A new experimental procedure to obtain titania powders as anatase phase by a sol-gel process

Titania powders were synthesized by a sol-gel process using titanium tetrabutoxide as precursor. The syntheses were performed in water or in solutions of dimethylformamide (dmf) or dimethylsulfoxide (dmso). It is demonstrated, by X-ray diffraction patterns of the synthesized powders, that the samples obtained in dmf or dmso solutions are crystalline (anatase phase) with some minor amount of brookite phase, whereas the sample synthesized in water is amorphous. The anatase phase can be obtained independently of any previous or further treatment of the synthesized powder, such as hydrothermal or heat treatment, providing a new, simple, quick and inexpensive route to synthesize anatase powders. From the peak broadening of the anatase (101) diffraction, the crystallite sizes were calculated as 6 nm.

A simplified procedure for determination of clofentezine residues in fruits by liquid chromatography with UV detection

A rapid and sensitive method is described for the determination of clofentezine residues in apple, papaya, mango and orange. The procedure is based on the extraction of the sample with a hexane:ethyl acetate mixture (1:1, v/v) and liquid chromatographic analysis using UV detection. Mean recoveries from 4 replicates of fortified fruit samples ranged from 81% to 96%, with coefficients of variation from 8.9% to 12.5%. The detection and quantification limits of the method were of 0.05 and 0.1 mg kg-1, respectively.

Henkilöstöresurssien hallintatyökalun vaatimukset asiantuntijaorganisaatiossa

Yrityksen organisaatiomallin pitää palvella tehokasta toimintaa. Tällä hetkellä tässä yrityksessä resurssipooleihin perustuva organisaatio on katsottu sopivaksi. Sen toivotaan mahdollistavan henkilöstöresurssien tehokas hyödyntäminen. Organisaation muutos vaatii myös toimintatapojen ja joissain tapauksissa tietojärjestelmien muutosta. Tässä tapauksessa siirtyminen uudenlaiseen organisaatioon loi tarpeen uudelle resurssien varaus- ja etsintätoiminnolle ja sitä tukeville tietovarastoille. Vaatimusmäärityksen tuloksena voidaan todeta, että nykyinen ERP-ohjelmisto ei ole paras mahdollinen yrityksen käyttöön, vaikka senkin kanssa yritys kyllä tulee toimeen. Tärkeimpinä vaatimuksina hyvälle hallintasovellukselle voidaan pitää mahdollisuutta seurata työntekijöiden osaamisen ja tietämyksen kehitystä sekä arvioida niiden tasoa, mahdollisuutta varata niin henkilöitä kuin osaamisia ja tehokasta ja muunneltavaa mekanismia henkilöiden valintaan projekteihin. Nykyisessä toteutuksessa henkilöstön osaamisten käsittely on hiukan rajoittunutta eikä mitään historiatietoja tallenneta tai käytetä hyödyksi missään vaiheessa. Myös resurssien haku projekteihin olisi mahdollista toteuttaa paremmin. Hakuihin pitäisi saada lisää hakuehtoja ja mahdollistaa yleisluontoisemmat ehdot yksityiskohtien sijaan, vaikka tiedot olisivatkin tarkemmalla tasolla. Näistä syistä uuden työkalun rakentamista henkilöstöresurssien paremman hyödyntämisen takaamiseksi voidaan pitää perusteltuna.

An expeditious and consistent procedure for tetrahydrofuran (THF) drying and deoxygenation by the still apparatus

Despite the availability of alternative methods for drying tetrahydrofuran (THF), the use of the still apparatus, wherein a THF solution containing Na-bezophenone ketyl is heated to reflux, remains widespread. We herein propose a set of procedures to solve the problems usually faced in applying this drying technique. Moreover, a discussion is made on the chemical knowledge underlying such procedures. Safety and economy issues concerned with the operation of the THF still apparatus are also discussed.

Photometric procedure for quantitative analysis of Aflatoxin B1 in peanuts by thin-layer chromatography using charge coupled device detector

A photometric procedure was developed for determination of aflatoxin B1 in peanuts by TLC-CCD technique. The quantification and detection limit were 1.2 μg kg-1 and 0.4 ng per spot, respectively, with mean recovery of 98%. The CCD camera is sufficiently sensitive to detect small changes in spots fluorescence intensity and the results for performance confirmed the efficiency of the method. Another important property of CCD detector is its linearity for a wide range of luminous stimulus determined by analysis of five-point calibration curves using the intensity of AFB1 fluorescence versus AFB1 concentration (0.8 to 4.8 ng per spot). The method was applied to the analysis of thirty nine peanut samples and aflatoxin B1 levels ranged from 16 to 115 μg kg-1. The TLC-CCD and the photometric procedure developed in this study demonstrated to be a simple and efficient tool for quantitative analyses of AFB1 in peanut samples.

MSPD procedure combined with GC-MS for the determination of procymidone, bifenthrin, malathion and pirimicarb in honey

A method based on matrix solid-phase dispersion and gas chromatography-mass spectrometry to determine procymidone, malathion, bifenthrin and pirimicarb in honey is described. The best results were obtained using 1.0 g of honey, 1.0 g of silica-gel as dispersant sorbent and acetonitrile as eluting solvent. The method was validated by fortified honey samples at three concentration levels (0.2, 0.5 to 1.0 mg kg-1). Average recoveries (n=7) ranged from 54 to 84%, with relative standard deviations between 3.7 and 8.5%. Detection and quantification limits attained by the developed method ranged from 0.02 to 0.08 mg kg-1 and 0.07 to 0.25 mg kg-1 for the honey, respectively.

Optimization of a HPLC procedure for simultaneous determination of cisplatin and the complex cis,cis,trans-diamminedichlorodihydroxoplatinum(IV) in aqueous solutions

A RP-HPLC procedure for the simultaneous determination of cisplatin and the complex cis,cis,trans-diamminedichlorodihydroxo-platinum(IV), was development. The developed procedure was validated in terms of linearity, accuracy, precision, limits of detection (LOD), limits of quantification (LOQ) and specificity. The limits of detection (LOD) were 0.47 x 10-4 and 0.53 x 10-4 mol L-1 and the limits of quantification (LOQ) were 1.57 x 10-4 and 1.75 x 10-4 mol L-1, for cisplatin and cis,cis,trans-diamminedichlorodihydroxopla-tinum(IV), respectively. The average recoveries of cisplatin and cis,cis,trans-diamminedichlorodihydroxoplatinum(IV) was 100.6% ± 1.4 and 101.2% ± 1.1, respectively. Intermediate (inter-day) precision, repeatability and specificity of the procedure for hydrolysis products of cisplatin were studied. The results of the study showed that the proposed RP-HPLC procedure is simple, rapid, precise, accurate and specific.

EVALUATION OF A BUFFERED SOLID PHASE DISPERSION PROCEDURE ADAPTED FOR PESTICIDE ANALYSES IN THE SOIL MATRIX

An evaluation of the pesticides extracted from the soil matrix was conducted using a citrate-buffered solid phase dispersion sample preparation method (QuEChERS). The identification and quantitation of pesticide compounds was performed using gas chromatography-mass spectrometry. Because of the occurrence of the matrix effect in 87% of the analyzed pesticides, the quantification was performed using matrix-matched calibration. The method's quantification limits were between 0.01 and 0.5 mg kg-1. Repeatability and intermediate precision, expressed as a relative standard deviation percentage, were less than 20%. The recoveries in general ranged between 62% and 99%, with a relative standard deviation < 20%. All the responses were linear, with a correlation coefficient (r) ≥0.99.

Characteristics of pyridine adsorption on Au(111) and Au(210) by EIS parameters fitting procedure

Some aspects of the application of electrochemical impedance spectroscopy to studies of solid electrode / solution interface, in the absence of faradaic processes, are analysed. In order to perform this analysis, gold electrodes with (111) and (210) crystallographic orientations in an aqueous solution containing 10 mmol dm-3 KF, as supporting electrolyte, and a pyridine concentration varying from 0.01 to 4.6 mmol dm-3, were used. The experimental data was analysed by using EQUIVCRT software, which utilises non-linear least squares routines, attributing to the solid electrode / solution interface behaviour described by an equivalent circuit with a resistance in series with a constant phase element. The results of this fitting procedure were analysed by the dependence on the electrode potential on two parameters: the pre-exponential factor, Y0, and the exponent n f, related with the phase angle shift. By this analysis it was possible to observe that the pyridine adsorption is strongly affected by the crystallographic orientation of the electrode surface and that the extent of deviation from ideal capacitive behaviour is mainly of interfacial origin.

Determination of hydroquinone in a square wave voltammetry procedure using a graphite-polyurethane composite electrode

In order to a better characterization of a graphite-polyurethane composite intended to be used as a voltammetric sensor, the performance in a square wave voltammetric procedure was investigated. Using hydroquinone (HQ) as a probe, the electrode showed to be useful in square wave voltammetry with limit of detection of 0.28 µmol L-1, with recoveries between 99.1 and 101.5%. The results of the proposed method agreed with HPLC ones within 95% confidence level.

Spectrophotometric flow injection procedure to indirect determination of paracetamol in pharmaceutical formulations using o-tolidine as reagent

A spectrophotometric flow injection method for the determination of paracetamol in pharmaceutical formulations is proposed. The procedure was based on the oxidation of paracetamol by sodium hypochloride and the determination of the excess of this oxidant using o-tolidine dichloride as chromogenic reagent at 430 nm. The analytical curve was linear in the paracetamol concentration range from 8.50 x 10-6 to 2.51 x 10-4 mol L-1 with a detection limit of 5.0 x 10-6 mol L-1. The relative standard deviation was smaller than 1.2% for 1.20 x 10-4 mol L-1 paracetamol solution (n = 10). The results obtained for paracetamol in pharmaceutical formulations using the proposed flow injection method and those obtained using a USP Pharmacopoeia method are in agreement at the 95% confidence level.

Quality of beans stored under hermetic conditions

This study aimed to evaluate the quality of beans (Phaseolus vulgaris L.) stored with different moisture contents under hermetic conditions. Beans with 12.3%, 15.7%, and 17.8% moisture content were used in the experiment. They were packed in bag type silos (3 kg), PET bottles (1.5 L), and glass containers (3 L), covered with organza fabric (control), and stored at 25 ºC and 70±5% relative humidity, for 120 days. The evaluated characteristics included moisture content, apparent density, electrical conductivity, germination percentage, cooking time, and bean classification, every 30 days. Except for the electrical conductivity and cooking time, the other characteristics were kept for 120 days in the stored product with moisture contents of 12.3% and 15.7% in hermetic conditions. Beans with 17.8% of the moisture content, electrical conductivity and cooking time increased, and apparent density and germination were reduced. Beans stored in the control, with any of the moisture contents, showed high quality loss during the long storage. It was concluded that it is possible to storage beans with moisture contents of 12.3% and 15.7%, with quality, for until 120 days, in hermetic conditions.

Development of a project control procedure

The aim of this study is to develop a suitable project control procedure for a target company that can be used in engineering, procurement, and construction or con-struction management contracts. This procedure contains suitable project control software and a model for the use of the software in practice. This study is divided into two main sections. Theoretical part deals with project management, focusing on cost and time dimensions in projects. Empirical part deals with the development of the project control procedure for the target compa-ny. This development takes place in two parts. In the first part, semi-structured interviews are used to find out the company’s employees’ demands and desires for the project control software which will then be used in the developed procedure. These demands and desires are compared to available software in the market and the most suitable one will be chosen. Interview results show that important factors are cost tracking, integration with other software, English language availability, references, helpdesk, and no need for regular updates. The most suitable one is CMPro5 cost control software. The chosen software is used in a pilot project, where its functions and use are analyzed. Project control procedure which will be used in the future is developed based on these procedures. The five steps in developed procedure include employment of a cost engineer, whose task is to maintain the procedure in the target company.