Tekstil boyası parçalanma ürünlerinin kromatografik tekniklerle belirlenmesi
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Date
2005-01-11
Authors
Bilgi, Saliha
Journal Title
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Publisher
Bursa Uludağ Üniversitesi
Abstract
Son yıllarda azo boyarmaddelerinin tekstil endüstrisinde kullanımı artmaktadır. Yapılan çalışmalarda azo boyarmaddeleri ve parçalanma ürünlerinin kanserojenik ve mutajenik özellikleri olduğu ve ekolojik sistem için tehdit oluşturduğu belirlenmiştir. Bu yüzden boyama sonrası atık suda kalan boyarmadde miktarı ve varsa parçalanma ürünleri belirlenmelidir. Bu amaçla ilk olarak C.I. Reactive Orange 16 boyarmaddesi belli sürelerle UV ışığı ile fotookside edilerek oluşan parçalanma ürünleri araştırılmıştır. Bu çalışmada fotooksidasyon süresine bağlı olarak absorbans değişimleri UV-VIS spektrofotometresi ile, bağıl yoğunluk değişimleri de GC-MS ile takip edilmiştir. Boyarmaddenin parçalanma hızı ile ilgili kinetik çalışmalar yapılmıştır. Boyarmaddenin 1 00. dk içinde tamamen renginin giderildiği gözlemlenmiştir. Oluşan parçalanma ürünleri GC-MS ile belirlenmiştir. Bu parçalanma ürünleri 6-asetilamino-3-amino -naftalen-2-sülfonik asit, N-(3,4-Bis-hidroksimetil-fenil)-asetamit and ftalik asittir. C.I. Reactive Orange 16 boyarmaddesinin fotookside edilerek oluşan parçalanma ürünleri için uygun mekanizma önerilmiştir. İkinci olarak reaktif ve dispers boyarmaddelerden oluşan 10 adet azo sınıfı boyarmadde ile boyama yapılarak atık suda kalan boyarmadde miktarları HPLC-DAD yöntemiyle belirlenmiştir. Boyama sonrası kumaşlı atık suda bulunan boyarmadde miktarları dispers boyarmaddeler için 0,028-11,374 mg/L arasında iken reaktif boyarmaddeler için 4982,401-10283,710 mg/L arasında bulunmuştur. Katı faz ekstraksiyon geri kazanım değerleri ise % 39,86-84,37 arasındadır. Boyama sonrası oluşan atık suların kimyasal oksijen ihtiyacı ve toplam organik karbon ölçümleri de yapılmıştır. Karışım halindeki atık suda düşük seviyelerde bulunan dispers boyarmaddelerin üst üste çakışan absorbans örtüşmeleri olduğu için spektrofotometrik olarak ayrılamamaktadırlar. Bu örtüşmeleri dikkate alarak çok değişkenli kalibrasyon metotlarından PLS ve PCR ile karışımda bulunan dispers boyarmadde miktarları tayin edilmiştir.
The photodegradation of aqueous solutions of C.I. Reactive Orange 16 was investigated under UV irradiation. The degradation was studied by monitoring the change in absorption and relative intensity employing UV-spectroscopic and GC-MS analysis as functions of irradiation time. The rate of degradation of the dye was evaluated. The solution was completely decolorized after 100 min of photooxidation. The generated degradation products were detected by GC-MS. 6-acetylamino-3 -amino - naphthalene-2-sulfonic acid, N-(3,4-Bis-hydroxymethyl-phenyl)-acetamide and phthalic acid were found during the degradation of C.I. Reactive Orange 16. The probable pathways for the formation of the degradation products were proposed. GC-MS analysis and degradation pathways demonstrated that naphthalene and benzene rings were observed during photooxidation. The concentrations of azo dyes in wastewater samples with fabric after dyeing process were found between 0,028 mg/L and 11,734 mg/L for disperse dyes and between 4982,401 and 10283,710 mg/L for reactive dyes. The SPE recoveries were varied from 39,86 to 84,37 %. The levels of COD and TOC in wastewater with fabric were lower than the wastewater for dyeing without fabric and synthetic wastewater. It was observed that TOC and COD levels of wastewater for dyeing without fabric were lower than synthetic wastewater. It shows that the reactions depend on operation conditions such as temperature, time, etc. in dyeing process. The concentrations of dyes in wastewater after dyeing process are at low level. PCR and PLS calibration techniques are necessary in order to determine at low level and overlapped spectra. Multi level calibration design was used to model the calibration. RMSEs were evaluated to see how the calibration model is fitted to the concentration of each dye.
The photodegradation of aqueous solutions of C.I. Reactive Orange 16 was investigated under UV irradiation. The degradation was studied by monitoring the change in absorption and relative intensity employing UV-spectroscopic and GC-MS analysis as functions of irradiation time. The rate of degradation of the dye was evaluated. The solution was completely decolorized after 100 min of photooxidation. The generated degradation products were detected by GC-MS. 6-acetylamino-3 -amino - naphthalene-2-sulfonic acid, N-(3,4-Bis-hydroxymethyl-phenyl)-acetamide and phthalic acid were found during the degradation of C.I. Reactive Orange 16. The probable pathways for the formation of the degradation products were proposed. GC-MS analysis and degradation pathways demonstrated that naphthalene and benzene rings were observed during photooxidation. The concentrations of azo dyes in wastewater samples with fabric after dyeing process were found between 0,028 mg/L and 11,734 mg/L for disperse dyes and between 4982,401 and 10283,710 mg/L for reactive dyes. The SPE recoveries were varied from 39,86 to 84,37 %. The levels of COD and TOC in wastewater with fabric were lower than the wastewater for dyeing without fabric and synthetic wastewater. It was observed that TOC and COD levels of wastewater for dyeing without fabric were lower than synthetic wastewater. It shows that the reactions depend on operation conditions such as temperature, time, etc. in dyeing process. The concentrations of dyes in wastewater after dyeing process are at low level. PCR and PLS calibration techniques are necessary in order to determine at low level and overlapped spectra. Multi level calibration design was used to model the calibration. RMSEs were evaluated to see how the calibration model is fitted to the concentration of each dye.
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Keywords
Tekstil atik suyu, Azo boyarmaddeler, Fotooksidasyon, Parçalanma ürünleri, GC-MS, UV-VIS, HPLC-DAD, PLS, PCR, Textile wastewater, Photooxidation, Degradation products
Citation
Bilgi, S. (2005). Tekstil boyası parçalanma ürünlerinin kromatografik tekniklerle belirlenmesi. Yayınlanmamış yüksek lisans tezi. Bursa Uludağ Üniversitesi Fen Bilimleri Enstitüsü.