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3.—3.1 3.1.1 In the absence of nitrates, the sample is subjected to direct Kjeldahl digestion.
3.1.2In the presence of nitrates, the sample is subjected to Kjeldahl digestion after reduction with the aid of metallic iron and stannous chloride. In both cases, the ammonia is determined according to Method 2.
If analysis shows an insoluble nitrogen content of more than 0.5%, it is presumed that the fertiliser contains other forms of insoluble nitrogen not specified for fertilisers covered by the list in paragraph 2.
If analysis shows an insoluble nitrogen content of more than 0.5%, it is presumed that the fertiliser contains other forms of insoluble nitrogen not specified for fertilisers covered by the list in paragraph 2.
3.2 The following are determined from different aliquot parts taken from the same solution of the sample:
3.2.1.1In the absence of nitrates, by direct Kjeldahl digestion.
3.2.1.2In the presence of nitrates, by Kjeldahl digestion on an aliquot portion taken from the solution after reduction according to Ulsch, the ammonia being determined in both cases as described in Method 2.
3.2.2Total soluble nitrogen with the exception of nitric nitrogen, by Kjeldahl digestion after elimination in an acid medium of nitric nitrogen with ferrous sulfate, the ammonia being determined as described in Method 2.
3.2.3.1In the absence of calcium cyanamide, between (3.2.1.2) and (3.2.2) or between total soluble nitrogen (3.2.1.2) and the sum of ammoniacal nitrogen and ureic nitrogen (3.2.4 + 3.2.5).
3.2.3.2In the presence of calcium cyanamide, between (3.2.1.2) and (3.2.2) and between (3.2.1.2) and the sum of (3.2.4 + 3.2.5 + 3.2.6).
3.2.4.1Solely in the presence of ammoniacal nitrogen and ammoniacal + nitric nitrogen, by applying Method 2.
3.2.4.2In the presence of ureic nitrogen and/or cyanamide nitrogen, by cold distillation after making slightly alkaline, the ammonia being absorbed in a standard solution of sulfuric acid and determined as described in Method 2.
3.2.5Either
3.2.5.1By conversion using urease into ammonia which is titrated with a standard solution of hydrochloric acid.
or:
3.2.5.2By gravimetry with xanthydrol, although biuret will also be precipitated by xanthydrol, this should not give rise to a significant error in the determination since its level is generally low in absolute value in compound fertilisers.
or:
3.2.5.3.By difference, according to the following table:
Case | Nitric Nitrogen | Ammoniacal Nitrogen | Cyanamide Nitrogen | Difference |
---|---|---|---|---|
1 | Absent | Present | Present | (3.2.1.1)-(3.2.4.2 + 3.2.6) |
2 | Present | Present | Present | (3.2.2)-(3.2.4.2 + 3.2.6) |
3 | Absent | Present | Absent | (3.2.1.1)-(3.2.4.2) |
4 | Present | Present | Absent | (3.2.2)-(3.2.4.2) |
3.2.6Cyanamide nitrogen, by precipitation as a silver compound, the nitrogen being estimated in the precipitate by the Kjeldahl method.
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