.EXPRESSION OF THE RESULT

        20. TABLE FOR METHOD 2

        21. Variant (a)

        22. Variant (b)

        23. Variant (c)

      4. 3a. DETERMINATION OF NITRIC AND AMMONIACAL NITROGEN — ULSCH METHOD

        1. 1.SCOPE

        2. 2.FIELD OF APPLICATION

        3. 3.PRINCIPLE

        4. 4.REAGENTS

        5. 4.1.Hydrochloric acid solution, 50% (V/V): dilute an appropriate volume of...

        6. 4.2.Sulphuric acid, 0.1 N solution.

        7. 4.3.Sodium or potassium hydroxide, 0.1 N solution, carbonate free.

        8. 4.4.Sulphuric acid solution, approximately 30% H2SO4 (W/V), ammonia free.

        9. 4.5.Powdered iron reduced in hydrogen. (The prescribed quantity of iron...

        10. 4.6.Sodium hydroxide solution, 30 g per 100 ml, ammonia free....

        11. 4.7.Indicator solutions: Mixed indicator: (4.7.1) Solution A: dissolve 1 g...

        12. 4.8.Anti-bump granules of pumice stone, washed in hydrochloric acid and...

        13. 4.9.Sodium nitrate.

        14. 5.APPARATUS

        15. 6.PREPARATION OF SAMPLE

        16. 7.PROCEDURE

        17. 7.1.Preparation of the solution

        18. 7.2.Determination

        19. 7.3.Blank test

        20. 7.4.Control test

        21. 8.EXPRESSION OF THE RESULTS

      5. 3b. DETERMINATION OF NITRIC AND AMMONIACAL NITROGEN — ARND METHOD

        1. 1.SCOPE

        2. 2.FIELD OF APPLICATION

        3. 3.PRINCIPLE

        4. 4.REAGENTS

        5. 4.1.Hydrochloric acid solution, 50% (V/V): dilute an appropriate volume of...

        6. 4.8.Sodium hydroxide solution, approximately 2 N.

        7. 4.9.Arnd’s alloy—powdered so as to pass through a sieve with...

        8. 4.10.20% Magnesium chloride solution: dissolve 200 g magnesium chloride (MgC12.6H2O)...

        9. 4.11.Indicator solutions: Mixed indicator: (4.11.1) Solution A: dissolve 1 g...

        10. 4.12.Anti-bump granules of pumice stone washed in hydrochloric acid and...

        11. 4.13.Sodium nitrate.

        12. 5.APPARATUS

        13. 6.PREPARATION OF SAMPLE

        14. 7.PROCEDURE

        15. 7.1.Preparation of the solution for analysis

        16. 7.2.Determination

        17. Note:

        18. 7.3.Blank test

        19. 7.4.Control test

        20. 8.EXPRESSION OF THE RESULTS

      6. 3c. DETERMINATION OF NITRIC AND AMMONIACAL NITROGEN — DEVARDA METHOD

        1. 1.SCOPE

        2. 2.FIELD OF APPLICATION

        3. 3.PRINCIPLE

        4. 4.REAGENTS

        5. 4.1.Hydrochloric acid solution, 50% (V/V): dilute an appropriate volume of...

        6. 4.8.Devarda’s alloy—powdered so that 90 to 100% will pass through...

        7. 4.9.Sodium hydroxide solution, 30 g per 100 ml ammonia free....

        8. 4.10.Indicator solutions: Mixed indicator: (4.10.1) Solution A: dissolve 1 g...

        9. 4.11.Ethanol, 95%.

        10. 4.12.Sodium nitrate.

        11. 5.APPARATUS

        12. 5.1.Distillation apparatus consisting of a round bottomed flask of suitable...

        13. 6.PREPARATION OF THE SAMPLE

        14. 7.PROCEDURE

        15. 7.1.Preparation of the solution for analysis

        16. 7.2.Determination

        17. (Note:

        18. 7.3.Blank test

        19. 7.4.Control test

        20. 8.EXPRESSION OF RESULTS

      7. 4a DETERMINATION OF THE TOTAL NITROGEN IN CALCIUM CYANAMlDE — IN THE ABSENCE OF NITRATE

        1. 1.SCOPE

        2. 2.FIELD OF APPLICATION

        3. 3.PRINCIPLE

        4. 4.REAGENTS

        5. 4.1.Sulphuric acid solution 50% (V/V): dilute an appropriate volume of...

        6. 4.2.Potassium sulphate.

        7. 4.3.Copper oxide (CuO) — 0.3 to 0.4 g for each...

        8. 4.4.Sodium hydroxide solution, 30 g per 100 ml, ammonia free....

        9. 4.11.Indicator solutions: Mixed indicator: (4.11.1) Solution A: dissolve 1 g...

        10. 4.12.Anti-bump granules of pumice stone, washed in hydrochloric acid and...

        11. 4.13.Potassium thiocyanate.

        12. 5.APPARATUS

        13. 5.1.Distillation apparatus. See Method 2.

        14. 6.PREPARATION OF SAMPLE

        15. 7.PROCEDURE

        16. 7.1.Preparation of the solution

        17. 7.2.Determination

        18. 7.3.Blank test

        19. 7.4.Control test

        20. 8.EXPRESSION OF THE RESULT

      8. 4b. DETERMINATION OF TOTAL NITROGEN IN CALCIUM CYANAMIDE — IN THE PRESENCE OF NITRATE

        1. 1.SCOPE

        2. 2.FIELD OF APPLICATION

        3. 3.PRINCIPLE

        4. 4.REAGENTS

        5. 4.1.Sulphuric acid. (d = 1.84 g/ml).

        6. 4.2.Powdered iron reduced in hydrogen.

        7. 4.3.Potassium sulphate, finely pulverised. Sulphuric acid. 0.1 N solution. Sodium or potassium hydroxide, 0.1 N solution, carbonate free. for...

        8. 4.10.Indicator solutions:

        9. 4.11.Solution of stannous chloride:

        10. 4.12.Sodium hydroxide solution, 30 g per 100 ml, ammonia free....

        11. 4.13.Standard nitrate-ammoniacal solution:

        12. 4.14.Anti-bump granules of pumice stone, washed in hydrochloric acid and...

        13. 5.APPARATUS

        14. 6.PREPARATION OF THE SAMPLE

        15. 7.PROCEDURE

        16. 7.1.Preparation of the solution

        17. 7.2.Determination

        18. 7.3.Blank test

        19. 7.4.Control test

        20. 8.EXPRESSION OF THE RESULTS

      9. 5. DETERMINATION OF TOTAL NITROGEN IN UREA

        1. 1.SCOPE

        2. 2.FIELD OF APPLICATION

        3. 3.PRINCIPLE

        4. 4.REAGENTS

        5. 4.1.Sulphuric acid, concentrated, (d = 1.84 g/ml).

        6. 4.2.Sodium hydroxide solution, 30 g per 100 ml, ammonia free....

        7. 4.9.Indicator solutions:

        8. 4.10.Anti-bump granules of pumice stone, washed in hydrochloric acid and...

        9. 4.11.Urea.

        10. 5.APPARATUS

        11. 5.1.Distillation apparatus. See Method 2.

        12. 6.PREPARATION OF THE SAMPLE

        13. 7.PROCEDURE

        14. 7.1.Preparation of the solution

        15. 7.2.Determination

        16. 7.3.Blank test

        17. 7.4.Control test

        18. 8.EXPRESSION OF THE RESULT

      10. 6. DETERMINATION OF CYANAMIDE NITROGEN

        1. 1.SCOPE

        2. 2.FIELD OF APPLICATION

        3. 3.PRINCIPLE

        4. 4.REAGENTS

        5. 4.1.Glacial acetic acid.

        6. 4.2.Ammonia solution: dilute 1 volume of ammonia (d = 0.88...

        7. 4.3.Ammoniacal silver solution, according to Tollens, freshly prepared: mix 500...

        8. 4.4.Concentrated sulphuric acid (d = 1.84 g/ml).

        9. 4.5.Potassium sulphate.

        10. 4.6.Copper oxide (CuO), 0.3-0.4 g for each determination or an...

        11. 4.7.Sodium hydroxide solution, 30 g per 100 ml, ammonia free....

        12. 4.8.Sulphuric acid, 0.1 N solution.

        13. 4.9.Sodium or potassium hydroxide, 0.1 N solution.

        14. 4.10.Indicator solutions: Mixed indicator: (4.10.1) Solution A: dissolve 1 g...

        15. 4.11.Anti-bump granules of pumice stone, washed in hydrochloric acid and...

        16. 4.12.Potassium thiocyanate.

        17. 5.APPARATUS

        18. 5.1.Distillation apparatus. See Method 2

        19. 5.2.500 ml graduated flask (for example Stohmann).

        20. 5.3.Rotary shaker, 35-40 turns per minute.

        21. 6.PREPARATION OF THE SAMPLE

        22. 7.PROCEDURE

        23. 7.1.Safety precaution

        24. 7.2.Preparation of the solution for analysis

        25. 7.3.Determination

        26. 7.4.Blank test

        27. 7.5.Control test

        28. 8.EXPRESSION OF RESULTS

      11. 7. DETERMINATION OF BIURET IN UREA

        1. 1.SCOPE

        2. 2.FIELD OF APPLICATION

        3. 3.PRINCIPLE

        4. 4.REAGENTS

        5. 4.1.Methanol.

        6. 4.2.Sulphuric acid solution, approximately 0.1 N.

        7. 4.3.Sodium hydroxide solution, approximately 0.1 N.

        8. 4.4.Alkaline solution of potassium sodium tartrate: in a 1 litre...

        9. 4.5.Copper sulphate solution:

        10. 4.6.Biuret standard solution:

        11. 4.7.Methyl red indicator solution:

        12. 5.APPARATUS

        13. 5.1.Spectrophotometer.

        14. 6.PREPARATION OF SAMPLE

        15. 7.PROCEDURE

        16. 7.1.Preparation of the standard curve

        17. 7.2.Preparation of solution for analysis

        18. 7.3.Determination

        19. 8.EXPRESSION OF RESULTS

      12. 8a. DETERMINATION OF DIFFERENT FORMS OF NITROGEN IN THE SAME SAMPLE — IN THE PRESENCE OF CYANAMIDE NITROGEN

        1. 1.SCOPE

        2. 2.FIELD OF APPLICATION

        3. 3.PRINCIPLE

        4. 3.1.Total soluble and insoluble nitrogen

        5. 3.2.Forms of soluble nitrogen

        6. 4.REAGENTS

        7. 4.1.Potassium sulphate.

        8. 4.2.Iron powder, reduced with hydrogen (the prescribed quantity of iron...

        9. 4.3.Potassium thiocyanate.

        10. 4.4.Potassium nitrate.

        11. 4.5.Ammonium sulphate.

        12. 4.6.Urea.

        13. 4.7.Sulphuric acid solution: dilute an appropriate volume of sulphuric acid...

        14. 4.8.Sulphuric acid, 0.2 N solution.

        15. 4.9.Sodium hydroxide solution, 30 g per 100 ml. ammonia free....

        16. 4.10.Sodium or potassium hydroxide, 0.2 N solution, free from carbonates....

        17. 4.11.Stannous chloride solution: dissolve 120 g of stannous chloride (SnC...

        18. 4.12.Sulphuric acid, concentrated (d = 1.84 g/ml).

        19. 4.13.Hydrochloric acid solution: dilute an appropriate volume of hydrochloric acid...

        20. 4.14.Glacial acetic acid.

        21. 4.15.Sulphuric acid solution, approximately 30% (W/V) H2SO4.

        22. 4.16.Ferrous sulphate, crystalline, FeSO4.7H2O.

        23. 4.17.Sulphuric acid, 0.1 N solution.

        24. 4.18.Octan-1-o 1.

        25. 4.19.Potassium carbonate, saturated solution.

        26. 4.20.Sodium or potassium hydroxide, 0.1 N solution, free from carbonate....

        27. 4.21.Barium hydroxide, saturated solution.

        28. 4.22.Sodium carbonate solution, 10 g per 100 ml.

        29. 4.23.Hydrochloric acid, 2 N solution.

        30. 4.24.Hydrochloric acid, 0.1 N solution.

        31. 4.25.Urease solution:

        32. 4.26.Xanthydrol solution, 5 g per 100 ml in ethanol or...

        33. 4.27.Copper oxide (CuO): 0.3 to 0.4 g per determination or...

        34. 4.28.Anti-bump granules washed in hydrochloric acid and ignited.

        35. 4.29.Indicator solutions: Mixed indicator solution: (4.29.1) Solution A: dissolve 1...

        36. 4.30.Indicator papers:

        37. 4.3.Ethanol or methanol: solution 95%.

        38. 5.APPARATUS

        39. 5.1.Distillation apparatus. See Method 2.

        40. 5.2.Apparatus for the determination of ammoniacal nitrogen according to analytical...

        41. 5.3.Apparatus for I-tie estimation of urea nitrogen according to the...

        42. 5.4.Rotary shaker, 35-40 turns per minute.

        43. 5.pH meter.

        44. 5.6.Laboratory oven.

        45. 5.7.Sintered glass crucibles, diameter of pores 5 to 15 microns....

        46. 6.PREPARATION OF THE SAMPLE

        47. 7.PROCEDURE

        48. 7.1.Total soluble and insoluble nitrogen

        49. 7.2.Forms of soluble nitrogen

        50. 8.VERIFICATION OF THE RESULTS

        51. 8.1.In certain cases, a difference may be found between the...

        52. 8.2.Before each analysis, check that the apparatus is working properly...

      13. 8b. DETERMINATION OF DIFFERENT FORMS OF NITROGEN IN THE SAME SAMPLE — IN THE ABSENCE OF CYANAMIDE NITROGEN

        1. 1.SCOPE

        2. 2.FIELD OF APPLICATION

        3. 3.PRINCIPLE

        4. 3.1.Total soluble nitrogen

        5. 3.2.Total soluble nitrogen except nitric nitrogen, by Kjeldahl digestion after...

        6. 3.3.Nitric nitrogen, by difference: between 3.1.2 and 3.2 and/or between...

        7. 3.4.Ammoniacal nitrogen, by cold distillation of a weak alkaline solution;...

        8. 3.5.Urea nitrogen, either: (3.5.1) By conversion using urease, into ammonia,...

        9. 4.REAGENTS

        10. 4.1.Potassium sulphate.

        11. 4.2.Iron powder, reduced with hydrogen (the prescribed quantity of iron...

        12. 4.3.Potassium nitrate.

        13. 4.4.Ammonium sulphate.

        14. 4.5.Urea.

        15. 4.6.Sulphuric acid, 0.2 N solution.

        16. 4.7.Sodium hydroxide solution, 30 g per 100 ml, ammonia free....

        17. 4.8.Sodium or potassium hydroxide, 0.2 N solution, free of carbonates....

        18. 4.9.Sulphuric acid (d = 1.84 g/ml).

        19. 4.10.Hydrochloric acid solution: dilute an appropriate volume of hydrochloric acid...

        20. 4.11.Glacial acetic acid.

        21. 4.12.Sulphuric acid, solution approximately 30% (W/V) H2SO4.

        22. 4.13.Ferrous sulphate, crystalline FeSO4.7H2O.

        23. 4.14.Sulphuric acid, 0.1 N solution.

        24. 4.15.Octal-l-ol.

        25. 4.16.Potassium carbonate, saturated solution.

        26. 4.17.Sodium or potassium hydroxide, 0.1 N solution.

        27. 4.18.Barium hydroxide, saturated solution.

        28. 4.19.Sodium carbonate solution, 10 g per 100 ml.

        29. 4.20.Hydrochloric acid, 2 N solution.

        30. 4.21.Hydrochloric acid, 0.1 N solution.

        31. 4.22.Urease solution: suspend 0.5 g active unease in 100 ml...

        32. 4.23.Xanthydrol solution, 5 g per 100 ml in ethanol or...

        33. 4.24.Catalyst: copper oxide (CuO), 0.3 to 0.4 g per determination,...

        34. 4.25.Anti-bump granules of pumice stone washed with hydrochloric acid and...

        35. 4.26.Indicator solutions: Mixed indicator (4.26.1) Solution A: dissolve 1 g...

        36. 4.27.Indicator papers: litmus, bromothymol blue (or other papers sensitive to...

        37. 4.28.Ethanol or methanol, 95% (V/V).

        38. 5.APPARATUS

        39. 5.1.Distillation apparatus. See Method 2.

        40. 5.2.Apparatus for determination of ammoniacal nitrogen. An example of recommended...

        41. 5.3.Apparatus for determination of urea nitrogen by the urease method...

        42. 5.4.Rotary shaker: 35 — 40 turns per min.

        43. 5.5.pH meter.

        44. 5.6.Sintered glass crucibles, diameter of pores 5 to 15 microns....

        45. 6.PREPARATION OF SAMPLE

        46. 7.PROCEDURE

        47. 7.1.Preparation of solution for analysis

        48. 7.2.Total nitrogen

        49. 7.3.Total nitrogen excluding nitric nitrogen

        50. 7.4.Nitric nitrogen is obtained: by difference between (7.2.4) — (7.5.3...

        51. 7.5.Ammoniacal nitrogen

        52. 7.6.Ureic nitrogen

        53. 1.Remarks

        54. 2.The titration may also be carried out using an indicator...

        55. 8.VERIFICATION OF RESULTS

        56. 8.1.Before each analysis, check the functioning of the apparatus and...

      14. 9a. EXTRACTION OF TOTAL PHOSPHORUS BY MINERAL ACIDS

        1. 1.SCOPE

        2. 2.FIELD OF APPLICATION

        3. 3.PRINCIPLE

        4. 4.REAGENTS

        5. 4.1.Sulphuric acid (d = 1.84 g/ml).

        6. 4.2.Nitric acid (d = 1.40 g/ml).

        7. 5.APPARATUS

        8. 5.1.A Kjeldahl flask, with a capacity of at least 500...

        9. 6.PREPARATION OF THE SAMPLE

        10. 7.PROCEDURE

        11. 7.1.Extraction

        12. 7.2.Determination

      15. 9b. EXTRACTION OF PHOSPHORUS BY 2% FORMIC ACID

        1. 1.SCOPE

        2. 2.FIELD OF APPLICATION

        3. 3.PRINCIPLE

        4. 4.REAGENT

        5. 4.1.Formic acid, 2% (20 g per litre): dilute 82 ml...

        6. 5.APPARATUS

        7. 5.1.500 ml graduated flask (for example Stohmann).

        8. 5.2.Rotary shaker, 35 — 40 turns per minute.

        9. 6.PREPARATION OF THE SAMPLE

        10. 7.PROCEDURE

        11. 7.1.Extraction

        12. 7.2.Determination

      16. 9c. EXTRACTION OF PHOSPHORUS BY 2% CITRIC ACID

        1. 1.SCOPE

        2. 2.FIELD OF APPLICATION

        3. 3.PRINCIPLE

        4. 4.REAGENT

        5. Note:

        6. 5.APPARATUS

        7. 6.PREPARATION OF THE SAMPLE

        8. 7.PROCEDURE

        9. 7.1.Extraction

        10. 7.2.Determination

      17. 9d. EXTRACTION OF PHOSPHORUS BY NEUTRAL AMMONIUM CITRATE

        1. 1.SCOPE

        2. 2.FIELD OF APPLICATION

        3. 3.PRINCIPLE

        4. 4.REAGENTS

        5. 4.1.Neutral ammonium citrate solution (pH = 7.0). This solution must...

        6. 5.APPARATUS

        7. 5.1.pH meter.

        8. 5.2.Water bath which can be set thermostatically at 65°C, equipped...

        9. 6.PREPARATION OF THE SAMPLE

        10. 7.PROCEDURE

        11. 7.1.Extraction

        12. 7.2.Determination

      18. 9e. EXTRACTION OF PHOSPHORUS BY ALKALINE AMMONIUM CITRATE (PETERMANN'S METHOD) AT 65°C

        1. 1.SCOPE

        2. 2.FIELD OF APPLICATION

        3. 3.PRINCIPLE

        4. 4.REAGENTS

        5. 4.1.Petermann’s solution

        6. Characteristics:

        7. Preparation ,from diammonium citrate:

        8. Preparation from citric acid and ammonia:

        9. Check the ammoniacal nitrogen content as follows:

        10. 5.APPARATUS

        11. 5.1.Water bath which can be maintained at a temperature of...

        12. 5.2.500 ml graduated flask (for example Stohmann flask).

        13. 6.PREPARATION OF SAMPLE

        14. 7.PROCEDURE

        15. 7.1.Extraction

        16. 7.2.Determination

      19. 9f EXTRACTION OF PHOSPHORUS BY ALKALINE AMMONIUM CITRATE (PETERMANN'S METHOD) AT AMBIENT TEMPERATURE

        1. 1.SCOPE

        2. 2.FIELD OF APPLICATION

        3. 3.PRINCIPLE

        4. 4.REAGENT

        5. 5.APPARATUS

        6. 5.1.250 ml graduated flask (for example Stohmann).

        7. 5.2.Rotary shaker, 35 — 40 turns per minute.

        8. 6.PREPARATION OF THE SAMPLE

        9. 7.PROCEDURE

        10. 7.1.Extraction

        11. 7.2.Determination

      20. 9g. EXTRACTION OF PHOSPHORUS BY JOULIE'S ALKALINE AMMONIUM CITRATE

        1. 1.SCOPE

        2. 2.FIELD OF APPLICATION

        3. 3.PRINCIPLE

        4. 4.REAGENTS

        5. 4.1.Joulie’s alkaline solution of ammonium citrate: This solution contains 400...

        6. 4.2.8 — Hydroxyquinoline, (oxine), powdered.

        7. 5.APPARATUS

        8. 5.1.Rotary shaker, 35 — 40 turns per minute.

        9. 6.PREPARATION OF THE SAMPLE

        10. 7.PROCEDURE

        11. 7.1.Extraction

        12. 7.2.Determination

        13. 8.APPENDIX

      21. 9h. EXTRACTION OF PHOSPHORUS BY WATER

        1. 1.SCOPE

        2. 2.FIELD OF APPLICATION

        3. 3.PRINCIPLE

        4. 4.APPARATUS

        5. 4.1.500 ml graduated flask (for example Stohmann).

        6. 4.2.Rotary shaker, 35 — 40 turns per minute.

        7. 5.PREPARATION OF THE SAMPLE

        8. 6.PROCEDURE

        9. 6.1.Extraction

        10. 6.2.Determination Determine the phosphorus according to Method 10, on an...

      22. 10. DETERMINATION OF EXTRACTED PHOSPHORUS

        1. 1.SCOPE

        2. 2.FIELD OF APPLICATION

        3. 3.PRINCIPLE

        4. 4.REAGENTS

        5. 4.1.Concentrated nitric acid (d = 1.40 g/ml).

        6. 4.2.Molybdate reagent: Preparation of the reagent based on sodium molybdate:...

        7. 5.APPARATUS

        8. 5.1.Filter crucible with porosity of 5 to 20 microns.

        9. 5.2.Drying oven regulated at 250°C f 10°C.

        10. 5.3.Sintered glass funnel with porosity of 5 to 20 microns....

        11. 6.PROCEDURE

        12. 6.1.Treatment of the solution

        13. 6.2.Hydrolysis Bring the contents of the Erlenmeyer flask to the...

        14. 6.3.Weighing the crucible

        15. 6.4.Precipitation

        16. 6.5.Filtering and washing

        17. 6.6.Drying and weighing

        18. 6.7.Blank test

        19. 6.8.Control test

        20. 7.EXPRESSION OF THE RESULTS

      23. 11. DETERMINATION OF WATER-SOLUBLE POTASSIUM

        1. 1.SCOPE

        2. 2.FIELD OF APPLICATION

        3. 3.PRINCIPLE

        4. 4.REAGENTS

        5. 4.1.Formaldehyde, 25 — 35% solution, filter if necessary before use....

        6. 4.2.Potassium chloride.

        7. 4.3.Sodium hydroxide. 10 N solution. Care should be taken to...

        8. 4.4.Indicator solution: dissolve 0.5 g phenolphthalein in 100 ml 90%...

        9. 4.5.EDTA solution: 4 g of the dihydrated disodium salt of...

        10. 4.6.STPB solution: dissolve 32.5 g sodium tetraphenylborate in 480 ml...

        11. 4.7.Liquid for washing: dilute 20 ml of the STPB solution...

        12. 4.8.Bromine water: saturated bromine solution in water.

        13. 5.APPARATUS

        14. 5.1.Filter crucibles with a porosity of 5 to 20 microns....

        15. 5.2.Oven regulated at 120 ± 10°C.

        16. 6.PREPARATION OF THE SAMPLE

        17. 7.PROCEDURE

        18. 7.1.Extraction Weigh to the nearest 0.001 g, 10 g of...

        19. Note:

        20. 7.2.Determination

        21. 7.3.Weighing the crucible

        22. 7.4.Precipitation

        23. 7.5.Filtering and washing

        24. 7.6.Drying and weighing

        25. 7.7.Blank test

        26. 7.8.Control test

        27. 8.EXPRESSION OF RESULTS

        28. 8.1.Method of calculation and formulae

      24. 12a. DETERMINATION OF WATER-SOLUBLE MAGNESIUM — ATOMIC ABSORPTION SPECTROPHOTOMETRlC METHOD

        1. 1.SCOPE

        2. 2.FIELD OF APPLICATION

        3. 3.PRINCIPLE

        4. 4.REAGENTS

        5. 4.1.Hydrochloric acid, N solution (approximately).

        6. 4.2.Hydrochloric acid, 0.5 N solution.

        7. 4.3.Magnesium standard solution: dissolve 1.013 g magnesium sulphate (MgSO4.7H2O) in...

        8. 4.4.Strontium chloride solution: dissolve 15 g strontium chloride (SrCl2.6H2O) in...

        9. 5.APPARATUS

        10. 5.1.Atomic absorption spectrophotometer with a magnesium lamp (285.2 nm).

        11. 6.PREPARATION OF SAMPLE

        12. 7.PROCEDURE

        13. 7.1.Extraction

        14. 7.2.Preparation of the sample solution

        15. 7.3.Blank solution

        16. 7.4.Standard solutions for calibration

        17. 7.5.Measurement

        18. 8.EXPRESSION OF THE RESULTS

      25. 2b. DETERMINATION OF WATER-SOLUBLE MAGNESIUM —EDTA METHOD

        1. 1.SCOPE

        2. 2.FIELD OF APPLICATION

        3. 3.PRINCIPLE

        4. 4.REAGENTS

        5. 4.1.Magnesium solution, 0.05 M: weigh out 2.016 g magnesium oxide,...

        6. 4.2.EDTA solution, 0.05 M: dissolve 18.61 g of the dihydrated...

        7. 4.3.Calcium solution 0.05 M: weigh out 5.004 g of dry...

        8. 4.4.Calcein indicator: carefully mix in a mortar 1 ,g calcein...

        9. 4.5.Calcon carbonic acid indicator: dissolve 400 mg calcon carbonic acid...

        10. 4.6.Eriochrome black-T indicator: dissolve 300 mg eriochrome black-T in a...

        11. 4.7.Potassium cyanide solution, 2 g per 100 ml.

        12. 4.8.Solution of potassium hydroxide and potassium cyanide: dissolve 280 g...

        13. 4.9.pH 10 buffer solution: dissolve 33 g ammonium chloride in...

        14. 5.APPARATUS

        15. 5.1.Magnetic or mechanical stirrer.

        16. 5.2.pH-meter.

        17. 6.PREPARATION OF THE SAMPLE

        18. 7.PROCEDURE

        19. 7.1.Extraction

        20. 7.2.Control test

        21. 7.3.Determination

        22. 8.EXPRESSION OF THE RESULTS

      26. 13a. DETERMINATION OF TOTAL MAGNESIUM -ATOMIC ABSORPTION SPECTROPHOTOMETRIC METHOD

        1. 1.SCOPE This method is for the determination of total magnesium....

        2. 2.FIELD OF APPLICATION

        3. 3.PRINCIPLE

        4. 4.REAGENT

        5. 4.1.Hydrochloric acid solution 50% (V/V): dilute an appropriate volume of...

        6. 4.2.Hydrochloric acid, N solution (approximately).

        7. 4.3.Hydrochloric acid, 0.5 N solution.

        8. 4.4.Magnesium solution: dissolve 1 ,013 g magnesium sulphate (MgSO4.7H2O) in...

        9. 4.5.Strontium chloride solution: dissolve 75 g strontium chloride (SrCl2.6H2O) in...

        10. 5.APPARATUS

        11. 5.1.Atomic absorption spectrophotometer with a magnesium lamp (285.2 nm).

        12. 6.PREPARATION OF SAMPLE

        13. 7.PROCEDURE

        14. 7.1.Extraction

        15. 7.2.Preparation of the sample solution

        16. 7.3.Blank solution

        17. 7.4.Standard solutions for calibration

        18. 7.5.Measurement

        19. 8.EXPRESSION OF THE RESULTS

      27. 13b. DETERMINATION OF TOTAL MAGNESIUM —EDTA METHOD

        1. 1.SCOPE

        2. 2.FIELD OF APPLICATION

        3. 3.PRINCIPLE

        4. 4.REAGENTS

        5. 4.1.Magnesium solution, 0.05 M: weigh out 2.016 g of magnesium...

        6. 4.2.EDTA solution 0.05 M: dissolve 18.61 g of the dihydrated...

        7. 4.3.Calcium solution 0.05 M: weigh out 5.004 g of dry...

        8. 4.4.Calcein indicator: carefully mix in a mortar 1 g of...

        9. 4.5.Calcon carbonic acid indicator: dissolve 400 mg of calcon carbonic...

        10. 4.6.Eriochrome black-T indicator: dissolve 300 mg of eriochrome black-T in...

        11. 4.7.Potassium cyanide solution, 2 g per 100 ml.

        12. 4.8.Solution of potassium hydroxide and potassium cyanide: dissolve 280 g...

        13. 4.9.pH 10.5 buffer solution: dissolve 33 g ammonium chloride in...

        14. 4.10.Hydrochloric acid solution: 50% (V/V): dilute an appropriate volume of...

        15. 4.11.Sodium hydroxide solution, 5 N.

        16. 5.APPARATUS

        17. 5.1.Magnetic or mechanical stirrer.

        18. 5.2.pH meter.

        19. 6.PREPARATION OF THE SAMPLE

        20. 7.PROCEDURE

        21. 7.1.Extraction

        22. 7.2.Control test

        23. 7.3.Determination

        24. Note:

        25. 8.EXPRESSION OF THE RESULTS

      28. 14. DETERMINATION OF CHLORIDES IN THE ABSENCE OF ORGANIC MATERIAL

        1. 1.SCOPE

        2. 2.FIELD OF APPLICATION

        3. 3.PRINCIPLE

        4. 4.REAGENTS

        5. 4.1.Nitrobenzene or diethyl ether.

        6. 4.2.Nitric acid, 10 N solution.

        7. 4.3.Indicator solution: dissolve 40 g of ferric ammonium sulphate [Fe2(SO4)3.(NH4)2SO4.24H2O]...

        8. 4.4.Silver nitrate, 0.1 N solution.

        9. 4.5.Ammonium thiocyanate, 0.1 N solution. Preparation: since this salt is...

        10. 5.APPARATUS

        11. 5.1.Rotary shaker, 35 — 40 turns per minute.

        12. 6.PREPARATION OF SAMPLE

        13. 7.PROCEDURE

        14. 7.1.Extraction

        15. 7.2.Determination

        16. Note:

        17. 7.3.Blank test

        18. 7.4.Control test

        19. 8.EXPRESSION OF THE RESULT

      29. 15a. DETERMINATION OF FINENESS OF GRINDING — DRY METHOD

        1. 1.SCOPE

        2. 2.FIELD OF APPLICATION

        3. 3.PRINCIPLE

        4. 4.APPARATUS

        5. 4.1.Mechanical sieve shaker.

        6. 4.2.Sieves with apertures of 0.160 mm and 0.630 mm respectively...

        7. 5.PROCEDURE

        8. 6.EXPRESSION OF THE RESULTS

      30. 15b. DETERMINATION OF THE FINENESS OF GRINDING OF SOFT NATURAL PHOSPHATES

        1. 1.SCOPE

        2. 2.FIELD OF APPLICATION

        3. 3.PRINCIPLE

        4. 4.REAGENTS

        5. 5.APPARATUS

        6. 5.1.Sieves with apertures of 0.063 mm and 0.125 mm respectively...

        7. 5.2.Glass funnel of 20 cm diameter mounted on a stand....

        8. 5.3.Laboratory oven.

        9. 6.PROCEDURE

        10. 7.EXPRESSION OF THE RESULTS

        11. 8.REMARK

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

        1. A.

          Methods for the Application of Thermal Cycles

          1. 1.SCOPE AND FIELD OF APPLICATION

          2. 2.THERMAL CYCLES

          3. 2.1.Field of application This procedure is for thermal cycling prior...

          4. 2.2.Principle and definition

          5. 2.3.Apparatus

          6. 2.4.Procedure

        2. B.

          Determination of Oil Retention

          1. 1.SCOPE AND FIELD OF APPLICATION

          2. 2.DEFINITION

          3. 3.PRINCIPLE

          4. 4.REAGENT

          5. 5.APPARATUS

          6. 5.1.Balance, capable of weighing to the nearest 0.01 gram.

          7. 5.2.Beakers, of capacity 500 ml.

          8. 5.3.Funnel, of plastic materials, preferably with a cylindrical wall at...

          9. 5.4.Test sieve, aperture 0.5 mm, fitting into the funnel (5.3)....

          10. Note:

          11. 5.5.Note:

          12. 5.6.Absorbent tissue (laboratory grade).

          13. 6.PROCEDURE

          14. 6.1.Two individual determinations are carried out in quick succession on...

          15. 6.3.Remove particles smaller than 0.5 mm using the test sieve...

          16. 6.3.Filter the entire contents of the beaker through the funnel...

          17. 6.4.Lay two sheets of filter paper (5.5) (about 500 ×...

          18. 6.5.Repeating the rolling procedure and reweighing

          19. 7.EXPRESSION OF RESULTS

          20. 7.1.Method of calculation and formula

        3. C.

          Determination of the Combustible Ingredients

          1. 1.SCOPE AND FIELD OF APPLICATION

          2. 2.PRINCIPLE

          3. 3.REAGENTS

          4. 3.1.Analytical-grade chromium VI oxide; Cr-(VI)-03.

          5. 3.2.Sulphuric acid diluted to 60% by volume: pour 360 ml...

          6. 3.3.Silver nitrate: 0.1 M solution.

          7. 3.4.Barium hydroxide: weigh out 15 grams of barium hydroxide (Ba(OH)2.8H2O),...

          8. 3.5.Hydrochloric acid: 0.1 M standard solution.

          9. 3.6.Sodium hydroxide: 0.1 M standard solution.

          10. 3.7.Bromophenol blue: solution of 0.4 grams per litre in water....

          11. 3.8.Phenolphthalein: solution of 2 grams per litre in 60% by...

          12. 3.9.Soda lime: particle dimensions, about 1.0 to 1.5 mm.

          13. 3.10.Demineralised water, freshly boiled to remove carbon dioxide.

          14. 4.APPARATUS

          15. 4.1.Standard laboratory equipment, in particular: filter crucible with a plate...

          16. 4.2.Compressed nitrogen supply.

          17. 4.3.Apparatus made up of the following parts and assembled, if...

          18. Caution:

          19. 5.PROCEDURE

          20. 5.1.Sample for analysis

          21. 5.2.Removal of carbonates

          22. 5.3.Oxidation and absorption

          23. 5.4.Measurement of the carbonates originating from organic material

          24. 6.BLANK TEST

          25. 7.EXPRESSION OF RESULTS

        4. D.

          Determination of the pH Value

          1. 1.SCOPE AND FIELD OF APPLICATION

          2. 2.PRINCIPLE

          3. 3.REAGENTS

          4. 3.1.Buffer solution. pH 6.88 at 20°C

          5. 3.2.Buffer solution pH 4.00 at 20°C

          6. 3.3.Commercially available pH standard solutions may be used.

          7. 4.APPARATUS

          8. 5.PROCEDURE

          9. 5.1.Calibration of the pH meter

          10. 5.2.Determination

          11. 6.EXPRESSION OF RESULTS

        5. E.

          Determination of the Particle Size

          1. 1.SCOPE AND FIELD OF APPLICATION

          2. 2.PRINCIPLE

          3. 3.APPARATUS

          4. 3.1.200 mm diameter woven-wire test sieves to BS 410 (1986)...

          5. 3.2.Balance to weigh to 0.1 gram.

          6. 3.3.Mechanical sieve shaker (if available) capable of imparting both vertical...

          7. 4.PROCEDURE

          8. 4.1.The sample is divided representatively into portions of approximately 100...

          9. 4.2.Weigh one of these portions to the nearest 0.1 gram....

          10. 4.3.Arrange the nest of sieves in ascending order; receiver 0.5...

          11. 4.4.Shake by hand or machine, imparting both a vertical and...

          12. 4.5.Remove the sieves from the nest in turn and collect...

          13. 4.6.Weigh the material retained on each sieve and that collected...

          14. 5.EVALUATION OF THE RESULTS

          15. 5.1.Convert the fraction masses to a percentage of the total...

          16. 5.2.At least two separate analyses should be carried out and...

          17. 6.EXPRESSION OF RESULTS

        6. F.

          Determination of the Chlorine Content (as Chloride Ion)

          1. 1.SCOPE AND FIELD OF APPLICATION

          2. 2.PRINCIPLE

          3. 3.REAGENTS

          4. 3.1.Acetone AR.

          5. 3.2.Concentrated nitric acid (density at 20°C = 1.40 g/ml).

          6. 3.3.Silver nitrate 0.1 M standard solution. Store this solution in...

          7. 3.4.Silver nitrate 0.004 M standard solution — prepare this solution...

          8. 3.6.Potassium chloride, 0.1 M standard reference solution. Weigh, to the...

          9. 3.6.Potassium chloride, 0.004 M standard reference solution — prepare this...

          10. 4.APPARATUS

          11. 4.2.Bridge, containing a saturated potassium nitrate solution, connected to the...

          12. 4.3.Magnetic stirrer, with a Teflon-coated rod.

          13. 4.4.Microburette with fine-pointed tip, graduated in 0.01 ml divisions.

          14. 5.PROCEDURE

          15. 5.1.Standardisation of the silver nitrate solution

          16. 5.2.Blank Test

          17. 5.3.Check test

          18. 5.4.Determination

          19. 6.EXPRESSION OF RESULTS

        7. G.

          Determination of Copper

          1. 1.SCOPE AND FIELD OF APPLICATION

          2. 2.PRINCIPLE

          3. 3.REAGENTS

          4. 3.1.Hydrochloric acid (density at 20°C = 1.18 g/ml).

          5. 3.2.Hydrochloric acid, 6 M solution.

          6. 3.3.Hydrochloric acid, 0.5 M solution.

          7. 3.4.Ammonium nitrate.

          8. 3.5.Hydrogen peroxide, 30%.

          9. 3.6.Copper solution (stock): weigh, to the nearest 0.001 gram, 1...

          10. 4.APPARATUS

          11. 5.PROCEDURE

          12. 5.1.Preparation of the solution for analysis

          13. 5.2.Blank solution

          14. 5.3.Determination

          15. 5.4.Measurement

          16. 6.EXPRESSION OF THE RESULTS

      32. PART II

        1. 1.General

        2. 2.Reagents and Apparatus

        3. 3.Methods of Analysis

        4. 1. Preparation of the sample for analysis

        5. 2. Determination of moisture

        6. 3. Determination of total nitrogen — chromium powder reduction method

        7. 4. Determination of urea

        8. 5.a Extraction of phosphorus — by mineral acids (total phosphorus)

        9. b Extraction of phosphorus — by 2% citric acid

        10. 6. Determination of extracted phosphorus — spectrophotometric method

        11. 7.a Determination of potassium — gravimetric method

        12. b Determination of potassium — flame photometric method

        13. 8. Determination of total magnesium

        14. 9.a Determination of boron — titrimetric method

        15. b Determination of boron — spectrophotometric method

        16. 10. Determination of cobalt

        17. 11. Determination of molybdenum

        18. 12. Determination of copper

        19. 13. Determination of iron

        20. 14. Determination of manganese

        21. 15. Determination of the neutralising value in liming materials

        22. 16. Determination of fineness of products other than potassic basic slag

        23. 17. Determination of fineness of potassic basic stag

        24. 1. PREPARATION OF THE SAMPLE FOR ANALYSIS

          1. 1.INTRODUCTION

          2. 2.SCOPE AND FIELD OF APPLICATION

          3. 3.PRINCIPLE

          4. 3.1.Solid fertilisers: the whole final sample is ground to the...

          5. 3.2.Fluid fertilisers: the final sample is thoroughly mixed before each...

          6. 4.APPARATUS

          7. 4.1.Sample grinder capable of grinding the fertiliser to pass the...

          8. 4.2.Mortar and pestle of suitable material and size.

          9. 4.3.Sieves having square apertures of 0.18 mm, 0.5 mm and...

          10. 4.4.Sample containers of non-corrodible materials, with air-tight closures.

          11. 5.PROCEDURE

          12. WARNING

          13. 5.1.Grinding and sieving

          14. 5.2.Place the prepared sample in a clean container (4.4) and...

          15. 5.3.Before taking each test portion for analysis, the whole sample...

          16. 5.4.If the sample contains foreign matter which cannot be ground...

          17. 6.SPECIAL CASES

          18. 6.1.Samples not to be ground

          19. 6.2.Products which may be difficult to grind mechanically, including products with abnormal moisture or products which become doughy through grinding

          20. 6.3.Organic materials

          21. 6.4.Fertilisers comprising several different materials

          22. 7.FLUID FERTILISERS

        25. 2. DETERMINATION OF MOISTURE

          1. 1.SCOPE AND FIELD OF APPLICATION

          2. 2.PRINCIPLE

          3. 3.APPARATUS

          4. 3.1.Suitable containers with lids ensuring air-tight closure; the dimensions should...

          5. 3.2.Electricially heated oven, suitably ventilated and capable of being maintained...

          6. 4.PREPARATION OF SAMPLE

          7. 5.PROCEDURE

          8. 6.EXPRESSION OF THE RESULT

        26. 3. DETERMINATION OF TOTAL NITROGEN — CHROMIUM POWDER REDUCTION METHOD

          1. 1.SCOPE AND FIELD OF APPLICATION

          2. 2.PRINCIPLE

          3. 3.REAGENTS

          4. 3.1.Sodium hydroxide solution: 40 g per 100 ml, ammonia free....

          5. 3.2.Sulphuric acid, 0.1 N solution.

          6. 3.3.Sulphuric acid, 0.2 N solution.

          7. 3.4.Sulphuric acid, 0.5 N solution.

          8. 3.5.Sodium hydroxide, 0.2 N solution, carbonate free.

          9. 3.6.Chromium metal powder, 100 mesh, low nitrogen content.

          10. 3.7.Anti-bump granules of pumice stone, washed in hydrochloric acid and...

          11. 3.8.Anti-foaming agent, paraffin wax.

          12. 3.9.Sulphuric acid (d = 1.84 g/ml).

          13. 3.10.Hydrochloric acid (d = 1.18 g/ml).

          14. 3.11.Catalyst mixture: 1,000 g potassium sulphate and 50 g copper...

          15. 3.12.Indicator solutions: Mixed indicator: (3.12.1) mix 50 ml of 2...

          16. 3.13.pH indicator paper, wide range.

          17. 4.APPARATUS

          18. 5.PREPARATION OF SAMPLE

          19. 6.PROCEDURE

          20. 6.1.Reduction

          21. 2.0.g of the prepared sample, containing not more than 0.06...

          22. 6.2.Hydrolysis, when the fertiliser is known not to contain organic matter

          23. 6.3.Digestion, when the fertiliser is known to contain organic matter

          24. Note:

          25. 6.4.Distillation

          26. 6.5.Blank test

          27. 7.EXPRESSION OF THE RESULTS

        27. 4. DETERMINATION OF UREA

          1. 1.SCOPE AND FIELD OF APPLICATION

          2. 2.PRINCIPLE

          3. 3.REAGENTS

          4. 3.1.Activated charcoal.

          5. 3.2.Carrez solution I: dissolve 21.9 g zinc acetate dihydrate in...

          6. 3.3.Carrez solution II: 10.6 g potassium ferrocyanide per 100 ml....

          7. 3.4.Hydrochloric acid solution, 0.02 N.

          8. 3.5.Sodium acetate solution: 136 g sodium acetate trihydrate per litre....

          9. 3.6.4-dimethylamino-benzaldehyde solution: dissolve 1.6 g of 4-dimethylamino-benzaldehyde (4-DMAB) in 100...

          10. 3.7.Urea standard solution: 1 .O g per 100 ml (1...

          11. 4.APPARATUS

          12. 5.PREPARATION OF SAMPLE

          13. 6.PROCEDURE

          14. 6.1.Preparation of the solution for analysis

          15. 6.2.Determination

          16. 6.3.Calibration curve

          17. 7.EXPRESSION OF THE RESULTS

        28. 5a. EXTRACTION OF PHOSPHORUS BY MINERAL ACIDS (TOTAL PHOSPHORUS)

          1. 1.SCOPE AND FIELD OF APPLICATION

          2. 2.PRINCIPLE

          3. 3.REAGENTS

          4. 3.1.Sulphuric acid (d = 1.84 g/ml).

          5. 3.2.Nitric acid (d = 1.42 g/ml).

          6. 4.APPARATUS

          7. 4.1.A Kjeldahl flask, with a capacity of at least 500...

          8. 5.PREPARATION OF THE SAMPLE

          9. 6.PROCEDURE

          10. 6.1.Extraction

          11. 6.2.Determination

          12. Note

        29. 5b. EXTRACTION OF PHOSPHORUS BY 2% CITRIC ACID

          1. 1.SCOPE AND FIELD OF APPLICATION

          2. 2.PRINCIPLE

          3. 3.REAGENT

          4. 3.1.2% citric acid solution (20 g per litre), prepared from...

          5. 4.APPARATUS

          6. 4.1.Rotary shaker: 35 — 40 turns per minute.

          7. 5.PREPARATION OF THE SAMPLE

          8. 6.PROCEDURE

          9. 6.1.Extraction

          10. 6.2.Determination

        30. 6. DETERMINATION OF EXTRACTED PHOSPHORUS — SPECTROPHOTOMETRIC METHOD

          1. 1.SCOPE AND FIELD OF APPLICATION

          2. 2.PRINCIPLE

          3. 3.REAGENTS

          4. 3.1.Nitric acid (d =.42 g/ml).

          5. 3.2.Molybdovanadate reagent: dissolve separately 20 g ammonium molybdate and 0.47...

          6. 3.3.Phosphorus standard solution: dissolve 4.387 g potassium dihydrogen phosphate, previously...

          7. 3.4.Sodium hydroxide, approximately 5 N solution.

          8. 5.APPARATUS

          9. 5.PROCEDURE

          10. 5.1.Determination

          11. 5.2.Calibration

          12. 6.EXPRESSION OF THE RESULTS

        31. 7a. DETERMINATION OF POTASSIUM — GRAVIMETRIC METHOD

          1. 1.SCOPE AND FIELD OF APPLICATION

          2. 2.PRINCIPLE

          3. 3.REAGENTS

          4. 3.1.Formaldehyde, 25 – 35% solution, filtered if necessary before use....

          5. 3.2.Potassium chloride.

          6. 3.3.Sodium hydroxide, 10 N solution. Care should be taken to...

          7. 3.4.Indicator solution: Dissolve 0.5 g phenolphthalein in 100 ml 90%...

          8. 3.5.EDTA solution: 4 g of the dihydrated disodium salt of...

          9. 3.6.STPB solution: dissolve 32.5 g sodium tetraphenylborate in 480 ml...

          10. 3.7.Liquid for washing: dilute 20 ml of the STPB solution...

          11. 3.8.Hydrochloric acid (d = 1.18 g/ml).

          12. 4.APPARATUS

          13. 4.1.Filter crucibles with a porosity of 5 to 20 microns....

          14. 4.2.Oven regulated at 120°C + 10°C.

          15. 5.PREPARATION OF SAMPLE

          16. 6.PROCEDURE

          17. 6.1.Preparation of the solution for analysis

          18. 6.2.Determination

          19. 6.3.Weighing the crucible

          20. 6.4.Precipitation

          21. 6.5.Filtering and washing

          22. 6.6.Drying and weighing

          23. 6.7.Blank test

          24. 6.8.Control test

          25. 7.EXPRESSION OF THE RESULTS

        32. 7b. DETERMINATION OF POTASSIUM — FLAME PHOTOMETRIC METHOD

          1. 1.SCOPE AND FIELD OF APPLICATION

          2. 2.PRINCIPLE

          3. 3.REAGENTS

          4. 3.1.Ammonia solution (30% V/V): dilute 30 ml concentrated ammonia solution...

          5. 3.2.Ammonium oxalate solution: saturated aqueous solution.

          6. 3.3.Hydrochloric acid (d = 1.18 g/ml).

          7. 3.4.Potassium dihydrogen phosphate: dried for one hour at 105°C.

          8. 3.5.Potassium solution (stock): dissolve 3.4807 g potassium dihydrogen phosphate (3.4)...

          9. 3.6.Potassium solution (dilute): dilute 50 ml stock solution (3.5) to...

          10. 4.APPARATUS

          11. 4.1.Flame photometer.

          12. 5.PREPARATION OF SAMPLE

          13. 6.PROCEDURE

          14. 6.1.Preparation of the solution for analysis

          15. 6.2.Blank solution

          16. 6.3.Determination

          17. 6.4.Measurement

          18. 7.EXPRESSION OF THE RESULTS

        33. 8. DETERMINATION OF TOTAL MAGNESIUM

          1. 8.1.EXTRACTION OF TOTAL MAGNESIUM

          2. 1.SCOPE AND FIELD OF APPLICATION

          3. 1.1.This method is applicable to all fertilisers.

          4. 2.PRINCIPLE

          5. 2.1.Solubilisation by boiling in dilute hydrochloric acid.

          6. 3.REAGENTS

          7. 3.1.Diluted hydrochloric acid: One volume of hydrochloric acid (d =...

          8. 4.APPARATUS

          9. 4.1.Electric hot plate with adjustable temperature.

          10. 5.PREPARATION OF THE SAMPLE

          11. 5.1.See Method 1.

          12. 6.PROCEDURE

          13. 6.1.Test sample

          14. 6.2.Preparation of the solution

        34. 8.2 DETERMINATION OF MAGNESIUM BY ATOMIC ABSORPTION SPECTROPHOTOMETRY

          1. 1.SCOPE AND FIELD OF APPLICATION

          2. 2.PRINCIPLE

          3. 2.1.Determination of magnesium by atomic absorption spectrophotometry after appropriate dilution...

          4. 3.REAGENTS

          5. 3.1.Hydrochloric acid, 1 M solution.

          6. 3.2.Hydrochloric acid, 0.5 M solution.

          7. 3.3.Standard solution of magnesium, 1.00 mg/ml. (3.3.1) Dissolve 1.013 grams...

          8. 3.4.Strontium chloride solution

          9. 4.APPARATUS

          10. 4.1.Spectrophotometer fitted for atomic absorption, with a magnesium lamp, set...

          11. 4.2.Air-acetylene flame.

          12. 5.PREPARATION OF THE SAMPLE

          13. 5.1.See Method 8.1

          14. 6.PROCEDURE

          15. 6.1.Test sample

          16. 6.2.Preparation of the solution

        35. 8.2 DETERMINATION OF MAGNESIUM BY ATOMIC ABSORPTION SPECTROPHOTOMETRY

          1. 1.SCOPE AND FIELD OF APPLICATION

          2. 2.PRINCIPLE

          3. 2.1.Determination of magnesium by atomic absorption spectrophotometry after appropriate dilution...

          4. 3.REAGENTS

          5. 3.1.Hydrochloric acid, 1 M solution.

          6. 3.2.Hydrochloric acid, 0.5 M solution.

          7. 3.3.Standard solution of magnesium, 1.00 mg/ml. (3.3.1) Dissolve 1.013 grams...

          8. 3.4.Strontium chloride solution

          9. 4.APPARATUS

          10. 4.1.Spectrophotometer fitted for atomic absorption, with a magnesium lamp, set...

          11. 4.2.Air-acetylene flame.

          12. 5.PREPARATION OF THE SAMPLE

          13. 5.1.See Method 8.1

          14. 6.PROCEDURE

          15. 6.1.If the fertiliser has a declared magnesium (Mg) content of...

          16. 6.2.Using a pipette, take 10 ml of the extraction solution...

          17. 6.3.Dilute this solution (6.2) with the 0.5 M hydrochloric acid...

          18. 6.4.Preparation of blank solution

          19. 6.5.Preparation of calibration solutions

          20. 6.6.Measurement

          21. 7.EXPRESSION OF RESULTS

        36. 9a. DETERMINATION OF BORON — TITRIMETRIC METHOD

          1. 1.SCOPE AND FIELD OF APPLICATION

          2. 2.PRINCIPLE

          3. 3.REAGENTS

          4. 3.1.Calcium oxide.

          5. 3.2.Mannitol.

          6. 3.3.Sodium carbonate.

          7. 3.4.Hydrochloric acid solution 50% (V/V): dilute 50 ml concentrated hydrochloric...

          8. 3.5.Hydrochloric acid, 0.5 N solution.

          9. 3.6.Lead nitrate solution, 10 g per 100 ml.

          10. 3.7.Sodium hydroxide, 0.5 N solution.

          11. 3.8.Sodium hydroxide, 0.05 N solution, carbonate free.

          12. 3.9.Methyl red indicator solution: dissolve 0.1 g of methyl red...

          13. 3.10.Phenolphthalein indicator solution: dissolve 0.25 g phenolphthalein in 1.50 ml...

          14. 4.APPARATUS

          15. 4.1.pH meter.

          16. 5.PREPARATION OF SAMPLE

          17. 6.PROCEDURE

          18. 6.1.Preparation of the solution for analysis

          19. 6.2.Determination

          20. 7.EXPRESSION OF THE RESULT

        37. 9b. DETERMINATION OF BORON — SPECTROPHOTOMETRIC METHOD

          1. 1.SCOPE AND FIELD OF APPLICATION

          2. 2.PRINCIPLE

          3. 3.REAGENTS

          4. 3.1.Calcium oxide.

          5. 3.2.Sulphuric acid (d = 1.84 g/ml).

          6. 3.3.Carminic acid solution: dissolve 0.025 g carminic acid in sulphuric...

          7. 3.4.Hydrochloric acid solution 20% (V/V): dilute 20 ml hydrochloric acid...

          8. 3.6.Hydrazine hydrate (approximately 60% W/W solution).

          9. WARNING:

          10. 4.APPARATUS

          11. 4.1.Spectrophotometer with 10 mm cells.

          12. 5.PREPARATION OF THE SAMPLE

          13. 6.PROCEDURE

          14. 6.1.Preparation of the solution for analysis

          15. 6.2.Blank test

          16. 6.3.Determination

          17. 6.4.Calibration curve

          18. 7.EXPRESSION OF THE RESULTS

          19. Note

        38. 10. DETERMINATION OF COBALT

          1. 1.SCOPE AND FIELD OF APPLICATION

          2. 2.PRINCIPLE

          3. 3.REAGENTS

          4. 3.1.Sodium sulphate, anhydrous.

          5. 3.2.Toluene.

          6. 3.3.Hydrochloric acid, 2 N solution.

          7. 3.4.Hydrochloric acid solution, 50% (V/V): dilute 50 ml concentrated hydrochloric...

          8. 3.5.Hydrogen peroxide solution, 3% (10 volume).

          9. 3.6.Nitric acid solution, 30% (V/V): dilute 30 ml nitric acid...

          10. 3.7.2-nitroso-I-naphthol solution: dissolve 1 g of 2-nitroso-1-naphthol in 100 ml...

          11. 3.8.Sodium citrate solution: 40 g per 100 ml.

          12. 3.9.Sodium hydroxide, 2 N solution.

          13. 3.10.Cobalt solution (stock): weigh to the nearest 0.001 g, 0.670...

          14. 3.11.Cobalt solution (working standard): dilute the stock cobalt solution (3.10)...

          15. 4.APPARATUS

          16. 4.1.Spectrophotometer with 10 mm cells.

          17. 5.PREPARATION OF THE SAMPLE

          18. 6.PROCEDURE

          19. 6.1.Preparation of the solution for analysis

          20. 6.2.Determination

          21. 6.3.Calibration Curve

          22. 7.EXPRESSION OF THE RESULTS

        39. 11. DETERMINATION OF MOLYBDENUM

          1. 1.SCOPE AND FIELD OF APPLICATION

          2. 2.PRINCIPLE

          3. 3.REAGENTS

          4. 3.1.Hydrochloric acid, 50% (V/V): dilute 50 ml concentrated hydrochloric acid...

          5. 3.2.Hydrochloric acid, 2 N solution.

          6. 3.3.Hydrochloric acid, N solution.

          7. 3.4.Nitric acid solution, 30% (V/V): dilute 30 ml nitric acid...

          8. 3.6.Ammonium ferrous sulphate solution, 4 g per 100 ml.

          9. 3.7.Potassium thiocyanate solution, 40 g per 100 ml.

          10. 3.8.Sodium sulphate, anhydrous.

          11. 3.9.Stannous chloride solution: suspend 40 g stannous chloride dihydrate in...

          12. 3.10.Solvent mixture: mix equal volumes of carbon tetrachloride and 3-methylbutan-1-01....

          13. 4.APPARATUS

          14. 4.1.Spectrophotometer with 10 mm cells.

          15. 5.PREPARATION OF THE SAMPLE

          16. 6.PROCEDURE

          17. 6.1.,Preparation of the solution for analysis

          18. 6.2.Determination

          19. Note:

          20. 6.3.Note:

          21. 7.EXPRESSION OF THE RESULTS

        40. 12. DETERMINATION OF COPPER

          1. 1.SCOPE AND FIELD OF APPLICATION

          2. 2.PRINCIPLE

          3. 3.REAGENTS

          4. 3.1.Hydrochloric acid (d = 1.18 g/ml).

          5. 3.2.Hydrochloric acid, 6 N solution.

          6. 3.3.Hydrochloric acid, 0.5 N solution.

          7. 3.4.Hydrogen peroxide, approximately 100 volume, 30% by weight. Copper solution...

          8. 4.APPARATUS

          9. 4.1.Atomic absorption spectrophotometer with a copper lamp (324.8 nm).

          10. 5.PREPARATION OF SAMPLE

          11. 6.PROCEDURE

          12. 6.1.Preparation of the solution for analysis

          13. 6.2.Blank Solution

          14. 6.3.Determination

          15. 6.4.Measurement

          16. 7.EXPRESSION OF THE RESULTS

        41. 13. DETERMINATION OF IRON

          1. 1.SCOPE AND FIELD OF APPLICATION

          2. 2.PRINCIPLE

          3. 3.REAGENTS

          4. 3.1.Hydrochloric acid (d = 1.18 g/ml).

          5. 3.2.Hydrochloric acid, 6 N solution.

          6. 3.3.Hydrochloric acid, 0.5 N solution.

          7. 3.4.Hydrogen peroxide, approximately 100 volume, 30% by weight.

          8. 3.6.Lanthanum chloride solution: dissolve 12 g lanthanum oxide in 150...

          9. 4.APPARATUS

          10. 4.1.Atomic absorption spectrophotometer with an iron lamp (248.3 nm).

          11. 5.PREPARATION OF SAMPLE

          12. 6.PROCEDURE

          13. 6.1.Preparation of the solution for analysis

          14. 6.2.Blank solution

          15. 6.3.Determination

          16. 6.4.Measurement

          17. 7.EXPRESSION OF THE RESULTS

        42. 14. DETERMINATION OF MANGANESE

          1. 1.SCOPE AND FIELD OF APPLICATION

          2. 2.PRINCIPLE

          3. 3.REAGENTS

          4. 3.1.Hydrochloric acid (d = 1.18 g/ml).

          5. 3.2.Hydrochloric acid, 6 N solution.

          6. 3.3.Hydrochloric acid, 0.5 N solution. Manganese solution (stock):

          7. 3.5.Lanthanum chloride solution: dissolve 12 g lanthanum oxide in 150...

          8. 4.APPARATUS

          9. 4.1.Atomic absorption spectrophotometer with a manganese lamp (279.5 nm).

          10. 5.PREPARATION OF SAMPLE

          11. 6.PROCEDURE

          12. 6.1.Preparation of the solution for analysis

          13. 6.2.Blank solution

          14. 6.3.Determination

          15. 6.4.Measurement

          16. 7.EXPRESSION OF THE RESULTS

        43. 15. DETERMINATION OF THE NEUTRALISING VALUE IN LIMING MATERIALS

          1. 1.SCOPE AND FIELD OF APPLICATION

          2. 2.PRINCIPLE

          3. 3.REAGENTS

          4. 3.1.Hydrochloric acid, 0.5 N solution.

          5. 3.2.Sodium hydroxide, 0.5 N solution of carbonate free).

          6. 3.3.Phenolphthalein indicator solution: dissolve 0.25 g phenolphthalein in 150 ml...

          7. 4.PREPARATION OF SAMPLE

          8. 5.PROCEDURE

          9. 5.1.Determination

          10. 6.EXPRESSION OF THE RESULTS

        44. 16. DETERMINATION OF FINENESS OF PRODUCTS OTHER THAN POTASSIC BASIC SLAG

          1. 1.SCOPE AND FIELD OF APPLICATION

          2. 2.PRINCIPLE

          3. 3.APPARATUS

          4. 4.PROCEDURE

          5. 4.1.For sieving through 3.55 mm, 1.0 mm and 150 micron sieves

          6. 4.2.For sieving through 6.7 mm, 6.3 mm and 5 mm sieves

          7. 4.3.For sieving through a 45 mm sieve

          8. 4.4.Sieving

          9. 5.EXPRESSION OF THE RESULTS

        45. 17. DETERMINATION OF FINENESS OF POTASSIC BASIC SLAG

          1. 1.SCOPE AND FIELD OF APPLICATION

          2. 2.PRINCIPLE

          3. 3.APPARATUS

          4. 4.PROCEDURE

          5. 4.1.Preparation of the sample

          6. 4.2.Sieving

          7. 5.EXPRESSION OF THE RESULTS

      33. APPENDIX TO SCHEDULE 2

        1. KEY TO FIGURE 1

        2. KEY TO FIGURE 2

        3. KEY TO FIGURE 3

        4. KEY TO FIGURE 4

        5. KEY TO FIGURE 5

        6. KEY TO FIGURE 6

        7. KEY TO FIGURE 7

        8. KEY TO FIGURE 8

    3. SCHEDULE 3

  12. Explanatory Note

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