Upload
lamliem
View
215
Download
0
Embed Size (px)
Citation preview
G R A Q – G r u p o d e R e a c ç ã o e A n á l i s e s Q u í m i c a s
A N N U A L R E P O R T
2009
RRREEELLLAAATTTÓÓÓRRRIIIOOO DDDEEE AAACCCTTTIIIVVVIIIDDDAAADDDEEESSS
222000000999
REQUIMTE-ISEP
Rua Dr. António Bernardino de Almeida, 431
4200-072 Porto
Portugal
tel.:+351-228340500
INDEX
GRAQ – ANNUAL REPORT – 2009
BRIEF HISTORY 3
MEMBERS 4
A. RESEARCH AREAS 7
1. ANALYTICAL CHEMISTRY 7
1.1. SUB-AREAS IN ANALYTICAL CHEMISTRY 8 1.1.1. Quality control and authenticity of food products 8 1.1.2. Environmental analysis 10 1.1.3. Health and pharmaceutical analysis 11
1.2. OUTPUT INDICATORS 13 1.2.1. FCT funded projects 13 1.2.2. non-FCT funded projects 14 1.2.3. Papers (ISI) 14 1.2.4. Papers (non-ISI) 15 1.2.5. Books 15 1.2.6. Ph.D. theses 15 1.2.7. MSc theses 15 1.2.8. International conferences 16 1.2.9. National conferences 19
1.3. OTHER ACTIVITIES 20
1.4. FUTURE RESEARCH 22
2. ENVIRONMENTAL CONTROL AND REMEDIATION 23
2.1. SUB-AREAS IN ENVIRONMENTAL CONTROL AND REMEDIATION 24 2.1.1. Waste management and toxicological evaluation 24 2.1.2. Soil and groundwater remediation 24 2.1.3. Removal of toxic compounds by means of adsorption strategies 25
2.2. OUTPUT INDICATORS 26 2.2.1. FCT funded projects 26 2.2.2. non-FCT funded projects 26 2.2.3. Papers (ISI) 26 2.2.4. Papers (non-ISI) 27 2.2.5. Books 27 2.2.6. Ph.D. theses 27 2.2.7. MSc theses 27 2.2.8. International conferences 27 2.2.9. National conferences 29
2.3. OTHER ACTIVITIES 29
2.4. FUTURE RESEARCH 30
3. RESEARCH METRICS 31
3.1. OUTPUT INDICATORS 31 3.1.1. International conferences 31
B. SCIENTIFIC EVALUATION 32
BRIEF HISTORY
GRAQ – ANNUAL REPORT – 2009
[ 3 ]
BRIEF HISTORY
The “Grupo de Reacção e Análises Químicas” (GRAQ) was formed in January 1999 by researchers from
the Instituto Superior de Engenharia do Porto (ISEP), and is located on the campus of ISEP. In 1999 the
group joined the Centro de Química da Universidade do Porto (CEQUP).
GRAQ became part of REQUIMTE in 2000 through the partnership of CEQUP with the Centro de
Química Fina e Biotecnologia (CQFB) da Faculdade de Ciências e Tecnologia da Universidade Nova de
Lisboa.
REQUIMTE is the largest network in Chemistry and Chemical Engineering established in Portugal and
was recognized as the Laboratório Associado para a Química Verde (Green Chemistry) by the
Portuguese Ministério da Ciência e do Ensino Superior in November 2001.
The objectives of REQUIMTE are:
a) To encourage the use of clean products and technologies;
b) To assist industry in the design and implementation of non-aggressive chemical processes;
c) To train young researchers in interdisciplinary areas related with the practice of sustainable
chemistry;
d) To publicise the principles of Green Chemistry and to alert society for the necessity of a
sustainable practice in everyday life.
Research is presently focused in the following thematic areas of: i) natural products, (ii) food quality and
safety, (iii) clean production technologies and processes, (iv) environmental control and remediation and
(v) catalysts, solvents and non-toxic compounds.
The sharing of multidisciplinary scientific knowledge, technology and equipment between researchers of
the two centres that form the network, has significantly contributed to the development of new projects in
Green Chemistry and to the enrichment and training of graduate students by making easier the mobility of
human resources.
At present the network REQUIMTE can be described as a big Laboratory that has two operating sites,
one at the Universidade Nova de Lisboa and the other at the Universidade do Porto
In this concept, the GRAQ research lines mainly focus on Analytical Chemistry and Environmental
Control and Remediation.
Scientific Coordinator: Cristina Maria Fernandes Delerue Alvim de Matos ([email protected])
Internet: www.graq.isep.ipp.pt | www.requimte.pt
MEMBERS
GRAQ – ANNUAL REPORT – 2009
[ 4 ]
MEMBERS Permanent Members
1. Ph.D. Cristina Maria Fernandes Delerue Alvim de Matos Professor Coordenador (ISEP)
2. Ph.D. Maria do Carmo Veiga Fernandes Vaz Professor Coordenador (ISEP)
3. Ph.D. Maria Teresa Pereira de Oliva Teles Moreira Professor Adjunto (ISEP)
4. Ph.D Maria Conceição Carvalho Benta de Oliveira Neves Professor Adjunto (ISEP)
5. Ph.D. Maria Goreti Ferreira Sales eq. Professor Adjunto (ISEP)
6. Ph.D. Maria Manuela Barbosa Correia eq. Professor Adjunto (ISEP)
7. Ph.D. Sónia Adriana Ribeiro da Cunha Figueiredo eq. Professor Adjunto (ISEP)
8. Ph.D. Simone Barreira Morais eq. Professor Adjunto (ISEP)
9. Ph.D. Susana Maria Ribeiro e Sousa Mendes de Freitas eq. Professor Adjunto (ISEP)
10. Ph.D. Valentina Maria Fernandes Domingues eq. Professor Adjunto (ISEP)
11. Ph.D. Florinda Figueiredo Martins eq. Assistante (ISEP)
12. Ph.D. Hendrikus Petrus Antonius Nouws eq. Assistante (ISEP)
13. Ph.D. Olga Manuela Matos de Freitas eq. Assistante (ISEP)
14. Ph.D. Subramanian Viswanathan Auxiliary Investigator (REQUIMTE)
15. MSc Abel José Assunção Duarte eq. Assistante (ISEP)
16. MSc Maria João Dantas Ramalhosa Ferreira eq. Assistante (ISEP) (50% FFUP)
17. MSc Salomé Sousa Teixeira eq. Assistante (ISEP)
18. MSc José Tomás Veiga Soares de Albergaria Técnico Superior (ISEP)
19. MSc Maria Aurora Soares da Silva Técnico Superior (ISEP)
20. MSc Bruno José Rocha Pereira Técnico Superior (ISEP)
21. MSc Sérgio Alberto Cruz Monteiro de Morais Técnico Superior (ISEP)
22. MSc Paula Celeste Baptista Paíga Técnico Superior 2ª Classe (REQUIMTE)
23. BEng Maria Isabel Viana de Brito Limpo de Serra Técnico Superior (ISEP)
MEMBERS
GRAQ – ANNUAL REPORT – 2009
[ 5 ]
MEMBERS Non-permanent members
Ph.D. students
1. BEng Díonisia Maria Oliveira Castro FCT Grant: SFRH/BD/23605/2005
2. MSc Maria de Fátima de Sá Barroso 50% FFUP FCT Grant: SFRH/BD/29440/2006
3. MSc Sofia Alexandra Alves Almeida 50% FFUP FCT Grant: SFRH/BD/42509/2007
4. MSc Marta Maria Pereira da Silva Neves FCT Grant: SFRH/BD/46351/2008
5. BEng Mónica Alexandra Oliveira Dias Teixeira FCT Grant: n/a
6. Msc Antonio Vega Y de la Fuente 75% FEUP FCT Grant: n/a
7. MSc Maria Manuela Martins de Carvalho FCT Grant: n/a
8. MSc Virgínia Maria Monteiro Cruz Fernandes FCT Grant: SFRH/BD/47200/2008
9. MSc Raquel Barbosa Queirós 75% FCUP FCT Grant: SFRH/BD/49072/2008
10. BSc Débora Liliana Gutierres M. F. Soares 50% FFUP FCT Grant: SFRH/BD/48771/2008
MSc students
1. Ana Catarina Dias Vieira da Silva FFUP
2. Ana Isabel Ribeiro de Pinho ISEP
3. Bie van der Vliet Karel de Grote Hogeschool (BE)
4. Carla Alexandra Moreira Vieira ISEP
5. Cleusa Lopes da Luz ISEP
6. Diana Margarida Ferreira Pinheiro ISEP
7. Diana Paula Cunha de Aguilar de Azevedo Machado ISEP
8. Elisa Alexandra Mota Ferreira FMUP
9. Fernando Odeberto Gonçalves Pereira ISEP
10. Helena Maria Vaz de Oliveira ISEP
11. Joana Alves Ferreira da Cruz ISEP
12. Joana Gomes Martins ISEP
13. Joana Maria Cesar Veloso Ferreira ISEP
14. José Alberto Nunes da Silva Ferreira FCUP
15. José António Sousa FEUP
16. José Camilo Carvalinho Sousa Pinto ISEP
17. Magda Cristina Teixeira de Passos Guimarães University of Southern Denmark
18. Maria Adelaide Rocha de Sousa ISEP
19. Maria Isabel Mesquita Guimarães Seguro Pereira de Soares FCUP
20. Marta Gonçalves Varanda ISEP
21. Marta Madalena Marques Oliveira FFUP
22. Nuno Miguel Simões Leal Ribeiro ISEP
23. Susana Natércia Oliveira Ribeiro ISEP
24. Tânia Sofia Cardoso Ribeiro Rebelo ISEP
MEMBERS
GRAQ – ANNUAL REPORT – 2009
[ 6 ]
MEMBERS Non-permanent members (cont.) Grant holders
1. MSc Joana Rafaela Lara Guerreiro FCT project: PTDC/AGR-AAM/68359/2006
2. MSc Felismina Teixeira Coelho Moreira FCT project: PTDC/AGR-AAM/68359/2006
3. MSc Mónica Rosas da Silva FCT project: PTDC/ECM/68056/2006
4. MSc António Carlos Alves Soares FCT project: PTDC/ECM/68056/2006
5. -- Pedro Romeu da Silva Soares FCT project: BII 2008-2009
6. -- Adão Batista Martins Pinto FCT project: BII 2008-2009
7. -- Ana Raquel dos Reis Ferreira FCT project: BII 2008-2009
8. -- Laura Cristina Oliveira Sousa FCT project: BII 2008-2009
9. -- Liliana Adelina Afonso N. Almeida Truta FCT project: BII 2008-2009
10. -- Isa de Sousa Matos FCT project: BII 2008-2009
11. ..-- Marcela de Jesus da Cunha Oliveira FCT project: BII 2009-2010
12. ..-- Isabel Patrícia Ribeiro Moreira FCT project: BII 2009-2010
13. ..-- Irene Cristina de Sousa Azevedo FCT project: BII 2009-2010
RESEARCH AREAS – ANALYTICAL CHEMISTRY
GRAQ – ANNUAL REPORT – 2009
[ 7 ]
A. RESEARCH AREAS
1. ANALYTICAL CHEMISTRY
TEAM MEMBERS
Permanent Members
Cristina Maria Delerue-Matos
Maria do Carmo Veiga Fernandes Vaz
Maria Teresa Pereira de Oliva Teles Moreira
Maria Goreti Ferreira Sales
Maria Manuela Barbosa Correia
Simone Barreira Morais
Susana Maria Ribeiro e Sousa Mendes de Freitas
Valentina Maria Fernandes Domingues
Hendrikus Petrus Antonius Nouws
Subramanian Viswanathan
Abel José Assunção Duarte
Maria João Dantas Ramalhosa Ferreira
Salomé Sousa Teixeira
José Tomás Veiga Soares de Albergaria
Paula Celeste Baptista Paíga
Non-permanent members
Ph.D.
Dionísia Maria Oliveira Castro
Maria de Fátima de Sá Barroso
Sofia Alexandra Alves Almeida
Marta Maria Pereira da Silva Neves
Mónica Alexandra de Oliveira Dias Teixeira
Virgínia Maria Monteiro da Cruz Fernandes
Raquel Barbosa Queirós
Débora Liliana Gutierres Mirones F. Soares
Non-permanent members
MSc
Ana Catarina Dias Vieira da Silva
Ana Isabel Ribeiro de Pinho
Cleusa Lopes da Luz
Elisa Alexandra Mota Ferreira
Fernando Odeberto Gonçalves Pereira
Helena Maria Vaz de Oliveira
Joana Gomes Martins
José Alberto Nunes da Silva Ferreira
José António Sousa
José Camilo Carvalinho Sousa Pinto
Maria Adelaide Rocha de Sousa
Maria Isabel Mesquita G. Seguro Pereira de Soares
Marta Madalena Marques Oliveira
Tânia Sofia Cardoso Ribeiro Rebelo
Grant holders
Joana Rafaela Lara Guerreiro
Felismina Teixeira Coelho Moreira
Mónica Rosas da Silva
Laura Cristina Oliveira Sousa
Liliana Adelina Afonso N. Almeida Truta
Isa de Sousa Matos
Marcela de Jesus da Cunha Oliveira
Isabel Patrícia Ribeiro Moreira
OUTPUT INDICATORS (SUMMARY)
FCT funded projects 3
non-FCT funded projects 4
Papers (ISI) 13
Papers (non-ISI) 1
Books --
Ph.D. theses --
MSc theses 13
Conferences (international) Oral presentations 2 Poster presentations 33 Proceedings papers 1
Conferences (national) Oral presentations -- Poster presentations 13 Proceedings papers 4
Conferences (organization) 1
RESEARCH AREAS – ANALYTICAL CHEMISTRY
GRAQ – ANNUAL REPORT – 2009
[ 8 ]
The purpose of analytical chemistry is to answer the following questions: which elements and/or
compounds are present in a sample (qualitative analysis) and in which concentration (quantitative
analysis)? There is a wide variety of analytical techniques available to answer these questions.
Historically the determinations were based on direct measurements of mass and/or volume. Nowadays
the majority of determinations are based on the measurement of a large variety of properties, like, optical,
piezoelectrical, thermal, and electrochemical.
Some recent trends in analytical chemistry are the automatization and miniaturization of measuring
devices in order to speed up the analysis time and to allow point-of-care analysis. As in many areas,
nanotechnology has also been introduced in this field of study.
One of the most promising and rapidly growing areas in analytical chemistry is the development and use
of sensors based on chemical and/or biochemical mechanisms. In the construction of a sensor a selective
recognition element is coupled to a transducer. Nanotecnological approaches for the construction of the
transducer can significantly improve the selectivity and sensitivity of the analysis and greatly reduce the
measuring device. The term biosensor is used when the sensing layer is based on biochemical
recognition/binding elements. Electrochemical biosensors are used in point-of-care devices since they are
portable, simple, easy to use, cost effective and in most cases disposable (for example for the
measurement of blood glucose). The electrochemical instruments used with the biosensors have also
been miniaturized to small pocket size devices which make them applicable for home use or the doctor’s
office.
Besides the development of the analytical technique itself, sample preparation has also received much
attention, particularly regarding solid-phase- and microwave-aided extractions.
1.1. SUB-AREAS IN ANALYTICAL CHEMISTRY
In the subsequent sections a summary of several achievements in analytical chemistry in 2009 are
presented, for further reading the consultation of the published papers is recommended.
1.1.1. Quality control and authenticity of food products
Concentrations of eleven trace elements (Al, As, Cd, Cr, Co, Hg, Mn, Ni, Pb, Se, and Si) were measured
in 39 (natural and flavoured) water samples. Determinations were performed using graphite furnace
electrothermetry for almost all elements (Al, As, Cd, Cr, Co, Mn, Ni, Pb, and Si). For Se determination
hydride generation was used, and cold vapour generation for Hg. These techniques were coupled to
atomic absorption spectrophotometry. The trace element content of still or sparkling natural waters
changed from brand to brand. Significant differences between natural still and natural sparkling waters
(p < 0.001) were only apparent for Mn. The Mann–Whitney U-test was used to search for significant
differences between flavoured and natural waters. The concentration of each element was compared with
the presence of flavours, preservatives, acidifying agents, fruit juice and/or sweeteners, according to the
labelled composition. It was shown that flavoured waters generally increase the trace element content.
RESEARCH AREAS – ANALYTICAL CHEMISTRY
GRAQ – ANNUAL REPORT – 2009
[ 9 ]
The addition of preservatives and acidifying regulators had a significant influence on Mn, Co, As and Si
contents (p < 0.05). Fruit juice can also be correlated to the increase of Co and As. Sweeteners did not
provide any significant difference in Mn, Co, Se and Si content.
Macro (Ca, Mg, K, Na) and micromineral (Fe, Zn, Cu) composition of 39 waters was analysed.
Determinations were made by atomic flame spectrophotometry for macrominerals and electrothermic
atomization in graphite furnace for microminerals. Mineral contents of still or sparkling natural waters
(without flavours) changed from brand to brand. Mann–Whitney test was used to search for significant
differences between flavoured and natural waters. For that, the concentration of each mineral was
compared to the presence of flavours, preservatives, acidifying agents, fruit juice and/or sweeteners,
according to the labelled composition. The statistical study demonstrated that flavoured waters generally
have increased contents of K, Na, Fe and Cu. The added preservatives also led to significant differences
in the mineral composition. Acidifying agents and fruit juice can also be correlated to the increase of Mg,
K, Na, Fe and Cu. Sweeteners do not provide any significant difference in Ca, Mg, Fe and Zn contents.
QuEChERS method was evaluated for extraction of 16 PAHs from fish samples. For a selective
measurement of the compounds, extracts were analysed by LC with fluorescence detection. The overall
analytical procedure was validated by systematic recovery experiments at three levels and by using the
standard reference material SRM 2977 (mussel tissue). The targeted contaminants, except naphthalene
and acenaphthene, were successfully extracted from SRM 2977 with recoveries ranging from 63.5 –
110.0 % with variation coefficients not exceeding 8 %. The optimum QuEChERS conditions were the
following: 5 g of homogenised fish sample, 10 mL of ACN, agitation performed by vortex during 3 min.
Quantification limits ranging from 0.12 – 1.90 ng/g wet weight (0.30 – 4.70 µg/L) were obtained. The
optimized methodology was applied to assess the safety concerning PAHs contents of horse mackerel
(Trachurus trachurus), chub mackerel (Scomber japonicus), sardine (Sardina pilchardus) and farmed
seabass (Dicentrarchus labrax). Although benzo(a)pyrene, the marker used for evaluating the
carcinogenic risk of PAHs in food, was not detected in the analysed samples (89 individuals
corresponding to 27 homogenized samples), the overall mean concentration ranged from 2.52 ±
1.20 ng/g in horse mackerel to 14.6 ± 2.8 ng/g in farmed seabass. Significant differences were found
between the mean PAHs concentrations of the four groups.
An analytical method, based on microwave-assisted extraction and LC with diode array detection, for the
determination of six carbamate and three urea pesticides in fresh and processed tomato samples is
described. Significant parameters affecting extraction efficiency were optimized. Under optimum
microwave-assisted extraction conditions (20 mL acetonitrile, for 10 minutes, at 60 ºC), pesticides were
extracted with recoveries ranging from 57.6 to 102% (RSD < 7%). Quantification limits between 6.5 and
39.6 µg/kg were obtained. A total number of 28 different fresh tomato samples and 6 processed tomato
products were analysed. Confirmation of suspicious samples was performed by LC-MS.
RESEARCH AREAS – ANALYTICAL CHEMISTRY
GRAQ – ANNUAL REPORT – 2009
[ 10 ]
An analytical multiresidue method for the simultaneous determination of seven pesticides in fresh
vegetable samples, namely, courgette (Cucurbita pepo), cucumber (Cucumis sativus), lettuce (Lactuca
sativa, Romaine and Iceberg varieties) and peppers (Capsicum sp.) is described. The procedure, based
on microwave-assisted extraction (MAE) and analysis by liquid chromatography–photodiode array (LC–
PDA) detection was applied to four carbamates (carbofuran, carbaryl, chlorpropham and EPTC) and
three urea pesticides (monolinuron, metobromuron and linuron). Extraction solvent and the addition of
anhydrous sodium sulphate to fresh vegetable homogenate before MAE were the parameters optimised
for each commodity. Recovery studies were performed using spiked samples in the range 250 –
403 µg/kg in each pesticide. The pesticide residues were extracted using 20 mL acetonitrile at 60 ºC, for
10 min. Acceptable recoveries and RSDs were attained (overall average recovery of 77.2 % and RSDs
are lower than 11 %). Detection limits ranged between 5.8 µg/kg for carbaryl to 12.3 µg/kg for carbofuran.
The analytical protocol was applied for quality control of 41 fresh vegetable samples bought in Oporto
Metropolitan Area (North Portugal). None of the samples contained any detectable amounts of the
studied compounds.
A flow-spectrophotometric method is proposed for the routine determination of tartaric acid in wines. The
reaction between tartaric acid and vanadate in acetic media is carried out in flowing conditions and the
subsequent colored complex is monitored at 475 nm. The stability of the complex and the corresponding
formation constant are presented. The effect of wavelength and pH was evaluated by batch experiments.
The selected conditions were transposed to a flow-injection analytical system. Optimization of several
flow parameters such as reactor lengths, flow-rate and injection volume was carried out. Using optimized
conditions, a linear behavior was observed up to 1000 μg mL-1 tartaric acid, with a molar extinction
coefficient of 450 L/mg.cm and ± 1 % repeatability. Sample throughput was 25 samples per hour. The
flow-spectrophotometric method was satisfactorily applied to the quantification of tartaric acid (TA) in
wines from different sources. Its accuracy was confirmed by statistical comparison to the conventional
Rebelein procedure and to a certified analytical method carried out in a routine laboratory.
DNA-based biosensors are developed after immobilization and electrooxidation of guanine and adenine
on a glassy carbon electrode. Both the guanine and the adenine biosensors are employed for the
voltammetric detection of antioxidant capacities of flavoured waters. The method relies on monitoring the
changes of the intrinsic anodic response of the surface-confined guanine and adenine species, resulting
from its interaction with free radicals from Fenton-type reaction in absence and presence of antioxidant.
Ascorbic acid is used as standard to evaluate antioxidant capacities of samples.
1.1.2. Environmental analysis A methodology based on microwave-assisted extraction (MAE) and LC with fluorescence detection (FLD)
was investigated for the efficient determination of 15 polycyclic aromatic hydrocarbons (PAHs) regarded
as priority pollutants by the US Environmental Protection Agency and dibenzo(a,l)pyrene in atmospheric
RESEARCH AREAS – ANALYTICAL CHEMISTRY
GRAQ – ANNUAL REPORT – 2009
[ 11 ]
particulate samples. PAHs were successfully extracted from real outdoor particulate matter (PM) samples
with recoveries ranging from 81.4 ± 8.8 to 112.0 ± 1.1 %, for all the compounds except for naphthalene
(62.3 ± 18.0 %) and anthracene (67.3 ± 5.7 %), under the optimum MAE conditions (30.0 mL of ACN for
20 min at 110 ºC). No clean-up steps were necessary prior to LC analysis. LOQs ranging from
0.0054 ng/m3 for benzo(a)anthracene to 0.089 ng/m
3 for naphthalene were reached. The validated MAE
methodology was applied to the determination of PAHs from a set of real world PM samples collected in
Oporto (north of Portugal). The sum of particulate-bound PAHs in outdoor PM ranged from 2.5 and
28 ng/m3.
Seven pyrethroids (bifenthrin, fenpropathrin, k-cyhalothrin, permethrin, a-cypermethrin, fenvalerate, and
deltamethrin) were extracted from water using C18 solid-phase extraction disks, followed by gas
chromatography with an electron capture detector (GC-ECD) analysis. The limits of detection in water
samples ranged from 0.5 ng/L (fenpropathrin) to 110 ng/L (permethrin), applying the calibration graph.
The effects of different numbers of (re)utilizations of the same disks (up to four times with several
concentrations) on the recoveries of the pyrethroids were considered. The recoveries were all between 70
and 120 % after four utilizations of the same disk. There was no difference between these recoveries at a
confidence level of 95 %.
The industrial manufacturing of metallic objects results in a high level of foundry waste sands that may
contain toxic compounds such as formaldehyde. The formaldehyde content of foundry waste sands was
evaluated by liquid chromatography. Samples were collected during various steps of the industrial
processes. Results showed that the phenolic alkaline process generated waste sands with higher
formaldehyde content than the furanic process; the highest value was 7.6×10-3
% (w/w). In this work,
formaldehyde content decreased with time in all of the samples studied, revealing that most formaldehyde
was released to the occupational environment. Also research is done to assess the evidence for organic
pollutants and heavy metals in aquatic environment and food and the development of methodologies
concerning the quantification of these compounds that exists in extremely low concentration and, in
future, establish a monitoring and controlling program for them. Target analytes will be selected on the
basis of their presumable presence in the water matrices and their environmental significance and include
compounds of different sources of contamination: estrogens (domestic), pesticides (agriculture), heavy
metals and plasticizers (industrial).
1.1.3. Health and pharmaceutical analysis
Because of the mutagenic and/or carcinogenic properties, Polycyclic Aromatic Hydrocarbons (PAH), have
a direct impact on human population. Consequently, there is a widespread interest in analysing and
evaluating the exposure to PAH in different indoor environments, influenced by different emission
sources. The information on indoor PAH is still limited, mainly in terms of PAH distribution in indoor
particles of different sizes; thus, this study evaluated the influence of tobacco smoke on PM10 and PM2.5
RESEARCH AREAS – ANALYTICAL CHEMISTRY
GRAQ – ANNUAL REPORT – 2009
[ 12 ]
characteristics, namely on their PAH compositions, with further aim to understand the negative impact of
tobacco smoke on human health. Samples were collected at one site influenced by tobacco smoke and at
one reference (non-smoking) site using low-volume samplers; the analyses of 17 PAH were performed by
Microwave Assisted Extraction combined with Liquid Chromatography (MAE–LC). At the site influenced
by tobacco smoke PM concentrations were higher 650 % for PM10, and 720 % for PM2.5. When influenced
by smoking, 4 ring PAH (fluoranthene, pyrene, and chrysene) were the most abundant PAH, with
concentrations 4600 – 21000 % and 5100 – 20800 % higher than at the reference site for PM10 and
PM2.5, respectively, accounting for 49 % of total PAH (SPAH). Higher molecular weight PAH (5–6 rings)
reached concentrations 300 – 1300 % and 140 – 1700 % higher for PM10 and PM2.5, respectively, at the
site influenced by tobacco smoke. Considering 9 carcinogenic PAH this increase was 780 % and 760 %
in PM10 and PM2.5, respectively, indicating the strong potential risk for human health. As different
composition profiles of PAH in indoor PM were obtained for reference and smoking sites, those 9
carcinogens represented at the reference site 84 % and 86 % of SPAH in PM10 and PM2.5, respectively,
and at the smoking site 56 % and 55 % of SPAH in PM10 and PM2.5, respectively. All PAH (including the
carcinogenic ones) were mainly present in fine particles, which corresponds to a strong risk for
cardiopulmonary disease and lung cancer; thus, these conclusions are relevant for the development of
strategies to protect public health.
The purpose of this work was to assess the acute toxicity on male mice to a chromated copper arsenate
(CCA) solution, a widespread wood preservative used in building industry until 2002. Animals were
subcutaneously injected with CCA (7.2 mg/kg arsenic and 10.2 mg/kg chromium per body weight), CrO3
(10.2 mg/kg), As2O5 (7.2 mg/kg) and NaCl (0.9%) per se, during 48 h and 96 h, for histopathology,
histochemistry, chromium and arsenic analysis. The results showed some histopathological changes
within renal tubules lumen of CCA exposed animals (during 48 h, and 96 h), and CrO3 (for the period of
96 h). Furthermore, the renal levels of arsenic and chromium in treated animals were statistically more
evident than controls. Although, the same contents of pentavalent arsenic and hexavalent chromium were
injected into treated animals with CCA and with the prepared solutions of As2O5 and CrO3, a different
distribution of the pattern of these compounds was observed in kidneys; the arsenic concentration on
kidneys of CCA-exposed animals was much higher than those in animals exposed to As2O5 (32- and 28-
fold higher at 14 and 24h, respectively). However, the elimination of chromium seems to occur similarly in
the kidneys of animals treated with CCA and CrO3 per se. Interactions among the components of CCA
result in a marked decrease of the ability of kidney to eliminate simultaneously both analytes. The
nephrotoxicity of CCA was higher than its components per se, evidencing a possible synergetic effect.
New PVC membrane electrodes for the potentiometric determination of sulfadiazine (SDZ) were
developed. The electrodes were fabricated with conventional and tubular configurations with a graphite-
based electrical contact, and no internal reference solution. The selective membranes consist of
bis(triphenylphosphoranilidene)ammonium·SDZ (electrode A), tetraoctylammonium bromide (electrodeB),
RESEARCH AREAS – ANALYTICAL CHEMISTRY
GRAQ – ANNUAL REPORT – 2009
[ 13 ]
or iron(II)-phthalocyanine (FePC) (electrode C) electroactive materials dispersed in a PVC matrix of o-
nitrophenyl octyl ether (o-NPOE) plasticizer. The sensors A, B, and C displayed linear responses over the
concentration ranges 1.0×10–2
– 1.0×10–5
, 1.0×10–2
– 7.5×10–6
, and 3.2×10–2
– 7.0×10–6
mol/L (detection
limits of 1.09, 2.04 and 0.87 mg/mL) with anionic slopes of –57.3 ± 0.1, –46.7 ± 0.5, and –65.1 ± 0.2 mV
decade–1
, respectively. No effect from pH was observed within 4.0 – 5.5, 4.8 – 10, and 4.5 – 8,
respectively, and good selectivity was found. The sensors were applied to the analysis of
pharmaceuticals and biological fluids in steady state and in flow conditions.
Currently a nanostructured biosensor is being developed for the diagnosis of celiac disease. The
transducer part of the sensor is based on a screen-printed carbon electrode modified with carbon
nanotubes/nanofibers and gold nanoparticles. The sensing layer of the sensor is based an antibody-
antigen interaction.
1.2. OUTPUT INDICATORS
1.2.1. FCT funded projects Project reference: PTDC/AGR-AAM/68359/2006 Project title: Detection and quantification of antimicrobials in fish and in waters from
aquaculture Duration: July 2007 – June 2010 Responsible investigator: Maria Goreti Fereira Sales Principal contractor: Instituto de Ciências e Tecnologias Agrárias e Agro-Alimentares-Porto (ICETA-
Porto/UP) Participating institution(s): Instituto Nacional de Recursos Biológicos, I.P. (INRB/MADRP) Funding (total): € 131 553 Funding (ICETA): € 64 664
Project reference: PTDC/AGR-ALI/65528/2006 Project title: Evaluation of ochratoxin A exposure level of Portuguese population: bread
consumption and urine levels Duration: June 2007 – May 2010 Responsible investigador: Celeste Matos Lino (Universidade de Coimbra) Principal contractor: Universidade de Coimbra Participating institution(s): Instituto de Ciências e Tecnologias Agrárias e Agro-Alimentares-Porto (ICETA-
Porto/UP) Instituto Politécnico de Bragança Funding (total): € 74 866 Funding (ICETA): € 12 977
Project reference: PTDC/QUI/71001/2006 Project title: SenRONS - Development of optical fiber sensors for the determination of reactive
oxygen (ROS) and nitrogen (RNS) species in biological systems Duration: January 2008 – December 2010 Responsible investigador: Joaquim Carlos Gomes Esteves da Silva (Universidade do Porto) Principal contractor: Associação para o Desenvolvimento da Faculdade de Ciências (ADFC/FC/UP) Participating institution(s): Instituto de Ciências e Tecnologias Agrárias e Agro-Alimentares-Porto (ICETA-
Porto/UP) Universidade de Coimbra (UC) Instituto de Engenharia de Sistemas e Computadores do Porto (INESC
Porto/FE/UP) Funding (total): € 104 200 Funding (ICETA): € 3 900
RESEARCH AREAS – ANALYTICAL CHEMISTRY
GRAQ – ANNUAL REPORT – 2009
[ 14 ]
1.2.2. non-FCT funded projects Project reference: CESPU01 Project title: Monitorização de triazinas em águas e no homem. Mecanismo patogénico. Duration: January 2009 – December 2010 Responsible investigator: Mónica Alexandra de Oliveira Dias Teixeira Funding source: CESPU Funding (total): € 5 000 Funding (ICETA): € 5 000
Project reference: ------- Project title: Protective role of antioxidants at DNA oxidative damage: biosensors, mechanism
and screening Duration: January 2008 – December 2009 Responsible investigador: Maria Goreti Ferreira Sales Principal contractor: Instituto de Ciências e Tecnologias Agrárias e Agro-Alimentares - Porto (ICETA) Participating institution(s): Centro de Química Fina e Biotecnologia da Universidade Nova de Lisboa – CQFB. Funding source: REQUIMTE Funding (total): € 8 000 Funding (ICETA): € 4 000
Project reference: ------- Project title: Avaliação da Contaminação de Águas Residuais Hospitalares Duration: January 2009 – December 2009 Responsible investigador: Conceição Montenegro (FFUP) Principal contractor: Instituto de Ciências e Tecnologias Agrárias e Agro-Alimentares - Porto (ICETA) Funding source: University of Porto Funding (total): € 4 000 Funding (ICETA): € 4 000
Project reference: ------- Project title: Componentes da fracção azotada do leite - influência na qualidade e implicações
na saúde dos consumidores Duration: January 2009 – December 2009 Responsible investigador: Beatriz Oliveira (FFUP) Principal contractor: Instituto de Ciências e Tecnologias Agrárias e Agro-Alimentares - Porto (ICETA) Funding source: University of Porto Funding (total): € 4 000 Funding (ICETA): € 4 000
1.2.3. Papers (ISI)
1. K. Slezakova, D. Castro, M.C. Pereira, S. Morais, C. Delerue-Matos, M.C. Alvim-Ferraz
Influence of tobacco smoke on carcinogenic PAH composition in indoor PM10 and PM2.5 Atmospheric Environment 43 (40) (2009) 6376-6382.
2. M.F. Barroso, S. Ramos, M.T. Oliva-Teles, C. Delerue-Matos, M.G.F. Sales, M.B.P.P. Oliveira Survey of trace elements (Al, As, Cd, Cr, Co, Hg, Mn, Ni, Pb, Se, and Si) in retail samples of flavoured and bottled waters Food Additives and Contaminants Part B - Surveillance 2 (2) (2009) 121-130.
3. Maria João Ramalhosa, Paula Paíga, Simone Morais, Cristina Delerue-Matos, Maria Beatriz Prior Pinto Oliveira Analysis of polycyclic aromatic hydrocarbons in fish: evaluation of a quick, easy, cheap, effective, rugged, and safe extraction method Journal of Separation Science 32 (20) (2009) 3529-3538.
4. Rita Cerejeira Matos, Catarina Vieira, Simone Morais, Maria de Lourdes Pereira, Júlio Pedrosa Nephrotoxicity effects of the wood preservative chromium copper arsenate on mice: Histopathological and quantitative approaches Journal of Trace Elements in Medicine and Biology 23 (3) (2009) 224-230.
RESEARCH AREAS – ANALYTICAL CHEMISTRY
GRAQ – ANNUAL REPORT – 2009
[ 15 ]
5. Sandra S.T. Bastos, Paula A.R. Tafulo, Raquel B. Queiros, Cristina D. Matos, M. Goreti F. Sales Rapid Determination of Tartaric Acid in Wines Combinatorial Chemistry & High Throughput Screening 12 (7) (2009) 712-722.
6. M. Fátima Barroso, Aurora Silva, Sandra Ramos, M.T. Oliva-Teles, Cristina Delerue-Matos, M. Goreti F. Sales, M.B.P.P. Oliveira Flavoured versus natural waters: Macromineral (Ca, Mg, K, Na) and micromineral (Fe, Cu, Zn) contents Food Chemistry 116 (2) (2009) 580-589.
7. A.H. Kamel, S.A.A. Almeida, M.G.F. Sales, F.T.C. Moreira Sulfadiazine-Potentiometric Sensors for Flow and Batch Determinations of Sulfadiazine in Drugs and Biological Fluids Analytical Sciences 25 (3) (2009) 365-371.
8. V. Domingues, A. Alves, M. Cabral, C. Delerue-Matos Use and reuse of SPE disks for the determination of pyrethroids in waters by GC-ECD Analytical Letters 42 (4) (2009) 706-726.
9. M.T. Oliva-Teles, P. Paíga, C.M. Delerue-Matos, M.C.M. Alvim-Ferraz Evaluation of Formaldehyde in Foundry Waste Sands Using Liquid Chromatography Analytical Letters 42 (3) (2009) 492-504.
10. P. Paíga, S. Morais, M. Correia, C. Delerue-Matos, A. Alves Screening of Carbamates and Ureas in Fresh and Processed Tomato Samples using Microwave-Assisted Extraction and Liquid Chromatography Analytical Letters 42 (2) (2009) 265-283.
11. D. Castro, K. Slezakova, M.T. Oliva-Teles, C. Delerue-Matos, M.C. Alvim-Ferraz, S. Morais, M.C. Pereira Analysis of Polycyclic Aromatic Hydrocarbons in Atmospheric Particulate Samples by Microwave-assisted Extraction and Liquid Chromatography Journal of Separation Science 32 (4) (2009) 501-510.
12. R.C. Matos, C. Vieira, S. Morais, M.L. Pereira, J.P. de Jesus Nephrotoxicity of CCA-treated wood: a comparative study with As2O5 and CrO3 on mice Environmental Toxicology and Pharmacology 27 (2) (2009), 259-263.
13. P. Paíga, S. Morais, M. Correia, C. Delerue-Matos, A. Alves Determination of Carbamate and Urea Pesticide Residues in Vegetables Using Microwave-assisted Extraction and Liquid Chromatography International Journal of Environmental Analytical Chemistry 89 (3) (2009), 199-210.
1.2.4. Papers (non-ISI)
1. Correia, M., Delerue-Matos, C., Beatriz Oliveira
Avaliação de nitratos e nitritos em vegetais Revista de Segurança e Qualidade Alimentar, N. 7 (2009), 14-16.
1.2.5. Books
No books were published during 2009.
1.2.6. Ph.D. theses
No Ph.D. theses were concluded during 2009.
1.2.7. MSc theses
1. Ana Catarina Dias Vieira da Silva Evaluation of the levels of Hg, Cd, Pb and As in fish (sardine, horse mackerel and mackerel) FFUP, February 2009.
2. José António Sousa Benzene in Indoor Air and Exterior Air FEUP, April 2009.
3. Helena Maria Vaz de Oliveira Development of sensors for antibiotics ISEP, July 2009.
RESEARCH AREAS – ANALYTICAL CHEMISTRY
GRAQ – ANNUAL REPORT – 2009
[ 16 ]
4. Tânia Sofia Cardoso Ribeiro Rebelo Implementation, validation and technical-economic analysis of some analytical parameters in the control of water ISEP, July 2009.
5. José Alberto Nunes da Silva Ferreira Determination of pesticides in lettuce and irrigation water in the vulnerable zone of the free aquifer of Esposende FCUP, August 2009.
6. Marta Madalena Marques Oliveira Evaluation of the mineral composition of soluble coffee and coffee substitutes FFUP, September 2009.
7. Maria Isabel Mesquita Guimarães Seguro Pereira Soares Development of methodologies for analysis of metals in natural waters by continuous-source atomic absorption spectroscopy FCUP, October 2009.
8. Felismina Teixeira Coelho Moreira Determination of Norfloxacin in aquaculture FCUP, November 2009.
9. Joana Rafaela Lara Guerreiro Determination of chlortetracycline residues in aquaculture FCUP, November 2009.
10. Joana Gomes Martins Development of analytical methodologies for the determination of pesticides in wines of the Douro and Port wines ISEP, November 2009.
11. Fernando Odeberto Gonçalves Pereira Voltammetric analysis of ciprofloxacin – application to pharmaceuticals and remediation ISEP, December 2009.
12. Cleusa Lopes da Luz Evaluation of Concentration of Minerals in Fish ISEP, December 2009.
13. Elisa Alexandra Mota Ferreira Evaluation of different disinfection treatments of lettuce: A chemical and toxicological approach FCNAUP, December 2009.
1.2.8. International conferences
1.2.8.1. Oral presentations
1. Castro D., Slezakova K., Delerue-Matos C., Alvim-Ferraz M.C., Morais S., Pereira M.C. Contribution of traffic and tobacco smoke in the distribution of Polycyclic aromatic hydrocarbons on outdoor and indoor PM25 11th International Conference on Environmental Science and Technology CEST2009, 2009, Chania, Crete, Greece.
2. Marta Maria Pereira da Silva Neves, Maria Begoña González-Garcia, Hendrikus Petrus Antonius Nouws, Maria Alice dos Santos Silva Gomes Martins, Cristina Delerue-Matos, Agustín Costa-García A novel transducer surface: screen-printed carbon electrodes modification with carbon-nanostructures and gold nanoparticles III Workshop Nanociencia y Nanotecnología Analíticas, 2009, Oviedo, Spain, Communication XXX.
3. L. Pinho, D. Castro, A. Begonha, S. Morais, M.C. Pereira, M.C. Delerue-Matos, M.C. Alvim-Ferraz, Films Negros en Edifícios Históricos de Oporto: Caracterización y Experiencias de Limpieza 1º Congresso Iberoamericano e VIII Jornada de Técnicas de Restauração e Conservação do Patrimônio – COIBRECOPA, 2009, La Plata, Argentina.
RESEARCH AREAS – ANALYTICAL CHEMISTRY
GRAQ – ANNUAL REPORT – 2009
[ 17 ]
1.2.8.2. Poster presentations
1. Mónica Rosas, Teresa Oliva-Teles, Valentina Domingues, Cristina Delerue-Matos, António Crispim Development of a methodology for evaluation of free-formaldehyde in leather Fourth International Symposium on the Separation and Characterization of Natural and Synthetic Macromolecules, P004, 2009, Amsterdam, Netherlands.
2. M.J. Ramalhosa, P. Paíga, S. Morais, M.B.P.P. Oliveira, C. Delerue-Matos Polycyclic aromatic hydrocarbons in wild and cultured fishes 6th European Conference on Marine Natural Products PC35, 2009, Porto, Portugal.
3. Felismina T.C. Moreira, M.Goreti F. Sales Biomimetric sensors for leucomalachite green 6th European Conference on Marine Natural Products PC72, 2009, Porto, Portugal.
4. Ayman H. Kamel, Felismina T.C. Moreira, J. Rafaela L. Guerreiro, M. Goreti F. Sales New enrofloxacin sensors for aquaculture environment 6th European Conference on Marine Natural Products PC89, 2009, Porto, Portugal.
5. M.J. Ramalhosa, P. Paíga, S. Morais, M.B.P.P. Oliveira, C. Delerue-Matos Analysis of priority polycyclic aromatic hydrocarbons in marine fish EuroAnalysis 2009, P033-A1, 2009, Innsbruck, Austria.
6. A.C. Silva, S. Morais, C. Delerue-Matos, M.B.P.P. Oliveira Heavy metal levels in muscle tissue of hurse mackerel (Trachurus Trachurus) EuroAnalysis 2009, P036-A1, 2009, Innsbruck, Austria.
7. R.C. Alves, I.M.C. Almeida, S. Casal, C. Delerue-Matos, MBPP. Oliveira Method development for daidzein, genistein and formononetin quantification in coffee EuroAnalysis 2009, P065-A1, 2009, Innsbruck, Austria.
8. J.R.L. Guerreiro, M.G.F. Sales Chlortetracycline-imprinted materials for its potentiometric determination in food and biological samples EuroAnalysis 2009, P122-A1, 2009, Innsbruck, Austria.
9. F.T.C. Moreira, A.H. Kamel, M.G.F. Sales Man-Tailored biomimetric sensor of molecularly-imprinted materials for the potentiometric measurement of oxytetracycline EuroAnalysis 2009, P123-A1, 2009, Innsbruck, Austria.
10. V.C. Fernandes, A. Dequeant, V.F. Domingues, N. Mateus, C. Delerue-Matos Comparison of different QuEChERS for organochlorine pesticide determination in strawberries EuroAnalysis 2009, P052-A2, 2009, Innsbruck, Austria.
11. M. Oliveira, S. Morais, S. Casal, C. Delerue-Matos, M.B.P.P. Oliveira Application of high resolution continuum source flame atomic absorption spectrometry to sequential analysis of Fe and Mn in instant coffee substitutes EuroAnalysis 2009, P053-A2, 2009, Innsbruck, Austria.
12. Luz, A.C. Silva, C. Delerue-Matos, S. Morais, M.B.P.P. Oliveira Macrominerals composition of sardine (Sardine Pilchardus) by microwave-assisted digestion and flame atomic absorption spectrometry EuroAnalysis 2009, P064-A2, 2009, Innsbruck, Austria.
13. T.J.R. Fernandes, E. Mendes, S. Casal, C. Delerue-Matos, M.B.P.P. Oliveira Fat content and fatty acid composition of traditional dry cured sausages from Portugal EuroAnalysis 2009, P067-A2, 2009, Innsbruck, Austria.
14. D. Castro, C. Delerue-Matos, M. C. Alvim-Ferraz, S. Morais, M. C. Pereira Microwave-Assisted extraction of polycyclic aromatic hydrocarbons from polyurethane foam adsorbents EuroAnalysis 2009, P054-B1, 2009, Innsbruck, Austria.
15. D. Castro, C. Delerue-Matos, M. C. Alvim-Ferraz, S. Morais, M. C. Pereira Gas-Particle concentration and distribution of polycyclic aromatic hydrocarbons at an urban atmosphere EuroAnalysis 2009, P055-B1, 2009, Innsbruck, Austria.
16. C. Pinho, P. Gameiro, C. Delerue-Matos, C. Pizarro, C. Coelho, A. Heitor, A. Tavares, C. Mansilha Analysis of oils and greases in portuguese bathing waters. Implementation and validation of a FT-IR method EuroAnalysis 2009, P069-B1, 2009, Innsbruck, Austria.
RESEARCH AREAS – ANALYTICAL CHEMISTRY
GRAQ – ANNUAL REPORT – 2009
[ 18 ]
17. I. Seguro, J. Pinto, C. Mansilha, C. Delerue-Matos, M.T. Oliva-Teles, P. Gameiro Analysis of metals in natural waters by high-Resolution continuum source atomic absorption spectrometry EuroAnalysis 2009, P077-B1, 2009, Innsbruck, Austria.
18. C. Delerue-Matos, H.P.A. Nouws, M.M.P.S Neves Carbon surfaces for the oxidative quantification of pravastatin: glassy-carbon vs. SPCE EuroAnalysis 2009, P094-B1, 2009, Innsbruck, Austria.
19. D. Castro, L. Pinho, M.C. Alvim-Ferraz, C. Delerue-Matos, A. Begonha, S. Morais, M.C. Pereira Characterization of the black cruts composition of an historic monument exposed to urban atmospheric pollution EuroAnalysis 2009, P107-B1, 2009, Innsbruck, Austria.
20. A.M.M. Sousa, S. Morais, C. Delerue-Matos, Maria P. Gonçalves Optimization of native agar from the red seaweed Gracilaria Vermiculophylla by microwave-assisted extraction using response surface methodology EuroAnalysis 2009, P162-B1, 2009, Innsbruck, Austria.
21. J.R.L. Guerreiro, A.H. Kamel, M.G.F. Sales FIA potentiometric system based on periodate polymeric membrane sensors for the assessment of ascorbic acid in commercial drinks EuroAnalysis 2009, P034-B1, 2009, Innsbruck, Austria.
22. F.T.C. Moreira, G.G. Aguilar, M.G.F. Sales New sulfadiazine-selective sensors of molecularly imprinted sol-gel material EuroAnalysis 2009, P102-B1, 2009, Innsbruck, Austria.
23. M.F. Barroso, N. de-los-Santos-Álvarez, M.J. Lobo-Castanon, A.J. Miranda-Ordieres, M.G. Ferreira Sales, M.B.P.P. Oliveira, C. Delerue-Matos Investigations on the electrocatalytic assessment of antioxidant capacity using a DNA-Modified carbon paste electrode EuroAnalysis 2009, P081-B2, 2009, Innsbruck, Austria.
24. J.R.L. Guerreiro, M.G.F. Sales Selective recognition in potentiometric transduction of amoxicillin by molecularly-imprinted materials EuroAnalysis 2009, P097-B2, 2009, Innsbruck, Austria.
25. F.T.C. Moreira, G.G. Aguilar, M.G.F. Sales Novel potentiometric sensors of ion-imprinted polymers for specific binding of iron and potentiometric transduction EuroAnalysis 2009, P098-B2, 2009, Innsbruck, Austria.
26. Dionisia Castro, Cristina Delerue-Matos, M.C. Alvim-Ferraz, Simone Morais, Maria C. Pereira Impact of tobacco smoke on polyclic aromatic hydrocarbons levels in indoor PM2.5 ECNIS International Workshop biomarkers and Cancer, 2009, P7, 2009, Porto, Portugal.
27. V.C. Fernandes, V.F. Domingues, N. Mateus, C. Delerue-Matos Organochlorine pesticides and biological evaluation in strawberries obtained from organic farming and integrated pest management farming New challenges in Food Preservation, P188, 2009, Budapeste, Hungria.
28. E. Ferreira, V.F. Domingues,C. Calhau, C. Delerue-Matos Evaluation of different disinfecting treatments of lettuce: a chemical approach New challenges in Food Preservation, P194, 2009, Budapeste, Hungria.
29. M. Fátima Barroso, J. Paulo Noronha, M. Goreti F. Sales, Cristina Delerue-Matos, M. Beatriz P.P. Oliveira Development of a DNA-modified sensor to evaluate the total antioxidant capacity of flavoured waters 4th International Symposium on recent advances in food analysis, N-23, 2009, Prague, Czech Republic.
30. S. Duarte, J. Bento, A. Pena, C.M. Lino, J.A. Pereira, C. Delerue-Matos, T. Oliva-Teles, S. Morais, M. Correia, M.B.P.P. Oliveira Ochratoxin A contamination of bread-Portugal nationwide survey during the winter 2007/2008 4th International Symposium on recent advances in food analysis, G-7, 2009, Prague, Czech Republic.
31. Manuela Correia, Sandrine Eap, Artur Dias, Cristina Delerue-Matos Head-space solid-phase microextraction for the determination of selected pesticides in water and apple samples using gas chromatography-electron capture detection 4th International Symposium on recent advances in food analysis, E-1, 2009, Prague, Czech Republic.
RESEARCH AREAS – ANALYTICAL CHEMISTRY
GRAQ – ANNUAL REPORT – 2009
[ 19 ]
32. S. Duarte, J. Bento, A. Pena, C.M. Lino, J.A. Pereira, C. Delerue-Matos, T. Oliva-Teles, S. Morais, M. Correia, M.B.P.P. Oliveira, S. Casal Ochratoxin A content in urine from Porto inhabitants: is there a relationship with season? 4th International Symposium on recent advances in food analysis, G-6, 2009, Prague, Czech Republic.
33. M.M.P. da S. Neves, M.B. González García, C. Delerue-Matos, A. Costa García Superficies nanoestructuradas modificadas con estreptavidina como transductores de biosensores XXX Reunión del Grupo de Electroquímica de la RSEQ y del XI Encontro Ibérico de Electroquímica. 2009. Tenerife, Spain.
34. S.A.A. Almeida, A.M. Heitor, M.C.B.S.M. Montenegro, M.G.F.Sales Selective sensors for sulfadiazine potentiometric transduction 23
rd Eurosensors Conference, PX, 2009, Lausanne, Switzerland.
1.2.8.3. Proceedings papers
1. S.A.A. Almeida, A.M. Heitor, M.C.B.S.M. Montenegro, M.G.F.Sales Selective sensors for sulfadiazine potentiometric transduction Proceedings of the Eurosensors xxiii Conference, Procedia Chemistry 1 (1) 1031-1034 (2009).
2. D. Castro, K. Slezakova, C. Delerue-Matos, M. C. Alvim-Ferraz, S. Morais, M. C. Pereira Contribution of Traffic and Tobacco Smoke in The Distribution of Polycyclic Aromatic Hydrocarbons on Outdoor and Indoor PM2.5
Proceedings of the CEST2009, Chania, Crete, Greece, A131-137
3. L. Pinho, D. Castro, A. Begonha, S. Morais, M.C. Pereira, M.C. Delerue-Matos, M.C. Alvim-Ferraz Films Negros en Edifícios Históricos de Oporto: Caracterización y Experiencias de Limpieza Proceedings of the 1º Congresso Iberoamericano e VIII Jornada de Técnicas de Restauração e Conservação do Patrimônio – COIBRECOPA, 2009, La Plata, Argentina, 1-13.
4.
1.2.9. National conferences
1.2.9.1. Oral presentations
No oral presentations in national conferences were made during 2009.
1.2.9.2. Poster presentations
1. Almeida, R. Coelho, M.J. Ramalhosa, E. Mendes, P. Paíga, S. Casal, S. Morais, C. Delerue-Matos, M.B.P.P. Oliveira Characterization of the fatty acid profiles of sardine and chub mackerel II Encontro de Jovens Investigadores da Universidade do Porto, 2009, Porto, Portugal, pp.220.
2. M. Oliveira, S. Morais, S. Casal, C. Delerue-Matos, M.B.P.P. Oliveira Determination of Ca and Mg in instant coffee substitutes by high resolution continuum source II Encontro de Jovens Investigadores da Universidade do Porto, 2009, Porto, Portugal, pp.224.
3. J. Ferreira, V. Domingues, N. Mateus, C. Delerue-Matos Determination of pesticides in irrigation water using SPE and GC-ECD II Encontro de Jovens Investigadores da Universidade do Porto, 2009, Porto, Portugal, pp.226.
4. C. Luz, A.C. Silva, A. Novo, E. Pinho, S. Conceição, S. Morais, C. Delerue-Matos, M.B.P.P. Oliveira Arsenic analysis of chub mackerel muscle tissue II Encontro de Jovens Investigadores da Universidade do Porto, 2009, Porto, Portugal, pp.228.
5. A.C. Silva, S. Morais, C. Delerue-Matos, M.B.P.P. Oliveira Biometric characteristics of northeast Atlantic Ocean sardine (sardine pilchardus) and horse macherel (Trachurus trachurus) II Encontro de Jovens Investigadores da Universidade do Porto, 2009, Porto, Portugal, pp. 267.
6. P. Martins, D. Direito, N. Simões, P. Paíga, S. Morais, M. J. Ramalhosa, C. Delerue-Matos, M.B.P.P. Oliveira Microwave-assisted extraction of fat fishes II Encontro de Jovens Investigadores da Universidade do Porto, 2009, Porto, Portugal, pp.327.
7. J. Ferreira, A.M.M. Sousa, H. K. Souza, S. Morais, C. Delerue-Matos, M. P. Gonçalves Rheological and UV properties of WPI/agar systems II Encontro de Jovens Investigadores da Universidade do Porto, 2009, Porto, Portugal, pp.350.
RESEARCH AREAS – ANALYTICAL CHEMISTRY
GRAQ – ANNUAL REPORT – 2009
[ 20 ]
8. Morais S., Direito D., Simões N., Martins P., Ramalhosa M.J., Paíga P., Delerue-Matos C., Oliveira M.B.P.P. Comparison of several extraction procedures for lipid determination in fish 9º Encontro Quimica dos Alimentos P37, 2009, Angra do Heroismo, Açores, Portugal.
9. Barroso M.F., Ramos S., Delerue-Matos C., Sales M.F., Oliveira M.B.P.P. Aguas naturais versus aromatizadas: Influência dos ingredientes adicionados na composição mineral 9º Encontro Quimica dos Alimentos P42, 2009, Angra do Heroismo, Açores, Portugal.
10. Silva A.C., Morais S., Delerue-Matos C., Oliveira M.B.P.P. Determinação do teor de mercúrio e cádmio em cavala (Scomber japonicus) 9º Encontro Quimica dos Alimentos P154, 2009, Angra do Heroismo, Açores, Portugal.
11. Ramalhosa M.J., Paíga P., Morais S., Delerue-Matos C., Oliveira M.B.P.P One step microwave-assisted alkaline digestion and extration of PAHs from fishes 9º Encontro Quimica dos Alimentos P155, 2009, Angra do Heroismo, Açores, Portugal.
12. C. Mansilha, A. Tavares, A. Melo, I. Ferreira, O. Pinho, V. Domingues, P. Gameiro Detection and quantification of selected endocrine disrupters in drinking waters supplies in the north of Portugal 6º Encontro Nacional de Cromatografia, 2009, P-1, 2009, Madeira, Portugal.
13. Débora Soares, Manuela Correia, Cristina Delerue-Matos, M. Beatriz P.P. Oliveira Analysis of selected pesticides in bovine milk by dispersive solid-phase extraction pollowed by gas chromatography-electron capture detection 6º Encontro Nacional de Cromatografia, P-53, 2009, Madeira, Portugal.
1.2.9.3. Proceedings papers
1. Morais S., Direito D., Simões N., Martins P., Ramalhosa M.J., Paíga P., Delerue-Matos C., Oliveira M.B.P.P. Comparison of several extraction procedures for lipid determination in fish Proceedings of the 9º Encontro Quimica dos Alimentos, CD-ROM version, (2009).
2. Ramalhosa M.J., Paíga P., Morais S., Delerue-Matos C., Oliveira M.B.P.P One step microwave-assisted alkaline digestion and extration of PAHs from fishes Proceedings of the 9º Encontro Quimica dos Alimentos, CD-ROM version, (2009).
3. Barroso M.F., Ramos S., Delerue-Matos C., Sales M.F., Oliveira M.B.P.P. Aguas naturais versus aromatizadas: Influência dos ingredientes adicionados na composição mineral Proceedings of the 9º Encontro Quimica dos Alimentos, CD-ROM version, (2009).
4. Silva A.C., Morais S., Delerue-Matos C., Oliveira M.B.P.P. Determinação do teor de mercúrio e cádmio em cavala (Scomber japonicus) Proceedings of the 9º Encontro Quimica dos Alimentos, CD-ROM version, (2009).
1.3. OTHER ACTIVITIES
Organization of conferences
On the 2nd and 3th of March of 2009 a seminar entitled "From Security to Food Quality" (“Da Segurança
à Qualidade do Alimento”) was organized at ISEP and had the following objectives:
i) start a "culture of quality" in students, as potential employees of the food industry and just as
ordinary consumers;
ii) confront the students with the idea of quality and strategies that could be adopted by different
industries and small food producers
iii) contact with different ways to implement safety measures and guarantee quality of products.
The seminar was a large success, with around 400 participants.
RESEARCH AREAS – ANALYTICAL CHEMISTRY
GRAQ – ANNUAL REPORT – 2009
[ 21 ]
Internationalization
Co-orientation with the University of Léon (Spain) of the PhD studies of Mónica Alexandra Oliveira Dias
Teixeira.
Co-orientation with the University of Oviedo (Spain) of the PhD studies of Marta Maria Pereira da Silva
Neves.
Collaboration with the University of Oviedo (Spain) and the University of Pernambuco (Brasil) of the PhD
studies of Maria de Fátima de Sá Barroso (FFUP).
Governmental funding (pre-graduation)
In 2008 and 2009 7 grants from the “Concurso de Bolsas de Integração na Investigação para 5000
estudantes do Ensino Superior” (FCT) were given to the following students:
1. Adão Batista Martins Pinto, Sistema de apoio ao tratamento e gestão de resíduos laboratoriais.
2. Ana Raquel dos Reis Ferreira, Bioremediação de solos.
3. Laura Cristina Oliveira Sousa, Desenvolvimento de metodologia para a análise de ocratoxina A por
cromatografia líquida com detecção por espectrometria de massa.
4. Liliana Adelina Afonso N. Almeida Truta, Sistemas Automáticos de Análise: Aplicação ao Método TRAP.
5. Isa de Sousa Matos, Investigação de métodos electroquímicos para o doseamento de antidepressivos em
formulações farmacêuticas.
6. Marcela de Jesus da Cunha Oliveira, em curso.
7. Isabel Patrícia Ribeiro Moreira, em curso.
Launched in June 1996, the Ciência Viva programme is the contribution of the Ministry of Science and
Technology to the promotion of a scientific and technological culture among the Portuguese population. In
the sub-category “Science in the Holidays” 3 programs, with the duration of 1 week (40 hours) were
organized: “Análise Química de Produtos Farmacêuticos”, “Segurança à tua mesa”, “Crime Sob
Investigação no ISEP”.
In cooperation with a local professional high school (Escola Secundária Infante D. Henrique), 8 students
realized a professional training period of 160 hours:
1. Carlos Manuel Teixeira Amorim, Análise de antibióticos por potenciometria - Tetraciclina.
2. Cátia Maria Oliveira da Silva Carvalho, Determinação da gordura total em carapau recorrendo a vários
métodos.
3. Cristiana Silva, Determinação de ocratoxina no pão.
4. Joana Raquel da Silva Alves, Determinação de antibióticos por potenciometria - Clorpromazina.
5. Patrícia Alexandra Santos Pacheco, Determinação do pesticida carbaril em fezes de rato e determinação de
pesticidas organoclorados em amostras de morangos.
6. Rui Nuno Magalhães Brandão da Silva, Determinação de fósforo em cafés.
7. Sara Eduarda da Costa Gonçalves, Determinação da gordura total em sardinha recorrendo a vários métodos.
8. Vânia Alexandra Oliveira Marques, Determinação de nitratos e nitritos em vegetais.
RESEARCH AREAS – ANALYTICAL CHEMISTRY
GRAQ – ANNUAL REPORT – 2009
[ 22 ]
In cooperation with a local professional high school (Escola Secundária Infante D. Henrique), 2 students
realized a professional training period of 240 hours:
1. Andreia Patrícia Oliveira Toriz, Nitratos e nitritos em alfaces.
2. Gustavo Vilaça Vale, Determinação de fósforo em peixe.
1.4. FUTURE RESEARCH Approved funding (projects to be started in 2010):
PTDC/AGR-AAM/102316/2008, “Cephalopods: -Benefits and risks of consumption; -Evaluation of biomarkers
responses to organic pollution”, January 2010 - December 2012, € 80.296.
PTDC/AGR-AAM/102447/2008, “Spent coffee grounds: horticultural recovering program and implications in the
vegetables quality and safety”, January 2010 - December 2012, € 64.548.
Pending funding (projects submitted in 2009):
PTDC/AAC-AMB/112342/2009, “Endocrine disruptors and pesticides environmental pollution. An integrated risk
analysis approach”, € 134.090.
PTDC/AGR-ALI/111753/2009, “Organic farmed products versus others agricultural pratices. Strawberries as a case
study”, € 71.956.
PTDC/AGR-ALI/114303/2009, “TraceNutALL - Tracing tree nut allergens for improving the safety of food chain:
development of novel analytical methodologies and effect of processing on allergen detection”, € 186.768.
PTDC/AGR-ALI/114782/2009, “Nanobiosensor for rapid detection of brucella in milk and other dairy products”, €
199.188
PTDC/AGR-ALI/115070/2009, “SafeBio-Leite ao longo da vida humana: segurança e compostos bioactivos do
recém-nascido ao sénior”, € 123.332.
PTDC/MAR/113739/2009, “PPFISH – Aquatic species under psicopharmaceuticals neuroendocrine effects”, €
23.210.
PTDC/QUI-BIQ/115330/2009, “Development of a novel nanostructured electrochemically-based transducer surface:
application in the construction of immunosensors for the diagnosis of celiac disease and quality control of gluten-free
products”, € 124.157.
PTDC/SAU-ENB/114786/2009, “Nano-electrode arrays Biosensor for Early and Decentralized Breast-Cancer
Diagnosis”, € 171.270.
PTDC/ SAU-SAP/ 111921/ 2009, “Occupational Exposure and Environmental Impact of Polycyclic Aromatic
Hydrocarbons: Influence of Forest Fires”, € 67.012.
PTDC/AGR-ALI/114319/2009, “Propriedades antioxidantes dos Vinhos Verdes: autenticidade, caracterização e
intensificação”, € 47.234.
RESEARCH AREAS – ENVIRONMENTAL CONTROL AND REMEDIATION
GRAQ – ANNUAL REPORT – 2009
[ 23 ]
2. ENVIRONMENTAL CONTROL AND REMEDIATION
TEAM MEMBERS
Permanent Members
Cristina Maria Delerue-Matos
Maria Teresa Pereira de Oliva Teles Moreira
Maria Conceição Carvalho Benta de Oliveira Neves
Sónia Adriana Ribeiro da Cunha Figueiredo
Valentina Maria Fernandes Domingues
Florinda Figueiredo Martins
Olga Manuela Matos de Freitas
José Tomás Veiga Soares de Albergaria
Maria Aurora Soares da Silva
Bruno José Rocha Pereira
Sérgio Alberto Cruz Monteiro de Morais
Paula Celeste Baptista Paíga
Maria Isabel Viana de Brito Limpo de Serra
Non-permanent members
Ph.D.
Antonio Vega Y de la Fuente
Maria Manuela Martins de Carvalho
Virgínia Maria Monteiro Cruz Fernandes
Non-permanent members
MSc
Bie van der Vliet
Carla Alexandra Moreira Vieira
Diana Margarida Ferreira Pinheiro
Diana Paula Cunha de Aguilar de Azevedo Machado
Joana Alves Ferreira da Cruz
Joana Maria Cesar Veloso Ferreira
Magda Cristina Teixeira de Passos Guimarães
Marta Gonçalves Varanda
Nuno Miguel Simões Leal Ribeiro
Susana Natércia Oliveira Ribeiro
Grant holders
Mónica Rosas da Silva
António Carlos Alves Soares Pedro Romeu da Silva Soares
Adão Batista Martins Pinto
Ana Raquel dos Reis Ferreira
Irene Cristina de Sousa Azevedo
OUTPUT INDICATORS (SUMMARY)
FCT funded projects 1
non-FCT funded projects 2
Papers (ISI) 5
Papers (non-ISI) --
Books --
Ph.D. theses --
MSc theses 10
Conferences (international)
Oral presentation -- Poster presentation 17 Proceedings papers 3
Conferences (national)
Oral presentation -- Poster presentation -- Proceedings papers --
Conferences (organization) --
RESEARCH AREAS – ENVIRONMENTAL CONTROL AND REMEDIATION
GRAQ – ANNUAL REPORT – 2009
[ 24 ]
2.1. SUB-AREAS IN ENVIRONMENTAL CONTROL AND REMEDIATION
In the subsequent sections a summary of several achievements in environmental control and remediation
in 2009 are presented, for further reading the consultation of the published papers is recommended.
2.1.1. Waste management and toxicological evaluation
The treatment efficiency of laboratory wastewaters was evaluated and ecotoxicity tests with Chlorella
vulgaris were performed on them to assess the safety of their environmental discharge. For chemical
oxygen demand wastewaters, chromium (VI), mercury (II) and silver were efficiently removed by chemical
treatments. A reduction of ecotoxicity was achieved; nevertheless, an EC50 (effective concentration that
causes a 50% inhibition in the algae growth) of 1.5% (v/v) indicated still high level of ecotoxicity. For
chloride determination wastewaters, an efficient reduction of chromium and silver was achieved after
treatment. Regarding the reduction of ecotoxicity observed, EC50 increased from 0.059% to 0.5%, only a
0.02% concentration in the aquatic environment would guarantee no effects. Wastewaters containing
phenanthroline/iron (II) complex were treated by chemical oxidation. Treatment was satisfactory
concerning chemical parameters, although an increase in ecotoxicity was observed (EC50 reduced from
0.31% to 0.21%). The wastes from the kinetic study of persulphate and iodide reaction were treated with
sodium bisulphate until colour was removed. Although they did not reveal significant ecotoxicity, only over
1% of the untreated waste produced observable effects over algae. Therefore, ecotoxicity tests could be
considered a useful tool not only in laboratory effluents treatment, as shown, but also in hazardous
wastewaters management
2.1.2. Soil and groundwater remediation
The application of soil remediation technologies have been increasing in the last decades due the
identification and discovery of contaminated sites. In recent years, new technologies have been
developed and some well established technologies have been combined aiming the increase of the
remediation efficiency. The combination of soil vapor extraction (SVE) and bioremediation (BR) to
remediate soils contaminated with petroleum hydrocarbons is one successful example. SVE is the most
used remediation technology worldwide. It is an in-situ technology that is applicable to soils contaminated
with volatile or semi-volatile contaminants such as petroleum products and it uses vacuum pumping to
extract contaminated vapors from the unsaturated zone of the soil. BR is one of the most popular
remediation technologies due its low cost. It commonly uses native microorganisms of the soil to degrade
the contaminants but can also use inoculated microorganisms that degrade specific contaminants present
in soil, creating faster remediations. In the first stages of the remediation, SVE presents high extraction
rates that decrease significantly has the remediation time increases. At this point the SVE is stopped and
initiated the BR reducing the remediation cost and the energy consumption. Our team has been focused
on the evaluation of the impact on the remediation time and process efficiency of some soil properties
(contents of organic matter and water), operational parameters (airflow rate) and contaminant properties
(vapor pressure). It is also being developed an artificial neural network to the prediction of the remediation
time of a SVE process based only on some soil properties and the contaminant involved.
RESEARCH AREAS – ENVIRONMENTAL CONTROL AND REMEDIATION
GRAQ – ANNUAL REPORT – 2009
[ 25 ]
2.1.3. Removal of toxic compounds by means of adsorption strategies
One of the most widely used processes for the removal of low concentration pollutants, present in
industrial wastewaters, has been through adsorption with activated carbon as a final treatment. Due to the
high price of the activated carbon, research has recently been directed towards alternative sorbents.
Some of the alternative sorbents are native natural materials, like cork, peanut hulls and marine algae,
which are renewable resources and are available in huge quantities in Portugal. These materials are also
natural wastes originated from the cork industry, agriculture and the pharmaceutical/cosmetic industry,
respectively. Some of these of low-cost sorbents have been investigated as a replacement for current
costly methods of removing metals from solution. The sorption process using these materials are
becoming more accessible, making the process applicable even in small and medium scale industries.
A Box–Behnken factorial design coupled with surface response methodology was used to evaluate the
effects of temperature, pH and initial concentration in the Cu(II) sorption process onto the marine
macroalgae Ascophyllum nodosum. The effect of the operating variables on metal uptake capacity was
studied in a batch system and a mathematical model showing the influence of each variable and their
interactions was obtained. Study ranges were 10 – 40 ºC for temperature, 3.0 – 5.0 for pH and 50 –150
mg/L for initial Cu(II) concentration. Within these ranges, the biosorption capacity is slightly dependent on
temperature but markedly increases with pH and initial concentration of Cu(II). The uptake capacities
predicted by the model are in good agreement with the experimental values. Maximum biosorption
capacity of Cu(II) by A. nodosum is 70 mg/g and corresponds to the following values of those variables:
temperature = 40 ºC, pH= 5.0 and initial Cu(II) concentration = 150 mg/L. The use of peanut hulls, an
agricultural and food industry waste, for copper and lead removal through equilibrium and kinetic
parameters evaluation was studied. Equilibrium batch studies were performed in a batch adsorber. The
influence of initial pH was evaluated (3– 5) and it was selected between 4.0 and 4.5. The maximum
sorption capacities obtained for the Langmuir model were 0.21 ± 0.03 and 0.18 ± 0.02 mmol/g,
respectively for copper and lead. In bi-component systems, competitive sorption of copper and lead was
verified, the total amount adsorbed being around 0.21 mmol of metal per gram of material in both mono
and bi-component systems. In the kinetic studies equilibrium was reached after 200 min contact time
using a 400 rpm stirring rate, achieving 78 % and 58 % removal, in mono-component system, for copper
and lead respectively. Their removal follows a pseudo-second-order kinetics. These studies show that
most of the metals removal occurred in the first 20 min of contact, which shows a good uptake rate in all
systems. In another work we isolated from soil and characterized several bacterial strains capable of
either resisting high concentrations of heavy metals (Cd2+
or Hg2+
or Pb2+
) or degrading the common soil
and groundwater pollutants MTBE (methyl-tertbutyl ether) or TCE (trichloroethylene). We then used soil
microcosms exposed to MTBE (50 mg/l) or TCE (50 mg/l) in the presence of one heavy metal (Cd 10
ppm or Hg 5 ppm or Pb 50 or 100 ppm) and two bacterial isolates at a time, a degrader plus a
metalresistant strain. Some of these two-membered consortia showed degradation efficiencies well
higher (49 – 182 % higher) than those expected under the conditions employed, demonstrating the
occurrence of a synergetic relationship between the strains used. Our results show the efficacy of the
dual augmentation strategy for MTBE and TCE bioremediation in the presence of heavy metals.
RESEARCH AREAS – ENVIRONMENTAL CONTROL AND REMEDIATION
GRAQ – ANNUAL REPORT – 2009
[ 26 ]
2.2. OUTPUT INDICATORS
2.2.1. FCT funded projects
Project reference: PTDC/ECM/68056/2006 Project title: Remediation of contaminated soils combining vapour extraction and biological
processes: time and efficiency forecasting Duration: January 2008 – December 2010 Responsible investigator: Cristina Maria Fernandes Delerue Alvim de Matos Principal contractor: Instituto de Ciências e Tecnologias Agrárias e Agro-Alimentares-Porto (ICETA-
Porto/UP) Participating institution(s): Faculdade de Engenharia da Universidade do Porto Funding (total): € 52 555 Funding (ICETA): € 39 955
2.2.2. non-FCT funded projects
Project reference: 5551 Project title: FILMEQUE Duration: April 2009 – March 2011 Responsible investigator: Antonio Alfredo Crispim Ribeiro Principal contractor: Curtumes Aveneda, Lda Participating institution(s): Instituto Superior de Engenharia do Porto
Faculdade de Engenharia da Universidade do Porto Funding source: Agência de Inovação (ADI) Funding (total): € 261 049 Funding (ICETA): € 78 137 (divided with CIETI-ISEP)
Project reference: ------- Project title: Avaliação da eficiência de um coagulante/floculante de origem vegetal no
tratamento de águas e efluentes Duration: November 2009 – October 2010 Responsible investigador: Rui Boaventura (FEUP) Principal contractor: Faculdade de Engenharia da Universidade do Porto Participating institution(s): ICETA/Instituto Superior de Engenharia do Porto Funding source: Universidade do Porto Funding (total): € 4 000 Funding (ICETA): € 2 000
2.2.3. Papers (ISI)
1. F.D. Oliveira, J.H. Paula, O.M. Freitas, S.A. Figueiredo Copper and lead removal by peanut hulls: Equilibrium and kinetic studies Desalination 248 (1-3) (2009) 931–940.
2. Olga Freitas, Cristina Delerue-Matos, Rui Boaventura Optimization of Cu(II) biosorption onto Ascophyllum nodosum by factorial design methodology Journal of Harzardous Materials 167 (1) (2009) 449-454.
3. Aurora Silva, Sónia A. Figueiredo, M. Goreti Sales, Cristina Delerue-Matos Ecotoxicity tests using the green algae Chlorella vulgaris—A useful tool in hazardous effluents management Journal of Harzardous Materials 167 (1) (2009) 179-185.
4. V.C. Fernandes, J.T. Albergaria, T. Oliva-Teles, C. Delerue-Matos, P. de Marco Dual augmentation for aerobic bioremediation of MTBE and TCE pollution in heavy metal-contaminated soil Biodegradation 20 (3) (2009) 375-382.
5. G.A. Pinto, E.F. Gomes, F.O. Durão, C.M.N. Madureira, M.M.B.L. Guimarães, S. Morais Multi-criteria design optimization study of solvent extraction in mixer-settler units Hydrometallurgy 98 (3-4) (2009) 224-234.
RESEARCH AREAS – ENVIRONMENTAL CONTROL AND REMEDIATION
GRAQ – ANNUAL REPORT – 2009
[ 27 ]
2.2.4. Papers (non-ISI)
No papers (non-ISI) were published during 2009.
2.2.5. Books
No books were published during 2009.
2.2.6. Ph.D. theses
No Ph.D. theses were concluded during 2009.
2.2.7. MSc theses
1. Bie van der Vliet Arsenic removal using natural and synthetic adsorbents Karel de Grote-Hogeschool, Antwerpen, Belgium, June 2009.
2. Magda Cristina Teixeira de Passos Guimarães Global analyis on phosphorus: flow, supply horizon and impact assessment of phosphorus depletion University of Southern Denmark, June 2009.
3. Joana Alves Ferreira da Cruz Energy Optimization of a Furnace of a Ceramic Industry Sector ISEP, July 2009.
4. Carla Alexandra Moreira Vieira Avaliação ecotoxicológica de lixiviados de Lamas provenientes de estações de Tratamento de águas. Capacidade de germinação de sementes de Alface (lactuca sativa) ISEP, November 2009.
5. Diana Pinheiro Oxidative leaching of metals from electronic waste with solutions based on quaternary ammonium salts ISEP, November 2009.
6. Marta Gonçalves Varanda Determination of the environmental impacts and life cycle analysis of biodiesel production ISEP, November 2009.
7. Nuno Miguel Simões Leal Ribeiro Audit and Optimization for Energy Section of the impregnation of a textile industry November 2009.
8. Susana Natércia Oliveira Ribeiro Comparative study of changes in chemical characteristics of soil subjected to controlled burning and mechanical thinning ISEP, December 2009.
9. Diana Paula Cunha de Aguilar de Azevedo Machado Simulation of the production of paraxylene ISEP, December 2009.
10. Joana Maria César Veloso Ferreira Distribution of mercury in thermal waters and bottled in northern Portugal ISEP, December 2009.
2.2.8. International conferences
2.2.8.1. Oral presentations
No oral presentations in international conferences were made during 2009.
2.2.8.2. Poster presentations
1. Ana C. Meira Castro, J.T. Albergaria, João Paulo Meixedo, C.M. Delerue Matos, António Vivas, João Paulo Carvalho, Eduarda Ferreira, Manuela Costa, Amélia Freitas Soil Attributes Dynamics Evaluation After Prescribed Burning Practice in Northwestern Portugal Forest FESP II - 2nd International Meeting of Fire Effects on Soil Properties, Marmaris, Turquia, 2009, pp. 56.
RESEARCH AREAS – ENVIRONMENTAL CONTROL AND REMEDIATION
GRAQ – ANNUAL REPORT – 2009
[ 28 ]
2. Serra I, Morais S, Martins F.F, Delerue-Matos C.
TRELAB - Um modelo de gestão de resíduos químicos de laboratório como um contributo para a eco-eficiência II Jornadas Luso-Brasileiras de Ensino e Tecnologia em Engenharia-JLBE 2009, pp.539, 2009, Porto, Portugal.
3. Cruz J., Barros H., Guedes A., Morais S. Optimização energética dos fornos de uma indústria do sector cerâmico II Jornadas Luso-Brasileiras de Ensino e Tecnologia em Engenharia-JLBE 2009, pp.205, 2009, Porto, Portugal.
4. Castro, A.C.M., Albergaria J.T., Meixedo J.P., Delerue-Matos C.M., Vivas A., Ferreira E., Costa M., Freitas A., Ribeiro S.R. Ensaios preliminares para caracterização de um solo sujeito a fogo controlado II Jornadas Luso-Brasileiras de Ensino e Tecnologia em Engenharia-JLBE 2009, pp.688, 2009, Porto, Portugal.
5. Carvalho, G., Silva A., Delerue-Matos C., La Fuente A.V., Fiúza A. Remediação do crómio usando ferro zerovalenete- Ensaios em coluna II Jornadas Luso-Brasileiras de Ensino e Tecnologia em Engenharia-JLBE 2009, pp.689, 2009, Porto, Portugal.
6. Oliveira F.D., Freitas A.M., Figueiredo S.A. Optimização da biosorção de cobre, níquel e zinco utilizando o planeamento factorial II Jornadas Luso-Brasileiras de Ensino e Tecnologia em Engenharia-JLBE 2009, pp.690, 2009, Porto, Portugal.
7. A.M.M. Sousa, V.D. Alves, S. Morais, C. Delerue-Matos, Maria P. Gonçalves Development and optimization of an ECO-Friendly agar extraction process from the red seaweed Gracilaria Vermiculophylla 6th European Conference on Marine Natural Products PC68, 2009, Porto, Portugal.
8. Aurora Silva, Olga Freitas, Sónia Figueiredo, Bie Vandervliet, Adelaide Ferreira, António Fiúza Arsenic removal using synthetic adsorvents: Kinetics, equilibrium and column study 12th EUCheMs International Conference on Chemistry and the Environment - ICCE2009, lno P35-231, 2009, Stockholm, Sweden.
9. Olga Freitas, Cristina Delerue-Matos, Rui Boaventura Continuos-flow copper biosorption in regenerable Ascophyllum nodosum seaweed
12th EUCheMs International Conference on Chemistry and the Environment - ICCE2009, lno P12-208, 2009, Stockholm, Sweden.
10. Oliveira F.D., Soares A.C., Freitas A.M., Figueiredo S.A. Copper, nickel, and zinc removal by peanut hulls: batch and column studies in mono and tri-component systems 11th International Conference on -Environmental Science and Technology CEST2009, B36, 2009, Chania, Crete, Greece.
11. Manuela Carvalho, António Fiúza, M. Teresa Oliva-Teles, Cristina Delerue-Matos, José Tomás Albergaria Remediation of granitic soils contamined by MTBE using SVE- a case study 2nd international environmental best practices conference, P-63, 2009, Kraków, Poland.
12. Mónica Rosas, Valentina Domingues, Paolo Marco, Teresa Oliva-Teles, José Tomás Albergaria, Cristina Delerue-Matos Remediation of humic soils contamined with benzene using bioremediation 2nd international environmental best practices conference, P-55, 2009, Kraków, Poland.
13. José Tomás Albergaria, Maria Conceição Alvim-Ferraz, Cristina Delerue-Matos Remediation of soils contamined with trichloroethylene 2nd international environmental best practices conference, P-64, 2009, Kraków, Poland.
14. Guedes, N. Ribeiro, J. Rocha, S. Morais Auditoria energética à secção de impregnação de uma industria têxtil 3rd international congress on energy and environment engineering and management, 2009, pp. 19, Portalegre, Portugal.
15. S. Teixeira, C. Delerue-Matos, L. Santos The role of pH on sulfamethoxazole removal by walnut shells INNOVA-MED conference, pp. 119, 2009, Girona, Spain.
16. S. Machado, M.T. Oliva-Teles, C. Mansilha, C. Delerue-Matos, P. Gameiro Waste management and treatment recovery of acetronitrile EuroAnalysis 2009, P117-B2, 2009, Innsbruck, Austria.
17. J. Ferreira, I. Seguro, T. Oliva-Teles, C.M. Matos, A. Veja Distribuição do mercúrio nas águas hidrotermais do norte de Portugal Encontro Internacional de termalismo e Turismo Termal/III Fórum Ibérico de águas engarrafadas e Termalismo, Furnas, Açores, Portugal, 2 a 9 Novembro 2009.
RESEARCH AREAS – ENVIRONMENTAL CONTROL AND REMEDIATION
GRAQ – ANNUAL REPORT – 2009
[ 29 ]
2.2.8.3. Proceedings papers
1. F. D. Oliveira, O. M. Freitas, S. A. Figueiredo
Copper, nickel and zinc removal by peanut hulls: batch and column studies in mono and tri-component systems, Proceedings of the 11th International Conference on -Environmental Science and Technology CEST2009, B676-B683 (2009).
2. Cruz J., Barros H., Guedes A., Morais S. Optimização energética dos fornos de uma indústria do sector cerâmico Proceedings of the II Jornadas Luso-Brasileiras de Ensino e Tecnologia em Engenharia - JLBE 2009, 205-211 (2009).
3. Serra I, Morais S, Martins F.F, Delerue-Matos C. TRELAB - Um modelo de gestão de resíduos químicos de laboratório como um contributo para a eco-eficiência Proceedings of the II Jornadas Luso-Brasileiras de Ensino e Tecnologia em Engenharia - JLBE 2009, 539-545 (2009).
2.2.9. National conferences
2.2.9.1. Oral presentations
No oral presentations in national conferences were made during 2009.
2.2.9.2. Poster presentations
No poster presentations in national conferences were made during 2009.
2.2.9.3. Proceedings papers
No poster presentations in national conferences were made during 2009.
2.3. OTHER ACTIVITIES
Governmental funding (pre-graduation)
In 2008 and 2009 2 grants from the “Concurso de Bolsas de Integração na Investigação para 5000
estudantes do Ensino Superior” (FCT) were given to the following students:
1. Pedro Romeu da Silva Soares, Adsorção de micropoluentes (metais) usando materiais naturais e sintéticos.
2. Irene Cristina de Sousa Azevedo, em curso.
Launched in June 1996, the Ciência Viva programme is the contribution of the Ministry of Science and
Technology to the promotion of a scientific and technological culture among the Portuguese population. In
the sub-category “Science in the Holidays” 3 programs, with the duration of 1 week (40 hours) were
organized: “Os Engenheiros Incendiários”, “Valorização de resíduos naturais”, “Vamos procurar
processos mais sustentáveis usando a Química Verde!”
In cooperation with a local professional high school (Escola Secundária Infante D. Henrique), 8 students
realized a professional training period of 160 hours:
1. Ana Cláudia Santos Silva, Pontos negros de contaminação e análise de solos.
2. Ana Isabel Ribeiro Meireles, Gestão de laboratório.
3. Cristiano Jorge Madeira Azevedo, Recuperação de solventes orgânicos.
4. Ivo Emanuel Moreira Rodrigues, Gestão e tratamento de resíduos laboratoriais.
5. Liliana Andreia Nogueira Oliveira, Gestão de laboratório.
RESEARCH AREAS – ENVIRONMENTAL CONTROL AND REMEDIATION
GRAQ – ANNUAL REPORT – 2009
[ 30 ]
6. Lisandra Bastos, Bioremediação de solos.
7. Rui Manuel Soares de Sousa, Tratamento e gestão de resíduos laboratoriais provenientes dos laboratórios do
ISEP.
8. Telma Magalhães, Pontos negros de contaminação e análise de solos.
2.4. FUTURE RESEARCH
Approved funding in 2009 (projects to be started in 2010):
PTDC/ECM/103141/2008, “Rehabilitation of pharmaceuticals-contaminated soils”, January 2010 - December 2012, €
98.764.
Pending funding (projects submitted in 2009):
PTDC/AAC-AMB/115154/2009, “Valorização de penas (resíduo da indústria avícola) para tratamento de águas e
efluentes“, € 86.653.
PTDC/AAC-AMB/112638/2009, “Sustainable management of laboratory chemicals and wastes”, € 54.993.
PTDC/AAC-AMB/113386/2009, “Sustainable chemical laboratories - energy optimization using standard domotic
infrastructures in indoor environment quality control”, € 80.730.
PTDC/ECM/114112/2009, “Cinética da Bioventilação – uma abordagem multidisciplinar”, € 15.320.
RESEARCH AREAS – RESEARCH METRICS
GRAQ – ANNUAL REPORT – 2009
[ 31 ]
3. RESEARCH METRICS
TEAM MEMBERS
Permanent Members
Cristina Maria Delerue-Matos
Hendrikus Petrus Antonius Nouws
José Tomás Veiga Soares de Albergaria
Non-permanent members
--
OUTPUT INDICATORS (SUMMARY)
Conferences (international) Oral presentation -- Poster presentation 1 Proceedings papers 1
The development of metrics to assess research outputs is recognized of increased importance worldwide.
For many years, ISI (Thomson Scientific, Inc.) has provided the sole standardized set of bibliometric data
that were used in all sort of studies. More recently, Elsevier has been developing an alternative database,
Scopus, which promises to be a useful competitor and provide a different point of view over scientific
publication. Other measures have been used in different countries, the case of the UK deserving
emphasis as the plan to abandon the costly periodic Research Assessment Exercises elicited heated
discussion and many serious studies.
It is common that university groups develop studies that are then used by government agencies for their
official studies and benchmarks of research performance. In Portugal no systematic work exists and
government publications (of GPEARI under the ministry of Science and Higher Education) depend
directly on data provided by Thomson Scientific. Requimte is developing bibliometric studies of
Portuguese research institutions and intends to develop other type of metrics to assess the outcomes of
scientific research.
3.1. OUTPUT INDICATORS
3.1.1. International conferences
3.1.1.1. Poster presentations
1. Elizabeth S. Vieira, Henri P.A. Nouws, José T. Albergaria, Cristina Delerue Matos, José A.N.F. Gomes Research Quality Indicators for Brazilian, Portuguese and Spanish Universities 12
th International Conference on Scientometrics and Informetrics – ISSI2009, P50, Rio de Janeiro,
Brasil.
3.1.1.2. Proceedings papers
1. Vieira E.S., Nouws H.P.A., Albergaria J.T., Delerue Matos C., Gomes J.A.N.F. Research Quality Indicators for Brazilian, Portuguese and Spanish Universities Proceedings of the ISSI2009 - 12
th International Conference on Scientometrics and Informetrics,
vol 2, 1000-1001 (2009).
FUNDING AND SCIENTIFIC EVALUATION
GRAQ – ANNUAL REPORT – 2009
[ 32 ]
B. SCIENTIFIC EVALUATION
Although there is no clear trend, the number of papers published in scientific journals included in the ISI
Web of Science database in 2009 was by far the highest for GRAQ in the period 2001-2009 (Figure 5.1).
However, the observed annual increase from 2007 is believed to continue in 2010, because already 12
papers have been published as of March 2010.
Figure 5.1 Number of papers published in scientific journals included in the ISI Web of Science by
GRAQ members (2001-2009)
The number of papers published per Ph.D. member of the permanent staff (Figure 5.2) varies between
0.3 and 1.5. The same tendency is observed for the number of papers: steady increase from 2007.
The results from a citation analysis for the period 2001-2009 are shown in Figure 5.3. An obvious
decrease in citations per paper is observed because of (i) the low number of papers and (ii) the short time
period. The average citation per paper is 3.4 and the Hirsch index (h-index) is 8.
0
2
4
6
8
10
12
14
16
18
20
2001 2002 2003 2004 2005 2006 2007 2008 2009
Pap
ers
ISI
We
b o
f Sc
ien
ce
Year
FINANCIAL AND SCIENTIFIC EVALUATION
GRAQ – ANNUAL REPORT – 2009
[ 33 ]
Figure 5.2 Number of papers published in scientific journals included in the ISI Web of Science per
Ph.D. member of the permanent staff (2001-2009)
Figure 5.3 Citation analysis (2001-2009)
0,0
0,2
0,4
0,6
0,8
1,0
1,2
1,4
1,6
2001 2002 2003 2004 2005 2006 2007 2008 2009
Pap
ers
/ P
hD
-sta
ff
Year
0,0
1,0
2,0
3,0
4,0
5,0
6,0
7,0
8,0
9,0
10,0
2001 2002 2003 2004 2005 2006 2007 2008 2009
Cit
atio
ns
/ p
ape
r
Year