微乳液介质 - 4- (6- 甲氧基 - 8- 喹啉偶氮 )- 间苯三酚分光光度法测定微量铜

研究了溴代十六烷基吡啶、正丁醇、正庚烷和水自制微乳溶液介质中,4-（6-甲氧基-8-喹啉偶氮）-间苯三酚与铜的显色反应,建立了分光光度法测定微量铜的新方法。在显色液中铜的质量浓度在0.010 mg/L～0.700 mg/L范围内符合比尔定律,方法检出限为0.003 mg/L,铝合金和水样测定的RSD为0.3%～1.7%,加标回收率为96.3%～104%。     

Simultaneous determination of selected endocrine disrupter compounds in wastewater samples in ultra trace levels using HPLC-ES-MS/MS

An analytical procedure for the simultaneous determination of six selected endocrine disrupter compounds (EDCs: diltiazem, progesterone, benzyl butyl phthalate (BBP), estrone, carbamazepine (Cbz), acetaminophen) was developed by liquid chromatography electrospray ionization tandem mass spectrometry (HPLC-ES-MS/MS). All of the parameters for HPLC and ES-MS/MS systems including mobile phase composition, flow rate, and sample injection volume were optimized to obtain not only the best separation of species interested but also low detection limits. Reverse phase chromatography coupled to ES-MS/MS was used for the separation and detection of EDCs. Formic acid (0.10% ) and 5.0 mM ammonium formate were selected as mobile phase composition in gradient elution. Detection limits for diltiazem, progesterone, BBP, estrone, Cbz, and acetaminophen were found to be 0.13, 0.12, 0.04, 0.13, 0.12, and 0.05 ng/mL, respectively. Influent and effluents from three different wastewater treatment plants located in Ankara, i.e., rotating flat-sheet membrane unit, pilot type flat-sheet membrane unit located at METU Campus and samples from Ankara central wastewater treatment plant were analyzed for their EDCs contents under the optimum conditions.     

Presence of steroid hormones and antibiotics in surface water of agricultural, suburban and mixed-use areas

The occurrence of pharmaceutically active chemicals (PACs) in the natural aquatic environment is recognized as an emerging issue due to the potential adverse effects these compounds pose to aquatic life and humans. This study presents the monitoring of two major categories of PACs in surface water: steroid hormones and antibiotics. Surface water samples were collected in the fall season from 21 locations in suburban (4), agricultural (5) and mixed (12) use suburban and agricultural areas. The water samples collected were analyzed using GC/MS for aqueous concentration of eleven steroid hormones: six natural (17alpha-estradiol, 17beta-estradiol, estrone, estriol, 17alpha-dihydroequilin, progesterone) and five synthetic (gestodene, norgestrel, levonorgestrel, medrogestone, trimegestone). In addition, 12 antibiotics (oxytetracycline, chlorotetracycline, tetracycline, sulfamethoxazole, sulfamethazine, trimethoprim, lincomycin, norfloxacin, ofloxacin, roxithromycin, erythromycin, tylosin tartrate) were analyzed using LC/MS. Steroid hormones detected in surface water were: 17alpha-estradiol, 17beta-estradiol, 17alpha-dihydroequilin, estriol, estrone, progesterone and trimegestone. Estrone had the highest detection frequency of >90% with concentrations ranging from 0.6 to 2.6 ng/l. The second most frequently detected estrogen was estriol (>80%) with concentrations ranging from 0.8 to 19 ng/l. The detection frequency varied at different sampling locations. No antibiotics were detected in the 21 streams sampled. This study aims to give a better understanding on the presence, fate and transport of PACs derived from humans and animals.     

气相色谱法测定空气和废气中8种烃类化合物

建立了针筒采样、大口径毛细管柱分离、气相色谱-氢火焰离子化检测器测定空气和废气中甲烷、乙烷、乙烯、乙炔、丙烷、异丁烷、正丁烷和正戊烷等8种烃类化合物的方法.优化了试验条件,方法线性良好,甲烷、乙烯、乙炔、乙烷、丙烷、异丁烷、正丁烷和正戊烷的检出限分别为0.09 mg/m3、0.20 mg/m3、0.18 mg/m3、0.29 mg/m3、0.28 mg/m3、0.37 mg/m3、0.16 mg/m3和0.56 mg/m3,RSD＜8.0%,加标回收率为80.5%～104%.     

Characterization of dissolved organic carbon at low levels in environmental waters by microfluidic-chip-based capillary gel electrophoresis with a laser-induced fluorescence detector

A microfluidic analytical system for characterization of dissolved organic carbon (DOC) in environmental waters, based on a capillary gel electrophoresis (CGE) device with a laser-induced fluorescence (LEF) detector, was developed. The applied voltage and the running buffer were investigated to control the simple floating injection and CGE separation for convenient cross-type microchips made from polymethylmethacylate. We obtained reproducible peaks for standard organic solutions and the determination time is less than 70 s. The values of the relative standard deviation (RSD) were 0.17–2.01% for repetitive injection (n?=?12). We demonstrated high-throughput characterization of DOC in environmental water from the Biwa Lake and the Hino River using microfluidic chip and determined that the content of DOC in the Biwa Lake changed with the seasons.     

毛细管柱气相色谱法测定环境空气中的樟脑

采用毛细管柱气相色谱氢火焰离子化检测器测定环境空气中的樟脑,选择硅胶为吸附剂,甲醇/丙酮混合溶剂(体积比90∶10)为解析剂.方法在0.544 mg/L～109 mg/L范围内线性良好,检出限为0.06 mg/L,当采样体积为20 L时,最低检出质量浓度为0.003 mg/m3,标准溶液平行测定的RSD≤3.8％,空白...     

液液萃取-高效液相色谱法测定水中四乙基铅

采用高效液相色谱紫外检测器测定水中四乙基铅,用二氯甲烷液液萃取,以甲醇/水混合溶液(体积比为95:5)为流动相,Z0RBAX Eclipse XDB-C18色谱柱分离,选择测定波长为280 nm.方法在0.100mg/L～1.00mg/L范围内线性良好,检出限和测定下限分别为0.01μg/L和0.04μg/L,水样平行...     

固相萃取-高效液相色谱法测定废水中的酚类化合物

建立了Supelclean ENVI-Chrom P柱固相萃取-高效液相色谱法测定废水中11种酚类化合物的分析方法,并对固相萃取条件和液相色谱条件进行了讨论。该方法分离效果良好,净化效果明显,方法检出限为2×10-3~2×10-2mg/L,平行分析(n=6)的RSD为2.7%~16.4%,废水加标回收率除2,4-二硝基酚偏低以外,其他化合物的回收率为61.4%~115.8%。     

On-site simultaneous determination of anions and cations in drainage water using a flow injection-capillary electrophoresis system with contactless conductivity detection

Drainage water diverted from a farm pasture, which was heavily loaded with manure, was monitored during a rain event. Concurrent anion and cation determinations at intervals of 10 min could be achieved with a new capillary electrophoresis system employing dual injection at opposite ends of the separation capillary. The flow injection approach enabled automation of the sampling process. Interruption of the separation voltage was not necessary. Contactless conductivity detection with an electrolyte solution optimized for the purpose allowed the facile simultaneous detection of the inorganic ions Cl(-), NO(3)(-), SO(4)(2-), HPO(4)(2-), NO(2)(-), NH(4)(+), K(+), Ca(2+), Na(+) and Mg(2+) and the acquisition of temporal concentration profiles of these species. The detection limits achieved were between 20 and 200 [micro sign]g l(-1) for all ions and the repeatability of peak areas and peak heights was better than 1%. The quantitative results were verified by analysing individual samples later in the laboratory with photometry and ion chromatography and the average deviations were found to be between 4 and 12%. This contribution presents a further step in the development of capillary electrophoresis towards a fully automated, low maintenance field method.     

饮用水源水中丙烯醛测定方法改进

对饮用水源水中丙烯醛的气相色谱标准测定方法作了改进,由直接进样改为吹扫捕集进样,由极性色谱柱改为中等极性色谱柱.方法在0.010 mg/L～0.100 mg/L范围内线性良好,最低检出限和检测下限分别为0.000 5 mg/L和0.002 mg/L,水样平行测定的RSD为2.8%～5.2%,平均加标回收率为90.0%～...