Uso de frascos de polipropileno descartáveis no pré-tratamento de amostras de água para determinação de chumbo, cobre e mercúrio por voltametria de onda quadrada

In this work a simple and versatile procedure is described for treating water samples using small polypropylene (PP) vials (4 mL) for determining heavy metals by square wave voltammetry (SWV). This procedure involves treatment with nitric acid (0.2 mol L-1) and boiling in a water-bath (~ 100 ºC). This process is completed after one hour and allows the pretreatment of several samples simultaneously. The accuracy was estimated using addition/recovery studies and certified water sample analysis, yielding an agreement near to 100%.

Passiiviset turvallisuusjärjestelmät tulevaisuuden kiehutusvesireaktorilaitoksissa

Kandidaatintyössä on esitelty passiivisten turvallisuusjärjestelmien hyödyntämistä seuraavan sukupolven kiehutusvesireaktorilaitoksissa.

Métodos de extração para quantificação de manganês disponível em fertilizantes

The solubility of Mn in different fertilizers (MnSO4.H2O-p.a., MnO2-p.a.+MnO-Ind., MnO2-Ind.+MnO-Ind., MnO2-p.a., MnO2-Ind. and MnO-Ind.) was determined using different methodologies: total content and soluble contents in water, 10% H2SO4, citric acid at 20 g L-1, diluted neutral ammonium citrate, (1+9) and DTPA at 0.005 mol L-1. The Mn solubilities in the latter three extractors were assessed after agitation of the sample for one hour and after boiling for 5 minutes. The extraction procedure using neutral ammonium citrate (1+9), at 1:100, with agitation for one hour, was shown to be the most adequate to assess the availability of Mn in fertilizers.

Experimento didático sobre cromatografia gasosa: uma abordagem analítica e ambiental

This paper describes an experiment to teach the principles of gas chromatography exploring the boiling points and polarities to explain the elution order of a series of alcohols, benzene and n-propanone, as well as to teach the response factor concept and the internal standard addition method. Retention times and response factors are used for qualitative identification and quantitative analysis of a hypothetical contamination source in a simulated water sample. The internal standard n-propanol is further used for quantification of benzene and n-butanol in the water sample. This experiment has been taught in the instrumental analysis course offered to chemistry and oceanography students.

Determinação de benzeno, tolueno, etilbenzeno e xilenos em gasolina comercializada nos postos do estado do Piauí

Automotive gasoline consists of a complex mixture of flammable and volatile hydrocarbons derived from crude oil with carbon numbers within the range of 4-12 and boiling points range of 30-225 ºC. Its composition varies with the kind of crude oil and the type of refinery process that they undergone. Aromatics hydrocarbons, in particular benzene, toluene, ethylbenzene and isomeric xylenes (BTEX) are the toxic group constituents presents. GC-FID was employed to quantify these hydrocarbons in 50 commercial gasoline samples from Piauí state. Statistical analysis techniques, such as PCA and HCA were used to analyze the data. Moreover, several validation parameters were evaluated.

The use of tribromoisocyanuric acid to distinguish among primary, secondary and tertiary alcohols

Primary, secondary and tertiary alcohols can be easily distinguished due to their reactivity towards tribromoisocyanuric acid (TBCA). The test is performed by adding TBCA to the alcohol in a test tube heated in a boiling water bath. Orange color develops in the tube containing the primary alcohol, light yellow is observed in the tube containing the secondary alcohol while the tertiary alcohol results in a colorless mixture.

Resgatando um método eficiente para determinação do ponto de ebulição de substâncias orgânicas: percolador versus Siwoloboff

The aim of this paper was to revive the accurate determination of the boiling point of organic compounds using the percolator technique developed in the 1960s. Although this method is simple, fast and efficient it is omitted from current textbooks. This method has several advantages over Siwoloboff such as high reproducibility and direct measurement of the boiling point of the sample obtained by observing the temperature of the vapor-liquid equilibrium. The experiments were performed in the organic chemistry laboratory but allow interdisciplinary integration with other disciplines of several academic areas.

DETERMINAÇÃO DE Cd E Pb EM AMOSTRAS DE GOMA XANTANA POR GF AAS

This paper describes the evaluation of a method for determination of Cd and Pb in xanthan gum samples by Graphite Furnace Atomic Absorption Spectrometry (GF AAS) using NH4H2PO4 as the chemical modifier. The sample preparation was performed using a reflux system adapted in the digestion tubes. With this system it was possible to increase the temperature of the digester block above the boiling point of the reaction medium, preventing loss of analyte and excessive evaporation of acids during heating. Samples were digested with HNO3 for 3 h in a digester block at 220 ºC. The limits of detection for Cd and Pb were 2.2 and 33.8 ng g-1, respectively. The RSDs for both analytes were, on average, lower than 5.0% and accuracy was verified by recovery tests, yielding values in the 83-100% range.

Kiehutusvesireaktorien polttoaineen kehityskaari

Tässä kirjallisuustyössä tutustutaan kiehutusvesireaktorien polttoainenipun kehitykseen. Työssä esitellään kolmen suurimman polttoainenippuvalmistajan polttoainemalleja ja muutoksia polttoainenippumallien välillä.

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.

Kiehutusvesireaktorien polttoaineen kehityskaari

Tässä kirjallisuustyössä tutustutaan kiehutusvesireaktorien polttoainenipun kehitykseen. Työssä esitellään kolmen suurimman polttoainenippuvalmistajan polttoainemalleja ja muutoksia polttoainenippumallien välillä.

CFD Modelling of Direct Contact Condensation in Suppression Pools by Applying Condensation Models of Separated Flow

The condensation rate has to be high in the safety pressure suppression pool systems of Boiling Water Reactors (BWR) in order to fulfill their safety function. The phenomena due to such a high direct contact condensation (DCC) rate turn out to be very challenging to be analysed either with experiments or numerical simulations. In this thesis, the suppression pool experiments carried out in the POOLEX facility of Lappeenranta University of Technology were simulated. Two different condensation modes were modelled by using the 2-phase CFD codes NEPTUNE CFD and TransAT. The DCC models applied were the typical ones to be used for separated flows in channels, and their applicability to the rapidly condensing flow in the condensation pool context had not been tested earlier. A low Reynolds number case was the first to be simulated. The POOLEX experiment STB-31 was operated near the conditions between the ’quasi-steady oscillatory interface condensation’ mode and the ’condensation within the blowdown pipe’ mode. The condensation models of Lakehal et al. and Coste & Lavi´eville predicted the condensation rate quite accurately, while the other tested ones overestimated it. It was possible to get the direct phase change solution to settle near to the measured values, but a very high resolution of calculation grid was needed. Secondly, a high Reynolds number case corresponding to the ’chugging’ mode was simulated. The POOLEX experiment STB-28 was chosen, because various standard and highspeed video samples of bubbles were recorded during it. In order to extract numerical information from the video material, a pattern recognition procedure was programmed. The bubble size distributions and the frequencies of chugging were calculated with this procedure. With the statistical data of the bubble sizes and temporal data of the bubble/jet appearance, it was possible to compare the condensation rates between the experiment and the CFD simulations. In the chugging simulations, a spherically curvilinear calculation grid at the blowdown pipe exit improved the convergence and decreased the required cell count. The compressible flow solver with complete steam-tables was beneficial for the numerical success of the simulations. The Hughes-Duffey model and, to some extent, the Coste & Lavi´eville model produced realistic chugging behavior. The initial level of the steam/water interface was an important factor to determine the initiation of the chugging. If the interface was initialized with a water level high enough inside the blowdown pipe, the vigorous penetration of a water plug into the pool created a turbulent wake which invoked the chugging that was self-sustaining. A 3D simulation with a suitable DCC model produced qualitatively very realistic shapes of the chugging bubbles and jets. The comparative FFT analysis of the bubble size data and the pool bottom pressure data gave useful information to distinguish the eigenmodes of chugging, bubbling, and pool structure oscillations.

Recovery of carboxylic acids from aqueous streams by extraction and back extraction

Separation of carboxylic acids from aqueous streams is an important part of their manufacturing process. The aqueous solutions are usually dilute containing less than 10 % acids. Separation by distillation is difficult as the boiling points of acids are only marginally higher than that of water. Because of this distillation is not only difficult but also expensive due to the evaporation of large amounts of water. Carboxylic acids have traditionally been precipitated as calcium salts. The yields of these processes are usually relatively low and the chemical costs high. Especially the decomposition of calcium salts with sulfuric acid produces large amounts of calcium sulfate sludge. Solvent extraction has been studied as an alternative method for recovery of carboxylic acids. Solvent extraction is based on mixing of two immiscible liquids and the transfer of the wanted components form one liquid to another due to equilibrium difference. In the case of carboxylic acids, the acids are transferred from aqueous phase to organic solvent due to physical and chemical interactions. The acids and the extractant form complexes which are soluble in the organic phase. The extraction efficiency is affected by many factors, for instance initial acid concentration, type and concentration of the extractant, pH, temperature and extraction time. In this paper, the effects of initial acid concentration, type of extractant and temperature on extraction efficiency were studied. As carboxylic acids are usually the products of the processes, they are wanted to be recovered. Hence the acids have to be removed from the organic phase after the extraction. The removal of acids from the organic phase also regenerates the extractant which can be then recycled in the process. The regeneration of the extractant was studied by back-extracting i.e. stripping the acids form the organic solution into diluent sodium hydroxide solution. In the solvent regeneration, the regenerability of different extractants and the effect of initial acid concentration and temperature were studied.

Ydinvoimalaitosten vesikemia ja korroosionesto

Ydinvoimalaitosten vesikemian optimointi ja korroosionesto on välttämätöntä laitosten taloudellisen ja turvallisen käytön kannalta. Eri laitoksiin liittyvää vesikemiaa ja järjestelmissä havaittavia korroosion muotoja on tutkittu laajasti ja tutkitaan yhä edelleen. Monien prosessien ymmärtäminen vaatii usean eri tieteenalan osaamista, kuten kemiantekniikan, energiatekniikan sekä materiaalitekniikan. Tässä työssä kerrotaan yksinkertaistaen vesikemiaan ja korroosioon liittyviä prosesseja ja reaktioita. Työssä käsitellään kevytvettä jäähdytteenä sekä moderaattorina käyttävien ydinvoimalaitosten eri korroosiomuotoja sekä säteilyn vaikutusta näihin suoraan tai vesikemian kautta. Työssä kerrotaan korroosio- ja aktivoitumistuotteiden muodostumisesta ja kulkeutumisesta sekä näiden tuotteiden vaikutuksista laitosten toimintaan. Korroosion ja materiaalien aktivoitumisen pohjalta tarkastellaan kattavasti ydinvoimalaitosten tyypillisimpiä vesikemian muokkauskeinoja sekä korroosionhallintaa. Tärkeimpiin asioihin syvennytään hieman lähemmin. Tarkastelun kohteena ovat eniten käytetyt ydinvoimalaitokset, eli länsimaiset paine- ja kiehutusvesilaitokset sekä venäläisvalmisteiset VVER-laitokset. Tarkoituksena on ollut luoda tiivis tietopaketti opiskelijoiden käyttöön muun opintomateriaalin tueksi.