Determination of free fatty acids in bryophyte plants and soil by HPLC with fluorescence detection and identification by online MS

A method for the determination of long and short chain free fatty acids (FFAs), using 1-[2-(ptoluenesulfonate)-ethyll-2-phenylimidazole-[4,5-f-9,10-phenanthrene (TSPP) as labeling reagent, has been developed. Identification of FFA derivatives was carried out by HPLC-MS with atmospheric pressure chemical ionization (APCI) in positive ion mode. Gradient elution on an Agilent Eclipse XDB-C-8 column gave good separation of the derivatives. Excellent linear responses were observed and good compositional data could be obtained from as little as 200 mg of bryophyte plants and soil samples. Facile TSPP derivatization coupled with HPLC-APCI-MS analysis allowed the development of a highly sensitive method for the quantitative analysis of trace level of FFAs from biological and natural environmental samples.

Determination of long-chain fatty acids in bryophyte plants extracts by HPLC with fluorescence detection and identification with MS

A sensitive method for the determination of long-chain fatty acids (LCFAs) (>C20) using 1-[2-(p-toluenesulfonate)-ethyl]-2-phenylimidazole-[4.5-f]-9,10-phenanthrene (TSPP) as tagging reagent with fluorescence detection and identification with post-column APCI/MS has been developed. The LCFAs in bryophyte plant samples were obtained based on distillation extraction with 1: 1 (v/v) chloroform/methanol as extracting solvent. TSPP could easily and quickly label LCFAs at 90 degrees C in the presence of K2CO3 catalyst in DMF. Eleven free LCFAs from the extracts of bryophyte plants were sensitively determined. Maximal labeling yields close to 100% were observed with a five-fold excess of molar reagent. Separation of the derivatized fatty acids exhibited a good baseline resolution in combination with a gradient elution on a reversed-phase Eclipse XDB-C-8 column. Calculated detection limits from 1.0 pmol injection, at a signal-to-noise ratio of 3, were 26.19-76.67 fmol. Excellent linear responses were observed with coefficients of >0.9996. Good compositional data were obtained from the analysis of the extracted LCFAs containing as little as 0.2 g of bryophyte plant samples. Therefore, the facile TSPP derivatization coupled with HPLC/APCI/MS analysis allowed the development of a highly sensitive method for the quantitation of trace levels of LCFAs from biological and natural environmental samples. (c) 2006 Elsevier B.V. All rights reserved.

Determination of 30 free fatty acids in two famous Tibetan medicines by HPLC with fluorescence detection and mass spectrometric identification

A simple and sensitive high-performance liquid chromatographic (HPLC) method with fluorescence detection and mass spectrometric identification has been developed for analysis of 30 long-chain and short-chain free Fatty acids (FFAs). The fatty acids were derivatized to their esters with 1-[2-(p-toluenesulfonate)ethyl]-2-phenylimidazole-[4,5-f]-9,10-phenanthrene (TSPP) in N,N-dimethylformamide (DMF) at 90 degrees C with anhydrous K2CO3 as catalyst. A mixture Of C-1-C-30 fatty acids was completely separated within 60 min by gradient elution on a reversed-phase C-8 column. Qualitative identification of the acids was performed by atmospheric-pressure chemical ionization mass spectrometry (APCI-MS) in positive-ion mode. The fluorescence excitation and emission wavelengths were 260 and 380 nm, respectively. Quantitative determination of the 30 acids in two Tibetan medicines Gentiana straminea and G. dahurica was performed. The results indicated that the medicines contained many FFAs. Linear correlation coefficients for the FFA derivatives were > 0.9991. Relative standard deviations (RSDs, n = 6) for the fatty acid derivatives were < 3%. Detection limits (at a signal-to-noise ratio of 3:1) were 3.1-38 fmol. When the fatty acid derivatives were determined in the two real samples results were satisfactory and the sensitivity and reproducibility of the method were good.

Structural Evolution and Property Changes in Nd_{60}Al_{10}Fe_{20}Co_{10} Bulk Metallic Glass During Crystallization

The structural evolution and property changes in Nd60Al10Fe20Co10 bulk metallic glass (BMG) upon crystallization are investigated by the ultrasonic method, x-ray diffraction, density measurement, and differential scanning calorimetry. The elastic constants and Debye temperature of the BMG are obtained as a function of annealing temperature. Anomalous changes in ultrasonic velocities, elastic constants, and density are observed between 600–750 K, corresponding to the formation of metastable phases as an intermediate product in the crystallization process. The changes in acoustic velocities, elastic constants, density, and Debye temperature of the BMG relative to its fully crystallized state are much smaller, compared with those of other known BMGs, the differences being attributed to the microstructural feature of the BMG.

Nd_(60)Al_(10)Fe_(20)Co_(10)金属玻璃的变形行为

利用材料测试系统(MTS)、X-Ray 衍射(XRD)和扫描电镜(SEM)等手段研究了Nd 基大块金属玻璃的变形行为和断裂特征。Nd 基大块金属玻璃样品在室温下是脆性断裂,大约在500 K 时变形模式从非均匀变形转变为均匀变形,在523 K 以上表现出显著的塑性变形。在5×10-4 m/s 的应变速率下,这种Nd 基大块金属玻璃材料在523 K~600 K 之间出现明显的屈服应力下降现象,随后进入1 种稳定的粘性流动状态,而且这种屈服下降现象与温度和应变速率有关。这种在过冷液相区的变形行为与其他大块金属玻璃变形特征相似。合金的这种塑性变形行为表明了其存在稳定的过冷液相区,同时对其变形行为的研究有助于进一步了解Nd 基大块金属玻璃的反常热稳定性。

Influence of Surface Stress on Frequency of Microcantilever-Based Biosensors (vol 10, pg 307, 2004)

Microcantilever-based biosensors have been found increasing applications in physical, chemical, and biological fields in recent years. When biosensors are used in those fields, surface stress and mass variations due to bio-molecular binding can cause the microcantilever deform or the shift of frequency. These simple biosensors allow biologists to study surface biochemistry on a micro or nano scale and offer new opportunities in developing microscopic biomedical analysis with unique characteristics. To compare and illustrate the influence of the surface stress on the frequency and avoid unnecessary and complicated numerical solution of the resonance frequency, some dimensionless numbers are derived in this paper by making governing equations dimensionless. Meanwhile, in order to analyze the influence of the general surface stress on the frequency, a new model is put forward, and the frequency of the microcantilever is calculated by using the subspace iteration method and the Rayleigh method. The sensitivity of microcantilever is also discussed. (19 refs.)

Nd65Al10Fe25-xCox (x=0,5,10) bulk metallic glasses with wide supercooled liquid regions

Bulk metallic glasses of Nd65Al10Fe25-xCox (x=0,5,10) have been prepared in the form of 3 mm diam rods. Results of differential scanning calrimetry, dynamic mechanical thermal analysis (DMTA), and x-ray diffraction are presented for these alloys. It is shown that the glass transition and crystallization have been observed by DMTA. The reduced glass transition temperature of these glasses, defined as the ratio between the glass transition temperature T-g and the melting temperature T-l is in the range from 0.55 to 0.62. All these glasses have a large supercooled liquid region (SLR), ranging from 80 to 130 K. The high value of reduced glass transition temperature and wide SLR agree with their good glass formation ability.

我国随机振动研究近10年来的进展

该文回顾了中国振动工程学会随机振动专业委员会成立后的10年间我国学者在随机振动领域所进行的理论、应用技术研究方面取得的一些重要进展。着重介绍了随机非线性响应时域积分方法与空间有限元结合的随机动力有限元方法的发展；对随机振动与其他相关学科的交叉渗透进一步发展的前景也作了展望。

Shock tube study of JP-10 ignition delay time

JP-10 (exo-tetrahydrodicyclopentadiene, C10H16) ignition delay times were measured in a preheated shock tube. The vapor pressures of the JP-10 were measured directly by using a high-precision vacuum gauge, to remedy the difficulty in determining the gaseous concentrations of heavy hydrocarbon fuel arising from the adsorption on the wall in shock tube experiments. The whole variation of pressure and emission of the OH or CH radicals were observed in the ignition process by a pressure transducer and a photomultiplier with a monochromator. The emission of the OH or CH radicals was used to identify the time to ignition. Experiments were performed over the pressure range of 151-556 kPa, temperature range of 1000-2100 K, fuel concentrations of 0.1%-0.55% mole fraction, and stoichiometric ratios of 0.25, 0.5, 1.0 and 2.0. The experimental results show that for the lower and higher temperature ranges, there are different dependency relationships of the ignition time on the temperature and the concentrations of JP-10 and oxygen.

10°尖锥标模高超声速动导数的实验测量

在中科院力学所JF-4B高超声速脉冲风洞中，用模型自由飞方法对10~。尖锥开展动态实验测量，并用参数微分法辨识得到了该模型的俯仰阻尼导数。实验结果表明，脉冲风洞中模型自由飞方法得到的10~。尖锥标模高超声速动态气动特性测量值与国外可比数据一致，重复测量精度与弹道靶试验相当。

国际尖端材料技术协会(SAMPE)第24届技术会议和第3届金属及金属加工会议(1992年10月20—22日,加拿大多伦多)

<正> 国际尖端材料技术协会(SAMPE:Society for the Advancement of Material and Process Engineering)于1992年10月20—22月在加拿大多伦多市召开了两个国际学术会议:第24届国际SAMPE技术会议(24th Int.SAMPE Techn。Coaf。)和第3届国际金属与金属加工会议(3rd Int.SAMPE Metals and Metals Processin Conf.)。两个会议同时举行,全体会议(Plenary Session)在一个会场举行。前者的主题是“先进材料迎接经济的挑战”;后者的主题是“合成与加工的新进展”.尽管此二会议是在西方发达国家经济很不景

DG-10型数字光栅测微仪

本文介绍一种0～10mm、分辨率1μm数字光栅测微仪,它是一种具有任意零点、高精度的测长系统,由光栅位移传感器和数显仪两部分组成。介绍了其工作原理、主要技术指标和应用。

在高超声速脉冲风洞中使用的六分量天平测力系统和10°尖锥模型的气动力测量

在中国科学院力学研究所的 JF-4B 高超声速脉冲风洞中,对于半锥角为10°的尖锥模型进行了来流马赫数为7.8和9.9的吹风实验,在不同的α角和β角下使用六分量的压电天平进行了气动力测量。用以鉴定六分量测力系统的可靠性,并检验了新的试验段和α角与β角分别单独可变的模型支架对模型测力实验是否有干扰。实验结果与文献给的结果进行比较表明:六分量压电天平测力系统给出的实验数据是比较可靠的。

DG-10数显光栅测微仪

<正> 由中国科学院力学研究所研制的DG-10数显光栅测微仪,经中国计量科学研究院检定,其主要技术指标: 1.量程0-10mm;2.分度值0.001mm;3.示值误差在全量程内为±0.001mm;4.回程误差0.001mm;5.测杆受径向力作用时示值变化0.001mm。