Metode Analisis T-N

Method: Persulfate Method (4500-N C)

Source : Standard Methods for the Examination of Water and Wastewater 23rd Edition by Roger B.Bard

Principle : Alkaline oxidation at 100 – 110 to convert organic and inorganic nitrogen to nitrate. Total nitrogen determined by
analyzing nitrate in the digestate.

Reagents :
1. Ammonia-free and nitrate free water
2. Stock nitrate solution and intermediate nitrate solution
3. Stock glutamic acid solution
4. Intermediate glutamic acid solution (glutamic acid diluted with water and preserved with CHCl 3
5. Digestion Reagent (low nitrogen dissolved with potassium persulfate, K2S2O8 and NaOH in water
6. Borate buffer solution (Boric acid dissolved with H3BO3 and NaOH in water)
7. Copper sulfate solution (Dissolved CuSO4 . 5 H2O in water)
8. Ammonium chloride solution (Dissolved NH4Cl in water. Adjust pH by adding NaOH)
9. Color reagent (combine water, phosphoric acid, sulfanilamide, and N-(1-naphthyl)-ethylenediamine dihydrochloride.
Add polyoxyethylene 23 lauryl ether.

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 T-N Analysis Method
Procedure :
1. (Calibration) Prepare NO3- calibration standard in the range of 0 to 2.9 mg NO 3- N/L by diluting to 100 ml the following
volumes of intermediate nitrate solution: 0,1.00, 2.00, 4.00,…., 29.0 mL. treat standards in the same manner as sample
2. (Digestion check standard) Prepare glutamic acid digestion check standard of 2.9 mg N/L by diluting to 100 mL a 29.0 mL
volume of intermediate glutamic acid solution.
3. (Digestion) sample preserved with acid cannot be analyzed by this method. To a culture tube, add 10.0 mL
sample/standard/ a portion diluted to 10.0 mL. Heat for 30 min in a autoclave or pressure cooker at 100-110oC. Slowly cool
to room temperature. Add 10.0 mL borate buffer solution. Mix by inverting at least twice.
4. (Blank) carry a reagent blank through all steps of the procedure and apply necessary corrections of the results.
5. (Nitrate measurement) Determine nitrate by cadmium reduction. Set up manifold as shown in Figure 4500-NO3-; but use
ammonium chloride and color reagents specified in 4500-N-C

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 Phosphate Analysis Method

Method : ICPS-Shimadzu

a. Separate the sample to take the filtrate only (by using vacuum pump) -> (request by user)
b. Sample then prepared with acid (HCL) and heating (up to 105oC) to destruct the water component
c. This sample then will be read in the equipment as P, and the measurement would not be disrupt except by turbidity
d. All of the organic/ anorganic P content in the sample would measured as long as it is already diluted with the water/ all
of the component has been destruct and became soluble

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