Polimerik malzemelerde kullanılan bazı katkı maddeleri ve metabolitlerinin tespitinde spektroskopik ve kromatografik yöntemlerin geliştirilmesi
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Date
2015
Authors
Kayar, Murat
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Publisher
Uludağ Üniversitesi
Abstract
Katı ve sıvı örneklerde majör, minör ve iz elementlerin ve aynı zamanda izotop oranlarının belirlenmesinde LA- ICP-MS (Lazer Ablasyon Indüktif Eşleşmiş Plazma Kütle Spektrometresi) tekniğinin kullanımı son yıllarda oldukça gelişmiştir. Şimdilerde esas olarak farklı dalga boylarında UV lazer ışığı ile çalışan bu sistem , inorganik eser element analizi alanında mevcut olan çok yönlü mikro analitik tekniklerden biridir. Bir numune hazırlama ve örnekleme tekniği olarak lazer ablasyon kullanımının çeşitli avantajları vardır: Hemen hemen hiçbir örnek hazırlama aşaması içermez, çözücüler ve asitlerden gelen kontaminasyon ve girişimlerden uzaktır düşük çözünürlüğe sahiptir (1-2 µm), element ve izotopik bilgilere ulaşmaya olanak verir, gözlenebilme sınırı diğer katı örnekleme tekniklerine göre üstündür, veri toplama hızı, yüksek sayıda örneklerin makul süreler içerisinde analiz edilmesine olanak verir. Lazer ablasyonun birçok avantajı olmasına rağmen, en büyük dezavantajı nicel analizdir. LA-ICP - MS ile nicel analiz birçok örnek türleri için zordur . Bu zorluk numune ile hem kimyasal hem de fiziksel olarak uygun olan standart eksikliğini yansıtmaktadır . Bu teknikte doğru sonuçlar genellikle numune ve standardın aynı matrise sahip olduğu durumda elde edilir. Numuneler ve standartların matriks uyumunun sağlanması için çeşitli stratejiler geliştirilmiştir. Bunlar arasında en sık kullanılan kalibrasyon standardı NIST referans camı olmuştur. Bu çalışmada kalibrasyon standardı olarak, eritiş disk tekniğini kullanılmış , polimerlerde brom ve kalay tespiti için kalibrasyon standartları hazırlanmıştır. Ayrıca laboratuvar ortamında hazırlanan standartların homojenliği kontrol edilmiş, lazer enerjisi, lazer frekansı, tarama hızı,spot büyüklüğü, taşıyıcı gaz hızı gibi önemli lazer parametreleri optimize edilmiştir. Daha sonra brom ve kalay için kalibrasyon eğrileri hazırlanmış, doğrusallığı kontrol edilmiş ve ayrıca metodun doğruluğu da değerlendirilmiştir. Elde edilen sonuçlar, bu tekniğin plastik malzemelerde özellikle Avrupa Birliği tarafından kullanımı kısıtlanmış polibromlu alev geciktiriciler ve organo kalay bileşiklerinin taranması için oldukça uygun olduğunu göstermiştir. Bunun yanında, lazer parametrelerinin amaca uygun optimizasyonu ile LA-ICP-MS metodu yine plastiklerde bulunması istenmeyen agır metallerin (Cr, Cd, Pb ve Hg) eş zamanlı tespitine de olanak vermekte ve ayrıca LA cihazının bir ekstraksiyon ekipmanı gibi kullanılarak, plastik malzemelerde bulunan katkı maddelerinin GC –MS cihazı ile taranmasına imkan vermektedir.
The using of laser ablation in combination with ICP–MS for the determination of major, minor and trace elements as well as isotopic ratios in solids and liquids has grown over the past decade. This sample introduction system, now mainly operating with UV laser light at different wavelengths, is one of the most versatile micro-analytical techniques currently available in the field of inorganic trace element analysis. There are several advantages using laser ablation as a sampling technique: Almost no sample preparation and no contamination from solvents and acids, less interferences due to the absence of solvents and acids, spatial resolution to as low as few µm (1-2 µm) are possible, elemental and isotopic information are obtainable, limits of detection are superior to other solid sampling techniques and the speed of data acquisition allows large quantities of samples to be analyzed within reasonable time. Although laser ablation has many advantages, the bigest disadvantages of this technique is quantitative analysis. Quantitative analysis by laser ablation ICP-MS is difficult to achieve for many sample types. This reflects a lack of suitable standards which ideally, though unobtainably, need to be identical to the sample both chemically and physically on all relevant spatial scales. Accurate results are generally obtained only when the sample and the standard are prepared in the same matrix. Various strategies have been investigated in order to obtain matches between samples and standards. However, still the most commonly used calibration standards are the NIST reference glasses. In this study, we use fusion disc technique for preparation of standarts for the determination of bromine and tin in polymers for the next studies. In this study,fusion discs were used as calibration standarts which are prepared in laboratory, then the homogenity was checked and some important laser parameters; laser energy, laser frequency, scan rate, carier gas flow and aperture size were optimized. By using optimized parameters calibration curves were prepared for bromine and tin, and checked by linearity evaluation software and also evaluation of the truness of this standart preparation and calibration technique. The results obtained have shown that this technique can be used for screening of plastics materials ın terms of polybrominated flame retardants and organotin compounds which are under regulation by most of the countries especially in EU countries. Besides the LA-ICP-MS method can be used for heavy metals (Cr,Cd, Pb and Hg) analysis in platics with optimization of some laser parameters and also using LA as an extraction technique some plastic additives can be screened by GC-MS.
The using of laser ablation in combination with ICP–MS for the determination of major, minor and trace elements as well as isotopic ratios in solids and liquids has grown over the past decade. This sample introduction system, now mainly operating with UV laser light at different wavelengths, is one of the most versatile micro-analytical techniques currently available in the field of inorganic trace element analysis. There are several advantages using laser ablation as a sampling technique: Almost no sample preparation and no contamination from solvents and acids, less interferences due to the absence of solvents and acids, spatial resolution to as low as few µm (1-2 µm) are possible, elemental and isotopic information are obtainable, limits of detection are superior to other solid sampling techniques and the speed of data acquisition allows large quantities of samples to be analyzed within reasonable time. Although laser ablation has many advantages, the bigest disadvantages of this technique is quantitative analysis. Quantitative analysis by laser ablation ICP-MS is difficult to achieve for many sample types. This reflects a lack of suitable standards which ideally, though unobtainably, need to be identical to the sample both chemically and physically on all relevant spatial scales. Accurate results are generally obtained only when the sample and the standard are prepared in the same matrix. Various strategies have been investigated in order to obtain matches between samples and standards. However, still the most commonly used calibration standards are the NIST reference glasses. In this study, we use fusion disc technique for preparation of standarts for the determination of bromine and tin in polymers for the next studies. In this study,fusion discs were used as calibration standarts which are prepared in laboratory, then the homogenity was checked and some important laser parameters; laser energy, laser frequency, scan rate, carier gas flow and aperture size were optimized. By using optimized parameters calibration curves were prepared for bromine and tin, and checked by linearity evaluation software and also evaluation of the truness of this standart preparation and calibration technique. The results obtained have shown that this technique can be used for screening of plastics materials ın terms of polybrominated flame retardants and organotin compounds which are under regulation by most of the countries especially in EU countries. Besides the LA-ICP-MS method can be used for heavy metals (Cr,Cd, Pb and Hg) analysis in platics with optimization of some laser parameters and also using LA as an extraction technique some plastic additives can be screened by GC-MS.
Description
Keywords
Plastikler, Laser ablation indüktif eşleşmiş plazma kütle spektroskopisi, Polibromlu difenil eterler, Organokalay bileşikleri, Ağır metaller, Plastics, Laser ablation inductively coupled mass spectrometry, Polybrominated diphenyl ethers, Organo-tin compounds, Heavy metals
Citation
Kayar, M. (2015). Polimerik malzemelerde kullanılan bazı katkı maddeleri ve metabolitlerinin tespitinde spektroskopik ve kromatografik yöntemlerin geliştirilmesi. Yayınlanmamış doktora tezi. Uludağ Üniversitesi Fen Bilimleri Enstitüsü.