Fritz Feigl: sua obra e novos campos tecno-científicos por ela originados

Fritz Feigl's scientific legacy of more than 500 original publications of spot reactions and new chemical concepts, includes a precise definition of identification limit, the difference between specific and selective reactions, and the masking/demasking of chemical reactions, the selective functionalization for the development of new reactions. It resulted in a considerable and varied number of new applications evident in hundreds of citations of his publications, up to 2003, throughout the thirty years following his passing away, and comprehending scientific as well as commercial fields, like that of kits for exploratory tests, based on his reactions and of his followers.

Fotodegradação de hidrocarbonetos policíclicos aromáticos em placas de sílica impregnadas com dióxido de titânio

Photodegradation of the PAHs anthracene, chrysene and benzo[k]fluoranthane on silica gel impregnated with TiO2 and over glass plates holding TiO2 was studied. Silica gel plates holding these substances were exposed to solar radiation, developed with hexane and photographed under ultra-violet light. The plates containing benzo[k]fluoranthene were also analysed by both diffuse reflectance and laser induced fluorescence. Diffuse reflectance spectra of the fluorescent spot from non irradiated plates showed small differences when compared with those obtained from irradiated plates. These spectral differences are compatible with formation of less conjugated compounds during irradiation. Fluorescence and time resolved fluorescence spectra observed after irradiation were identical to those obtained with benzo[k]fluoranthene in methanol. On plates holding silica, PAH degradation requires longer periods of solar irradiation when compared with those plates containing silica impregnated with TiO2. Glass plates impregnated with TiO2 also showed very rapid PAH degradation.

Hitsatun kerrossihtilevyrakenteen soveltuvuus sellutehtaan laitteiden suodatinpinnaksi

Tässä diplomityössä tutkittiin hitsaamalla valmistettavan kerrossihtilevyn soveltuvuutta eri sellutehtaan laitteisiin mekaanisen kuormituskokeen, korroosiokokeen ja syrjäytyskokeiden avulla. Tutkimusympäristönä käytettiin puukuitupesuria, sillä kerrossihtilevyrakenteen todennäköisimpiä käyttökohteita ovat erilaiset massan pesuun tarkoitetut laitteet. Mekaanisen kuormituksen kokeessa tarkasteltiin kerrossihtilevyn staattista ja dynaamista kuormituksen kestoa painevaihteluiden avulla pesurin koelokerossa ja verrattiin sitä porattuun reikälevyyn. Kokeessa käytetyn kerrossihtilevyversion todettiin olevan huomattavasti porattua saman paksuista reikälevyä heikompi dynaamisen kuormituksen alaisena. Syrjäytyskokeilla määritettiin syrjäytysnopeus erilaisilla reiänhalkaisijoilla ja –jaoilla sekä tutkittiin väriaineen avulla sokeiden tukikannasten vaikutusta syrjäytyspesun homogeenisuuteen levyn pinnassa. Syrjäytysnopeuden todettiin heikentyvän vapaan reikäpinta-alan pienentyessä. Väriaineellisissa kokeissa ei havaittu tukikannasten merkittävästi alentavan syrjäytysnopeutta. Korroosiokokeilla tutkittiin ja vertailtiin laser- ja vastuspistehitsien korroosionkestokykyä kloridipitoisissa olosuhteissa lämpötilan säätelyn mahdollistavan olosuhdekaapin avulla. Laserhitsauksessa parametrien ei havaittu vaikuttavan merkittävästi hitsin herkistymislämpötilaan. Vastuspistehitsaamalla on mahdollista saavuttaa laserhitsien korroosionkesto.

Leimuhitsauksen kokonaisvaltainen laadunhallinta päättymättömässä valssauksessa

Leimuhitsauksen laadunhallinnassa tärkeää on prosessimainen toiminta ja toimintojen kokonaisvaltaisuuden hahmottaminen. Leimuhitsauksen ollessa osana päättymätöntä valssausta hitsauksen laadunhallinta voidaan jakaa kolmeen päävaiheeseen: ennen hitsausta, hitsauksen aikana ja hitsauksen jälkeen vaikuttaviin laaduntuottotekijöihin. Leimuhitsauksen laaduntuottotekijöiden määritys ja jaottelu kaavioiksi on toteutettu tässä työssä. Leimuhitsin tekniseen laatuun vaikuttavat monet ilmiöt ja parametrit hitsauksen aikana. Tärkeimpiä hitsausparametreista ovat hitsausjännite, alustan liikenopeus, tyssäysmatka sekä leimutusaika. Väärät hitsausolosuhteet tai hitsausparametrit aiheuttavat erilaisia mekaanisia ja metallurgisia vikoja leimuhitsiin. Eräs metallurginen vikatyyppi ovat oksidisulkeumat hitsialueella. Nämä hapettuneet alueet voivat johtaa juurensa erilaisista syistä ja esimerkiksi leimutusajan ja epätasaisen liitospinnan yhteyttä sulkeumien syntyyn on epäilty. Pidennetyillä leimutusajoilla tehtyjen hitsauskokeiden ja hitsien rikkovien aineenkoetuskokeiden tuloksena todettiin tässä tutkittujen koehitsien oksidisulkeumien syntyvän hapettumalla leimutuksen aikana tai juuri hetkellä ennen tyssäystä, minkä lisäksi kosteat olosuhteet hitsausatmosfäärin ympärillä heikentävät lopputuloksen laatua. Leimutusajalla on tärkein osa leimutettavia pintoja tasaavana tekijänä ja mitä epätasaisempi liitettävä pinta on, sitä pidemmän leimutusajan se tarvitsee.

Perspectives for the Spanish Intervention in Macao in the 19th Century

The purpose of this paper is to analyse some essential events concerning the relationship between Spain and Macao in the middle of the 19th century. Macao remained as a privileged spot for the commercial activities of Spain in China after the opening of the international ports agreed upon in the Treaty of Nanjing in 1842. This encouraged Spanish diplomatic representatives to render special attention to the Portuguese enclave. This became the origin of a shocking proposal for the military conquest of Macao and its surrounding territories by one of these representatives, Sinibaldo de Mas. Although this proposal was never taken under consideration, it helps us to better understand the role Macao played in Spanish strategies in China. Years later, Mas participated as a mediator when the Chinese government attempted to regain sovereignty over Macao by paying an economic compensation to Portugal. The involvement of Sinibaldo de Mas in this project has a strong symbolic meaning, making him a key agent in the relations between Spain and Macao in the 19th century.

Determination of ambroxol in syrups using diffuse reflectance spectroscopy

This paper reports an analytical method for the determination of ambroxol in micellar medium by spot test-diffuse reflectance spectroscopy. The reflectance measurements were performed analyzing the colored compound (λ= 520 nm) produced from the reaction between ambroxol and p-dimethylaminocinnamaldehyde on the surface filter paper. The linear range was from 1.21 × 10"3 to 9.65 × 10"3 mol L-1 (500 - 4000 μg mL-1). The limit of detection and quantification were 3.50 x 10-4 mol L-1 (145 μg mL-1) and 1.16 x 10-3 mol L-1 (481 μg mL-1), respectively. Five commercial samples were analysed and the results obtained by the proposed method were in good agreement with those obtained by the literature method at 95% confidence level.

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.

Desenvolvimento de um método reflectométrico ambientalmente mais amigável para a determinação de metoclopramida em formulações farmacêuticas

A simple and more environmentally friendly method by combined spot test-diffuse reflectance spectroscopy for determining metoclopramide in pharmaceutical formulations is described. The method is based on the reaction between metoclopramide and p-dimethylaminocinnamaldehyde, in the presence of HCl, producing a colored compound (λmáx = 580 nm) on the filter paper. The linear range was from 5.65 x 10-4-6.21x10-3 mol L-1 (r = 0.999). The limit of detection was 1.27 x 10-4 mol L-1. The proposed reflectometric method was applied successfully to the determination of metoclopramide in pharmaceuticals and it was favorably compared with the Brazilian or British Pharmacopoeia methods at 95% confidence level.

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.

2-(4-IODO-2,5-DIMETOXIFENIL)-N-[(2-METOXIFENIL)METIL]ETAMINA OU 25I-NBOME: CARACTERIZAÇÃO QUÍMICA DE UMA DESIGNER DRUG

Drug trafficking and the introduction of new drugs onto the illicit market are one of the main challenges of the forensic community. In this study, the chemical profile of a new designer drug, 2-(4-iodine-2,5-dimethoxyphenyl)-n-[(2-methoxyphenyl)methyl]etamine or 25I-NBOMe was explored using thin layer chromatography (TLC), ultraviolet-visible spectrophotometry (UV-Vis), attenuated total reflection with Fourier transform infrared spectroscopy(ATR-FTIR), gas chromatography mass spectrometry (GC-MS) and electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry (ESI-FT-ICR MS). First, the TLC technique was effective for identifying spots related to 25C-, 25B- and 25I-NBOMe compounds, all with the same retention factor, Rf ≈ 0.50. No spot was detected for 2,5-dimethoxy-4-bromoamphetamine, 2,5-Dimethoxy-4-chloroamphetamine or lysergic acid diethylamide compounds. ATR-FTIR preserved the physical-chemical properties of the material, whereas GC-MS and ESI-MS showed better analytical selectivity. ESI(+)FT-ICR MS was used to identify the exact mass (m/z428.1706 for the [M + H]+ ion), molecular formula (M = C18H22INO3), degree of unsaturation (DBE = 8) and the chemical structure (from collision induced dissociation, CID, experiments) of the 25I-NBOMe compound. Furthermore, the ATR-FTIR and CID results suggested the presence of isomers, where a second structure is proposed as an isomer of the 25I-NBOMe molecule.

Controle da ferrugem da folha e da mancha bronzeada da folha de trigo pelo uso de fungicidas em tratamento de sementes

The control of leaf rust and tan spot of wheat by seed treatment with fungicides was evaluated during 1998 in Passo Fundo, RS. Except for treatments including triadimenol and iprodione, leaf rust and tan spot severity in above ground parts of wheat plants was drastically reduced by the fluquinconazole fungicide used.

Mancha foliar e podridão de frutos da acerola causadas por Calonectria ilicicola

A new leaf spot and fruit rot disease is reported on barbados cherry (Malpighia glabra), occurring in the State of Maranhão, Brazil, caused by the fungus Calonectria ilicicola.

RT-PCR and Dot Blot hybridization methods for a universal detection of tospoviruses

Transcriptase reverse - polymerase chain reaction (RT-PCR) and dot blot hybridization with digoxigenin-labeled probes were applied for the universal detection of Tospovirus species. The virus species tested were Tomato spotted wilt virus, Tomato chlorotic spot virus, Groundnut ringspot virus, Chrysanthemum stem necrosis virus, Impatiens necrotic spot virus, Zucchini lethal chlorosis virus, Iris yellow spot virus. Primers for PCR amplification were designed to match conserved regions of the tospovirus genome. RT-PCR using distinct primer combinations was unable to simultaneously amplify all tospovirus species and consistently failed to detect ZLCV and IYSV in total RNA extracts. However, all tospovirus species were detected by RT-PCR when viral RNA was used as template. RNA-specific PCR products were used as probes for dot hybridization. This assay with a M probe (directed to the G1/G2 gene) detected at low stringency conditions all Tospovirus species, except IYSV. At low stringency conditions, the L non-radioactive probe detected the seven Tospovirus species in a single assay. This method for broad spectrum detection can be potentially employed in quarantine services for indexing in vitro germplasm.

Molecular and pathogenic variability of Drechslera isolates from oats

Severe epidemics of leaf blotch and black leaf spot of oat (Avena sativa) caused by Drechslera avenae and Drechslera sp., respectively, are frequently observed in the State of Paraná, Brazil. Although some morphological differences between the isolates causing two different symptoms were noticed, the genetic relationship between them was not clear. Twenty-four isolates of D. avenae and Drechslera sp, collected between 1996-98, were assessed for the genetic variability by molecular and pathogenic analyses. The amplification products using primer pair ITS4/ITS5 showed a fragment length of approximately 600 bp for all the isolates except for one black spot isolate, where the fragment length was approximately 550 bp. Restriction enzymes Hinf I and Taq I, that cut in the ITS region, produced similar restriction patterns for all the isolates, whereas four others produced variable restriction patterns. RAPD analysis also showed distinctive patterns for some isolates. No clear difference between the black spot and the leaf blotch isolates was observed either by the molecular or by the pathogenicity analysis. Nonetheless, the rDNA analysis suggests that Drechslera probably comprises at least three distinct taxa. The results indicate that the difference observed between the isolates originating from two types of symptoms is due to intra-specific variants of D. avenae.

Detection of drechslera avenae in oat seeds

The fungus Drechslera avenae, the causal agent of Helminthosporium leaf spot on oats (Avena sativa), survives as mycelium in crop residues and in infected seeds. In trials carried out in the laboratory, ten methods were evaluated for their efficiency to detect D. avenae in oat seeds. In each experiment, groups of two or three methods were compared to a standard protocol, in which seeds were placed in Petri dishes containing the Reis selective medium and incubated at 25±2 °C for ten days. Data were submitted to analysis of variation and the means of the methods were compared using the Dunnett test at the 5% significance level. Overall, the highest levels of seed infection by D. avenae were observed on oat seeds plated in the osmotic, the oat-agar and the Reis media, or on seeds subjected to heat treatment previous to incubation in malt-agar. Therefore, these methods should be recommended for detection of D. avenae in oat seed testing.