SKA 3013 ANALYTICAL CHEMISTRY

Determination of MeEthHg and DiethHg in Pilot-Scale Activated Sludge wastewater Treatment Plant by Using GC/MS
Group members Click to edit Master subtitle style : Kan Shieh Ting (D20091034924) Nor Izati binti Mat Yusoff (D20091035136) Siti Nurul Shahida binti Mohd Abd Hadi (D20091035137) 5/5/12

Sample Preparation
1. 200ml of sample 30 g NaCl + 2.72 g CH3COOH are added to the standard solution. 2. Drops CH3COOH or NaOH for pH adjustment to 4.5 3. The solution was placed in a magnetic stirrer for 5 min to obtain proper dilution. Then, transfer into a separatory funnel where 20 ml hexane and 2 ml NaBet4 1% were added.

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4. Performed a 20 min liquid-liquid extraction with simultaneous ethylation and then the solution was left undisturbed for approximately 40 min for phase separation. 5. The solution was centrifuged for 10 min at 200 rpm. 6. The supernatant was concentrated under a gentle stream of nitrogen. 7. 1l of the final extract was injected into the GC-MS.

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GC Condition

Column : DB-624 , 30 m 0.32 mm 1.8 m Inlet (injection) : split / splitless , 200C , split 1:25 Oven : 60 C (2 min) 80 C @ 20 C/min 200 C Gas : Helium , 1.25 ml/min

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Peak 2

Peak 1

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Peak 1
Number of plate, N = 16 (tR/WB)2 = 16(6.65/0.2)2 = 17689

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Retention factor, k = (tR -tm)/tm = (6.65 1.6)/1.6 = 3.16 Neff = N (K/K+1)2 = 17689 (3.16/4.16)2 Click to edit Master subtitle style = 10206
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Peak 2
Number of plate, N = 16 (tR/WB)2 = 16 (8.2/0.1)2 = 107584

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Retention factor, k = (tR -tm)/tm = (8.2-1.6)/1.6 = 4.13 Neff = N (K/K+1)2 = (107584)(4.13/5.13)2 = 69728
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Resolution, Rs = (tr2-tr1)/ (wb1+wb2)/2 = (8.2-6.65)/ (0.2+0.1)/2 = 10.33 Separation factor, = K2/K1 = 4.13/3.16 = 1.3
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Technique and theory applied

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Gas chromatography mass spectrometry (GC-MS)

hyphenated technique consisting of two analytical procedures in sequence, namely a Gas Chromatography (GC) separation followed by Mass Spectroscopy (MS) detection. GC step is to separate multiple compounds in a sample so that they reach the MS detector one at the time. The GC-MS is composed of two major building blocks: the gas chromatograph and the mass spectrometer.
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The gas chromatograph utilizes a capillary column which depends on the column's dimensions (length, diameter, film thickness) as well as the phase properties. molecules are retained by the column and then elute (come off of) from the column at different times (called the retention time) mass spectrometer downstream to capture, ionize, accelerate, deflect, and detect the ionized molecules separately using their mass to charge ratio.

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