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3.3.3 Un-reacted alkanolamine and identification of degradation product using HPLC
An Agilent series 1100 brand of HPLC was used to monitor the degradation products and un-
reacted alkanolamine after Fenton’s treatment. YMC-Pack PolymerC18 reverse phase column was used with 100mM Na
2
HPO
4
100mM NaOH 6040, pH 12 as eluent and UV 215 nm and 253nm detector. Flow rate of the
eluent was 1 mlminute. Degradation product determination was performed by comparison of the sample with the standard compound which was assumed.
Qualitative analysis was based on the retention time of each compound in the chromatogram, while quantitative un-reacted alkanolamine analysis was based on the
calibration curve prepared using standard alkanolamine. The calibration curve for MEA and DEA are expressed below:
MEA : Area = 0.210[MEA]
– 2.267 3.4
DEA : Area = 0.443[DEA] + 10.076
3.5
3.3.4 Identification of the functional groups using FTIR
The method to characterize the functional groups of the degradation product after Fenton’s treatment was done by infrared spectroscopy. A Perkin Elmer
Spectrum One Fourier Transform Infrared Spectrometer was used to obtain the spectra.
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3.3.5 Un-reacted H
2
O
2
determination
Determination of the un-reacted H
2
O
2
in the Fenton’s process was performed using 0.05 KMnO
4
solutions. Titration of acidified sample after filtration from Fenton’s process was conducted. Change color from colorless to light pink is the end
point of titration. Sodium thiosulphate NaS
2
O
3
was used to standardize the KMnO
4
by iodometry with 1 starch solution as indicator Mendham, 2000.
3.3.6 pH
The pH of the mixed liquor was measured using pH probe of HACH sens ion 1 pH meter. This pH meter was calibrated regularly. The pH of Fenton’s process was
used to monitor the oxidation process in the reactor, while pH of bioreactor to monitor the activity of microorganism in the bioreactor. The range of pH
measurement was 2-5 on Fenton oxidation and 6.5-8 on biological oxidation.
3.3.7 DO Dissolved Oxygen
Dissolved oxygen was measured using HQ30d flexi HACH DO meter. LD0101 DO Probe was used for measurement of the dissolved oxygen in the
bioreactor during the biodegradability test. The rate of oxygen consumption also can be monitored by this parameter.
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3.3.8 MLVSS Mixed liquor volatile suspended solid
Total suspended solid was measured using method 2540-E that has been approved by APHA 2001. An increase in the MLVSS in the bioreactor represented
the growth of microorganism and yield of biomass. The residue from method 2540-E was ignited to a constant weight at 550°C. The remaining solid represent the fixed
suspended solid while the weight lost on ignition was the volatile suspended solid. Further, the MLVSS was calculated by:
mg volatile solidL = 3.6
mg fixed solidL = 3.7
Where: A = weight of residue + dish before ignition, mg
B = weight of residue + dish or paper filter after ignition, mg, and C = weight of dish or paper filter, mg
A – B x 1000
sample volume ml
B – C x 1000
sample volume ml
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3.3.9 MLSS Mixed liquor suspended solid
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