Determination of fluorinated quinolone antibacterials by ion chromatography with fluorescence detection

For preparing fluorinated quinolone antibiotic medicine locally used in stomatology, simultaneous determination of norfloxacin, ciprofloxacin, and enoxacin was carried out by multiphase ion chromatography with fluorescence detection. Quinolone antibiotics were separated by Dionex OmniPac PAX-500 column with an eluent of 15 mmol/L H2SO4 and 35% methanol (v/v) at a flow-rate of 1.0 ml/min and detected with fluorescence with excitation and emission wave lengths of 347 nm and 420 nm respectively. The detection limits (S/N=3) of norfloxacin, ciprofloxacin and enoxacin were 50, 105 and 80 ng/ml respectively. The relative standard deviations of retention time, peak area and peak height were less than 1.1% and good linear relationship resulted. The developed method was applied to pharmaceutical formulations and biological fluids.

Simultaneous determination of fluorine and iodine in urine by ion chromatography with electrochemical pretreatment

A new method for the simultaneous determination of fluorine and iodine in urine by ion chromatography （IC） with electrochemical pretreatment has been developed. The pretreatment was performed in a novel electrochemical oxidationneutralization device （EOND）, in which iodide of the sample was oxidized to iodate and the alkaline digestion sample solution was neutralized. Under the optimized conditions, the limits of detection （LOD, S/N = 3） were 2.5 μg/L for fluoride and 20 μg/L for iodate, respectively. The recoveries were in the range of 93-102% for fluoride and 86-98% for iodate.

Exploring high-voltage fluorinated carbonate electrolytes for LiNi0.5Mn1.5O4 cathode in Li-ion batteries

Ethyl-(2,2,2-trifluoroethyl)carbonate(ETFEC)is investigated as a solvent component in high-voltage electrolytes for LiNi0.5Mn1.5O4(LNMO).Our results show that the self-discharge behavior and the high temperature cycle performance can be significantly improved by the addition of 10%ETFEC into the normal carbonate electrolytes,e.g.,the capacity retention improved from 65.3%to 77.1%after 200 cycles at 60℃.The main reason can be ascribed to the high stability of ETFEC which prevents large oxidation of the electrolyte on the cathode surface.In addition,we also explore the feasibility of electrolytes using single fluoriated-solvents with and without additives.Our results show that the cycle performance of LNMO material can be greatly improved in 1 MLiPF6+pure ETFEC-solvent system with 2 wt%ethylene carbonate(EC)or ethylene sulfate(DTD).The capacity retention of the LNMO materials is 93%after 300 cycles,even better than that of carbonate-based electrolytes.It is shown that the additives are oxidized on the surface of LNMO particles and contribute to the formation of cathode/electrolyte interphase(CEI)films.This composite CEI film plays a crucial role in suppressing the serious decomposition of the electrolyte at high voltage.

High Density Fluorine Negative-Ion Source Generated by Utilizing Magnetized SF₆

In a magnetized plasma column generated from an electronegative gas, negative-ions accumulate around the plasma column via radial diffusion. In this study, a dc discharge is applied in SF6 gas to produce a plasma column, and the radial density profile of negative-ions is measured by Langmuir probes using the modified Bohm criterion. The gas pressure and discharge current dependences of negative-ion density are also measured. It is found that the negative-ion density of 8.0 × 1017 m-3 is obtained around the plasma column at r = 1.0 cm when SF6 pressure is 0.13 Pa and discharge current is 0.50 A. The negative-ion density has radial gradient, and the electron density is much lower in this region.

Effects of Fluorine and Silicon Incorporation on Tribological Performance of Diamond-Like Carbon Films

Diamond-like carbon (DLC) is a metastable amorphous film that exhibits unique properties. However, a number of limitations exist regarding the use of DLC, for instance, its tribological characteristics. In this article, the fluorine and silicon incorporated diamond-like carbon (F-DLC and Si-DLC) films are studied, taking into account the tribological properties of these films compared with pure DLC. The structures of the films were characterized using Auger electron spectroscopy and Raman spectroscopy. The hardness and elastic modulus were evaluated by nanoindentation hardness testing. The friction behavior was assessed using ball-on-disk friction testing and optical microscopy. The results indicated that the deposited DLC films contained 0.6 - 2.1 at.% F and 26.7 - 38.4 at.% Si. A decrease in the hardness and elastic modulus was obtained as F increased in content, which was the opposite of the behavior observed in the Si-DLC films. This was due to the shifting in the G-peak position, which is related to the sp3 bonding fraction in the film. When measured in ambient air, the addition of Si into the DLC film strongly influenced the friction coefficient, whereas doping with F only slightly influenced the films, as evidenced by their wear scars. In addition, only a 26.7 at.% Si-DLC film showed a very low friction coefficient when measured in dry air. This was attributed to the formation of silicon-rich transfer layer on the ball surfaces. Therefore, the addition of Si with 26.7 at.% content to a DLC film can be considered beneficial for improving tribological performance.

Addition of Pyridine to Dye-Sensitized Solar Cell Including Fluorinated Oligomer Gel Electrolyte

Fluorinated oligomer gel is suitable to the electrolyte of dye-sensitized solar cell for low cost production. In this article, addition of pyridine was investigated for the purpose of enhancing the short current density. Two kinds of ionic liquids were tested: imidazolium and pyrazolium systems. The two different stages of adding pyridine to the electrolyte were considered and the amount of pyridine was studied. It was found that the electrolyte including pyrazolium ionic liquids to which pyridine was added before the mixing with fluorinated oligomer showed the highest electric conductivity, short current density and open voltage. This resulted in the highest conversion efficiency of 4%. As the amount of pyridine increased, the fill factor and the open voltage were improved at first, and then the short current density increased. If the pyridine was added more, the short current density conversely decreased.

Electric Conductivity of Fluorinated Oligomer Gel Electrolyte Including Ionic Liquid and Performance of Dye Sensitized Solar Cell

Fluorinated oligomer gel is suitable to the electrolyte of dye sensitized solar cell. This article studied mainly in the scope of electric conductivity, including ionic liquid in the electrolyte. It was found that the ratio of mixing with dimetyl sulfoxide and the concentration of LiI affect the conductivity. The behavior is different depending on the type of ionic liquid. Although the mixing ionic liquid enhances the conductivity, the short circuit current density of assembled solar cell with it was suppressed so much.

兰州不同城镇功能区地下水氟赋存特征及影响因素

高氟地下水对生态环境及人类健康存在潜在威胁。城镇化地区受地质背景与人类活动双重影响,地下水中氟的来源及其分布较为复杂,探讨地下水中氟的赋存特征对于保障地下水供水安全具有重要意义。以西北干旱区最大的工业城市兰州为例,采用数理统计、离子比、饱和指数分析等方法,研究了兰州不同城镇功能区高氟地下水的赋存环境特征及主要水文地球化学过程,阐明了人为活动对氟化物迁移富集的影响。结果表明:(1)研究区地下水中F-的质量浓度介于0~4.8mg/L之间,超出地下水质量Ⅲ类标准(1.0mg/L)的高氟水共计13组,超标率为20.3%。(2)受人类活动强度与不同人为源输入影响,不同城镇功能区地下水中氟的赋存特征差异明显,其中西固工业区地下水中氟含量最高,高氟地下水样品占47.4%;城关老城区和断陷盆地新城区地下水中的氟含量相对较低,高氟地下水占比依次为7.1%和9.7%。(3)研究区高氟地下水以SO_(4)•Cl—Na和Cl•SO_(4)—Na型水为主,表现出贫钙富钠弱碱性特点。(4)含氟矿物的溶解、方解石与白云石的沉淀/溶解、黏土矿物表面钙与钠之间的阳离子交换、强烈的蒸发浓缩作用和盐效应是导致研究区地下水中氟化物富集的主要水文地球化学过程。研究表明城镇化、工业化导致天然高氟水进一步劣变恶化,工业废水的泄漏是西固工业区地下水氟浓度升高的重要驱动力。结果可为高氟背景区人为干扰下的氟化物迁移富集研究提供借鉴。

选择性电极法测定粗氢氧化钴中氟含量

建立了一种选择性电极法测定粗氢氧化钴中微量氟的方法。样品经硝酸溶解后,用氟离子选择电极在离子电位计上测定溶液的电位差计算样品中氟含量。本文实验了样品的溶样方法、总离子强度调节缓冲溶液的最佳加入量,进行了共存离子干扰实验,证明样品中钴、锰、镁、铜、铝、铁、钙对氟元素的测定无明显干扰。对刚果(金)某中资企业实际生产的粗氢氧化钴样品进行测定,氟元素的相对标准偏差(RSD,n=11)在1.59%~4.59%之间,加标回收率为98.29%~102.19%,氟离子的线性范围为0.05~20.0μg/mL,本法可准确测定粗氢氧化钴中0.0025%~0.5%的氟含量,测定结果和外检结果相比较,结果吻合,令人满意。

全自动高温水解-离子色谱法测定氧化镧铈中氟、氯

为探究稀土氧化物中氟(F)和氯(Cl)元素含量的快速检测方法,通过全自动高温水解仪对氧化镧铈样品进行前处理,并利用氢氧根体系离子色谱仪检测吸收液中F^(-)、Cl^(-)的含量,建立了基于全自动高温水解-离子色谱法测定氧化镧铈中的F、Cl元素含量的快速检测方法,有效避免了传统前处理方法过程复杂、分析时间长、极易受人为干扰的问题。将氧化镧铈样品,在氧气流量为300 mL/min,1100℃高温燃烧水解20 min,以NaOH(15 mmol/L)作为淋洗液,经色谱柱分离,测得F^(-)与Cl^(-)在质量浓度为1.00~15.00 mg/L时,质量浓度与离子色谱峰面积呈线性关系,相关系数均为0.9999,检出限分别为0.003 mg/L和0.12 mg/L。全自动高温水解仪联用离子色谱仪检测系统对氧化镧铈中F^(-)的平均加标回收率为98.4%,标准偏差RSD为0.94%;对Cl^(-)的加标回收率为97.8%,RSD为2.9%。方法具有较高准确度及精密度,测试结果准确、可靠,满足测试要求,为稀土氧化镧铈中氟、氯元素含量的研究及相关产品的开发提供了理论基础。

氟离子选择电极法测定含铜蚀刻废液中氟含量方法探讨

准确测定含铜蚀刻废液中氟含量是含铜蚀刻废液中铜盐回收的关键,本文就含铜蚀刻废液中氟含量离子选择电极测定方法[1~3]进行探讨与验证。通过样品前处理与试验,离子选择电极一次标准加入法测定下限为0.9mg·L^(-1),离子选择电极标准曲线法测定下限为1.2 mg·L^(-1);两种方法的相对标准偏差在1.2%~1.7%,两种方法的加标回收率在77%~102%,满足工程应用要求。

含氟物质在提升动力锂离子电池安全性方面的应用

随着新能源汽车渗透率的提升,动力用锂离子电池能量密度不断攀升,研制高性能高能量密度电池体系,满足续航里程、充电时间和高安全性能,是目前重要的研究方向。锂离子电池热失控是其安全性研究中亟待解决的问题,含氟物质在提高锂离子电池热稳定性、预防热失控措施中具有广泛应用。本文从动力锂离子电池热失控现象出发,分类概述了电池热失控的诱导因素、含氟物质在优化单体电池材料(阳极、阴极、电解质和隔膜)、电池热管理技术中的应用以及提高锂电池热安全性的方法,为解决动力锂离子电池的热失控问题提供参考。

煤中氟和氯含量的检测方法研究

阐述了煤中氟和氯元素对生态环境的危害,试验测试了天水市域内煤中氟、氯元素含量范围,氟含量分布区间为20~197μg/g,氯含量分布区间为0.003%~0.139%。同时,研究发现,高温燃烧水解—离子色谱法适用于煤炭中氟和氯的快速检测,适用于实验室日常检验检测。

Low power fluorine plasma effects on electrical reliability of AlGaN/GaN high electron mobility transistor

The new electrical degradation phenomenon of the AlGaN/GaN high electron mobility transistor（HEMT） treated by low power fluorine plasma is discovered. The saturated current, on-resistance, threshold voltage, gate leakage and breakdown voltage show that each experiences a significant change in a short time stress, and then keeps unchangeable. The migration phenomenon of fluorine ions is further validated by the electron redistribution and breakdown voltage enhancement after off-state stress. These results suggest that the low power fluorine implant ion stays in an unstable state. It causes the electrical properties of AlGaN/GaN HEMT to present early degradation. A new migration and degradation mechanism of the low power fluorine implant ion under the off-stress electrical stress is proposed. The low power fluorine ions would drift at the beginning of the off-state stress, and then accumulate between gate and drain nearby the gate side. Due to the strong electronegativity of fluorine, the accumulation of the front fluorine ions would prevent the subsequent fluorine ions from drifting, thereby alleviating further the degradation of AlGaN/GaN HEMT electrical properties.

Substitution Process and Valent State of Samarium Ion in Perovskite Binary Fluorides

The lattice sites occupied by samarium ions in KMgF3 were ascertained. The relationship between valent state of samarium ion in hosts and substituted lattice sites was investigated using fluorescent spectra. It is found that the valent state of samarium in different cationic lattice sites is different. The internal relation between the valent state of samarium ion and occupied lattice site was discussed.

FLUORINE BEHAVIOR IN BF_2^+ IMPLANTED POLYSILICON FILMS SUBJECTED TO RAPID THERMAL ANNEALING

The physical and electrical properties of BF2+ implanted polysilicon films subjectedto rapid thermal annealing（RTA）are presented.It is found that the out diffusion of F and itssegregation at polysilicon/silicon oxide interface during RTA are the major causes of F anomalousmigration.Fluorine bubbles were observed in BF2+ implanted samples at doses of 1×1015 and5×1015cm-2 after RTA.

管式炉燃烧-离子色谱法测定石墨烯粉体中氟、氯、溴、硫元素的含量

提出了管式炉燃烧-离子色谱法测定石墨烯粉体中氟、氯、溴、硫元素含量的方法。样品经冷冻研磨,分取5~10 mg置于燃烧舟中,选择自动推进模式,设置燃烧室温度为1 050℃,后燃烧时间为160 s。样品充分燃烧后,以30%(质量分数)过氧化氢溶液为吸收液,Metrosep A Supp5阴离子色谱柱为分析柱,含3.2 mmol·L^(-1)Na_(2)CO_(3)和1.0 mmol·L^(-1)NaHCO_(3)的混合溶液为淋洗液,采用电导检测器测定其中F^(-)、Cl^(-)、Br^(-)、SO_(4)^(2-)的含量,进而换算为氟、氯、溴、硫元素的含量。结果显示:F^(-)、Cl^(-)、Br^(-)、SO_(4)^(2-)的质量浓度在一定范围内与其对应的峰面积呈线性关系,检出限(3S/N)为0.05~0.10 mg·L^(-1);方法用于测定标准物质ERM-EC-680K中氯、溴、硫的含量,所得测定值均在认定值的不确定度范围内;方法用于实际样品分析,未检出溴元素,并且氯、氟、硫元素的测定值与另外6家实验室的基本一致。

超声提取—离子选择电极法测定化肥样品中的氟

全国土地质量地球化学调查结果显示,我国氟过剩的土地面积约31.5万km2。氟作为一种与人体健康密切相关的元素而得到广泛关注和研究,尤其近年来农业活动中高氟化肥的使用成为土壤中氟的潜在来源,其在土壤、动植物体中的循环迁移方式尚待深入研究。为了迎接新一轮全国土壤普查和现代健康地质调查,需要研究建立准确测定化肥中的氟含量的分析方法。本次实验对比研究了HCl煮沸提取、HCl常温超声提取、NaOH熔融水提取、Na_(2)O_(2)熔融水提取4种不同的样品分解方式,结果表明:采用HCl常温超声提取分解样品,NaOH-H_(2)SO_(4)调节酸度,柠檬酸钠做离子缓冲剂是最佳的样品前处理方式;并对超声提取时间及提取温度进行了考察,确定了超声提取时间为20 min,提取温度为20℃;在最佳的样品前处理条件下,测定了方法的主要质量参数:检出限1.63×10^(-6)、精密度0.98%、回收率在91%~108%。该方法前处理简便快速、易于操作,以分段建立标准曲线的模式,测定的质量参数完全能够满足化肥的分析要求。

Dye-Sensitized Solar Cell with Fluorinated Gel Electrolyte: Effect of TiO₂Particle Size on Performance

We fabricated dye-sensitized solar cells including fluorinated gel electrolyte and studied about the relationship between the performance of the solar cells and the aggregation state of TiO2 nano-particles on electrodes. As for the performance of the cell, the I-V characteristics were measured under irradiation. The combination of TiO2 nanoparticles with different size plays an important role in bringing unevenness to realize a large surface area, which is critical for the high performance of the cells.