用于XRF分析的U-Nb合金试样制备方法

用X射线荧光光谱法(XRF)测量U-Nb合金样品时,其试样制备至关重要。本文用XRF测量U-Nb合金试样的制备方法:首先用HNO3+HF溶样,然后加入柠檬酸溶液,依次经过加热、除酸、络合、定容等过程,最后定量移取试液于滤纸片上,在红外灯下烤干,即制成试样片。该方法制备的U-Nb合金试样片具有平整、不变形、易于封装、可长期存放等特点。     

银离子络合法提取核桃油中不饱和脂肪酸

对皂化后的核桃油进行酸化获得混合脂肪酸,再对其进行甲酯化得混合脂肪酸甲酯,采用硝酸银络合萃取法提取混合脂肪酸甲酯中的不饱和脂肪酸甲酯。实验结果表明,以1mol/L氢氧化钾-无水乙醇溶液进行皂化,40%甲醇水溶液溶剂,硝酸银浓度为2mol/L,0℃的条件下络合萃取2h效果最佳,不饱和脂肪酸含量由72.3%增加到96.3%。     

Characteristic ion clusters as determinants for the identification of pyrrolizidine alkaloid N-oxides in pyrrolizidine alkaloid-containing natural products using HPLC-MS analysis

Pyrrolizidine alkaloid (PA)-containing plants are widely distributed in the world. PAs are hepatotoxic, affecting livestock and humans. PA N-oxides are often present together with PAs in plants and also exhibit hepatotoxicity but with less potency. HPLC-MS is generally used to analyze PA-containing herbs, although PA references are unavailable in most cases. However, to date, without reference standards, HPLC-MS methodology cannot distinguish PA N-oxides from PAs because they both produce the same characteristic ions in mass spectra. In the present study, the mass spectra of 10 PA N-oxides and the corresponding PAs were systemically investigated using HPLC-MS to define the characteristic mass fragment ions specific to PAs and PA N-oxides. Mass spectra of toxic retronecine-type PA N-oxides exhibited two characteristic ion clusters at m/z 118-120 and 136-138. These ion clusters were produced by three unique fragmentation pathways of PA N-oxides and were not found in their corresponding PAs. Similarly, the nontoxic platynecine-type PA N-oxides also fragmented via three similar pathways to form two characteristic ion clusters at m/z 120-122 and 138-140. Further application of using these characteristic ion clusters allowed successful and rapid identification of PAs and PA N-oxides in two PA-containing herbal plants. Our results demonstrated, for the first time, that these characteristic ion clusters are unique determinants to discriminate PA N-oxides from PAs even without the availability of reference samples. Our findings provide a novel and specific method to differentiate PA N-oxides from PAs in PA-containing natural products, which is crucial for the assessment of their intoxication.     

An efficient three-component, one-pot synthesis of 2-alkylthio-4-amino-5-cyano-6-aryl(alkyl)pyrimidines in water

A convenient and practical method for the synthesis of 2-alkylthio-4-amino-5-cyano-6-aryl(alkyl)pyrimidines has been developed via a three-component, one-pot reaction from aldehydes, malononitrile and S-alkylisothiouronium salts in water at room temperature. A series of polysubstituted pyrimidines were prepared by this method in moderate to excellent yields. In addition, two kinds of pyrimidine-fused heterocyclic derivatives with potential pharmacological activity were constructed from our 2-alkylthio-4-amino-5-cyano-6-arylpyrimidines.     

Residual symmetries for neutrino mixing with a large θ13 and nearly maximal δD

The residual Z(2)(s)(k) and Z(2)(s)(k) symmetries induce a direct and unique phenomenological relation with θx (≡ θ13) expressed in terms of the other two mixing angles θs(≡ θ12) and θa(≡ θ23) and the Dirac CP phase δD. Z(2)(s)(k) predicts a θx probability distribution centered around 3°-6° with an uncertainty of 2°-4°, while those from Z(2)(s)(k) are approximately a factor of 2 larger. Either result fits the T2K, MINOS, and Double Chooz measurements. Alternately, a prediction for the Dirac CP phase δD results in a peak at ± 74° (± 106°) for Z(2)(s)(k) or ± 123° (± 57°) for Z(2)(s)(k) which is consistent with the latest global fit. We also give a distribution for the leptonic Jarlskog invariant Jν which can provide further tests from measurements at T2K and NOνA.     

The study on neural contrast sensitivity function at temporal frequencies

The neural contrast sensitivity function (NCSF) of human eye at temporal frequencies is acquired with a new method in this paper. Firstly the human eye's contrast sensitivity function (CSF) at temporal frequencies is measured by means of travelling-wave stimuli, and the modulation transfer function (MTF) of the eye's optics is obtained by constructing the eye model of the subject. Then the NCSF at temporal frequencies is calculated with the two functions. It is shown that the overall value of the NCSF decreases as the temporal frequency increases. As the temporal frequency increases from 0 cycles per second (c/s) to 1 c/s, 16 c/s and 30 c/s, the NCSF curve changes from the band-pass shape to the low-pass, and then to almost monotonic variation. The attenuation factor of the NCSF, which represents the sensitivity of visual neural system to the temporal frequency, varies little as spatial frequency increases, while that of the CSF declines dramatically in the region of high spatial frequencies. Because it is the NCSF, rather than the CSF, that reflects the characteristics of visual neural system, the investigation of the NCSF at temporal frequency is more essentially.     

Effect of stirring on striae in glass melts

Chemical striae have often negative effect on the glass properties, and hence, elimination of striae has been a key issue in glass science and technology. To produce highly homogeneous glasses, it is necessary to stir melts during the melting process. To explore the physical origin of the stria elimination during stirring, and to optimise the homogenisation process, both simulations of striation and homogenisation experiments are performed. The results show that stirring broadens the stria size distribution in the melt through conversion of larger striae into smaller ones. Only the striae with a size below half the diffusion length in the melt can be eliminated during the melting process. Stirring itself does not homogenise the melt, but enhances the stria elimination rate by generating small striae.     

Ugi reaction-assisted rapid assembly of affinity-based probes against potential protein tyrosine phosphatases

The multi-component Ugi reaction has been employed to assemble a small library of affinity-based probes (AfBPs) that target potential protein tyrosine phosphatases. The probes showed good labelling of PTP1B and MptpB, and were subsequently used to label endogenous PTP1B in MCF-7 cell lysates.     

Unique biocatalytic resolution of racemic tetrahydroberberrubine via kinetic glycosylation and enantio-selective sulfation

In this communication, we document a facile kinetic glycosylation resolution of racemic tetrahydroberberrubine. We also demonstrate that the enantiomeric excess of the resolved products is increased via a second resolution of the minor product of the first glycosylation resolution. This provides a rare example of tandem kinetic resolution of racemates.