Tris(Trifluoroacetylacetonato)(4,4′-bipyridyl-N,N′-dioxido)Lanthanum(III)∶ A One-dimensional Polynuclear Complex

A novel one-dimensional polynuclear complex, tris(trifluoroacetylacetonato)(4,4'-bipyridyl- N , N '-dioxido)lathanum(III), was synthesized and characterized by elemental analysis and IR spectroscopy. X-ray structure analysis revealed that the complex has an infinite one-dimensional polynuclear structure with the 4,4'-bipyridyl- N , N '-dioxide as a bridge. La(III) is coordinated to eight oxygen atoms, six from three trifluoroacetylacetonate anions and two from two 4,4'-bipyridyl- N , N '-dioxide molecules to form a slightly distorted square antiprismatic coordination polyhedron. The coordination moiety was linked through 4,4'-bipyridyl- N , N '-dioxide forming a one-dimensional chain.     

Separation of geometric isomers of metal β-diketonates by supercritical fluid chromatography

The separation of the geometric isomers of chromium and rhodium chelates of trifluoroacetylacetone and thenoyltrifluor-oacetone was investigated using packed column supercritical fluid chromatography. Mobile phases consisting of neat and alcohol-modified carbon dioxide were used, and the most favorable isomeric resolution was obtained with a phenyl stationary phase. The chromatographic performance was better for chelates with trifluoroacetylacetone than for the corresponding chelates with thenoyltrifluoroacetone. Chromatographic peak area analysis of the metal chelates investigated showed appropriate isomeric concentrations in the final diastereomeric products resulting from the synthetic procedures.     

三氟乙酰丙酮—Gd（Ⅲ）—CTMAB配合物体系荧光法研究及应用

本文研究了Ｇｄ－三氟乙酰丙酮－ＣＴＭＡＢ的三元配合物荧光体系，并用钇的测定，最低检测限为：０．００３μｇ／ｍＬ，Ｇｄ在０．００５－０．４μｇ／ｍＬ范围内呈线性关系，回归方程Ｆ＝３１．６５ｃ＋０．２１，相关系数为ｒ＝０．９９９６，将此法用于稀土矿的痕量Ｇｄ的测定，与ＩＣＰ－ＡＥＳ法相比，结果令人满意。     

Development of non-aqueous single stage derivatisation method for the determination of putrescine and cadaverine using GC-MS

A single step derivatisation for the determination of putrescine and cadaverine by gas chromatography using trifluoroacetylacetone (TFAA) in methanol or ethanol was studied and optimised. The derivatives were analysed by an iontrap gas chromatograph-mass spectrometer (GC-MS) operating with electron impact ionisation with selective ion storage (EI-SIS) mode. The optimised mole ratios for TFAA/putrescine and TFAA/cadaverine reactions were 5/1 and 5.8/1 respectively with a reaction time of 15 minutes at 95oC. The retention times for the derivatised putrescine and cadaverine were 11.3 and 12.2 minutes respectively using the capillary column, CP-Sil 8CB; 30 m length x 0.25 mm i.d. x 0.25 mm film. The correlation coefficients (R²) of calibration curves for putrescine and cadaverine were 0.991 and 0.990 respectively over a concentration range of 100 ng cm⁻³ to 1500 ng cm⁻³. The method developed was found to be simple (single-stage derivatisation), rapid (15 minutes derivatisation & 14 minutes GC/MS run) and accurate (putrescine and cadaverine recoveries 94.8%–97.7%).