1070-4272/02/7509-1427$27.00C2002 MAIK [Nauka/Interperiodica]
Russian Journal of Applied Chemistry, Vol. 75, No. 9, 2002, pp. 1427!1429. Translated from Zhurnal Prikladnoi Khimii, Vol. 75, No. 9,
2002, pp. 1459!1461.
Original Russian Text Copyright + 2002 by Baksanova, Val’tsifer, Budnikov, Kondrashova.
OF CHEMISTRY AND TECHNOLOGY
Gas-Chromatographic Determination of Acrylic Acid
in Aqueous Solutions
L. E. Baksanova, V. A. Val’tsifer, V. I. Budnikov, and N. B. Kondrashova
Institute of Technical Chemistry, Ural Division, Russian Academy of Sciences, Perm, Russia
Received April 22, 2002
Abstract-A procedure was developed for determining acrylic acid in aqueous solutions at its concentration
within 0.5!20 MPC.
Analysis of water from reservoirs and especially
wastewater for the content of microimpurities of
harmful substances is a complicated problem, because,
first, the substances to be determined have low maxi-
mum permissible concentrations (MPC), and, second,
the analysis results can be affected by numerous con-
comitant impurities present in wastewater from both
a given enterprise and neighboring plants.
In the past years, the production and consumption
of acrylic monomers, polymers, and composites
based on them considerably increased; new applica-
tions arose, and new countries became involved in
the production. Therefore, environmental control
of plants producing these substances is an urgent
At the majority of plant laboratories, wastewater
is analyzed using unified procedures. However, as the
requirements to potable water and to wastewater treat-
ment became more stringent, it appeared necessary
to develop advanced analytical procedures with low
detection limits for determining impurities of highly
toxic substances. Major attention is given to reducing
the time required for analysis, since at many plants the
composition of natural water and especially waste-
water varies with time.
The most widely used procedure for determining
trace amounts of organic substances in multicompo-
nent mixtures is gas chromatography. To determine
organic pollutants, such methods are recommended
as capillary gas chromatography, high-performance
liquid chromatography, supercritical fluid chromatog-
raphy, IR spectroscopy, and exclusion chromatog-
raphy [1, 2].
Aqueous solutions containing more than 10%
organic acids can be, in principle, chromatographed
without pretreatment. However, analysis of aqueous
solutions of polar compounds such as free acids is
complicated by sorption; this is a serious problem not
only with traces but even with macroamounts of acids.
Gas-chromatographic determination of organic acids
is also complicated by their low volatility, requiring
the use of high temperatures, close to the limiting
working temperatures of the majority of available
stationary phases; furthermore, acids tend to associate
in the vapor phase. To overcome these difficulties,
especially in analysis of trace amounts, acids are con-
verted to more volatile and less polar derivatives,
most often to esters . This increases the analysis
sensitivity and eliminates interferences caused by ad-
sorption. However, lower acids, in contrast to their
higher homologs, cannot be esterified quantitatively.
High-molecular-weight acids can be efficiently
recovered and concentrated from sea and ground
waters by extraction with organic solvents . Extrac-
tion of acids with diethyl ether in the presence of a
salting-out agent allows the acid detection limit to be
decreased. However, this concentrating procedure is
time- and labor-consuming.
All these problems pertain equally to chromato-
graphic determination of traces of acrylic acid (AA)
Traditional methods for preliminary concentration
of a sample (sorption on solid adsorbents, extraction
followed by solvent evaporation, distillation, head-
space analysis) show poor efficiency in concentrating
AA from aqueous solutions and do not ensure the
required sensitivity of analysis .
The goal of this work was to develop a simple,
reliable, and highly sensitive procedure for determina-
tion of AA microimpurities in aqueous solutions.