This laboratory consists of three of four themes including those in Laboratory II; Theme A: X ray diffraction, C: Polymer solution properties and the volume-phase transition of polymer gel, and D: Conductive polymers.
This laboratory is a prerequisite class for students majoring polymer science to obtain necessary experimental skills. The aims are to enable the students to understand the crystalinne structure, phase separation, solution- and gel properties, and fundamental electrical properties of polymers together with obtaining skills for polymer property analyses such as X-ray diffraction and so on.
It is also aimed for students to learn how to summarize a research report and present the analysis results and discussion as an oral presentation.
Students will learn to do the followings
Theme A: 1) Have an understanding of the basic elements of X-ray diffraction,and measure diffraction patterns using a powder X-ray diffractometer.
2) Analyze diffraction patterns of simple crystal systems (i.e., the cubic and hexagonal systems).
3) Determine crystallite size and crystallinity for polymer crystals.
Theme C:1)Give a theoretical explanation for the phase speparation and the volume-phase transition on the basis of Flory-Huggins equation.
2)Give a qualitative explanation on the mechanism for the temperature-induced phase transition of thermo-sensitive polymers.
3)Give an explanation on the correlation between the intrinsic viscosity and the polymer molecular weight.
4)Give an explanation on the relation between the gel preparation by crosslinkage and the gel properties.
Theme D: １）Have an understanding of the basic principal of conductivity of conjugated polymers, and measure conductance using electrochemical analyzer.
２）Have an understanding of the mechanism of electrochemical polymerization, and explain the relationship between the reaction
conditions and conductivity of obtained films.
３）Have an understanding of the structure of conjugated polymer, and explain the mechanism of solvatochromism and thermochromism.
X-ray diffraction, Crystal lattices, Miller indices, Structure factor, Cｒｙstallinity, Ｃｒｙｓｔａｌｌｉｔｅ ｓｉｚｅ, Gel, Volume-phase transition, Phase separation, Intrinsic viscosity, Condugated polymer, Conductivity, Electrochemical polymerization, Solvato- and thermochromism
|✔ Specialist skills||Intercultural skills||✔ Communication skills||✔ Critical thinking skills||✔ Practical and/or problem-solving skills|
This laboratory course consists of three parts; 1st (Class 1 for guidance), 2nd (Class 2-8 for first theme), 3rd (Class 9-15 for second theme). Students are divided into three groups; One half is for theme A, two quarters are for theme C or D. Students who started with theme A will be grouped into theme C or D for the second theme, and vice versa. The course schedule below is for the former case. For the latter case, the schedule of the 2nd and 3rd parts should be exchanged. Students who conducted theme C or D in this laboratory course will be grouped into theme D or C in addition to theme B in the laboratory II for all the students to conduct all the themes A - D.
|Course schedule||Required learning|
|Class 1||Guidances on the whole course and the respective themes||Understanding the course aims and the theoretical backgrounds of the respective themes.|
|Class 2||Theme A: Measurements of cubic structure crystals||To measure the X-ray diffraction pattern of cubic structure crystals.|
|Class 3||Theme A: Crystal Structure Determination (I) Cubic structures||To index the X-ray diffraction pattern and calculate the lattice parameters of materials with a cubic structure.|
|Class 4||Theme A: Measurements of hexagonal structure crystals / Crystal Structure Determination (II) Hexagonal structures||To index the X-ray diffraction pattern and calculate the lattice parameters of materials with a hexagonal structure.|
|Class 5||Theme A: Identification of an unknown specimen / Precise lattice parameter measurements||To identify an unknown specimen by X-ray diffraction procedures. / To determine the precise lattice parameters of materials by X-ray diffraction methods.|
|Class 6||Theme A: X-ray diffraction of polymer crystals||To measure the X-ray diffraction pattern of polymer crystals.|
|Class 7||Theme A: Determination of crystallite size and crystallinity of polymer crystals||To determine the average crystallite size and crystallinity of polymer crystals by X-ray diffraction pattern analysis.|
|Class 8||Theme A: Data reduction/Oral examination||To organize the diffraction data and show the analysis results / Oral examination for evaluation of students' achievement.|
|Class 9||Theme C:Synthesis of linear polymer and gel samples or Theme D:Synthesis and electronic property of conjugated polymer: Electrochemical polymerization of pyrrole||Theme C: Prepare the polymer solution and gel samples by radical polymerization of NIPA in the absence and the presence of crosslinking agent. ThemeD:Syntheize polypyrrole via electrochemical polymerization under certain conditions|
|Class 10||Theme C:Measurements on the turbidity of polymer solution and swelling ratio of polymer gel or Theme D:Measurement of conductivity||Theme C:Measure the turbidity and the swelling ratio of solution and gel samples. ThemeD:Analyze conductivity of obtained polymer|
|Class 11||Theme C:Estimation of the molecular weight by the viscosity measurement and determination of the original research theme or ThemeD: Electrochemical polymerization of pyrrole and measurement of conductivity||Theme C:Estimate the molecular weight by viscometry of the aq.polymer solution and determine a group-original research theme. ThemeD:Synthesize polypyrrole with different conditions, and analyze conductivity. Synthesize de-doped polypyrrole|
|Class 12||Theme C: Synthesis of linear polymer or gel samples for the original research theme or Theme D: Oxidative polymerization of decylthiophene and anaylsis of its structure||Theme C: Prepare the polymer solution or gel samples depending on the group-original research theme. ThemeD:Synthesize polythiophene via oxidative polymerization. Chacterize thiophene monomer by H NMR and IR spectroscopy.|
|Class 13||Theme C: Synthesis of linear polymer or gel samples for the original research theme or Theme D: Purification of polydecylthiophene||Theme C: Measure and analyze the turbidity or swelling ratio depending on the group-original research theme. ThemeD:Collect the polymer, and have an understanding of polymerization mechanism.|
|Class 14||Theme C: Conducting original research theme or Theme D: Observation of solvato- and thermochromism of polydecylthiophene||ThemeC：Measure and analyze the turbidity or swelling ratio depending on the group-original research theme. ThemeD:Measure the UV–vis spectra of polymer, and observe the solvato- and thermo-chromism.|
|Class 15||Theme C: Oral presentation and Q&A or Theme D: Oral presentation||Theme C:Oral presentation on each group-original theme and Q&A. ThemeD：Have an oral presentation about the structure and electronic property of conjugated polymer to check the understanding level.|
Textbook for Polymer Chemistry Laboratory I & II
Assessment on the reports and the oral presentations or examination.
Chemical Engineering and Industrial Chemistry Laboratory I～III