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ChE 3131L Experiment On Nitrates

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ChE 3131L Experiment On Nitrates

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crystahsoo
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© © All Rights Reserved
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MODULE IN

CHEMICAL ENGINEERING

CHE 3131L

Department of Chemical Engineering

SCHOOL OF ENGINEERING AND ARCHITECTURE


REF SEA-BSCHE-CHE3131L-2022

DETERMINATION OF NITRATES CONTENT OF WATER/WASTEWATER BY ULTRAVIOLET


SPECTROPHOTOMETRIC SCREENING METHOD

I. OBJECTIVES

To determine the nitrates content of water or wastewater by Ultraviolet Spectrophotometric


Screening Method

II. THEORETICAL BACKGROUND

In waters and wastewaters the forms of nitrogen of greatest interest are, in order of
decreasing oxidation state, nitrate, nitrite, ammonia, and organic nitrogen. All these forms
of nitrogen, as well as nitrogen gas (N 2), are biochemically interconvertible and are
components of the nitrogen cycle. They are of interest for many reasons.

Determination of nitrate (NO3–) is difficult because of the relatively complex procedures


required, the high probability that interfering constituents will be present, and the limited
concentration ranges of the various techniques.

An ultraviolet (UV) technique that measures the absorbance of NO3– at 220 nm is suitable for
screening uncontaminated water (low in organic matter).

Ultraviolet Spectrophotometric Screening Method

The NO3– calibration curve follows Beer’s law up to 11 mg N/L.

Measurement of UV absorption at 220 nm enables rapid determination of NO 3–. Because


dissolved organic matter also may absorb at 220 nm and NO 3– does not absorb at 275 nm,
a second measurement made at 275 nm may be used to correct the NO 3– value. The extent
of this empirical correction is related to the nature and concentration of organic matter and
may vary from one water to another. Consequently, this method is not recommended if a
significant correction for organic matter absorbance is required, although it may be useful
in monitoring NO3– levels within a water body with a constant type of organic matter.
Correction factors for organic matter absorbance can be established by the method of
additions in combination with analysis of the original NO 3– content by another method.
Sample filtration is intended to remove possible interference from suspended particles.
Acidification with 1N HCl is designed to prevent interference from hydroxide or carbonate
concentrations up to 1000 mg CaCO3/L. Chloride has no effect on the determination.

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III. A. APPARATUS AND REAGENTS

APPARATUS

Spectrophotometer Graduated Cylinder


Erlenmeyer Flask Burette
Pipet Wash Bottle
Pipetol

REAGENTS

1. Nitrate-free water:

Use redistilled or distilled, deionized water of highest purity to prepare all solutions and
dilutions.

2. Stock nitrate solution:

Dry potassium nitrate (KNO3) in an oven at 105°C for 24 h.


Dissolve 0.7218 g in water and dilute to 1000 mL. Preserve with 2 mL CHCl 3/L. This solution is
stable for at least 6 months. 1.00 mL = 100 µg NO3–-N

3. Intermediate nitrate solution:

Dilute 100 mL stock nitrate solution to 1000 mL with water. Preserve with 2 mL CHCl 3/L. This
solution is stable for 6 months. 1.00 mL = 10.0 µg NO3–-N

Hydrochloric acid solution, HCl, 1N:

Dilute sufficient amount of concentrated laboratory grade HCl to prepare a desired volume
of 1 N HCl.

IV. METHODOLOGY

a. Treatment of the Sample

1. Shake the water sample well


2. Pour 50 mL of water sample into an Erlenmeyer flask.
3. Add 1 mL HCl solution and mix thoroughly.
4. Read absorbance or transmittance against redistilled water set at zero absorbance
or 100% transmittance. Use a wavelength of 220 nm to obtain NO 3– reading and a
wavelength of 275 nm to determine interference due to dissolved organic matter.
5. Repeat all procedures for two more trials.

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means, electronic, mechanical, photocopying, recording, or otherwise of any part of this document, without the prior written permission of SLU, is strictly prohibited.
b. Preparation of Standard Curve

1. Prepare NO3– calibration standards in the range 0 to 7 mg NO3–-N/L by diluting to 50


mL the following volumes of intermediate nitrate solution: 0, 1.00, 2.00, 4.00, 7.00 . . . 35.0 mL.
Treat NO3– standards in same manner as samples.

Calculation

For samples and standards, subtract two times the absorbance reading at 275 nm from
the reading at 220 nm to obtain absorbance due to NO 3–. Construct a standard curve by
plotting absorbance due to NO3– against NO3–-N concentration of standard. Using
corrected sample absorbances, obtain sample concentrations directly from standard
curve. NOTE: If correction value is more than 10% of the reading at 220 nm, do not use
this method.

V. REFERENCES

Standard Methods for the Examination of Water and Wastewater, 20th Edition.

HOATHER, R.C. & R.F. RACKMAN. 1959. Oxidized nitrogen and sewage effluents observed
by ultraviolet spectrophotometry. Analyst 84:549. GOLDMAN, E. & R. JACOBS. 1961.

Determination of nitrates by ultraviolet absorption. J. Amer. Water Works Assoc. 53:187.

ARMSTRONG, F.A.J. 1963. Determination of nitrate in water by ultraviolet spectrophotometry.


Anal. Chem. 35:1292.

NAVONE, R. 1964. Proposed method for nitrate in potable waters. J. Amer. Water Works
Assoc. 56:781.

Property of and for the exclusive use of SLU. Reproduction, storing in a retrieval system, distributing, uploading or posting online, or transmitting in any form or by any
means, electronic, mechanical, photocopying, recording, or otherwise of any part of this document, without the prior written permission of SLU, is strictly prohibited.

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