The Fourier Transform Infrared spectrum was performed in the range 400–4000 cm−1 using a PerkinElmer Spectrum 2, USA instruments. NMR spectra were recorded on a Bruker 400 MHz Ultrashield spectrometer at 400 MHz (1H) and 100 MHz (13C) using DMSO-d6 as solvent. The structure of the nanocatalyst was recognized by X-ray diffraction (XRD) measurements (Rigaku Ultima IV, Japan). Field emission-scanning electron microscopy (FE-SEM) images were taken using the FE-SEM TESCAN MIRA3. Transmission electron microscopy (TEM) images were examined using a Philips EM208S apparatus. The energy dispersive X-ray (EDX) spectrum was measured using a TESCAN VEGA model of the instrument. Thermogravimetric analysis (TGA) of the catalyst was performed using a PerkinElmer STA 6000 instrument. The N2 adsorption–desorption isotherm was performed to determine the specific surface areas by Brunauer–Emmett–Teller (BET) (BELSORP miniII, Japan). Vibration Sample Magnetometry (VSM) was studied by the Kavir Magnet VSM.
Ultrashield 400 mhz spectrometer
Manufactured by Bruker
Sourced in Australia, United Kingdom
The Ultrashield 400 MHz spectrometer is a laboratory instrument designed for nuclear magnetic resonance (NMR) spectroscopy. It operates at a frequency of 400 MHz and is capable of analyzing various samples to provide detailed information about their molecular structure and composition.
Automatically generated - may contain errors
Lab products found in correlation
Mira3, by TESCAN (1 mentions)
Em 208, by Philips (1 mentions)
Ultima 4, by Rigaku (1 mentions)
Spectrum 2, by PerkinElmer (1 mentions)
Belsorp miniii, by Microtrac (1 mentions)
Sta 6000, by PerkinElmer (1 mentions)
Em10c 100 kv, by Zeiss (1 mentions)
Sta 409 pc pg, by Netzsch (1 mentions)
Sodium hydroxide (naoh), by Thermo Fisher Scientific (1 mentions)
Acetonitrile, by Thermo Fisher Scientific (1 mentions)
Phenol, by Thermo Fisher Scientific (1 mentions)
Ethyl acetate, by Thermo Fisher Scientific (1 mentions)
Acetone, by Thermo Fisher Scientific (1 mentions)
Dichloromethane, by Thermo Fisher Scientific (1 mentions)
Na2co3, by Thermo Fisher Scientific (1 mentions)
Petroleum ether, by Thermo Fisher Scientific (1 mentions)
K2co3, by Thermo Fisher Scientific (1 mentions)
1 6 dibromohexane, by Thermo Fisher Scientific (1 mentions)
1 bromododecane, by Thermo Fisher Scientific (1 mentions)
1 bromooctane, by Thermo Fisher Scientific (1 mentions)
11 protocols using ultrashield 400 mhz spectrometer
1
Physico-Chemical Characterization of Nanocatalyst
2
Microwave and Ultrasonic Synthesis of Nanoparticles
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All of the chemicals were purchased
from Merck Company and used
without further purification. Microwave radiation was obtained by
a domestic microwave oven (LG, Model: MC-3223CS/00, power: 360 W)
at atmosphere pressure. Ultrasonic generation was carried out by an
ultrasonic instrument (FAPA, Model: UP400) with a standard probe.
The powder X-ray diffraction was performed by a STOE-STADV instrument
(Cu Kα = 1.5418 Å). SEM images were obtained using TESCAN
and ZEISS (Sigma VP-WDS detector) instruments. TEM images were obtained
using a Zeiss-EM10C-100 kV instrument. FT-IR spectra were recorded
with a Shimadzu spectrometer (KBr pellets) from 400 to 4000 cm–1. ICP–OES was obtained by a VISTA-PRO instrument. 1H NMR spectra of products were taken with a Bruker 400 MHz
ultrashield spectrometer using CDCl3 and TMS as the solvent
and internal standard, respectively.
from Merck Company and used
without further purification. Microwave radiation was obtained by
a domestic microwave oven (LG, Model: MC-3223CS/00, power: 360 W)
at atmosphere pressure. Ultrasonic generation was carried out by an
ultrasonic instrument (FAPA, Model: UP400) with a standard probe.
The powder X-ray diffraction was performed by a STOE-STADV instrument
(Cu Kα = 1.5418 Å). SEM images were obtained using TESCAN
and ZEISS (Sigma VP-WDS detector) instruments. TEM images were obtained
using a Zeiss-EM10C-100 kV instrument. FT-IR spectra were recorded
with a Shimadzu spectrometer (KBr pellets) from 400 to 4000 cm–1. ICP–OES was obtained by a VISTA-PRO instrument. 1H NMR spectra of products were taken with a Bruker 400 MHz
ultrashield spectrometer using CDCl3 and TMS as the solvent
and internal standard, respectively.
3
Synthesis and Characterization of Iron-Containing Silica Nanoparticles
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Chemicals such as tetraethyl orthosilicate (TEOS), resorcinol, formaldehyde, ammonia solution (25–28%), FeCl3·6H2O, FeCl2·4H2O, ethanol, HCl, malononitrile, dimedone, and all applied aldehydes were purchased from Merck, Fluka, and Aldrich. All solvents were dried and purified before application in the reactions. Purification of reaction products was performed via TLC on silica gel polygram SILG/UV 254 plates. The melting points were determined by a Barnstead Electrothermal (BI 9300) apparatus. FTIR spectra were obtained using an FT-IR JASC0-680 spectrometer. NMR spectra were obtained with a Bruker 400 MHz Ultrashield spectrometer at 400 MHz (1H) and 100 MHz (13C) using CDC13 or DMSO-d6 as the solvent with TMS as the internal standard. Filed-emission scanning electron microscopy (FESEM) analysis was conducted by a Philips, XL30 emission electron microscope. Thermogravimetric analysis (TGA) was performed by NETZSCH STA 409 PC/PG from room temperature to 800 °C.
4
NMR Spectral Analysis Protocol
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NMR spectra were recorded
on a Bruker 400 MHz Ultrashield spectrometer (400 MHz for 1H NMR). Deuterated solvents used are indicated in each case. Chemical
shifts (δ) are expressed in ppm and are assigned to the residual
peak of the solvent peak; multiplicity is abbreviated as follows:
s, singlet; d, doublet; t, triplet; dt, doublet of triplets; ddt,
doublet of doublets of triplets; td, triplet of doublets; tt, triplet
of triplets; q, quartet; qd, quartet of doublets; and m, multiplet.
on a Bruker 400 MHz Ultrashield spectrometer (400 MHz for 1H NMR). Deuterated solvents used are indicated in each case. Chemical
shifts (δ) are expressed in ppm and are assigned to the residual
peak of the solvent peak; multiplicity is abbreviated as follows:
s, singlet; d, doublet; t, triplet; dt, doublet of triplets; ddt,
doublet of doublets of triplets; td, triplet of doublets; tt, triplet
of triplets; q, quartet; qd, quartet of doublets; and m, multiplet.
5
Synthetic Procedures and Characterization
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N,N-Dimethylethanolamine (99%), ethanol (99.9%), ethyl iodide (98%), 2-propanol (99%), HCl conc. (35%), NaNO2 (99%), phenol (98%) K2CO3 (99.5%), Na2CO3 (99.5%), NaOH (98%), 1-bromododecane (99%), 1-bromoheptane (99%), 1-bromooctane (99%) and 1,6-dibromohexane (99%) were purchased from Acros Organics and used without further purification. Petroleum ether (b.p. 60–90 °C), acetonitrile (99.9%), dichloromethane (99.9%), acetone (99%) and ethyl acetate (99%) were commercial products obtained from Acros Organics. 1H NMR (400 MHz) and 13C NMR (100 MHz) were recorded on a Bruker 400 MHz Ultrashield™ spectrometer. Elemental analysis was performed using a CHN elemental analyser.
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N,N-Dimethylethanolamine (99%), ethanol (99.9%), ethyl iodide (98%), 2-propanol (99%), HCl conc. (35%), NaNO2 (99%), phenol (98%) K2CO3 (99.5%), Na2CO3 (99.5%), NaOH (98%), 1-bromododecane (99%), 1-bromoheptane (99%), 1-bromooctane (99%) and 1,6-dibromohexane (99%) were purchased from Acros Organics and used without further purification. Petroleum ether (b.p. 60–90 °C), acetonitrile (99.9%), dichloromethane (99.9%), acetone (99%) and ethyl acetate (99%) were commercial products obtained from Acros Organics. 1H NMR (400 MHz) and 13C NMR (100 MHz) were recorded on a Bruker 400 MHz Ultrashield™ spectrometer. Elemental analysis was performed using a CHN elemental analyser.
6
Spectroscopic Characterization of Ligand Receptor
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An X-4 digital melting-point device was used to determine the melting point, which was not corrected. Using a quartz cuvette with a 10 mm path length, UV-visible spectra were captured by a Shimadzu UV-vis 1800 spectrophotometer. A Hitachi spectrophotometer (RF-6000) was used to capture the fluorescence spectra. 1H NMR and 13C NMR spectra of the ligand were obtained with a Bruker Ultra Shield 400 MHz spectrometer, and the chemical shifts are given in ppm in relation to TMS. With a waters mass spectrometer, ESI-mass spectra were captured using a mixed solvent of HPLC methanol and triple-distilled water. All of the chemicals and metal salts were bought from Merck, and sodium was used as the counter ion for anions and nitrate for metals. In triple-distilled water, solutions of the receptor L (1 × 10−5 M) and metal salts (1 × 10−4 M) were made.
7
Polymer Analysis via GPC and NMR Spectroscopy
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Gel Permeation Chromatography analyses of the polymers were carried out on a Shimadzu modular system comprised of an SIL-20AD auto-injector, a PL 5.0-mm bead-size guard column (50 x 7.8 mm) followed by four 300 x 7.8 mm linear columns (500, 104, 103, and 105 Å pore size) using N,Ndimethylacetamide [DMAC; w/v LiBr, 0.05% 2, 7-di-Butyl-4-methylphenol (BHT)] at 50°C as the eluent (flow rate = 1 mL/min). An RID-20A differential refractive-index detector was used. Samples were filtered through 0.45 μm PTFE filters before injection. Calibration was performed with narrowpolydispersity polystyrene standards ranging from 104 to 106 000 g/mol. Structures of synthesised compounds were analysed by 1 H NMR spectroscopy using a Bruker UltraShield 400 MHz spectrometer (Bruker Daltronics Inc., NSW, Australia) running Topspin, version 1.3. All spectra were recorded in CDCl 3. DLS measurements of the stars in MilliQ water (1mg/mL) were carried out using a Malvern Zetasizer Nano Series running DTS software (laser, 4 mW, λ = 633 nm; angle 173°). We caution that the GPC molecular weight results are not given as absolute values (because of limitations with calibration), but rather estimateswherever possible we compared NMR and GPC results.
8
Synthesis of Phosphonate-Containing Peptides
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All amines, 2-chloracetamide, Boc anhydride, trifluoroacetic acid, hydrochloric acid 37% were purchased from Merck Poland. Methanol (MeOH), cyclohexane, aqueous ammonia 25%, isopropyl alcohol (purchased from Avantor Performance Materials Poland) were analytical grade and used without further purification. Ethyl acetate (EtOAc), chloroform (CHL) and dichloromethane (DCM) were refluxed over P2O5 and distilled. Reaction progress was monitored by thin-layer chromatography on Merck 60 silica plates using methanol/dichloromethane mixture as eluent. The spots were visualized by chlorine/o-tolidine reaction. Purification of synthesized compounds was performed using silica gel 60 (0.040–0.063 mm) from Merck. The NMR analyses were performed on a Bruker Ultrashield 400 MHz spectrometer operating at 400 MHz (1H), 162 MHz (31P) and 101 MHz (13C). The samples were dissolved in d6-DMSO (99.8 at% D) containing 0.03% TMS or D2O (99.9 at% D) and measured at 297 K. High-resolution mass spectra (HRMS) were recorded on a Waters LCT Premier XE mass spectrometer equipped with an ESI source in the positive ion mode (Waters, Milford, MA, USA). The preparation protocols of Ac-PO(OEt)2, Ac-ΔAla-PO(OEt)2 (1), Z-ΔAla-PO(OEt)2 (3) are described elsewhere.19,41,42 (link) The detailed preparation of Boc-Gly-ΔAla-PO(OEt)2 (5) is presented in a recently published paper.43 (link)
9
Synthesis and Characterization of Bombesin Analogs
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[Asn3, Lys6, Thr10, Phe13]3–14-bombesin and [Asn3, Lys6, Phe13]3–14-bombesin were synthesized by using the solid-phase peptide synthesis technique through an automated solid phase 2-channel peptide synthesizer (Tribute®, Gyros Protein Technologies, United States) along with Rink Amide MBHA resin (100–200 mesh) and Fmoc chemistry. An optimized cleavage cocktail was developed for removing the peptides from resin and side chain-protecting groups as described elsewhere (Marquez et al., 2000 (link)). The synthetic peptides were lyophilized instantly after being washed using cold diethyl ether. Finally, each synthetic peptide was purified using RP-HPLC (Phenomenex C-5 column, 0.46 cm × 25 cm). The collected fractions were reserved and analyzed by LCQ™-Fleet electrospray ion-trap mass spectrometry (Thermo Fisher Scientific, San Francisco, CA, United States) and RP-HPLC to verify the molecular masses and the purity (>90 %) of the target peptides (Supplementary Figures S1, S2 ). The HPLC fractions containing the purified peptide of interest were lyophilized and subsequently subjected to nuclear magnetic resonance spectroscopy (NMR). The 1H-NMR spectrum (Supplementary Figure S3 ) of each pure peptide (6 mM in deuterium oxide) was recorded on a Bruker Ultrashield 400 MHz spectrometer (Bruker, Coventry, UK) at 25°C.
10
Biotransformation Scale-up and Characterization
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Eight repetitions of the same experiment were performed in 1000-mL Erlenmeyer flasks containing 250 mL of the cultures to scale-up the biotransformation process. After 14 days of incubation, the mixtures were extracted with ethyl acetate (each repetition, 3 × 80 mL), dried over anhydrous MgSO4 and the solvent was removed. The products of transformation were separated by preparative thin layer chromatography (PTLC) using a CAMAG system and silica gel glass plates without a fluorescent indicator and were extracted with ethyl acetate, which was then evaporated under a stream of nitrogen. Then, the structures of the isolated products were determined and confirmed by mass spectrometry (MS) and nuclear magnetic resonance techniques: 1H NMR and 13C NMR, including COSY and HSQC correlation experiments. The NMR spectra were measured in DMSO-d6 using a Bruker UltraShield 400 MHz spectrometer with tetramethylsilane (TMS) as an internal reference.
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