The Malaysian Journal of Analytical Sciences Vol 17 No 1 (2013): 38 – 49

 

 

 

AN EXPERIMENTAL DESIGN APPROACH FOR  THE ANALYSIS OF LIQUID PHASE PRODUCTS IN  WATER FOR HYDROGENOLYSIS OF GLYCEROL  USING  IMMERSED SOLID-PHASE MICROEXTRACTION

 

(Pendekatan Reka Bentuk Eksperimen Untuk Analisis Produk Fasa Cecair Dalam Air Bagi Tindak Balas Hidrogenolisis Gliserol Menggunakan Rendaman Mikroekstraksi Fasa Pepejal)

 

Noraini Hamzah^1,2*, Rozita Osman¹,  Mohd Ambar Yarmo²

¹Faculty of Applied Sciences,

Universiti Teknologi MARA, 40450 Shah Alam, Selangor Darul Ehsan, Malaysia

²Faculty of Science and Technology,

Universiti Kebangsaan Malaysia, 43600 Bangi, Selangor Darul Ehsan, Malaysia

 

*Corresponding author: norainihamzah@gmail.com

 

 

Abstract

In this study, a response surface methodology (RSM) was applied to optimize the immersed-solid-phase microextraction (immersed-SPME) conditions for the first time using a polyacrylate (PA) coated fiber. This was to determine liquid phase compounds in water for hydrogenolysis  reaction of glycerol. There are a three-factor response surface experimental design was used to evaluate the interactive effects of extraction temperature (30-70 ºC), extraction time (10-30 minutes) and desorption time (2-18 minutes) on the analysis of liquid phase compounds in water for hydrogenolysis of glycerol using immersed-solid-phase microextraction (immersed-SPME). The extraction conditions using immersed-SPME were optimized in order to achieve high enrichment of the analytes from aqueous samples. The isolated compounds from the SPME fiber were desorbed  and separated on a capillary polar column of a gas chromatography-flame ionization detector (GC-FID). The extraction time and desorption time were found significant in increasing the  amount of glycerol in aqueous hydrogenolysis of glycerol. Nevertheless, the effect of extraction temperature was not significant. In terms of interactions between the effects, the relation between extraction temperature and extraction time was the most significant. The optimised immersed-SPME conditions were at extraction temperature of 27 °C, extraction time of 30 minutes and 15 minutes of desorption time. Thus, the application of SPME was found to be a rapid and effective technique in the determination of glycerol and  propylene glycol compounds in aqueous hydrogenolysis glycerol.

 

Keywords: Solid phase microextraction (SPME), Hydrogenolysis ,Glycerol, Response Surface Method (RSM)

 

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