Titanium and silver were deposited using an e-beam evaporator (Kurt J Lesker, Model#LAB18). Ag nanopyramid arrays were characterized under a JEOL JSM-7600F scanning electron microscope (SEM). The Au nanostars were characterized using a JEOL JEM-2100F transmission electron microscope (TEM). An Ocean Optics USB 4000 spectrometer was used to acquire the reflection spectra of the fabricated Ag nanopyramid arrays. Raman spectra were acquired using the iRaman plus (Model# BWS465, B&W Tek) with an excitation wavelength of 785 nm.
I raman plus
Manufactured by B&W Tek
Sourced in United States
The I-Raman Plus is a compact, high-performance Raman spectrometer designed for laboratory applications. It provides high-quality Raman spectroscopic data collection and analysis. The device features an integrated design, advanced optics, and user-friendly software for efficient data processing and visualization.
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Lab products found in correlation
Jem 2100f, by JEOL (2 mentions)
Jsm 7600f, by JEOL (1 mentions)
Invia spectrometer, by Renishaw (1 mentions)
T64000, by Horiba (1 mentions)
Alliance 2695 hplc system, by Waters Corporation (1 mentions)
Talos f200x, by Thermo Fisher Scientific (1 mentions)
Nicolet 6700 spectrometer, by Thermo Fisher Scientific (1 mentions)
Uv 2550 spectrometer, by Shimadzu (1 mentions)
Usb4000 spectrometer, by OceanOptics (1 mentions)
Zetasizer nano zs90, by Malvern Panalytical (1 mentions)
Pilatus 100 k detector, by Dectris (1 mentions)
Tga q500, by TA Instruments (1 mentions)
Jem 1200ex 2, by JEOL (1 mentions)
Jms 7001f, by JEOL (1 mentions)
Jem 2100, by Hitachi (1 mentions)
S 4800, by Hitachi (1 mentions)
Jsm 6700f, by JEOL (1 mentions)
Dmax γa, by Rigaku (1 mentions)
28 protocols using i raman plus
1
Characterization of Ag Nanopyramid Arrays
2
Raman Spectroscopy Instrumentation Protocols
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Raman experiments were conducted on four instruments: T64000 Horiba Jobin-Yvon with 670 nm laser for powder sample of 4MBA, Thermo Scientific DXR Raman microscope with 785 laser illumination which was used for SERS droplet experiments, BWTek i-Raman Plus with 785 nm laser for SERS immersion experiments, and Renishaw InVia spectrometer with 785 nm laser source for Raman mapping. Each of these four setups is described in detail:
3
Raman and SERS Spectroscopy for Materials Characterization
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Raman and SERS spectra at 785 nm excitation wavelength were recorded with a JASCO NRS-3300 Raman Spectrometer equipped with a CCD detector (−69°C) using an Olympus UMPLFL ×100 objective, 600 lines/mm grating, 0.2 × 6 mm slit at 2.8 mW power and optical density (OD)2 attenuation. The spectra were recorded in 78–1823 cm−1 frequency range with a resolution of 0.1 cm−1 at 10 s exposure time and 10 accumulations per sample. The calibration was performed using a sharp peak of Si at 521 cm−1. Raman and SERS spectra were recorded also using a Renishaw InVia Reflex Raman confocal spectrometer equipped with the 633 nm and a Leica microscope equipped with a ×100 objective. The signal was collected in the range 100–1600 cm−1 using a filter with edge >100 cm−1. The spectral resolution was 1 cm−1. The acquisition conditions were: 10 s integration time, one accumulation, 1% laser power of 17 mW total power. We also used a portable spectrometer, i-Raman Plus from B&W TEK, equipped with a 532 nm laser line (total power 50 mW) connected via an optical fiber to a BW-TEK optical microscope equipped with a ×20 objective. The acquisition conditions were 10 s integration time, five accumulations, and 10% laser power.
4
SERS Measurements for Molecular Detection
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Some SERS measurements were performed using a 632.8 nm laser with a power of 1 mW and the x‐polarization on a Raman spectroscopy (Renishaw inVia, Renishaw company, UK) equipped with a 50× objective (NA = 0.5) and an integration time of 10 s. Others were performed using a 532 nm laser with a power of 30 mW on a portable Raman spectrometer (i‐Raman plus, B&W TEK INC., USA) equipped with a 40× objective (NA = 0.65) and an integration time of 8 s. For detections of R6G and MEL, the samples were first immersed into R6G aqueous solution and MEL absolute ethanol solution respectively for 12 h, and then dried naturally in air as SERS chips for molecules detections. For detection of Hg ions, the samples were first immersed into BPY absolute ethanol solution with a concentration of 10−5m for 4 h, and then dried naturally in air as SERS chips for Hg ions detection. 35 µL of Hg ion solutions with different concentrations were dropped onto the SERS chips, respectively, then kept for 10 min, and finally dried in air. Likewise, 35 µL of deionized water was prepared with the same procedure as SERS chips for the blank control group. For each sample, measurements on at least five different positions were taken.
5
Characterization of Nanoparticles Using Advanced Analytical Techniques
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The morphologies were observed using a transmission electron microscope (Talos F200X, FEI, Newark, DE, USA) and a scanning electron microscope (Zeiss Merlin, Oberkochen, Germany). A Zetasizer Nano ZS instrument was used to perform the dynamic light scattering measurements (Marlvern 3000, Southborough, UK). UV-vis spectra were recorded using a UV-vis spectrophotometer TU-1901 (Persee Instrument Co., Ltd., Beijing, China) with working wavelengths of 300–700 nm. The SERS measurements were conducted using a Raman spectrometer with a 785-nm laser at room temperature (i-Raman Plus, B&W Tek, Waltham, MA, USA). Each sample was excited at 25 mW over a 5-s acquisition time. All of the Raman spectra were collected between 700 and 1800 cm−1.
A Nicolet iS 5 Frontier transform infrared spectrophotometer (Thermo Fisher Scientific, Waltham, MA, USA) was used to acquire FT-IR spectra with wave numbers ranging between 4000 and 500 cm−1. Liquid chromatography was performed using a Waters Alliance-2695 HPLC system.
A Nicolet iS 5 Frontier transform infrared spectrophotometer (Thermo Fisher Scientific, Waltham, MA, USA) was used to acquire FT-IR spectra with wave numbers ranging between 4000 and 500 cm−1. Liquid chromatography was performed using a Waters Alliance-2695 HPLC system.
6
Comprehensive Nanoparticle Characterization
7
Portable Raman Spectrometer SERS Protocol
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The SERS spectra were acquired by a portable Raman spectrometer (B&W TEK, i-Raman plus, USA) as indicated in Figure 1 a. Before the SERS measurement, the working distance of the portable Raman spectrometer was optimized with a Si wafer ranging from 2 to 8 mm. Figure 1 b illustrates the Raman spectra of different working distances from the Raman probe tip to the Si wafer. The Raman peak of the Si at 518 cm−1 was used to optimize the working distance, which shows that 5-mm is the optimal working distance. This is demonstrated in Figure 1 c. Subsequently, all SERS measurements were conducted at a 5-mm working distance using a 420 mW and 785 nm wavelength excitation laser. The laser spot size is 85 μm in diameter. The SERS spectra were acquired using 10-s integration time in the spectral range from 400 to 1800 cm−1. The SERS spectra was averaged from 20 consecutive measurements.
8
SERS Measurements of Iron Oxide Nanostructures
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SERS measurements were performed using a Raman
portable instrument
(iRaman Plus, BWTEK), using a 785 nm excitation laser and equipped
with a microscope accessory. The amount of iron oxide of all nanostructures
was dosed according to the Fe content, so that the same amount of
particles, despite different Au coverages, was used for all measures.
0.2 mM Fe (4.69 × 109 NPs/mL) of the core@shell structures
was therefore mixed with analytes of study (MBA or CIP). After 15
min, 15 μL of this mixture was then inserted in 1 mm glass capillary
and mounted on a hand-made holder that allows locating the capillary
and the magnet under the microscope of the portable Raman. For measurements
of magnetically accumulated samples, a neodymium magnetic disc, 10
nm in diameter and 4 mm height (380 mT), was placed below the capillary
forming approximately 45° angle, so NPs could accumulate close
to the magnet edge forming a small line instead of a bigger area.
SERS spectra were then measured after 15 min of accumulation. For
measurements of samples in suspension, the same holder without the
magnet was used. All SERS spectra were collected using a 10 objective
magnification (numerical aperture NA = 0.25) with an integration time
of 50 s and a laser power of about 5 mW. All spectra were treated
by correcting the background using MATLAB R2020b software and smoothing
with Origin 8.5 software.
portable instrument
(iRaman Plus, BWTEK), using a 785 nm excitation laser and equipped
with a microscope accessory. The amount of iron oxide of all nanostructures
was dosed according to the Fe content, so that the same amount of
particles, despite different Au coverages, was used for all measures.
0.2 mM Fe (4.69 × 109 NPs/mL) of the core@shell structures
was therefore mixed with analytes of study (MBA or CIP). After 15
min, 15 μL of this mixture was then inserted in 1 mm glass capillary
and mounted on a hand-made holder that allows locating the capillary
and the magnet under the microscope of the portable Raman. For measurements
of magnetically accumulated samples, a neodymium magnetic disc, 10
nm in diameter and 4 mm height (380 mT), was placed below the capillary
forming approximately 45° angle, so NPs could accumulate close
to the magnet edge forming a small line instead of a bigger area.
SERS spectra were then measured after 15 min of accumulation. For
measurements of samples in suspension, the same holder without the
magnet was used. All SERS spectra were collected using a 10 objective
magnification (numerical aperture NA = 0.25) with an integration time
of 50 s and a laser power of about 5 mW. All spectra were treated
by correcting the background using MATLAB R2020b software and smoothing
with Origin 8.5 software.
9
Raman Spectroscopic Zinc Titration
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The spectra were acquired on a BWTEK iRaman Plus portable spectrometer equipped with a 785 nm laser having a maximal power of 420 mW. Excitation and collection were performed in backscattering configuration using a coaxial optical fibre Raman probe. The spectrometer resolution is ~4.5 cm−1. The spectral acquisition range was set to 300–2000 cm−1. The acquisition time was set to 7 s and the laser power to 70%. Each spectrum was averaged over 3 spectral recordings. A titration series consists of 16 spectra acquired as follows. In a 4.5 mL spectrophotometry quartz cuvette, 100 µL of NP stock solution were mixed with 100 µL of XO stock solution using a vortex mixer. Next 10 µL of spermine solution were added and the mixture was rapidly homogenised. Then 1790 µL of ultrapure water having a pH of 7 were added in the cuvette and the mixture further homogenised to give rise to a Zn-free standard sample of which a spectrum was acquired exactly 2 min after the addition of spermine. Subsequently, 10 µL of Zn standard solution were spiked into the cuvette and the mixture was homogenised with a vortex mixer before acquiring its spectrum. In total over a titration series, 15 aliquots of 10 µL of Zn standard solution were mixed in the cuvette to achieve an upper Zn concentration of 2.23 µM. 10 titrations series were conducted.
10
Raman Spectroscopic Analysis of CAR-SCS
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Raman spectrometric analysis was performed for the CAR, mannitol, and optimized CAR-SCS (F8) formulation using I-Raman Plus (B&W TEK, Plainsboro, NJ, USA) fitted with an Ar-Ne instrument. For all the experiments, the excitation wavelength of 785 nm of 35 mW power was utilized, and the integration time was 10 sec.
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