Analytical Chemistry II + Laboratory
Code 068CC
Credits 9
Learning outcomes
The course enables students to acquire the theoretical knowledge of instrumental techniques based on chromatography and mass spectrometry for the characterisation of compounds in complex matrices.
The course enables students to acquire the knowledge for checking the analytical data quality. The laboratory part of the course enables students to perform qualitative and quantitative chemical analyses by means of chromatographic and spectrophotometric techniques for the determination of organic and inorganic compounds in matrices with different complexity. The course enables students to be able to use statistical methods for the treatment of experimental errors.
Topics of the course.
The concept of analytical procedure. Detection limit of an analytical procedure.Certified reference materials and their use in the validation of analytical procedures. Intercalibration exercises. Quality control charts. Control of analytical data quality.
Sampling and sample pre-treatment. Methods based on matrix digestion, on the extraction of the analytes from the matrix: : liquid/liquid extraction (not continuous and continuous), solid/liquid extraction (soxhlet,SPE, SPME), supercritical fluid extraction, purge and trap extraction.
Chromatographic techniques: basic information on separation techniques and their classification. Plate and rate theory of chromatography. Equations for chromatography. Temperature program in gas chromatography. Elution gradient in HPLC. Injection systems and detectors in GC and HPLC. The use of mass spectrometry as detector in GC and HPLC. Basic information on supercritical phase chromatography.
Spectrometric techniques: atomic absorption spectrometry. Radiation emitters. Atoms emitters: graphite oven. Methods for the correction of no-specific absorptions: correction with deuterium lamp; Smith-Hjeftie correction; Zeeman correction. Factors that limit linear dynamic range in AAS. Matrix effects and matrix modifiers.
Safety in laboratory. Statistical treatment of experimental data. Distribution of means. Confidence limits. Significativity test. Outliers
Application of chromatographic and spectrophotometric in the determination of elements and compounds in samples collected from various matrices.
Laboratory exercises with chromatographic techniques. TLC, GC, HPLC and exchange ionic chromatography.
Laboratory exercises with atomic absorption spectrometry. Calculation of the linear dynamic range and of detection limit. Determination of trace elements in several samples.
Exercises in the computer laboratory; data treatment for GC/MS chromatography.
The course enables students to acquire the knowledge for checking the analytical data quality. The laboratory part of the course enables students to perform qualitative and quantitative chemical analyses by means of chromatographic and spectrophotometric techniques for the determination of organic and inorganic compounds in matrices with different complexity. The course enables students to be able to use statistical methods for the treatment of experimental errors.
Topics of the course.
The concept of analytical procedure. Detection limit of an analytical procedure.Certified reference materials and their use in the validation of analytical procedures. Intercalibration exercises. Quality control charts. Control of analytical data quality.
Sampling and sample pre-treatment. Methods based on matrix digestion, on the extraction of the analytes from the matrix: : liquid/liquid extraction (not continuous and continuous), solid/liquid extraction (soxhlet,SPE, SPME), supercritical fluid extraction, purge and trap extraction.
Chromatographic techniques: basic information on separation techniques and their classification. Plate and rate theory of chromatography. Equations for chromatography. Temperature program in gas chromatography. Elution gradient in HPLC. Injection systems and detectors in GC and HPLC. The use of mass spectrometry as detector in GC and HPLC. Basic information on supercritical phase chromatography.
Spectrometric techniques: atomic absorption spectrometry. Radiation emitters. Atoms emitters: graphite oven. Methods for the correction of no-specific absorptions: correction with deuterium lamp; Smith-Hjeftie correction; Zeeman correction. Factors that limit linear dynamic range in AAS. Matrix effects and matrix modifiers.
Safety in laboratory. Statistical treatment of experimental data. Distribution of means. Confidence limits. Significativity test. Outliers
Application of chromatographic and spectrophotometric in the determination of elements and compounds in samples collected from various matrices.
Laboratory exercises with chromatographic techniques. TLC, GC, HPLC and exchange ionic chromatography.
Laboratory exercises with atomic absorption spectrometry. Calculation of the linear dynamic range and of detection limit. Determination of trace elements in several samples.
Exercises in the computer laboratory; data treatment for GC/MS chromatography.