--> Project: Controlled Synthesis of Methacrylate and Acrylate Diblock Copolymers via End-Capping using CCTP and FRP --> Folder Structure: The files are organised by technique used for the characterisation of the final products --> Abbreviations: DOSY NMR: Diffusion ordered spectroscopy Nuclear Magnetic Resonance GPC: Gel permeation chromatography MALDI-ToF: Matrix-Assisted Laser Desorption/Ionization-Time Of Flight (MALDI-TOF) mass spectrometry (MS) NMR: Nuclear Magnetic Resonance pLMA: poly(lauryl methacrylate) pBzMA: poly(benzyl methacrylate) pMA: poly(methyl acrylate) pBA: poly(butyl acrylate) pMMA: poly(methyl methacrylate) MMAD8: deuterated methyl methacrylate DCTB: trans-2-[3-(4-tert-Butylphenyl)-2-methyl-2-propenylidene] malononitrile NaI: sodium iodide THF: tetrahydrofuran pMMAx: poly(methyl methacrylate) with average degree of polymerisation x --> Software needed to open files according to technique used: for NMR files: ACD-LABS for MALDI-ToF files: Bruker Data Analysis for Gas Chromatography files: Origin for Oxygen Probe files: Origin for GPC files: Agilent GPC --> Protocols, parameters, details of equipment used: Nuclear Magnetic Resonance (1H NMR, 13C NMR, and DOSY NMR): All spectra were recorded on Bruker DPX-300, DPX-400 and DPX-500 MHz spectrometers using deuterated chloroform (CDCl3) purchased from Aldrich. Chemical shifts are given in ppm downfield from the internal standard tetramethylsilane. Gel Permeation Chromatography (GPC): All chromatography measurements were conducted using an Agilent 390-LC MDS instrument equipped with a differential refractive index (DRI) and dual wavelength UV detectors. The system was equipped with 2 x PLgel Mixed C columns (300 x 7.5 mm) and a PLgel 5 µm guard column. The eluent is THF with 2 % TEA (triethylamine) and 0.01 % BHT (butylated hydroxytoluene) additives. Samples were run at 1mL/min at 30’C. Poly(methyl methacrylate) and polystyrene standards (Agilent EasyVials) were used for calibration. Analyte samples were filtered through a GVHP membrane with 0.22 µm pore size before injection. Respectively, experimental molar mass (MnSEC) and dispersity (Ð) values of synthesized polymers were determined by conventional calibration using Agilent GPC/SEC software. Matrix-assisted laser desorption/ionization-time of flight mass spectrometry (MALDI-TOF MS): Matrix-assisted laser desorption ionization mass spectrometry was conducted by the use of a Bruker Daltonics Ultra flex II MALDI-ToF-MS mass spectrometer, equipped with a nitrogen laser delivering 2 ns laser pulses at 337 nm with positive ion ToF detection performed using an accelerating voltage of 25 kV. Solutions were prepared as follows: trans-2-[3-(4-tert-Butylphenyl)-2-methyl-2-propenylidene] malononitrile (DCTB) as matrix (20 mg/mL), sodium iodide as cationization agent (6 mg/mL) in tetrahydrofuran (20 µl) and sample (10 mg/mL) were mixed, and 0.5 µL of the mixture was applied on the target plate. Spectra recording was made in linear mode calibrating PEG-Me 1900-10000 Da. Gas Chromatography-Flame Ionisation Detection (GC-FID): Gas chromatography-flame ionisation detection (GC-FID) was performed on a Shimadzu GC-2014 equipped with a Shimadzu AO20i autosampler. The carrier gas is hydrogen, supplied by an external hydrogen generator. The GC is fitted with a polar Stabilwax-DA column (30 m length, 0.32 mm ID and 0.25 µm film thickness). The injection volume is 1 µl with a 39 split ratio. The injection temperature is 250oC and the flame temperature is 300oC. The heating profile is 60-200oC at a rate of 10oC/minute and then 200-240oC at 15oC/minute and held for 3 minutes.