Nitrite

I. Scope

This method is applicable to determine nitrite in water and industrial wastewater. Determination range: NO2- - N: 0.01mg/L to 0.1 mg/L. II. 1. General Dicussion Principle

Nitrite is determined through formation of a pink azo dye at pH 1.9 by coupling diazotized sulfanilamide (4 aminobenzene sulfonamide) with N-1-Naphthyl ethylene diammonium dichloride. The intensity of color of azo dye is proportional to concentration of nitrite in sample. Measure absorbance at wavelength 540 nm by cell 1 cm. 2. Interferes Generally, nitrite ion can not coexist with oxidizing substance such as residual chlorine, but the existence of residual chlorine and chloroamines (monochloroamine, dichloroamine, nitrogen trichloride), and so on , may be misunderstood as nitrite ion owing to red coloring, even when there is no nitrite ion in sample. III. Sample with high alkalinity also cause interferes. Apparatus 1. 2. IV. Reagents 1. 2. Acid orthophosphoric, CM = 15mol/L Acid orthophosphoric, CM = 1.5mol/L Spectrophotometer Cell 1cm

Pipette 25 mL of acid orthophosphoric, dilute with distilled water to 250 mL. Store the solution in the dark bottle, the selflife of solution is 6 months. 3. 3.1. Reagent 4-Aminobenzenesulfonamide Solution

Dissolve 40 0.5g of Sulfanilamide (NH2C6H4SO2NH2) in mixture of 100 mL of 15M H3PO4 and 500 50mL distilled water. 3.2. N-1-Naphthyl ethylene diammonium Dichloride Solution Dissolve 2.0 0.02g N-1-Naphthyl ethylene diammonium dichloride [N-(1-naphthyl) ethylenediamine dihydrochloride] in the above 4-Aminobenzenesulfonamide Solution and dilute to 1000mL. Store in dark bottle and never use for one month or more after preparation. Page 1of 3

4.

Nitrite Ion Standard Solution (100 mg as NO2--N /L)

Dissolve 0.4922 0.0002g of NaNO2 (dried at 105-110oC about 2 hr., allow it to cool in desiccator) in distilled water and dilute to 1L. Store in dark bottle in one month. 5. Nitrite Ion Standard Solution (2.5 mg as NO2--N /L) Pipette 25 mL of Nitrite Ion Standard Solution (100 mg as NO2--N /L) dilute with distilled water to 1000 mL. (This standard solution should be prepared fresh weekly.) 6. Nitrite Ion Standard Solution (0.25 mg as NO2--N /L) Pipette 25 mL of Nitrite Ion Standard Solution (2.5 mg as NO2--N /L) dilute with distilled water to 250 mL. V. Testing Procedure 1.
2.

Pipette a suitable volume of sample into the volumetric flask 50mL. Add 1mL of reagent, agitate and dilute to the mark, agitate and stand for about 20 minutes. Measure absorbance at wavelength 540 nm by cell 1 cm. Take distilled water 10 mL for blank and carry out the procedure as same as the sample, use blank to set zero. Obtain the amount of nitrite ion (NO2- - N) from the calibration curve and calculate the concentration of nitrite ion (NO2- - N) in the sample (mg NO2- - N/L)

3. 4.
5.

6. 6.1.

Calibration curve NO2- N absorbance

Pipette 0 - 25 mL(0, 2, 5, 10, 20, 25) of Nitrite Ion Standard Solution (0.25 mg as NO2-N /L) to the volumetric flask 50 mL. Carry out the procedure same as the sample. Measure absorbance and plot the relative curve between the amount of nitrite ion (NO2- N) and its absorbance. Calculation mg/L as NO2- - N =

6.2.
6.3.

VI.

Where: VII. 1. 2.

C: concentration from calibration curve (mg/L) Reporting the result Reporting unit: mg/L Reported value: - From 0.01 mg/L to less than 10 mg/L: report as x.xx Page 2of 3

- From 10 mg/L to less than 100 mg/L: report as xx.x - From 100 mg/L to less than 1000 mg/L: report as xxx - From 1000 mg/L and above: report as xxxx VIII. Reference Water quality Determination of nitrite- Molecular absorption spectrometric method, TCVN 6178: 1996 (ISO 6777: 1984)

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