Screening of conditions controlling spectrophotometric sequential injection analysis

Background  

Despite its potential benefits over univariate, chemometrics is rarely utilized for optimizing sequential injection analysis (SIA) methods. Specifically, in previous vis-spectrophotometric SIA methods, chemometrically optimized conditions were confined within flow rate and reagent concentrations while other conditions were ignored.     

On Ordered Division Rings

Prestel introduced a generalization of the notion of an ordering of a field, which is called a semiordering. Prestel's axioms for a semiordered field differ from the usual (Artin-Schreier) postulates in requiring only the closedness of the domain of positivity under x xa ² for nonzero a, instead of requiring that positive elements have a positive product. In this work, this type of ordering is studied in the case of a division ring. It is shown that it actually behaves the same as in the commutative case. Further, it is shown that the bounded subring associated with that ordering is a valuation ring which is preserved under conjugation, so one can associate a natural valuation to a semiordering.     

Quantitative and physical evaluation of patchouli essential oils obtained from different sources of Pogostemon cablin

Patchouli essential oil can be obtained from fresh, dried and fermented plant material. It is a highly valuable product in the fragrance industry and its quality changes depending upon raw material age and oil storage. In this work, patchouli essential oils derived from different treatments have been subjected to GC-FID quantitative analysis using an internal standard (ISTD) method with response factors (RF). Samples were obtained from i) fresh plants; ii) hydrodistillation of one year mature and fermented plants; iii) hydrodistillation of one year mature plants; iv) commercial products from Indonesia and Malaysia. Linear Retention Indices (LRI) for both polar and non-polar GC-MS analyses were also measured as a tool for qualitative analysis towards a homologous series of C7-C30 n-alkanes. The results obtained confirmed that, in all samples, patchouli alcohol was the main volatile constituent, with higher amount in lab-scale produced oils, compared with commercial samples. Other major compounds, in lab oils and commercial samples respectively, were: delta-guaiene, alpha-guaiene, pogostol, seychellene and alpha-patchoulene. Another 36 compounds were also found.     

Comparison theorem for Brownian multidimensional BSDEs via jump processes

In this Note, we provide an original proof of the comparison theorem for multidimensional Brownian BSDEs in the case where at each line k the generator depends on the matrix variable Z only through its row k.     

Humic-makeup approach for simultaneous functionalization of polyacrylonitrile nanofibers during electrospinning process,and dye adsorption study

A useful methodology is represented to functionalize polyacrylonitrile nanofibers by using humic acid as a makeup agent in electrospinning process. Both morphology and surface chemistry of polyacrylonitrile nanofiber mats were understood to be influenced by incorporation of humic acid into the structure. Physicochemical changes were evidenced by Fourier transform infrared spectroscopy, scanning electron microscope, and surface charge measurements. Unlike some anionic dyes (i.e., methyl orange, methyl red, and Congo red), there was an enhancement in crystal violet (a cationic dye) adsorption after incorporation of humic acid. The Langmuir model fitted well to crystal violet data, and monolayer adsorption capacity was calculated as 81.6 mg/g (r² = 0.998).     

The usage of computer-aided cooling curve thermal analysis to optimise eutectic refiner and modifier in Al–Si alloys

Bismuth, antimony and strontium concentrations were optimised to alter the eutectic Al?CSi phase in a commercial Al?CSi?CCu?CMg alloy by way of computer-aided cooling curve thermal analysis. The results show that the eutectic growth temperature shifted to lower temperatures for all three inoculants. However, addition of Sr resulted in more depression of growth temperature compared with Bi and Sb. No further significant changes were observed with increasing the concentrations to more than 1, 0.5 and 0.04?wt% of Bi, Sb and Sr, respectively. The recalescence of these concentrations, meanwhile, showed a significant increase of magnitude. A good correlation was found between the results of thermal and microstructural analysis. For Bi and Sb, the eutectic depression temperature can be used as an individual criterion to gauge optimal levels of content in the refinement of Si, whereas for Sr, both depression temperature and recalescence magnitude must be considered. Based on the observed depression in eutectic growth temperature and recalescence, it can be concluded that the optimal concentrations to refine the eutectic Al?CSi phase with Bi and Sb and to modify it with Sr at the given solidification conditions were 1, 0.5 and 0.04?wt%, respectively.     

Inter- and intramolecular mechanisms for chlorine rearrangements in trimethyl-substituted N-chlorohydantoins

The antimicrobial compounds 1-chloro-3,5,5-trimethylhydantoin and 3-chloro-1,5,5-trimethylhydantoin (1 and 2, respectively) have been synthesized and examined via a joint experimental and computational study. The measured rate of loss of oxidative chlorine in the absence and presence of exposure to UVA irradiation determined 2 to be less stable than 1. An interesting migration reaction was observed during UVA irradiation that featured the production of chlorine rearrangement and dechlorinated compounds. Two novel hydrogen atom transfer reaction (HATR) mechanisms have been proposed: (1) an intramolecular process in which a hydrogen atom undergoes a series of sigmatropic shifts, and (2) an intermolecular pathway in which a radical abstracts a hydrogen atom from a neighboring molecule. Density functional theory (DFT) calculations at the UB3LYP/6-311G++(2d,p) theory level have been employed to elucidate the preferred reaction pathway. Both proposed HATR mechanisms predicted 2 to possess a lower free energy of activation, ΔG(?), relative to 1 in accordance with the experimental stability measurements. However, the intermolecular route had an overall lower absolute ΔG(?) and was more consistent with measured product ratios in solution. The intermolecular reaction pathway, unlike the intramolecular route, also predicted the lack of formation of a migration product featuring a Cl covalently bonded to a methylene group at the 5-position of the hydantoin moiety, which was verified by NMR experiments.     

Separation and determination of selenium(IV) and molybdenum(VI) in mixtures by selective precipitation with potassium thiocarbonate

A simple method for the separation and determination of selenium(IV) and molybdenum(VI) in mixtures, based on selective precipitation with potassium thiocarbonate, has been developed. The procedure allows quantitative determination of 10-100 mg of selenium or 10-70 mg of molybdenum at pH 0.5-1.0. No interference by a wide range of other metal ions is observed.     

Assessment of heavy metals pollution in Sudanese harbours along the Red Sea Coast

The levels of some heavy metals in sediments of two harbours along the Sudanese Coast of the Red Sea were examined and reported for the first time. A total of thirty-six surface sediment samples were collected from Port-Sudan and Sawakin harbours. Part of each sample was partitioned into five fractions with grain-size ranges of 1000–500, 500–250, 250–125, 125–63 and less than 63 μm. The Mn, Fe, Ni, Cu, Zn and Pb concentration in bulk samples and sub-samples were determined by atomic absorption spectrophotometry. The spatial distribution pattern of heavy metal content of crustal origin in the sediments is more uniform in Port-Sudan harbour than in Sawakin harbour. The granulometric normalization revealed that some sites in Port-Sudan harbour and one site in Sawakin harbour have been exposed to different levels of heavy metal contamination, which probably originated from ships, industrial and domestic activities.     

Preparation,Optimisation, and In Vitro Evaluation of [18F]AlF-NOTA-Pamidronic Acid for Bone Imaging PET

[¹⁸F]sodium fluoride ([¹⁸F]NaF) is recognised to be superior to [⁹⁹mTc]-methyl diphosphate ([^99mTc]Tc-MDP) and 2-deoxy-2-[¹⁸F]fluoro-D-glucose ([¹⁸F]FDG) in bone imaging. However, there is concern that [¹⁸F]NaF uptake is not cancer-specific, leading to a higher number of false-positive interpretations. Therefore, in this work, [¹⁸F]AlF-NOTA-pamidronic acid was prepared, optimised, and tested for its in vitro uptake. NOTA-pamidronic acid was prepared by an N-Hydroxysuccinimide (NHS) ester strategy and validated by liquid chromatography-mass spectrometry analysis (LC-MS/MS). Radiolabeling of [¹⁸F]AlF-NOTA-pamidronic acid was optimised, and it was ensured that all quality control analysis requirements for the radiopharmaceuticals were met prior to the in vitro cell uptake studies. NOTA-pamidronic acid was successfully prepared and radiolabeled with ¹⁸F. The radiolabel was prepared in a 1:1 molar ratio of aluminium chloride (AlCl₃) to NOTA-pamidronic acid and heated at 100 °C for 15 min in the presence of 50% ethanol (v/v), which proved to be optimal. The preliminary in vitro results of the binding of the hydroxyapatite showed that [¹⁸F]AlF-NOTA-pamidronic acid was as sensitive as [¹⁸F]sodium fluoride ([¹⁸F]NaF). Normal human osteoblast cell lines (hFOB 1.19) and human osteosarcoma cell lines (Saos-2) were used for the in vitro cellular uptake studies. It was found that [¹⁸F]NaF was higher in both cell lines, but [¹⁸F]AlF-NOTA-pamidronic acid showed promising cellular uptake in Saos-2. The preliminary results suggest that further preclinical studies of [¹⁸F]AlF-NOTA-pamidronic acid are needed before it is transferred to clinical research.