Comparison of three analytical methods for the determination of quinolones in pig muscle samples

This work presents a comparison between three analytical methods developed for the simultaneous determination of eight quinolones regulated by the European Union (marbofloxacin, ciprofloxacin, danofloxacin, enrofloxacin, difloxacin, sarafloxacin, oxolinic acid and flumequine) in pig muscle, using liquid chromatography with fluorescence detection (LC-FD), liquid chromatography-mass spectrometry (LC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). The procedures involve an extraction of the quinolones from the tissues, a step for clean-up and preconcentration of the analytes by solid-phase extraction and a subsequent liquid chromatographic analysis. The limits of detection of the methods ranged from 0.1 to 2.1 ng g−1 using LC-FD, from 0.3 to 1.8 using LC-MS and from 0.2 to 0.3 using LC-MS/MS, while inter- and intra-day variability was under 15 % in all cases. Most of those data are notably lower than the maximum residue limits established by the European Union for quinolones in pig tissues. The methods have been applied for the determination of quinolones in six different commercial pig muscle samples purchased in different supermarkets located in the city of Granada (south-east Spain).

Particle detector link system modifications in RE1/1 sector

The large hadron collider constructed at the European organization for nuclear research, CERN, is the world’s largest single measuring instrument ever built, and also currently the most powerful particle accelerator that exists. The large hadron collider includes six different experiment stations, one of which is called the compact muon solenoid, or the CMS. The main purpose of the CMS is to track and study residue particles from proton-proton collisions. The primary detectors utilized in the CMS are resistive plate chambers (RPCs). To obtain data from these detectors, a link system has been designed. The main idea of the link system is to receive data from the detector front-end electronics in parallel form, and to transmit it onwards in serial form, via an optical fiber. The system is mostly ready and in place. However, a problem has occurred with innermost RPC detectors, located in sector labeled RE1/1; transmission lines for parallel data suffer from signal integrity issues over long distances. As a solution to this, a new version of the link system has been devised, a one that fits in smaller space and can be located within the CMS, closer to the detectors. This RE1/1 link system has been so far completed only partially, with just the mechanical design and casing being done. In this thesis, link system electronics for RE1/1 sector has been designed, by modifying the existing link system concept to better meet the requirements of the RE1/1 sector. In addition to completion of the prototype of the RE1/1 link system electronics, some testing for the system has also been done, to ensure functionality of the design.

Determinação de carbaril utilizando testes ELISA (Enzyme-linked immunosorbent assay) e CLAE com detecção por arranjo de diodos

ELISAs have been applied to pesticide residue analysis due to their high sensitivity and selectivity. However, some ELISAs performance may be affected by matrix components. In this work, ELISA for carbaryl in water samples was checked for interference by naturally occurring fulvic acids. The results suggested that the high fulvic acid concentration (ž³30 mg L-1) and acidic pH conditions (pH 4.0) interfere with the signal detection decreasing the method sensitivity. A dilution of the samples and adjust to pH 8.0 are appropriate to minimize the matrix interferences in the ELISA method. Good correlation between ELISA and HPLC-DAD results was observed.

Relato de uma experiência: recuperação e cadastramento de resíduos dos laboratórios de graduação do Instituto de Química da Universidade Federal do Rio Grande do Sul

An experience aiming to promote a residue interchange and recovery between the teaching laboratories of the Chemistry Institute of this University is described. At the present, several residues interchange have already appeared as advantageous. To make the work easier, a software has been developed in order to keep a record of all the residues generated by the teaching laboratories. Standard labels have been developed for the residues in order to organize them. The software and the label design are described.

Extração por fluido supercrítico de alguns inseticidas carbamatos em amostras de batata, com determinação por HPLC/fluorescência e confirmação por HPLC/espectrometria de massas

Six supercritical fluid extraction (SFE) methods were tested, by varying the following operational parameters: CO2 pressure, time and temperature of extraction, type and proportion of static modifier, and Hydromatrix®/sample rate into cell. Firstly, insecticide carbamates were extracted from spiked potatoes samples (fortification level of 0,5 mg.Kg-1) by using SPE procedures, and then final extracts were analyzed HPLC/fluorescence. Good performance was observed with SFE methods that operated with values of temperature and CO2 pressure of 50 ºC and 350 bar, respectively. Best efficiency was obtained when it was used acetonitrile as a modifier (3% on the cell volume), and Hydromatrix®/sample rate of 2:1. Static time was of 1 min; total extraction time was of 35 min; dynamic extraction was performed with 15 mL of CO2, and it was used methanol (2 mL) for the dissolution of the final residue. In such conditions, pesticide recoveries varied from 72 to 94%, depending on the analyzed compound. In higher extraction temperatures, a rapid degradation was observed for some compounds, such as aldicarb and carbaryl; presence of their metabolites was further confirmed by HPLC-APCI/MS in positive mode. Detection limits for chromatographic analysis varied from 0,2 to 1,3 ng.

Reciclagem de cobre proveniente de analisador automático de carbono e nitrogênio

Isotopic and elemental analysis of N, C and S in liquid and solid samples has been simplified with the advent of automated systems. The simplest method of automation for this kind of analysis involves an elemental analyzer interfaced directly to the ion source of an IRMS (Isotope Ratio Mass Spectrometry). In the analyzer reduction system, an expressive amount of oxidized copper is generated as solid residue. This material is normally imported and the price is very high. A methodology was proposed for the recovery of metallic copper in order to recycle this reagent in the reduction system of a GC-IRMS, using the hydrogen gas in the vacuum line. Results show that it is possible to obtain a recycle of about 95 % of the initial metallic copper used in the reduction system.

Nano vitrocerâmica de escória de aciaria

The manufacture of glass-ceramics is an alternative route for the commercial use of metallurgical slags. Such types of glass-ceramics may find commercial applications owing to their low cost, good mechanical properties and superior visual aspect. Besides, due to the elimination of that industrial residue from the environment and also due to the possibility of replacement of natural stones such as marbles and granites, the use of slags is an activity with strong ecological appeal. While the use of blast-furnace slags for the production of glass-ceramics is well known, the utilization of steel making slags constitutes a challenge, because these materials possess low concentration of SiO2. In this work a novel composition for producing glasses and glass-ceramics from a steelmaking slag is presented. The crystal nucleation kinetics, the characterization of the resulting microstructures for two different thermal treatments and mechanical properties of the glass-ceramics are discussed. A glass-ceramic having a marble aspect, fine volumetric crystallization, high degree of crystallization and improved mechanical strength was obtained.

Integration of a Bioethanol Process to a Pulp Mill

Tässä diplomityössä tutkittiin puuhakkeen esihydrolyysi- ja hakkuujätteen hydrolyysiprosessien integroimista sellutehtaaseen bioetanolin tuottamiseksi. Tällaisesta ns. biojalostamosta luotiin WinGEMS-simulointiohjelmalla simulointimalli, jonka avulla tutkittiin bioetanoliprosessin vaikutusta sellutehtaan massa- ja energiataseisiin sekä alustavaa biojalostamon kannattavuutta. Simuloinnissa tarkasteltiin kolmea eri tapausta, joissa mäntysellun tuotannon ajateltiin olevan 1000 tonnia päivässä ja hakkuujätettä käytettävän 10 % tarvittavan kuitupuun määrästä: 1) Puuhakkeen esihydrolyysi ja hakkuujätteen hydrolyysi etanolin tuottamiseksi 2) Puuhakkeen esihydrolyysi, hakkuujäte kuorikattilaan poltettavaksi 3) Ei esihydrolyysiä, hakkuujäte kuorikattilaan poltettavaksi Verrattuna tapaukseen 3, puun kulutus kasvaa 16 % esihydrolysoitaessa puuhake ennen keittoa tapauksissa 1 ja 2. Kasvaneella puun kulutuksella tuotetaan tapauksessa 1 149 tonnia etanolia ja 240 MWh enemmän ylimääräsähköä päivässä. Tapauksessa 2 tuotetaan 68 tonnia etanolia ja 460 MWh enemmän ylimääräsähköä päivässä. Tämä tuottaisi vuotuista lisäkassavirtaa 18,8 miljoonaa euroa tapauksessa 1 ja 9,4 miljoonaa euroa tapauksessa 2. Hydrolyysin tuoteliuoksen, hydrolysaatin, haihduttaminen sekä hydrolyysiprosessien orgaanisten jäännöstuotteiden haihduttaminen ja polttaminen kasvattavat haihduttamon ja soodakattilan kuormitusta. Verrattuna tapaukseen 3, tapauksissa 1 ja 2 haihduttamon vaiheiden määrä on kasvatettava viidestä seitsemään ja tarvittavat lämmönsiirtopinta-alat lähes kaksinkertaistettava. Soodakattilan kuormitus kasvaa 39 % tapauksessa 1 ja 26 % tapauksessa 2.

Brideshead Revisited (1945) by Evelyn Waugh (1903-1966): the benefit of an Arcadian experience in confronting the human tragedy

As the frontispiece of Book One of Evelyn Waugh’s Brideshead Revisited, the phrase ‘Et in Arcadia ego’ announces the author’s intention of making the classical Arcadian theme a key reference in a text that speaks of nostalgia for a joyful past in times marked by sadness and pain. However, an interpretation may be approached from several directions even within the classical tradition. Thus, without ignoring philological or artistic aspects of the topic, this article focuses on a close study of the author’s most original message: the notion that a youthful Arcadian experience confers on young men and women a ‘residue of happiness’ able to sustain their future development and assist them in dealing with the challenges of personal tragedy.

Role of PheE15 gate in ligand entry and nitric oxide detoxification function of Mycobacterium tuberculosis truncated hemoglobin N

The truncated hemoglobin N, HbN, of Mycobacterium tuberculosis is endowed with a potent nitric oxide dioxygenase (NOD) activity that allows it to relieve nitrosative stress and enhance in vivo survival of its host. Despite its small size, the protein matrix of HbN hosts a two-branched tunnel, consisting of orthogonal short and long channels, that connects the heme active site to the protein surface. A novel dual-path mechanism has been suggested to drive migration of O(2) and NO to the distal heme cavity. While oxygen migrates mainly by the short path, a ligand-induced conformational change regulates opening of the long tunnel branch for NO, via a phenylalanine (PheE15) residue that acts as a gate. Site-directed mutagenesis and molecular simulations have been used to examine the gating role played by PheE15 in modulating the NOD function of HbN. Mutants carrying replacement of PheE15 with alanine, isoleucine, tyrosine and tryptophan have similar O(2)/CO association kinetics, but display significant reduction in their NOD function. Molecular simulations substantiated that mutation at the PheE15 gate confers significant changes in the long tunnel, and therefore may affect the migration of ligands. These results support the pivotal role of PheE15 gate in modulating the diffusion of NO via the long tunnel branch in the oxygenated protein, and hence the NOD function of HbN.

Procedimentos para recuperação de Ag de resíduos líquidos e sólidos

A simple procedure for recovering Ag, generated as residual solutions, from three different analytical methods, is presented. Based on the rate of the total Ag mass recovered, to the initial one in the initial residual solutions, efficiency as high as 97,9 ± 2,9% was obtained in the process. The purity of Ag, as Ag2O, was verified by employing this reagent in the determination of S in plant tissue. This leads to the generation of a solid metallic Ag as waste. In this situation, an 88,7 ± 0,6% Ag recovery was acquired, when a HNO3 solution was employed as solvent.

Gerenciamento de resíduos laboratoriais: recuperação de elementos e preparo para descarte final

This work shows some laboratory waste management developed in order to recover some elements or to prepare the waste for a correct final disposal. The 25 elements chosen cover basically all chemical behaviors found for the metals in the Periodic Table. The treatments adopted were based on the classical behavior in aqueous solution (wet chemistry) but an important condition for a full success was the previous knowledge of the qualitative composition of the wastes treated. Some general trends were found: the final liquid waste was always saline and normally presented a higher volume than the original waste; most original wastes were acid in nature; steps such as solid-liquid separation, washing, evaporating and calcining were currently performed. This work was also a very good experience in chemistry in solution for students and showed them the need of treating wastes for a better environment.

Tratamento dos resíduos gerados na síntese de polianilina em escala pré-piloto

Polyaniline (PAni) is one of the most studied conducting polymer. It can be synthesized by two methods: electrochemical or chemical oxidation. The chemical oxidation is more adequate to produce large quantities of polymer. Regardless of the synthesis scale, the treatment of the residues before its final destination is very important and necessary because it contains toxic aniline derivatives (carcinogens in some cases), acids and inorganic salts, both with low toxicity. In this work we discuss the methods used to treat these residues and to eliminate and discard the toxic substances. These were extracted from the reaction residues by using activated coal and the pH of the residue was neutralized.

Reciclagem química de zeólitas comerciais desativadas

Pyro and hydrometallurgical processes were applied to the treatment of spent commercial zeolites (a molecular sieve and a ZSM-5 sample). Both catalysts were employed in pilot plant units. They were kept in their original shape, they were not regenerated and were not subjected neither to mechanical stress nor to overheating zones during their time on-stream. Two recycling processes were tested: (i) direct solubilization of samples in mixtures of HF + H2O2 (60 ºC, 1 h). Although silicon was solubilized, insoluble matter was found in both samples, particularly in the molecular sieve, due to its high amounts of alkaline and alkaline-earth metals; (ii) fusion with KHSO4 (5 h, 600 ºC) with KHSO4/zeolite mass ratio 6:1. After fusion the solid was solubilized in water (100 ºC), leaving silicon as SiO2 residue. In both processes, solubilized metals were isolated by conventional selective precipitation techniques. Analysis of final products by common analytical methods shows that metals present in the original catalysts were recovered with very high yields except when the molecular sieve was treated with HF + H2O2. This reactant mixture proved to be suitable for processing zeolites with a low alkaline and alkaline-earth metal content whereas fusion with KHSO4 appeared to be adequate for all types of zeolites.

Recuperação de bromo em soluções aquosas residuais

A laboratory procedure was devised to recover bromine from waste alkaline aqueous solutions used in the isotopic determination of N-15. The laboratory apparatus comprises two round bottom flasks (1 and 2 L), a dropping funnel, a gas bubbler, a gas regulator and glass fittings. The waste solution is acidified with sulfuric acid forming molecular bromine that is stripped out by a flow of nitrogen gas bubbled through the solution. This gas is then bubbled through a solution of lithium hydroxide generating lithium bromide and lithium hypobromite. The efficiency of bromine recovery was estimated to be 82±2%. This resulting solution was successfully reused in the isotopic determination of N-15. The procedure can recycle most of the bromine used in the laboratory saving resources and preserving the environment. The procedure can be adapted to recover bromine of other laboratory waste streams.