共查询到19条相似文献,搜索用时 125 毫秒
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微波皂化萃取气相色谱法测定生物样品中的多氯联苯 总被引:3,自引:0,他引:3
1引言 多氯联苯(PCBs)的性质稳定、毒性大,贻贝等海洋生物能摄取和富集海水中的PCBs,因此研究其中PCBs的测定具有重要意义。生物样品中 PCBs的测定一般要进行预分离处理,索氏萃取分离 PCBs耗时至少8h,加碱皂化生物组织再以液-液萃取提取PCBs需要在沸水浴中回流1~2h,微波直接革取能有效地分离环境样品中的PCBs。本文利用微波皂化萃取(MASE)气相色谱法(GC)测定生物样品中的多氯联苯,实验以未受PCBs污染的淡水鱼为空白,用正交试验系统优化了微波功率、微波加热时间、皂化及萃取溶… 相似文献
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P204萃取剂皂化过程中的物理化学性质及相区变化 总被引:3,自引:0,他引:3
P204萃取剂皂化过程中的物理化学性质及相区变化曾平,王贵清(湘潭大学化学系,湘潭,411105)关键词皂化P204萃取剂,物理化学性质,相区,微乳状液二-(2-乙基己基)磷酸(简称P204或HA)是一种良好的工业螫合萃取剂,在湿法冶金中得到广泛应用... 相似文献
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酸性磷萃取剂在皂化过程中的结构变化与萃合物的组成 总被引:15,自引:1,他引:14
本文研究了酸性磷酸酯(D2EHPA等)皂化过程和萃取前后有机相结构的变化,证实了酸性磷酸酯萃取剂在皂化过程中生成微乳状液,进一步阐明萃取稀土离子时,在微乳状液的油水界面上发生离子交换反应,生成具有螫合型结构的萃合物,同时伴随着有机相中微乳状液的破乳过程。在用完全皂化的D2EHPA-仲辛醇-煤油溶液萃取二价离子时,得到萃取有机相中苹合物的组成为MA2,而不是通常认为的MA2·2HA,从而可以提高萃取容量。 相似文献
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针对工业上广泛应用的氨水皂化HEHEHP[2-乙基己基磷酸单乙基己基脂]萃取剂分离稀土元素产生含有很高浓度NH+4的废水,对环境污染严重的问题,通过在稀土氯化物溶液中加入配合剂醋酸钠(CH3COONa),采用非皂化的HEHEHP萃取剂萃取重稀土元素Tm。研究了该体系中水相酸度、有机相浓度、乙酸钠浓度等因素对Tm3+分配比的影响。结果表明:HEHEHP-HCl-Na AC体系对Tm3+萃取过程遵循阳离子交换机制;萃取液中形成的乙酸-乙酸盐缓冲溶液能够维持萃取水相酸度恒定,萃取过程中有机相不再需要皂化,有效避免HEHEHP皂化产生含NH+4废水污染环境的问题。 相似文献
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稀土与酸性萃取剂形成的溶液聚集态结构 总被引:7,自引:0,他引:7
用Fourier变换红外光谱(FT—IR)和光子相关光谱(PCS)研究了皂化的有机磷酸酯类萃取剂和环烷酸萃取剂在正庚烷或正庚烷与2-辛醇的混合溶剂中所形成的聚集物,以及萃取稀土元素后有机相聚集物的变化.结果表明,有机磷酸酯在正庚烷中皂化后形成反向胶团((?)_h<5.0nm),其平均流体力学半径与萃取剂分子的长度相当;2-辛醇的加入可增大反向胶团的粒径.环烷酸皂化后能在混合溶剂中形成W/O型微乳状液(5.0 nm<(?)_h<100 nm).皂化萃取剂萃取稀土元素后,有机相中形成不稳定的聚集物,继而产生聚凝.讨论了聚凝过程的可能机理. 相似文献
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微波技术在有机合成中的应用 总被引:48,自引:1,他引:48
评述了微波加热技术在有机合物的烃基化,酯化和皂化,磺化,烯烃加成,Diels-Alder缩合,氧化,环化与开环及重排等反应中的应用,参考文献73篇。 相似文献
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Ozcan S 《Journal of separation science》2011,34(5):574-584
A method was developed for viable and rapid determination of seven polychlorinated biphenyls (PCBs) in water samples with vortex-assisted liquid-liquid microextraction (VALLME) using gas chromatography-mass spectrometry (GC-MS). At first, the most suitable extraction solvent and extraction solvent volume were determined. Later, the parameters affecting the extraction efficiency such as vortex extraction time, rotational speed of the vortex, and ionic strength of the sample were optimized by using a 2(3) factorial experimental design. The optimized extraction conditions for 5 mL water sample were as follows: extractant solvent 200 μL of chloroform; vortex extraction time of 2 min at 3000 rpm; centrifugation 5 min at 4000 rpm, and no ionic strength. Under the optimum condition, limits of detection (LOD) ranged from 0.36 to 0.73 ng/L. Mean recoveries of PCBs from fortified water samples are 96% for three different fortification levels and RSDs of the recoveries are below 5%. The developed procedure was successfully applied to the determination of PCBs in real water and wastewater samples such as tap, well, surface, bottled waters, and municipal, treated municipal, and industrial wastewaters. The performance of the proposed method was compared with traditional liquid-liquid extraction (LLE) of real water samples and the results show that efficiency of proposed method is comparable to the LLE. However, the proposed method offers several advantages, i.e. reducing sample requirement for measurement of target compounds, less solvent consumption, and reducing the costs associated with solvent purchase and waste disposal. It is also viable, rapid, and easy to use for the analyses of PCBs in water samples by using GC-MS. 相似文献
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植物内源激素的反相高效液相色谱法测定 总被引:37,自引:0,他引:37
报道了以6-N-苄基腺嘌呤(BA)为内标的反相高效液相色谱法测定玉米素(ZT)、赤霉素(GA3)、激动素(KT)、3-吲哚乙酸(IAA)和脱落酸(ABA)等5种植物内源激素的条件;采用μBondapakC18柱、乙腈-甲醇-0.6%(φ)乙酸流动相、检测波长254nm,建立了一种从植物中提取5种激素的样品处理方法,并测定了马铃薯块茎中的5种植物内源激素的含量。 相似文献
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《Analytical letters》2012,45(15):2161-2175
An on-line Soxtec extraction and cleanup method is optimized for PCBs determination in mussel samples. Soxtec extraction conditions have been optimized using two factorial designs. Optimized extraction parameters were sample weight, anhydrous sodium sulfate weight, solvent volume, alumina weight, and boiling and rinsing times. The results suggest that all PCBs congeners extracted by Soxtec appeared statistically affected by solvent volume. Soxtec quantitative recoveries (8– ?115%) were achieved for all PCBs and method precision (RSD <12%) was satisfactory. The optimized method is compared with three different applied extraction methods, Soxhlet, accelerated solvent extraction, and microwave-assisted extraction. This latter presents the cleanup step on column or assisted by polypropylene membranes. The extraction effectiveness of the four different applied extraction methods for the determination of PCBs in mussel was similar. 相似文献
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Xinsheng Fang Yingzi Wang Jianhua Wang Jin Zhang Xin Wang 《Journal of separation science》2013,36(16):2672-2679
An optimized microwave‐assisted extraction (MAE) method and RP‐HPLC method were developed for the simultaneous extraction and determination of rutin, forsythiaside A, and phillyrin in the fruits of Forsythia suspensa. The key parameters of the open‐vessel MAE process were optimized. A mixed solvent of methanol and water (70:30, v/v) was most suitable for the simultaneous extraction of the three components. The sample was soaked for 10 min before extraction. The optimized conditions were: microwave power 400 W, temperature 70°C, solvent‐to‐material ratio 30 mL/g, and extraction time 1 min. Compared to conventional extraction methods, the proposed method can simultaneously extract the three components in high yields and was proved to be a more rapid method with a lower solvent consumption. The optimized HPLC–photodiode array detection analysis was validated to have good linearity, precision, accuracy, and sensitivity. The developed MAE followed by RP‐HPLC is a fast and appropriate method for the simultaneous extraction and determination of rutin, forsythiaside A, and phillyrin in the fruits of F. suspensa. 相似文献
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Ming-Yuen Tsai Ponnusamy Vinoth Kumar Hong-Ping Li Jen-Fon Jen 《Journal of chromatography. A》2010,1217(12):1891-1897
A microwave-assisted headspace controlled-temperature liquid-phase microextraction (HS-CT-LPME) technique was applied for the one-step sample extraction of hexachlorocyclohexanes (HCHs) from aqueous samples with complicate matrices, followed by gas chromatographic (GC) analysis with electron capture detector (ECD). Microwave heating was applied to accelerate the evaporation of HCHs into the headspace and an external-cooling system was used to control the temperature in the sampling zone for HS-LPME. Parameters affecting extraction efficiency, such as LPME solvent, sampling position and temperature, microwave power and irradiation time (the same as sampling time), sample pH, and salt addition were thoroughly investigated. From experimental results, the following conditions were selected for the extraction of HCHs from 10-mL water sample (pH 2.0) by using 1-octanol as the LPME solvent, with sampling done at 38 °C for 6 min under 167 W of microwave irradiation. The detections were linear in the concentration of 0.1–10 μg/L for α-HCH and γ-HCH, and 1–100 μg/L for β-HCH and δ-HCH. Detection limits were 0.05, 0.4, 0.03 and 0.1 μg/L for α-, β-, γ- and δ-HCH, respectively. Environmental water samples were analyzed with recovery between 86.4% and 102.4% for farm-field water, and between 92.2% and 98.6% for river water. The proposed method proved to serve as a simple, rapid, sensitive, inexpensive, and eco-friendly procedure for the determination of HCHs in aqueous samples. 相似文献
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Optimization of a microwave-assisted extraction method for the analysis of polychlorinated biphenyls in ash samples 总被引:2,自引:0,他引:2
Ramil Criado M Rodríguez Pereiro I Cela Torrijos R 《Journal of chromatography. A》2003,985(1-2):137-145
An alternative method for the extraction of polychlorinated biphenyls (PCBs) in ash samples, which is less time and solvent consuming than Soxhlet extraction, is presented. A study was carried out to evaluate the possibilities of microwave-assisted extraction (MAE) to determine exactly which parameters affect the efficiency of the process, since direct extrapolation of extraction conditions for PCBs in other solid matrices, failed when applied to coplanar congeners in ash samples. Influence of the organic solvent on the yield of the extraction was first evaluated using two ash samples with different percentages of carbon. Once the extraction solvent was fixed, the effects of solvent volume, extraction temperature and extraction time were investigated using an experimental design. It was found that the volume of organic solvent played a more important role in the extraction efficiency than the other factors. In the optimal conditions microwave extractions were performed at 110 degrees C. for 10 min and using 30 ml of toluene. Recoveries higher than 80% were obtained for all the highly chlorinated congeners. including coplanar species, in a spiked ash sample containing a relatively high concentration of carbon. The proposed method was also applied to the determination of PCBs in a reference material of urban dust. Recoveries were similar to those obtained for spiked ash samples. 相似文献