Environmental Analytical Methods (1599), 2013/14

AUTHOR:

Miguel Ángel Sogorb
Jorge Estévez

Dept. Applied Biology

Area Toxicology

This subject has been teached in 
Degree in Environmental Science

  • To list and describe the stages of a quantitative chemical analysis.
  • To list and describe the general principles of the sampling methodology.
  • To calculate the residual concentration of an analyte after a liquid-liquid extraction in certain conditions.
  • To explain the basis for microwave digestion and sonication.
  • To explain the differences among by dry, wet and proteolytic digestions.
  • To explain the operation of a Soxhlet extractor.
  • To explaining at least one technique deproteinization of biological tissues.
  • To recognize the basic components of a supercritical fluid extractor.
  • To explain which bases its efficiency technique supercritical fluid extraction.
  • To differentiate between different modes of supercritical extraction.
  • To explain the differences between the different modes of solid-liquid extraction.
  • To name at least 3 different types of stationary phases used in solid-liquid extraction.
  • To describe the physical and chemical fundamentals of the interactions (polar, non-polar and ionic) that occur between analytes and stationary phases in solid-liquid extractions with minicolumns.
  • To define the terms solvation, retention, elution, capacity and selectivity (based on solid-liquid extraction with minicolumns).
  • To predict how a change of solvent conditions to the retention or elution of an analyte in a liquid-solid extraction minicolumns.
  • To describe the stages of a solid phase microextraction.
  • To describe the stages of a solid phase micro magnetic bar.
  • To qualitatively describe the areas of the electromagnetic radiation spectrum.
  • To establish appropriate relationships between wavelength, frequency and energy of an electromagnetic wave.
  • To define the concepts of transmittance and absorbance.
  • To solve problems by applying the Lambert-Beer law.
  • To describe the parts of a spectrophotometer.
  • To explain the differences between absorption spectroscopy, and fluorescence emission.
  • To draw a diagram of a molecular absorption spectrophotometer, a fluorometer, and atomic emission spectrometry.
  • To explaining the operation of sources of visible, ultraviolet and infrared spectroscopy most common.
  • To describe the operation of a concentric type nebulizer and of at least two different types of atomizers used in atomic spectroscopy.
  • To describe the operation of a hollow cathode lamp.
  • To describe the operation of a plasma torch.
  • To explain the basis for the determination of mercury by cold vapor technique.
  • To explain the advantages of the hydride generation system for the determination of Pb, As, Ge and Bi.
  • To define the concepts of stationary phase support, eluent and mobile phase.
  • To calculate for a given chromatogram following chromatographic parameters: retention volume, number of theoretical plates equivalent to theoretical plate height, capacity factor, separation factor and resolution.
  • To establish a classification of chromatographic techniques based on the arrangement of the stationary phase and the physical state of the mobile phase.
  • To describe the basic principles of chromatography separation of analytes by normal phase adsorption, reverse-phase adsorption, distribution, ion exchange, gel filtration and affinity.
  • To explain the principles of operation of the thin layer chromatography.
  • To define the Rf factor in thin layer chromatography.
  • To predic Rf factor as affect a given change in the polarity of the solvent in a separation thin layer chromatography.
  • To describe the basic components of a system of high-performance liquid chromatography.
  • To explainin the operation of the following liquid chromatography detectors such as fluorescence, conductivity , amperometric and UV-visible diode array.
  • To describe the basic components of a gas chromatography system.
  • To describe the types of common stationary phase in gas chromatography.
  • To describe the differences between the injection modes «with» and «without» flow division in gas chromatographic system.
  • To explain the influence of temperature on the gas chromatographic separations.
  • To explain the operation of the following gas chromatography detectors: flame ionization, electron capture, nitrogen and phosphorus thermal conductivity.
  • To describe the basic components of a capillary electrophoresis system.
  • To define the following concepts: electroosmotic flow, electrical mobility and effective mobility on a capillary electrophoresis system.
  • To explain how works most common detectors in capillary electrophoresis.
  • To describe the basic operating principles of capillary electrophoresis micellar free zone, and isoelectric focusing gel.
  • To describe the basic principles that govern the gravimetric and volumetric methods.
  • To describe the basis of a volumetric method of neutralization, precipitation and complex formation.
  • To enumerate least three different analytes analyzable by each of the following techniques: 1) an assessment by neutralization , 2 ) precipitation titration , and 3 ) assessment for complex formation.
  • To describe the general principles of gravimetric methods of precipitation and volatilization.
  • To describe the basic parts of a mass spectrometer .
  • To explain the operation of these systems: ionization impact, electronic assisted laser desorption ionization, atmospheric pressure chemical and atmospheric pressure ionization electrospray.
  • To explain how the following mass spectrometry analyzers: magnetic sector double sector and quadrupole time of flight.
  • To explain the operation of a mass spectrometry detector.
  • To describe the differences between SIM detection mode and SCAN mode.
  • To explain what a tandem mass spectrometer.
  • To describe the advantages of a detector mass against another type of detector coupled to a gas chromatograph.
  • To write the advantages of a detector mass against another type of detector coupled to a liquid chromatograph.
  • To describe the advantages of a system coupled to mass spectrometry with inductively coupled plasma (ICP) compared to other systems of nuclear detection and quantification.
  • To list several applications of mass spectrometry coupled to inductively coupled plasma.
  • To perform the calculations necessary to prepare solutions of the required concentrations.
  • To pipet skill.
  • To calculate, having suitable patterns, the problem of an analyte concentration using colorimetric and chromatographic analytical techniques.
  • To perform appropriate procedures for determining the alkalinity of a water sample by an acid-base titration.
  • To separate two analytes using a technique of solid-liquid extraction.
  • To use, following the teacher’s instructions, the following equipment: 1) Soxhlet extraction equipment, 2) liquid chromatograph high resolution, 3) a gas chromatograph; 4) an induction-coupled plasma mass spectrometer.

Materials

Theory Practice Solved practice Exercise Solved Exercises Proyectos Case studies Exams Self-assessment Seminar Presentation

Type of documents

pdf ppt avi swf xls html

Description

All the materials here included are used by students during the year 2013/14 in the subject 1599 called Environmental analytical methods.

In particular, they match to :

Theory Practice Solved practice Exercise Solved Exercises Proyectos Case studies Exams Self-assessment Seminar Presentation

Subject name Number CT CP CTOT
ENVIRONMENTAL ANALYTICAL METHODS 1599 3 3 6
Type Elective Semester 2 Course 4
Description Treatments analytical samples. Chromatographic techniques. Atomic absorption spectroscopy. Chemical and biological biomarkers of exposure and effect.
Departamento APPLIED BIOLOGY
Área TOXICOLOGY
Grado DEGREE IN ENVIRONMENTAL SCIENCE
Centro FACULTY OF EXPERIMENTAL SCIENCES

 

Learning objectives

  • To list and describe the stages of a quantitative chemical analysis.
  • To list and describe the general principles of the sampling methodology.
  • To calculate the residual concentration of an analyte after a liquid-liquid extraction in certain conditions.
  • To explain the basis for microwave digestion and sonication.
  • To explain the differences among by dry, wet and proteolytic digestions.
  • To explain the operation of a Soxhlet extractor.
  • To explaining at least one technique deproteinization of biological tissues.
  • To recognize the basic components of a supercritical fluid extractor.
  • To explain which bases its efficiency technique supercritical fluid extraction.
  • To differentiate between different modes of supercritical extraction.
  • To explain the differences between the different modes of solid-liquid extraction.
  • To name at least 3 different types of stationary phases used in solid-liquid extraction.
  • To describe the physical and chemical fundamentals of the interactions (polar, non-polar and ionic) that occur between analytes and stationary phases in solid-liquid extractions with minicolumns.
  • To define the terms solvation, retention, elution, capacity and selectivity (based on solid-liquid extraction with minicolumns).
  • To predict how a change of solvent conditions to the retention or elution of an analyte in a liquid-solid extraction minicolumns.
  • To describe the stages of a solid phase microextraction.
  • To describe the stages of a solid phase micro magnetic bar.
  • To qualitatively describe the areas of the electromagnetic radiation spectrum.
  • To establish appropriate relationships between wavelength, frequency and energy of an electromagnetic wave.
  • To define the concepts of transmittance and absorbance.
  • To solve problems by applying the Lambert-Beer law.
  • To describe the parts of a spectrophotometer.
  • To explain the differences between absorption spectroscopy, and fluorescence emission.
  • To draw a diagram of a molecular absorption spectrophotometer, a fluorometer, and atomic emission spectrometry.
  • To explaining the operation of sources of visible, ultraviolet and infrared spectroscopy most common.
  • To describe the operation of a concentric type nebulizer and of at least two different types of atomizers used in atomic spectroscopy.
  • To describe the operation of a hollow cathode lamp.
  • To describe the operation of a plasma torch.
  • To explain the basis for the determination of mercury by cold vapor technique.
  • To explain the advantages of the hydride generation system for the determination of Pb, As, Ge and Bi.
  • To define the concepts of stationary phase support, eluent and mobile phase.
  • To calculate for a given chromatogram following chromatographic parameters: retention volume, number of theoretical plates equivalent to theoretical plate height, capacity factor, separation factor and resolution.
  • To establish a classification of chromatographic techniques based on the arrangement of the stationary phase and the physical state of the mobile phase.
  • To describe the basic principles of chromatography separation of analytes by normal phase adsorption, reverse-phase adsorption, distribution, ion exchange, gel filtration and affinity.
  • To explain the principles of operation of the thin layer chromatography.
  • To define the Rf factor in thin layer chromatography.
  • To predic Rf factor as affect a given change in the polarity of the solvent in a separation thin layer chromatography.
  • To describe the basic components of a system of high-performance liquid chromatography.
  • To explainin the operation of the following liquid chromatography detectors such as fluorescence, conductivity , amperometric and UV-visible diode array.
  • To describe the basic components of a gas chromatography system.
  • To describe the types of common stationary phase in gas chromatography.
  • To describe the differences between the injection modes «with» and «without» flow division in gas chromatographic system.
  • To explain the influence of temperature on the gas chromatographic separations.
  • To explain the operation of the following gas chromatography detectors: flame ionization, electron capture, nitrogen and phosphorus thermal conductivity.
  • To describe the basic components of a capillary electrophoresis system.
  • To define the following concepts: electroosmotic flow, electrical mobility and effective mobility on a capillary electrophoresis system.
  • To explain how works most common detectors in capillary electrophoresis.
  • To describe the basic operating principles of capillary electrophoresis micellar free zone, and isoelectric focusing gel.
  • To describe the basic principles that govern the gravimetric and volumetric methods.
  • To describe the basis of a volumetric method of neutralization, precipitation and complex formation.
  • To enumerate least three different analytes analyzable by each of the following techniques: 1) an assessment by neutralization , 2 ) precipitation titration , and 3 ) assessment for complex formation.
  • To describe the general principles of gravimetric methods of precipitation and volatilization.
  • To describe the basic parts of a mass spectrometer .
  • To explain the operation of these systems: ionization impact, electronic assisted laser desorption ionization, atmospheric pressure chemical and atmospheric pressure ionization electrospray.
  • To explain how the following mass spectrometry analyzers: magnetic sector double sector and quadrupole time of flight.
  • To explain the operation of a mass spectrometry detector.
  • To describe the differences between SIM detection mode and SCAN mode.
  • To explain what a tandem mass spectrometer.
  • To describe the advantages of a detector mass against another type of detector coupled to a gas chromatograph.
  • To write the advantages of a detector mass against another type of detector coupled to a liquid chromatograph.
  • To describe the advantages of a system coupled to mass spectrometry with inductively coupled plasma (ICP) compared to other systems of nuclear detection and quantification.
  • To list several applications of mass spectrometry coupled to inductively coupled plasma.
  • To perform the calculations necessary to prepare solutions of the required concentrations.
  • To pipet skill.
  • To calculate, having suitable patterns, the problem of an analyte concentration using colorimetric and chromatographic analytical techniques.
  • To perform appropriate procedures for determining the alkalinity of a water sample by an acid-base titration.
  • To separate two analytes using a technique of solid-liquid extraction.
  • To use, following the teacher’s instructions, the following equipment: 1) Soxhlet extraction equipment, 2) liquid chromatograph high resolution, 3) a gas chromatograph; 4) an induction-coupled plasma mass spectrometer.

Contents

Unit 1: sample pretreatments. (no disponible)
Unit 2: Spectroscopic techniques. (no disponible)
Unit 3: Separation techniques: chromatography and electrophoresis. (no disponible)
Unit 4: Other chemical analysis techniques. (no disponible)

Teaching method

  • Case studies: Learning acquisition through the analysis of actual or simulated cases, in order to understand and solve them by using alternative procedures.
  • Exercise and problem resolution: Exercising, rehearsing and putting in practice prior knowledge through routine repetition.
  • Presentation/Master class: To pass on knowledge and to activate cognitive processes in the students, involving their participation.
  • Problem based learning: Developing active learning strategies through problem solving that promote thinking, experimentation, and decision making in the student.

Evaluation system

  • The final grade is obtained by the following equation:

    Final Grade = 0.75 x 0.25 x rated theory + practical qualification

    To pass the course will be essential to have completed and passed the practical module.

    Qualification of theory

    The rating of theory is obtained from the following equation:

    Rating theory exam score = 0.75 x + 0.25 x theory qualification activities

    Theory exam

    The theory exam will account for 75 % of the theory grade and will consist of 2 questions or problems each worth 1 point plus a multiple choice test of 32 questions where each question will be offered five possible answers of which only one will be true. All questions are worth 0.25 points and for each wrong question 0.25 will be deducted right questions.

    Activities

    At the end of each teaching unit the teacher will propose one or more activities (test solving, problems, etc¿). The resolution within these activities is 10 days after which not accept or qualify any activity and the teacher posted on the website of the course grades as well as solutions to the proposed activity.

    Each activity will be judged according to the criteria that will be announced in due course but overall, all activities will involve 25% of the rating of theory.

    The only acceptable way to deliver the implementation activities will be designed for that purpose within the course website.

    The rating of the activities shall be valid for three calls of the academic year (June, September and December) , but not for the next academic year.

    Rating practices

    To pass the course will be essential to overcome the practical module.

    The practical module will be considered passed when they find each and every one of the following circumstances:

    1) The student attends more than 50% of the practical sessions (minimum 4 sessions)
    2) To deliver the reports for each single practice
    3) Students during practical sessions show the necessary respect toward peers , teachers and practice material as well as maintain a positive attitude toward learning.

    The rating practices will be obtained using the following equation:

    Rating = average grading practices reporting practices

    In the absence of any qualifying practice session of the lab report for that session is 0 points if the practice had developed in one session , 50 % lower than that of other group members in case practice had developed in 2 sessions the student having missed 1 session , or 33% lower than the remains of members of the group if the practice had developed in 3 sessions the student having missed one session, or 66% lower than the remains of members of the group if the practice had developed in 3 sessions the student having missed 2 sessions .

    In case the student does not pass the practice has the right to make a written exam to pass the subject allows. This exam will consist of two problems related to the contents developed during practical sessions. To pass the course the rating of this examination shall be equal to or greater than 5 points and will account for 25 % of the final grade.

Instructor(s)

Nombre E-mail
JORGE ESTEVEZ DOMENECH
MIGUEL ANGEL SOGORB SANCHEZ

Learning materials

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