Iron(II) and Iron(III) Perchlorate Complexes of Ciprofloxacin and Norfloxacin

The reactions of ciprofloxacin (CIP) and norfloxacin (NOR) with iron(II) and iron(III) perchlorate have been investigated. The optical spectra support the formation of four complexes for each oxidation state with 1 : 1, 1 : 2, 1 : 3 and 1 : 4 metal to ligand molar ratios. The electrical conductivity and magnetic susceptibility measurements show that the isolated complexes are high spin and the Fe(ClO 4 ) 2 and Fe(ClO 4 ) 3 complexes behave as 1 : 2 and 1 : 3 electrolytes, respectively. The IR spectra indicate that CIP and NOR bind to the iron ion as bidentate ligands through the carbonyl oxygen atom and one of the oxygen atoms of the carboxylate group.     

Electro membrane extraction of biological anions with ion chromatographic analysis

A simple and sensitive single step electro membrane extraction (EME) procedure was demonstrated for biological organic anions with determination by ion chromatography (IC). Nitrite, adipate, oxalate, iodide, fumarate, thiocyanate and perchlorate were extracted from aqueous donor solutions, across a supported liquid membrane (SLM) consisting of methanol impregnated in the walls of a porous polypropylene membrane bag and into an alkaline aqueous acceptor solution in the lumen of the propylene envelope by the application of potential of 12 V applied across the SLM. The acceptor solution was analyzed by IC. Parameters affecting the extraction performance such as type of SLM, extraction time, pH of the donor and acceptor solution, and extraction voltage were studied. The most favorable EME conditions were methanol as the SLM, extraction time of 5 min, pH of acceptor and sample solutions of 12 and 4, respectively, and a voltage of 12 V. Portable 12 V batteries were used in the study. Under these optimized conditions, all anions had enrichment factors ranging from 3.6 to 36.2 with relative standard deviations (n = 3) of between 6.6 and 17.5%. Good linearity ranging from 0.1 to 10 μg mL⁻¹ with coefficients of correlation (r) of between 0.9981 and 0.9996 were obtained. The limits of detection of the EME-IC method were from 0.01 to 0.14 μg mL⁻¹. The developed methodology was applied to amniotic fluid samples to evaluate the feasibility of the method for real applications.     

Two‐Dimensional Divalent Metal Coordination Polymers Containing 3,4′‐Dipyridylketone Tethers: Layer Topology Tuning by Anion Binding Preferences

Slow diffusion of aqueous cobalt thiocyanate or cadmium perchlorate and ethanolic solutions of 3,4′‐dipyridylketone (3,4′‐dpk) generated the coordination polymers {[Co(NCS)₂(3,4′‐dpk)₂]·2H₂O}_n ( 1 ) and {[Cd(H₂O)₂(3,4′‐dpk)₂](ClO₄)₂·2H₂O}_n ( 2 ), which were structurally characterized by single‐crystal X‐ray diffraction. The structure of 1 consists of interdigitated neutral [Co(NCS)₂(3,4′‐dpk)₂]_n (4,4) rectangular grid coordination polymer layers. However, compound 2 manifests cationic [Cd(H₂O)₂(3,4′‐dpk)₂]_n²ⁿ⁺ two‐dimensional (6,3) herringbone lattices connected through hydrogen bonding mediated by interlamellar unligated perchlorate anions. Upon excitation with ultraviolet radiation, 2 emits blue‐violet light, ascribed to π–π* transitions within the pyridyl rings of the 3,4′‐dpk ligands. Thermal decomposition behavior of 1 is also discussed.     

氧阴极用于高氯酸盐电化生产的研究

利用氧阴极和铂或二氧化铅阳极组装成电解槽，用直接测量电解系统析气量的方法，确定了高氯酸盐电化生产过程的电流效率，考察了溶液的组成（ＣｌＯ－３、Ｃｌ－、ＣｌＯ－４）、操作参数（电流密度、电解槽温度、溶液的酸碱度）、重金属离子对电流效率的影响．并提出氧阴极用于高氯酸盐电化生产的主要障碍及其解决途径．     

The perchlorate anion is more effective than the trifluoroacetate anion as an ion-pairing reagent for reversed-phase chromatography of peptides

The addition of salts, specifically sodium perchlorate (NaClO4), to mobile phases at acidic pH as ion-pairing reagents for reversed-phase high-performance liquid chromatography (RP-HPLC) has been generally overlooked. To demonstrate the potential of NaClO4 as an effective anionic ion-pairing reagent, we applied RP-HPLC in the presence of 0-100 mM sodium chloride (NaCl), sodium trifluoroacetate (NaTFA) or NaClO4 to two mixtures of synthetic 18-residue peptides: a mixture of peptides with the same net positive charge (+4) and a mixture of four peptides of +1, +2, +3 and +4 net charge. Interestingly, the effect of increasing NaClO4 concentration on increasing peptide retention times and selectivity changes was more dramatic than that of either NaCl or NaTFA, with the order of increasing anion effectiveness being Cl- < TFA- < C104-. Such effects were more marked when salt addition was applied to eluents containing 10 mM phosphoric acid (H3PO4) compared to 10 mM trifluoroacetic acid (TFA) due to the lesser starting anion hydrophobicity of the former mobile phase (containing the phosphate ion) compared to the latter (containing the TFA- ion).     

Trace level perchlorate analysis by ion chromatography-mass spectrometry

Perchlorate is commonly used as an oxidant in solid fuel propellant for rockets and missiles. Recently perchlorate contamination was found in many aquifers associated with Colorado River and other sites. Perchlorate was also found at elevated level in crops that use contaminated water for irrigation. Ion chromatography with conductivity detection could be used to measure perchlorate levels in drinking and wastewaters as per United States Environmental Protection Agency method 314, but at lower levels and with complexity of the matrix there could be false positive and/or false negative. This study was done to demonstrate the detection of perchlorate with lower detection limit with high ionic matrix by ion chromatography-mass spectrometry.     

Determination of trace level perchlorate in drinking water and ground water by ion chromatography

Ammonium perchlorate, a key ingredient in solid rocket propellants, has recently been found in ground and surface waters in the USA in a number of states, including California, Nevada, Utah, and West Virginia. Perchlorate poses a health risk and preliminary data from the US Environmental Protection Agency reports that exposure to less than 4–18 μg/l provides adequate human health protection. An ion chromatographic method was developed for the determination of low μg/l levels of perchlorate in drinking and ground waters based on a Dionex IonPac AS11 column, a 100 mM hydroxide eluent, large loop (1000 μl) injection, and suppressed conductivity detection. The method is free of interferences from common anions, linear in the range of 2.5–100 μg/l, and quantitative recoveries were obtained for low μg/l levels of perchlorate in spiked drinking and ground water samples. The method detection limit of 0.3 μg/l permits quantification of perchlorate below the levels which ensure adequate health protection. A new polarizable anion analysis column, the IonPac AS16, and its potential applicability for this analysis is also discussed.     

(Hg2)Hg(OH)2(ClO4)2: Das erste gemischtvalente Quecksilberperchlorat

(Hg₂)Hg(OH)₂(ClO₄)₂: The First Mixed Valent Mercury Perchlorate Colorless single crystals of (Hg₂)Hg(OH)₂(ClO₄)₂ (C2/c, Z = 4, a = 1847.7(5), b = 490.8(1), c = 1086.2(3) pm, β = 93.80(2)°, R_all = 0.0610) were obtained as a side product during the dehydration of Hg₂(ClO₄)₂ · 2H₂O. The crystal structure consists of infinite zig‐zag chains {_∞¹[(Hg₂)_1/2(OH)Hg_1/2]⁺}₂ which are separated by the ClO₄^— ions.     

Nitrate and perchlorate salts of a silver(I) complex from 5-methyl-2-(2,3-diaza-4-(5-methyl-2-thienyl)buta-1,3-dienyl)thiophene

Bis(5-methyl-2-(2,3-diaza-4-(5-methyl-2-thienyl)buta-1,3-dienyl)thiophene) silver(I) complex was synthesized in high yield by refluxing 5-methyl-2-(2,3-diaza-4-(5-methyl-2-thienyl)buta-1,3-dienyl)thiophene (L) with silver nitrate or silver perchlorate in anhydrous acetonitrile. The product thus formed was well characterized by NMR, IR, UV–Vis and mass spectroscopies as well as elemental analysis and electrochemical analysis. Molecular structures of compounds L, [L₂Ag]NO₃ and [L₂Ag]ClO₄ were determined by single crystal X-ray diffraction analysis. It was found that the C=N double bond of the ligand rotated during the course of ligand coordination in the case of the perchlorate salt but not in the case of the nitrate salt.     

智能手机图形比色法快速测定水中的高氯酸盐

高氯酸盐是水环境中一种典型的难降解的持久性无机污染物,具有高度水溶性及扩散性。地表水及地下水中的高氯酸盐可以通过多种方式保存在食物和饮用水中,对人体健康造成严重危害。针对传统的高氯酸盐检测技术操作复杂、检测周期长、成本高且不便于即时检测等问题,本文提出了一种智能手机快速测定高氯酸盐含量的新方法,以充分发挥其能简便、准确、快速现场检测水高氯酸盐的优势。本研究采用由3D打印箱、扩散板、补光灯和智能手机构建的数字图像比色装置完成了水中高氯酸盐浓度的快速检测,探讨了手机型号、光源、干扰离子对数字图像比色装置检测结果R（红）、G（绿）、B（蓝）值的影响。结果表明,以R-通道数字信号值作为测定值时,高氯酸盐在0 μg/L~600 μg/L浓度范围内呈良好的线性关系,线性方程为y=-0.1505 x+150.66,相关系数为R2=0.995,加标回收率为96~107%,检出限为27.7 μg/L,测定限为88 μg/L。选择白光、iPhone 11检测两组不同浓度高氯酸盐的实际水样,以探究重现性,测定结果的相对标准偏差为3.2%~4.0%,回收率为95%-107%,本方法具有一定的可行性和准确性,为现场快速测定水中高氯酸盐提供了一个新思路。