SCHEDULE 2METHODS OF ANALYSIS

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

Remarks

2.

The titration may also be carried out using an indicator (4.26), although the change of colour is more difficult to observe.

7.6.2.Blank test

See 7.2.3.

7.6.3Expression of result

%nitrogen(ureic)=(a-A)×0.14Mmath

where:

  • a = ml of standard solution of sodium or potassium hydroxide (0.1 N) (4.17) used for the blank, carried out in exactly the same conditions as the analysis.

  • A = ml of standard solution of sodium or potassium hydroxide (0.1 N) (4.17) used for the analysis.

  • M = weight of the sample, in grams, present in the aliquot part taken for analysis.

7.6.4Gravimetric method using xanthydrol

Transfer by pipette into a 100 ml beaker a portion of the filtrate (7.1) containing not more than 20 mg urea. Add 40 ml acetic acid (4.11). Stir with a glass rod for one minute. Allow any precipitate to settle for five minutes. Filter, wash with a few ml acetic acid (4.11). Add 10 ml xanthydrol solution (4.23) to the filtrate drop by drop, stirring continuously with a glass rod. Allow to stand until the precipitate appears, then stir again for one or two minutes. Allow to stand for one and a half hours. Filter through a sintered glass crucible (5.6) which has been previously dried and weighed, using a slight reduction in pressure. Wash three times with 5 ml ethanol (4.28), without trying to remove all the acetic acid. Place in an oven at a temperature of 130°C for one hour (do not exceed 145°C). Allow to cool in a desiccator and weigh.

7.6.5Expression of result

%N(urea)=6.67×mMmath

where:

  • m = weight of the precipitate in grams.

  • M = weight of the sample, in grams, present in the aliquot part taken for analysis.

Correct for the blank.

Note: 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.

7.6.6Difference method

Ureic N can also be calculated as indicated in the following table:

Case

Nitric N

Ammoniacal N

Ureic N

1

Absent

Present

(7.2.4)–(7.5.3)

2

Present

Present

(7.3.3)–(7.5.3)