Short Note No.

118/2013
TKN determination in water and waste water
KjelDigester K-449, KjelMaster K-375 with KjelSampler K-376:
Determination of TKN (Total Kjeldahl Nitrogen) in water and waste water according to the Kjeldahl Method

The determination of TKN (Total Kjeldahl Nitrogen) in Table 3: Parameters for distillation and titration with the
water and waste water is a routine procedure for KjelMaster system K-375/K-376.
quality assurance. A simple and fast procedure for the 50 mL
TKN determination in water, according to ISO 5663, Receiving
H2O volume 50 mL H3BO3
solution
DIN EN 25 663 and 40 CFR part 136.3, is introduced 2 % + KCl
below. The sample is digested with sulfuric acid and Titration H2SO4
the Kjeldahl Tablet Titanium using the KjelDigester NaOH volume 40 mL
solution 0.01 mol/l
K-449, followed by distillation and titration with the
Reaction time 5s Titration mode Standard
KjelMaster system K-375/K-376.
Dist. mode fixed time Endpoint pH 4.65
1. Introduction Dist. time 180 s Stirrer sp. Tir. 7
Stirrer sp. dist 5 Titr. algorithm Optimal
TKN is one of the key parameters for the evaluation of
water and its pollution. The samples require digestion Steam output 100%
with sulfuric acid to convert nitrogen into ammonium
sulfate. After conversion to ammonia through the 3. Results
alkalinization with sodium hydroxide, the sample is
The determined TKN values of the urea stock solution
distilled into a boric acid receiver by steam distillation,
and the recoveries are presented in Table 4.
followed by a titration with sulfuric acid solution.
Table 4: Determined TKN contents and recoveries (rsd in
2. Experimental brackets, n=5)

Equipment: KjelDigester K-449 / KjelMaster K-375 Sample TKN Recovery

with KjelSampler K-376 volume [mg/L] [%]
59.1 99.9 (0.6)
Samples: Urea stock solution 0.493 mg N/ mL,
25 mL 78.3 99.4 (0.4)
surface water from lake constance and surface water
from pond threelinden. 97.9 99.4 (0.4)
29.4 99.6 (0.3)
Determination: The samples were added directly into
a sample tube, depending on the nitrogen content as 50 mL 39.2 99.6 (0.2)
described in Table 1. One Titanium tablet, boiling aids 49.0 99.5 (0.3)
to avoid bumping and 8 mL of sulfuric acid (conc. 12.2 99.3 (0.5)
98 %) were added. Before starting the digestion the 100 mL 14.7 99.3 (0.4)
user protection shiel must be affixed.
19.6 99.3 (0.0)
Table 1: Volume for each sample 1.2 97.0 (4.3)
Digestion 2.4 98.5 (1.0)
Nitrogen content Sample volume [mL]
Time 200 mL
4.9 98.7 (0.3)
50 – 100 mg N/L 25 50
9.8 99.2 (0.2)
20 – 50 mg N/L 50 70
10 - 20 mg N/L 100 90
4. Conclusion
< 10 mg N/L 200 160
The determination of TKN in water and waste water
The digestion was performed using the K-449, applied
with sulfuric acid and the Kjeldahl Tablet Titanium
by the parameters specified in Table 2, the total
using the KjelDigester K-449 and KjelMaster system
digestion time depends on the sample volume
K-375/K-376 provides reliable and reproducible
described in Table 1. The method was verified by using
results.
an urea stock solution as the reference.
Table 2: Temperature profile for digestion with the K-449 5. References
Temperature ISO 5663
Step Time [min]
[°C] DIN EN 25 663
1 250 0 40 CFR part 136.3
2 420 See Table 1
Operation Manual of KjelDigester K-446/K-449
Cooling --- 25 Operation Manual of KjelMaster system K-375/K376

After digestion the ammonia of the sample was For more detailed information and safety conside-
distilled into a boric acid solution by steam distillation rations please refer to the Application Note no.
and titrated with sulfuric acid (Table 3) performed by 118/2013.
the KjelMaster system K-375/K-376.