脱蜡剂DF-1的气相色谱-傅里叶变换红外光谱联用分析

脱蜡剂ＤＦ－１是一种含多种有机成分的碳氢化合物，经气相色谱－红外光谱联用分析后，确定了这些组分的组成与含量。     

Thermal decomposition and indirect structural determination of rare earth element picrates with the dtso ligand

The complexes [Ln(pic)₃(DTSO)₃] (Ln=La, Lu and Y; pic=picrate; DTSO=1,3-dithiane-1-oxide) were synthesized and characterized. Indirect structural determination by far infrared spectroscopy is presented. Results from thermal decomposition of these complexes by TG/DTG and DSC techniques are reported. This revised version was published online in August 2006 with corrections to the Cover Date.     

Thermal decomposition of struvite

Struvite (NH₄MgPO₄·6H₂O) is a mineral often found in urinary tracts and kidneys. Thermal decomposition using slow low heating shows that the 'kidney' stone can be decomposed at temperatures below 40°C. At this temperature both ammonia and water are evolved. If more rapid heating is employed the decomposition occurs at around 80°C. The implication of this work rests with the use of low slow heat for the decomposition of the kidney stones. This revised version was published online in July 2006 with corrections to the Cover Date.     

Fourier interferometric stimulation (FIS) in biology and medicine

A continuously scanning Michelson interferometer was developed to modulate an intensive light source spectrally. The interferogram is used as a stimulus to investigate spectral sensitivities in insects and man. The FIS-method is fast and precise and shows many advantages which are partly based on the advantages of Fourier spectroscopy. The existing applications are summarized.     

Crystallization of chiral compounds. 1. Spectroscopic,thermochemical, and crystallographic investigation of homochiral and racemic glycidyl p-toluenesulfonate

Crystalline specimens of homochiral and racemic glycidyl p-toluenesulfonate were studied by IR spectroscopy, differential scanning calorimetry, and X-ray diffraction analysis. The melting phase diagram of glycidyl p-toluenesulfonate was constructed. The stacking effect in the crystals of the racemic sulfonate is responsible for a more dense molecular packing, with the result that a heterochiral type of crystallization becomes more favorable.     

Synthesis and characterization of liquid‐crystalline polyphosphonates containing disubstituted ferrocene esters as mesogens

A series of ferrocene‐containing liquid‐crystalline polyphosphonates with an even number of methylene groups are reported. All the polymers gave birefringent melts. The mesophase was identified as transparent with an increase in the spacer. The effects of pendant substitution and the spacer were studied with thermogravimetric analysis and differential scanning calorimetry. The effects of the phosphonate group in the spacer and the ferrocene ester group in the mesogen were examined. The presence of a steplike mesogenic structure and a pendant phenyl group in the spacer led to reductions in the glass‐transition and melting temperatures. The ferrocene moiety in the mesogen might be one of the reasons for the increased thermal stability and decreased liquid crystallinity. An energy‐minimized structure for the mesogenic and spacer segments was created with computer‐modeling programs, and it suggested the reason for the reductions in the glass‐transition and melting temperatures. © 2002 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 40: 2256–2263, 2002     

Magnetic phase transitions in nanostructures induced by shear stress under high pressure

Magnetic phase transitions of the first and second order were revealed by Mössbauer spectroscopy in nanosystems of - and -ferric oxides and metallic europium subjected to shear stress (240°) under high pressure (20 kbar). For - and -ferric oxide nanoclusters, the Curie (Neel) points decreased to 300 K, whereas for nanostructured europium the Neel point increased from 90 to 100 K. The thermodynamic model of magnetic phase transitions predicting a change in the character of magnetic phase transitions and a decrease (increase) in the critical Neel (Curie) points in nanoclusters was developed. The type of magnetic phase transitions and the change in the critical points were caused by defects in nanoclusters, whose maximum concentration was observed for the clusters with the 20—50 nm size range.     

Nontrivial structural organization of pivalate complexes with the fragment {Fe2Li(μ3-O)}

1. Download : Download high-res image (228KB)
2. Download : Download full-size image

     

Improved accuracy of quantitative XPS analysis using predetermined spectrometer transmission functions with UNIFIT 2004

The accuracy of quantitative XPS analysis can be improved using predetermined transmission functions. Two different calibration methods are used for estimating the transmission function T(E) of a photoelectron spectrometer, applying a survey spectra approach (SSA) and a quantified peak‐area approach (QPA) to minimize the quantification error. For the SSA method, Au, Ag and Cu spectra measured with the Metrology Spectrometer II have been used. The new QPA method was built up from Au 4f, Au 4d, Au 4p_3/2, Ag 3d, Ag 3p_3/2, Cu 3p, Cu 2p_3/2, Ge 3p and Ge 2p_3/2 standard peak areas, applying adequate ionization cross‐sections and mean free path lengths for different pass energies (10 and 50 eV), lens modes (large area, large area XL, small area 150) and x‐ray sources (Al/Mg Twin and Al Mono). In the energy range 200–1500 eV a transmission function T(E) = a₀ + b₁E (where a₀, b₁ and b₂ are variable parameters) was found to give an appropriate approximation for eight tested spectrometer settings, implementing the largest changes in the case of pass energy variations. Determination and application of the transmission functions were integrated in the XPS analysis software (UNIFIT 2004) and tested by means of an Ni90Cr10 alloy. The results demonstrate the practicability of the SSA and QPA methods, giving decreased errors of <8% in comparison with errors up to 38% obtained using Wagner's sensitivity factors. Copyright © 2005 John Wiley & Sons, Ltd.