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61.
A method has been developed to determine the boiling point distribution of sulfur compounds in light cycle oils (LCO'S). The method chosen for this analysis was GC with a flame photometric detector (FPD) and pyrolyzer. Tests were carried out to evaluate the recovery efficiency, repeatability, and accuracy of the method. Repeatabilities within 2% were obtained. The recovery of benzothiophenes and dibenzothiophenes was close to 100%; this was important because these are the major sulfur components in LCO's. No hydrocarbon or solvent interferences were observed with the use of the pyrolyzer, even for a 95% solvent level. Comparison with results from other techniques showed that the method accurately determined the levels of sulfur compounds in the LCO boiling point range. 相似文献
62.
Nitro musks in cosmetic products—determination by headspace solid-phase microextraction and gas chromatography with atomic-emission detection 总被引:1,自引:0,他引:1
Summary The combination of headspace solid-phase microextraction with atomic-emission detection enables highly selective and sensitive
determination of itro musk compounds in cosmetic products. Sample preparation is considerably simplified; there is no solvent
extraction step. Enrichment is influenced by the type and amount of cosmetic product investigated. The lowest amount giving
well detectable peaks is 1 mg musk compound per kg sample. Calibration curves obtained from spiked solutions of selected reference
cosmetics in water show very good linearity. Relative standard deviations of peak areas from repeated measurements are usually
<10%.
Presented at the 21st ISC held in Stuttgart, Germany, 15th–20th September, 1996 相似文献
63.
Thermal diffusivity, heat capacity, and density of polyvinyl chloride/polycaprolactone (PVC/PCL) blends were measured by the laser flash method, DSC, and pycnometry, respectively. The thermal conductivity of the PVC/PCL blends was determined from the results. The miscibility of the blend and crystallinity of PCL were determined by DSC. The effect of blend structure on thermal conductivity is discussed. The phase compositions of the PVC/PCL blends are of three types depending on PCL content: i.e., up to 33%, from 33 to 70%, and above 70% PCL by weight. Thermal conductivity, thermal diffusivity, and heat capacity of the PVC/PCL blends are strongly affected by the phase composition of the blend, which changes in a complicated way with PCL content. © 1994 John Wiley & Sons, Inc. 相似文献
64.
Data about the existence of native HO? CH2? CH2? OH (MEG) in natural wines and champagne has led to delicate questions because of legal decisions already made to declare wine or champagne illegal for sale if the MEG concentrations found are above 10 mg/liter. Action has been taken because of the DEG (diethylene glycol) disaster in European wines of 1985…86. An incorrect legal decision was made due to the belief that MEG cannot be produced biochemically by grape vines. A further reason may be lack of correct data on native MEG trace concentrations, as a result of the special behavior of this diol. As first member of a homologous series whose higher members (C4) are normally found in all wines at quite high concentration levels, MEG shows extremely adsorptive behavior. The solution of the chromatographic problems is summarized in this paper. MEG concentrations in Riesling as example are in the range of 2 to 6 mg/liter and can easily be increased by biotechnological steps to a level of around 10 to 60 mg/liter. This is again due to the specific adsorptive behavior of MEG, which can be enriched on filter surfaces and displaced when the wine acidity changes with changing types. In order to control and guarantee the qualitative and quantitative results of MEG analyses we used a combination of Deans heart cutting on-line with Multi-Chromatography. It was easy to produce false data by many otherwise useful single column or two-dimensional separation processes, etc. 相似文献
65.
鲤鱼体中鱼腥味物质的提取和鉴定 总被引:2,自引:0,他引:2
采用同时蒸馏萃取法提取鲤鱼鱼体中的挥发和半挥发性有机物,用GC/MS从提取物中分析鉴定出鱼腥味和疑是鱼腥味物质16种。包括醛、烯醛、酮和呋喃4类化合物。其中己醛、庚醛和2,4-二烯癸醛被确认为鱼腥味的化合物。研究发现,这些物质总量在鲤鱼体的鱼鳞、鱼鳃和鱼肉的分布呈现下降趋势,且其总量与鱼腥味强度之间具有可比较的对应关系。 相似文献
66.
From flash photolysis data of benzil and 2,2′-dichlorobenzil, the role of conformeric triplets in the formation of hydrogen
adduct radicals has been discussed. The planar relaxed triplet absorbing at 470 nm is less efficient in forming a hydrogen
adduct radical as compared to its puckered conformeric partner. Among the hydrogen donors, triethyl amine and isopropanol,
the former is more efficient in converting puckered triplets and less efficient in the case of planar conformers. Absorptions
of radicals and radical anions of 2,2′-dichlorobenzil appear at 355 nm and 460 nm respectively. These are blue-shifted as
compared to those of the parent compound benzil appearing at 370 nm and 540 nm, respectively. This blue-shift has been discussed
in terms of steric hindrance due to ortho-substitution. 相似文献
67.
A new, high performance liquid chromatography method has been developed for the separation of monovinyl- and divinyl-protochlorophyllides, using commercially available, C30 reverse phase column and isocratic elution. This method can be used both for analytical applications and preparative scale purification of monovinyl- and divinyl-protochlorophyllides using the same column where submilimolar concentrations of the crude protochlorophyllide extract can be separated in one run. The purity of the obtained protochlorophyllides was demonstrated by spectroscopic methods, as well by the formation of aggregates in toluene. 相似文献
68.
Arsenic speciation analysis in marine samples was performed using ion chromatography (IC) with inductively coupled plasma mass spectrometry (ICP‐MS) detection. The separation of eight arsenic species, viz. arsenite, monomethyl arsonic acid, dimethylarsinic acid, arsenate, arsenobetaine, tetramethylarsine oxide, arsenocholine and tetramethylarsonium ion was achieved on a Dionex AS4A (weaker anion exchange column) by using a nitric acid pH gradient eluent (pH 3.3 to 1.3). The entire separation was accomplished in 12 min. The detection limits for the eight arsenic species by IC–ICP‐MS were in the range 0.03–1.6 µ g l?1, based on 3σ of the blank response (n = 6). The repeatability and day‐to‐day reproducibility were calculated to be less than 10% (residual standard deviation) for all eight species. The method was validated by analyzing a certified reference material (DORM‐2, dogfish muscle) and then successfully applied to several marine samples, e.g. oyster, fish muscle, shrimp and marine algae. The low power microwave digestion was employed for the extraction of arsenic from seafood products. Copyright © 2004 John Wiley & Sons, Ltd. 相似文献
69.
František Toman Ludvík Beneš 《Journal of inclusion phenomena and macrocyclic chemistry》2007,59(3-4):231-236
Differential molar adsorption enthalpies (DMAE) were determined by gas chromatographic measurements of specific retention
volume of vapors on the surface of two forms of Mg–Al hydrotalcite. A linear dependence of the DMAE on the number of the carbon
atoms in hydrocarbons was observed for both form of hydrotalcite. The dependence of the differential molar adsorption enthalpies
on the number of chlorine atoms in organic molecules is discussed. A linear dependence of DMAE on the molecular weight of
chloroderivatives of methane and ethylene on the basic form in an order monochloromethane < dichloromethane < trichloromethane
or vinylidene chloride < 1,1-dichloroethylene < trichloroethylene was found. 相似文献
70.
A liquid chromatography-mass spectrometry method for the determination of the coccidiostats metronidazole, ronidazole, dimetridazole,
secnidazole, tinidazole and ipronidazole in feedstuff was developed. The 5-nitroimidazoles were extracted from animal feed
with a pH 2 phosphate buffer solution followed by a solid phase extraction procedure based on HLB cartridges. The liquid chromatographic
separation of the extracts was performed on a C18 bonded silica column applying a gradient of elution with pH 4.3 ammonium acetate buffer solution and acetonitrile. Quantification
for each 5-nitroimidazole was carried out monitoring its molecular ion [M + H]+ obtained by positive electrospray ionisation mode. A pool of feedstuffs was used to optimise and validate the method. Linearity,
quantification limit, intra-day and inter-day reproducibility and accuracy were estimated using this pool of feedstuffs spiked
with the drugs. For the confirmatory assay, several fragment ions from each 5-nitroimidazole were obtained and monitored.
The method was applied successfully to determine 5-nitroimidazoles in feedstuff at level of 0.05 mg kg−1. 相似文献