The characterization of all components of pharmaceutical preparations, especially in the analysis of impurities present at levels higher than 0.05% of the main component, is a challenge in the pharmaceutical industry because no single detector can detect all impurities present. All commercial detection methods suffer from certain disadvantages. Universal sensitive detection with a wide dynamic range is strongly demanded. This results in an increasing interest in the development of universal sensitive detection methods for the pharmaceutical industry, which was the goal of this project. In this project, universal detection of analytes by HPLC-FID coupling was explored. Due to the large volume of the vapours of the mobile phase in HPLC, flame-based detection systems are prone to flame instability. To overcome this problem, a series of improvements were evaluated: 1) a fraction of the total volume of the effluent was delivered to the flame of the FID in a split mode; 2) a tubular oven was used before the FID to preheat the effluent and remove a large fraction of the mobile phase before the detector; 3) oxygen gas and a modified FID with an elongated burner were used to improve the performance of the FID. Finally, optimization of the FID design and parameters was performed by running a series of tests in flow injection mode using simplex optimization method.

The characterization of all components of pharmaceutical preparations, especially in the analysis of impurities present at levels higher than 0.05% of the main component, is a challenge in the pharmaceutical industry because no single detector can detect all impurities present. All commercial detection methods suffer from certain disadvantages. Universal sensitive detection with a wide dynamic range is strongly demanded. This results in an increasing interest in the development of universal sensitive detection methods for the pharmaceutical industry, which was the goal of this project. In this project, universal detection of analytes by HPLC-FID coupling was explored. Due to the large volume of the vapours of the mobile phase in HPLC, flame-based detection systems are prone to flame instability. To overcome this problem, a series of improvements were evaluated: 1) a fraction of the total volume of the effluent was delivered to the flame of the FID in a split mode; 2) a tubular oven was used before the FID to preheat the effluent and remove a large fraction of the mobile phase before the detector; 3) oxygen gas and a modified FID with an elongated burner were used to improve the performance of the FID. Finally, optimization of the FID design and parameters was performed by running a series of tests in flow injection mode using simplex optimization method.

ABSTRACT A new, non-pathogenic bioaugmentation product was formulated specifically for underground use in South African mines, using local bacterial isolates. This was designed for the remediation of various hydrocarbons via biochemical breakdown by sub-surface microorganisms. The active microorganisms were isolated from hydrocarbon-polluted areas of a gold mine. Many commercially available bioaugmentation products are already in existence however, all, to our knowledge, have been developed and tested primarily for use in the northern hemisphere. None have been formulated and tested in Africa. Our series of bacterial isolates are the first to be isolated from mine soils for hydrocarbon biodegradation purposes. Such isolates have further, not previously been tested on sub-surface contamination. The safety associated with the use of such a product in a closed mine-environment is of paramount importance. Initial batch-flask experiments were conducted using a readily-available commercial bioremediation product. This was tested on simple surfactant molecules and compared to the biodegradation observed under standard waste water treatment plant conditions. The bioremediation product increased biodegradation by 6% on average. Bacteria in the product were identified by 16S rDNA gene sequence analysis and found to be homologous to potentially pathogenic Bacillus cereus, known especially to effect immunocompromised individuals, this was of particular concern in the closed mine system. South African isolates were sourced from various hydrocarbon-polluted sources, with six bacteria ultimately being selected from deep sub-surface mine soil and water samples. The ability of these isolates to biodegrade waterborne monograde engine oil was assessed via GC-FID. The isolate showing average percentage growth increase, homologous to Pseudomonas pseudoalcaligenes, was found to degrade the motor oil by 98%. The new isolates were, on average, 16% more efficient at biodegrading petroleum hydrocarbons than the commercial bioremediation product isolates. Formulation of these isolates into the first commercially-available South African developed and tested bioaugmentation product will prove a successful conclusion to this study.

The international harbors and fishing ports in Taiwan are nearly not installed the wastewater or oil treatment facilities, which would cause the ocean pollution by the ballast and bilge water from the boats. The purpose of this research is to study the feasibility of treatment of diesel fuel and the polycyclic aromatic hydrocarbons (PAHs) in diesel by aerobic biofiltreation in salty environment. According to the experimental results, the mineral oil and PAHs in the diesel fuel present high good removal efficiencies. Both of the contaminants were decomposed fast at the first 8 hours, and then slow down. The emulsified diesel fuel were found able to be reduced 83% within 8 hours, and the concentrations of phenanthrene would found decreased from 1.5 to 0.1 mg/L. After 8 hours, we observed that the PAHs with high number of rings kept a mild diminish trend, while the PAHs with less rings exhibited arrearage and irregular indicated by some peaks appearing in the chromatography diagram of HPLC, which were not found in the diagram in the initial of test run. In conclusion, the aerobic biofiltreation systems were found able to degrade n-alkanes and PAHs in diesel fuel effectively. Thus we suggested to install the systems at the greasiness accepting facilities in the harbor. However, we still have to keep studying the influence of the interrelationship between the contaminants in diesel fuel and the environment factors.

The Abraham solvation parameter model is a good approach for analyzing and predicting biological activities and partitioning coefficients. The general solvation equation has been used to predict the solute property (SP) behavior of drug compounds between biological barriers. Gas chromatography (GC) retention time can be used to predict molecular descriptors, such as E, S, A, B & L for existing and newly developed drug compounds. In this research, six columns of different stationary phases were used to predict the Abraham molecular descriptors more accurately. The six stationary phases used were 5% phenylmethyl polysiloxane, 6% cyanopropylphenyl 94% dimethylpolysiloxane, 5% diphenyl 95% dimethylpolysiloxane, 100% dimethylpolysiloxane, polyethylene glycol and 35% diphenyl 65% dimethylpolysiloxane. Retention times (RT) of 75 compounds have been measured and logarithm of experimental average retention time Ln(RTexp) are calculated. The Abraham solvation model is then applied to predict the process coefficients of these compounds using the literature values of the molecular descriptors (Acree Compilation descriptors). Six correlation equations are built up as a training set for each of the six columns. The six equations are then used to predict the molecular descriptors of the illegal drugs as a test set. This work shows the ability to extract molecular information from a new compound by utilizing commonly used GC columns available with the desired stationary phases. One can simply run the new compound in GC using these columns to get the retention time. Plugging in the retention time into the developed equations for each of the column will predict the molecular descriptors for the test compound and will give some information about the properties of the compound.

The aim of the diploma thesis was the aroma active compounds assessment and sensory profile determination of various types of sea buckthorn (Hippopha rhamnoides L.). The theoretical part provides the detailed description of this plant, comprising the occurence, taxonomy, chemical composition and use. Experimental part summarizes the data obtained: identification and quantification of aroma compounds using the SPME – GC –FID and GC-MS method and evaluation of complete sensory profile. Various cultivars of sea buckthorn harvested in 2009-2012 were analysed. In total 23 various types of sea buckthorn were measured, 23 alcohols, 10 aldehydes, 11 esters, 14 ketones and 5 acids were found.

Demands for plant-based diets sufficient in all required amino acids are increasing due to health and environmental advantages. As legumes offer a complementing source of quality protein to the already heavily consumed cereals, methods for determining amino acid compositions in legumes are needed. The aim of this thesis was to establish a GC-FID method for analyzing amino acids in legumes and to apply the method to analyze six locally grown legumes: Black beans, brown beans, red kidney beans, white beans, yellow and grey peas. White bean flour was used as an inhouse control sample. Legumes were hydrolyzed with acid and alkaline treatments;hydrolysates were purified and derivatized using an amino acid analysis kit (EZ:faast, Phenomenex) and quantified with GC-FID. All legumes were rich in Asp + Asn, Glu + Gln, Lys and Leu while limited in Met, Cys and Trp. Quality control trials showed a generally good precision of the method (between day CVs were ≤ 10% for 12 of 16amino acids ) and good linearity (r2 were 0,99 or above for 16 of 19 calibration curves). Limits of detection and quantification ranged from 2-46 nmol/mL and 7-154nmol/mL, respectively, depending on the amino acid. No accuracy trial was performed. In conclusion, a rapid GC-FID method for amino acid analysis was established and amino acid compositions of locally grown legumes was tentatively determined. However, further quality control trials are required to validate the method. / Efterfrågan av växt-baserade dieter med komplett innehåll av aminosyror ökar på grund av både hälso- och miljömässiga fördelar. Då baljväxter erbjuder en kompletterande källa till protein av hög kvalitet till cerealier, som redan konsumeras i hög grad, krävs metoder för att analysera aminosyra innehåll i baljväxter. Målet med detta arbete var att etablera en GC-FID metod för att analysera aminosyror i baljväxter och att applicera metoden för att analysera aminosyror för att analysera sex lokala baljväxter: Svarta bönor, bruna bönor, röda kidney bönor, vita bönor, gula och gråa ärtor. Mjöl på vita bönor användes som in-house kontroll prov. Baljväxterna hydrolyserades med både syra och bas behandlingar, hydrolysaterna renades och derivatiserades med ett kit för aminosyraanalys (EZ:faast, Phenomenex) och kvantifierades med GC-FID. Alla baljväxter hade höga halter av Asp + Asn, Glu + Gln, Lys och Leu men låga halter av Met, Cys och Trp. Kvalitetskontroller visade på en generellt hög precision (CV mellan dagar ≤ 10% för 12 av 16 aminosyror) och god linjäritet (r2var 0,99 eller högre för 16 av 19 kalibreringskurvor). Detektions- och kvantifierings-gränser varierade mellan 2-46 nmol / mL respektive 7 – 154 nmol / mL beroende på aminosyran. Inga tester gjordes för att bestämma metodens riktighet.Slutsatsen drogs att en snabb GC-FID metod för aminosyra analys har framtagits och indikativa värden av lokala baljväxters aminosyra innehåll fastställts. Däremot krävs flera kvalitetskontroller för att validera metoden.

Syftet med detta examensarbete var att utveckla en GC-metod för analys av etylenglykoler i förorenade vattenprover, exempelvis industriavloppsvatten. Detta skulle åstadkommas med en GC-FID och MMI (Multimode Inlet), samt helst utan provupparbetning. Ett annat av målen var att kunna kvantifiera inom området 1 ppm till 100 ppm, och att metoden skulle vara tillräckligt stabil för att kunna ackreditera den.Ett flertal kolonner testades, där en HP-5 med dimensionerna 30 m*0,53 mm*0,88 μm från Agilent var den som gav bäst resultat. Även två olika liners provades, dels en med glasull och dels en 2 mm dimpled liner, där dimpled linern gav bäst resultat, och minst ”carry-over” mellan analyserna. Bland de parametrar som gav störst effekt utmärker sig trycket i injektorn, och tiderna som de olika flödena är igång. För fullständiga inställningar, se bilaga 2.En metod redo för ackreditering hann ej tas fram, det finns ett flertal parametrar som bör undersökas för en effektivare och stabilare analys. Men metoden som är framtagen är redo för omfattande repeterbarhetstest. / The purpose of this bachelor’s thesis was to develop a GC method for analysis of ethylene glycols in polluted water samples, for example industrial sewage water. This was meant to be accomplished with a GC FID and MMI (Multimode Inlet), preferably without sample preparation. One of the goals was to be able to quantify between 1 ppm and 100 ppm, and that the method was stable enough for accreditation.A number of columns were tested, from where a HP-5 with the dimensions 30 m*0,53 mm*0,88 μm from Agilent gave the best results. Also, two different liners were tested, one with glass wool and one 2 mm dimpled liner, where the dimpled liner gave the best results and the least carry-over between samples. Amongst the parameters which gave the biggest effect, the inlet pressure and the different flow times stands out. For a full set of settings, see Bilaga 2.A method ready for accreditation was not developed due to short of time. There are still a number of parameters which should be investigated for a more efficient and stabile analysis. But the method developed is ready for extensive repeatability tests.

This research was initiated after a 100-year flood caused an oil spill on the San Jacinto River (Houston, Texas) in October of 1994. After the floodwaters subsided the released petroleum floating on the water was deposited on the surrounding lands. The petroleum spill was used as an opportunity to research intrinsic petroleum biodegradation in a 9-acre petroleum impacted estuarine wetland. The first phase of this research (Phase I) began in December 1994, approximately 1.5 months after the spill of opportunity and involved the study and quantification of in-situ petroleum biodegradation. The second phase of the research (Phase II) began in March 1996 with a controlled oil release to study and evaluate the success of two bioremediation treatments versus natural biodegradation. The study of in-situ petroleum hydrocarbon degradation and the evaluation of bioremediation amendments were successfully quantified using GC-MS analytical techniques. However, the GC-MS technique is limited to the analyses of hydrocarbon compounds, a disadvantage that precludes the overall characterization of petroleum degradation. The research presented here details an analytical technique that was used to provide a full characterization of temporal petroleum biodegradation. This technique uses thin layer chromatography coupled with flame ionization detection (TLC-FID) to characterize the saturate and aromatic (hydrocarbon) fractions and the resin and asphaltene (non-hydrocarbon, polar) fractions. Other analysis techniques, such as HPLC-SARA analysis, are available for the full characterization of the four petroleum fractions. However, these techniques do not lend themselves well to the application of large sample set analysis. A significant advantage of the TLC-FID analysis to other petroleum analysis techniques is the ability to analyze several samples concurrently and quickly with relative ease and few resources. For the purposes of the Phase I and Phase II research the TLC-FID analysis method was evaluated, refined and applied to quantify the temporal biodegradation and bioremediation of petroleum. While the TLC-FID analysis produces a full characterization, it cannot supplant the GC-MS analysis for petroleum bioremediation research. However, it can be used in conjunction with the GC-MS to expand the knowledge of petroleum bioremediation and remediation strategies.

abstract: This thesis provides a cost to benefit analysis of the proposed next generation of distribution systems- the Future Renewable Electric Energy Distribution Management (FREEDM) system. With the increasing penetration of renewable energy sources onto the grid, it becomes necessary to have an infrastructure that allows for easy integration of these resources coupled with features like enhanced reliability of the system and fast pro-tection from faults. The Solid State Transformer (SST) and the Fault Isolation Device (FID) make for the core of the FREEDM system and have huge investment costs. Some key features of the FREEDM system include improved power flow control, compact design and unity power factor operation. Customers may observe a reduction in the electricity bill by a certain fraction for using renewable sources of generation. There is also a possibility of huge subsidies given to encourage use of renewable energy. This thesis is an attempt to quantify the benefits offered by the FREEDM system in monetary terms and to calculate the time in years required to gain a return on investments made. The elevated cost of FIDs needs to be justified by the advantages they offer. The result of different rates of interest and how they influence the payback period is also studied. The payback periods calculated are observed for viability. A comparison is made between the active power losses on a certain distribution feeder that makes use of distribution level magnetic transformers versus one that makes use of SSTs. The reduction in the annual active power losses in the case of the feeder using SSTs is translated onto annual savings in terms of cost when compared to the conventional case with magnetic transformers. Since the FREEDM system encourages operation at unity power factor, the need for installing capacitor banks for improving the power factor is eliminated and this re-flects in savings in terms of cost. The FREEDM system offers enhanced reliability when compared to a conventional system. The payback periods observed support the concept of introducing the FREEDM system. / Dissertation/Thesis / Masters Thesis Electrical Engineering 2015