A Novel Atomic Force Microscope with High Stability and Scan Speed

Abstract

A novel atomic force microscope (AFM) has been developed. Unlike conventional AFM systems, its cantilever and tip were set up in the X direction with respect to the sample. It can practically eliminate the crawling effect of the probe itself. Meanwhile, using a beam splitter, we devised a unique path optical beam deflection method for the measurement of the cantilever's displacement with its minimized structure and an optimal light‐amplifying ratio; the position of the sensitive detector (PSD) is just in front of the visual sight of operator. This makes observation and operation easier. Furthermore, the PSD attached to the translation stage can be adjusted and, thus, adapts the setpoint of imaging force to different samples. In this way, our new AFM provides high stability and scan speed. The highest scan rate is about 40 lines/s or 10s for a 400×400‐pixel, 3 µm×3 µm image.     

Characterization and application of lornoxicam,europium(III), and lysozyme fluorescence

A novel and sensitive spectrofluorimetric method was developed for the determination of lornoxicam. The method was based on the fluorescence enhancement of europium(III) by formation of a ternary complex with lornoxicam in the presence of lysozyme as the co-ligand. The fluorescence signal for the lornoxicam-europium (III)-lysozyme system was monitored at an excitation wavelength of 620 nm and an emission wavelength of 390 nm. The parameters affecting the fluorescence intensity were optimized systematically and under these conditions the signal was directly proportional to the concentration of lornoxicam from 9.0 × 10^?5 to 1.0 × 10^?2 µg · mL^?1. The detection limit was 2.7 × 10^?5 µg · mL^?1. The relative standard deviation for thirteen replicate measurements of 1.0 × 10^?3 µg · mL^?1 lornoxicam was 1.8%. This method was employed for the determination of lornoxicam in pharmaceutical formulations and biological fluids. The mechanism of fluorescence for the lornoxicam-europium(III)-lysozyme system was discussed.     

Stereological measures of trabecular bone structure: comparison of 3D micro computed tomography with 2D histological sections in human proximal tibial bone biopsies

Stereology applied on histological sections is the ‘gold standard’ for obtaining quantitative information on cancellous bone structure. Recent advances in micro computed tomography (µCT) have made it possible to acquire three-dimensional (3D) data non-destructively. However, before the 3D methods can be used as a substitute for the current ‘gold standard’ they have to be verified against the existing standard. The aim of this study was to compare bone structural measures obtained from 3D µCT data sets with those obtained by stereology performed on conventional histological sections using human tibial bone biopsies. Furthermore, this study forms the first step in introducing the proximal tibia as a potential bone examination location by peripheral quantitative CT and CT. Twenty-nine trabecular bone biopsies were obtained from autopsy material at the medial side of the proximal tibial metaphysis. The biopsies were embedded in methylmetacrylate before µCT scanning in a Scanco µCT 40 scanner at a resolution of 20 × 20 × 20 µm³, and the 3D data sets were analysed with a computer program. After µCT scanning, 16 sections were cut from the central 2 mm of each biopsy and analysed with a computerized method. Trabecular bone volume (BV/TV) and connectivity density (CD) were estimated in both modalities, whereas trabecular bone pattern factor (TBPf) was estimated on the histological sections only. Trabecular thickness (Tb.Th), number (Tb.N) and separation (Tb.Sp), and structure model index (SMI) were estimated with the µCT method only. Excellent correlations were found between the two techniques for BV/TV (r = 0.95) and CD (r = 0.95). Additionally, an excellent relationship (r = 0.95) was ascertained between TBPf and SMI. The study revealed high correlations between measures of bone structure obtained from conventional 2D sections and 3D µCT data. This indicates that 3D µCT data sets can be used as a substitute for conventional histological sections for bone structural evaluations.     

大型车载光电跟踪设备隔振基础的主动控制

为了保证大型车载光电跟踪设备的稳定工作,提出了一种跟踪架的隔振方法。采用空气弹簧加上电磁作动器实施减振,其电磁作动器采取差动布置方案,使电磁作动器的输出力与控制电流成线性关系。对几种控制方法进行了对比分析,选用绝对速度反馈控制,保证隔振基础对高频振动的隔振能力,同时避免低频振动时产生共振。最后,通过MAT-LAB进行仿真分析。仿真和实验结果显示,z向低频振动振幅已从5×10-5m减至1.8×10-5m,θx向低频振动振幅从2.2×10-5m减至0.6×10-5m,θy向低频振动振幅从2.0×10-5m减至0.4×10-5m,同时能够避免产生共振,表明采用绝对速度反馈主动控制方法可以起到较好的减振作用。     

PVC Membrane Sensor for Potentiometric Determination of Fluoxetine in Some Pharmaceutical Formulations

Abstract

The construction and general performance of a novel potentiometric membrane sensor for determination of fluoxetine has been developed. It is based on the formation of the ion association complex of fluoxetine with picrolonic acid as electroactive material, dispersed in a PVC matrix and o‐nitrophenyl octyl ether as a plasticizer. The sensor shows a fast, stable, and near Nernstian response for 1×10^?2 M to 8×10^?6 M fluoxetine at 25°C over the pH range of 1–5 with a cationic slope of 51±0.5 mV/decade. The lower detection limit is 6×10^?6 M and the response time 20–35 sec. Selectivity coefficients for fluoxetine, related to number of interfering substances, were investigated. There are negligible interferences from the studied cations, anions, and pharmaceutical excipients. The determination of fluoxetine in aqueous solution shows an average recovery of 98.6% and a mean relative standard deviation (RSD) of 1.5% at 100 µg/mL. The direct determination of fluoxetine in some formulations gave results that compare favorably with those obtained by a spectrophotometric method. The developed membrane electrode has been used as an end point indicator electrode, e.g., potentiometric titration of fluoxetine with sodium tetraphenylborate as a titrant has been monitored.     

PVC Membrane Sensor for Potentiometric Determination of Atropine in Some Pharmaceutical Formulations

Abstract

The construction and general performance of a novel potentiometric membrane sensor for determination of atropine has been developed. It is based on the formation of the ion association complex of the atropinium cation with phosphotungstate counter anion as electroactive material dispersed in a PVC matrix, β‐Cyclodextrin and o‐nitrophenyl octyl ether serve as a plasticizer. The sensor shows a fast, stable, near Nernstian response for 1×10^?2 M to 1×10^?6 M atropine at 25°C over the pH range of 3–8 with a cationic slope of 51±0.5 mV/decade. The lower detection limit is 8×10^?7 M and the response time is 20–45 sec. Selectivity coefficients of atropine, relative to a number of interfering substances, were investigated. There are negligible interferences caused by most of the studied cations, anions, and pharmaceutical excipients. The direct determination of atropine shows an average recovery of 98.6% and a mean relative standard deviation (RSD) of 1.6% at 100 µg/mL. The results obtained by determination of atropine in some formulations (atropine injection and eye drops) are favorably comparable with those obtained by the British Pharmacopoeia method. The developed membrane electrode has been used as end point indicator electrode for some potentiometric titrations.     

适用于光电跟踪初始目标区域的估计方法

在光电跟踪中，由于噪声对非对称目标比较敏感，传统质心算法定位效果不好，而宏像素划分算法具有较好的抗噪声能力，但计算量太大。采用宏像素法来估计初始目标区域减少了计算量。对目标占4×4 pixel左右，大小为128×128 pixel的非对称光斑图像，选择宏像素大小为36 pixel，目标宏像素扩大2个像素区域，可在较少的运算时间、较好的抗噪声能力间达到最佳化。在SNR为5 dB时，r值达到1。动态图像模拟表明，改进算法处理速度可达18~20 frame/s。     

A convenient and rapid sample repositioning approach for atomic force microscopy

A novel repositioning approach is described for repeated observations of a specimen at a close proximal location in the atomic force microscope. The approach is similar to keystone architecture, whereby the repositioning is achieved by forming a male structured base for the specimen, and a corresponding female counterpart as the frame. For the combination of an acrylic acid frame and a metal base, 90% translation shifts are less than 10 µm, and almost all angular disorientations are within +3° to ?3°. Nanometre‐scale surface features can be relocated easily and reliably even after 40 imaging–removal–imaging cycles, dipping the specimen in solutions or heating up to 500 °C.     

Microstructuring of optical surfaces: Technology and device for direct laser writing of diffractive structures

Results of development and testing of a scanning system of interference lithography are presented. The system is designed to form diffractive microstructures consisting of microgratings with a specified orientation, a size of 5–10 µm, and a period ranging from 0.6 to 1.5 µm. The total writing field of the system is 300 × 300 mm. The system is used to study direct laser writing of microgratings on chromium and amorphous silicon films applied by the method of magnetron sputtering onto the glass substrate surfaces. The device and technology of direct writing of microgratings can be further used to form antireflective subwave coatings of optical elements and graphical microstructured identification marks for product protection and also to manufacture diffractive attenuators of laser radiation.     

双视场无盲点全景成像仪

折返式全景成像技术作为一种新型的成像技术是光学设计领域近十几年的研究热点,但该技术有一个重大缺陷——在镜头的正前方存在观测盲区。本文设计了一种拥有双观测模式的新型全景成像仪。相比于传统的折返式全景成像仪,该仪器可以同时对前向视场360°×(0°~55°)和环形视场360°×(55°~95°)进行观测。其中,前向视场很好地补充了折返式光学系统的中央观测盲区,并增加了CCD探测器的面积利用率。该成像仪光学系统由前置透镜组、全景环形透镜和中继转像系统三部分组成。所有的透镜表面均为球面,具有易加工、低成本的特点。最后针对这种光学系统设计了对应的机械结构,从而为以后成像仪的加工、装调服务。该成像仪设计为折返式全景成像技术提供了一个新思路。     

SIMULTANEOUS QUANTITATIVE DETERMINATION OF SEVEN POLYPHENOL CONSTITUENTS FROM HERBA LOPHATHERI BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

The goal of this research was to develop a simple, rapid, and sensitive method for the simultaneous quantitative determination of trans-p-coumaric acid, isoorientin, orientin, swertiajaponin, vitexin, isovitexin, and luteolin-7-O-β-D-glucoside in Herba Lophatheri by high performance liquid chromatographic (HPLC) with photodiode array detection (PAD). The chromatographic separation was performed on a C18 column (4.6 mm × 250 mm, 5 µm), with a gradient elution program using the mixture of acetonitrile and 1.0% acetic acid (v/v) as mobile phase. The seven components of the standards achieved baseline separation. Regression analysis revealed a linear relationship between the contents and the peak areas of the mixed standard substances. The average recovery rates were 98.11%～100.23%, and RSD values were less than 5.0%. In summary, a reliable HPLC method for simultaneous determination of the seven compounds in Herba Lophatheri was developed, and provided a scientific basis for the quality control of herbal medicine.     

Evaluation of surface topography changes in three NiTi file systems using rotary and reciprocal motion: An atomic force microscopy study

Aim: To evaluate the surface topography changes in three nickel‐titanium (NiTi) file systems using either rotary or reciprocal motion using atomic force microscopy (AFM), and to determine the effect of scanning area on the AFM results in this study. Methodology: Five points on a F2 Protaper file, R25 Reciproc file, and a Primary file from WaveOne systems were scanned preoperatively in 1 × 1 and 5 × 5 µm² with an AFM device that can scan an intact (not sectioned) file. One standardized resin block was used for each instrument, according to the manufacturer's recommendations. Points were re‐scanned postoperatively using the same AFM and settings. Root‐mean‐square (RMS) and roughness average (Ra) values were obtained. The preoperative and postoperative surface topographies were compared separately in terms of RMS and Ra values. The surface topography change scores were analyzed using Kruskal–Wallis and Mann–Whitney U tests using a 0.10 significance level. Results: There were no significant differences preoperatively among the NiTi file systems in 1 × 1 or 5 × 5 µm² areas. Postoperatively, the WaveOne Primary had more surface irregularities (significant for 5 × 5 µm² scan in Ra evaluation). Conclusions: Three‐dimensional AFM images of instrument surfaces showed topographic irregularities preoperatively and postoperatively. AFM results differ depending on the scanning area and file used. Microsc. Res. Tech. 77:177–182, 2014. © 2013 Wiley Periodicals, Inc.     

A Shielded 800-kV Pulse Generator at an Energy of 32 kJ

The electric circuit, design, and characteristics of a shielded oil-insulated Marx pulse-voltage generator (PVG) with a stored energy of 32 kJ and an output voltage of 800 kV are described. The PVG charges a water-insulated forming line of the STRAUS-R accelerator of a pulsed electron beam to 700 kV within a time of <1 μs. Two И ЭПM-100-0.4 УXЛ 4 capacitors are installed in each of its eight stages. The switches of the three first stages are 100-kV trigatrons filled with a 40% SF₆ + 60% N₂ gaseous mixture to a pressure of 0.7 MPa. The switches of the other stages are two-electrode spark gaps. The PVG-operation delay time is 108 ± 5 ns at a breakdown-strength margin of each spark gap of ∼80%. The PVG-circuit inductance is ∼1.4 μH. The overall dimensions of the PVG's steel tank are 2400 × 800 × 800 mm (without an output device); the PVG mass is 1700 kg. __________ Translated from Pribory i Tekhnika Eksperimenta, No. 6, 2005, pp. 21–27. Original Russian Text Copyright ? 2005 by Gerasimov, Gordeev, Kul'gavchuk, Myskov, Nazarenko, Pavlov, Sofronova, Suvorov, Shejnov.     

INHIBITIVE KINETIC SPECTROPHOTOMETRIC DETERMINATION OF PROTEIN

A novel inhibitive kinetic spectrophotometric method for the determination of protein is proposed based on the principle that serum albumin (SA) has an inhibitive effect on the oxidation discoloring of p-acetylchlorophosphonazo (CPApA) by potassium periodate in the medium of 4.0 × 10^?4 mol/L H₂SO₄ at 100°C. The maximum absorption peak of SA – CPApA – KIO₄ system is located at 550 nm. The absorbance difference (ΔA) is linearly related with the concentration of SA over the range of 0.80–7.50 µg/mL at the wavelength and fitted the equation: ΔA = 0.064C (C: µg/mL) – 0.0173, with a correlation coefficient γ = 0.9973. The detection limit of the method was 0.30 μg/mL. The method was successfully used to determine protein content in milk and milk powder samples and the determined results were in good agreement with those of tribromoarsenazo spectrophotometry. The relative standard deviation for 13 replicate determinations of the method was 3.64–3.76%. The standard addition recovery of the method was 99.50–101.6%.     

DETERMINATION OF CINACALCET HYDROCHLORIDE BY CAPILLARY ELECTROPHORESIS WITH PHOTODIODE ARRAY DETECTION

This article reports a validated stability-indicating capillary electrophoresis method using a photodiode array detector at 220 nm for the determination of cinacalcet hydrochloride. The best electrophoretic separation between the analyte and internal standard (lamotrigine) was achieved within 5 min in a deactivated fused silica capillary (55 cm effective length × 75 µm internal diameter) maintained at 24°C using a background electrolyte solution consisted of phosphate buffer (50 mM, pH 6.4):methanol (95:5, v/v) at a separation voltage of 30 kV. The linear range of the method was 0.5–30 µg/mL (r = 0.9999) with limits of detection and quantitation of 0.1 and 0.5 µg/mL, respectively. The assay precision and accuracy were favorable as the relative standard deviations did not exceed 1.09%, and the recovery values were 98.99–100.33 ± 0.19–1.09%. The induced degradation products, when any, did not interfere with the detection of analyte. The proposed method was successfully applied for the determination of cinacalcet hydrochloride in bulk and pharmaceutical formulations; the percentage recovery values were 98.16–102.00 ± 0.24–1.08%. The results demonstrated the value of the method.     

Simultaneous Determination of Six Trace Elements in Plant Medicines by Derivative Adsorption Waves in Conjunction with a Microwave Technique

Abstract

Complex adsorption waves of Cu(II), Pb(II), Cd(II), Ni(II), Co(II), and Zn(II) in substrate solution (pH=9.26) of diacetyldioxime‐ammonia‐ammonium chloride‐sodium citrate‐gelatin‐sodium sulfite were studied and a new method for determination of the six trace elements in aqueous solutions was developed. The results show that there are sensitive adsorption waves of Cu(II), Pb(II), Cd(II), Ni(II), Co(II), and Zn(II) complexes at about ?0.45, ?0.61,?0.78, ?1.07, ?1.23, and ?1.38 V, respectively. The method is easy to operate and is able to determine these trace elements in aqueous solutions rapidly and simultaneously. When the signal‐to‐noise ratio equals 3, the detection limits of copper, lead, cadmium, nickel, cobalt, and zinc are 3.2×10^?4, 4.8×10^?3, 1.9×10^?3, 1.7×10^?5, 2.1×10^?6, and 1.0×10^?3 µg/cm³. Good linear relationships exist between the concentrations and the current peaks when copper, lead, cadmium, nickel, cobalt, and zinc concentrations are within 6.5×10^?4～10⁰, 9.3×10^?3～10, 4.1×10^?3～10, 3.2×10^?5～10^?1, 4.0×10^?6～10^?2, and 2.1×10^?3～10 µg/cm³, respectively. In conjunction with a microwave assimilation technique, the method has been used in the rapid and simultaneous determination of these trace elements in some plant medicines with satisfactory results.     

Three-colour x-ray mapping using digital storage

Computer-controlled scanning of a scanning electron microscope (SEM) fitted with an energy-dispersive x-ray analyser has been carried out. This has been achieved by building an SEM interface module which controls the scanning of the electron beam and also provides a communication link between the x-ray analyser and an enhanced BBC micro. The digitised x-ray data pulses can be collected from three elements simultaneously to produce colour-coded x-ray distribution maps. Some such maps from two different specimens are presented and an effect of x-ray shadowing is clearly demonstrated. A comparison between images acquired using a frame size with 256 × 256 pixels and those with 128 × 128 pixels is made.     

Effect on Particle Size to Emitted X-Ray Intensity in Pellet Cement Sample Analyzed with WDXRF Spectrometer

Abstract

The particle size and heterogeneity effects on the analyte line were investigated for the analysis of powdered samples by X-ray fluorescence technique. In the analysis of samples utilizing the powder method, these effects caused serious errors with variations in particle size for the emitted intensity. The fluorescence intensities of some elements in pellet samples of cement (the range of particle sizes, < 32 µm, 32–38 µm, 38–45 µm, 45–63 µm, 45–75 µm, 75–106 µm, and 106–150 µm and, at press pressure 3.50 and 1.41 × 10⁷ kg/m²), are measured using a wavelength dispersive X-ray fluorescence (WDXRF) spectrometer for 14 pellets prepared according to the powder method. The results show that the K _α X-ray fluorescence intensities from samples can effect about 17% maximum differences in normalized intensities within selected particle sizes. These experimental results were interpreted by comparing with the other experimental results in the literature.     

Novel determination of caffeine in human urine by direct analysis in real time mass spectrometry

Determination of caffeine is necessary for clinical research. A new method for the determination of caffeine in human urine was established by direct analysis in real time mass spectrometry using multiple reaction monitoring. The m/z 195.1 to 138.1 amu transition was employed in positive ionization mode. The preparation and analysis conditions were systemically optimized. The calibration curve was linear from 0.5–50 µg/mL with a limit of detection limit of 0.2 µg/mL. Intra-day and inter-day accuracy and precision were within the acceptable limits of ±15% at all concentrations. Moreover, the matrix effects for the determination of caffeine were evaluated. In conclusion, a simple, rapid, and reliable method without complex sample preparation and chromatographic separation was developed and validated for the determination of caffeine in human urine.     

Toxicity assessment of nano‐TiO2 in Apis mellifera L., 1758: histological and immunohistochemical assays

The aim of this study was to evaluate the toxicity of titanium dioxide nanoparticles (TiO₂NPs) by short‐term toxicity tests in Apis mellifera, considered an excellent bioindicator organism mainly due to its sensitivity. Bees have been exposed to several concentrations of TiO₂NPs (1 × 10^?3, 1 × 10^?4, 1 × 10^?5, 1 × 10^?6 mg/10 ml) for 10 days. Morphostructural and histological assays were done on gut and honey sac. The research of exposure biomarkers like metallothioneins 1 (MT1) and Heat Shock Protein 70 (HSP70) was performed to verify if a detoxification mechanism has been activated in the exposed animals. No histological alteration on the epithelium of the gut and honey sac were observed in exposed samples. A significant positivity for anti‐MT1 antibody was observed only in the honey sac cells. A weak positivity for HSP70 was observed in both structures analyzed. In several studies have shown the non‐toxicity of TiO₂NPs on other model organisms, in our study, titanium dioxide nanoparticles was proven to be highly toxic at the highest concentration tested (100% of lethality to 1 × 10^?3 mg/10 ml) and moderately toxic at lower concentrations. Honey bees proved to be excellent models for study of NPs toxicity and for monitoring environment.