Comparison of different Kjeldahl Tablets for the ......Three different types of Kjeldahl Tablets are...
Transcript of Comparison of different Kjeldahl Tablets for the ......Three different types of Kjeldahl Tablets are...
091/2012
SpeedDigester K-439
KjelMaster K-375 with KjelSampler K-376
Comparison of different Kjeldahl Tablets for the
Determination of TKN (Total Kjeldahl Nitrogen)
in Water using 500 ml Sample Tubes
091/2012 SHORT NOTE
SpeedDigester K-439 KjelMaster K-375 with KjelSampler K-376
Comparison of different Kjeldahl Tablets for the Determination of
TKN (Total Kjeldahl Nitrogen) in Water using 500 ml Sample
Tubes
The following introduces a simple and fast procedure for TKN (Total Kjeldahl Nitrogen) in Water according to the Kjeldahl method, as described in the ISO 5663-1984, Method PAI-DK01 and APHA Standard method 4500 Ammonia. This Short Note compares the behaviour of the different types of Kjeldahl Tablets and summarizes their individual advantages. All the samples were digested with sulfuric acid and Kjeldahl Tablets using the SpeedDigester K-439 and then distilled and titrated with the Kjeldahl sampler system K-375/K-376. Both this application note and methods referenced comply with 40 CFR 136.3.
Introduction
BUCHI offers different types of catalyst tablets for performing the standard Kjeldahl method. The Kjeldahl Tablet “Titanium” containsoxide and potassium sulfate. The copper sulfate and potassium consists of a very low content of copper sulfate and potassium sulfate [1]. In this Short Note, a urea stock solution was selected as sample material. The main focus of the experiments was to determine the individual behavior of the different catalysts and to find out more about their influence on the total digestion time and the results. To see all results please refer to Application Note 089/2012.
Experimental
Instrumentation: SpeedDigester K-439,
Scrubber K-415 Triple ScrubECO
KjelMaster K-375 with KjelSampler K-376
Samples: Urea stock solution [4]
Determination: 4 ml of the urea stock solution were placed
into the 500 ml sample tubes and filled up with distilled water to the total volume [2;3] described in Table 1. For every experiment with the different types of Kjeldahl Tablets, 1 tablet, a digestion rod and the corresponding volume of sulfuric acid were added. The digestion was performed according to the “tkn 500 (250 ml)”method (K-439), with varied total digestion times, depending on the total sample volume of 10, 100 and 400 ml (see Table 1). After the digestion, the ammonia of the sample was distilled into a boric acid solution by steam distillation and titrated with sulfuric acid by the Kjeldahl sampler system K-375/K-376.
Table 1: Parameters for the digestion depending on the nitrogen content and
the sample volume
Vsample
Digestion time
< 5 mg N/l 400 ml 185 min
10 –20 mg N/l 100 ml 80 min
> 100 mg N/l 10 ml 45 min
Results
Figure 1 presents the recovery of the nitrogen content in urea determined with different types of tablets and after the corresponding digestion times described in Table 1.
Figure 1: Results of the nitrogen recovery (%) with different catalysts (n=3) In account with the Application Note 001-437_370-03C “Operational Quality,the averageCheckof Pro recovery (%) of every determination was within the specification of 98 - 102% (Figure1).
Conclusion
No elongation of the digestion time is necessary, all three types of catalyst showed the same performance, depending on the total sample volume. Based on this finding, the composition of the catalysts and the needed volume of sulfuric acid are in focus to evaluate the three different Kjeldahl tablets. The catalyst “ECO” seems to be kind of application. For an optimal ration between the tablet and the amount of sulfuric acid, just 8 ml were required. The comparison of the composition of the catalysts [1] shows, that “ECO” has the lowe three types of Kjeldahl tablets and is therefore the environment-friendliest alternative for the determination of TKN in water and waste water samples. References
[1] 070/2011 Technical Note [2] Method PAI-DK01, Nitrogen, Total Kjeldahl, Block Digestion, Steam Distillation, Titrimetric Detection. Revised December 22, 1994. OI Analytical. [3] APHA Standard method 4500 Ammonia [4] ISO 5663-1984 BUCHI Application Note M06_Quality check 001-437_370-03C Operation manual SpeedDigester K-439 Operation manual Scrubber K-415 Operation manual KjelMaster K-375 with KjelSampler K-376/377
For more detailed information please refer to Application Note 089/2012
www.buchi.com Quality in your hands
1 Introduction
An easy and reliable method for determining TKN (Total Kjeldahl nitrogen) in water
according to the Kjeldahl method, as described in the ISO 5663-1984, Method PAI-
DK01 and APHA Standard method 4500 Ammonia, is introduced in chapter 8. All
described water samples were digested with the SpeedDigester K-439. The distillation
and boric acid titration were performed with the Kjeldahl sampler system K-375/K-376.
In a first step, the new BUCHI Kjeldahl Tablets for performing standard Kjeldahl were
compared with each other in order to learn more about the advantages of each type of
tablet. For the experiments a urea stock solution [1] was selected as a reference
solution, waste water from the clarification plant was selected as sample material.
2 Equipment
SpeedDigester K-439 (500 ml configuration) Scrubber K-415 TripleScrub
ECO
KjelMaster K-375 with KjelSampler K-376 TKN set for Scrubber (11057333) Digestion rods to prevent bumping (043087) Rack 12 complete for 500 ml sample tubes (043970) Volumetric pipettes 10, 25, and 50 ml Adjustable micropipettes 1 and 5 ml Graduated cylinder 100, 250, and 500 ml Volumetric flask 500 and 2000 ml Analytical balance (accuracy ± 0.1 mg)
NOTE: - Working with the SpeedDigester K-436 is also possible. For more
information please refer to Application Note 049/2010
3 Kjeldahl Tablets
Three different types of Kjeldahl Tablets are available for performing standard Kjeldahl.
Due to the different weight of the tablets, different volumes of sulfuric acid had to be
used during the experiments in order to obtain the optimal ratio of catalyst to sulfuric
acid. The composition of each tablet, their weight and the used volume of sulfuric acid
are summarized in Table 1.
Table 1: Composition of the Kjeldahl Tablets Titanium, ECO and Missouri
Name Weight Potassium Copper sulfate Titanium(IV) Sulfuric acid
[g] sulfate [%] pentahydrate [%] oxide [%] [ml]
Titanium 3.7 94.3 2.8 2.8 8
ECO 4 99.9 0.06 - 8
Missouri 5 99.6 0.4 - 10
Application Note 091/2012 Version B, Copyright © 2010 Büchi Labortechnik AG 3/14
4 Chemicals and Materials
Sulfuric acid conc 98 %, Fluka (84727) Titanium, BUCHI Kjeldahl Tablet (11057980) Missouri, BUCHI Kjeldahl Tablet (11057982) ECO, BUCHI Kjeldahl Tablet (11057983) Sodium hydroxide 32 %, Brenntag (81980-452) Boric acid 2 %,100 g boric acid, Brenntag (80948-155) diluted to 5 l with
deionized water und 3 g/l potassium chloride, pH adjusted to 4.65 Sulfuric acid 0.01 mol/l; 100.00 ml sulfuric acid 0.1 mol/l Fluka (35357) standard
solution, diluted to 1 l with deionized water. Neutralization solution for the Scrubber: 600 g sodium carbonate, calcined,
technical, Synopharm (0179420) about 2 ml ethanol and a spatula tip of bromthymol blue, Fluka (18460) diluted to 3 l with distilled water
Urea, Merck (108488)
5 Samples
Urea stock solution: - a) 0.5058 g/ 500 ml 0.4743 mg N/ ml1.897 mg/ 4 ml - b) 2.0371 g/ 2 l0.4751 mg N/ ml1.900 mg/ 4 ml - c) 0.2105 g/ 2 l0.0491 mg N/ ml0.030 mg/ 610 µl
Waste Water from the clarification plant ARA Oberglatt
6 Procedure
The determination of TKN in water and waste water includes the following steps:
Homogenization of the sample by shaking Depending on the storage time, add 1 ml sulfuric acid per litre sample for
acidification
Digestion of the sample, using SpeedDigester K-439 Distillation and titration of the sample, using
Kjeldahl sampler system K-375/K-376
6.1 Digestion method - urea (verification of the method)
Preheat the digestion unit according to Table 3 Add 1 tablet of catalyst to each sample tube Place one digestion rod in each sample tube to prevent bumping Place 4 ml of the urea stock solution (0.474 mg N/ml) into the sample tube using
volumetric or micro pipettes Dilute the stock solution with deionized water to the required volume (e.g., dilute
4 ml of stock solution by adding 396 ml deionized water for a sample volume of 400 ml, see Table 2)
Add a portion of sulfuric acid (98%), depending on the type of catalyst, see Table 1
Prepare additional blanks, only chemicals and deionized water without stock solution
Connect the Scrubber K-415 to the SpeedDigester K-439 to absorb the acid fumes created during digestion
Insert the rack containing the samples into the preheated unit Digest the samples according to the Table 3, depending on the total sample
volume Drain the TKN vessel of the Scrubber when required, therefor reduce the suction
power of the scrubber to the minimum, with the adjustable bypass valve
Application Note 091/2012 Version B, Copyright © 2010 Büchi Labortechnik AG 4/14
6.2 Digestion method - samples
Preheat the digestion unit according to Table 3 Add 1 tablet of catalyst to each sample tube Place one digestion rod in each sample tube to prevent bumping Place the required sample amount (as specified in Table 1) in the sample tube
using a graduated cylinder (if the sample contains suspended particles) or volumetric pipettes
Table 2: Amount of sample and digestion time depend on the expected nitrogen content
Sample amount Time
[ml] [min]
< 5 mg N/l 400 185
5 –10 mg N/l 250 135
10 –20 mg N/l 100 80
20 –50 mg N/l 50 60
50 –100 mg N/l 25 50
> 100 mg N/l 10 45
Add a portion of sulfuric acid (98%), depending on the type of catalyst, see Table 1
Prepare additional blanks, only chemicals and deionized water without sample Suspend the sample carefully by gently swirling the tube Connect the Scrubber K-415 to the SpeedDigester K-439 to absorb the acid
fumes created during digestion
Insert the rack containing the samples into the preheated unit Digest the samples according (250mlto)”themethod“tkn forml500 the sample or to the
parameters listed in Tables 2 and 3 Drain the TKN vessel of the Scrubber when required, therefor reduce the suction
power of the scrubber to the minimum with the adjustable bypass valve
Table 3: Digestion parameters for SpeedDigester K-439
K-439
Step Temperature Time
[°C] [min]
Preheating 380
1 520 See Table 2
Cooling - 30
NOTE:
If a sample tends to foam, add a small amount of stearic acid. Let the samples cool down to room temperature beside the SpeedDigester
(Cooling position of the SpeedDigester can only be used with 300 ml sample tubes!).
Depending on the amount of copper in the different Kjeldahl tablets, the color of the solution can vary from light green to pale green or transparent after the digestion!
Application Note 091/2012 Version B, Copyright © 2010 Büchi Labortechnik AG 5/14
6.3 Distillation and titration
Distill the samples according to the parameters listed in Table 4.
Table 4: Distillation and titration with the Kjeldahl sampler system K-375/K-376 Method parameters KjelMaster K-375
H2O volume 60 ml Titration solution H2SO4 0.01 mol/l
NaOH volume 50 ml Sensor type Potentiometric
Reaction time 5 s Titration mode Online
Distillation mode Autodest. Titration start time 0 sec
Distillation time 150 s Measuring mode Endpoint pH
Stirrer speed distillation 5 Endpoint pH 4.65
Steam output 100 % Stirrer speed titration 7
Titration type Boric acid Titration start volume 0 ml
Receiving solution vol. 60 ml Titration algorithm Optimal
6.4 Calculation of Nitrogen and TKN
The results are calculated as a percentage of nitrogen. The following equations (1) and (2) are used to calculate the recovery of the nitrogen content in urea.
mN(actual) = (VSample - VBlank ) •z •c •f• MN (1)
Recovery % = mN (actual)
•100
(2)
mN (theoretical)
For the calculation of TKN, the equation (3) was used.
TKN = (VSample - VBlank ) •z •c •f•MN •1000 (3)
Sample Vol.
TKN : Total Kjeldahl Nitrogen [mg/l]
VSample : amount of titrant for the sample [ml]
VBlank : mean amount of titrant for the blank [ml]
z : molar valence factor (1 for HCl, 2 for H2SO4)
c : concentration of the titrant [mol/l]
f : titrant factor (for commercial solutions normally 1.000)
MN : molecular weight of nitrogen (14.007 g/mol)
Sample Vol. : sample volume [ml]
1000 : conversion factor [mg/g] or [ml/l]
Recovery : recovery of the amount of nitrogen [%]
mN(actual) : determined amount of nitrogen in a sample tube [mg]
mN(theoretical) : theoretical amount of nitrogen from spiking or stock solution [mg]
Application Note 091/2012 Version B, Copyright © 2010 Büchi Labortechnik AG 6/14
6.5 Estimation of Limit Of Detection (LOD) and Limit Of
Quantification (LOQ) of the method
The “blank method” from or the DI determination 32645 of the detection was used f limit (LOD) and the quantification limit (LOQ). Based on this limits the performance of the method can be evaluate.
First, six blanks were determined using 50 ml deionized water, one ECO tablet and 8 ml sulfuric acid. The blanks were digested and determined according to the parameters listed in Table 2 and 4, the results are presented in Table 5.
Table 5: Results of the blank determination
Blank Average SD RSD
volume [ml] [ml] [ml] [%]
0.419
0.433
0.425
0.428
0.423
0.429 0.010 2.31 0.447
6.5.1 LOD
The following equation was used to calculate the limit of detection (LOD).
LOD = ᶲn;α • SD (4) LOD = 0.0361 ml ᶲn;α : factor 3.0; depending on the number of blanks (n=10) and the level of significance (α=0.01)
SD : standard deviation of the blank determination (SD=0.010 ml)
6.5.2 LOQ
Depending on the LOD, the limit of quantification can be calculated (5). Then, the LOQ can be used to control the method by spiking the samples with the calculated
nitrogen content. Both, LOD and LOQ, are necessary to evaluate the results.
LOQ = k· ᶲn;α·SD
(5)
LOQ = 0.1083 ml
k
: factor 3 (for more information refer to DIN 32645)
Application Note 091/2012 Version B, Copyright © 2010 Büchi Labortechnik AG 7/14
The calculated volume can be inserted into equation (1) and the amount of nitrogen for spiking the sample can be calculated.
0.1083 ml · 2 · 0.01 mol/l · 1 · 14.007 g/mol = 0.030 mg
To spike the samples, 0.030 mg nitrogen was added to each sample tube (see
chapter 8.2). To calculate the recovery of the sample spiking, equation (6) and (7) were used.
TKN •Sample Vol (6)
mN(total)-TKN = (VSample - VBlank ) •z •c •f•MN • 1000
Recovery = (mN(total)-TKN)
•100
(7) 0.03 mg
7 Results for the comparison of the Kjeldahl Tablets
7.1 Recovery of urea stock solution
For the determination of the recovery of nitrogen, 4 ml of the urea stock solution were
used. Three different sample volumes, 10, 100 and 400 ml were digested, using the
different Kjeldahl Tablets. The recovery of nitrogen and the theoretical TKN value
were calculated in Table 6-8.
Table 6: Results of the recovery of nitrogen and TKN with K-439 after 45 min, total sample volume 10 ml Stock VSample mN(theoretical) mN(actual) Recovery TKN Average RSD solution [ml] [mg] [mg] [%] [mg N/l] [%] [%]
Titaniuma
7.233 1.897 1.921 101.3 192.1 100.9 0.78
Titaniuma
7.245 1.897 1.924 101.4 192.4
Titaniuma
7.147 1.897 1.897 100.0 189.7
ECOb
7.196 1.897 1.914 100.9 191.4 100.3 0.88
ECOb
7.181 1.897 1.910 100.7 191.0
ECOb
7.086 1.897 1.883 99.3 188.3
Missouric
7.182 1.897 1.912 100.9 191.2 100.6 0.27
Missouric
7.176 1.897 1.911 100.7 191.1
Missouric
7.147 1.897 1.902 100.3 190.2 a Blank 0.377 ml (n=2)
b Blank 0.365 ml (n=2)
c Blank 0.356 ml (n=2)
Application Note 091/2012 Version B, Copyright © 2010 Büchi Labortechnik AG 8/14
Table 7: Results of the recovery of nitrogen in urea with K-439 after 80 min, total sample volume 100 ml Stock VSample mN(theoretical) mN(actual) Recovery TKN Average RSD solution [ml] [mg] [mg] [%] [mg N/l] [%] [%]
Titaniuma
7.207 1.897 1.907 100.5 19.1 99.5 1.02
Titaniuma
7.132 1.897 1.886 99.4 18.9
Titaniuma
7.070 1.897 1.868 98.5 18.7
ECOb
7.247 1.897 1.914 100.9 19.1 100.5 0.48
ECOb
7.250 1.897 1.907 100.5 19.1
ECOb
7.210 1.897 1.896 99.9 19.0
Missouric
7.207 1.897 1.907 100.6 19.1 100.7 0.09
Missouric
7.219 1.897 1.911 100.7 19.1
Missouric
7.215 1.897 1.910 100.7 19.1 a Blank 0.401 ml (n=2)
b Blank 0.442 ml (n=2)
c Blank 0.398 ml (n=2)
Table 8: Results of the recovery of nitrogen in urea with K-439 after 185 min, total sample volume 400 ml
Stock VSample mN(theoretical) mN(actual) Recovery TKN Average RSD solution [ml] [mg] [mg] [%] [mg N/l] [%] [%]
Titaniuma
7.123 1.879 1.878 99.9 4.7 100.3 0.33
Titaniuma
7.168 1.879 1.890 100.6 4.7
Titaniuma
7.146 1.879 1.884 100.3 4.7
ECOb
7.189 1.879 1.888 100.5 4.7 100.8 0.27
ECOb
7.223 1.879 1.897 101.0 4.7
ECOb
7.219 1.879 1.896 100.9 4.7
Missouric
7.170 1.879 1.877 99.9 4.7 100.1 0.14
Missouric
7.182 1.879 1.881 100.1 4.7
Missouric
7.189 1.879 1.883 100.2 4.7
a Blank 0.420 ml (n=2)
b Blank 0.451 ml (n=2)
c Blank 0.469 ml (n=2)
Application Note 091/2012 Version B, Copyright © 2010 Büchi Labortechnik AG 9/14
7.3 Conclusion drawn from the comparison of the different
types of Kjeldahl Tablets
According to ISO 5663-1984, urea as example for an organic nitrogen-containing
compound which is easy to digest, was chosen. In Figure 1, the results of the recovery
of nitrogen from urea in water are presented. Three different TKN values were chosen
to compare the Kjeldahl catalysts with each other. The results in detail are presented
in Table 6-8.
102
101.5
101
(%)
100.5
100 R e c o v e r y
98.5
99.5
99
98 < 5 mg N/L 10-20 mg N/L > 100 mg N/L
TKN
Figure 1: Recovery of nitrogen with different types of Kjeldahl Tablets.
ECO
Missouri
Titanium
All recoveries are within the specification of 98-102°% [1]. No elongation is necessary, all three types of catalyst need the same digestion time, depending on the sample volume. Based on this finding, the composition of the catalysts and the needed volume of sulfuric acid are in focus, both are presented in Table 1. The Kjeldahl Tablets ECO and Titanium, due to their weight, need 8 ml sulfuric acid instead of 10 ml for the catalyst Missouri. Taking a closer look to the composition of the catalysts shows that ECO contains the lowest copper content [3] of all three types of Kjeldahl Tablets and is therefore the most environment-friendly choice for the following experiments.
8 Results for the digestion conducted with the
Kjeldahl Tablet ECO
The tablet ECO”“ was chosen because no differentiation of the digestion performance
between the catalyst tablets, but ECO shows the environment-friendly benefit of
containing less copper [3] and needing less sulfuric acid.
The preparation of the samples and the calculation of the results are similar to the
ones described in chapter 6 and 7. One tablet “ECO” and 8 ml of sulfuric acid (98 %)
were used (Table 1) for the experiment. All parameters for the digestion and the
distillation/titration are specified in Table 3 and 4.
Application Note 091/2012 Version B, Copyright © 2010 Büchi Labortechnik AG 10/14
8.1 Recovery of urea stock solution
The results of the recovery of nitrogen in urea are presented in Table 9. The nominal
value of urea is 46.64 % of nitrogen. The determined values are within the specification of 98-102 % [2].
Table 9: Results of the recovery of nitrogen with Kjeldahl Tablet ECO
Sample VSample mN(theoretical) mN(actual) Recovery TKN Average RSD vol. [ml] [ml] [mg] [mg] [%] [mg N/l] [%] [%]
400a
7.189 1.897 1.888 100.5 4.7 100.8 0.27
7.223 1.897 1.897 101.0 4.7
7.219 1.897 1.896 100.9 4.7
250b
7.357 1.900 1.902 100.1 7.6 100.8 0.86
7.472 1.900 1.934 101.8 7.7
7.395 1.900 1.912 100.7 7.7
100c
7.274 1.897 1.914 100.9 19.1 100.5 0.48
7.250 1.897 1.907 100.5 19.1
7.210 1.897 1.896 99.9 19.0
50d
7.204 1.900 1.901 100.1 38.0 100.8 0.67
7.275 1.900 1.921 101.1 38.4
7.289 1.900 1.925 101.3 38.5
25e
7.264 1.900 1.904 100.2 76.2 100.4 0.35
7.263 1.900 1.904 100.2 76.2
7.305 1.900 1.916 100.8 76.6
10f
7.193 1.897 1.914 100.9 191.4 100.8 0.88
7.181 1.897 1.910 100.7 191.0
7.086 1.897 1.883 99.3 188.3 a Blank 0.451 mL (n=2)
b Blank 0.569 ml (n=2)
c Blank 0.442 ml (n=2)
d Blank 0.418 ml (n=2)
e Blank 0.467 ml (n=2)
f Blank 0.365 ml (n=2)
Application Note 091/2012 Version B, Copyright © 2010 Büchi Labortechnik AG 11/14
8.2 Determination of TKN in waste water
The results of the determination of nitrogen in waste water from the clarification plant ARA Oberglatt are presented in Table 10.
Table 10: Results of the determination of nitrogen and TKN in waste water
Waste Water Sample Vol. VSample TKN [ml] [ml] [mg N /l]
Sample 1 50 8.215 43.6
Sample 2 50 8.203 43.6
Sample 3 50 8.186 43.4
Average 43.5
Rsd [%] 0.19 The mean blank volume for this sample was 0.430 ml (n = 2).
To check the performance of the method the waste water sample was spiked with
0.03 mg nitrogen per sample tube. This amount of nitrogen was calculated according
to DIN 32645, see chapter 6.5.
Table 11: Results of the determination of nitrogen and TKN in spikes waste water
Spiking VSample TKN mn(Total)-TKN Recovery [ml] [mg N/l] [mg] [%]
Sample 1 8.286 44.1 0.028 92.8
Sample 2 8.289 44.1 0.029 95.6
Sample 3 8.282 44.0 0.027 89.0
Sample 4 8.289 44.1 0.029 95.6
Average - - 0.028 93.2
Rsd [%] - - 3.32 3.32
The mean blank volume for this sample was 0.423 ml (n = 3).
The recovery of the spiking and the resulting relative standard deviation shows good values.
Application Note 091/2012 Version B, Copyright © 2010 Büchi Labortechnik AG 12/14
9 Comparison to standard methods
The differences between this application and the official methods ISO 5663, Standard method (4500-NH3 B-2011, C-2011) and Method PAI-DK01 are shown in Table 12.
Table 12: Differentiation to the official methods
This application ISO 5663 Method PAI-DK01 Notes/Impact
note 4500-NH3 B and C
Catalyst 4 g Tablets cont. 5 g mixture K2SO4 The choice of
- 99.9% K2SO4 -1000±20 g K2SO4 CuSO4 catalyst does not
- 0.06% CuSO4
influence the result. -10±0.2g Se More eco-friendly
as no toxic Se/Hg!
Sulfuric 8 ml 10 ml Concentrated No impact. Same
acid ratio of sulfuric acid
(98 %) / catalyst.
Reduction of
chemicals!
Water 60 ml 250 ml For 4500-NH3 B and C, no digestion procedure is needed, sample is directly distilled.
The K-375
generates steam in
a separated vessel;
therefore it is not
necessary to add
such a high amount
of water to the
digested sample as
described in the
standard methods.
Sodium 50 ml 50 ml 4500-NH3: 6 N NaOH solution is used for pH adjustment to 9.5
No impact for the AN and ISO 5663;
hydroxide (Conc.: 32 %) (Conc.: 36 %) No extra NaOH is
needed during
distillation.
Na2S2O3 no no no Only necessary addition to when Hg is used as
NaOH catalyst
Titration Boric acid/ Boric acid/ Boric acid/ No impact. The
potentiometric colorimetric, potentiometric results are equal
titrimetric with boric acid
(4500-NH3:
titration and
colorimetric, potentiometric)
potentiometric or
titrimetric endpoint
detection.
Application Note 091/2012 Version B, Copyright © 2010 Büchi Labortechnik AG 13/14
10 Conclusion
The determination of nitrogen and TKN contents in urea stock solution and waste
water sample with the help of the different types of Kjeldahl Tablets provides reliable
and reproducible results with low relative standard deviations. The total digestion time
can vary depending on the sample volume, but the type of catalyst didn’t show any
differentiation. Therefore the catalyst “ECO”, as environment–friendly alternative can be chosen without the disadvantage of an elongation of the digestion time. Two important characteristics of the latest version of the fully-automatic Kjeldahl
sampler system, KjelMaster K-375 and KjelSampler K-376, are the short processing
time as well as the reduced need for user attendance. In combination with the unique
SpeedDigester models, the time needed for sample analysis is significantly reduced
and the throughput is therefore increased.
11 References
[1] ISO 5663-1984 “Water quality –Determination of Kjeldahl nitrogen”
[2] Application Note 001-437_370-03C “Operational Quality Check Procedure”
[3] 070/2011 Technical Note: “ New Assortment of Kjeldahl Tablets”
[4] Method PAI-DK01, Nitrogen, Total Kjeldahl, Block Digestion, Steam
Distillation, Titrimetric Detection. Revised December 22, 1994. OI
Analytical.
[5] APHA Standard method 4500 Ammonia
Application note 049/2010 “Determination of Total Nitrogen (TKN) in Water and Waste Water using 500 ml Sample Tubes”
Operation manual of SpeedDigester K-439 Operation manual of Scrubber K-415 Operation manual of KjelMaster K-375 with KjelSampler K-376/377
BÜCHI Labortechnik AG CH-9230 Flawil 1/Switzerland
T +41 71 394 63 63 F +41 71 394 65 65
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Application Note 091/2012 Version B, Copyright © 2010 Büchi Labortechnik AG 14/14