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991.
Analytical methods for the simultaneous analysis of lindane, chlorpyriphos, z-chlorfenvinphos, endosulfan A and B, 4,4'-DDE, 4,4'-TDE, acrinathrine, bromopropylate, tetradifon, coumaphos and fluvalinate in pure beeswax samples are studied. For the analysis of bleached beeswaxes, a liquid-liquid extraction with acetonitrile followed by a clean-up on polymeric cartridges is the best option in terms of recovery and precision. However, some interferences that hinder the identification and quantification of important varroacides are found when non-bleached beeswaxes are analyzed. The analysis of all compounds in the latter samples require a clean-up by coupling an ODS cartridge before the polymeric cartridge. Considerations about the influence of the matrix in the quantitative analysis by a classical external standard calibration are also made and the use of a matrix-matched calibration is advised. Recoveries resulted to be about 100% with coefficients of variation between 10% and 20% (n = 5) for concentrations of 0.5 and 5 mg/kg. 相似文献
992.
The D/L ratio of aspartic acid enantiomers in proteins of low turnover is generally accepted as a reliable procedure for age determination. In our study, twelve samples of eyetooth dentin were analyzed for age determination. The pure insoluble collagen isolated from eyetooth dentin was obtained by an EDTA demineralization process. Free amino acids obtained after collagen hydrolysis were converted into o-phthaldialdehyde-N-acetyl-L-cysteine (OPA-NAC) derivatives for HPLC analysis under modified conditions and into trifluoroacetic acid isopropyl esters for GC analysis, respectively. The modified HPLC procedure used phosphate buffer and acidified sample matrix prior to injection which resulted in suppression of peak tailing of both diastereomers, thus allowing achievement of both good selectivity and good resolution. To ensure the high accuracy of the developed method the other parameters, i.e. specificity, precision, linearity, LOD, and LOQ, were also determined. Nine collagen samples covering the age range of 18 to 84 years were used for the determination of coefficient of racemization (KR) and calculation of parameters for age estimation. The regression equations for the data set analyzed were as follows: KR= 0.0005 x age + 0.0262 (R2 = 0.9639) for HPLC, and KR= 0.0006 x age + 0.0319 (R2 = 0.9374) for GC, respectively. 相似文献
993.
Regert M 《Journal of separation science》2004,27(3):244-254
Although organic materials are very sensitive to biochemical alteration processes, they may be preserved for millennia in various archaeological contexts. Remains of adhesives made during prehistory were discovered at different sites, in the form of residues adhering to flint tools and ceramic vessels or as free lumps in sediment. To characterise the natural substances exploited for adhesive production during late prehistory, we undertook GC and GC/MS analysis of 90 samples from 8 sites dating from the Neolithic to Iron Age periods. This paper discusses our approach to the study of organic adhesives preserved in archaeological contexts, with a particular focus on the presentation of the various categories of organic adhesives that we analysed and the choice of chromatographic conditions adapted to the specificity of such samples. The results obtained show that birch bark tar, a triterpenoid adhesive made by destructive distillation of white birch bark, was predominantly used during the neolithic period even though other materials such as various barks or organic fossil substance were also used. During the Bronze and Iron ages, which follow the Neolithic period, adhesive production is evolving through the expansion of the range of the natural substances used (identification of diterpenoid pine resin) and the addition of beeswax as a plasticiser to birch bark tar. By combining chromatographic analysis and archaeological data, it was thus possible to follow the evolution of adhesive making at the end of prehistory, testifying to the inventiveness of the craftsmen whatever the period considered. 相似文献
994.
Magnetic field has been applied to a copper vapor laser with an intention of improving the laser characteristics by inner gas convection. The convection induced by the J×B cross-field discharge (the Lorentz force) is used for partially replacing or mixing the laser medium in a highly heated discharged region with relatively cold gas surrounding the region. It is observed that the output power increases with the increase of the magnetic field. A 23% increase in the output power is obtained with a magnetic field of 150 gauss. The cross-field discharge causes an increase in the peak discharge voltage and a reduction in the initial part of discharge current (Phantom current). Based on the results observed, the possible mechanisms for increasing the power are discussed. 相似文献
995.
996.
三烷基氧膦是用于高放废液处理的萃取剂,本文试验了在辐照剂量为1×10^4Gy-1×10^6Gy时TRPO损失率。结果表明,100%(V/V)TRPO在λ辐照剂量10^4Gy-10^6Gy变化时,辐解损失率为1.2%-1.6%;30%(V/V)TRPO-煤油在辐照剂量10^4Gy-10^5Gy时,辐解损失率基本不变(0.33%-0.34%),而在1×10^6Gy时增加到0.77%。均低于磷酸三丁酯的 相似文献
997.
998.
GC headspace analyses of various aromatizing herbs have been compared with those relating to the essential oils, obtained by steam distillation, of the same plants. In this way it was possible to establish the most significant differences between the composition of a herb flavor and that of its essential oil. In particular, we observed some very volatile compounds in the headspace samples which were absent from the essential oil; these components may make an important contribution to the herb flavor. The identification of these substances is still in progress. 相似文献
999.
Christian J. Simensen 《Fresenius' Journal of Analytical Chemistry》1978,292(3):207-212
Summary A quantitative gas-chromatographic method (molecular sieve column, FID) for the determination of Al4C3 in aluminium and magnesium has been developed. The effect of methane from external sources has been investigated and eliminated. Metallographic analysis of carbides in polished specimens were consistent with the gas-chromatographic measurements within a factor of 2. The discrepancy can be explained by the large uncertainties in light microscopy analysis of the small carbides. Analysis of commercial magnesium shows that the metal contains ca. 2–9 ppm of Al4C3. The concentration of carbides in aluminium from the electrolysis cell is in the range of 10–35 ppm and in the final product of ca. 2–12 ppm Al4C3. CaC2 has been detected in a few magnesium and aluminium samples by means of gas-chromatography and microprobe analysis.
Gas-chromatographische Analyse von Carbiden in Aluminium und Magnesium
Zusammenfassung Zur Bestimmung von Al4C3 in Aluminium und Magnesium wurde eine quantitative gas-chromatographische Methode (MolekularsiebSäule, FID) entwickelt. Der Einfluß von Methan aus äußeren Quellen, wurde untersucht und ausgeschaltet. Die metallographischen Untersuchungen von Carbiden an polierten Proben stimmten mit den Ergebnissen der gas-chromatographischen Messungen mit einem Faktor von 2 überein. Der Unterschied kann durch die großen Unsicherheiten bei der lichtmikroskopischen Analyse der kleinen Carbide erklärt werden. Die Analyse des technisch reinen Magnesiums zeigt, daß das Metall ca. 2–9 ppm Al4C3 enthält. Die Konzentration von Carbiden in elektrolytisch raffiniertem Aluminium liegt im Bereich 10–35 ppm und im Endprodukt bei ca. 2–12 ppm Al4C3. CaC2 wurde in einigen Magnesium- und Aluminiumproben mit Hilfe von gas-chromatographischen und Mikrosondenuntersuchungen festgestellt.相似文献
1000.
A procedure is described in which a wide bore capillary column is used as an alternative to the more traditional packed column for the quantitative analysis of amino acids as their N-heptafluorobutyryl isobutyl ester (HBB) derivatives. The column, installed in a gas chromatograph previously configured for use with a packed column, is shown to give good reproducibility by repeated determination of amino acid response factors (RSD values for all amino acids are below 3%). A number of problems, encountered during the use of this column, are discussed and suitable techniques to overcome them are reported. 相似文献