Selective Determination of Verapamil in Pharmaceutics and Urine Using a Boron‐doped Diamond Electrode Coupled to Flow Injection Analysis with Multiple‐pulse Amperometric Detection

This work presents a simple and low‐cost method for fast and selective determination of Verapamil (VP) in tablets and human urine samples using a boron‐doped diamond working electrode (BDD) coupled to a flow injection analysis system with multiple pulse amperometric detection (FIA‐MPA). The electrochemical behaviour of VP in 0.1 mol L⁻¹ sulfuric acid showed three merged oxidation peaks at around +1.4 V and upon reverse scan, one reduction peak at 0.0 V (vs. Ag/AgCl). The MPA detection was performed applying a sequence of three potential pulses on BDD electrode: (1) at +1.6 V for VP oxidation, (2) at +0.2 V for reduction of the oxidized product and (3) at +0.1 V for cleaning of the working electrode surface. The FIA system was optimized with injection volume of 150 μL and flow rate of 3.5 mL min⁻¹. The method showed a linear range from 0.8 to 40.0 μmol L⁻¹ (R>0.99) with a low limit of detection of 0.16 μmol L⁻¹, good repeatability (RSD<2.2 %; n=10) and sample throughput (45 h⁻¹). Selective determination of VP in urine was performed at+0.2 V due to absence of interference from ascorbic and uric acids in this potential. The addition‐recovery tests in both samples were close to 100 % and the results were similar to an official method.     

气相色谱法测定榄香烯水针剂中有效成分含量

建立了测定榄香烯水针剂的有效成分含量的气相色谱方法,解决了多次进样造成对色谱柱和检测器的污染以及色谱柱效下降的问题,方法操作,灵敏度高,重现性好,相关系数为0．9999,相对标准偏差为0．41％。     

Comparison of analytical methods for ozone precursors using adsorption tube and canister

Recently, ozone concentrations have increased dramatically as a result of vehicle usage in metropolitan areas. Ozone precursors are composed of hydrocarbons of organic compounds. Because hydrocarbons are indicative of ozone formation, they need to be monitored in ambient air. Since ozone precursor are present at very low levels (from ppb to ppt) in ambient air, they are difficult to analyze accurately. This study investigates ozone precursors in ambient air. The main purpose of this study is to compare analytical methods for the measurement of ozone precursors in atmosphere. Two measurement methods were evaluated using canister (Silco-canister) and adsorbent (300-mg Carbopack B+150-mg Carbosieve SIII) tube. Differences in measurements for total ozone precursor emissions were 54.1% between the adsorption tube and canister-GC/MS, 51.1% between adsorption tube and canister-GC/FID, and 16.3% between canister-GC/MS and canister-GC/FID.     

Thermal behaviour of amorphous Li2ZrO3 prepared by sol-gel technique

The results of the investigations of thermal behaviour of Li₂ZrO₃, prepared in the amorphous state by means of sol-gel technique are demonstrated. The thermal treatment was carried out in air under constant heating rate of 5 deg·min^–1 and cooling rate of 2.5 deg·min^–1. The methods of DTA, TG, Emanation Thermal Analysis (ETA) and dilatometry were used, for characterization of the thermal behaviour in dynamic conditions. The X-ray diffraction patterns were used for characterization of the phase changes observed by TA Methods.

---

Zusammenfassung Ergebnisse aus Untersuchungen des thermischen Verhaltens von Li₂ZrO₃, hergestellt mittels einer Sol-Gel-Technik im amorphen Zustand werden dargelegt. Die thermische Behandlung wurde in Luft bei einer konstanten Aufheizgeschwindigkeit von 5 Grad·min^–1 und einer Abkühlgeschwindigkeit von 2,5Grad·min^–1 durchgeführt. Zur Beschreibung des thermischen Verhaltens unter dynamischen Verhältnissen wurden DTA, TG, Emanationsthermoanalyse und Dilatometrie angewendet. Zur näheren Charakterisierung der bei TG beobachteten Phasenumwandlungen wurde Röntgendiffraktion verwendet.

     

Preparation,purification, and analysis of alkylated cyclodextrins

Methods of alkylation of α-, β- and γ-cyclodextrins have been optimized with regard to the parameters of reaction, degree of alkylation and yields. The analysis of the reaction mixtures and of the isolated single species has been performed by high temperature GC and HPLC. The phase systems of the preferably applied HPLC have been carefully adjusted by variation of both the stationary and mobile phases to the very different hydrophobicities of the various alkylated CD species which have been synthesized. Several partially or fully alkylated CD species were isolated from preparative scale HPLC separations in high purity.     

可拆分有调整时间的平行机排序问题的一个算法

考虑有独立调整时间的同型号平行机排序问题,极小化最迟完工时间,产品允许拆分,同一产品被拆分后各部分可以在不同机器上同时加工,该问题是ＮＰ－ｈａｒｄ问题。本文首先给出该问题的一个启发式算法ＭＬ,然后证明了其最坏情况估计不超过７／４－１／ｍ（ｍ≥２）。     

流动注射-电感耦合等离子体发射光谱法测定天然水中的钙和镁

本文采用流动注射－电感耦合等离子体发现光谱联用技术测定了天然水中的钙、镁元素。考察了试液的雾化和曝光时间及载气压力等因素对分析信号的影响。通过与气动连续进样的对比，测出了钙、镁在流动注射进样下的分散系数。本法在测定钙、镁含量高的水性时，不需对试样进行稀释处理。对五个水样中钙、镁的分析结果与EDTA络合滴定法相吻合。     

Effective Hamiltonian approach to doubly degenerate electronic states

Effective vibronic Hamiltonian models are built for E ⊗e Jahn-Teller systems and analytical solutions are obtained through Lie algebraic methods. Although approximate, we show that these models allow in particular to recover the possible ground state crossover when quadratic couplings are present. The equivalence of E ⊗e and G' ⊗e vibronic systems in cubic symmetry is precisely established through a particular realization of the electronic operators for an orbital quadruplet. We show how this equivalence is broken by a rovibronic interaction which, for a G' ⊗e system, still gives an exactly solvable model.     

Total analysis of surface structure and properties by UHV transfer system

We have developed an ultrahigh-vacuum (UHV) complex sample preparation and analysis system, which realizes a reliable surface science analyzing various characters on an identical surface. The system contains three sample-preparation-and-characterization chambers and five analysis chambers. They are (1) an electronic-properties-characterization chamber, (2) a magnetic-properties-characterization chamber, (3) an organic-molecule chamber, (4) UHV SEM, (5) a high-energy-resolution angle-resolved photoelectron spectrometer, (6) a high-energy-resolution display-type spherical mirror analyzer, (7) a room-temperature (RT) STM, and (8) an optical-properties characterization chamber. A special sample holder is used with six electrodes on it, which enables accurate temperature measurement of a sample by connecting a thermocouple directly to the sample even if it is transferred. Four other electrodes can be used for construction of various circuits including evaporators. Some examples are shown.     

Analysis of signal fluctuations of Cortical Spreading Depression: Preliminary findings

In this work, we apply Detrended Fluctuation Analysis (DFA) to study the dynamics of electrical cortical activity in rats during the phenomenon of Cortical Spreading Depression (CSD), as well as the periods before and after this phenomenon. The characteristic of CSD is reduced electrical activity that occurs and spreads in the cerebral cortex after the application of electrical, chemical or mechanical stimulus. Our results show that the electrocorticogram signal shows long range temporal correlations and scaling behavior, except during the pre-CSD burst phase (significant increase of amplitude provoked by stimulus).