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101.
A capillary gas chromatographic method is described for the quantitative determination of liquid paraffin in blood. Paraffin is extracted from blood into n-heptane. After solvent evaporation and dissolution of the residue in 100–200 μl n-heptane one μl is injected into a gas chromatograph fitted with a fused silica capillary column (Permabond® OV-1-CB-0.1, 10 m × 0.32 mm i.d.) and flame ionization detector. Analysis is performed by using an oven program [50°C (3 min)?285°C (5 min), rise 10%min]. The sensitivity (1.5 ng hexadecane) and the reproducibility prove the applicability of the method for the determination of liquid paraffin in blood and for the study of the stability of the liquid paraffin hollow fiber membranes used in an extracorporeal liver support system. 相似文献
102.
Diglycidyl ether of 4,4′-dihydroxybiphenol (BPDGE) is a liquid crystalline epoxy. The biphenyl epoxy (diglycidyl ether of 3,3′,5,5′-tetramethyl-4,4′-biphenyl, TMBPDGE) has found great applications in plastic encapsulated semiconductor packaging. Phenol novolac (PN) was used as curing agent. The reaction kinetics of BPDGE/PN and TMBPDGE/PN systems in the presence of triphenylphosphine (TPP) were characterized by an isoconversional method under dynamic conditions using differential scanning calorimetry (DSC) measurements. The results showed that the curing of epoxy resins involves different reaction stages and the values of activation energy are dependent on the degree of conversion. The effects of curing temperature on their phase structure have been investigated with polarized optical microscopy and Wide-angle X-ray diffraction. With proper curing process, BPDGE showed a nematic phase when cured with PN. 相似文献
103.
Laure Gouriou Štěpán Vysko?il Pavel Ko?ovský 《Journal of organometallic chemistry》2003,687(2):525-537
The reaction of iso-cinnamyl acetate with NaC(Me)(CO2Me)2, catalysed by Pd-‘MOP’ (MOP=2-methoxy-2′-diphenylphosphino-1,1′-binaphthalene) is known to proceed with a regiochemical memory effect that results in the predominant generation of the branched alkylation product. The analogous reaction employing ‘MAP’ as ligand (MAP=2-N,N-dimethylamino-2′-diphenylphosphino-1,1′-binaphthalene) proceeds with ‘normal’ regioselectivity to generate predominantly the linear isomer of product. A 2H-NMR based analysis, employing quadrupolar coupling in a chiral liquid crystal matrix, has been developed to facilitate the simultaneous study of the regiochemical and stereochemical outcome of the reaction of both enantiomers of iso-cinnamyl ester substrates in 2H-labelled but racemic samples. The analysis allows the comparison of relative rates of two competing isomerisation processes occurring in the π-allyl intermediates in the Pd-catalysed reaction, one of which facilitates asymmetric induction, the other resulting in loss of regiochemical memory. It is demonstrated that the two processes are partially coupled and that this then limits the attainment of high global enantiomeric excess in the branched product to reactions that proceed with low regiochemical retention. A key factor for the observation of high regiochemical memory is found to be the nucleophilicity of the malonate anion and the electrophilicity of the Pd-π-allyl intermediate with reduction in the reactivity of either partner resulting in the onset of substantial loss of memory. 相似文献
104.
Sodium-dicyclohexyl- 18-crown-6 complex cation was used as carrier for the uphill transport of zinc as Zn(SCN)42? complex anion. By using L-cysteine as a metal ion acceptor in the receiving phase at the optimized pH of 7.6, the amount of zinc transport through the liquid membrane after 90 min was 97.2 ± 1.0%. The selectivity and efficiency of zinc transport from aqueous solutions containing equimolar mixtures of Ag+, Cd2+ Co2+, Cu2+, Fe2+, Ni2+, Pb2+, Pd2+, Sr2+, Bi3+, Cr3+ and Fe3+ ions was investigated. In the presence of NH2OH.HCl as a suitable masking agent in the source phase, the interfering effect of Cu2+ and Pb2+ ions was diminished drastically. 相似文献
105.
Using cotton as a solid-phase extraction sorbent of the precolumn, an on-line coupled precolumn preconcentration-liquid chromatography system with fluorescence detection was developed for the determination of PAHs in aqueous samples. Four PAHs including fluorene, phenanthrene, fluoranthene and benzo[k]fluoranthene were preconcentrated by a precolumn packed with 30 mg of absorbent cotton and then separated by C18 analytical column. When 100 ml of sample was enriched, the proposed procedure provided detection limits in the range of 0.5-57 ng l−1. Several water samples spiked with PAHs were analyzed with recoveries in the range of 92-119% at spiking level of 100 ng l−1 for fluorene, phenanthrene and fluoranthene, and 10 ng l−1 for benzo[k]fluoranthene, respectively. 相似文献
106.
As12Se44—: a New Selenoarsenate Anion with a Polyarsenic Cage in the Compound [Co(NH3)6]2As12Se4 · 12 NH3 Orange coloured crystals of [Co(NH3)6]2As12Se4 · 12 NH3 were prepared by the reduction of As4Se4 with a solution of sodium in liquid ammonia and subsequent precipitation with CoBr2. The X‐ray structure determination shows them to contain the selenoarsenate anion As12Se44—, which consists of a central As12‐cage with four exo‐bonded, formally negatively charged Se atoms. The structure of the As12‐cage is equivalent to the main polyphosphorus building unit of a known organopolyphosphane and of tubular P12 in the compound (CuI)3P12. 相似文献
107.
Summary The analysis of several phenylurea herbicides in different waters is described using an immunoaffinity column clean-up and
determination by high performance liquid chromatography. The pesticides were selectively retained on a solid phase extraction
column containing antibodies to chlortoluron and to isoproturon immobilised onto silica. Selected phenylureas were eluted
using a simple phosphate buffered saline/ethanol mixture at low pH. The immunoaffinity approach gave extracts free of interfering
substances and allowed detection limits comparable to those required for pesticides in water in the European Community. The
proposed method was successfully applied to the determination of chlortoluron, isoproturon, linuron and chlorbromuron in tap
and river water.
Presented at the 21st ISC held in Stuttgart, Germany, 15th–20th September, 1996 相似文献
108.
液晶聚酯与环氧嵌段共聚物的合成及表征 总被引:5,自引:0,他引:5
近年来 ,人们利用高分子液晶作为热固性环氧树脂的改性剂 ,不仅可以提高环氧树脂的韧性和强度 ,而且可以改善其热性能 ,为制备高性能的环氧树脂提供了一条新的途径[1,2 ] .目前报道所使用的液晶聚合物大多为液晶聚酯[3 ] 或液晶性聚氨酯[4] ,这些液晶聚合物与环氧树脂由于存在相容性不好的问题 ,给其实际应用带来了困难 .为了改善二者的相容性 ,本文采用溶液法合成了末端带有反应活性基团的聚酯型液晶聚合物 ,将它再与双酚A环氧预聚物反应 ,制得了高分子液晶环氧嵌段共聚物 ,其合成路线如下 :2HOCOOCH3+ HO(CH2 ) 6 OH H… 相似文献
109.
A delayed coincidence method, time-interval analysis (TIA), has been applied to successive – decay events on the millisecond time-scale. Such decay events are part of the 220Rn216Po (T1/2 145 ms) (Th-series) and 219Rn215Po (T1/2 1.78 ms) (Ac-series). By using TIA in addition to measurement of 226Ra (U-series) from -spectrometry by liquid scintillation counting (LSC), two natural decay series could be identified and separated. The TIA detection efficiency was improved by using the pulse-shape discrimination technique (PSD) to reject -pulses, by solvent extraction of Ra combined with simple chemical separation, and by purging the scintillation solution with dry N2 gas. The U- and Th-series together with the Ac-series were determined, respectively, from alpha spectra and TIA carried out immediately after Ra-extraction. Using the 221Fr217At (T1/2 32.3 ms) decay process as a tracer, overall yields were estimated from application of TIA to the 225Ra (Np-decay series) at the time of maximum growth. The present method has proven useful for simultaneous determination of three radioactive decay series in environmental samples. 相似文献
110.
二苯并-18-冠-6-甲醛聚合物柱色谱分离富集化学发光法测定痕量金 总被引:5,自引:0,他引:5
研究了用一种新的高分子冠醚聚合物(二苯并-18-冠-6-甲醛聚合物)作为色谱柱的固定相,分离富集痕量金,再用化学发光法进行测定;在盐酸介质中,高分子冠醚对金的吸附率可达100%,吸附的金可被硫脲完全解吸,吸附容量为19.40mg/g;化学发光法测定操作简便,效果令人满意;研究结果表明:把高分子冠醚聚合物作为分离富集手段与具有高灵敏度的化学发光法结合进行痕量分析是一种很有前途的方法。 相似文献