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The performance of single-drop microextraction (SDME), coupled with gas chromatography/mass spectrometry, was assessed for the determination of tributyltin compounds in water and solid samples. Experimental parameters impacting the performance of SDME, such as microextraction solvent and sampling and stirring time, were investigated. Analytical results obtained by SDME were compared with those generated by conventional solid phase microextraction (SPME) and liquid-liquid extraction (LLE) for the determination of TBT in PACS-2 sediment certified reference material (CRM). 相似文献
4.
The NMR titration methodology to determine acid dissociation constants in aqueous solutions is extended for pK(a) values between 0 and 2, where potentiometric titrations are no longer applicable. (1)H NMR spectra are acquired for single samples of constant acid concentration (e.g. 0.02M), controlled ionic strength (I=1M with HNO(3)/NaNO(3)) and varying pH. To avoid biased pH readings due to the acid error of the glass electrode, true, concentration-based pH values are deduced by combination of the charge balance equation with information from (1)H NMR chemical shifts of the investigated acid. The method has been tested on histidine (pK(1)=1.83+/-0.02) and yielded the dissociation constant of dichloroacetic acid (pK=1.06+/-0.01) for the first time with good accuracy and precision. Dichloroacetic acid is recommended as an NMR spectroscopical "indicator molecule" for in situ monitoring the pH in strong acidic solutions of other equilibrium systems. 相似文献
5.
Báthori M Pongrácz Z Tóth G Simon A Kandra L Kele Z Ohmacht R 《Journal of chromatographic science》2002,40(7):409-415
A new ecdysteroid glycoside, 2-deoxy-20-hydroxyecdysone 22-O-beta-D-glucopyranoside, is isolated from the herb Silene italica ssp. nemoralis (Waldst. and Kit.) Nyman. The compound is purified with multistep chromatography, such as classical column chromatography on alumina and droplet countercurrent distribution. Also, it is expanded using twice low-pressure reversed-phase liquid column chromatography. Chromatography in four steps results in the purified 2-deoxy-20-hydroxyecdysone 22-O-beta-D-glucopyranoside. Two other ecdysteroids have also been separated, including the formerly identified integristerone A and 24(28)-dehydromakisterone A. 相似文献
6.
Nitrogen bridgehead compounds part 21. Preparation of new quaternary 2,3a,6a-triazaphenalenium salts
István Bitter Béla Pete István Hermecz Gábor Tóth Kálmán Simon Mátyás Czugler Zoltán Mészáros 《Tetrahedron letters》1982,23(28):2891-2894
The first representatives of a new ring system, the 2,3a,6a-triazaphenalenium quaternary salts are prepared by the cycloaddition of tetrahydro-4H-pyrido[1,2-a] pyrimidin-4-ones containing an α-chloroenamine moiety with azomethines. 相似文献
7.
Seymour (1981) proved that the cut criterion is necessary and sufficient for the solvability of the edge-disjoint paths problem when the union of the supply graph and the demand graph is planar and Eulerian. When only planarity is required, Middendorf and Pfeiffer (1993) proved the problem to be NP-complete. For this case, Korach and Penn (1992) proved that the cut criterion is sufficient for the existence of a near-complete packing of paths. Here we generalize this result by showing how a natural strengthening of the cut criterion yields better packings of paths.Analogously to Seymour's approach, we actually prove a theorem on packing cuts in an arbitrary graph and then the planar edge-disjoint paths case is obtained by planar dualization. The main result is derived from a theorem of Seb (1990) on the structure of ±1 weightings of a bipartite graph with no negative circuits.Research partially supported by the Hungarian National Foundation for Scientific Research Grants OTKA 2118 and 4271. 相似文献
8.
Zoltán Füredi 《Journal of Geometry》1993,46(1-2):55-65
Let s1 (n) denote the largest possible minimal distance amongn distinct points on the unit sphere
. In general, let sk(n) denote the supremum of thek-th minimal distance. In this paper we prove and disprove the following conjecture of A. Bezdek and K. Bezdek: s2(n) = s1([n/3]). This equality holds forn > n0 however s2(12) > s1(4).We set up a conjecture for sk(n), that one can always reduce the problem of thek-th minimum distance to the function s1. We prove this conjecture in the casek=3 as well, obtaining that s3(n) = s1([n/5]) for sufficiently largen.The optimal construction for the largest second distance is obtained from a point set of size [n/3] with the largest possible minimal distance by replacing each point by three vertices of an equilateral triangle of the same size . If 0, then s2 tends to s1([n/3]). In the case of the third minimal distance, we start with a point set of size [n/5] and replace each point by a regular pentagon. 相似文献
9.
This perspective article describes the combination of experimental data and quantum chemical methods for the determination of structure and reaction mechanisms of uranyl(vi) complexes in aqueous solution. The first part assesses the accuracy of the chemical and thermodynamic properties of solvated uranyl(vi) complexes as obtained by various quantum chemical methods. The second part discusses structure determination, mechanisms for ligand exchange and the lability of coordinated water molecules for various uranyl(vi) complexes using a combination of NMR and quantum chemical data. 相似文献
10.
Varga I Mészáros R Szakács Z Gilányi T 《Langmuir : the ACS journal of surfaces and colloids》2005,21(14):6154-6156
A simple one-step synthesis is described for the functionalization of poly(vinyl chloride) used for the preparation of anionic surfactant-selective membrane electrodes. The method is based on the nucleophilic substitution of a fraction of the chlorine atoms bound to the poly(vinyl chloride) backbone by trimethylamine. The prepared slightly charged polymer gave rise to high-quality surfactant-selective electrode membranes, which had a Nernstian response, short response time, and appropriate stability. 相似文献