Possibilidades e limitações no uso da temperatura em cromatografia líquida de fase reversa

High-temperature liquid chromatography (HTLC) is a technique that presents a series of advantages in liquid phase separations, such as: reduced analysis time, reduced pressure drop, reduced asymmetry factors, modified retentions, controlled selectivities, better efficiencies and improved detectivities, as well as permitting green chromatography. The practical limitations that relate to instrumentation and to stationary phase instability are being resolved and this technique is now ready to be applied for routine determinations.

Cromatografia gasosa ultrarrápida: uma visão geral sobre parâmetros, instrumentação e aplicações

Since the introduction of GC there has been an ongoing interest in reducing time of analysis resulting in new terms and definitions such as ultra fast gas chromatography (UF-GC). One of the most used definitions describes UF-GC as a technique that combines the employment of short narrow bore column with very fast temperature programming rates producing chromatographic peaks in the range of 50 ms and allowing separations times in 1-2 min or less. This paper summarizes the analytical approaches, the main parameters involved and the instrumentation towards UF-GC.

Construção de espectrômetro de emissão atômica com atomização eletrotérmica em filamento de tungstênio (WCAES)

It is here discussed the development of a low cost analytical instrument with capacity for metals determination using atomic emission measurements in an electrothermal atomization system with a tungsten coil atomizer. The main goal was to show a new frontier for using this atomizer and to demonstrate that the simple instrumental arrangement here proposed has potential for portability and for solving analytical tasks related to metals determination. Atomic emission of calcium was selected for the adjustment of instrumental parameters and to evaluate the main characteristics of the lab-built instrument. Cobalt was determined in medicines and one alloy to demonstrate its feasibility.

Análise por injeção em fluxo com detecção amperométrica de múltiplos pulsos: potencialidades e aplicações

The potentialities and applications of the Multiple Pulse Amperometric detection (MPA) coupled with Flow Injection Analysis (FIA) are evaluated. Important aspects as cleaning and activation of electrode surface, indirect and simultaneous analysis of electroactive compounds and the use of the internal standard method for quantifications utilizing FIA-MPA are presented. The main parameters concerning the detection of electroactive analytes by multiple pulse amperometric detection in flowing solutions were also discussed. In addition, aspects such as flow rate, sample volume, application time of the potential pulses and instrumentation necessary for implementing of the method were also addressed.

Ozonólise: a busca por um mecanismo

The ozonolysis reaction is widely used in the academy and in industry. The first reports about the existence of the ozone molecule were made over 200 years ago. Several ideas and assumptions were made to understand the chemical properties of the ozone molecule and the ozonolysis mechanism. The intent of this paper is not to be an extensive review about ozone chemistry or ozonolysis reactions, but to highlight how the rational process was developed and how conclusions were drawn at a time with limited instrumentation.

Avaliação de dispositivos de captura de imagens digitais para detecção colorimétrica em microzonas impressas

This report describes a study about the feasibility of using a conventional digital camera, a cell-phone camera, an optical microscope, and a scanner as digital image capture devices on printed microzones. An array containing nine circular zones was drawn using graphics software and printed onto transparency film by a laser printer. Due to its superior analytical performance, the scanner was chosen for the quantitative determination of Fe2+ in pharmaceutical samples. The data achieved using scanned images did not differ statistically from those attained by the reference spectrophotometric method at the confidence level of 0.05.

O Estado da arte da cromatografia líquida bidimensional: conceitos fundamentais, instrumentação e aplicações

The constant evolution of science and the growing demand for new technologies have led to new techniques in instrumentation that can improve detection, separation, resolution, and peak capacity. Comprehensive two-dimensional liquid chromatography (LC×LC) is presented as a powerful tool in complex sample analyses. During an analysis, a sample is subjected to two independent separation mechanisms that are combined, resulting in increased resolving power. For appropriate application of LC×LC, understanding the influence of parameters that require optimization is necessary. The main purpose of optimization is to predict the combination of stationary phases, separation conditions, and instrumental requirements to obtain the best separation performance. This review discusses theoretical, intrumental, and chemometric aspects of LC×LC and focuses on its applications in foods. It aims to provide a clear understanding of the aspects that can be used as strategies in the optimization of this analytical method.

KIT COLORIMÉTRICO PARA DETECÇÃO DE METANOL EM ETANOL COMBUSTÍVEL PARA O MONITORAMENTO DA QUALIDADE DE COMBUSTÍVEIS

A colorimetric kit for methanol detection in ethanol-containing fuels and ease of use in the field was developed and tested. The analysis can detect the presence of methanol in fuels when exceeding specification (0.5% v/v) in about 20 min and its simple instrumentation does not require a specialist. The kit method was successfully validated at gas stations located in São Paulo State and the Federal District.

SMB-laitteiston suunnittelu hydrometallurgisiin sovelluksiin

Työn tarkoituksena oli suunnitella, ohjelmoida ja koekäyttää SMB-laitteisto (Simulated Moving Bed) hydrometallurgisiin erotuksiin. Simuloitu liikkuvapeti saadaan aikaan vaihtamalla sisään- ja ulostuloporttien paikkaa nestevirran suuntaan. Tällöin aikaansaadaan kiintoaineen vastavirtaus minkä johdosta erotustehokkuus kasvaa. Komponenttien retentiotaipumuseroista johtuen komponentit liikkuvat eri nopeuksilla kolonnijärjestelmässä. Enemmän pidättäytyvät komponentit liikkuvat nestevirtaa vastaan ja vähemmän pidättäytyvät komponentit nestevirran mukana. Hydrometallurgiassa vastavirtauksen käyttöä ei ole tieteellisissä julkaisuissa käsitelty laajalti ja saatavilla oleva informaatio onkin kaupallisten yritysten tuottamaa. Hydrometallurgiassa vastavirtausta käyttävissä ioninvaihtolaitteistoissa hyödynnetään irrallisia regenerointivyöhykkeitä. Venttiilijärjestelmän osalta päädyttiin ratkaisuun jossa käytetään yhtä kiertoventtiiliä kullekin virralle, minkä lisäksi kolonnien väleillä käytetään solenoidiventtiiliä. Tämä järjestelmä mahdollistaa yleisimpien SMB-menetelmien käytön mukaan lukien irralliset vyöhykkeet. Laitteiston ohjauksesta vastaa LabVIEW 2010:llä ohjelmoitu ohjelmisto, joka sisältää kaikkien tarvittavien laitteiden ohjausrutiinit. Se mahdollistaa venttiilien synkroniset ja epäsynkroniset vaihdot. Laitteiston puhdistusta varten on ohjelmistoon rakennettu oma rutiini venttiilejä varten. Pumppujen osalta ohjelmisto mahdollistaa vakiovirtauksen sekä lineaaristen ja porrasmuotoisten gradienttien käytön. Ongelmatilanteita varten ohjelmisto valvoo pumppujen ja venttiilien toimintaa ja pysäyttää laitteiston tarvittaessa. Koekäytön avulla pystyttiin todentamaan laitteiston toimivuus.

Musikalisk lärandemiljö : planerade musikaktiviteter med småbarn i daghem

A musically stimulating nvironment is of great significance when considering the opportunities for development and learning that are offered to children in day nurseries. Moreover, the quality of musical activities also has great significance for the musical development of growing children. Young children are always striving to create meaning and understanding; they influence and are influenced by the context in which they are situated. The purpose of this study is to investigate the planned music activities in the musical learning environment of seven toddler’s groups in day nurseries, based on four different aspects: the texts of children’s songs, the melodies of children’s songs, the basic elements of music and the use of instrumentation. The data has been gathered by video observation of the planned music activities. The age of the children studied ranged from 11 months to 3 years and 11 months, and on average there were 13 children in each group. The study involved a total of just over 90 children and nine educators. The methodological approaches are hermeneutic as well as videographic, and they are applied to the analysis as required. The approaches are well suited to an understanding of the planned music activities where the individual’s communications and actions are studied. The results of the study show that educators impart a cultural heritage to the children in the form of old traditional songs, but they also act as intermediaries for newer children's songs. They focus on actively on the text content of the children’s songs in their interaction with the children, but do not address the meaning of the text. Furthermore, while the educators use music sessions for the children to develop, among other things, an understanding of language and social skills, they do not use the sessions to develop the children’s musical skills. The educators could, to a much greater extent than they now do, direct the children's attention to the basic elements of music, and conduct meta-cognitive dialogues with the children. They use a large repertoire of children's songs, which are, however, often too demanding for the children’s voices to cope with. In addition, the educators do not plan, in any significant way, activities for the toddlers in order to help them develop the accuracy of their vocal tones. With regard to the use of instruments, the educators focus, in their interaction with the children, is placed on both the usage of the instruments and knowledge about the instruments. Regarding the use of instruments the study shows that the children’s musical expression takes place in an environment that includes both melody and rhythm instruments. It is clear that children are actively interested in the constructed instrument environment, because for long periods of time they independently play and experiment with instruments.

Electrical Equivalent Circuit for Dry Bacteriorhodopsin Sensor

Bacteriorhodopsin (BR) is a photosensitive protein which functions as a light-driven proton pump. Due to its photoactivity, BR could be used in photosensing and information processing which has inspired researchers to study the photoelectric response and the appropriate measurement instrumentation for BR. In this thesis, the measurement instrumentation connected to a dry BR sensor was confirmed to affect the photovoltage response measured by using voltage amplifiers. Changing of the input impedance of the measurement instrumentation was shown to alter a part of the measured photovoltage response. The photocurrent measurements using transimpedance amplifier and the presented electrical equivalent circuit were used to show that the photocurrent measurements have no significant effect on the photoelectric response. The photocurrent was shown to be a derivate of the photovoltage response measured from the dry BR sensor when it was compared to the response measured with a voltage amplifier. This confirmed that another part of the photovoltage response was not affected by the measurement instrumentation. The time-variant behavior of the dry BR sensor was confirmed in both the photocurrent and the photovoltage measurements. This was caused by the fact that the capacitance of the dry BR sensor changes with the excitation light intensity.

Compton scattering tomography for agricultural measurements

This paper presents a new approach in tomographic instrumentation for agriculture based on Compton scattering, which allows for the simultaneous measurements of density and moisture of soil samples. Compton tomography is a technique that can be used to obtain a spatial map of electronic density of samples. Quantitative results can be obtained by using a reconstruction algorithm that takes into account the absorption of incident and scattered radiation. Results show a coefficient of linear correlation better than 0.81, when comparison is made between soil density measurements based on this method and direct transmission tomography. For soil water contents, a coefficient of linear correlation better than 0.79 was found when compared with measurements obtained by time domain reflectrometry (TDR). In addition, a set of Compton scatter images are presented to illustrate the efficacy of this imaging technique, which makes possible improved spatial variability analysis of pre-established planes.

Reaktorisydämen valvontajärjestelmän modernisointi Olkiluodon kiehutusvesilaitoksella

Reaktorisydämen valvonnalla varmistetaan, että polttoaineelta vaaditut termiset marginaalit toteutuvat ja polttoaineen suojakuori säilyy ehjänä. Olkiluodon kiehutusvesilaitoksen nykyinen sydämen valvontajärjestelmä koostuu SIMULATE-3-sydänsimulaattoriohjelmasta, reaktorisydämen instrumentoinnista, termisen tehon laskentaohjelmasta, tiedonkeruuohjelmista ja käynnistysautomatiikasta. Uusi järjestelmä koostuu näiden lisäksi GARDEL-ohjelmasta, joka on kehitetty kevytvesireaktoreiden sydämen käytön suunnitteluun ja valvontaan. GARDEL käyttää laskentaan samoja ohjelmia, jotka ovat jo Olkiluodon kiehutusvesilaitoksella käytössä. Tämän työn tarkoituksena oli verrata nykyistä ja uutta sydämen valvontajärjestelmää Olkiluodon kiehutusvesilaitoksella. Työssä tutkittiin LPRM-detektorien kalibroinnin jälkeisen datan käsittelyä, palamapäivitystä, stabiilisuuslaskentaa ja adaptiivisia menetelmiä. Järjestelmien vertailuun käytettiin Olkiluoto 2 -laitosyksiköltä käyttöjaksolta 31 (2011–2012) saatuja laskentuloksia. Tulosten perusteella havaittiin uuden järjestelmän laskennassa yksittäisiä virheitä, jotka tulee korjata. Lisäksi uuden järjestelmän toiminnasta tarvitaan lisäselvitystä.

Analogisten erotusvahvistimien nykytilan kartoitus

Erotusvahvistin on instrumentointivahvistin, jonka tulo ja lähtö ovat galvaanisesti erotettu toisistaan. Erotusvahvistimia käytetään galvaanista erotusta vaativissa sovelluksissa, muun muassa sairaalalaitteissa. Teollisuudessa on olemassa sovelluksia, joihin tarvittaisiin analogisia erotusvahvistimia, mutta ei tiedetä onko analogisilla erotusvahvistimilla riittävän hyvät komponenttiarvot. Tässä työssä selvitetään analogisten erotusvahvistimien tämänhetkisiä ominaisuuksia, hintoja ja komponenttiarvoja neljältä eri valmistajalta.

Control system for forced-air cooling of horticultural products

This work is a study of the implementation of a classical controller using a tuning method referred to as IMC (Internal Model Control) and aimed at the reduction of electrical energy consumption by the appropriate relation between energy consumption and the cooling time with forced air. The supervisory system installed was able to manipulate the variable of frequency of the signal power of the exhaust fan engine (forced air module), to accelerate or decelerate the loss of heat from the product to be cooled by airflow variation that passes through the mass of the produce. The results demonstrated a reduction in energy consumption from 64% and an increase of only 8% in the cooling time to the system using PI/IMC (Proportional - Integral with IMC) tuning method compared with the system in its operating nominal condition. This PI/IMC control may be implemented directly in a frequency converter, without the need to purchase a computer or PLC (programmable logic controller) to run the dedicated application, increasing its economical viability.