Difference between revisions of "Team:TU Darmstadt/Notebook/LJ-Chems"

Chemie lab group

PLGA and PLGC polymer and nanosphere production

June
Week 1 (28^th of May – 3^rd of June)
- destillation and Schlenk apparatus were built up
- toluol was dried under argon atmosphere (destillation)
- DCM was dried using a molecular sieve

Week 2 (4^th of June – 10^th of June)
- stock solutions of initiator Lanthane-III-Isoproxide and of the lactide monomer were generated and filled into flasks under argon atmosphere

Week 3 (11^th of June – 17^th of June)
- glycolic acid stock solution was generated and stored at – 20 °C
- anionic-ring opening polymerisation of PLGA (ratio 1:1), purification of the product through recrystallization in methanole, desiccation in dry box under vacuum

July
Week 4 (25^th of June – 1^st of July)
- determination of yield (produced polymer from week 11.06.-15.06.)
- anionic-ring opening polymerization with doubled initiator concentration
- NMR analysis of produced polymer

Week 5 (2^nd of July – 8^th of July)
- toluol was dried under argon atmosphere (destillation)
- new polymerization technique: polymerization directly out of the melt of the monomers, using tin(II)ethylene-hexanoate (ratio 1:3 glycolid acid, lactide)

Week 6 (9^th of July – 15^th of July)
- GPC sample preparation
- GPC analysis

Week 7 (23^rd of July – 29^th of July)
- NMR analysis of polymers produced out of the melt
- solubility tests with products in different solvents (THF, DCM, methanole)
- test of nanosphere synthesis with a test polymer

August
Week 8 (30^th of July – 5^th of August)
- nanosphere synthesis with self-produced polymer, analysis of nanospheres with light microscope
- new ring-opening polymerization with initiator and co-initiator, product purification in methanol, GPC of product
- solving of old polymer products in THF

Week 9 (6^th of August – 12^th of August)
- PLGC production with octadecanole and tin-organyl, polymerization out of the melt
Week 10 (13^th of August – 19^th of August)
- purification of PLGC product in THF and methanol (washing process)
- new PLGA production
- nanosphere synthesis with produced polymers, freeze-drying of spheres for later analysis

Week 11 (20^th of August – 26^th of August)
- three nanosphere syntheses, once with THF as solvent, once using DCM (standard protocol), once with doubled polymer concentration
- analysis of spheres via light microscope and dynamic light scattering technique (DLS)

September
Week 12 (27^th of August – 2^nd of September)
- new PLGA and PLGC polymerization in larger scale
- dilution series of nanospheres with ddH2O
Week 13 (3^rd of September – 9^th of September)
- nanosphere synthesis, this time with extra cleaned snap-on cap bottles and filtered solutions(PTFE filter 4.5 µm)
- DLS measurements
- purification of PLGA and PLGC polymerization products

Week 14 (10^th of September – 16^th of September)
- GPC of PLGC polymerization product
- nanospheres of PLGC and PLGA generated and measured via DLS

Week 15 (17^th of September – 23^rd of September)
- new DLS analyses of freeze-dried samples, of centrifuged samples and of directly synthesized samples

Week 16 (24^th of September – 30^th of September)
- nanosphere synthesis including fluorescein, 5 times in different concentrations between 3 and 7,5 % (w/w) with both PLGA and PLGC
- analysis with DLS of both fresh and freeze-dried samples

October
Week 17 (1^st of October – 7^th of October)
- confocal microscopy of fluorescent spheres
- REM picture of spheres
- lab cleaning

Fly to Boston and attend the Giant Jamboree!

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