Sample handling and contamination encountered when coupling offline normal phase high performance liquid chromatography fraction collection of petroleum samples to Fourier transform ion cyclotron resonance mass spectrometry

Normal phase high performance liquid chromatography (HPLC) is used to separate a gas oil petroleum sample, and the fractions are collected offline and analyzed on a high resolution Fourier Transform Ion Cyclotron Resonance Mass Spectrometer (FT-ICR MS). The separation prior to MS analysis dilutes the sample significantly; therefore the fractions need to be prepared properly to achieve the best signal possible. The methods used to prepare the HPLC fractions for MS analysis are described, with emphasis placed on increasing the concentration of analyte species. The dilution effect also means that contamination in the MS spectra needs to be minimized. The contamination from molecular sieves, plastics, soap, etc. and interferences encountered during the offline fraction collection process are described and eliminated. A previously unreported MS contamination of iron formate clusters with a 0.8 mass defect in positive mode electrospray is also described. This interference resulted from the stainless steel tubing in the HPLC system. Contamination resulting from what has tentatively been assigned as palmitoylglycerol and stearoylglycerol was also observed; these compounds have not previously been reported as contaminant peaks.     

“化学一步法”制备电磁功能化聚吡咯/γ-Fe2O3复合物纳米球及结构表征

在不添加掺杂剂的条件下, 以吡咯为单体, 三氯化铁为氧化剂, 采用"化学一步法"合成了电磁功能化的聚吡咯/γ-Fe2O3 复合物纳米结构. 研究了不同氯化亚铁用量对聚吡咯/γ-Fe2O3 复合物形貌、 电学性能以及磁学性能的影响. 结果表明, 氯化亚铁的用量对聚吡咯/γ-Fe2O3复合物的形貌影响不大, 都得到了聚吡咯/γ-Fe2O3复合物纳米球; 然而, 聚吡咯/γ-Fe2O3复合物纳米球的电学和磁学性能却明显受到氯化亚铁用量的影响. 聚吡咯/γ-Fe2O3复合物纳米球的电导率和最大饱和磁化强度随着氯化亚铁用量的增加而增大, 并在氯化亚铁用量增加到150 mg时达到最大值, 分别为72.1 S/cm和10.07 A·m2/kg, 实现了高电学性能和高磁学性能兼顾的电磁功能化导电聚合物纳米结构的制备.     

Continuous Lactate Measurement that Combines a Portable Ultrafiltration Storage Device with an Enzyme Sensor

ABSTRACT|A simple portable continuous L-lactate monitoring system combining elegant ultrafiltration sample collection and storage with a lactate biosensor has been developed.|The sensor has a detection range from 0.05mM to 30mM lactate dependent on different assignments of the PCS hydrogel complex layer.|The sensor shows excellent performance on sensitivity and validity as well as operational stability over one month.|Samples containing different concentrations of lactate were collected in six hours with an ultrafiltration probe and stored in a 6m long PEEK tube of 125μm in internal diameter.|The ultraslow flow rate of 100 to 350nl/min was controlled by adjusting the restriction in the portable plastic syringe pump and a constant flow can be maintained over 24 hours.|The collected samples were then detected after reversing the flow with a lactate sensor.

The total weight of the collection system is only 8g, allowing free movement of the person being tested.     

Temperature dependence of the P-hit single event transient pulse width in a three-transistor inverter chain

A comparison of the temperature dependence of the P-hit single event transient (SET) in a two-transistor (2T) inverter with that in a three-transistor (3T) inverter is carried out based on a three-dimensional numerical simulation.Due to the significantly distinct mechanisms of the single event change collection in the 2T and the 3T inverters,the temperature plays different roles in the SET production and propagation.The SET pulse will be significantly broadened in the 2T inverter chain while will be compressed in the 3T inverter chain as temperature increases.The investigation provides a new insight into the SET mitigation under the extreme environment,where both the high temperature and the single event effects should be considered.The 3T inverter layout structure (or similar layout structures) will be a better solution for spaceborne integrated circuit design for extreme environments.     

ICP-AES检测云南稻核心种质矿质元素含量的地带性特征

采用电感耦合等离子体原子发射光谱法(ICP-AES)测定了云南省5个稻作区16个州市的789份地方水稻糙米中的八种矿质元素, 该方法简单快速、灵敏度高、准确性好和多元素同时测定, 加标回收率为97.1%～110.2%, RSD为0.7%～4.4%。结果表明: 糙米元素含量(mg·kg-1)依次为P(3834.83±486.49)>K(2567.72±336.74)>Mg(2567.72±336.74)>Ca(153.67±55.90)>Zn(33.35±13.65)>Fe(32.08±25.51)>Cu(14.22±11.85)>Mn(13.58±3.22); 世界生物多样性最丰富及有色金属富集的滇西北糙米P含量高,早寒武纪动物群及磷矿富集的滇中糙米Ca,Mg,Fe和Zn含量高,作物多样性突出的滇西南糙米Cu和Mn含量高; 糙米高磷钾、中钙镁锰和低铁锌分布区是世界生物多样性最丰富及矿产资源富集区。首次提出云南糙米矿质元素含量的地带性特征与生物多样性中心、矿产资源富集区、生命起源及其山脉、河流有关;进一步推断地球矿质元素分布不均匀性及其山脉、河流的相互作用是生命起源的关键。文章研究为解决人类Fe,Zn和Ca等矿质营养不良和生命起源问题以及功能稻米育种生产提供参考。     

Two Feasible Schemes for Preparing Cluster States with Ion-Trap Setup

We present two schemes for preparing cluster states with atomic qubits in an ion-trap system. In the first scheme an auxiliary atomic level is needed. While in the second scheme an additional classical driven field is used, and the multi-ion cluster states can be generated by one step. Both the schemes are insensitive to thermal motion of the ions, all the facilities used in them are well within state of the art.     

铁硅分子筛Fe-Silicalite-1催化剂的一步合成与应用

利用一步水热合成法,在有机模板剂1,6-己二胺结构导向作用下,合成了具有MFI骨架结构的铁硅酸盐分子筛晶体Fe-Silicalite-1.并通过XRD、TG-DTA、IR和SEM等测试方法对其结构和性能进行了表征.ICP-AES及EDS分析结果表明:Fe原子进入到分子筛骨架上,质量分数约为0.66;.在以过氧化氢为氧化剂,羟化苯酚的催化反应中,苯酚的转化率为22.2;,其中65.8;为邻苯二酚,34.2;为对苯二酚.Fe-Silicalite-1分子筛晶体是一种良好的合成二酚的催化剂,具有潜在的应用价值.     

An improved loopless mounting method for cryocrystallography

Based on a recent loopless mounting method, a simplified loopless and bufferless crystal mounting method is developed for macromolecular crystallography. This simplified crystal mounting system is composed of the following components: a home-made glass capillary, a brass seat for holding the glass capillary, a flow regulator, and a vacuum pump for evacuation. Compared with the currently prevalent loop mounting method, this simplified method has almost the same mounting procedure and thus is compatible with the current automated crystal mounting system. The advantages of this method include higher signal-to-noise ratio, more accurate measurement, more rapid flash cooling, less x-ray absorption and thus less radiation damage to the crystal. This method can be extended to the flash-freeing of a crystal without or with soaking it in a lower concentration of cryoprotectant, thus it may be the best option for data collection in the absence of suitable cryoprotectant. Therefore, it is suggested that this mounting method should be further improved and extensively applied to cryocrystallographic experiments.     

The Study of Full Light Speech Signal Collection System

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螺旋型旋风分离器两相流场的数值模拟

对螺旋型旋风分离器进行了两相流场的三维数值模拟．气体流场通过求解三维N-S方程得到,湍流模型采用了雷诺应力模型．计算结果表明,旋风分离器内部的流场分为两部分:螺旋通道内比较稳定的流场和筒体中心区域的复合涡结构流场．对颗粒运动轨迹的计算表明,颗粒在入口处的初始位置对颗粒分离有比较显著的影响．同时得到了不同入口速度下颗粒的分级效率曲线,并给出了气体流量对旋风分离器性能的影响,结果显示:气体流量的增加会提高分离效率,但同时导致压力损失的急剧增加．