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991.
Single crystals of potassium iron hydrogen phosphate, KFe3(HPO4)2(H2PO4)6 · 4 H2O, were prepared hydrothermally by heating a mixture of Fe2O3, H3PO4 and K2CO3 with a small amount of water. It crystallizes monoclinic, space group C2/c (N° 15 Int. Tab.) with Z = 4 and a = 1701(2), b = 960.4(5), c = 1750(1) pm, β = 90.88(7)°. The crystal structure was solved by using 1716 unique reflections F0 > 4σ(F0) with a final wR2 value of 0.126 (SHELXL-93). The main feature of the crystal structure are layers formed by PO4-tetrahedra around the FeO6-octahedra parallel to (001). K+ and H2O molecules connect these layers. Effective Coordination Numbers (ECoN), Mean Fictive Ionic Radii (MEFIR), Charge Distribution (CHARDI) and the Madelung Part of Lattice Energy (MAPLE) are calculated for the title compound. The existence of hydrogen bonds is confirmed by these calculations. 相似文献
992.
Reactions of organo(trichloromcthyl)silanes RMc2SiCCl3 (R = Me, Ph, Mc3Si) with aluminum chloride have been studied. The interaction of trimetltyl(tricltlorometltyl)silane with AlCl3 carried out in cyclohexane or in benzene leads to Me3SiCHCI2 (in 75 % yield) or ClMe2SiCPh2Me (in 70 % yield), respectively; whereas no conversions are observed inn-hexane and methylene chloride. Treatment of dimetltyl(phenyl)(ricltloromethyl)silane with aluminum chloride in an-C5H12/CH2CI2 mixture gives an aromatic cross-linked insoluble polymer. The reaction of pentamethyl(trichloromcthyl)disilane (R = Mc3Si) with AICl3 in pentane affords the rearrangement product, Me3SiCCl2SiMc2Cl, in 65 % yield. In methylene chloride the further cleavage of the disilane occurs to yield Me2SiCl2 and CH2=CHMe2SiCl.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1511-1515, June, 1996. 相似文献
993.
On the Sodium Tetrahydroxoaluminate Chloride Na2[Al(OH)4]Cl The hitherto unknown compound Na2[Al(OH)4]Cl was prepared by crystallisation from a NaCl containing sodium aluminate solution. According to the X-ray single crystal investigation (tetragonal, space group P4/nmm, a = 7.541 Å, c = 5.059 Å, Z = 2) the compound represents the first example of a crystalline hydroxoaluminate with monomeric [Al(OH)4]? anions. Cl? shows a quadratic anti prismatic coordination to 4 Na+ and over hydrogen bonds to 4 O2? while Na+ is octahedrally coordinated by 4 O2? and 2 Cl? (axial). The results of the crystal structure analysis are confirmed by 27Al and 23Na MAS NMR investigations. Na2[Al(OH)4]Cl decomposes at about 200°C without intermediates under formation of β-NaAlO2 and NaCl. 相似文献
994.
995.
R. Holm und S. Storp 《Fresenius' Journal of Analytical Chemistry》1978,290(4):273-288
Zusammenfassung ESCA (nach Siegbahn: Electron Spectroscopy for Chemical Analysis) beruht auf dem Photoeffekt an inneren Atomorbitalen und ist auf alle Substanzen anwendbar. Die Routineuntersuchungen werden überwiegend an Festkörpern durchgeführt. Informationsträger sind Photo- und Augerelektronen, die verlustfrei von der Festkörperoberfläche emittiert werden. Auf Grund der Oberflächenempfindlichkeit gehört ESCA zu den mikrochemischen Verfahren. Die erfaßte Schichtdicke ist gegeben durch die Austrittstiefe der Photo- und Augerelektronen. Sie beträgt einige Monolagen, maximal 100 Å. Man kann davon ausgehen, daß bei einer untersuchten Fläche von 0,5 cm2 und homogener Verteilung eines Elementes in den obersten 100 Å eine Konzentration von 1 % noch sicher nachgewiesen wird. Die Empfindlichkeitsunterschiede von Element zu Element liegen innerhalb eines Faktors 10. Matrixeffekte sind noch wesentlich geringer. Deshalb sind gute Voraussetzungen für eine quantitative Analyse gegeben. ESCA ist zwar nicht direkt ein Verfahren zur Spurenanalyse, wohl aber nach geeigneter Anreicherung. Der besondere Vorteil von ESCA liegt darin, daß man nicht nur Elemente nachweist, sondern an Hand von chemischen Verschiebungen, Linienaufspaltungen und Shake-up-Satelliten zuverlässige Aussagen über ihren Bindungszustand erhält. Weiterhin kann innerhalb des Bereiches der Austrittstiefe der Photoelektronen differenziert werden; dadurch ergeben sich Möglichkeiten zur zerstörungsfreien Aufnahme von Tiefenverteilungen von Elementen und Verbindungen. Zum Vordringen in tiefere Schichten kann ESCA mit abbauenden Verfahren gekoppelt werden. Nach Ionenbeschußabbau ist wegen ioneninduzierter Reaktionen in der Regel jedoch kein Verbindungsnachweis mehr möglich.
ESCA: A method for the determination of elements and their valence states in the surfaces of solids
Summary ESCA — or Electron Spectroscopy for Chemical Analysis (the term used by its inventor, Siegbahn)-is based on the effects of X-rays on the inner orbitals of atoms and is applicable to all substances. Routine ESCA investigations are carried out chiefly on solids. The information is provided by photo- and Auger electrons, which are emitted from the surfaces of solids without energy losses. Because of its surface sensitivity ESCA may be regarded as a microchemical method. The comprehended layer thickness is given by the escape depths of the photo- and Auger electrons. The range is from a few monolayers to 100 Å. As a rule, an element that is distributed homogeneously in the uppermost 100 Å of an area of 0.5 cm2 can still be detected reliably at a concentration of 1%. The differences in sensitivity from element to element are within a factor of ten. Matrix effects are considerably smaller still. ESCA is therefore well suited for quantitative analysis. Though not directly suitable for trace analysis, ESCA can be used for that purpose after appropriate enrichment techniques have been applied. The special advantage of ESCA is that, in addition to detecting elements, it provides reliable information on their valence states by means of chemical shifts, line splitting and shake-up satellites. Apart from this, ESCA permits in-depth discrimination within the range of the escape depths of the photo electrons; it therefore provides opportunities for the non-destructive recording of the depth distributions of elements and compounds. For investigation of lower layers, ESCA can be combined with methods which involve the removal of outer layers. After removal of layers by ion bombardment, however, ion-induced reactions generally prevent the detection of compounds.
Hauptvortrag auf dem Internationalen Symposium für mikrochemische Arbeitsmethoden (ISM) Davos, Mai 1977 相似文献
996.
A method is described for the gas-chromatographic determination of the diastereomers of vitamin K1 (phylloquinone) in the form of their dihydro dimethyl ethers. The reported method of derivatization and chromatographic analysis in conjunction with optical rotation measurements are useful approaches for characterization of vitamin K1 samples with respect to their origin. 相似文献
997.
The main approaches that have been taken to chemically modify polymer surfaces are introduced and reviewed. These are wet chemical oxidation, plasma treatment, classical organic chemistry, and attachment of polymer chains. The extent to which each of these approaches can produce the specific modifications desired is discussed, and any unwanted effects that commonly occur are cited. Finally, the need for using several methods of surface analysis in concert to obtain adequate surface characterization is described. 相似文献
998.
Y. Li N. Obando F. Tschen R. J. Morgan 《Journal of Thermal Analysis and Calorimetry》2006,85(1):125-129
Thermal analysis of phenylethynyl end-capped imide oligomer AFR-PEPA-4
was performed to characterize cure reaction, thermal stabilities and semicrystalline
behavior of AFR-PEPA-4 oligomer and its cured polyimide. Cured AFR-PEPA-4
polyimide showed high T
gs
up to 418°C. Both AFR-PEPA-4 oligomer and polyimide exhibit excellent
thermal stabilities comparable to PETI-5 polyimides. AFR-PEPA-4 imide oligomer
has a T
m of 330°C
and exhibits spherulite crystalline morphology in the film. The crystallinity
in AFR-PEPA-4 films could not be regenerated under any annealing conditions
after the initial melt. 相似文献
999.
通过表面张力和等温滴定量热方法,研究了非离子表面活性剂Tween-20与牛血清白蛋白(BSA)的相互作用. 结果表明,BSA与Tween-20的相互作用较弱,当Tween-20浓度增大时,能将吸附于表面上的BSA分子取代. BSA/Tween-20混合体系的性质随温度的变化趋势与单一非离子型表面活性剂相似. BSA浓度在3.7×10-5~11.1×10-5 kg•L-1范围内,Tween-20的cmc不随BSA浓度的变化而变化. 当Tween-20的含量一定时,Tween-20与BSA相互作用过程的热效应也与BSA 的浓度无关. BSA/Tween-20混合体系的热力学参数表明, BSA的存在使Tween-20的cmc减小,体系的熵变增大. 相似文献
1000.
Sorel Tchewonpi Sagu Eva Landgrber Michal Rackiewicz Gerd Huschek Harshadrai Rawel 《Molecules (Basel, Switzerland)》2020,25(24)
Sorghum is of growing interest and considered as a safe food for wheat related disorders. Besides the gluten, α-amylase/trypsin-inhibitors (ATIs) have been identified as probable candidates for these disorders. Several studies focused on wheat-ATIs although there is still a lack of data referring to the relative abundance of sorghum-ATIs. The objective of this work was therefore to contribute to the characterization of sorghum ATI profiles by targeted proteomics tools. Fifteen sorghum cultivars from different regions were investigated with raw proteins ranging from 7.9 to 17.0 g/100 g. Ammonium bicarbonate buffer in combination with urea was applied for protein extraction, with concentration from 0.588 ± 0.047 to 4.140 ± 0.066 mg/mL. Corresponding electrophoresis data showed different protein profiles. UniProtKB data base research reveals two sorghum ATIs, and P81367; both reviewed and a targeted LC–MS/MS method was developed to analyze these. Quantifier peptides ELAAVPSR ( P81368) and TYMVR ( P81367) were identified and retained as biomarkers for relative quantification. Different reducing and alkylating agents were assessed and combination of tris (2 carboxyethyl) phosphine/iodoacetamide gave the best response. Linearity was demonstrated for the quantifier peptides with standard recovery between 92.2 and 107.6%. Nine sorghum cultivars presented up to 60 times lower ATI contents as compared to wheat samples. This data suggests that sorghum can effectively be considered as a good alternative to wheat. P81368相似文献