Total Nitrogen determination
Verification using an Ammonium Chloride Standard for UDK Distillation Units
In order to verify the VELP Distillation units, the nitrogen content of the ammonium chloride
standard is determined by direct distillation.
Ammonium salt solutions with a known content, prepared with ammonia free water, are more
practical to be used. In this case the used volume is to be precisely measured.
The commonly used salts is:
Ammonium chloride, NH4Cl, reagent grade, minimum purity 99.5%. Molecular weight 53.492.
Nitrogen 26.18%. Slightly hygroscopic salt. It is to be dried two hours in an oven (105°C) before
weighing. It sublimates without melting.
Ammonium chloride standard solution preparation:
The solution can be prepared with 3.819 g of ammonium chloride (dried 2 hours at 105°C) to
1000 ml with ammonia free water.
3.819 g x 26.18% = 1 g N.
One millilitre of this solution contains 1 mg of nitrogen.
Distilling 25 ml of this solution (25 mg of nitrogen) it will be theoretically consumed a volume of
17,84 ml of a 0,1N strong acid.
Blank preparation:
The nitrogen content of all the reagents used during analysis must be determined by blank
distillation with all chemicals and without sample.
Setting UDK distillation unit for the 10 samples distillation:
Condition the UDK unit by performing the Check up and a Wash down (see operating manual).
Distill the samples according to the following parameters:
H2O (dilution water): 50 ml Protein factor: 0
NaOH (32 %): 20 ml HCl (0.1N) as titrant solution
H3BO3 (4 % with indicators) 30 ml or pH end point for Kjeldahl analysis is 4.7.
VReceiver TKN formula for 1L sol., 40g
code A00000316
Distillation time goes from 3 to 5 minutes (depends on the distillation unit model) in order to
collect 100ml of distillate for each sample (see operating manual).
Calculate mg N as follow:
mg N = (ml sample – ml blank) * 14.007 * 0.1
ml sample: titrant volume used for sample
ml blank: average of titrant volume used for blanks
14.007: nitrogen molecular weight (g/mol)
0.1: normality titrant solution (N)
This calculation is performed automatically by UDK159 and UDK169
Analytical Standard 1/2 03.04.2023
Ammonium Chloride Rev 4
Results:
SAMPLE N° ml titrant solution mg Nitrogen
1
2
3
4
5
6
7
8
9
10
Blank: average of titrant volume used for blanks …….
average value as mgN: …….
nitrogen recovery %: …….
where:
mgN sample1 + mgN sample2 +…+ mgN sample10
average mgN:
sample3…………..+ mgNcamp.10
10
average mgN
* 100
nitrogen recovery%:
25 mgN (theoretical value)
The nitrogen recovery (respect to the theoretical value) should be ± 1% (not less than 99% and
not higher than 101%) for 10-20 repetitions.
The precision of Kjeldahl method is generally given within 1%, to be considered as Relative
Standard Deviation (RSD), where:
RSD % = Standard deviation * 100
Average mg N
Analytical Department
[email protected]
Warranty: The details given here are merely intended for information purpose and are in no way legally binding.
Consequently we accept no responsibility in the broadest sense of the word for damage that may result from
application based upon this information.
Analytical Standard 2/2 03.04.2023
Ammonium Chloride Rev 4
