I am trying to come up with a research on the levels of these two in waste water from the industrial effluents. I need someone who has done the same research to give me some light.
Today, compounds in trace concentrations as low as parts per trillion may be identified with the appropriate detector. The analytical methods most frequently used for determination of the carcinogenic PAH, MTBE are HPLC with fluorescence detection and GC –MS. The HPLC detector most often used in petroleum environmental analysis is the fluorescence detector. These detectors are particularly sensitive to aromatic molecules, especially the PAHs. A UV detector may be used to measure compounds which do not fluoresce.
previous study that i have read is on detection of PAH on groundwater. so, i guess the same method can be used for your research. for the preparation method, filtration through prebaked glass-fiber filters to remove suspended sediments; cleanup with bonded-phase extraction column; elution of organics from column with acetonitrile followed by methylene chloride; water removal (Na2SO4);concentration by nitrogen blow-down.. not just that, PAH also can be detected using biosensor.
But have you tried to sample and analyze the waste water? I would say that first you need to analyze few samples, so that you can check if levels of PAHs are detectable.
Most of the times, they're not (either because extraction method is not appropriate or because concentrations are too low). In that case, you may use biosensors/biomonitors (a living organism), which will accumulate PAHs over time and will for sure (if PAHs are present) show detectable concentrations. You just need to optimize their use to your specific case.
In past I have used GC with FID detector for analyzing PAHs in soil and water. Details of those analysis can be found in my PH.D dissertation and also in related papers as are listed in my publication list.
At that time I also tried to use HPLC and GC-MS but as analysis by those equipments were done by people other than me, I had difficulty in getting reproducible and understandable results so I preferred to use GC with FID by myself other than letting other people do such analysis.
GC/MS analysis with head space sampling (i.e. EPA 8260 + EPA 5021) can be a very useful method for determine MTBE (and also VOC, BTEXs, organohalogenated cpds...) and the lightest of the PAH (i.e. Naphtalene). This can be don also with GC/MS and purge & trap techinques, but this sistem is much more sensitive and delicate with potential problematic matrices like waste water. MS destector used in sca mode could provide you a very reliable identification and quantification of compounds. On the other hands, for semivolatile and heaviest PAH a wide range method like EPA 8270 (GC/MS) also works very well. In my laboratory we extract by liquid-liquid extraction, purify on silica and analyze ba GC/MS single quadrupole. Also you can absorb waste water sample onto a solid support and extract with ASE (accelerated solvent extraction) or MAE (microwave assisted extractions) techniques. Be careful when using diatomaceous earth and MAE techniques and non selective detectors (FID) because we had great problems with interferences.
We have analyzed PAHs in wastewater, after solid phase extraction, by HPLC (HPLC-1100 system, Agilent, Santa Clara, CA, USA), using Vydac C18-RF column, 5 µm, 250 mm × 4.6 mm I.D. (Grace, Columbia, MD, USA) and coupled with a fluorescence detector (Agilent-1100).The column was kept at 30 °C. Mobile phase was composed of a solvent A (water) and a solvent B (acetonitrile) at a constant flow rate of 1.5 mL min-1. The gradient was programmed to increase the amount of solvent B from an initial 30% to 100% in 35 min, returning to the initial conditions (70% A) in 5 min. This condition was maintained until 5 min. The sample volume injected into the HPLC system was 20 µL.
GC-MS is a useful technique. We have used this technique in Asian. water.You can see our publications with Tokyo University of Technology and Agriculture.
The best method for measuring PAH in environmental samples using HPLC methods . The best method to measure MTBE purge-and-trap gas chromatography or Headspace-Gas Chromatography Please refer to Attachment ( Headspace-Gas Chromatography).
My Ph. D thesis was on the biodegradation of PAHs. We used GC-FID and GC/MS and HPLC for analysis using UV and Fl detectors. They worked well
Today the best way of detection and quantitation by HPLC is UHPLC C-18 RP sub 2 micron particle column attached to FL detector. GC is good but the process is slow. GC-MS is robust technique for detection and quantification of PAHs