1. Teknologi Dan Rekayasa
Kompetensi Keahlian
Analisis Kimia

2. Analisis of Cemical Parameters
SMK Negeri 13 Bandung

3. NITROGEN COMPOUND
SMK Negeri 13 Bandung

4. Objectives After this session, the students are expected to be able :
to explain the steps of determination of ammonium, nitrate and nitrite
to explain the objectives of every step
to explain the function of reagents
to conduct the determination of ammonium, nitrate and nitrite
to do the calculation in the determination of ammonium, nitrate and nitrite
to arrange the report of the determination of ammonium, nitrate and nitrite
Teknologi dan Rekayasa

5. Nitrogen Compound in water
Ammonia (NH3)
NH4+ appear at low pH
Nitrogen gas (N2)
Nitrite (NO2-)
Nitrate (NO3-)
NH4+
NH4+- Protein

6. Nitrogen Gas (N2) in water
Presence of N2 in water produced from air, used by seaweed and groups of bacteria to growth
N2 un reactiv
N2 easy to get from water low level of saturation
 Presence in water not harmful

7. Ammonia (NH3) in water
Ammonia, at low pH  NH4+ (amonium), high pH  NH3 (ammonia)
In surface water proceed against :
- wastes of human (urine)
- Microbiological decomposition of organic substances
C,H,O,N,S + O2  CO2 + H2O + NH3
- Contamination of using fertilizer in agriculture
Content of ammonia in surface water (30 mg/L) higher than groundwater
Content ammonia in high level in water indicates high contamination (odor and taste)
Condition for drinking water, NH3 must have 0 ppm, in river up to standard 0,5 ppm
Removal process by aeration and chlorination

8. Determination of Ammonia (NH3)
Determined as :
- NH4+ (ammonium),dissolved in water
- NH4+
- Protein, nitrogen compound formed as protein
Method of determination by colorimetric with constant height, using Nessler and comparator
Disrupt ion at analysis process :
High level of Sulfide
 add Zn(CH3COO)2, filtrate continued
High level of Ca2+ and Mg2+
 add caustic soda, filtrate continued
Turbidity
 add coagulant (tawas Al), filtrate continued

9. Determination of Ammonium (NH4+)
Method of determination by colorimetric with constant height, using Nessler and comparator
Reactant for colour formation Nessler
Principle :
NH4+ in water react to Nessler formed yellow-brown
compound, compare the colour to standard solution
Reactions : Nessler reactant : HgI2, KI, NaOH (K2HgI4) NH4+ + 2[HgI4]2- + 4OH-  HgO.Hg(HH2)I(s) + 7I- + 3H2O

10. Determination of Ammonium (NH4+)
Making of stock NH4+ solution 100 ppm from NH4Cl
Making of standard measurement 0,1 – 0,5 ppm
In to Nessler tube
Preparation of sample :
Put 100 mL of sample (use graduated glass) in to
Nessler tube
(if there is disrupt must have losed before measurement)
Add 1 mL Siegnette solution, shake it well and 1 mL
Nessler reactant, shake in to sample and standard
Let for 15 minutes, and compare the colour formed

11. Calculation (NH4+, mg/L)
Method: colorimetric constant height (Nessler method)  Same intensity, same colour indicates same consentration
According Lambert-Beer’s Law
A1 = A2
1.b1.c1 = 2.b2.c2
b1= b2 ; 1 = 2
 c1 = c2

12. Calculation (NH4+, mg/L)
Method colorimetric with different height
Same intensity,same colour indicates same concentration
According Lambert-Beer’s Law
A1 = A2
1.b1.c1 = 2.b2.c2
1= 2 , so :
b1.c1 = b2.c2
if : 1 standard, 2 sample, so :
b1.c1
c2 = b2

13. Determination of Ammonium-Protein (NH4+-Protein)
Method of determination colorimetric constant height
Reactant for colour formation is Nessler
Principle :
Protein in sample oxidized by K2S2O8 in acid condition
to NH4+ salt, NH4+ through Nessler reactant
formed yellow-brown compound
,compare the colour formation to standard solution
Reactions : Nessler reactant : HgI2, KI, NaOH (K2HgI4) R-CNH2COOH + H+ + S2O82-  CO2 + H2O + (NH4)2SO4 NH4+(*) + 2[HgI4]2- + 4OH-  HgO.Hg(NH2)I(s) + 7I- + 3H2O

14. Determination of NH4+ Making of standard measurement 0,1 – 0,5 ppm
In to nessler tube from stock solution 100 ppm
Preparation of sample :
Put 100 mL of sample in to Erlenmeyer flask
Add H2SO4 4 N ( congo paper red  blue)
Add 0,1g K2S2O8, heat for 15’ on steam bath
Let it cool then put in to nessler tube
add1 mL Siegnette solution shake it well and 1 mL
Nessler reactant, shake in to sample and standard
Let it for 15 minutes, compare the colour

15. Calculation NH4+-Protein, mg/L
Method colorimetric different height
 Same intensity of colour indicates same concentration
According Lambert-Beer’s Law
A1 = A2
1.b1.c1 = 2.b2.c2
1= 2 , so :
b1.c1 = b2.c2
if 1 standar, 2 sample, so :
b1.c1
c2 = b2

16. Calculation NH4+-Protein, mg/L
When oxidizing proces, nitrogen in protein changed to NH4+ salt  then NH4+ which soluble increase from the process
In order to detect consentration NH4+-Protein in water must corrected to free NH4+ dissolved in water
NH4+-Protein = ppm NH4+(total) - ppm NH4+(free)

17. Nitrite (NO2-) in Water
Nitrite : unstable (not long lasting )  temporary condition from oxidizing process NH4+ to NO3- (nitrification)
2NH O2  2NO2- + 4H+ +2H2O + energy
2NO2- + O2  2 NO3- + energy
Nitrite in water from inhibitor corrosive substances mostly used in manufacturer
Nitrogen compound in formation of nitrite is the most harmful to human body cause :
1. React with hemoglobin on blood, until blood could not carry away oxygen
2. Formation of nitrosin (RR’N-NO)  carsinogenic

18. Determination of Nitrite (NO2-)
Method of determination colorimetric constant height
Reactant for colour formation: Griez-Romyn
Principle :
Nitrite in sample react with Griez-Romyn formed
Red compound, compare the colour to standard solution
Reaction : Diazotisation of sulfonil acid by nitrite acid, followed by coupling reaction wiht -naftilamina formed red dye azo

19. Determination of Nitrite (NO2-)
Making of standard measurement 0,01 – 0,05 ppm
in nessler tube from stock solution 100 ppm
Preparation sample:
Put 100 mL of sample in to nessler tube
Add 100 mg nitrite reactant(Griez-Romyn), shake it well
Let it for 10’  do simultaneously
between sample and standard
Compare the colour, under 30 minutes

20. Calculation (Nitrite, mg/L)
Method determination colorimetric different height
 Same intensity of colour indicates same consentration
According Lambert-Beer’s Law
A1 = A2
1.b1.c1 = 2.b2.c2
1= 2 , so :
b1.c1 = b2.c2
If : 1 standard, 2 sample, so :
b1.c1
c2 = b2

21. Nitrate (NO3-) in water
Nitrite of nitrogen compound which has stable characteristic.
In the water, it comes from :
- Industrial banishment of explosive material, fertilizer, paint, etc.
- The use of fertilizer in farming.
The degree of nitrite in the water is not more than 10 ppm.
The height of nitrite compound can cause :
- the stimulation of algae and water plants growth which is unlimited -> if the level of DO is low means water animals are dead.

22. Nitrate (NO3-) in water
- Metamoglobenia disease (cynose/blue disease which happens to babies). Nitrite is reduced by the bacterial of lactic acid in mother’s milk to become nitrite. Nitrite has a bond with the hemoglobin in the blood.

23. Determination of Nitrate (NO3-)
Method of colorimetry of permanent height.
Reactant of Nessler color shaper.
Principle :
Nitrate and nitrite in the sample is reduced by H2 from Al
and NaOH to become NH4+ , NH4+ by nessler reactant which
form yellow-brown substance, then the colour which is
formed later is compared with the color standard solution.

24. Determination of Nitrate (NO3-)
Reaction :
6NaOH + 2Al  3H2 + 2Na3AlO3
NO2- + 3H2  NH3 +OH- + H2O
NO3- + 4H2  NH3 + OH- + 2H2O
NH4+ + 2[HgI4]2- + 4OH-  HgO.Hg(NH2)I(s) + 7I- + 3H2O

25. Determination of Nitrate (NO3-)
The make of measurement standard of NH4 + 0,1 – 0,5 ppm
In nessler tube from stock solution 100 ppm
Sample preparation :
Put 100 mL to erlenmeyer flask
Add 25 % of NaOH solution and Al metal, save it for 1 night
The gas is put in 0,01 N of HCl solution
Put into nessler tube
Add 1 mL of Siegnette solution. And then shake. After that
add 1 mL of nessler reactant to the sample and standard
Save it for 15 minutes, and compare the color which
Happens later

26. Calculation (Nitrate, mg/L)
Method : Colorimetry
the height changes
 Intensity of the same colour shows the same concentration
According to Lambert-Beer law
A1 = A2
1.b1.c1 = 2.b2.c2
1= 2 , maka :
b1.c1 = b2.c2
If : 1 standard, 2 sample, so :
b1.c1
c2 = b2

27. Calculation (Nitrate, mg/L )
When the reduction happens, nitrate and nitrite in the sample is changed into NH4 +
 so NH4 + measured becomes total ammonium of nitrite, nitrate and free ammonium.
So, to count the nitrate concentration in the water has to be corrected to free NH4 + and nitrite.
NH4+ from NO3- = NH4+(total) - NH4+dari NO2- - NH4+(free) Mr. NH4+ ppm NH4+from NO2- = x ppm NO Mr. NO2- Mr. NO3- Ppm NO3- = x ppm NH4+ dari NO3- Mr. NH4+