br Experimental design materials and methods br Acknowledgme

Experimental design, materials and methods
Acknowledgments This work was supported by Grants #16791 (EA, AK, CC, SS) and #16442 (JJL, BC), thesis fellowship (EA) and Post-doctoral fellowship (JJL) from the Association Française Contre les Myopathies – Telethon. We thank the imaging platform of Université de Poitiers “ImageUP” for its technical assistance.
Data
Experimental design, materials and methods
Data analysis The data assembled is analyzed in Figs. 2–4.
Value of the data
Data The FTIR of the fresh and used SOB particles at wave numbers from 500 to 4000cm−1 are shown in Fig. 1. The X-ray photoelectron spectroscopy (XPS) of fresh SOB and Cd2+, Cu2+, and Hg2+ loaded SOB is also depicted in Fig. 2. Data of this article including, kinetics, isotherms, and thermodynamic analysis was calculated using models provided in Table 1. The data of kinetics and isotherms for biosorption of heavy metals (cadmium, copper, and mercury ions) onto SOB were first depicted in Fig. 3 and 4. Through Fig. 3 and 4 and Table 1, the kinetics, isotherms, and thermodynamic parameters were calculated and summarized in Tables 2 and 3.
Experimental design, materials and methods
Acknowledgments
Specifications Table
Data This paper deals about the identification of the products from the chemical reaction between N-Cbz-3-aminopropanal (β-CHO) and tert-butyl hydroperoxide (t-BuOOH) or H2O2. It describes the preparation of the samples prior the NMR measurements, and the concerted analysis of the NMR spectra and 2D correlations.
Experimental design, materials and methods Three preparative reactions were carried out in order to obtain enough amounts of by-products (compounds 6–8, Scheme 1) for further analyses. β-CHO (17mM, maximum solubility) was dissolved in 10mL water. Selected peroxide was added to the reaction medium and left in incubation for 24h. For order RGFP966 6 preparation, 250mM t-BuOOH was employed (ca 50% yield); for 7, 600mM H2O2 (ca 65% yield); for 8, 72mM H2O2 (ca 99% yield). All reactions were performed at 25°C, 1000rpm of MultiTherm™ orbital stirring. Compounds 6–7 were carefully filtered prior the analysis to eliminate impurities. Compound 8 was isolated by filtration and cautiously dried at 35°C. For the identification of the product from reaction between β-CHO and t-BuOOH, the reaction medium (containing product 6) was directly analyzed. 200µL of D2O (99.96% D), containing 0.3% of TSP (trimethylsilyl propanoic acid), were added to a 400µL aliquot of the aqueous crude and the dissolution was transferred to a 5-mm-diameter NMR tube. To analyze the reaction intermediate in the β-CHO-H2O2 reaction (compound 7), 200µL of D2O (99.96% D), containing 0.3% of TSP, were added to a 400µL aliquot of the aqueous sample of the reaction crude. The solution was transferred to a 5-mm-diameter NMR tube. For compound 8 identification, the dried reaction by-product (20.2mg) of the oxidation reaction between β-CHO and H2O2 was dissolved in 600µL of CDCl3 (99.96% D). 1H (600.13MHz) and 13C (150.13MHz) NMR spectra were recorded at 298.0K of temperature on a Bruker Avance II 600 nuclear magnetic resonance spectrometer (Bruker Biospin, Rheinstetten, Germany) equipped with a 5mm TBI probe with Z-gradients and a TCU (temperature control unit). Initially, 1D 1H NMR spectra of all samples were acquired. For that, a standard 90° pulse sequence, with an acquisition time of 1.71s and a relaxation delay of 2s was recorded. Data were collected into 32K computer data points, with a spectral width of 9590Hz and as the sum of 1024 transients. The resulting free induction decays (FIDs) were Fourier transformed manually phased and baseline corrected. In the case of samples containing H2O, the peak of the protonated water was suppressed by the standard presaturation of the signal. The structural characterization of compounds was carried out with the aid of 2D NMR experiments, such as COSY (Correlated Spectroscopy), HSQC (Heteronuclear Single Quantum Correlation), HMBC (Heteronuclear Multiple Bond Correlation), NOESY (Nuclear Overhauser and Exchange Spectroscopy), DOSY (Diffusion Spectroscopy) and 1D selective NOESY experiments performed under standard conditions. When required, solvent suppression techniques were applied. Spectra of CDCl3 samples were calibrated using the residual solvent signal (7.26ppm for 1H and 77.16 for 13C) and spectra of aqueous samples using TSP as internal reference.