The crystal structure of Cu4(PO4)2O

Cu₄(PO₄)₂O crystallizes in the space group $\text{P}\text{1}$ with a = 7.5393(8) Å, b = 8.1021(9) Å, c = 6.2764(8) Å, α = 113.65(1)°, β = 98.42(1)° and γ = 74.19(1)°. The structure was refined by full-matrix least-squares techniques using automatic diffractometer data to R = 0.046 (R_w = 0.056). Four unique copper atoms are in six, five-, and four-coordinated polyhedra which are linked together to form a three-dimensional network. The structure is best described in terms of a cubic close-packed array of oxygen atoms with one-tenth of the possible anion sites vacant.     

TECRA Unique test for rapid detection of Salmonella in food: collaborative study

The TECRA Unique Salmonella test uses the principle of immunoenrichment to allow rapid detection of Salmonellae in food. A collaborative study was conducted to compare the TECRA Salmonella Unique test with the reference culture method given in the U.S. Food and Drug Administration's Bacteriological Analytical Manual. Three food types (milk powder, pepper, and soy flour) were analyzed in Australia and 2 food types (milk chocolate and dried egg) were analyzed in the United States. Forty-one collaborators participated in the study. For each of the 5 foods at each of the 3 levels, a comparison showed no significant differences (p > or = 0.05) in the proportion of positive test samples for Unique and that for the reference method using the Chi-square test for independence with continuity correction.     

Relative Lewis basicities of six AI(ORF)4- superweak anions and the structures of LiA

The relative Lewis basicities of six Al(ORF)4- ions, Al[OC(CH3)(CF3)2]4-, Al(OC(CF3)3]4-, Al(OCPh(CF3)2]4-, Al[OC[4-C6H4(tBu)](CF3)2]4-, Al(OC(Cy)(CF3)2]4-, and Al(OCPh2(CF3)]4-, have been determined by measuring their relative coordinating abilities towards Li+ in dichloromethane. The relative Li- Lewis basicities of the Al(ORF)4- ions are linearly related to the aqueous pKa values of the corresponding parent HORF fluoroalcohols. The Lewis basicity of Al[OCH(CF3)2]4- could not be measured because two of these anions can coordinate to one Li+ cation. The structures of LiAl[OCH(CF3)2]4 and [1-Et-3-Me-1,3-C3H3N2][Li[Al[OCH(CF3)2)4]2] were determined.     

A dynamic ion cooling technique for FTICR mass spectrometry

A fast dynamic ion cooling technique based upon the adiabatic invariant phenomenon for Fourier transform ion cyclotron resonance mass spectrometry (FTICR) is presented. The method cools ions in the FTICR trap more efficiently, within a few hundred milliseconds without the use of a buffer gas, and results in a substantial signal enhancement. All performance aspects of the FTICR spectrum, e.g., peak intensities, mass resolution, and mass accuracy, improve significantly compared with cooling based on ion-ion interactions. The method may be useful in biological applications of FTICR, such as in proteomic studies involving extended on-line liquid chromatography (LC) separations, in which both the duty cycle and mass accuracy are crucially important.     

Separation of lidocaine and its metabolites by capillary electrophoresis using volatile aqueous and nonaqueous electrolyte systems

The separation of the basic drug lidocaine and six of its metabolites has been investigated both by using volatile aqueous electrolyte system, at low pH and by employing non-aqueous electrolyte systems. In aqueous systems, the best separation of the compounds under the investigated conditions was achieved by using the electrolyte 60 mM trifluoroacetic acid (TFA)/triethylamine (TEA) at pH 2.5 containing 15% methanol. With this electrolyte, all seven compounds were well separated with high efficiency and migration time repeatability. The separations with bare fused-silica capillaries and polyacrylamide-coated capillaries were compared with higher separation efficiency with the latter. On the other hand, near baseline separation of all the seven compounds was also obtained by employing the non-aqueous electrolyte, 40 mM ammonium acetate in methanol and TFA (99:1, v/v), with comparable migration time repeatability but lower separation efficiency relative to the aqueous system.     

Platinum-catalyzed enantioselective tandem alkylation/arylation of primary phosphines. Asymmetric synthesis of P-stereogenic 1-phosphaacenaphthenes

Enantioselective tandem alkylation/arylation of primary phosphines with 1-bromo-8-chloromethylnaphthalene catalyzed by Pt(DuPhos) complexes gave P-stereogenic 1-phosphaacenaphthenes (AcePhos) in up to 74% ee. Diastereoselective formation of four P-C bonds in one pot with bis(primary) phosphines gave C2-symmetric diphosphines, including the o-phenylene derivative DuAcePhos, for which the rac isomer was formed with high enantioselectivity. These reactions, which appear to proceed via an unusual metal-mediated nucleophilic aromatic substitution pathway, yield a new class of heterocycles with potential applications in asymmetric catalysis.     

Synthesis of copolyimides based on room temperature ionic liquid diamines

Block copolyimides based on aromatic dianhydrides and diamines copolymerized with diamino room temperature ionic liquid (RTIL) monomers were synthesized over a range of compositions. Specifically, two diamino RTILs, 1,3‐di(3‐aminopropyl) imidazolium bis[(trifluoromethyl)sulfonyl] imide ([DAPIM] [NTf₂]) and 1,12‐di[3‐(3‐aminopropyl) imidazolium] dodecane bis[(trifluoromethyl) sulfonyl] imide ([C₁₂ (DAPIM)₂] [NTf₂]₂) were synthesized using a Boc protection method. The two RTILs were reacted with 2,2‐bis(3,4‐carboxylphenyl) hexafluoropropane dianhydride (6FDA) to produce 6FDA‐RTILs oligomers that formed the RTIL component for the block copolyimides. The oligomers were reacted with 6FDA and m‐phenylenediamine (MDA) at oligomer concentration from 6.5 to 25.8 mol % to form block copolyimides. Increasing the concentration of the 6FDA‐RTIL oligomer in the block copolyimides resulted in a decrease in the thermal degradation temperature, glass transition temperature and an increase in the density. The gas permeability of the RTIL based block copolyimide decreased but the ideal permeability selectivity for CO₂/CH₄ gas pair increased relative to the pure 6FDA‐MDA. © 2010 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 48: 4036–4046, 2010     

Determination of the mineral composition of fresh bovine milk from the milk-producing areas located in the State of Sergipe in Brazil and evaluation employing exploratory analysis

In this work, the mineral composition of fresh bovine milk obtained from the milk-producing areas of the Brazilian State of Sergipe was examined. A dry-ashed digestion method and the ICP OES technique were used for the quantification of mineral elements (e.g., Ca, Mg, K, Na, P, Sr and Zn) in 27 samples of milk collected from properties located in milk-producing areas around Nossa Senhora da Glória. The following ranges of values (% m/v) were obtained: 0.063 to 0.117 for Ca; 0.060 to 0.114 for P; 0.024 to 0.064 for Na; and 0.087 to 0.164 for K. The ranges of values (mg L^− 1) for the other mineral elements were also found: 0.68 to 1.89 for Sr; 2.46 to 5.73 for Zn; and 54.2 to 109.9 for Mg. Additionally, the exploratory evaluation of the 27 milk samples was performed using principal component analysis (PCA) involving seven variables dealing with the effect of different management systems (conventional and organic) on milk composition. The results show that there are indeed differences between the mineral composition of milk from properties that use organic practices and those that use conventional management practices.