Studies on the Mass Spectra of N‐Aryl α,β‐Unsaturated γ‐Lactams

The mass spectra of a series of N‐aryl α,β‐unsaturated γ‐lactams were studied. Besides the molecular ion, the three characteristic fragments such as [M⁺‐29], [M⁺‐55], and [M⁺‐82] were commonly found in a series of N‐Aryl α,β‐unsaturated γ‐lactams in EI/MS. Further more the mechanism for the interpretation of these fragments is also de scribed.     

Applying local model approach for tidal prediction in a deterministic model

In recent years, a practice of tidal prediction based on a deterministic model or by a time series forecasting model has been established. A deterministic model can predict tidal movement and capture the dynamics of the flow pattern over the entire domain. However, due to the simplification of model settings and near shore effects, the accuracy of the numerical model can diminish. Time series forecasting is capable of capturing the underlying mechanism that may not be revealed in the deterministic model simulation. However, such data‐driven forecast fails to maintain accuracy with the progress of forecast horizon. In this paper, a scheme that combines the advantages of these two methods is introduced. The model errors are forecasted to different time horizons using a data‐driven approach, and are then superimposed on the simulation results in order to correct the model output. Based on the proposed method, it is found that the accuracy is significantly improved with more than 50% of the errors removed on the average. Copyright © 2008 John Wiley & Sons, Ltd.     

煤矸石中微量锰的催化光度法测定

在HAc NaAc介质中痕量锰 (Ⅱ )对高碘酸钾氧化亮绿SF(BGSF)的褪色反应有强的催化作用 ,催化程度与Mn(Ⅱ )量在一定范围内线性相关。建立了测定痕量Mn(Ⅱ )的分光光度法。实验表明 ,有色溶液的最大吸收波长为 6 5 1nm ,方法检出限为 0 0 6 0 μg·L-1,催化程度与Mn(Ⅱ )量在 0 0 3～ 0 3μg·5 0mL-1范围内符合比耳定律 ,选择性较好 ,可用于测定煤矸石中的微量锰。     

Radiochemical Feasibility of Mixing of 99mTc-MAA and 90Y-Microspheres with Omnipaque Contrast

Yttrium-90 (⁹⁰Y) microspheres are widely used for the treatment of liver-dominant malignant tumors. They are infused via catheter into the hepatic artery branches supplying the tumor under fluoroscopic guidance based on pre-therapy angiography and Technetium-99m macroaggregated albumin (^99mTc-MAA) planning. However, at present, these microspheres are suspended in radiolucent media such as dextrose 5% (D5) solution. In order to monitor the real-time implantation of the microspheres into the tumor, the ⁹⁰Y microspheres could be suspended in omnipaque contrast for allowing visualization of the correct distribution of the microspheres into the tumor. The radiochemical purity of mixing ⁹⁰Y-microspheres in various concentrations of omnipaque was investigated. The radiochemical purity and feasibility of mixing ^99mTc-MAA with various concentrations of a standard contrast agent were also investigated. Results showed the radiochemical feasibility of mixing ⁹⁰Y-microspheres with omnipaque is radiochemically acceptable for allowing real-time visualization of radioembolization under fluoroscopy.     

金属离子负载修饰阳离子树脂在酯化反应中的研究

将催化精馏中常用作催化填料的强酸性阳离子交换树脂用金属离子负载修饰后，考察了树脂催化性能的改变及树脂结构对催化性能的影响。实验表明，经修饰后树脂的催化能力都高于原树脂，在不分水的情况下，合成乙酸乙酯时乙酸的转化率最高可达73％，具有很好的选择性，金属离子能与树脂的磺酸基团产生络合，提高了树指的催化性能，所形成的新酸中心不会被阳离子交换而失活。     

Identification of 2D-gel proteins: a comparison of MALDI/TOF peptide mass mapping to mu LC-ESI tandem mass spectrometry

A comparative analysis of protein identification for a total of 162 protein spots separated by two-dimensional gel electrophoresis from two fully sequenced archaea, Methanococcus jannaschii and Pyrococcus furiosus, using MALDI-TOF peptide mass mapping (PMM) and mu LC-MS/MS is presented. 100% of the gel spots analyzed were successfully matched to the predicted proteins in the two corresponding open reading frame databases by mu LC-MS/MS while 97% of them were identified by MALDI-TOF PMM. The high success rate from the PMM resulted from sample desalting/concentrating with ZipTip(C18) and optimization of several PMM search parameters including a 25 ppm average mass tolerance and the application of two different protein molecular weight search windows. By using this strategy, low-molecular weight (<23 kDa) proteins could be identified unambiguously with less than 5 peptide matches. Nine percent of spots were identified as containing multiple proteins. By using mu LC-MS/MS, 50% of the spots analyzed were identified as containing multiple proteins. mu LC-MS/MS demonstrated better protein sequence coverage than MALDI-TOF PMM over the entire mass range of proteins identified. MALDI-TOF and PMM produced unique peptide molecular weight matches that were not identified by mu LC-MS/MS. By incorporating amino acid sequence modifications into database searches, combined sequence coverage obtained from these two complimentary ionization methods exceeded 50% for approximately 70% of the 162 spots analyzed. This improved sequence coverage in combination with enzymatic digestions of different specificity is proposed as a method for analysis of post-translational modification from 2D-gel separated proteins.     

An Efficient Method for the Preparation of Nitriles via the Dehydration of Aldoximes with Phthalic Anhydride

A new and highly efficient method for the conversion of aldoximes to nitriles was established. By fusing with phthalic anhydride, aldoximes were efficiently and smoothly converted into nitriles, in high yields (over 85%) and in a short time (within 5 minutes). The mixture of phthalic anhydride, a cyclic anhydride, and aldoximes in fusing state set up an ideal transition state for a selective [3.3]‐sigmatropic rearrangement of the acylated aldoximes to nitriles.     

An acoustooptic method of measuring the noise equivalent power of optical heterodyne systems

The noise equivalent power of optical heterodyne detection at 10.6 m has been measured with a method based on Raman-Nath diffraction of a CO₂ laser beam. One of the frequency shifted first order diffracted beams is used as the signal radiation. The local oscillator radiation is obtained by splitting off a part of the laser beam incident upon the device used for the acoustooptic diffraction. The signal power can be varied over a large dynamic range by changing the acoustic input power. A study of the probable errors shows that the total error in the NEP measurement is less than 30%.