Ion pair-dispersive liquid-liquid microextraction of trace amount of rhodium ion in water and road dust samples prior to flame atomic absorption spectrometry determination

A simple ion pair-dispersive liquid-liquid microextraction method was proposed for preconcentration trace amounts of rhodium. An ion association complex of RhCl4- and tetradecyldimetylbenzylamonium was extracted into cholorobenzene. The volume and the type of extractive and dispersive solvents, the extraction time and the pH of the aqueous solutions were optimized. The calibration curve was linear in the range of 0.6-500 ng mL-1 of rhodium. The limit of detection was 0.10 ng mL-1 in initial solution and preconcentration factor was 40. The proposed method was successfully applied to the extraction and determination of rhodium in road dust and water samples.

Polímeros impressos com íons: fundamentos, estratégias de preparo e aplicações em química analítica

Chemical imprinting technology has been widely used as a valuable tool in selective recognition of a given target analyte (molecule or metal ion), yielding a notable advance in the development of new analytical protocols. Since their discovery, molecularly imprinted polymers (MIPs) have been extensively studied with excellent reviews published. However, studies involving ion imprinted polymers (IIPs), in which metal ions are recognized in the presence of closely related inorganic ions, remain scarce. Thus, this review involved a survey of different synthetic approaches for preparing ion imprinted adsorbents and their application for the development of solid phase extraction methods, metal ion sensors (electrodes and optodes) and selective membranes.

Synthesis, characterization and application of ion imprinted poly(vinylimidazole) for zinc ion extraction/preconcentration with faas determination

In this paper, we describe the synthesis of an ion imprinted polymer (IIP) by homogeneous polymerization and its use in solid-phase to extract and preconcentrate zinc ions. Under optimal conditions (pH 5.0, preconcentration flow rate of 12.0 mL min-1, and eluted with 1.0 mol L-1 HNO3) this procedure allows the determination of zinc with an enrichment factor of 10.2, and with limits of detection and quantification of 1.5 and 5.0 µg L-1, respectively. The accuracy of our results was confirmed by analysis of tap water and certified reference materials: NIST 1570a (Spinach leaves) and NIST 1515 (Apple leaves).

Ultrafiltration membranes from waste polyethylene terephthalate and additives: synthesis and characterization

The synthesis and characterization of asymmetric ultrafiltration membranes from recycled polyethylene terephthalate (PET) and polyvinylpyrrolidone (PVP) is reported. PET is currently used in many applications, including the manufacture of bottles and tableware. Monomer extraction from waste PET is expensive, and this process has not yet been successfully demonstrated on a viable scale. Hence, any method to recycle or regenerate PET once it has been used is of significant importance from scientific and environmental research viewpoints. Such a process would be a green alternative due to reduced raw monomer consumption and the additional benefit of reduced manufacturing costs. The membranes described here were prepared by a phase-inversion process, which involved casting a solution containing PET, m-cresol as solvent, and polyethylene glycol (PEG) of different molecular weights as additives. The membranes were characterized in terms of pure water permeability (PWP), molecular weight cut-off (MWCO), and flux and membrane morphology. The results show that the addition of PEG with high molecular weights leads to membranes with higher PWP. The presence of additives affects surface roughness and membrane morphology.

Potentiometric determination of Nickel (II) ion using 2-hydroxy-1-naphthylidene-N-cyanoacetohydrazone as electroactive material

A potentiometric Nickel sensor was prepared using 2-hydroxy-1-naphthylidene-N-cyanoacetohydrazone as electro-active material and epoxy resin as a binding material. A membrane composed of 40% Schiff's base and 60% epoxy resin exhibited the best performance. The membrane showed excellent response in the concentration range of 0.15 ppm to 0.1 mol L- 1 Ni+2 ions with non-Nernstian slope of 22.0 mV/decade, had a rapid response time (less than 10 s), and can be used for three months without any considerable loss of potential. The sensor was useful within the pH range of 1.3 to 9.6, and was able to discriminate between Ni2+ and a large number of alkaline earth and transition metal ions. The practical utility of the sensor has been demonstrated by using it successfully as an indicator electrode in the potentiometric titration of Ni2+ with EDTA and oxalic acid.

Determination of Mn2+ ion by solution scanometry as a new, simple and inexpensive method

In this research, scanometry was used as a new, simple, fast and inexpensive method for a colorimetric determination of Mn2+ ion in water samples and thermocouple wire through the use of periodate reagent in an acidic medium. The results showed the oxidization of colorless Mn2+ ion by periodate and the formation of a purplish MnO4- ion. The system had a linear range of 1.0 to 70.0 µg mL-1 Mn2+ ion with a detection limit of 0.314 µg mL-1 and a relative standard deviation of 2.77% for G color value. This method has the capability to determine low levels of Mn2+ ion in thermocouple wire and water samples.

Uses of nitrate ion sensitive electrodes

Some models of ion-selective electrodes (ISE) and other methods have been elaborated, to quantify nitrate levels in environmental samples (water, fruits, vegetables and others), using direct potentiometry

The Li+, Na+ and K+ ion exchange reaction process on the surface of mixed oxide SiO2/TiO2/Sb2O5 surface prepared by the sol-gel processing method

The porous mixed oxide SiO2/TiO2/Sb2O5 obtained by the sol-gel processing method presented a good ion exchange property and a high exchange capacity towards the Li+, Na+ and K+ ions. In the H+/M+ ion exchange process, the H+ / Na+ could be described as presenting an ideal character. The ion exchange equilibria of Li+ and K+ were quantitatively described with the help of the model of fixed tetradentate centers. The results of simulation evidence that for the H+ / Li+ exchange the usual situation takes place: the affinity of the material to the Li+ ions is decreased with increasing the degree of ion exchange. On the contrary, for K+ the effects of positive cooperativity, that facilitate the H+ / K+ exchange, were revealed.

Interaction study of moxifloxacin with Cu(II) ion using square-wave voltammetry and its application in the determination in tablets

This work presents an electroanalytical method for the determination of moxifloxacin (MOXI) in tablets by its interaction with Cu(II) ion and subsequent electrochemical reduction at hanging mercury drop electrode (HMDE). A well-defined reduction peak at -0.21 V vs. Ag/AgCl in Phosphate buffer 0.04 mol L-1 pH 8.0 was observed for the complex reduction MOXI-Cu(II), using square-wave voltammetry (SWV). Using a 10 s of accumulation time at -0.40 V was found a limit detection of 3.60x10-8 mol l-1. The obtained results have shown good agreement with those obtained by spectrophotometric method.

Spectrophotometric determination of nevirapine using tetrathiocyanatocobalt(II) ion as a reagent

A simple and rapid spectrophotometric method for the determination of nevirapine is described. The method is based on the reaction of nevirapine with tetrathiocyanatocobalt(II) ion in buffer of pH 4 to form the corresponding complex. Beer's law is obeyed in the range of 0.2 - 2.0 µg mL-1 for nevirapine. The optical parameters such as molar absorptivity, Sandell's sensitivity, detection limit and quantitation limit were found to be 1.16× 10(4) Lmol-1cm-1, 2.09 X 10-3 µg cm-2, 0.073 µg mL-1 and 0.222 µg mL-1 respectively. The optimum reaction conditions and other analytical parameters were evaluated. The statistical evaluation of the method was examined by determining intra-day and inter-day precision. The proposed method has been successfully applied for the determination of nevirapine in pharmaceutical formulations.

Synthesis and characterization of Fe(III)-doped ceramic membranes of titanium dioxide and its application in photoelectrocatalysis of a textile dye

Pure and Fe(III)-doped TiO2 suspensions were prepared by the sol gel method with the use of titanium isopropoxide (Ti(OPri)4) as precursor material. The properties of doped materials were compared to TiO2 properties based on the characterization by thermal analysis (TG-DTA and DSC), X-ray powder diffractometry and spectroscopy measurements (FTIR). Both undoped and doped TiO2 suspensions were used to coat metallic substrate as a mean to make thin-film electrodes. Thermal treatment of the precursors at 400ºC for 2 h in air resulted in the formation of nanocrystalline anatase TiO2. The thin-film electrodes were tested with respect to their photocatalytic performance for degradation of a textile dye in aqueous solution. The plain TiO2 remains as the best catalyst at the conditions used in this report.

Ion modulated organic transistors

I likhet med vanliga plaster är de π-konjugerade polymererna flexibla, lösliga och processbara vid låga temperaturer (< 150 ºC). Därutöver har de egenskapen att leda ström. Konduktivitetsintervallet är brett och omfattar nästintill metallisk ledningsförmåga å ena sidan, via halvledarkonduktiva till isolerande å andra sidan. Polymererna utgörs av regelbundna kedjor av kolatomer och associeras sålunda till organiska material. Sedan de första vetenskapliga rapporterna publicerades vid slutet av 1970-talet har π-konjugerade polymerer använts och utvecklats i exempelvis solceller, dioder, lysdioder och transistorer. Nobelpriset i kemi tilldelades år 2000 åt Hideki Shirakawa, Alan J. Heeger och Alan G. MacDiarmid för upptäckten och utvecklandet av ledande polymerer. I min avhandling har jag arbetat med att utveckla och förstå lågspännings jonmodulerade organiska transistorer. Två typer av jonmodulerade organiska transistorer studeras: (1) den jonmodulerade organiska fälteffekt transistorn (jonmodulerade OFETen), som utgör den centrala transistorn i avhandlingen, samt (2) den elektrokemiska transistorn. Den första typen fungerar som en konventionell OFET. Strömmen i halvledaren moduleras av det elektriska fältet över isolatorn. Med användandet av en elektrolyt ”isolator” orsakar polariseringen av jonerna däremot ett högt elektriskt fält vid elektrolyt/halvledargränssnittet och man åstadkommer modulering av strömmen redan vid några volts drivspänningar. I den andra typen utnyttjas elektrokemi för att medelst reduktion/oxidation modulera strömmen i den π-konjugerade polymeren. Ett viktigt ändamål i avhandlingen har också varit att kunna tillverka transistorerna med masstillverkningsmetoder. I avhandlingen presenteras de jonmodulerade organiska transistorernas möjlighet att framställas med masstillverkningsmetoder. Nya koncept introduceras och svagheter identifieras. Skillnaderna mellan OFETen, jonmodulerade OFETen och den elektrokemiska transistorn klargörs. Arbetet skall däremot inte anses fullbordat utan forskningen fortgår för att kringgå svagheterna, öka på transistorernas stabilitet och framförallt tillämpa dem i innovativa applikationer.

Avaliação técnica e econômica da extração de madeira de eucalipto com "Track-Skidder" em região montanhosa

O presente estudo teve como objetivo central avaliar técnica e economicamente atividades de extração em área montanhosa, utilizando um trator florestal arrastador com esteiras (Track-Skidder). O estudo foi conduzido em povoamentos de eucalipto de uma empresa florestal do Estado de Minas Gerais, nos quais o sistema de colheita foi o de árvore inteira, sendo o sistema mecanizado utilizado nas suas atividades de corte, extração e traçamento. A avaliação técnica consistiu em detectar e dimensionar os fatores de interrupções operacionais e mecânicas, como também em determinar os índices de produtividade, eficiência operacional, disponibilidade mecânica e grau de utilização. A avaliação econômica consistiu na determinação dos custos operacionais, bem como em determinar a distribuição destes custos. As áreas de estudo foram estratificadas em três níveis de declividades e três níveis de distâncias de extração. De acordo com o estudo os estratos de menor declividade e distância de extração apresentaram melhor produtividade em relação aos estratos de maior declividade e distância de extração. Ao final do período de avaliação a máquina atingiu disponibilidade mecânica de 79% e eficiência operacional de 76%. Seu custo operacional foi de US$57,00 por hora efetiva, sendo a depreciação e os juros os maiores elementos deste custo.

Nanosuodatuksen käyttö voimalaitoksen lisäveden valmistuksessa

Työssä selvitettiin nanosuodatuksen soveltuvuutta ja kannattavuutta voimalaitoksen lisäveden valmistuksessa. Kirjallisuusselvityksen ja nanosuodatuskokeiden tavoitteena oli arvioida nanosuodatukseen perustuvien lisäveden valmistusprosessien toiminnallista ja taloudellista kilpailukykyä perinteisiin prosesseihin verrattuna. Voimalaitoksen lisävedellä tarkoitetaan vesi-höyrykiertoon syötettävää vettä, joka korvaa kierrossa menetetyn veden. Nykyisin se valmistetaan vesijohto- tai pintavedestä käänteisosmoosiin ja ioninvaihtoon perustuvilla menetelmillä. Nanosuodatus on käänteisosmoosin tapaan kalvotekniikkaan perustuva erotusprosessi. Kaikki kalvot poistivat orgaanisen aineksen tehokkaasti (>90 %). Suolaretentioissa oli suuria eroja kalvojen välillä, vaikka kalvotoimittajien ilmoittamat retentiot olivat samaa tasoa. NF90-kalvo tuotti puhtainta permeaattia. Kahden kalvon (NF90 ja ESNA1-LF2) kohdalla havaittiin vuon alenemista, kun vuo oli kokeiden alussa noin 30 ja 40 L/m2/h. Likaantumisen merkkejä ei havaittu minkään kalvon kohdalla, kun vuoarvo oli maltillinen (n. 20 L/m2/h). Raakaveden vaikutus NF90-permeaatin laatuun oli vähäinen. Muilla kalvoilla raakaveden vaikutus permeaatin laatuun oli merkittävä. Investointi- ja käyttökustannusten perusteella nanosuodatukseen perustuvat lisäveden valmistusprosessit ovat kilpailukykyisiä nykyisiin lisäveden valmistusprosesseihin verrattuna. Pintavettä raakavetenä käyttävät nanosuodatusprosessit maksavat itsensä takaisin 3–5 vuodessa vesijohtovettä raakavetenä käyttävään käänteisosmoosiprosessiin verrattuna.

Kalvosuodatuksen ja adsorption yhdistäminen biojalostamon erotusprosesseissa

Tässä diplomityössä tutkittiin kalvosuodatuksen ja adsorption yhdistämistä biojalostamon erotusprosesseissa. Työn kirjallisuusosassa käsitellään hemiselluloosien erottamista puusta, kalvosuodatusta hemiselluloosien käsittelyssä sekä hemiselluloosien pilkkomista sokereiksi ja sokereiden kromatografista erotusta. Kokeellisessa osassa tutkittiin hemiselluloosahydrolysaatin fraktioimista kalvosuodatuksella ja adsorbenttikäsittelyn vaikutusta hydrolysaatin suodatettavuuteen. Kokeellisessa osassa tutkittiin myös fraktioinnin vaikutusta hartsien likaantumiseen happohydrolyysin jälkeisessä kromatografisessa erotuksessa. Työssä kokeiltiin useita erilaisia kalvoja, mutta suurin osa suodatuksista tehtiin regeneroidusta selluloosasta valmistetulla kalvolla UC030 ja polyeetterisulfoni kalvolla UFX5. Esikäsittelyyn käytettiin XAD16 adsorbenttia ja hartsien likaantumista tutkittiin CS12GC Na+ hartsilla. Suodatuskokeet tehtiin sekä laboratoriomittakaavan Amicon-suodattimella että pilot-mittakaavan CR- suodattimella. Työn tulokset osoittivat, että konsentroituneen hemiselluloosafraktion tuottaminen tehokkaasti ei onnistu kalvosuodatuksella ilman esikäsittelyä. Kalvon likaantumisen vuoksi permeaattivuo laski hyvin nopeasti niin alhaiseksi, ettei suodatuksen jatkaminen olisi taloudellisesti kannattavaa. Hydrolysaatin esikäsittely XAD16 adsorbentillä poisti tehokkaasti kalvoja likaavia uuteaineita ja ligniiniä. Adsorbenttikäsittelyn jälkeen hydrolysaatin suodattaminen onnistui ilman permeaattivuon huomattavaa alenemista toisessa suodatusvaiheessa ja saatiin aikaiseksi hyvin konsentroitunut hemiselluloosafraktio.