Elmas ÖKTEM OLGUN, Oltan CANLI, Barış GÜZEL

Suda Uçucu Aromatik Hidrokarbonların (UAH’lar) Hassas ve Doğru Analizi için Gaz Kromatografisi Yöntemi Doğrulama Çalışması

Endüstriyel faaliyetlerin sonucunda çok çeşitli kimyasallar ortaya çıkmaktadır. Bunlar, insan sağlığı ve su ortamı üzerinde oldukça toksik ve kanserojenik etkilere sahip olabilirler. Bu nedenle, ulusal ve uluslararası listelerde yasaklanmış kimyasallar olarak yer alan bu maddeler, hem su kaynakları hem de potansiyel alıcı su ortamlarında çevre ve insan sağlığı açısından sürekli olarak izlenmelidir. Bu çalışmanın amacı, farklı su örneklerinde tasfiye & tutma (PT) işlemi ile gaz kromatografisi - kütle spektrometresi (GC-MS) kullanılarak benzen, toluen, ksilenler, stiren ve klorobenzenler gibi oldukça tehlikeli maddeler içeren bazı uçucu aromatik hidrokarbonların (UAH’lar) hassas ve doğru tespitine yönelik yöntemi sunmaktır. Önerilen metot, seçicilik, doğrusallık, tespit ve tayin limitleri (LOD ve LOQ), metot ve cihazın kesinlik çalışmaları ile doğrulanmıştır. Çalışmada incelenen tüm analitler, PT-GC-MS için maksimum performans sınırları içinde güvenilir şekilde ölçülmüştür. Seçicilik çalışması, altı boş su örneğinin çift analizi ile gerçekleştirilmiştir. Su örneklerindeki analitlerin alıkonma süreleri arasında herhangi bir bulgu veya gözleme rastlanmamıştır. Kalibrasyon eğrilerinin doğrusallığı, dokuz konsantrasyon seviyesinde hazırlanan standart çözeltilerin analizi ile çizilmiştir. Çalışma aralığındaki analitik tepki doğrusallığı, tüm analitlerin korelasyon katsayıları 0,9996 'dan büyük olduğu için mükemmel olarak değerlendirilebilir. Metot doğruluğu, geri kazanım deneyi yapılarak gerçekleştirilmiştir. Analitlerin geri kazanımları % 88,4 ile % 94,6 arasında değişmektedir ve bağıl standart sapma (RSD) sonuçları % 3,52 ile % 6,35 arasında bulunmuştur. Geliştirilen metodun uygulanabilirliği, su örneklerinde ilgili analitlerin tespiti ile doğrulanmıştır.

Gas Chromatography Method Validation Study for Sensitive and Accurate Determination of Volatile Aromatic Hydrocarbons (VAHs) in Water

A wide range of chemicals comes to exist at the end of the industrial activities. They could have highly toxic and carcinogenic effects on the human health and water environment. Therefore, these substances, which are listed as prohibited chemicals on national and international lists, must be monitored permanently with regards to environmental and human health both in the water resources and potential receiving waterbodies. The objective of this study was to present the method for the sensitive and accurate determination of some volatile aromatic hydrocarbons (VAHs), including quite dangerous substances such as benzene, toluene, xylenes, styrene and chlorobenzenes by using gas chromatography - mass spectrometry (GC-MS) with purge & trap (PT) process in different water samples. The proposed method was verified with the selectivity, linearity, limits of detection and quantification (LOD and LOQ), precision studies of the method and instrument. All analytes examined in the study were trustworthily measured within the maximum performance limits for PT-GC-MS. The selectivity work was carried out by duplicate analysis of six blank water samples. There is no finding or observation within the interval of the retention time of the analytes in the water samples. The linearity of calibration curves was drawn by analysis of prepared standard solutions at nine concentration levels. The analytical response linearity in the working range can be assessed as an excellent since the correlation coefficients higher than 0.9996 for all analytes. The method accuracy was carried out by doing recovery experiment. Recoveries of analytes have been changed from 88.4 % to 94.6 % and the relative standard deviation (RSD) results were found between 3.52 % and 6.35 %. The applicability of developed method was confirmed by the determination of related analytes in the water samples.

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