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7 protocols using ft ir tensor 27 spectrometer

1

Spectroscopic Analysis of Natural Compounds

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Optical rotations were measured with a Jasco P-1020 polarimeter. UV spectra were obtained using a Shimadzu UV-2401 PC spectrophotometer. IR spectra were obtained with a Bruker FT-IR Tensor 27 spectrometer using KBr pellets. 1D and 2D NMR spectra in CDCl3 were recorded on an AVANCE III 500 and 600 MHz spectrometers. HREIMS spectra were recorded on an Agilent 1290 UPLC/6540 Q-TOF mass spectrometer. ECD spectra were recorded on an Applied Photophysics spectropolarimeter. Column chromatography (CC) was performed on silica gel (200–300 mesh, Qingdao Marine Chemical Ltd., Qingdao, China) and RP-18 gel (20–45 µm, Fuji Silysia Chemical Ltd., Tokyo, Japan). Semi-preparative HPLC were performed on an Agilent 1260 instrument with a ZORBAX SB-C18 column (9.4 × 250 mm, 5 μm) or an Agilent 1100 instrument with a CHIRALPAK IC column (10 × 250 mm, 5 μm). TLC (GF254, Qingdao Haiyang Chemical Co., Ltd. Qingdao, China or RP-18 F254, Merck, Darmstadt, Germany) was used to monitor the fractions. Spots were detected by a UV light (254 nm) and followed by dipping in 10% H2SO4 in EtOH and heating at 110 °C.
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2

Comprehensive Analytical Characterization

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Optical rotations were performed on a P-1020 polarimeter. IR spectra were measured on a Bruker FT-IR Tensor 27 spectrometer with KBr pellets. UV spectra were obtained on Shimadzu UV-2401A spectrometer. 1D and 2D-NMR spectra were recorded on Bruker AV-600 MHz spectrometer. Coupling constants were expressed in Hertz and chemical shifts were given on a ppm scale with tetramethylsilane as an internal standard. HRESIMS were recorded on an API QSTAR Pulsar 1 spectrometer. Column chromatography (CC) was performed on silica gel (200–300 mesh, Qingdao Marine Chemical Ltd., Qingdao, People’s Republic of China), Sephadex LH-20 (Pharmacia Fine Chemical Co., Ltd., Sweden), and MCI-gel CHP 20P (75–100 μm, Mitsubishi Chemical Co., Ltd). Thin-layer chromatography (TLC) was carried out on pre-coated silica gel plates (Qingdao Marine Chemical Co., Ltd.) with CHCl3/MeOH (15:1, 4:1, v/v) as developing solvents and spots were visualized by Dragendorff’s reagent. High performance liquid chromatography (HPLC) was performed using Waters 600 pump with semi-preparative C18 columns (150 × 9.4).
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3

Comprehensive Spectroscopic Analysis of Compounds

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Optical rotations were performed on a JASCO P-1020 polarimeter. IR spectra were measured on a Bruker FT-IR Tensor 27 spectrometer with KBr pellets. UV spectra were obtained on Shimadzu UV-2401A spectrometer. 1D-NMR and 2D-NMR spectra were recorded on an AV-600 MHz or a Bruker DRX-400 MHz spectrometer. Coupling constants were expressed in Hz and chemical shifts were given on a ppm scale with tetramethylsilane as internal standard. HRESIMS were recorded on an API QSTAR Pulsar 1 spectrometer. CD spectra were obtained on a JASCO 810 spectrometer. Column chromatography (CC) was performed on silica gel (200–300 mesh, Qingdao Marine Chemical Ltd., Qingdao, People’s Republic of China), Sephadex LH-20 (Pharmacia Fine Chemical Co., Ltd., Sweden), and MCI-gel CHP 20P (75–100 μm, Mitsubishi Chemical Co., Ltd). Thin-layer chromatography (TLC) was carried out on silica gel H-precoated plates (Qingdao Haiyang Chemical Co., Ltd.) with CHCl3/MeOH (9:1, 4:1, v/v) as developing solvents and spots were visualized by Dragendorff’s reagent. High performance liquid chromatography (HPLC) was performed using waters 600 equipment with semi-preparative and preparative C18 columns (150 × 9.4 and 250 × 21.2 mm, respectively).
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4

FTIR Analysis of Lyophilized ASC and PSC

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The lyophilized ASC and PSC samples (1 mg) were mixed with 100 mg dried potassium bromide and pressed into pellets under dry conditions. The FTIR spectra of ASC and PSC were then determined using an FTIR Tensor 27 spectrometer (Bruker, Rheinstetten, Germany) [22 (link),37 (link)]. The spectra were recorded at wavelengths ranging from 4000 cm−1 to 500 cm−1 at a resolution of 1 cm−1 for a single scan.
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5

Structural and Rheological Characterization of PNIPAAm-Based Hydrogels

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Structural characterization of the synthesized PNIPAAm-COOH, CS-g-PNIPAAm, and hydrogels was carried out by FT-IR Tensor 27 spectrometer (Bruker Optik GmbH, Ettlingen,
Germany) in the range of 4000 to 400 cm−1 using KBr powder. Scanning electron microscopy (SEM) was applied to evaluate the structure and morphology of the prepared hydrogels by TESCANMIRA3 electron microscope (FE-SEM, MIRA3 FEG-SEM Tescan, Czech). For the SEM analysis, freeze-dried samples were first coated with a gold layer. The storage (G′) and loss modulus (G″) of the prepared hydrogels were measured with the frequency dependence in the range from 0.1 to 10 Hz via a parallel plate rheometer (Anton Paar, MCR-301, Austria). The samples were placed between parallel plates (25 mm in diameter) with a gap distance of 400 μm and conductions were performed at 37°C at 0.2 % strain and angular frequency of 1 rad s−1.
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6

FTIR Analysis of Biofilm Composition

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Biofilms grown for 24 h were harvested by centrifugation at 10,000×g for 10 min and suspended in 100 µL PBS. 30 µl of the biofilm suspension was transferred to a ZnSe optical plate and dried for 40 min at 40 °C. FTIR spectra were acquired using a FTIR Tensor 27 spectrometer coupled to the microplate adapter HTS-XT (Bruker Optics GmbH). The infrared spectra were recorded in transmission mode in the spectral range between 4000 and 500 cm−1 using the spectrometer parameter as described elsewhere59 (link). For principal component analysis (PCA), vector-normalized, second derivative spectra were computed and scores/loading plots were performed at the spectral region for protein constituents (1800–1500 cm−1) by using the Unscrambler X software (Camo analytics, v11.0; https://www.camo.com/spectroscopy/44 (link).
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7

Analytical Characterization of Compounds

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FT-IR spectra were obtained on a FT-IR Tensor 27 spectrometer (Bruker). NMR spectra were recorded on a Bruker AM400 FTNMR spectrometer using TMS as an internal standard. ESI-MS and HRESI-MS were performed on a MicrOTOF-Q mass spectrometer (Bruker). All measurements were made at the Department of Chemistry (Faculty of science and medicine, University of Fribourg, Switzerland). TLC was performed on silica gel 60 F 254 (1.05554.0001, Merck, Darmstadt, Germany) and RP-18 F 254S plates (1.15685.0001, Merck, Darmstadt, Germany). Column chromatography was performed on silica gel (240-430 mesh, Merck, Darmstadt, Germany).
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