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Análise quantitativa de alcanolaminas e CO2 no processo de absorção química via espectroscopia no infravermelho / Quantitative analysis of alkanolamines and CO2 in chemical absorption process by infrared spectroscopyTavares, Denise Trigilio 15 December 2015 (has links)
Em virtude da necessidade de se quantificar os carbamatos provenientes de processos de absorção química do gás CO2 por monoetanolamina (MEA) e dietanolamina (DEA), curvas analíticas por espectroscopia no infravermelho (IV) foram construídas visando à determinação do teor de carbamatos de MEA e DEA, além da quantificação de MEA, DEA e metildietanolamina (MDEA) em soluções puras e em misturas. O procedimento analítico compreendeu o preparo das amostras-padrão constituintes das curvas de calibração e suas quantificações com o emprego de técnicas instrumentais de referência titulação potenciométrica, pesagem e GC-FID. As amostras-padrão de aminas puras foram quantificadas por titulação potenciométrica, sendo possível a detecção exata do ponto de equivalência. As composições dos padrões analíticos de misturas foram estabelecidas segundo um diagrama triangular para misturas e o teor de cada componente foi determinado por gravimetria e GC-FID. Tanto a hidrólise quanto a degradação térmica dos carbamatos foram fatores que restringiram o emprego da titulação potenciométrica, HPLC-MS/MS e GC-FID como técnicas de referência em suas quantificações. Essas restrições, somadas ao fato de não haver disponibilidade comercial desses carbamatos, levaram ao uso da espectroscopia de RMN de 1H na determinação quantitativa. As curvas de calibração apresentaram ótimo ajuste dos valores preditos com relação aos de referência e erro máximo de predição de 0,594 %. Dois processos de absorção química do gás CO2 foram realizados em escala semipiloto e os resultados obtidos foram de 1,02 % e 0,98 % de CO2 absorvido por solução de MEA e DEA, respectivamente. Os mesmos processos foram simulados no software Aspen Plus, obtendo-se 1,18 % de CO2 absorvido por solução de MEA e 1,00 % por solução de DEA. / Due to the need to quantify carbamates from the CO2 gas chemical absorption process by monoethanolamine (MEA) and diethanolamine (DEA), analytical curves by IR spectroscopy were obtained with the aim of quantifying MEA and DEA carbamates and MEA, DEA and methyldiethanolamine (MDEA) in pure solutions and mixtures. The analytical procedure considered the preparation of standard samples constituents of the calibration curves and their quantification using reference instrumental techniques potentiometric titration, gravimetry and GC-FID. The standard samples of pure amines were quantified by potentiometric titration, getting the accurate detection of the equivalence point. The compositions of the analytical standards of the mixtures were established according to a triangular diagram for mixtures and the content of each component was determined by gravimetry and GC-FID. The carbamate hidrolysis and its thermal degradation were factors that limited the use of potentiometric titration, HPLCMS/ MS and GC-FID as reference techniques in their quantitation. These restrictions, added to the fact of not having commercial availability of these carbamates, led the use of 1H NMR spectroscopy for the quantitative determination. The calibration curves resulted in an excellent adjustment of the expected values related to the reference values and maximum error of prediction of 0.594 %. Two chemical absorption processes of CO2 gas were performed in semi-pilot scale and the obtained results were of 1.02 % and 0.98 % of absorbed CO2 by MEA and DEA solutions, respectively. Both processes were simulated using Aspen Plus software, presenting 1.18 % of CO2 absorbed by MEA solution and 1.00 % by DEA solution.
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Análise quantitativa de alcanolaminas e CO2 no processo de absorção química via espectroscopia no infravermelho / Quantitative analysis of alkanolamines and CO2 in chemical absorption process by infrared spectroscopyDenise Trigilio Tavares 15 December 2015 (has links)
Em virtude da necessidade de se quantificar os carbamatos provenientes de processos de absorção química do gás CO2 por monoetanolamina (MEA) e dietanolamina (DEA), curvas analíticas por espectroscopia no infravermelho (IV) foram construídas visando à determinação do teor de carbamatos de MEA e DEA, além da quantificação de MEA, DEA e metildietanolamina (MDEA) em soluções puras e em misturas. O procedimento analítico compreendeu o preparo das amostras-padrão constituintes das curvas de calibração e suas quantificações com o emprego de técnicas instrumentais de referência titulação potenciométrica, pesagem e GC-FID. As amostras-padrão de aminas puras foram quantificadas por titulação potenciométrica, sendo possível a detecção exata do ponto de equivalência. As composições dos padrões analíticos de misturas foram estabelecidas segundo um diagrama triangular para misturas e o teor de cada componente foi determinado por gravimetria e GC-FID. Tanto a hidrólise quanto a degradação térmica dos carbamatos foram fatores que restringiram o emprego da titulação potenciométrica, HPLC-MS/MS e GC-FID como técnicas de referência em suas quantificações. Essas restrições, somadas ao fato de não haver disponibilidade comercial desses carbamatos, levaram ao uso da espectroscopia de RMN de 1H na determinação quantitativa. As curvas de calibração apresentaram ótimo ajuste dos valores preditos com relação aos de referência e erro máximo de predição de 0,594 %. Dois processos de absorção química do gás CO2 foram realizados em escala semipiloto e os resultados obtidos foram de 1,02 % e 0,98 % de CO2 absorvido por solução de MEA e DEA, respectivamente. Os mesmos processos foram simulados no software Aspen Plus, obtendo-se 1,18 % de CO2 absorvido por solução de MEA e 1,00 % por solução de DEA. / Due to the need to quantify carbamates from the CO2 gas chemical absorption process by monoethanolamine (MEA) and diethanolamine (DEA), analytical curves by IR spectroscopy were obtained with the aim of quantifying MEA and DEA carbamates and MEA, DEA and methyldiethanolamine (MDEA) in pure solutions and mixtures. The analytical procedure considered the preparation of standard samples constituents of the calibration curves and their quantification using reference instrumental techniques potentiometric titration, gravimetry and GC-FID. The standard samples of pure amines were quantified by potentiometric titration, getting the accurate detection of the equivalence point. The compositions of the analytical standards of the mixtures were established according to a triangular diagram for mixtures and the content of each component was determined by gravimetry and GC-FID. The carbamate hidrolysis and its thermal degradation were factors that limited the use of potentiometric titration, HPLCMS/ MS and GC-FID as reference techniques in their quantitation. These restrictions, added to the fact of not having commercial availability of these carbamates, led the use of 1H NMR spectroscopy for the quantitative determination. The calibration curves resulted in an excellent adjustment of the expected values related to the reference values and maximum error of prediction of 0.594 %. Two chemical absorption processes of CO2 gas were performed in semi-pilot scale and the obtained results were of 1.02 % and 0.98 % of absorbed CO2 by MEA and DEA solutions, respectively. Both processes were simulated using Aspen Plus software, presenting 1.18 % of CO2 absorbed by MEA solution and 1.00 % by DEA solution.
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Kol-14 datering : En litteraturstudie över hur kol-14 isotopen används för datering, samt utveckling och tillämpning av djup-åldersmodeller inom naturgeografin.Magnusson, Erik January 2013 (has links)
This literature study concerned the use and function of the radioactive isotope carbon-14, as a dating method of organic material, within the scientific field of physical geography. In this report it is presented the need of atmospheric calibration curves and the development of these as a necessity to translate carbon-14 years to calibrated calendar years. A number of common age-depth models that is used to give an approximation of an accumulation sequence and its related dates over the actual time period in different natural archives is presented and discussed. Different problems that commonly occur when age-depth models are utilized as for instance reservoir effects, contaminations or other age deviations are addressed and analyzed. The software CLAM in presented and discussed and was also used to produce age-depth models. In order to test the impact of different age-depth models used to date the immigration of Picea Abies in the Swedish landscape during Holocene, five lake sediment cores and their pollen profiles was remodeled using CLAM. The outcome of the remodeling suggest that the impact of choosing “wrong” age-depth model was of little importance for these chosen lakes, as the deviating ages between the statistically best and the statistically worst model, was just 2% on average. Calendar years derived from carbon-14 dating should not be considered an absolute truth as it is always an uncertainty involved, and the choice of age-depth model for dating a sequence should be based on scientific knowledge of the actual area.
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Characterization of Ethylene/α-Olefin Copolymers Made with a Single-Site Catalyst Using Crystallization Elution FractionationAlkhazaal, Abdulaal January 2011 (has links)
A new analytical technique to measure the chemical composition distribution (CCD) of polyolefins, crystallization elution fractionation (CEF), was introduced in 2006 during the First International Conference on Polyolefin Characterization. CEF is a faster and higher resolution alternative to the previous polyolefin CCD analytical techniques such as temperature rising elution fractionation (TREF) and crystallization elution fractionation (CRYSTAF) (Monrabal et al., 2007).
Crystallization elution fractionation is a liquid chromatography technique used to determine the CCD of polyolefins by combining a new separation procedure, dynamic crystallization, and TREF. In a typical CEF experiment, a polymer solution is loaded in the CEF column at high temperature, the polymer is allowed to crystallize by lowering the solution temperature, and then the precipitated polymer is eluted by a solvent flowing through the column as the temperature is raised. CEF needs to be calibrated to provide quantitative CCD results.
A CEF calibration curve consists of a mathematical relationship between elution temperature determined by CEF and comonomer fraction in the copolymer that could be estimated by Fourier transform infrared spectroscopy (FTIR) and carbon-13 nuclear magnetic resonance (13C NMR). Different comonomer types in ethylene/α-olefin copolymers will have distinct calibration curves.
The main objective of this thesis is to obtain CEF calibration curves for several different ethylene/α-olefin copolymers and to investigate which factors influence these calibration curves. A series of homogeneous ethylene/α-olefin copolymers (1-hexene, 1-octene and 1-dodecene) with different comonomer fractions were synthesized under controlled conditions to create CEF calibration standards. Their average chemical compositions were determined by 13C NMR and FTIR and then used to establish CEF calibration curves relating elution temperature and comonomer molar fraction in the copolymer.
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Characterization of Ethylene/α-Olefin Copolymers Made with a Single-Site Catalyst Using Crystallization Elution FractionationAlkhazaal, Abdulaal January 2011 (has links)
A new analytical technique to measure the chemical composition distribution (CCD) of polyolefins, crystallization elution fractionation (CEF), was introduced in 2006 during the First International Conference on Polyolefin Characterization. CEF is a faster and higher resolution alternative to the previous polyolefin CCD analytical techniques such as temperature rising elution fractionation (TREF) and crystallization elution fractionation (CRYSTAF) (Monrabal et al., 2007).
Crystallization elution fractionation is a liquid chromatography technique used to determine the CCD of polyolefins by combining a new separation procedure, dynamic crystallization, and TREF. In a typical CEF experiment, a polymer solution is loaded in the CEF column at high temperature, the polymer is allowed to crystallize by lowering the solution temperature, and then the precipitated polymer is eluted by a solvent flowing through the column as the temperature is raised. CEF needs to be calibrated to provide quantitative CCD results.
A CEF calibration curve consists of a mathematical relationship between elution temperature determined by CEF and comonomer fraction in the copolymer that could be estimated by Fourier transform infrared spectroscopy (FTIR) and carbon-13 nuclear magnetic resonance (13C NMR). Different comonomer types in ethylene/α-olefin copolymers will have distinct calibration curves.
The main objective of this thesis is to obtain CEF calibration curves for several different ethylene/α-olefin copolymers and to investigate which factors influence these calibration curves. A series of homogeneous ethylene/α-olefin copolymers (1-hexene, 1-octene and 1-dodecene) with different comonomer fractions were synthesized under controlled conditions to create CEF calibration standards. Their average chemical compositions were determined by 13C NMR and FTIR and then used to establish CEF calibration curves relating elution temperature and comonomer molar fraction in the copolymer.
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Měřicí a linearizační zobrazovací jednotka pro průtokoměry / Measurement and linearization unit for flow metersMaštera, Martin January 2015 (has links)
Thesis describes the design and realization of linearization display unit that will receive pulses from a gear flow meter KRACHT whose frequency corresponds to a flow. The measured value is flow that nonlinearly depends on the temperature and viscosity of the medium. The dependency is described by calibration curves for each flow meter. The task of the diploma thesis is to design, implement, and verify the operation of the display unit, which calculates the actual flow rate from the input data (pulse rate, temperature, viscosity, and flow meter calibration curves). The device will contain a suitable user interface to display all measured values, inputs for connecting measuring sensors, and outputs for transmission of measured data. A part of the device will be a USB interface for configuration and uploading calibration curves from a PC application, which is designed by diploma student.
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Estimating Molecular Weights of Organometallics in Solution with Diffusion NMR Techniques / Estimating Molecular Weights of Organometallics in Solution with Diffusion NMR TechniquesBachmann, Sebastian 01 March 2017 (has links)
No description available.
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Poisson, Bayes, Futebol e DeFinetti / Poisson, Bayes, Soccer and DeFinettiArruda, Marcelo Leme de 28 April 2000 (has links)
Nesta dissertação é abordado o problema de previsões probabilísticas para eventos tricotômicos, além da questão de comparação de qualidade das previsões através de curvas de calibração e da Medida de DeFinetti. É feita uma aplicação paraprevisões de resultados de futebol / This dissertation deals with the problem of probabilistic previsions for tricotomic events, in addiction with the question of comparison of quality of the previsions, by using calibration curves and the DeFinetti Measure. An application is developed for previsions of soccer games results.
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Poisson, Bayes, Futebol e DeFinetti / Poisson, Bayes, Soccer and DeFinettiMarcelo Leme de Arruda 28 April 2000 (has links)
Nesta dissertação é abordado o problema de previsões probabilísticas para eventos tricotômicos, além da questão de comparação de qualidade das previsões através de curvas de calibração e da Medida de DeFinetti. É feita uma aplicação paraprevisões de resultados de futebol / This dissertation deals with the problem of probabilistic previsions for tricotomic events, in addiction with the question of comparison of quality of the previsions, by using calibration curves and the DeFinetti Measure. An application is developed for previsions of soccer games results.
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DOSY External Calibration Curve Molecular Weight Determination as a Valuable Methodology in Characterizing Reactive Intermediates in SolutionNeufeld, Roman 14 March 2016 (has links)
No description available.
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