Triple quadrupole mass spectrometry as applied to flame diagnostics: study of the C2H4/N2O/Ar flame

A recently developed research apparatus for characterization of low-pressure premixed flames has been developed and was used to characterize the C₂H₄/N₂O/Ar flame at 20 torr. This instrument incorporates several diagnostic techniques in one apparatus so that individual techniques can be quantitatively compared and the usable detection range (both in terms of resolution and species detection) expanded. Results discussed in this report include mass analysis by triple quadrupole mass spectrometer and temperature measurement by thermocouple. Concentration profiles in the one-dimensional flame include CO, N₂, and C₂H₄, at nominal m/z 28 as well as CO₂ and N₂O at m/z 44.     

Preparation of niobium and tantalum organoimido complexes from reactions of the pentahalides with amines: The crystal and molecular structure of bis(t-butylamine)bis(t-butylimido)bis(μ-ethoxy)tetrachloroditantalum

MCl₅ (M = Nb, Ta) reacts with 2 equivalents of Me₃SiNHCMe₃ to give [M(NCMe₃)Cl₃(NH₂CMe₃)] from which [M(NCMe₃)Cl₃(PMe₃)₂] is obtained on addition of PMe₃. One equivalent of Me₃SiNHCMe₃ reacts with MCl₅ in the presence of 3 equivalents of PMe₃ to give [M(NCMe₃)Cl₃(PMe₃)₂] and PMe₃HCl. MCl₅ reacts with excess RNH₂ (R = CMe₃, CHMe₂, CH₂Me) to give [M(NR)(NHR)Cl₂(NH₂R)] and 3 equivalents of RNH₃Cl. One equivalent of alcohol replaces the amido ligand in [M(NCMe₃)(NHCMe₃)Cl₂(NH₂CMe₃)] to give [M(NCMe₃)(OR)Cl₂(NH₂CMe₃)]₂ (M = Nb, R = OCMe₃; M = Ta, R = OEt). The structure of [Ta(NCMe₃)(μ-OEt)Cl₂(NH₂CMe₃)]₂ was determined by single-crystal X-ray diffraction methods. Crystals are triclinic, space group P$\text{1}$ with a = 9.900(5), b = 10. 161(17), c = 9.017(6) Å and α = 103.91(8), β = 97.77(4), γ = 64.40(7)°. The structure was solved by Patterson and Fourier methods and refined to an R value of 0.062 for 1319 observed data. The TaN_imido and TaN_amino bond lengths are 1.70(2) Å and 2.28(2) Å, respectively; the bridging TaO bond lengths are 2.01(2) Å and 2.32(2) Å, the longer one lying trans to the imido function.     

Wirkung von Actinomycin D auf die RNS-Synthese und die synchrone Mitosetätigkeit in Physarum polycephalum

Zusammenfassung Actinomycin D (250 /ml) hemmt in Suspensionskulturen vonPhysarum polycephalum spezifisch die RNS-Synthese, während die DNS- und Proteinsynthese innerhalb der ersten drei Stunden nur wenig beeinträchtigt werden. Die Auslösung einer synchronen Kernteilung in Makroplasmodien kann durch 250 /ml Actinomycin D verhindert oder stark verzögert werden, sofern der Hemmstoff spätestens zu Beginn des letzten Drittels der Interphase ( 2 Stdn. vor Prophase) dem Medium zugesetzt wird. Die Mitosehemmung ist durch Auswaschen des Hemmstoffes reversibel. Die Ergebnisse sprechen dafür, daß zur Vorbereitung einer Mitose während des größten Teiles der Interphase DNS-abhängige RNS neu gebildet werden muß, die möglicherweise als Informationsüberträger die Synthese mitosespezifischer Proteine kontrolliert. Es wird eine Arbeitshypothese diskutiert, nach der die Mitose als ein durch Genregulation gesteuerter Vorgang aufzufassen wäre.

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Actinomycin D (250 /ml) specifically inhibits RNA synthesis in suspension cultures ofPhysarum polycephalum whereas DNA and protein synthesis are less affected within the first three hours. Onset of synchronous mitoses in macroplasmodia is prohibited or largely delayed by 250 /ml actinomycin D if the inhibitor is added to the medium at or prior to the beginning of the last third of interphase ( 2 hrs. prior to prophase). Removal of the inhibitor from the medium reverses the inhibitory effect on mitosis. The results indicate that preparation of mitosis requires synthesis of DNA dependent RNA during the major part of interphase. These RNA molecules possibly carry information for the synthesis of proteins specifically involved with mitosis. A working hypothesis is discussed suggesting that mitotic activities may by controlled by gene regulation.

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Mit 4 Abbildungen

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Herrn Prof. Dr.Hermann Bretschneider zum 60. Geburtstag gewidmet.     

Organo-imido alkoxides of tungsten(VI). The crystal and molecular structures of [W(NPh)(μ-OMe)(OMe)3]2 and [W(NPh)(OCMe3)3Cl(NH2CMe3)]

Reaction of phenylimido tungsten tetrachloride with MeOH and t-butylamine gave the dimeric complexes [W(NPh)(μ-OMe)(OMe)₃]₂ and [W(NPh)(μ-OMe)(OMe)₂Cl]₂. With ethanol [W(NPh)(μ-OEt)(OEt)₂Cl]₂ was formed whereas isopropyl and neopentyl alcohols gave the monomeric complexes [W(NPh)(OR)₄(NH₂CMe₃)](R = CHMe₂, CH₂CMe₃); t-butanol gave [W(NPh)(OCMe₃)3Cl(NH₂CMe₃)] which could not be converted to [W(NPh) (OCMe₃)₄]. Further reaction of [W(NPh)(μ-OMe)(OMe)₃]₂ with o-HOC₆H₄CH = NC₆H₃Me₂(salim-H) gave the salicylaldimine complex [W(NPh)(OMC)₃(salim)]. The products were characterised by analytical data, IR, ¹H NMR, ¹³C NMR and mass spectroscopy. The crystal and molecular structures of the title complexes have been determined from single crystal X-ray diffractometer data. Crystals of [W(NPh)(μ-OMe)(OMe)₃]₂are triclinic with a = 8.473(7), b = 10.776(5), c = 7.683(Å, α = 102.26(3), β = 102.68(4), γ = 71.13(6)°, space group P$\text{1}$ Crystals of 3) [W(NPh)(OCMe₃)₃Cl(NH₂CMe₃) are monoclinic with a = 9.341(2), b = 29.608(7), c = 10.257(2) Å, β = 106.28(2)°, space group, P2₁/c. Both structures were solved by Patterson and Fourier methods and refined to R = 0.075 for the 1022 observed data of [W(NPh) (μ-OMe)(OMe)₃]₂ and to R = 0.074. For the 2033 observed data of [W(NPh)(OCMe₃)₃Cl(NH₂CMe₃). The former molecule is shown to be a dimer, the two halves of the molecule being related by a centre of symmetry. Both W atoms adopt a distorted octahedral coordination geometry and they are linked by two methoxy bridges. Trans to one of the bridging donors is the phenyl imido group with a WN bond length of 1.61(4) Å; the remaining coordination sites are filled with methoxy groups. The structure of W(NPh)(OCMe₃)₃ Cl(NH₂CMe₃) is monomeric with the phenylimido group trans to the NH₂CMe₃ ligand in a distorted octahedral coordination geometry. Remaining sites are filled with the chloride and 3 OCMe₃ ligands. The WN (imido) bond length is 1.71(2) Å, whilst WN(amine) is 2.40(2) Å     

Potential for the use of ultrasound in the extraction of antioxidants from Rosmarinus officinalis for the food and pharmaceutical industry

Ultrasound was used to increase the extraction efficiency of carnosic acid from the herb Rosmarinus officinalis using butanone, ethyl acetate and ethanol as solvents. Both dried and fresh leaves of the herb were extracted and, when performed at the same temperature, sonication improved the yields of carnosic acid for all three solvents and shortened the extraction times. Sonication also reduced the solvent effect so that ethanol, which is a poor solvent under conventional conditions, reached a similar level of extraction efficiency to the other two when sonicated. The extraction of dried herb with ethanol proved to be more efficient than that of fresh material, probably due to the water present in the latter.     

Special Lagrangian Submanifolds with Isolated Conical Singularities. II. Moduli spaces

This is the second in a series of five papers studying special Lagrangiansubmanifolds (SLV m-folds) X in (almost) Calabi–Yau m-folds M with singularities x ₁ , ..., x _n locally modelled on specialLagrangian cones C ₁, ..., C _n in ^m with isolated singularities at 0.Readers are advised to begin with Paper V.This paper studies the deformation theory of compact SL m-folds X in Mwith conical singularities. We define the moduli space _X of deformations of X in M, and construct a natural topology on it. Then we show that _X is locally homeomorphic to the zeroes of a smooth map : _{X X} between finite-dimensional vector spaces.Here the infinitesimal deformation space _X depends only on the topology of X, and the obstruction space _X only on the cones C ₁, ..., C _n at x ₁, ..., x _n . If the cones C _i are stable then _X is zero, and _X is a smooth manifold. We also extend our results to families of almost Calabi–Yau structures on M.     

Evolution Equations for Special Lagrangian 3-Folds in C3

This is the third in a series of papers constructing explicit examples of special Lagrangian submanifolds in C ^m . The previous paper (Math. Ann. 320 (2001), 757–797), defined the idea of evolution data, which includes an (m – 1)-submanifold P in R ⁿ , and constructed a family of special Lagrangian m-folds N in C ^m , which are swept out by the image of P under a 1-parameter family of affine maps _t : R ⁿ C ^m , satisfying a first-order o.d.e. in t. In this paper we use the same idea to construct special Lagrangian 3-folds in C³. We find a one-to-one correspondence between sets of evolution data with m = 3 and homogeneous symplectic 2-manifolds P. This enables us to write down several interesting sets of evolution data, and so to construct corresponding families of special Lagrangian 3-folds in C³.Our main results are a number of new families of special Lagrangian 3-foldsin C³, which we write very explicitly in parametric form. Generically these are nonsingular as immersed 3-submanifolds, and diffeomorphic to R³ or ¹× R². Some of the 3-folds are singular, and we describe their singularities, which we believe are of a new kind.We hope these 3-folds will be helpful in understanding singularities ofcompact special Lagrangian 3-folds in Calabi–Yau 3-folds. This will beimportant in resolving the SYZ conjecture in Mirror Symmetry.     

Phenotype and in vitro function of mature MDDC generated from cryopreserved PBMC of cancer patients are equivalent to those from healthy donors

Background  

Monocyte-derived-dendritic-cells (MDDC) are the major DC type used in vaccine-based clinical studies for a variety of cancers. In order to assess whether in vitro differentiated MDDC from cryopreserved PBMC of cancer patients are functionally distinct from those of healthy donors, we compared these cells for their expression of co-stimulatory and functional markers. In addition, the effect of cryopreservation of PBMC precursors on the quality of MDDC was also evaluated using samples from healthy donors.