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

 

Diserahkan: 16 April 2009 / Diterima: 6 Julai 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 menunjukkan SPE yang dibangun boleh digunakan sebagai kaedah alternatif menggantikan kaedah ekstraksi cecair-cecair (LLE) bagi analisis HAA di dalam air. Prestasi kaedah SPE-GC-MS yang dibangun diuji terhadap sampel air sebenar.

 

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

 

RUJUKAN

 

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*Pengarang untuk surat-menyurat; email: mpauzi@ukm.my