Spelling suggestions: "subject:"[een] SOLID-PHASE EXTRACTION"" "subject:"[enn] SOLID-PHASE EXTRACTION""
41 |
Development and validation of sample clean-up using solid phase extraction prior oil spill fingerprintingLoorents, Cheryl January 2022 (has links)
In a forensic investigation involving oil, a comparative analysis named oil spill fingerprinting between a source and an oil spill is normally performed. It is based on detecting a certain selection of biomarkers with gas chromatography (GC) coupled to mass spectrometry (MS) which are later divided into diagnostic ratios (DRs). An international guideline formed by European Committee for Standardization (CEN) denoted CEN/TR 15522-2:2012 describes the process of conducting oil spill fingerprinting. This method is currently being inspected and adjusted for standardization into EN 15522-2:2022. One section of the upcoming standard describes sample clean-up which is important to inhibit possible matrix effect that could either enhance or reduce peak intensity in the chromatogram. There is yet no conclusive SPE (Solid Phase Extraction) protocol in the current draft version of EN 15522-2:2022. The aim with this study was to develop such a protocol. Development included comparative testing of the recommended stationary phases silica and Florisil®. Additionally, the effect of both elution solvent and elution volume were investigated. The protocol must pass validation criteria to be implemented at National Forensic Centre (NFC) and possibly be used in the final version of EN 15522-2:2022. A successful method for Heavy Fuel Oil (HFO), diesel and lubricating oil was achieved with activated Florisil® as stationary phase, eluted with 6 ml dichloromethane (DCM). If the evidence material is suspected to contain FAMEs (Fatty Acid Methyl Esters), then 2 % acetone should be added to the DCM. The final SPE column was packed with 0.5 glass wool, 4 cm Florisil® and 0.5 cm sodium sulfate. Based on successful validation result, the SPE protocol should be considered for the final version of EN 15522-2:2022 as well as for implementation at NFC.
|
42 |
Stability Study of Wastewater During Storage at Three Different Temperatures Over a Three-Day PeriodKaskel, Parker 24 May 2022 (has links)
No description available.
|
43 |
Optimization of a Method for the Extraction of Drugs of Abuse from WastewaterMartin, Danica Paige 24 May 2021 (has links)
No description available.
|
44 |
Utilization of Carbon Dioxide in Separation Science: Fabrication of a Solid Phase Extraction Sorbent and Investigation of the Greenness of Supercritical Fluid ChromatographyGIbson, Rebekah January 2021 (has links)
No description available.
|
45 |
Functionalization, Characterization, and Applications of Diamond Particles, Modification of Planar Silicon, and Chemoetrics Analysis of MS DataYang, Li 20 March 2009 (has links) (PDF)
In spite of the stablility (lack of reactivity) of diamond powder, I have developed a method for tethering alkyl chains and polymers to deuterium/hydrogen-terminated diamond. One method is through ether linkages via thermolysis of di-tert-amyl peroxide (DTAP). This reaction with DTAP has also been applied to grow polymers on the diamond surface. The other method is atom transfer radical polymerization (ATRP), which was applied to grow polystyrene at the surface of diamond. Both polystyrene-modified diamond and sulfonated polystyrene-modified diamond can be prepared by either method, and can be used for solid phase extraction. Diamond stationary phases are stable under basic conditions, which is not the case for silica-based stationary phases. Surface characterization was performed by X-ray photoelectron spectroscopy (XPS), time-of-flight secondary ion mass spectrometry (ToF-SIMS) and diffuse reflectance Fourier transform infrared spectroscopy (DRIFT). While the main focus of my graduate research has been the surface modification of diamond, I also describe other projects on which I have worked. The use of radical-based processes for modifying diamond is related to a different radical-based synthesis of monolayers or polymers I performed by scribing silicon (Siscr). After preparation of homogeneous olefin-terminated monolayers on scribed silicon made from 1,9-decadiene and chemisorption of Grubbs' catalyst, ring-opening metathesis polymerization (ROMP) of norbornene was demonstrated. These surfaces were characterized by XPS and ToF-SIMS. I also investigated the extent of PDMS oligomers transfer onto different surfaces with a wide range of hydrophobicities, using an uninked, unpatterned PDMS stamp. The effect of surface free energy on PDMS transfer in microcontact printing was investigated and the relationship between the amount of PDMS in ToF-SIMS spectra and the surface tensions of initial surfaces was revealed. Therefore, PDMS transfer can be applied as a probe of surface free energies using ToF-SIMS, where PDMS preferentially transfers onto more hydrophilic surface features during stamping, with little transfer onto very hydrophobic surface features. In much of my thesis work, I performed multivariate analysis of my data, especially of my ToF-SIMS data. Such chemometrics methods include principle components analysis (PCA), partial least squares (PLS) cluster analysis, and multivariate curve resolution (MCR). I also applied these tools to analyze electrospray ionization (ESI) mass spectrometry data from a lipidomics study.
|
46 |
Comparison of the Recovery of Drugs in Oral Fluid Using Biotage Evolute Express Solid Phase Extraction Columns with Active and Passive SolutionsMcGuire, Annamarie 30 August 2022 (has links)
No description available.
|
47 |
Analytical Method For Detecting Pcb Derivatives At Low Levels In Surface Water Samples By Solid Phase Extraction-Liquid Chromatography/Mass SpectrometryAlford, Shannon Recca 07 May 2005 (has links)
Polychlorinated biphenyls (PCBs) and their metabolic derivatives are ubiquitous environmental contaminants. These compounds are of concern because of their persistence and bioaccumulation in nature. PCBs and the hydroxylated metabolites have shown endocrine-disrupting activity. A method of detection in surface water samples is important to identify and quantify the environmental contamination. In this research we have attempted to develop a method of detection. Six representative polychloromethoxybiphenyls (PCMBs) were prepared. The corresponding polychlorobiphenylols, hydroxylated PCB metabolites (OH-PCBs), were prepared from the PCMBs. A method coupling solid phase extraction with liquid chromatography, on-line electrospray ionization, and mass spectrometry (SPE-LC/ESI/MS) was developed for detection of the OH-PCBs in distilled and surface water samples.
|
48 |
Aplicação de campos elétricos em procedimentos de extração em fase sólida. / Application of electric fields in solid phase extraction proceduresOrlando, Ricardo Mathias 06 March 2011 (has links)
Orientadores: Susanne Rath, Jarbas José Rodrigues Rohwedder / Tese (doutorado) - Universidade Estadual de Campinas, Instituto de Química / Made available in DSpace on 2018-08-19T11:12:21Z (GMT). No. of bitstreams: 1
Orlando_RicardoMathias_D.pdf: 5151319 bytes, checksum: 53a60cd9c94d86b8a9e269a87ef0c9ac (MD5)
Previous issue date: 2011 / Resumo: O preparo de amostra representa uma etapa determinante e crítica no processo de análise e a extração em fase sólida (SPE) é uma técnica amplamente empregada no preparo de matrizes complexas. O objetivo deste trabalho foi o desenvolvimento de dispositivos e procedimentos que permitem aplicar campos elétricos em SPE empregando cartuchos (E-SPE®), visando adicionar os mecanismos da eletroforese ao processo cromatográfico. Para tanto, foram desenvolvidos eletrodos e cartuchos que possibilitam a aplicação de campos elétricos, além de um sistema para monitorar e controlar parâmetros eletrocromatográficos tais como: vazão, corrente elétrica, potencial elétrico e temperatura. Com esses dispositivos foram realizadas extrações com aplicação de campo elétrico empregando compostos modelo aniônicos, catiônicos e anfotéricos. Para permitir uma melhor compreensão dos fenômenos envolvidos foram avaliados diversos parâmetros de extração, entre esses: concentração de íons em solução, pH, modificador orgânico, volume de solução de lavagem e tipo de sorvente. O sistema foi avaliado também na determinação de antimicrobianos em leite. Dependendo da polaridade empregada sobre os eletrodos, a aplicação do campo elétrico foi capaz de modular (acelerar ou retardar) a saída dos compostos modelo do cartucho. Os resultados de extração obtidos demonstraram a eficácia dos dispositivos desenvolvidos, além da grande potencialidade do uso de campos elétricos em SPE para obter maiores recuperações dos analitos de interesse e/ou remoção de interferentes / Abstract: Sample preparation is a crucial and determinant step for the analysis process and solid phase extraction (SPE) is a widely used technique in the preparation of complex matrices. The aim of this work was the development of devices and procedures for applying electric fields to SPE cartridges (SPE-E ®), in order to add the mechanisms of electrophoresis to the chromatographic process. For this purpose, electrodes and cartridges that allow the application of electric fields were developed, besides a system to monitor and control electrochromatographic parameters such as: flow, electric current, electric potential and temperature. By means of these devices, extractions with application of electric fields were performed using anionic, cationic and amphoteric model compounds. In order to allow a better understanding of the phenomena involved several extraction parameters were evaluated, among these: the concentration of ions in solution, pH, organic modifier, volume of washing solution and type of sorbent. The system was also evaluated for the determination of antibiotics in milk. Depending on the polarity of the electrodes used, the application of an electric field was able to modulate (accelerate or retard) the output of the model compounds from the cartridge. The extraction results obtained showed the effectiveness of the devices developed, and the immense potential of the use of electric fields in SPE to obtain better recoveries of the analytes and/or for removing interferents / Doutorado / Quimica Analitica / Doutor em Ciências
|
49 |
Vývoj a optimalizace SPE metody pro prekoncentraci a stanovení fluorotelomerních alkoholů ve vodách / Development and optimization of SPE method for preconcentration and determination of fluorotelomeric alcohols in waterŠevčík, Václav January 2012 (has links)
New GC-MS method combined with SPE preconcentration step has been developed and optimized for the determination of selected fluorotelomer alcohols in aqueous samples by advanced statistical method in this thesis. 1H,1H,2H,2H-perfluoro-1-octanol (6:2 FTOH) and 1H,1H,2H,2H-perfluoro-1-decanol (8:2 FTOH) have been selected as the analytes. The influence of several factors, such as the sample volume, the carrier gas pressure, the sampling time and the injector temperature on the system response have been studied during the optimization. Utilizing the statistical software Minitab 16 and series of experiments, the optimal values of relevant factors and a suitable type of ionization were found for both analytes. Limits of detection of GC-MS method are 0.24 ng/mL for 6:2 FTOH and 0.42 ng/mL for 8:2 FTOH. Several factors, such as the type and the volume of conditioning agent, the speed of conditioning, the speed of sample flow, the method of column drying, the type and the volume of eluent have been tested for SPE. The optima of these factors were determined using Minitab 16 software. The extraction efficiency dependence on the concentration and volume of the stock solution was used to set the limitation of SPE for the determination of fluorotelomer alcohols. The maximum volume of sample equals to 400 mL...
|
50 |
Method development and Validation for the determination of selected Polycyclic Aromatic Hydrocarbons (PAHs) in water by Solid Phase Extraction and High Performance Liquid ChromatographyXoliswa, Madlanga 12 February 2014 (has links)
Polycyclic Aromatic Hydrocarbons (PAHs) are one of the pollutants in the environment. They are organic compounds that consist of more than one aromatic ring (Kanchanamayoon & Tatrahun 2008). Due to less information forthcoming regarding the levels of PAHs in Vaal area, this study is to evaluate the levels of PAHs in the rivers around Vaal Triangle. Three river sites such as Vaal, Barrage and Klip Rivers were selected to investigate the concentration of polycyclic aromatic hydrocarbons in water. Validation of an analytical method is the process by which it is established by laboratory studies, that the performance characteristics of the method meet the requirements for the intended analytical application. (Stockl et al 2009). The validation parameters tested were, linearity detection limit of quantitation, sensitivity, accuracy, specificity, selectivity, robustness and ruggedness.
PAHs can be determined using High Performance Liquid Chromatography (HPLC) which is a technique for separation, identification and quantification of components in a mixture. The following ten compounds were identified and quantified with a HPLC: naphthalene, acenaphthylene, phenanthrene, anthracene, fluoranthene, benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(a)pyrene, dibenzo(a,h) anthracene and indeno(1,2,3-cd)pyrene. The linear calibration ranges from 0.1-5ppm.The linearity ranges between 0.9993-0.9999.Three reversed sorbent phases (Strata-X, MFC18 and C18) were tested for PAH retention efficiency. An optimised reverse solid phase extraction (SPE) method was used after conditioning the sorbent to extract and collect compounds of polycyclic aromatic hydrocarbons (PAHs) in river water samples. LC18 sorbent showed good recoveries after extracting PAHs standard mixture of 1 mg/l. The best performing eluting solvent was acetonitrile and very good percentage recoveries that ranged from 70% to over 100 % were obtained for eight compounds. Poor recoveries were also obtained for phenanthrene (61%) and benzo(b)fluoranthene (48%). The standard deviation ranged from 0.01 to 0.05 and the detection limits ranging from 0.01 – 0.17 mg/l were obtained. Average concentration ranges of PAHs identified within the study area were: phenanthrene (0.02 – 0.42 mg/l); anthracene (0.37 – 0.39 mg/l), fluoranthene (0.11 – 0.15 mg/l); benzo(b)fluoranthene (0.09 mg/l) and indeno(1,2,3-cd)pyrene (0.26 mg/l). However, naphthalene, acenaphthylene, benzo(k)fluoranthene, benzo(a)pyrene and dibenzo(a,h)anthracene were not detected.
|
Page generated in 0.2706 seconds