Silica Xerogel Doped with Iron(III) as Sensor Material for Salicylhydroxamic Acid Determination in Urine

Salicylhydroxamic acid (SHA) is used as antimicrobic medicine and its concentration has to be monitored in urine. For the first time, silica xerogels doped with iron(III) have been proposed as sensor materials for SHA determination in biological samples. Three xerogels with iron(III) content in the range of 0.04–1.74% wt have been synthesized. BET surface area of these xerogels has varied in the range of 696–529 m2/g and total pore volume has varied in the range of 0.92–0.23 cm3/g. Complex formation between immobilized iron(III) and salicylhydroxamic acid has been investigated with solid phase spectrophotometry and IR spectroscopy. Orange-brown iron(III)-SHA complex with 1:1 stoichiometry is formed at pH 1–4 with half-reaction time of 17 min. Silica xerogel doped with 0.33% wt iron(III)) has been used as sensor material for SHA solid phase spectrophotometric determination (LOD 1.4 mg/L (n = 3), analytical range 4–230 mg/L). Proposed sensor material has been applied for SHA determination in biological samples of synthetic and human urine. The proposed procedure is characterized by a good level of accuracy (recovery values 97–120%) and precision (RSD values 4–9%) and can be recommended for pharmacokinetic–pharmacodynamic studies of hydroxamic acid-based medications.

Hexa-μ-acetato-chlorido(μ-N,2-dioxodobenzene-1-carboximidato)-μ3-oxido-tetrairon(III)–water (1/1) and hexa-μ-acetato-(μ-N,2-dioxodobenzene-1-carboximidato)fluorido-μ3-oxido-tripyridinetetrairon(III)–pyridine–water (1/1/0.24)

The title compounds, [Fe4(C2H3O2)6(C7H4O3)FO(C5H5N)3]·C5H5N·0.24H2O (1-F) and [Fe4(C2H3O2)6(C7H4O3)ClO(C5H5N)3]·H2O (1-Cl) were synthesized using a self-assembly reaction in methanol and pyridine with stoichiometric addition of salicylhydroxamic acid (H3shi), acetic acid (HOAc), and the appropriate ferric halide salt. The compounds crystallize as solvates, where 1-F has one pyridine molecule that is disordered about a twofold axis and one water molecule with an occupancy of 0.24 (2); and 1-Cl has one water molecule that is disordered over two sites with occupancies of 0.71 (1) and 0.29 (1). The space groups for each analog differ as 1-F crystallizes in Fdd2 while 1-Cl crystallizes in P21. The difference in packing is due to changes in the intermolecular interactions involving the different halides. The two molecules are mostly isostructural, differing only by the torsion of the pyrine ligands and slight orientation changes in the acetate ligands. All of the iron(III) ions are in six-coordinate octahedral ligand field geometries but each one exhibits a unique coordination environment with various numbers of O (four to six) and N (nought to two) atom donors. Bond-valence sums confirm each iron is trivalent. The hydroximate ligand is bound to three iron(III) ions using a fused chelate motif similar to those in metallacrown compounds.

Study of the relationship between the zeta potential and floatability of cassiterite fine fractions

This article is a continuation of the authors’ research on improving the flotation process for fine tin products using zeta potential measurements on particle surfaces. The aim of the research is to establish the possibility of using certain reagents to intensify the flotation of fine cassiterite particles and to identify the mechanism behind the effect produced by the reagents on the surface of slurry particles in cassiterite flotation using zeta potential measurements. The results of experiments to select the best collector are presented, with salicylhydroxamic acid identified as the best option. Sodium hexametaphosphate pretreatment of a flotation slurry consisting of fine particles enables a more efficient cassiterite flotation, which is explained by the negative value of the z-potential for the particle surface. The use of sodium hexametaphosphate improves the yield by up to 3 %, with the mass fraction of tin growing from 1.2 to 1.75 %, and the recovery improving from 40 to 75 %. The results of z-potential measurements for the particle surface in the process of flotation indicate that its positive values are not always required and that the combined action of oxalic and sulfuric acids with salicylhydroxamic acid at a z-potential of –0.7 mV renders the maximum tin grade of 2.22 % in the froth flotation product. Gravity treatment of the flotation concentrate on concentration tables allows obtaining conditioned concentrates with the mass fractions of tin of 23.4 and 30.6 %. Finding the extremum of the z-potential for the particle surface during the flotation of tin minerals allows predicting the concentration results.

Inhibition of alternative respiration system of Scheffersomyces stipitis and effect on glucose or xylose fermentation

Scheffersomyces stipitis is a Crabtree-negative pentose fermenting yeast, which shows a complex respiratory system involving a cytochrome and an alternative salicylhydroxamic acid (SHAM)-sensitive respiration mechanism that is poorly understood. This work aimed to investigate the role of the antimycin A (AA) sensitive respiration and SHAM-sensitive respiration in the metabolism of xylose and glucose by S. stipitis, upon different agitation conditions. Inhibition of the SHAM-sensitive respiration caused a significant (p < 0.05) decrease in glycolytic flux and oxygen consumption when using glucose and xylose under agitation conditions, but without agitation, only a mild reduction was observed. The combination of SHAM and AA abolished respiration, depleting the glycolytic flux using both carbon sources tested, leading to increased ethanol production of 21.05 g/L at 250 rpm for 0.5 M glucose, and 8.3 g/L ethanol using xylose. In contrast, inhibition of only the AA-sensitive respiration, caused increased ethanol production to 30 g/L using 0.5 M glucose at 250 rpm, and 11.3 g/L from 0.5 M xylose without agitation. Results showed that ethanol production can be induced by respiration inhibition, but the active role of SHAM-sensitive respiration should be considered to investigate better conditions to increase and optimize yields.

Research on treatment and mechanism of salicylhydroxamic acid flotation wastewater by O3-BAF process

Salicylhydroxamic acid is an effective and selective collector for tungsten and molybdenum ores. However, the salicylhydroxamic acid flotation wastewater discharge may cause damage to the water environment for the residual processing reagents with poor biodegradability. Combined O3 and biological aerated filter (BAF) has a well-known potential for removing refractory or toxic organic pollutants. Combined process of O3 and BAF (O3-BAF) was applied to treat the simulated wastewater from W-Mo mineral processing in this study. Compared single ozonation to O3-BAF, various influencing factors were discussed like O3 dosage, reaction time, initial pH value, gas–water ratio and organic loading. Meanwhile, degradation mechanism of salicylhydroxamic acid was reduced. Under the optimal experiment conditions as pH value 8, O3 dosage 1.3 mg·L−1, reaction time 15 min, the five-day biochemical oxygen demand (BOD5)/chemical oxygen demand of potassium dichromate (CODCr) value increased to from 0.19 to 0.35. The effluent was pumped to the following BAF process, when the optimal experiment conditions was organic load = 0.82 kgCODCr (m−3·d−1), gas-water ratio = 6:1, CODCr concentration of effluent was 28.92 mg·L−1 and the removal ratio was 86.26%, while the removal ratio could higher to 91.12% for the O3-BAF combined process. The effluent could meet the discharge and reuse emission standards requirements in China. UV-vis absorption spectra and high performance liquid chromatography showed the degradation pathway of salicylhydroxamic acid by ozone oxidation was salicylhydroxamic acid → salicylic acid + hydroxylamine → catechol → maleic → small molecular organic acid → carbon dioxide + water.