TAAQI - Advanced Instrumental Techniques of Chemical Analysis

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1 Coordinating unit: Teaching unit: Academic year: Degree: ECTS credits: ESEIAAT - Terrassa School of Industrial, Aerospace and Audiovisual Engineering ETP - Department of Textile and Paper Engineering MASTER'S DEGREE IN FIBROUS MATERIAL TECHNOLOGY ENGINEERING (Syllabus 2012). (Teaching unit Optional) 5 Teaching languages: Spanish Teaching staff Coordinator: Others: Mª Carmen Gutiérrez Bouzán Diana Cayuela Marín Prior skills Knowledge of materials and textile processes Degree competences to which the subject contributes Specific: 1. METMF_The ability to develop new fibres or yarns, and woven or unwoven fabrics, for specific purposes meeting the prescribed specifications by using state-of-the-art technological innovations. 2. METMF_The ability to quantify colour and characterize dyes and pigments in order to select the most suitable detergents and ancillary products for a given textile process. 3. METMF_The ability to use suitable analytical techniques for the qualitative and quantitative analysis of the microstructure and composition of textile fibres and ancillary products. 4. METMF_The ability to optimize and manage textile eco-finishing processes, bleaching production, dyeing, printing, finishes and textile wastewater processing and purification, as well as to understand and manage chemical safety in textile products. 5. METMF_The ability to use multivariate analysis techniques to analyse the textile material and product market, and also to implement a flow production process. 6. METMF_A sound knowledge of mathematical, analytical, scientific, instrumental, technological and management concepts. 7. METMF_The ability to project, calculate and design products, processes, facilities and plants in the Textile, Paper and Graphic, and Leather Engineering domains. 8. METMF_The ability to direct, plan and supervise multidisciplinary teams. 9. METMF_The ability to conduct research, development and innovation activities within the scope of Textile, Paper and Graphic, and Leather Engineering. 10. METMF_The ability to develop strategic plans and apply them to production, quality assurance and environmental management systems within the scope of Textile, Paper and Graphic, and Leather Engineering. 11. METMF_The ability to manage in technical and economic terms projects, facilities, plants, enterprises and technological centres in the Textile, Paper and Graphic, and Leather Engineering domains. 12. METMF_The ability to undertake general, technical and RDI management functions in technological plants, enterprises and centres in the Textile, Paper and Graphic, and Leather Engineering domains. 13. METMF_The ability to apply legislation in force as a Textile, Paper and Graphic or Leather engineer. 1 / 9

2 Teaching methodology MD1. The session combines practical and theoretical aspects. Discussion of practical cases by the professor and the students MD2. Practical sessions where the teachers, with the help of the students, solve practical cases related to the theoretical contents of the subject. MD3. Guided laboratory work MD4. Self-work on the studied subject MD5. Teacher-guided student activities MD6. Teaching materials, text, articles, etc. MD7. Deliver problems and exercises. Answer doubts and questions through the virtual campus Atenea. Learning objectives of the subject 1. To know how the properties of the textile materials vary in the manufacturing process depending on the manufacturing parameters and on the study of the microstructure of textile fibres. 2. To know the analytical techniques for determining the microstructure of textile fibres. 3. To know the fundamentals of spectroscopic and chromatographic analytical techniques and the qualitative and quantitative information that they provide. 4. To know when the different analytical techniques can be applied. 5. To be able to select the most appropriate technique to solve a specific problem. Study load Total learning time: 125h Hours large group: 45h 36.00% Hours medium group: 0h 0.00% Hours small group: 0h 0.00% Guided activities: 0h 0.00% Self study: 80h 64.00% 2 / 9

3 Content Theme 1: Microstructure of synthetic fibres Learning time: 4h 30m Theory classes: 1h 30m Self study : 3h The microstructure of synthetic fibres based, mostly, on the importance of the crystallinity and orientation is described. Also how these properties change with the variables of the textile process and its impact on the properties of the substrates is analysed. AF1 Lectures on the theorical contents with active involvement of the students. Theme 2: Determination of fibres orientation Learning time: 2h 30m Theory classes: 1h 30m Self study : 1h The operation of Sonic Modulus measuring equipment is described. The example of application to the determination of the orientation of different speeds of spinning polyester multifilament is developed. The operation of a polarized light microscope used to determine the birefringence of fibres as an answer to orientation is developed. Application to the determination of the orientation of polyamide 6 multifilament with different draw ratios is analysed. 3 / 9

4 Theme 3: Determination of fibres crystallinity Learning time: 16h Theory classes: 6h Self study : 10h Three different methods to determine crystallinity are developed: from density, by x-ray and by differential scanning calorimetry. The measure of density is described and applied to the determination of the crystallinity of polyamide 6.6 heatset substrates. The X rays measure equipment and its application to the determination of crystallinity of polylactide textured substrates are described. DSC equipment and its application to the determination of crystallinity of heat-set polyester substrates is described Theme 4: Application of thermal analysis to the determination of the microstructure of synthetic fibres Learning time: 16h Theory classes: 6h Self study : 10h Apart from the determination of the crystallinity, thermal analysis allows other determinations of the fibres microstructure. Thus, by Differential Scanning Calorimetry (DSC), the effective heat treatment temperature is able to be determined and its application to different types of fibres is studied. The non-isothermal crystallization of polymers and the application to the study of compatibility of polymerinorganic particles will also be studied. Thermomechanical Analysis (TMA) equipment, phenomena measured by TMA and its application to the determination of the Tg of heat-set polyester substrates is described. Through the study of Thermogravimetrical Analysis (TGA) the porosity of polyamide 6.6 fibres may be determined. 4 / 9

5 Theme 5: Physical-Chemical techniques to characterize fibres microstructure Learning time: 14h 30m Theory classes: 4h 30m Self study : 10h The physical-chemical techniques of critical dissolution time, differential solubility and iodine sorption as techniques to study the microstructure of synthetic fibres and their variation with textile processing variables is studied. Theme 6: Spectroscopic Methods: UV-visible Spectroscopy. Learning time: 9h Self study : 6h 6.1. Definitions 6.2. Fundamentals of UV-visible spectroscopy: - Qualitative analysis - Lambert-Beer Law - Quantitative analysis - Colorimetric determinations - Analysis of mixtures Molecular Fluorescence: definition, instrumentation and applications 6.4. Practical: Determination of free formaldehyde according to UNE standard (Japanese method). AF7 5 / 9

6 Theme 7: Spectroscopic Methods: Atomic absorption spectroscopy Learning time: 9h Self study : 6h 7.1. Fundamentals of atomic absorption spectroscopy - Instrumentation - Comparison between flame electrothermal and plasma AA 7.2. Ratio between absorbance - concentration - Applications to the qualitative and quantitative analysis of metals Practice: Analysis of iron on a fabric by flame AA. Theme 8: Spectroscopic Methods: Infrared Spectroscopy Learning time: 5h Theory classes: 2h Self study : 3h 8.1. Fundamentals of IR spectroscopy - Instrumentation - FTIR-ATR-Sample preparation - Qualitative analysis: main functional groups - Interpretation of IR spectra - Applications to quantitative analysis Practice: Identification of a textile fiber by FTIR with KBr pellet. AF5 Attendance of seminars and lectures, and visits to firms engaged in activities related to the subject contents. 6 / 9

7 Theme 9: Spectroscopic Methods: Mass Spectroscopy Learning time: 2h Theory classes: 1h Self study : 1h 9.1. Fundamentals of mass spectroscopy: - Instrumentation 9.2. Qualitative analysis: interpretation of mass spectra. (ENG) Tema 10: Mètodes cromatogràfics Learning time: 6h Self study : 3h Definitions and characteristics of chromatographic techniques Different classifications of chromatographic methods Main chromatographic parameters. AF5 Attendance of seminars and lectures, and visits to firms engaged in activities related to the subject contents. 7 / 9

8 Theme 11: Liquid Chromatography Learning time: 9h Self study : 6h Instrumentation and techniques? Column Chromatography - Thin Layer Chromatography - High performance liquid chromatography (HPLC) - Ion Chromatography - Exclusion Chromatography - Liquid Chromatography Detectors - Applications of Liquid Chromatography Practice: Separation of dyes (or optical brighteners) by thin layer chromatography. Theme 12: Gas Chromatography Learning time: 9h Self study : 6h Parameters - Instrumentation - Columns - Injectors - Detectors - Gas chromatography coupled to mass spectrometry (GCMS) - Applications to the qualitative and quantitative analysis Practice: Analysis of volatile solvents on a fabric by GCMS and headspace (HS) injection. 8 / 9

9 Theme 13: Comparison of the different Chromatographic Techniques Learning time: 12h Self study : 9h Information provided by each chromatographic technique - Types of samples to be analysed - Selection of the separation technique - Selection of detector - Difficulty and cost of the analysis Practical work: Comparison of 3 chromatographic methods for determination of aromatic amines derived from azo dyes or description of other methods to analyse toxic compounds in textiles. AF4 Oral presentation to be given to the teachers and peers. Qualification system EV1: Evaluation of knowledge acquisition through written exams EV2: Evaluation of laboratory practice from written reports and oral presentations EV3: Evaluation of practical case and work through reports and oral presentations EV4: Evaluation of activities and exercises Weighting: EV1 = 70%; EV3 = 20%; EV2 +EV4 = 10% Regulations for carrying out activities - Attendance to practical classes is mandatory. - The practical reports and the oral presentation (Theme 13) are mandatory. Bibliography Others resources: 9 / 9

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