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

Yıl 2018, Cilt: 39 Sayı: 4, 970 - 982, 24.12.2018

Barış Güzel Oltan Canlı Elmas Öktem Olgun

https://doi.org/10.17776/csj.439764

Cited By: 6

Öz

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.

Anahtar Kelimeler

Gaz kromatografi, tasfiye & tutma, kantitatif analiz, uçucu aromatik hidrokarbon, su

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

Öz

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.

Anahtar Kelimeler

Gas chromatography, purge & trap, quantitative analysis, volatile aromatic hydrocarbon, water

Kaynakça

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