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61.
Summary Using a two-step liquid chromatographic separation on normalphase cartridges, crude extracts of diesel particulate matter
can be separated without time-consuming sample handling into special fractions which mainly contain slightly-polar oxygenated
polycyclic aromatic hydrocarbons (oxy-PAH) and nitrated polycyclic aromatic hydrocarbons (nitro-PAH). Subsequent analysis
was by fused-silica capillary gas chromatography on a SE54 column along with flame-ionisation (GC/FID) and positive-ion electron-impact
mass spectrometric detection (GC/MS) respectively. A number of individual oxy-PAH belonging to four different chemical classes
(ketones, quinones, anhydrides and aldehydes) and several individual nitro-PAH were characterized by their retention times
and mass spectra.
Presented at the 15th International Symposium on Chromatography, Nürnberg, October 1984 相似文献
62.
A sequential injection UV method was developed to determine benzophenone-4 (BZ4) and phenylbenzimidazole sulphonic acid (PBS) simultaneously, these being the most commonly used UV-filters in aqueous formulations used as sunscreen sprays. The selective elution of both was performed by on-line solid-phase extraction, by retention on a SAX microcolumn and separation by varying the pH of elution. The sensitivity obtained was 0.042±0.001 ml μg−1 for PBS and 0.0159±0.0003 ml μg−1 for BZ4. The limit of detection was 1.6 μg ml−1 for PBS and 0.6 μg ml−1 for BZ4. The R.S.D. of the results was 1-6% for PBS and 1-12% for BZ4. The method was validated using commercial sunscreen formulations with concentrations determined by a liquid chromatographic procedure. The two procedures gave comparable results. Automation of the method means the amount of reagents used and residues generated are decreased. The system allows the required analysis sequence to be programmed using suitable software. 相似文献
63.
S. V. Volkov S. V. Kutyakov A. N. Levov E. I. Polyakova Le Tuan An S. A. Soldatova P. B. Terentiev A. T. Soldatenkov 《Chemistry of Heterocyclic Compounds》2007,43(10):1260-1268
It has been established that on heating, 3-benzoyl-4-hydroxy-1-methyl-4-phenylpiperidine is ring-opened in the presence of
arylamines by a type of retroaldol reaction, with subsequent transamination of the intermediate Mannich base and the formation
of 3-arylamino-1-oxo-1-phenylpropanes. When using arylhydrazines this γ-piperidol is recyclized with the formation of 1,3-diarylpyrazoles
and their 4,5-dihydro derivatives. The mass spectral behavior of a series of 3-arylamino-substituted 1-phenylpropanones has
been studied.
__________
Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1486–1495, October, 2007. 相似文献
64.
The cure of a bismaleimide (BMI) neat resin modified with an aromatic diamine and a siloxane elastomer, has been studied by 13C solid state nuclear magnetic resonance. Two chemical reactions occur during the cure cycle; at a low temperature, Michael's reaction predominates, while at a high temperature the polymerization of the double bond maleimide creates the network. The degradation of this BMI material was characterized with isothermal and dynamic thermogravimetric analyses in air and in nitrogen. The BMI thermal stability is lower in nitrogen than in air. This behavior is an indication of oxygen participating in reactions at high temperatures. The activation energy (Ea) of thermal degradation was determined from isothermal data using an Arrhenius equation (In V vs. 1/T). The global Ea for the weight loss in air was found to be 91 kJ/mol. The nature and the evolution of the thermal degradation products were the combined analyzed by techniques of pyrolysis, gas chromatography and mass spectrometry. The major thermal decomposition products obtained in the temperature range of 300–700°C are identified as benzene, methyl formamide, aniline, toluene and isocyanate-derived products. 相似文献
65.
In this work, a kinetic study on the thermal degradation of carbon fibre reinforced epoxy is presented. The degradation is
investigated by means of dynamic thermogravimetric analysis (TG) in air and inert atmosphere at heating rates from 0.5 to
20°C min−1 . Curves obtained by TG in air are quite different from those obtained in nitrogen. A three-step loss is observed during
dynamic TG in air while mass loss proceeded as a two step process in nitrogen at fast heating rate. To elucidate this difference,
a kinetic analysis is carried on. A kinetic model described by the Kissinger method or by the Ozawa method gives the kinetic
parameters of the composite decomposition. Apparent activation energy calculated by Kissinger method in oxidative atmosphere
for each step is between 40–50 kJ mol−1 upper than E
a calculated in inert atmosphere.
The thermo-oxidative degradation illustrated by Ozawa method shows a stable apparent activation energy (E
a ≈130 kJ mol−1 ) even though the thermal degradation in nitrogen flow presents a maximum E
a for 15% mass loss (E
a ≈60 kJ mol−1 ).
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
66.
B. Kaufmann S. Souverain S. Cherkaoui P. Christen J. -L. Veuthey 《Chromatographia》2002,56(3-4):137-141
Summary A rapid analytical method has been developed for the mutual resolution of three steroidal compounds, withaferin A, iochromolide,
and withacnistin. Liquid chromatography was performed on a Chromolith analytical column (4.6 mm i.d.×50 mm), made from a cylindrical
silica rod, operated at a flow rate of 4 mL min−1 with a simple linear gradient prepared from 0.1% aqueous formic acid and 0.1% formic acid in acetonitrile. Under optimum
conditions simultaneous separation of the compounds was achieved in less than 7 min, one eighth the time required for conventional
LC separation. The overall analysis time was reduced without sacrificing chromatographic performance—essential for the resolution
of positional isomers such as iochromolide and withacnistin. The column was coupled to a single-quadrupole mass spectrometer
and the method was characterized by good performance in terms of repeatability, selectivity, linearity, and sensitivity. Detection
limits in the single-ion-monitoring mode were 0.15 μg mL−1 or below. Finally, the developed method was successfully applied to the determination of withanolides in extracts fromlochroma gesnerioides obtained by three different processes—traditional Soxhlet extraction and two faster methods, microwave-assisted extraction
and pressurized solvent extraction. 相似文献
67.
C. Maes J. Devaux R. Legras I. W. Parsons 《Journal of polymer science. Part A, Polymer chemistry》1995,33(12):1943-1955
A monofunctional maleimide-ended model compound was synthesized and purified. The thermal curing of this compound was followed by size exclusion chromatography and the molecular masses of the oligomers formed during the curing reaction were determined by mass spectroscopy. It was found that high molecular mass species were not thermally stable. At high temperature and after enough time, a strong decrease in the polydispersity of the oligomers and a significantly preferential formation of trimer were observed. From 13C-NMR characterization, a five membered ring structure was found for the trimer, which explains the thermal stability of this species. © 1995 John Wiley & Sons, Inc. 相似文献
68.
69.
稀土杂质元素直接影响高纯单金属稀土材料的整体性能,是高科技领域许多材料的重要组成部分。通过考察最佳的消解酸量、温度、时间、氧气反应气流量、稀释气流量,建立了基于三重四极杆电感耦合等离子体质谱仪(ICP-MS/MS)直接测定氧化铕中13种稀土杂质元素分析方法。该方法采用0.1%基体直接进样,可以很大程度提高前处理分析效率。利用碰撞模式测定氧化铕稀土中的Y、La、Pr、Nd、Sm、Gd、Tb、Dy、Ho、Er、Yb、Lu元素,氧气质量转移模式测定氧化铕中的Tm,两种模式结合可以有效去除多原子干扰,实现氧化铕的稳定测试分析。通过对氧化铕标准物质(GBW02902)直接测定分析,结果表明,在碰撞和氧气质量转移模式下,各元素线性相关系数(r)均大于 0.9999,方法检出限为0.001~0.023 mg/kg,测试精密度优于1.99%,13种元素的测试值都在认定值的不确定度范围之内。该分析方法操作简单,测试稳定,效率高,为实验室进行氧化铕材料中REE杂质的准确测试分析提供思路和借鉴。 相似文献
70.
自然界中砷和砷的化合物一般可通过水、大气和食物等途径进入人体,危害人体健康,原子荧光光谱法测定砷含量被广泛应用。为准确测定样品中砷的含量,以原子荧光光谱法(AFS)测定土壤中总砷含量为例,重点研究高价态砷(Ⅴ)还原为低价态砷(Ⅲ)的实验条件,采用正交实验进行条件优化,建立适合的实验方法。通过设计L9(34)正交实验,高价态砷的还原反应与四个因素有关,即与反应温度、反应时间、盐酸加入量和硫脲的用量呈一定的正相关,结果表明,四个因素中硫脲用量的影响最为显著,其次是盐酸加入量、反应时间和反应温度。通过对四个因素的多水平检验,优化后的实验条件为:硫脲用量2.0 mL、盐酸加入量10%、反应时间20 min、温度20~35 ℃(即普通室温)。采用土壤标准物质验证优化后条件的可行性,得出砷的测定值在标准值范围内,RSD在2.2%~4.2%,精密度和准确性均满足质控要求。优化后的实验条件使得操作简便易行,提高了工作效率。 相似文献