基于颗粒谱的FCC旋风分离器故障诊断技术的初步探索

旋风分离器在催化裂化工艺中用于完成催化剂与油气或烟气的分离,是保证装置长周期安全运行的重要设备,因此对其运行状态进行监测和故障诊断非常必要。当旋风分离器运行出现异常时,跑损催化剂的样本将发生改变。基于可测信号处理的故障诊断方法,以催化剂作为故障信息的载体,通过提取催化剂的颗粒谱特征信息,如堆积密度、粒度分布、微观形态等,建立颗粒谱与故障之间的关系模型,提出了基于颗粒谱的旋风分离器故障诊断技术。

采用有机硅聚合物包膜硅胶颗粒键合金刚烷基高效液相色谱柱检测舒更葡糖钠有关物质

目的建立一种简单、快速、准确分析舒更葡糖钠有关物质纯度的检测方法。方法针对于舒更葡糖钠及其游离酸合成过程中的副产物或降解杂质,采用有机硅聚合物包膜硅胶颗粒键合金刚烷基高效液相色谱柱(ADME),以0.025 mol/L磷酸二氢钠水溶液(用1.5 mol/L磷酸调节pH至3.0)∶乙腈=83∶20为流动相A,乙腈为流动相B,流速为0.27 mL/min,检测波长为200 nm,柱温为40℃,进样量为2.5μL。结果在该色谱条件下,舒更葡糖钠有关物质分离完全,线性良好,精密度良好,回收率在84.70%~119.99%。结论该方法灵敏度高,准确可靠,安全环保,可用于舒更葡糖钠有关物质纯度检测。

气团来源对瓦里关地区颗粒物数谱分布的影响

通过对2005年8月到2007年5月在瓦里关全球本底站观测的气溶胶数谱分布资料和同期后向轨迹资料分析,发现气团来源对瓦里关地区颗粒物的数浓度及其谱分布有显著影响.气团起源于瓦里关东北部地区或者途径东北部地区,传输路径较短,传输速度相对较慢,大气中出现较高数浓度的爱根核模态颗粒物;气团来源于瓦里关西部或者西北地区时,传输路径较长,传输速度较快,大气中一般出现较高浓度的核模态颗粒物.

利用单颗粒气溶胶质谱仪研究石家庄市采暖结束前后大气细颗粒物污染特征及成因

2016年3月1日~20日期间,石家庄市区于采暖期结束前后出现两次重污染天气。为探究重污染天气成因,利用位于石家庄市大气自动监测站(20 m)的单颗粒气溶胶质谱仪(SPAMS)对两次重污染天气期间的细颗粒物化学组成进行分析;并结合颗粒物质量浓度和气象条件等对重污染天气成因进行了推定。结果表明,3月采暖期(3月1日~15日)期间共发生为期1 d的重度污染天气,主要成因为来自燃煤(贡献率42.6%)和工业工艺源(26.4%)的颗粒物严重累积;采暖期结束后(3月16日~20日)出现了连续3 d的重度污染天气,前期主要成因为来自机动车尾气(25.5%~25.9%)和工业工艺源(23.0%~25.5%)的颗粒物严重累积;后期首要污染源变为燃煤(28.6%)和工业工艺(27.4%)。监测过程中,PM_(2.5)与气象条件的相关性较高,r_(湿度/2.5)=0.76,r_(大气压/2.5)=-0.58,r_(风速/2.5)=-0.65,r_(温度/2.5)=0.35。综合来看,高湿状态下空气的低压静稳和低空传输,共同促使燃煤及工业工艺源的颗粒物累积,二次转化加剧后导致3月4日的重污染天气;而采暖期结束后,在同样不利于扩散的气象条件下,机动车尾气及工业工艺源的颗粒物累积,二次转化加剧,从而导致3月17和18日污染小高峰;不同于前两日,燃煤和工业工艺源的累积,二次转化加剧,导致了3月19日凌晨的污染小高峰。

甘桔利咽颗粒的薄层色谱鉴别

目的建立甘桔利咽颗粒的鉴别方法。方法采用薄层色谱法,以甘草、玄参、柯子的对照药材为对照品,对成品的醋酸乙酯提取液进行薄层层析,并作阴性对照。结果同一薄层板上的成品色谱显示与3种对照药材相对应的特征斑点,阴性对照证明无干扰。结论所建立的方法可用于甘桔利咽颗粒的鉴别。

气溶胶飞行时间质谱仪单颗粒质谱偏移问题及其纠正算法

在单颗粒气溶胶质谱分析中,不同颗粒质谱图之间发生质谱偏移,谱峰质量数难以准确测定的现象已经被多次观察到。这种现象的存在使得应用单一的校准参数校准质谱图时,产生质谱峰辨认的不确定性。不同颗粒质谱图之间最大的偏移取决于电离激光光斑的大小。当校准参数不准确时,某质谱峰偏离正确m/z值的大小与该质谱峰的质量数呈线性相关。从理论上证明了这种偏移产生于颗粒物在激光光斑内电离位置的不同。为解决单一校准参数带来的不可避免的误差,提出了一种可编程的算法来自动找出每个颗粒物质谱的最优校准参数,以实现单颗粒质谱图的准确的质量校准。

机动车颗粒物数排放因子和特征

为了对现实环境中机动车颗粒物数排放因子及其排放特征进行研究,在丹麦哥本哈根市高速公路和城区分别设立了交通站点和背景站点,经过长期观测计算得到交通源排放的贡献,并结合机动车数据估算了颗粒物数浓度排放因子。结果表明,在高速公路和城区平均车流的颗粒物数排放因子分别是（215.4±5.3）×1012km 1和（187.1±3.1）×1012km 1。重型车和轻型车颗粒物数的排放因子都是在城区较高,重型车颗粒物数的排放因子大约是轻型车颗粒物数排放因子的20倍左右。机动车排放颗粒物数谱具有双峰特征,峰值因观测地点的不同而变化,高速公路边的峰值在10 nm左右,城区的峰值在20~30 nm之间,高速公路和城区都出现50~80 nm的第二峰值。颗粒物数排放因子主要由粒径小于100 nm的颗粒物数决定。轻型车和重型车的颗粒物数排放因子对机动车数量和类型有一定的依赖性,观测地点和环境等因素也会造成现实环境中机动车颗粒物数排放因子研究结果的不确定性。

无锡市分级颗粒物来源解析研究

在无锡市崇宁和旺庄环境监测子站,通过对分级颗粒物进行不同季节(2014年4、7、10、12月)的采样,同时对当地颗粒物主要排放源进行采样,并对受体和排放源样品浓度和化学成分进行特征分析,结合化学质量平衡(CMB)模型解析无锡市城区和工业区分级颗粒物来源,确定分级颗粒物不同排放源的贡献率.两个观测站点,PM10年均浓度分别为143.1μg·m^(-3)(崇宁站)、119.9μg·m^(-3)(旺庄站);PM_(2.1)平均质量浓度分别为71.9μg·m^(-3)(崇宁站)、65.3μg·m^(-3)(旺庄站);PM_(1.1)年平均质量浓度分别为53.7μg·m^(-3)(崇宁站)、49.9μg·m^(-3)(旺庄).崇宁站各级颗粒物平均质量浓度均要高于旺庄站,季节差异上,颗粒物浓度在冬季明显高于其他三个季节.分级颗粒物最主要的化学成分是NO_3^-、SO_4^(2-)、OC、NH_4^+、EC、Ca、Cl^-、K、Fe、Al、Na等,通过质量重构方法后最主要的化学组分依次是颗粒态有机物(POM)、硫酸根(SO2-4)、硝酸根(NO-3)、铵根(NH_4^+)、地壳元素(CM)、其它水溶性离子、元素碳(EC)和微量元素.利用CMB模型计算得到,无锡市PM10的排放源主要为二次硝酸盐(18.2%)、二次硫酸盐(17.3%)、土壤扬尘(9.0%),PM_(2.1)最主要的三类排放源依次是二次硝酸盐(26.4%)、二次硫酸盐(22.6%)和电厂燃煤(7.3%),PM_(1.1)的排放主要来自二次硝酸盐和二次硫酸盐,分别可以达到26.6%和22.5%.分级颗粒物来源解析结果可以看出,粗粒径颗粒物主要来自于扬尘类、汽车尾气和工业过程,细粒径颗粒物主要来自汽车尾气和工业过程.为了减轻无锡市颗粒物浓度水平,重点是控制燃煤、工业生产活动中大气污染物的排放,同时要加强城市建设中的扬尘和交通废气控制.

重污染和新粒子生成过程中城市大气颗粒物数谱分布演变过程

使用双电迁移性颗粒物粒径谱分析仪和空气动力学颗粒物粒径谱分析仪对北京城市大气颗粒物(3nm^10μm)数浓度谱分布进行长期观测.选取2006年春节期间出现的一次重污染事件和一次新粒子生成过程,对期间颗粒物数谱分布特征及演变过程进行分析.在重污染事件中3~10nm颗粒物(平均数浓度46cm?3)几乎在大气中消失,而新粒子生成事件中核模态颗粒物数浓度最高达到3.5×104cm?3.这种现象可以通过颗粒物的碰并汇和低挥发性气态前体物的凝结汇从颗粒物的汇和源两个角度进行解释:重污染事件中,3~10nm颗粒物的碰并汇为1.1×10?2~1.2×10?3s?1,显著高于新粒子生成过程(9.9×10?4~1.4×10?4s?1);在新粒子生成过程中,参与成核的低挥发性气态前体物的凝结汇为0.01s?1,显著低于重污染事件(0.13s?1).研究结果表明在分析极端大气环境中的颗粒物数谱分布时,除交通和气象因素外,碰并和凝结过程的影响也需要给予足够的重视.

300MW燃煤锅炉静电除尘器的现场实验和数值模拟

采用实验研究和数值模拟的方法对除尘装置收集烟尘颗粒的过程进行定量描述,是发展高效可吸入颗粒物（PM）除尘方案的理论基础。对300MW燃煤锅炉静电除尘器（ESP）前后的飞灰颗粒进行在线采样,以研究其尺度分布规律和排放特征,采样系统由高温水冷取样管、旋风分离器和低压撞击器组成。实验结果表明,ESP前后飞灰颗粒呈典型的双峰分布,峰值出现在0.08μm和2-5μm附近。然后以ESP进口实验结果为初始条件,采用事件驱动常体积法对ESP的除尘过程进行颗粒群平衡模拟,能够得到烟尘颗粒尺度谱在ESP纵向长度上演变过程的细节信息,ESP出口颗粒尺度分布的模拟结果与试验结果较为吻合。

实心核颗粒色谱分离-HPLC-MS/MS法同时测定性保健品中非法添加15种壮阳类化学成分

目的建立了性保健品中非法添加15种壮阳类化学成分的实心核颗粒色谱分离-HPLC-MS/MS检测方法。方法以高色谱性能的实心核颗粒色谱柱CORTECS-C18(150 mm×4.6 mm,2.7μm)分离,串联四级杆质谱仪检测,MRM模式进行定性定量分析,样品以甲醇为溶剂超声提取,检测添加在性保健品中的甲磺酸酚妥拉明、那红地那非、红地那非、伐地那非、西地那非、羟基豪莫西地那非、豪莫西地那非、氨基他达拉非、他达拉非、硫代艾地那非、伪伐地那非、那莫西地那非、甲睾酮、司坦唑醇和达那唑共15种化学成分。结果 15种壮阳类化学成分质谱检测的分离度较好,线性范围宽,相关性好,r2≥0.995 4;方法精密度以6次测定值的RSD表示,为0.9%~3.3%;方法回收率用3个质量浓度进行添加实验,回收率为88.3%~109.5%,RSD为0.9~5.2%;定量限范围为0.015~0.30μg/m L;日内精密度和日间精密度的RSD分别为0.9%~4.2%和1.0%~4.5%;25批次性保健品中检出阳性样品20批次,检出成分均为西地那非,不合格率达80%。结论本方法通用性强,操作简单,可作为性保健品中非法添加15种壮阳类化学成分的有效检测方法。

Effects of Water Stress on the Mssbauer Spectrum of Fe^(2+) /Fe^(3+) Components in Cucumber PSⅡ Particles

There were four doublets in the Mssbauer spectrum of cucumber (Cucumis sativus L.) photosystemⅡ (PSⅡ) particles. According to the value of isomer shift and quadrupole splitting, they represented oxidized cytochrome b559 (Cyt_b559), reduced Cyt_b559, Fe 3+ _quinone (Q) complex, and Fe 2+ _Q complex respectively. After water_stress, the electron transport rate between Q A (primary quinone electron acceptor of PSⅡ)/Q B(secondary quinone electron acceptor of PSⅡ) was affected and the absorption doublets of Fe 2+ disappeared, suggesting that the reduced Cyt_b559 and Fe 2+ _Q complex had been oxidized. The results indicated that water_stress had changed the redox status of iron in the iron_quinone complex. Iron took part in electron transport through the change from a state of reduction to oxidation.

Noble metal-like behavior of plasmonic Bi particles deposited on reduced TiO2 microspheres for efficient full solar spectrum photocatalytic oxygen evolution

Herein, novel plasmonic Bi metal in situ deposited in reduced Ti O2 microspheres(Bi@R-Ti O2) are fabricated via a bimetallic MOF-derived synthesized strategy by adjusting the synthesizing temperature. Different characterization techniques, including XRD, SEM, TEM, XPS, DRS, PL, EIS, and photocurrent generation, are performed to investigate the structural and optical properties of the as-prepared samples. The results indicate that the Bi particles are generated inside and outside of reduced Ti O2 microspheres via the reduction of Ti4+ and Bi3+ by ethylene glycol. When the annealing temperature is controlled at 300 o C, the corresponding Bi@R-Ti O2-300 sample with an appropriate amount of Bi nanoparticles exhibits the highest full solar spectrum photocatalytic oxygen evolution activity(4728.709 μmol h–1 g–1), which is 5.9 and 9.5 times higher than that of pure Ti O2 and Bi-Ti bimetal organic frameworks(Bi-Ti-MOFs). Several reasons are suggested for the above results:(1) Bi metal behaves as an "electron acceptor" to accelerate the charge carrier transfer from Ti O2 to Bi;(2) The surface plasmon resonance effect of loaded metallic Bi particles can enhance the visible and NIR light absorption capacity;(3) The generation of Ti3+ further narrows the band gap of TiO2.

保健食品中非法添加降糖药物的测定方法研究

目的探讨实心核颗粒色谱技术与反相高效液相色谱法在保健食品中非法添加降糖药物的测定效果。方法分别采用实心核颗粒色谱技术与反相高效液相色谱法对90批保健食品中非法添加的盐酸二甲双胍、盐酸苯乙双胍、甲苯磺丁脲、格列吡嗪、格列齐特、马来酸罗格列酮、盐酸吡格列酮、格列本脲、格列美脲、格列喹酮及瑞格列奈11种化学药品含量进行测定。实心核颗粒色谱技术与反相高效液相色谱法在降糖类保健食品非法添加降糖药物的测定中的分离度均较好,线性范围均较宽。结果实心核颗粒色谱技术平均回收率在96.8%~104.6%之间,RSD在0.52%~1.92%之间;反相高效液相色谱法平均回收率在96.4%~101.5%之间,RSD在0.43%~2.48%之间。实心核颗粒色谱技术检出19批保健食品存在非法添加降糖药物,检出率21%;反相高效液相色谱法检出18批保健食品存在非法添加降糖药物,检出率20%;两种方法检出率差异不明显。结论实心核颗粒色谱技术与反相高效液相色谱法均具有操作简便、准确及重现性好等优点,且实心核颗粒色谱技术不会受到高浓度盐酸影响从而避免管路堵塞问题,适用性更高。

Evaluation of nanometer-sized zirconium oxide incorporated Al-Mg-Ga-Sn alloy as anode for alkaline aluminum batteries

Zirconium oxide nanoparticles with 0.4 wt.%and 0.8 wt.%are incorporated into the Al-0.65 Mg-0.05 Ga-0.15 Sn(wt.%)alloy anode(base alloy)in order to improve the performance of the resulting anodes.Electrochemical characterization of the reinforced alloys was done by potentiodynamic polarization,electrochemical impedance spectroscopy and galvanostatic discharge and corrosion behavior was evaluated using self-corrosion rate and hydrogen evolution in 4 mol/L KOH solution.The surface morphology of the alloys was also studied using field emission scanning electron microscope(FESEM).The obtained results indicate that the base alloy shows high corrosion rate in 4 mol/L KOH solution by releasing 0.47 m L/(min·cm^2)hydrogen gas,whereas the alloy containing 0.8 wt.%Zr O2 provides the lowest hydrogen evolution rate by releasing 0.32 m L/(min·cm^2)hydrogen gas.Furthermore,by increasing zirconium oxide nanoparticles,the corrosion current density of the aluminum anodes is decreased and their corrosion resistance increases significantly compared to the base alloy in alkaline solution.In addition,nanometer-sized zirconium oxide incorporated anodes exhibit the improved galvanic discharge efficiencies,so that 0.8 wt.%nano-zirconium oxide incorporated base alloy displays the highest power density and anodic utilization compared with the others in 4 mol/L KOH solution.

Highly Ordered Lattice Orientation of ZnO Nanoparticles Formed in Confined Space

Oriented aggregation of nanoparticles has been accomplished by means of solid state reac- tion. Non-crystallized and crystallized ZnO nanoparticles/clusters could be accommodated in the lamellar spacing of inorganic-organic composite, which were prepared by thermolysis of layered solid zinc-oleate complex at 260 and 300 ℃ in air, respectively. High-resolution transmission electron microscopy and selected area electron diffraction patterns indicate that aggregates are single crystals with various defects. The photoluminescence excitation spectra of both samples show two bands at 272 and 366 nm. The former may originate from electron transfer from valence band to conduction band in ZnO clusters composed of less than 200 ZnO molecules （2R〈2 nm）.

Study on GC-MS fingerprint of petroleum ether fraction of Shenqi Jiangtang Granules

Objective To establish gas chromatography-mass spectrometry(GC-MS)fingerprint method for the petroleum ether fraction of Shenqi Jiangtang Granules(SQJTG)and evaluate the product quality.Methods The GC-MS fingerprint of petroleum ether fraction of SQJTG was established by GC-MS,and the chemical components corresponding to the fingerprint peaks were structurally identified on NIST2014.The batch consistency of SQJTG products was evaluated based on the chemical composition of petroleum ether parts by using fingerprint similarity evaluation and Principal components analysis(PCA)technology.At the same time,Hotelling's T2 and DMODX statistics are used to set the control range for the quality of different batches of products.Results Twenty-two components were identified from the petroleum ether part of SQJTG,accounting for 60.94%of the total components separated.The similarity of fingerprints of petroleum ether parts of 24 batches of SQJTG was greater than 0.95.The PCA of 24 batches of samples were all under the control limits of Hotellin’s T2 and DMODX statistics,indicating that the petroleum ether parts of different batches of SQJTG were consistent.Conclusion The developed GC-MS fingerprint method can be used to evaluate the quality of SQJTG.

Surface-sulfurized Ag_2O nanoparticles with stable full-solar-spectrum photocatalytic activity

Ag2O has attracted much recent attention,because of its high photocatalytic activity in the ultraviolet(UV)‐visible region.However,there have been few reports on the near‐infrared(NIR)photocatalytic activity of Ag2O.This paper reports the high NIR photocatalytic activity of Ag2O nanoparticles.Ag2O is unsuitable for application in full‐solar‐spectrum photocatalysis,because it is unstable under UV irradiation.A surface sulfurization process was carried out to address this issue.Specifically,a layer of Ag2S2O7nanoparticles was grown on the surface of the Ag2O nanoparticles,to improve the stability of the Ag2O photocatalyst and enhance its photocatalytic activity in the UV,visible and NIR regions.The Ag2O/Ag2S2O7heterostructure is a stable and efficient full‐solar‐spectrum photocatalyst.It has potential application in the photodegradation of organic pollutants,and more generally in environmental engineering where full utilization of the solar spectrum is required.

Determination of brominated diphenyl ethers in atmospheric particulate matter using selective pressurized liquid extraction and gas chromatography–mass spectrometry with a negative chemical ionization

This study describes the development and validation of a sensitive and reliable method for determination of polybrominated diphenyl ethers（PBDEs）in atmospheric particulate matter using selective pressurized liquid extraction（SPLE）and gas chromatography–mass spectrometry with a negative chemical ionization（GC-NCI-MS）.Extraction and clean-up were performed using PLE with 2 g florisil and 3 g silica placed in the extraction cells.Under optimal conditions,14 PBDEs were extracted at 70℃ using hexane/dichloromethane（50：50,v/v）as solvent.Validation of SPLE returned excellent recoveries for most analytes,with relative standard deviations mostly below20%.Method detection limits ranged from 0.13 to15.38 ng·mL^-1 for the GC-MS analyses.The method was successfully applied to atmospheric particulate matter of Beijing,where analytes were detected in the range of182.79 to 468.99 pg·m^-3.

Rapid Purification of Enhanced Green Fluorescent Protein from Escherichia coli

As an excellent reporter molecule, enhanced green fluorescent protein (eGFP) was widely used for gene expression and regulation and was generally expressed in Escherichia coli strain. A rapid procedure consisting of ammonium sulfate precipitation, size exclusion chromatography, and anion exchange chromatography was devel- oped for the purification of eGFP. Based on the proposed procedure, recombinant eGFP with an electrophoretic pu- rity was achieved in combination with an overall yield of 66% and a purification factor of 17.9. The fluorescent spectrometry of purified eGFP and lysate from E. coli strain expressing eGFP exhibited the same wavelength of ex- citation and emission maxima, indicating that the purification procedure did not influence the construct and fluo- rescent characteristics of desired protein. The procedure mentioned was easy to scale up for the purification of large quantities of eGFP.