Sains Malaysiana 39(2)(2010): 227–231

Validation of a Solid Phase Extraction Technique for the Determination of Halogenated Acetic Acids in Drinking Water

(Validasi Satu Teknik Pengekstrakan Fasa Pepejal bagi Penentuan Asid Asetik Terhalogen dalam Air Minum)

Sadia Waseem & Md. Pauzi Abdullah*

Centre for Water Research and Analysis, Faculty of Science and Technology

Universiti Kebangsaan Malaysia, 43600 Bangi, Selangor D.E., Malaysia

Received: 16 April 2009 / Accepted: 6 July 2009

ABSTRACT

Haloacetic acids (HAAs) are one of the most common disinfection by-products formed during chlorination of drinking water. An analytical method involving solid phase extraction (SPE) followed by gas-chromatograph mass-spectrometry (GC-MS) was developed and optimized using experimental design to determine the HAAs in water. Selectivity, percent recovery, and detection limit studies were carried out on a Silia-SAX (Trimethyl ammonium chloride) SPE. Under optimized conditions, average recoveries for nine HAAs spiked in drinking water samples range from 69.2% to 108.2 %. The relative standard deviation (RSD) data were found to range from 2.5 % to 12.5% based upon five repeat recovery experiments and detection limit range of 0.16 to 0.009μg/l were obtained. On this basis, SPE was studied as a possible alternative to liquid-liquid extraction (LLE) for the analysis of HAAs in water. The performance of the SPE-GC-MS with actual water samples was tested.

Keywords: Gas-chromatography mass-spectrometry; haloacetic acids; SPE

ABSTRAK

Asid haloasetik(HAA) merupakan salah satu hasil sampingan utama disinfeksi yang terbentuk semasa proses pengklorinan air minum. Satu kaedah analisis yang melibatkan pengekstrakan fasa pejal (SPE) diikuti oleh kromatografi gas-spektrometri jisim (GC-MS) telah dibangunkan dan dioptimumkan berdasarkan teknik reka bentuk eksperimen bagi menentukan HAA di dalam air minum. Faktor kepilihan, peratusan pemulihan dan had pengesanan telah dikaji menggunakan Silia-SAX (penukar anion ammonium kuaternari) SPE. Di bawah keadaan optimum, purata perolehan bagi sembilan komponen HAA dalam sampel air minum adalah dalam julat 69.2% sehingga 108.2%. Sisihan piawai relatif(RSD) bagi lima ulangan eksperimen didapati mempunyai julat antara 2.5% hingga 12.5% dan had pengesanan mempunyai julat 0.16 to 0.009μg/l. Hasil ini menunjukkanSPE yang dibangun boleh digunakan sebagai kaedah alternatif menggantikan kaedah ekstraksi cecair-cecair(LLE) bagi analisisHAA di dalam air. Prestasi kaedah SPE-GC-MS yang dibangun diuji terhadap sampel air sebenar.

Kata kunci: Asid haloasetik; kromatografi gas-spektrometri jisim; SPE

REFERENCES

Anastasia, D.N., Golfinopoulos, S.K. & Kostopoulou, M.N. 2002. Determination of haloacetic acids in water by acidic methanol esterification GC-ECD method. Water Research 36: 1089-1094.

Clesceri L.S., Greenberg A.E. & Eaton A.D. 1998. Standard Methods for Examination of Water and Wastewater. 20th ed., APHA, AWWA, and WEF. Washington, DC.

Huber, L. 2001. Validation of analytical methods: review and strategy. (on line ) http://www. Labcompliance.com/val/rev.html (27 August 2001).

IUPAC. 1995. Nomenclature in evaluation of analytical methods, including detection and quantification capabilities (IUPAC Recommendations 1995). Pure and Appl. Chem. 67: 1699-1723.

Klinefelter, G.R., Suarez, J.D., Roberts, N.L. & Deangelo, A.B. 1995. Preliminary screening for the potential of drinking water disinfection byproducts to alter male reproduction. Reprod. Toxicol. 9: 571-578.

Kronberg, L. & Christman, R.F. 1989. Chemistry of mutagenic by products of water chlorination. Sci. Tot. Environ. 81/82: 219-230.

Martinez, D., Borrull, F.M., Calull, M., Ruana, J. & A. Colom. 1998. Application of solid-phase extraction membrane disks in the determination of haloacetic acids in water by gas chromatography-mass spectrometry. Chromatographia 48: 811-816.

Pawlecki-Vonderheide, A.M., Munch, D.J. & Munch, J.W. 1997. Research associated with the development of EPA Method 552.2. J. Chromatogr. Sci. 35: 293-301.

Sadia, W. & Pauzi, A. 2009. SPE-GC-MS-SIM method for determination of halogenated acetic acids in drinking water system. Chromatographia DOI 10.1365/s10337-009-1065-4.

Singer, P.C. 1999. Humic substances as precursors for potentially harmful disinfection by-products. Wat. Sci. Technol. 40: 25-30.

Sukiman, S. & Pauzi, A. 1993. A chemical quality of Malaysian drinking water sources. Drinking water quality: Microbiological and Public Health Aspects. Bangi: Penerbit UKM p. 63-69.

Susan, D.R. 2003. Disinfection by-products and other emerging contaminants in drinking Water. Trends in Analytical Chemistry 22(10): 666-684.

USEPA. 1992. Method 552.1: determination of haloacetic acids and dalapon in drinking water by ion exchange liquid-solid extraction and gas chromatography with electron capture detection. Environmental monitoring and System Laboratory, Cincinnanti, Ohio.

USEPA. 1995. Method 552.2: determination of haloacetic acids and dalapon in drinking water by liquid–liquid extraction, derivatization and gas chromatography with electron capture detection. Environmental Monitoring and System Laboratory, Cincinnati, OH.

*Corresponding author; email: mpauzi@ukm.my