Colorimetric Determination of Ammonia in Air Using a Hanging Drop

Authors: Erika P. Felix a ; Arnaldo A. Cardoso a

Abstract
A simple and sensitive method for determining atmospheric ammonia (NH 3 ), using a hanging drop, is described. A colorimetric sensor is
composed of two optical fibers and the source of monochromatic light implemented was a red light emitting diode (LED) (635 nm). Preliminary
experiments were carried out in order to optimize the geometry of the sensor. These tests showed that the best signal absorbance was obtained
using a 22 µL deionized water drop for sampling the gas and as addition of 4 µL of each of the reactants to form the blue dye (indophenol). Some
important analytical parameters were also studied, including sampling time and flow rate. The analytical curve was constructed with a
concentration range of 3-20 ppbv of gaseous NH 3standard. The detection limit reached was of ca 0.5 ppbv. It was observed that formaldehyde
and diethylamine did not interfere. However, studies showed that hydrogen sulfide caused a negative interference of 20%, when present in the
atmosphere in a concentration equal to that of NH 3 . The method considered here was shown to be easy to apply, making it possible to make a
determination every 17 min.
Keywords: Ammonia in air; Hanging drop; Gas generation; Optical fibers; Air analysis; Droplet sensor

Collection and ion chromatographic determination of ammonia and methylamines in air.

Bouyoucos SA , Melcher RG .
Abstract
A method is described for the collection of ammonia (NH3), monomethylamine (MMA), dimethylamine (DMA), and trimethylamine (TMA)
from air and their subsequent determination by ion chromatography. Samples are collected with 800-mg silica gel sampling tubes at a flow rate of
1 L/min for 10 minutes or at 100 mL/min for up to 7.5 hours. Samples collected with sulfuric acid-treated tubes can be stored at room
temperature for at least 21 days with no loss in recovery. Untreated samples can be stored in a refrigerator up to 32 days. The method has been
validated from 2 to 50 ppm v/v when a 10 L air sample is taken. No loss in recovery was observed when sampling up to 23 L of air at 100%
relative humidity. The recovery and total precision (95% confidence level) for NH3, MMA, DMA, and TMA were 91 +/- 12.5%, 93 +/- 10.3%,
92 +/- 9.6% and 84 +/- 17.6%, respectively.
PMID: 6837437 [PubMed - indexed for MEDLINE]
MeSH Terms, Substances
Determination of Trace Amounts of Ammonia in Air Using a Batchwise Collection/Concentration Method by Spectrophotometry
Accession number; 05A0868201
Title; Determination of Trace Amounts of Ammonia in Air Using a Batchwise Collection/Concentration Method by
Spectrophotometry
Author; SUEKANE TAKASHI(Okayama Univ., Graduate School of Natural Sci. and Technol., JPN) OSHIMA
MITSUKO(Okayama Univ., Graduate School of Natural Sci. and Technol., JPN) MOTOMIZU SHOJI(Okayama Univ.,
Graduate School of Natural Sci. and Technol., JPN)
Journal Title; Bunseki Kagaku
Journal Code: F0008A
ISSN: 0525-1931
VOL. 54; NO. 10; PAGE. 953-957(2005)
Figure&Table&Reference; FIG.3, TBL.2, REF.11
Pub. Country; Japan
Language; Japanese
Abstract; Ammonia in the atmosphere can be determined by an improved indophenol method with 1-naphthol. Ammonia
dissolved in water reacts with sodium hypochlorite in the presence of sodium hydroxide and 1-naphthol to form an indophenol
blue dye, which can be measured at 720 nm (maximum absorbance). Since ammonia in the atmosphere can be absorbed in
purified water almost completely, a calibration graph using standard aqueous ammonium chloride solutions can be used. The
calibration graph showed a good linearity (y=0.37*10'5'x+0.027, R'2'=0.9992) and the detection limit was 0.9*10'-6' M. For
practical samples, the air was collected into a 50 ml plastic syringe with an air-tight cap containing 3.0 ml of purified water as the
absorbing solution, followed by shaking it by hand. The method was successfully applied to the determination of ammonia in
indoor and outdoor air samples. (author abst.)
[Method of determination of ammonia in the air].
[Article in Polish]
Rogaczewska T .
Abstract
The method for determination of ammonia in the air that has been used so far, based on the reaction with Nessler reagent, is outdated. In this
method the final colour solutions are not non-ideal solution (there occurs turbidity), which may result in smaller accuracy of
determination. Besides this method is not sufficiently specific. A newly-worked out method for determining ammonia in the air is based on
spectrophotometric measurement of the green product of ammonium ions reaction with sodium hypochlorite and sodium salicylate. This method
is more sensitive, precise and specific than the method for determination with Nessler reagent.
PMID: 607087 [PubMed - indexed for MEDLINE]

AMMONIA
7.2 ENVIRONMENTAL SAMPLES
Water and waste water samples can be analyzed for ammonia by EPA Test Methods 1689 (EPA 2001a), 1690 (EPA 2001b), and
349.0 (EPA 1997). Analogous procedures (ie, Method APHA 4500) have been approved and published jointly by the American
Public Health Association, American Water WorksAssociation, and Water Pollution Control Association. These methods are
suitable for drinking, surface,and saline waters, and domestic and industrial effluent, and can be applied to biosolids. These and
other methods for determining ammonia in environmental samples are listed in Table 7-2. Ammonia is reported as ammonia
nitrogen. Two methods that are suitable for water employ colorimetric techniques, Nesslerization, and phenate methods. Nessler's
reagent, an alkaline mixture of mercuric and potassium
iodide, produces a yellow to brown color with ammonia, whereas the phenate reagent, alkaline phenol, and hypochlorite produce
a blue color (EPA 2001a, 2001b; Greenberg et al. 1985). In the titrimetric method, the distillate is titrated with standard sulfuric
acid with an appropriate indicator. The ammonia electrode employs a hydrophobic gas-permeable membrane to separate the
sample solution from an
internal ammonium chloride solution: ammonia diffusing through the membrane changes the pH of the internal solution and is
sensed by a pH electrode. For determining NH3-N concentrations above 5 mg/L,the titrimetric and ammonia-selective electrode
methods are preferred. In contrast, gas chromatography/mass spectrometry methods have been developed that permit NH3
detection at concentrations near 20 µg/L for environmental waters (Mishra et al. 2001). Methods for determining ammonia in
water and soil measure ammoniacal nitrogen, the sum of
NH3 and NH4+. In the determination of ammoniacal nitrogen in soil, exchangeable ammonium should be distinguished from
nonexchangeable ammonium.
The former is usually defined as that which can be extracted with KCl (or K2SO4) at room temperature (Bremner
1965). Nonexchangeable ammonium ion is defined as nitrogen held by clays and not displaced by 2M KCl (Bremner 1965). In
the determination of nonexchangeable ammonium, organic forms of ammonia are first removed, the minerals containing the
nonexchangeable ammonium are then
decomposed with HF, and the ammonium ions released. In colorimetric procedures, turbidity and sample color may lead to
interference. To eliminate interference, the pH of the sample may be raised and the ammonia distilled. Care should be taken to
prevent losses in water samples due to volatilization and microbial transformation. To prevent such losses, samples should be
acidified soon after collection and refrigerated. Care should also be taken during storage and treatment of soil samples to prevent
ammonia