Boron Isotope Effect in Liquid Chromatography with Boron-specific Resins as Packing Material

1997 ◽  
Vol 52 (11) ◽  
pp. 821-827
Author(s):  
Takao Oi ◽  
Hirotsugu Takeuchi ◽  
Akiko Sakurai ◽  
Yoshifumi Taguchi ◽  
Morikazu Hosoe

Abstract Boron isotope separation by liquid chromatography using boron specific resins with N-methyl glucamine as the functional group was performed. The single-stage separation factor, S, is generally dependent on the resin in the sequence S (free base form resin) > S (F- form resin) >S (Cl- form resin) ≧S (Br- form resin) for given experimental conditions. This sequence is the same as that of the pH value expected in the resin phase and reasonably understandable by assuming in addition to the predominant four-coordinate species a three-coordinate boron species in the resin phase whose relative abundance increases with decreasing pH. Supporting evidence for three-coordinate species was obtained by 1: B NMR measurements of boric acid-glycerol and boric acid-1,3-propane-diol solutions.

2008 ◽  
Vol 1201 (1) ◽  
pp. 48-53 ◽  
Author(s):  
Masaaki Musashi ◽  
Takao Oi ◽  
Motoyuki Matsuo ◽  
Masao Nomura

2020 ◽  
Vol 16 (7) ◽  
pp. 905-913
Author(s):  
Youyuan Peng ◽  
Qingshan Miao

Background: L-Ascorbic acid (AA) is a kind of water soluble vitamin, which is mainly present in fruits, vegetables and biological fluids. As a low cost antioxidant and effective scavenger of free radicals, AA may help to prevent diseases such as cancer and Parkinson’s disease. Owing to its role in the biological metabolism, AA has also been utilized for the therapy of mental illness, common cold and for improving the immunity. Therefore, it is very necessary and urgent to develop a simple, rapid and selective strategy for the detection of AA in various samples. Methods: The molecularly imprinted poly(o-phenylenediamine) (PoPD) film was prepared for the analysis of L-ascorbic acid (AA) on gold nanoparticles (AuNPs) - multiwalled carbon nanotubes (MWCNTs) modified glass carbon electrode (GCE) by electropolymerization of o-phenylenediamine (oPD) and AA. Experimental parameters including pH value of running buffer and scan rates were optimized. Scanning electron microscope (SEM), fourier-transform infrared (FTIR) spectra, cyclic voltammetry (CV) and differential pulse voltammetry (DPV) were utilized for the characterization of the imprinted polymer film. Results: Under the selected experimental conditions, the DPV peak currents of AA exhibit two distinct linear responses ranging from 0.01 to 2 μmol L-1 and 2 to 100 μmol L-1 towards the concentrations of AA, and the detection limit was 2 nmol L-1 (S/N=3). Conclusion: The proposed electrochemical sensor possesses excellent selectivity for AA, along with good reproducibility and stability. The results obtained from the analysis of AA in real samples demonstrated the applicability of the proposed sensor to practical analysis.


1984 ◽  
Vol 49 (10) ◽  
pp. 2320-2331 ◽  
Author(s):  
Miroslav Březina ◽  
Martin Wedell

Reduction of oxygen and oxidation of hydrogen peroxide at the dropping mercury electrode are electrochemical processes strongly influenced both by the pH value and the anions in solution. With decreasing pH, both processes become irreversible, especially in the presence of anions with a negative φ2 potential of the diffusion part of the double layer. In the case of irreversible oxygen reduction, the concept that the rate-controlling step of the electrode process is the acceptance of the first electron with the formation of the superoxide anion, O2-, was substantiated. Oxidation of hydrogen peroxide becomes irreversible at a lower pH value than the reduction of oxygen. The slowest, i.e. rate-controlling step of the electrode process in borate buffers at pH 9-10 is the transfer of the second electron, i.e. oxidation of superoxide to oxygen.


Materials ◽  
2021 ◽  
Vol 14 (10) ◽  
pp. 2518
Author(s):  
Dorota Kołodyńska ◽  
Yongming Ju ◽  
Małgorzata Franus ◽  
Wojciech Franus

The possibility of application of chitosan-modified zeolite as sorbent for Cu(II), Zn(II), Mn(II), and Fe(III) ions and their mixtures in the presence of N-(1,2-dicarboxyethyl)-D,L-aspartic acid, IDHA) under different experimental conditions were investigated. Chitosan-modified zeolite belongs to the group of biodegradable complexing agents used in fertilizer production. NaP1CS as a carrier forms a barrier to the spontaneous release of the fertilizer into soil. The obtained materials were characterized by Fourier transform infrared spectroscopy (FTIR); surface area determination (ASAP); scanning electron microscopy (SEM-EDS); X-ray fluorescence (XRF); X-ray diffraction (XRD); and carbon, hydrogen, and nitrogen (CHN), as well as thermogravimetric (TGA) methods. The concentrations of Cu(II), Zn(II), Mn(II), and Fe(III) complexes with IDHA varied from 5–20 mg/dm3 for Cu(II), 10–40 mg/dm3 for Fe(III), 20–80 mg/dm3 for Mn(II), and 10–40 mg/dm3 for Zn(II), respectively; pH value (3–6), time (1–120 min), and temperature (293–333 K) on the sorption efficiency were tested. The Langmuir, Freundlich, Dubinin–Radushkevich, and Temkin adsorption models were applied to describe experimental data. The pH 5 proved to be appropriate for adsorption. The pseudo-second order and Langmuir models were consistent with the experimental data. The thermodynamic parameters indicate that adsorption is spontaneous and endothermic. The highest desorption percentage was achieved using the HCl solution, therefore, proving that method can be used to design slow-release fertilizers.


Minerals ◽  
2021 ◽  
Vol 11 (4) ◽  
pp. 359
Author(s):  
Liping Zhang ◽  
Shengnian Wu ◽  
Nan Zhang ◽  
Ruihan Yao ◽  
Eryong Wu

Salicylic hydroxamic acid is a novel flotation reagent used in mineral processing. However, it impacts the flotation wastewater leaving behind high chromaticity which limits its reuse and affects discharge for mining enterprises. This study researched ozonation catalyzed by the granular activated carbon (GAC) method to treat the chromaticity of the simulated mineral processing wastewater with salicylic hydroxamic acid. The effects of pH value, ozone (O3) concentration, GAC dosage, and reaction time on chromaticity and chemical oxygen demand (CODCr) removal were discussed. The results of individual ozonation experiments showed that the chromaticity removal ratio reached 79% and the effluent chromaticity exceeded the requirement of reuse and discharge when the optimal experimental conditions were pH value 3, ozone concentration 6 mg/L, and reaction time 40 min. The orthogonal experimental results of catalytic ozonation with GAC on chromaticity removal explained that the chromaticity removal ratio could reach 96.36% and the chromaticity of effluent was only 20 when the optimal level of experimental parameters was pH value 2.87, O3 concentration 6 mg/L, GAC dosage 0.06 g/L, reaction time 60 min respectively. The degradation pathway of salicylic hydroxamic acid by ozonation was also considered based on an analysis with ultraviolet absorption spectrum and high-performance liquid chromatography (HPLC).


2007 ◽  
Vol 90 (5) ◽  
pp. 1346-1353 ◽  
Author(s):  
Diego L García-González ◽  
María Viera-Macías ◽  
Ramón Aparicio-Ruiz ◽  
Maria T Morales ◽  
Ramón Aparicio

Abstract The difference between theoretical and empirical triglyceride content is a powerful tool to detect the presence of any vegetable oil in olive oil. The current drawback of the method is the separation between equivalent carbon number ECN42 compounds, which affects the reliability of the method and, hence, its cutoff limit. The determination of the triglyceride profile by liquid chromatography using propionitrile as the mobile phase has recently been proposed to improve their quantification, together with a mathematical algorithm whose binary response determines the presence or absence of hazelnut oil. Twenty-one laboratories from 9 countries participated in an interlaboratory study to evaluate the performance characteristics of the whole analytical method. Participants analyzed 12 samples in duplicate, split into 3 intercomparison studies. Statistically significant differences due to the experimental conditions were found in some laboratories, which were detected as outliers by use of Cochran's and Grubbs' tests. The relative standard deviations (RSD) for repeatability and reproducibility were determined following the AOAC Guidelines for Collaborative Studies. The analytical properties of the method were determined by means of the sensitivity (0.86), selectivity (0.94), and reliability (72) for a cutoff limit of 8 (probability 94).


RSC Advances ◽  
2017 ◽  
Vol 7 (26) ◽  
pp. 16022-16026 ◽  
Author(s):  
Jiafei Lyu ◽  
Hongxu Liu ◽  
Jingshuang Zhang ◽  
Zhouliangzi Zeng ◽  
Peng Bai ◽  
...  

A variety of MOFs were observed with ZIF-8, to our knowledge, showing the highest boron uptake and MIL-101(Cr) with an unprecedentedly high boron isotope separation factor.


2015 ◽  
Vol 51 (4) ◽  
pp. 823-832 ◽  
Author(s):  
Francine Rodrigues Ianiski ◽  
Luciane Varini Laporta ◽  
Alexandre Machado Rubim ◽  
Cristiane Luchese

abstract A method to ensure that an analytical method will produce reliable and interpretable information about the sample must first be validated, making sure that the results can be trusted and traced. In this study, we propose to validate an analytical high performance liquid chromatography (HPLC) method for the quantitation of meloxicam loaded PEGylated nanocapsules(M-PEGNC). We performed a validation study, evaluated parameters including specificity, linearity, quantification limit, detection limit, accuracy, precision and robustness. PEGylated nanocapsules were prepared by interfacial deposition of preformed polymer, and the particle size, polydispersity index, zeta potential, pH value and encapsulation efficiency were characterized. The proposed HPLC method provides selective, linear results in the range of 1.0-40.0 μg/mL; quantification and detection limits were 1.78 μg/mL and 0.59 μg/mL, respectively; relative standard deviation for repeatability was 1.35% and intermediate precision was 0.41% and 0.61% for analyst 1 and analyst 2, respectively; accuracy between 99.23 and 101.79%; robustness between 97.13 and 98.45% for the quantification of M-PEGNC. Mean particle diameters were 261 ± 13 nm and 249 ± 20 nm, polydispersity index was 0.15 ± 0.07 and 0.17 ± 0.06, pH values were 5.0 ± 0.2 and 5.2 ± 0.1, and zeta-potential values were -37.9 ± 3.2 mV e -31.8 ± 2.8 mV for M-PEGNC and placebo(B-PEGNC), respectively. In conclusion, the proposed analytical method is suitable for the quality control of M-PEGNC. Moreover, suspensions showed monomodal size distributions and low polydispersity index indicating high homogeneity of formulations with narrow size distributions, and appropriate pH and zeta potential. The extraction process was efficient for release of meloxicam from nanostructured systems.


2016 ◽  
Vol 2016 ◽  
pp. 1-8 ◽  
Author(s):  
Xiaodong Wei ◽  
Hongling Shen ◽  
Lijun Wang ◽  
Qingyan Meng ◽  
Wenjie Liu

A comprehensive two-dimensional (2D) reverse phase (RP) liquid chromatography (LC) method is developed for alkaloid analysis. This offline comprehensive 2D method is developed using different pH values. With a pH value of 10.5, most alkaloids appear in the form of neutral molecules possessing high retention factors based on their polarity, while the alkaloid polarity order is changed when the pH value decreased to 3.0. The performance of pH modulated 2D LC is demonstrated with 8 alkaloid standards which resulted in orthogonal separation. The developed method is then applied to total alkaloid separation inCorydalis yanhusuo. The first-dimension separation is carried out using methanol and water containing 1.0% ammonium hydroxide and a strong base-resistant RP column, which afforded a peak capacity of 94. The second-dimension analysis is carried out with a surface positive charge column providing a peak capacity of 205 using a mobile phase consisting of acetonitrile and water with 0.15% formic acid. 2D analyses of total alkaloid extract fromC. yanhusuoafford a total peak capacity of 9090. Sixteen compounds were tentatively identified based on their ultraviolet spectrum and MS/MS analyses. The proposed method provides an alternative approach to achieve high peak capacity for analysis of alkaloid extract.


1993 ◽  
Vol 71 (11) ◽  
pp. 1828-1833 ◽  
Author(s):  
Paul Rys ◽  
Ruth Weber ◽  
Qinglan Wu

To evaluate the experimental conditions for the light-induced change of the molecular charge, the dependence of the photochromic reaction behaviour of the indolino spiro naphthoxazine compound 1,3,3-trimethyl-spiro[2H-indol 2,3′-[3H]naphth[2,1-b]-[1,4]oxazine] on the pH value of the solution is investigated. In the absence of UV light an acid–base equilibrium between the spiro form and a protonated closed form is established. By irradiation under appropriate acidic conditions the spiro form can be transformed into an open cationic form through the merocyanine form. Between the two open forms an acid–base equilibrium is established. Except for the closed protonated form the structures are confirmed by mean of NMR. The kinetics of the thermal ring-closing reaction of both forms are investigated by flash photolysis. It is shown that the ring-closing reaction proceeds exclusively via the merocyanine form. The pK values determined for both equilibria give the pH range, in which the light-induced change of the molecular charge occurs.


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