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1. Mid-infrared Doppler-free saturation absorption spectroscopy of the Q branch of CH ₄ ν ₃ = 1 band using a rapid-scanning continuous-wave optical parametric oscillator

   https://doi.org/10.1364/OL.530567  

   Shah_Riyadh, S M; Telfah, Hamzeh; Jones, Ian W; Bersson, Jonathan S; Cheng, Cun-Feng; Hu, Shui-Ming; Foote, David B; Liu, Jinjun (January 2024, Optics Letters)

   We have developed a mid-infrared Doppler-free saturation absorption spectroscopy apparatus that employs a commercial continuous-wave optical parametric oscillator (CW OPO), complemented by a home-built automation and wavelength scanning system. Here, we report a comprehensive spectral scan of the Q branch transitions of theν₃= 1 band of methane (CH₄) with an average linewidth (FWHM) of 4.5 MHz. The absolute frequency calibration was achieved using previously reported transition frequencies determined using optical frequency combs, while a Fabry–Perot etalon was used for the relative frequency calibration. We report 15 transitions with improved accuracies of 1.13 MHz (3.76 × 10⁻⁵cm⁻¹). 

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2. Autocalibration based on dilution of a single concentrated standard is used for the determination of silicate in sea water by the modified molybdenum blue method

   https://doi.org/10.1016/j.talanta.2024.126183  

   Hatta, M; Ruzicka, J; Measures, C; Davis, M (August 2024, Talanta)

   The silicate (Si) molybdenum blue method was modified by combining oxalate and ascorbic acid into a single reagent and was used for determining Si in sea water samples. The first step of this automated assay protocol was designed to perform either a calibration by a single Si standard prepared in deionized (DI) water, or to dilute samples in the range of 0–160 μM Si to fit into 0–20 μM Si calibration range using a 20 cm flow cell. By designing the assay protocol to function in batch mode, the influence of salinity on calibration was eliminated, thus making the method suitable for analysis of samples collected in the open ocean, coastal areas, or rivers. Reproducibility and accuracy of this method were evaluated by analysis of certified sea water reference materials. Phosphate (P) does not interfere significantly if the Si:P ratio is 4:1 or larger. The limit of detection was 514 nM Si, r.s.d. 2.1 %, sampling frequency 40 s/h, reagent consumption 700 μL/sample, and using deionized water as the carrier solution. 

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3. Spatial Heterodyne Raman Spectrometer (SHRS) for In Situ Chemical Sensing Using Sapphire and Silica Optical Fiber Raman Probes

   https://doi.org/10.1177/0003702819868237  

   Ottaway, Joshua M.; Allen, Ashley; Waldron, Abigail; Paul, Phillip H.; Angel, S. Michael; Carter, J. Chance (July 2019, Applied Spectroscopy)

   null (Ed.)

   A spatial heterodyne Raman spectrometer (SHRS), constructed using a modular optical cage and lens tube system, is described for use with a commercial silica and a custom single-crystal (SC) sapphire fiber Raman probe. The utility of these fiber-coupled SHRS chemical sensors is demonstrated using 532 nm laser excitation for acquiring Raman measurements of solid (sulfur) and liquid (cyclohexane) Raman standards as well as real-world, plastic-bonded explosives (PBX) comprising 1,3,5- triamino- 2,4,6- trinitrobenzene (TATB) and octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX) energetic materials. The SHRS is a fixed grating-based dispersive interferometer equipped with an array detector. Each Raman spectrum was extracted from its corresponding fringe image (i.e., interferogram) using a Fourier transform method. Raman measurements were acquired with the SHRS Littrow wavelength set at the laser excitation wavelength over a spectral range of ∼1750 cm −1 with a spectral resolution of ∼8 cm −1 for sapphire and ∼10 cm −1 for silica fiber probes. The large aperture of the SHRS allows much larger fiber diameters to be used without degrading spectral resolution as demonstrated with the larger sapphire collection fiber diameter (330 μm) compared to the silica fiber (100 μm). Unlike the dual silica fiber Raman probe, the dual sapphire fiber Raman probe did not include filtering at the fiber probe tip nearest the sample. Even so, SC sapphire fiber probe measurements produced less background than silica fibers allowing Raman measurements as close as ∼85 cm −1 to the excitation laser. Despite the short lengths of sapphire fiber used to construct the sapphire probe, well-defined, sharp sapphire Raman bands at 420, 580, and 750 cm −1 were observed in the SHRS spectra of cyclohexane and the highly fluorescent HMX-based PBX. SHRS measurements of the latter produced low background interference in the extracted Raman spectrum because the broad band fluorescence (i.e., a direct current, or DC, component) does not contribute to the interferogram intensity (i.e., the alternating current, or AC, component). SHRS spectral resolution, throughput, and signal-to-noise ratio are also discussed along with the merits of using sapphire Raman bands as internal performance references and as internal wavelength calibration standards in Raman measurements. 

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4. Ultraviolet absorption spectra of acrylic acid and its conjugate base, acrylate, in aqueous solution

   https://doi.org/10.1016/j.jphotochem.2023.115371  

   Xue, Lei; Kieber, David J. (April 2024, Journal of Photochemistry and Photobiology A: Chemistry)

   Acrylic acid is an important compound widely used in industry with multiple commercial applications, and it is also a key intermediate in the marine organosulfur cycle. However, the fundamental ultraviolet (UV) absorption spectrum of acrylic acid or its conjugate base, acrylate (pKa = 4.25 at 20 oC) have not been determined in water. In this paper, we determined the absorption spectrum of acrylate in aqueous solution at pH 7.2 and 20 oC between 207 and 400 nm. The molar absorptivity decreased rapidly from 3958 M‒1 cm‒1 at 207 nm to a non-detectable value at wavelengths greater than 330 nm, with weak absorption at wavelengths greater than 290 nm (e.g., ɛ290nm 2.7 M‒1 cm‒1). No discernable absorption bands were observed in the absorption spectrum. Excellent agreement was observed when comparing absorption spectra obtained (1) with two different spectrophotometers and (2) with standards prepared from either newly purchased sodium acrylate or from the base hydrolysis of dimethylsulfoniopropionate. Wavelength-dependent molar absorptivities were constant at pH 7.2 over a range of acrylate concentrations from 25 to 135 μM. The absorption spectrum red shifted when the solution pH increased from 2.8 to 8.2, with an isosbestic point observed at 214 nm indicating two exchangeable species in solution. Our study provides the first detailed UV absorption spectra of acrylic acid and acrylate in aqueous solution, with important implications regarding the detection and study of these compounds in environmental settings and commercial applications. 

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5. Quantitative analysis of Δ9-tetrahydrocannabinol (Δ9-THC) in cannabis plants using the Fast Blue BB (FBBB) and 4-aminophenol (4-AP) colorimetric tests

   https://doi.org/10.1016/j.talo.2024.100287  

   Valdes, Nicole B; Gorziza, Roberta; Almirall, José R (August 2024, Talanta Open)

   Banks, Craig (Ed.)

   The Fast Blue BB (FBBB) and 4-aminophenol (4-AP) colorimetric tests have been reportedly used for the qualitative determination of Δ9-THC in plants and for the differentiation between marijuana and hemp-type cannabis. We report the miniaturization of the FBBB colorimetric reaction on a silicone treated filter paper substrate and the analytical figures of merit for a quantitative determination of Δ9-THC for the first time. The reaction between Δ9-THC and FBBB forms a red chromophore that fluoresces when irradiated with visible (480 nm) or UV (365 nm) light, providing a 3-fold increase in sensitivity. Portable instruments are introduced for the objective color determination for both tests and for the fluorescence reading of the THC + FBBB complex. We report a fluorescence signal with Δ9-THC, Δ8-THC, and CBN. The limit of detection (LOD) was determined to be 1.6 ng/μL with precision ~12 % RSD for standard Δ9-THC solutions ranging between 5 and 20 ng/μL. The linear dynamic range for this test is reported between 1.6 ng/μL and 20 ng/μL for the portable fluorescence detector. The miniaturization of both colorimetric tests and the increased sensitivity of the FBBB test using fluorescence analysis, coupled to portable instruments allows for limited quantitative analysis of cannabis plants in the field. 

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