Simultaneous Pre-Concentration of Cadmium and Lead in Environmental Water Samples with Dispersive Liquid-Liquid Microextraction and Determination by Inductively Coupled Plasma-Atomic Emission Spectrometry


Environmental Laboratory, NSTRI, Tehran, Iran


The dispersive liquid–liquid microextraction (DLLME) method for determination of Pb+2 and Cd+2 ions in the environmental water samples was combined with inductively coupled plasma-atomic emission spectrometry (ICP-AES). Ammonium pyrrolidine dithiocarbamate (APDC), chloroform and ethanol were used as chelating agent, extraction solvent and disperser solvent, respectively. Some effective parameters on the microextraction and the complex formation were selected and optimized. These parameters included extraction and disperser solvent type as well as their volume, extraction time, salt effect, pH, sample volume and amount of the chelating agent.   Under the optimum conditions, the enrichment factor of 75 and 105 for Cd+2 and Pb+2 ions respectively was obtained from only 5.00mL of water sample. The detection limit (S/N=3) was 12 and 0.8ngmL−1 for Pb and Cd respectively. The relative standard deviation (RSDs) for five replicate measurements of 0.50 mgL−1 of lead and cadmium was 6.5 and 4.4 % respectively. Mineral, tap, river, sea, dam and spiked water samples were analyzed for Cd and Pb amount.


Fassett D.W., in Metals in the Environment,
Academic Press, New York, 1980. pp 61-110.
Patriarca M., A. Menditto, B. Rossi, T. D. B.
Lyon, G. S. Fell, Environmental exposure to
metals of newborns, infants and young children,
Microchemical Journal, Volume 67, 2000. Pages
Hayes R.B., the carcinogenicity of metals in
humans, Cancer Causes Control. 1997 May;
Bergbäck B., Carlsson M., Heritage of cadmium
and lead, A case study of a Swedish accumulator
factory. Sci Total Environ 166:35ââ‚‌“42,1995.
Bellinger D. C., Lead neurotoxicity and
socioeconomic status: Conceptual and analytical
issues. Neurotoxicology, 2008. 29: 828-32.
Patocka J., K. Cerny, Inorganic Lead
Toxicology, Acta Medica (Hradec Kralove), V. 46,
No 2, 65-72, 2003.
Waalkes M.P., Cadmium Carcinogenesis,
Mutat.Res, 2003. 10:553,107-120
Tellez-Plaza M., Navas-Acien A., Crainiceanu
C. M., Cadmium exposure and hypertension in the
- 2004 National Health and Nutrition
Examination Survey (NHANES). Environmental
Health Perspectives, 2008. 116: 51-6.
International Agency for Research on Cancer
(IARC) Monographs on the Evaluation of
Carcinogenic Risks to Humans. Volume 58:
Beryllium, Cadmium, Mercury, and Exposures in
the Glass Manufacturing Industry. Summary of
Data Reported and Evaluation. 1997. Available at
/volume58.pdf.Accessed May 1, 2008.
Yang R.S.H., Goehl T. J. Brown R. D.,
Chatham A. T., Arneson D. W., Buchanan R. C.,
Harris R. K., 1989. Toxicological studies of a
chemical mixture of 25 ground water
contaminants. I. Chemistry development. Fundam.
Appl. Toxicol. 13:366ââ‚‌“376.
Batterham G. J., N.C. Munksgaard , D. L.
Parry, Determination of Trace Metals in Sea-water
by Inductively Coupled Plasma Mass
Spectrometry After Off-line Dithiocarbamate
Solvent Extraction, J. Anal. At. Spectrom.,
, 12, 1277 - 1280
Li X., Schramel P., Wang Z., Grill P., Yedile
A., Kettrup A., Determination of trace amounts of
Sb, Pb, Tl in water samples by inductively coupled
plasma atomic emission spectrometry after a
diantipyrylmethane-iodide third phase
preconcentration, Microchim. Acta, 124:171-178,
Chen J., Xiao S., Wu X., Fang K., Liu W.,
Determination of lead in water samples by
graphite furnace atomic absorption spectrometry
after cloud point extraction, Talanta, 67:992-996,
Batterham G. J., Munksgaard N.C., Parry D.L.,
Determination of Trace Metals in Sea-water by
Inductively Coupled Plasma Mass Spectrometry
After Off-line Dithiocarbamate Solvent Extraction,
J. Anal. At. Spectrom., 1997. 12, 1277 ââ‚‌“ 1280.
Mesquita R. B., Fernandes S. M. V., Rangel A.
O. S., A flow system for the spectrophotometric
determination of lead in different types of waters
using ion-exchange for pre-concentration and
elimination of interferences, Talanta 62:395-401,
Dogan C. E., Akcin G., Solid Phase Extraction
and Determination of Lead in Water Samples
Using Silica Gel Homogeneously Modified by
Thiosalicylic Acid, Anal Lett , 40: 2524-2543,
Rezaee M., Assadi Y., Milani Hosseini M. R.,
Aghaee E., Ahmadi F., Berijani S., Determination
of organic compounds in water using dispersive
liquid-liquid microextraction ,J chromatogr A
:1-9, 2006.
Fatahi N., Assadi Y., Milani Hosseini M. R.,
Zeini Jahromi E., 2007. Determination of
chlorophenols in water samples using
simultaneous dispersive liquidââ‚‌“liquid
microextraction and derivatization followed by gas
chromatography-electron-capture detection. J
Chromatogr A 1157:23ââ‚‌“29
Berijani S., Assadi Y., Anbia M., Milani
Hosseini M. R., Aghaee E., Dispersive liquidââ‚‌“
liquid microextraction combined with gas
chromatography-flame photometric detection:
Very simple, rapid and sensitive method for the
determination of organophosphorus pesticides in
water, J Chromatogr A, 1123:1-9, 2006.
Salahinejad M., Aflaki F., Optimization and
determination of Cd (II) in different environmental
water samples with dispersive liquidââ‚‌“liquid
microextraction preconcentration combined with
inductively coupled plasma optical emission
spectrometry, Environ. Monit. Assess. 177, 2011.
Liang P., Sang H., Determination of trace lead
in biological and water samples with dispersive
liquidââ‚‌“liquid microextraction preconcentration,
Anal. Biochem. 380, 2008. 21ââ‚‌“25
Jiang H., Qin Y., Hu B., Dispersive liquid
phase microextraction (DLPME) combined with
graphite furnace atomic absorption spectrometry
(GFAAS) for determination of trace Co and Ni in
environmental water and rice samples, Talanta 74,