Hava ortamında öncelikli organik kirleticilerin tayini için analitik metot optimizasyonu ve Konya kent atmosferinde izlenmesi
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Dosyalar
Tarih
2007-08-03
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Yayıncı
Selçuk Üniversitesi Fen Bilimleri Enstitüsü
Erişim Hakkı
info:eu-repo/semantics/openAccess
Özet
Bu çalışmanın ilk aşamasında, hava ortamında bulunan poliaromatik hidrokarbon (PAH), poliklorlu bifenil (PCB) ve organoklorlu pestisit (OCP) bileşiklerinin tek bir analitik metot ile kromatografik teknikler kullanılarak kantitatif olarak tayini için metot optimizasyonu gerçekleştirilmiştir. İkinci aşamasında ise oluşturulan metot ile Konya kent atmosferinde gaz ve partikül fazında bulunan PAH, PCB ve OCP bileşikleri izlenmiştir. ii Partikül fazda bulunan bileşiklerin tespiti için en iyi ekstraksiyon verimi ultrasonik ekstraksiyon tekniğinin kullanımı ile 15 dakika sonikasyon süresince, 25 mL n-hekzan/petroleteri (1/1, v/v) solvent karışımının üç defa solvent ekstraksiyonu sonucunda elde edilmiştir. Gaz fazda bulunan bileşiklerin tespiti için ise sokshlet ekstraksiyon tekniğinin kullanımı ile 16 saat ekstraksiyon süresince, 150 mL dietileter/n-hekzan (1/9, v/v) solvent karışımının kullanımı sonucunda elde edilmiştir. GC analizlerinden önce numunede girişim yapan maddelerin uzaklaştırılması ve eş zamanlı olarak bileşik gruplarının fraksiyonlanarak ayrılması için 10 g %5 deaktif silika jel kolon kullanılmıştır. Bileşiklerin elüsyonu Fraksiyon1: 70 mL n-hekzan ve Fraksiyon2: 3x20 mL n-hekzan/etilasetat (1:1, v/v) ile gerçekleştirilmiştir. PAH ve PCB bileşiklerinin tespiti GC/MS sistemi ile OCP bileşiklerinin tespit ise GC/ ? -ECD sistemi ile yapılmıştır. Optimize metodun standart ve surrogate eklenmiş filtrelere uygulanması sonucunda geri kazanım verimleri PCB bileşikleri için %86±2-%104±3 aralığında (RSD<±4), PAH bileşikleri için %66±6-%94±5 aralığında (RSD<±8), OCP bileşikleri içinse %67±5-%120±10 aralığında (RSD<±10) tespit edilmiştir. PUF pluglara eklenen bileşikler için elde edilen metot geri kazanım verimleri PCB bileşikleri için %94±9-%118±8 aralığında (RSD<±9), PAH bileşikleri için %88±1- %120±2 aralığında (RSD<±8), OCP bileşikleri içinse %65±4-%108±6 aralığında (RSD<±9) elde edilmiştir. Matriksin optimum metot üzerine etkisini tespit etmek amacıyla kent havası örneklenmiş filtre ve PUF pluglara standart ve surrogate eklenerek optimize metot geri kazanım verimleri incelenmiştir. Sonuçlar istatistiksel olarak değerlendirildiğinde matrikslerin ekstraksiyon verimleri üzerine önemli bir etkisi (P>0,05) görülmemiştir. Ağustos-2006 ve Mayıs-2007 tarihleri arasında Konya kent atmosferinde trafikten, sanayiden ve evsel ısınmadan kaynaklanan PAH, PCB ve OCP bileşiklerinin gaz ve partikül fazındaki konsantrasyonları, mevsimsel değişimi, meteorolojik parametreler ve diğer hava kirleticileri ile değişimi izlenmiştir. Ortalama PAH konsantrasyonu 30 ng/m3 ile 294 ng/m3 aralığında, PCB konsantrasyonu 0,04 ng/m3 ile 0,14 ng/m3 aralığında, OCP konsantrasyonu 0,81 ng/m3 ile 6,15 ng/m3 aralığında tespit edilmiştir. PAH, PCB ve OCP bileşiklerinin gaz fazında tespit edilen değerler toplam konsantrasyonunun sırasıyla %64-70, %75- iii 90, %45-70 oranındadır. Tüm bileşik grupları için gaz fazındaki konsantrasyon sıcaklık ile artarken, partikül fazındaki konsantrasyon ise azalmaktadır. Sıcaklık ile toplam PAH ve OCP konsantrasyonu arasında negatif, PCB konsantrasyonu arasında ise pozitif zayıf bir korelasyon görülmüştür. PM1.6, PM10, SO2 konsantrasyonu ile incelenen hedef bileşiklerin konsantrasyonları arasında iyi bir korelasyon gözlemlenmemiştir.
In the first phase of the thesis an analytical method was developed in order to determine three groups of priority organic pollutants simultaneously such as polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs) and organochlorine pesticides (OCPs) in atmosphere quantitatively by chromatographic techniques. In the second phase of the thesis, PAHs, PCBs and OCPs were monitored in gas and particle phases of the Konya City Atmosphere. ii In determining particle phase compounds, the best extraction efficiencies were obtained by ultrasonic extraction method using 25 mL of n-hexane/petroleum ether (1/1, v/v) solvent mixture three times for 15 minutes. For determining compounds in gas phase of air samples soxhlet extraction method was carried out for 16 hours with 150 mL diethyl ether/n-hexane (1/9, v/v) solvent mixture. 10 gram 5% deactivated silica gel column was used for cleaning up the interfering substances while simultaneously fractionation of target compounds prior to GC analyses. Elutions of compounds were carried out as follow: Fraction 1: 70 mL n-hexane, Fraction 2: 3 x 20 mL n-hexane/ethyl acetate (1/1, v/v). PAHs and PCBs compounds were determined with GC/MS systems while OCPs compounds were determined using GC/?-ECD system. Surrogate and standard spiked filters were analyzed after optimized method. Recovery were between 86%±2 and 104%±3 for PCBs with Relative Standard Deviation (RSD)< ±4, between 66%±6 and 94%±5 for PAHs with RSD<±8, between 67%±5 and 120%±10 for OCPs with RSD<10. Spiked PUF plugs were also analyzed following the optimized method. Recovery obtained from PUF plugs were between 94%±9 and 118%±8 for PCBs with RSD%±9 while the recovery chanced from 88%±1 to 120%±2 for PAHs with RSD<±8. Recovery of OCPs compounds were between 65%±4 and 108%±6 with RSD<±9. In order to determine the matrix effect on optimized method, air sampled filters and PUF plugs were spiked with standards and surrogate and analyzed according to the optimized method. Recovery of air sampled and spiked filters and PUF plugs were not statistically significantly different from the recoveries of non air sampled spiked filters and PUF plugs at 95% level. Gas phase and particle phase PAHs, PCBs and OCPs contents were analyzed in air samples taken from five different locations selected considering residential, industrial and trafficked areas between August 2006 and May 2007. Meteorological parameters, common air pollutants such as SO2 and particulate matters and seasonal changes of PAHs, PCBs and OCPs were evaluated. Mean PAHs concentrations were between 30 and 214 ng/m3 while mean PCBs and OCPs were between 0,04 and 0,14 ng/m3 and 0,81 and 6,15 ng/m3, respectively. Total concentration ratios found in gas phase were 64-70% for PAHs, 75-90% for PCBs and 45-70% for OCPs. With iii increase in temperature for all compounds concentration ratios in gas phase were increased while concentration ratios in particle phase decreased. There were negative correlation between temperature and PAHs and OCPs while there is a weak positive correlation between PCBs concentration and temperature. There is no good correlation observed between PM1,6, PM10, SO2 and investigated target compounds concentration.
In the first phase of the thesis an analytical method was developed in order to determine three groups of priority organic pollutants simultaneously such as polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs) and organochlorine pesticides (OCPs) in atmosphere quantitatively by chromatographic techniques. In the second phase of the thesis, PAHs, PCBs and OCPs were monitored in gas and particle phases of the Konya City Atmosphere. ii In determining particle phase compounds, the best extraction efficiencies were obtained by ultrasonic extraction method using 25 mL of n-hexane/petroleum ether (1/1, v/v) solvent mixture three times for 15 minutes. For determining compounds in gas phase of air samples soxhlet extraction method was carried out for 16 hours with 150 mL diethyl ether/n-hexane (1/9, v/v) solvent mixture. 10 gram 5% deactivated silica gel column was used for cleaning up the interfering substances while simultaneously fractionation of target compounds prior to GC analyses. Elutions of compounds were carried out as follow: Fraction 1: 70 mL n-hexane, Fraction 2: 3 x 20 mL n-hexane/ethyl acetate (1/1, v/v). PAHs and PCBs compounds were determined with GC/MS systems while OCPs compounds were determined using GC/?-ECD system. Surrogate and standard spiked filters were analyzed after optimized method. Recovery were between 86%±2 and 104%±3 for PCBs with Relative Standard Deviation (RSD)< ±4, between 66%±6 and 94%±5 for PAHs with RSD<±8, between 67%±5 and 120%±10 for OCPs with RSD<10. Spiked PUF plugs were also analyzed following the optimized method. Recovery obtained from PUF plugs were between 94%±9 and 118%±8 for PCBs with RSD%±9 while the recovery chanced from 88%±1 to 120%±2 for PAHs with RSD<±8. Recovery of OCPs compounds were between 65%±4 and 108%±6 with RSD<±9. In order to determine the matrix effect on optimized method, air sampled filters and PUF plugs were spiked with standards and surrogate and analyzed according to the optimized method. Recovery of air sampled and spiked filters and PUF plugs were not statistically significantly different from the recoveries of non air sampled spiked filters and PUF plugs at 95% level. Gas phase and particle phase PAHs, PCBs and OCPs contents were analyzed in air samples taken from five different locations selected considering residential, industrial and trafficked areas between August 2006 and May 2007. Meteorological parameters, common air pollutants such as SO2 and particulate matters and seasonal changes of PAHs, PCBs and OCPs were evaluated. Mean PAHs concentrations were between 30 and 214 ng/m3 while mean PCBs and OCPs were between 0,04 and 0,14 ng/m3 and 0,81 and 6,15 ng/m3, respectively. Total concentration ratios found in gas phase were 64-70% for PAHs, 75-90% for PCBs and 45-70% for OCPs. With iii increase in temperature for all compounds concentration ratios in gas phase were increased while concentration ratios in particle phase decreased. There were negative correlation between temperature and PAHs and OCPs while there is a weak positive correlation between PCBs concentration and temperature. There is no good correlation observed between PM1,6, PM10, SO2 and investigated target compounds concentration.
Açıklama
Anahtar Kelimeler
Hava kirliliği, Poliaromatik hidrokarbonlar, Poliklorlu bifeniller, Organoklorlu pestisitler, Metot optimizasyonu, Gaz kromatografi, Air pollution, Polycyclic aromatic hydrocarbon, Polychlorinated biphenyl, Organochlorine pesticides, Method optimization, Gas chromatography
Kaynak
WoS Q Değeri
Scopus Q Değeri
Cilt
Sayı
Künye
Özcan, S. (2007). Hava ortamında öncelikli organik kirleticilerin tayini için analitik metot optimizasyonu ve Konya kent atmosferinde izlenmesi. Selçuk Üniversitesi, Yayımlanmış doktora tezi, Konya.
