A Glimpse of Recent Developments in Brazilian Analytical Chemistry

A Glimpse of Recent Developments in BrazilianAnalytical Chemistry

Sergio L. C. Ferreira,1 Pedro Afonso de Paula Pereira,1 Joaquim A.

N�oobrega,2 Orlando Fatibello-Filho,2 Mario Almir Feres,3 Boaventura

F. Reis,3 Roy Edward Bruns,4 and Francisco Radler de Aquino Neto5

1Instituto de Quımica, Universidade Federal da Bahia, Salvador-BA, Brazil2Departamento de Quımica, Universidade Federal de Sao Carlos,

Sao Carlos-SP, Brazil3Centro de Energia Nuclear na Agricultura, Universidade de Sao Paulo,

Piracicaba-SP, Brazil4Instituto de Quımica, Universidade de Campinas, Campinas-SP, Brazil

5Instituto de Quımica, Universidade Federal do Rio de Janeiro, RJ, Brazil

Abstract: This review highlights some relevant contributions proposed byBrazilian analytical research groups mainly after 2004. This year was chosendue to an earlier publication of an overview with similar scope by Andradeet al. (2004). The selected papers are representative, but the authors have not triedto present a comprehensive overview of the aforementioned period. The chosenareas for discussion were automation in analytical chemistry, chemometrics, chro-matography, capillary electrophoresis and mass spectrometry, electroanalyticalchemistry, environmental analytical chemistry, preconcentration and separationprocedures, and spectrochemical analysis. A glimpse of the Brazilian contribu-tions shows the stage of development of analytical chemistry in Brazil, withemphasis on major advancements and critical needs.

Keywords: Automation, chemometrics, chromatography, electroanalytical,preconcentration, spectrochemical analysis

Received 25 March 2008; accepted 2 March 2008.The authors gratefully acknowledge financial support from Brazilian founda-

tions (CAPES, CNPq, FAPESP, FAPESB and FAPERJ).Address correspondence to Sergio L.C. Ferreira, Instituto de Quımica, Univer-

sidade Federal da Bahia, Grupo de Pesquisa em Quımica Analıtica, CampusUniversit�aario de Ondina, Salvador, BA 40170-290, Brazil. E-mail: [email protected]

Analytical Letters, 41: 1494–1545, 2008Copyright # Taylor & Francis Group, LLCISSN: 0003-2719 print/1532-236X onlineDOI: 10.1080/00032710802136289

1494

AUTOMATION IN ANALYTICAL CHEMISTRY

The current work comprises an overview of recent developments in auto-mation in analytical chemistry in Brazil, which may be considered mainlyin the context of Flow Injection Analysis (FIA), because the use of otherautomation techniques to develop analytical procedures is not at thesame pace in Brazil. In this sense, we think that a quick overview ofFIA history in Brazil, prior to describing recent developments, wouldbe helpful in the understanding of the current status of this area.

Brief History

It is well-known that the beginning of the Flow Injection Analysis (FIA)process by Ruzicka and Hansen occurred 33 years ago (Ruzicka andHansen 1975). The anthological series comprising the first ten papersrepresented a remarkable contribution, for its quick acceptance aroundthe world. The Brazilian researchers’ initiation into the FIA process tookplace when FIA was emerging as a tool for analytical proceduresdevelopment; thus, in the cited series, they participated as co-workersin the third and fourth papers (Stewart et al. 1976; Ruzicka et al.1976). Nowadays, the use of the FIA process is disseminated worldwide,and several innovative contributions have been proposed by Brazilianresearchers; among them, it is worthwhile to mention merging zonesfor saving reagents (Bergamin-Filho et al. 1978), zone-sampling to carryout line dilution (Reis et al. 1981), ion exchange resin (Bergamin-Filhoet al. 1980), monosegmented flow analysis for sensitivity improvement(Pasquini and de Oliveira 1985), flow-batch to perform true acid=basetitration (Honorato et al. 1999) and Multi-Commuted Flow InjectionSystem (MCFIA), which allows the handling of several solutionsemploying a single pumping channel (Reis et al. 1994).

Nowadays, in the context of flow analysis in analytical chemistry,there are three basic concepts identified as FIA (Simoes et al. 2006),Sequential Injection Analysis (SIA) (Santos et al. 2005) and Multi-Commuted Flow Injection Analysis (MCFIA) (Feres and Reis 2005).In the first one, a sample aliquot is collected and inserted into the analyti-cal path by means of a sampling loop coupled to the injecting device. Thisstep has been carried out by employing either a commutator injector(Diniz et al. 2004) or a six-port valve (Flores et al. 2007). These devicespresent as a common feature, two resting positions; thus, the flowsystems have been designed by considering this condition. In the SIA(Santos et al. 2005), a multi-port valve comprises the core of the mani-fold, which has been controlled by microcomputer to allow that aliquots

Recent Brazilian Analytical Chemistry 1495

of sample and reagent solution were inserted into the analytical path as atime function. In the multi-commuted flow injection analysis (MCFIA)(Feres and Reis 2005), the system manifold comprises a set of solenoidvalves assembled to work as an independent commuting device, andaliquots of sample and reagent solutions inserted into the analyticalpath are selected as a time function. The flow system can be arrangedto work either at the pushing mode or at the pulling mode (Lavoranteet al. 2006).

The system based on the FIA process employs a peristaltic pump forfluid propelling and requires one channel for each solution (Souza et al.2007; Oliveira et al. 2007; Silva et al. 2007; Bentlin et al. 2007; Lindinoand Bulhoes 2007; Neira et al. 2007). In the SIA approach, the solutionpropelling has been carried out using a single pumping channel (dosSantos and Masini 2007; Abate et al. 2006; Santos et al. 2005), thusallowing the use of an automatic syringe (Santos et al. 2005) or a peristal-tic pump (Oliveira et al. 2006). In the MCFIA approach, the peristalticpump is the most used device for solutions propelling (Borges et al.2007; Pires et al. 2007; Garcia and Reis 2006; Maruchi and Rocha2006; Vieira et al. 2006; Rodenas-Torralba et al. 2005). Recently, thesolenoid micro-pump has been introduced as an alternative to peristalticpump (Lapa et al. 2002; Rocha et al. 2005; Santos et al. 2007; Ribeiroet al. 2007; Santos et al. 2007; Carneiro et al. 2005), presenting, as advan-tages, small size and commuting features, and thus permitting its use toreplace both peristaltic pump and solenoid valve.

Automation of Analytical Procedures

A glance at the Brazilian contribution to the automation of analyticalprocedures in the period of 2004 to 2007 shows that 215 papers werepublished, where 138 studies were implemented employing the classicalFIA, in which the core of the flow system manifold was based on thecommutator injector (Diniz et al. 2004). Sequential injection analysisand multi-commuted flow injection analysis processes contributed with21 and 52 papers, respectively.

A close inspection of related works shows that UV-visible spectro-photometry was by far the most used detection technique, comprising64% of the published papers, while atomic absorption spectrometryand electrochemistry (voltammetry, amperometry, potentiometry, etc)participated each with 12% of the total. Chemiluminescence contributedwith 5%, while other detection techniques, such as ICP-OES, ICP-MS,fluorimetry, and conductometry have been also employed, but neverthe-less presented a modest participation.

1496 S. L. C. Ferreira et al.

The number of papers based on SIA and MCFIA comprise 10% and25%, respectively, of the total papers published in the considered period.The SIA score could be considered modest, taking into account that thisprocess was introduced 17 years ago (Ruzicka and Marshall 1990). Theinception of the MCFIA happened four years later (Reis et al. 1994);therefore, these data show that this process presented a good acceptanceas a reliable tool to develop analytical procedures. A glimpse of thepapers published in the investigated period shows that the FIA processhas been widely employed by several groups of Brazilian researchers,while MCFIA and SIA have been employed by only a few of them.

The contribution of Brazilian researchers to the FIA process beganwhen it was new (Stewart et al. 1976; Ruzicka et al. 1976), and hascontinued throughout the past 33 years. Sequential IA and MCFIA pro-cesses present similar advantages concerning reagent consumption,reduction of waste generation, and operational versatility; nevertheless,their dissemination in Brazilian research groups has been slow. Drasticreduction of both reagent consumption and waste generation are com-mon features afforded by the analytical procedures based on SIA andMCFIA processes. In this sense, we think that these processes presenta growing potential, considering that, at the present time, attention hasbeen paid to analytical procedures that are friendly to the environment,in agreement with the ‘‘green’’ chemistry paradigm.

Among the papers based on MCFIA, it was observed that 20%employed solenoid mini-pumps as solution-propelling and commutingunits. Taking into account that its inception as a solution-propellingdevice took place five years ago (Oliveira et al. 2007), these data wouldbe considered an indication that it would become a reliable alternativeto the peristaltic pump.

CHEMOMETRICS

Brazil received worldwide attention for chemometric activities in 2006, byhosting the Chemometrics in Analytical Chemistry (CAC) meeting, witha participation of about 150 researchers (Buydens and Ferreira 2007).Intense chemometric activity was in evidence at the biannual Braziliananalytical chemistry meeting (14th ENQA 2007) in 2007. There were atotal of 68 communications in the two chemometric poster sessions, aswell as 54 other poster communications reporting the application of che-mometric tools in other areas of analytical chemistry. Chemometrics hasbeen consolidated as a mature sub-area of analytical chemistry in Brazil,and recently a review of the first 25 years of Brazilian research inchemometrics has been published (Barros Neto et al. 2006).


Research activities of Brazilian groups have included most areas ofchemometrics, including multivariate design and optimization, classi-fication, and calibration. Besides applying recently developed techniques,new chemometric methods have also been developed.

Image analysis using least squares support-vector machines has beenapplied to the quantification of Lactobacillus in fermented milk (Borinet al. 2007). Digital color images of Petri plates easily obtained by useof a flatbed scanner were analyzed. Least squares support-vectormachines and Near Infrared (NIR) spectroscopy have also been usedto quantify common adulterants in powdered milk (Borin et al. 2006).A nonlinear behavior was present in the dataset, owing to spectral differ-ences of three different adulterants, limiting the effectiveness of linearmethods such as Partial Least Squares Regression (PLSR). Image analy-sis has also been carried out for the quality control of paints using chemo-metric strategies (Pereira and Bueno 2007). Digital image-based titrationshave also been carried out to determine HCl and H3PO4 in aqueous solu-tions and total alkalinity in mineral and tap waters. Their results werecompared to spectrophotometric (SPEC) titrations. By applying a pairedt-test, no statistical difference between the results of both methods wasverified at the 95% confidence level (Gaiao et al. 2006). A laboratory-developed algorithm was used and tested to characterize atomic forcemicroscopy images of hair samples that were classified using partial leastsquares discriminant analysis (Gurden et al. 2004).

The second-order advantage provided by Parallel Factor Analysis(PARAFAC) has been investigated using the standard addition methodfor the direct determination of salicylate in undiluted human plasma byspectrofluorimetry (Sena et al. 2006). A specific PARAFAC model wasbuilt from three-way arrays formed by 436 emission wavelengths, 7 exci-tation wavelengths, and 5 measurements (sample plus 4 additions). Thisadvantage was also used for the direct determination of propranolol inurine, using the same spectrofluorimetric technique (Silva et al. 2007).A three-way resolution method based on the PARAFAC model wasapplied to UV-Vis spectra to study the simultaneous degradation in the1 to 13 pH range of anthocyanins extracted from fresh calyces of flowersof the Hibiscus sabdariffa. Tautomeric constants and pK acidity valueswere determined (Marco et al. 2005). Second-order calibration and multi-variate spectroscopic-kinetic measurements in the visible region havebeen proposed to improve the Jaffe method for creatinine assay. Quanti-tative determinations of creatinine with the PARAFAC and directTrilinear Decomposition (TLD) methods were used (Guterres et al.2004). A review including contributions from Brazilian and Argentineauthors on second- and third-order multivariate calibration has recentlyappeared in the literature. (Escandar et al. 2007)


Method development in multivariate calibration has also receivedattention in Brazil. Focus has been placed on pre-processing techniques.Collinearity minimization is characteristic of the Successive ProjectionsAlgorithm (SPA) developed for variable selection in classifications(Pontes et al. 2005). The method was used for the simultaneous spectro-metric determination of Cu2þ , Mn2þ , and Zn2þ ions in pharmaceuticalpreparations of polivitaminic=polymineral drugs (Saldanha et al. 2005).The MLR-SPA results were compared with those found using MLR-GA and models based on latent variables, Principal ComponentRegression (PCR), and Partial Least Square regression (PLS).

An analytical method to determine directly and simultaneously fivephenolic compounds (4-nitrophenol, 2-nitrophenol, phenol, 2,4,6-trichlorophenol, and 4-chlorophenol) in seawater (Ria de Bahia Blanca,Argentine) has been based on MLR-SPA (Nezio et al. 2007). A statisticalcomparison of these results with those obtained using PLS demonstratedthe potentiality of MLR-SPA for solving complex analytical problems.

The use of the Successive Projections Algorithm to select variablesfor building robust transferable Multiple Linear Regression (MLR) mod-els has been investigated. Data sets consisting of spectral data of gasolineand corn were subjected to analysis. Robust MLR models were comparedto a PLS model employing Piecewise Direct Standardization (Honoratoet al. 2005). This work is part of a larger effort by this Recife groupstudying robust modeling for multivariate calibration transfer (Honoratoet al. 2007).

Intense studies in wavelet development have also been undertaken.Suboptimal wavelet de-noising of co-averaged spectra employing stat-istics from individual scans (Galvao et al. 2007), wavelet-packet identifi-cation of dynamic systems in frequency subbands (Paiva and Galvao2006), optimal wavelet filter construction using X and Y data (Galvaoet al. 2004), as well as a wavelet-based controller for a mobile robot(Sousa et al. 2004) have been reported.

Q-mode curve resolution of UV-vis spectra for structural transform-ation studies of anthocyanins in acid solution has resulted in the determi-nation of equilibrium and kinetic rate constants of complex chemicalsystems (Marco and Scarminio 2007). This group has also applied che-mometric techniques for the fingerprint optimization of chromatographicmobile phases and extraction solutions for several natural products(Scarminio and Almeida 2007; Scarminio et al. 2007; Soares et al. 2007).

Chemometric calibrations in Brazil have focused on a variety of dif-ferent samples. Most prominent are gasoline, oil, and other petroleumproducts, which have been investigated by a large number of groupsusing IR or NIR spectroscopy. (Caneca et al. 2006; Albuquerque et al.2005; Pimentel et al. 2006; Santos and Masini 2007; Pereira et al. 2006).


Interesting studies have been done on food products (Pedro and Ferriera2005; Pedro and Ferreira 2006), coffees and sugar cane spirits (Fernandeset al. 2005), wheat flour (Ferrao and Davanzo 2005), soybean ethanolysis(Peralta-Zamora et al. 2004) and sewage sludge (Petrucelli et al. 2007).

Experimental designs have been used in Brazil for the optimization ofanalytical methods. Two books on statistical experimental design andoptimization, one in Portuguese (Barros Neto et al. 2001), and the otherin English (Bruns et al. 2006), have been published by Brazilian authors.

Unreplicated split-plot procedures (Bortoloti and Cadore 2005) havebeen applied, using mixture-mixture designs for the fingerprint optimiza-tion of chromatographic mobile phases and extraction media of naturalproducts (Borges et al. 2007). These designs can be important for optimi-zation studies in which the experiments cannot be carried out in randomorder because of operational limitations.

Attention has also been given to the optimization of analyticalmethods characterized by large numbers of responses combining fac-torial, central composite, and mixture designs with principal componentanalysis (Penteado et al. 2006; Bezerra et al. 2006; Pasqualoto et al. 2007).Other groups have applied these designs to problems with smallernumbers of responses in electrochemistry (Luna et al. 2007) and analysisof seawater (Ferreira et al. 2004).

CHROMATOGRAPHY, CAPILLARY ELECTROPHORESIS AND

MASS SPECTROMETRY

Traditionally, analytical chemistry was mostly related to inorganic analy-sis as highlighted by Zagatto and S�aa (2003). The overwhelming analyticalneeds for organic compounds in ever-increasing complex mixtures led totheir development in the umbrella of organic chemistry, synthetic chem-istry, biochemistry, and their numerous applications concerning oureveryday life. More and more, chemistry is being considered as an encom-passing and fundamental field of knowledge that guarantees the improve-ment of quality of life and the sustainability of our planet and the humanrace. This has triggered a renewed interest in better analytical techniquesto cope with the urgent need to determine the molecular constitution ofalmost every single aspect of modern life and of natural and syntheticmaterials. Just as a brief example, the revolution in medical and relatedfields attained through the ‘‘-omics’’ concept, is yet to be fully under-stood. Genomics, proteomics, metabolomics, metallomics, etc., in thebiological framework are now being applied in other fields, such as theapplication of this concept to petroleum (petroleomics). These advanceswere made possible by the conjugation of an array of chromatographic


and related separation techniques, together with the myriad of mass spec-trometric techniques that are frequently released by all major instrumentmanufacturers. The importance of these ‘‘-omics’’ techniques hasattracted the attention of the analytical chemistry community, whichhas led to the need for their inclusion in the present review. Unfortu-nately, the breadth of their application and the speed of their develop-ment hinder a thorough approach to describing the participation of theBrazilian research community in their advancement. Therefore, only afew landmarks will be presented here, and a hint of the recent trends willbe highlighted. The thousands of application papers on this subject couldnot reasonably be covered.

Introduction of these techniques in Brazil dates back to their onsetworldwide. Gas chromatography theoretical advances were a matter ofconcern in the early 1960s (Costa-Neto et al. 1964), the introduction ofHigh Resolution Gas Chromatography (HRGC) with all new conceptsdevised by the Grob family in Switzerland in the late 1970s early 1980swere immediately transferred to Brazil in 1981 (Furtado and Cardoso1984; Grob 1985; Aquino Neto and Cardoso 1985), as well as Chiral-(Ramos et al. 2000) and High Temperature-HRGC (Pereira et al.2004). Recently, the new frontier of gas chromatography was alsobrought to Brazil, namely, The comprehensive GC�GC (Silva-Junioret al. 2007, Silva-Junior et al. 2008; Caramao et al. 2007). Liquid chro-matography has always been extensively used, and advances in HPLCapplications and column technology are the main present trends (Fariaet al. 2006). Carol Collins, one of the pioneers in the dissemination of thistechnique, organized a well-known book on chromatography (Collinset al. 2006). Stationary phase development continues to be an issue,and Collins’s group is currently developing immobilized and monolithicstationary phases (Faria et al. 2007; Faria et al. 2006) and Cass’s groupis developing Restricted Access Medium (RAM) columns (Cassiano et al.2006; Lima et al. 2006). Advances in hardware for hyphenated techniquesencompassing HPLC and supercritical fluid chromatography have beenundertaken by Lancas et al. more recently focusing on Solid PhaseExtraction (SPE) techniques (Chaves et al. 2007; Fernandes et al.2007). He also started the successful COLACRO Latin-American Chro-matography Congresses. Capillary electrophoresis applications are stillless widespread, but a few very active groups are taking charge of itsdevelopment and application. Tavares et al. introduced and applied thistechnique extensively in Brazil (Silva et al. 2007b; Tavares et al. 2003).Coltro et al. focused on instrumentation development (Coltro et al.2007) and Bonato et al., on drug analysis and chiral separations (Bonatoet al. 2006). Both were involved in the organization of two of the LatinAmerica Capillary Electrophoresis Symposia, LACE (1998 and 2005).


Hardware development was also undertaken by Saito et al. (Saito et al.2007). Mass spectrometry developed into a myriad of different techniquesand combinations of sources and mass analyzers. Despite the enormousinvestment represented to follow the state of the art, slowly theequipment has been incorporated in a few leading laboratories. Instru-mentation research has been focused mainly in TOF and soft ionizationtechnologies by Collado et al. (Collado et al. 2004). The most productivegroup, Thompson Laboratory, is involved in several instrument develop-ments for diverse applications—mainly sample introduction and ioniza-tion techniques (Haddad et al. 2008; Silva et al. 2007e; Eberlin et al.2005) and the development and operation of one of the few existing pen-taquadrupole instruments (Juliano et al. 1996). Genomics and proteomicsdevelopments have also occurred, following the establishment of theBrazilian Genomic network in 2000 and the Rio de Janeiro Proteomicsnetwork in 2001, to foster the development of these important areas inbiotechnology, highly dependent on electrophoretic techniques and massspectrometry, mainly ESI-MS-MS, MALDI-TOF, MALDI-TOF-TOFand Orbitrap mass spectrometry technologies (Cuervo et al. 2007; Leonet al. 2007; Kruger et al. 2006).

ELECTROANALYTICAL CHEMISTRY

The history of the first Brazilian chemist and probably the first Braziliananalytical chemist, Vicente Coelho de Seabra Silva Telles, who publishedthe book Elementos de Quımica (Elements of Chemistry) in Coimbra,Portugal, in 1788, one year before Lavoisier’s milestone book, Traite Ele-mentaire de Chimie, and the creation and evolution of courses in chemis-try in Brazil were recently discussed (Filgueiras 1985; Andrade et al.2004). There are several excellent articles describing the history and=orstatus of analytical chemistry in Brazil, published in Portuguese (Curtius1982; Neves 1984; N�oobrega et al. 1996; Fatibello-Filho et al. 2002) and inEnglish (Senise 1985; Galembeck 1999; de Oliveira-Neto et al. 2002;Zagatto and S�aa 2003; Andrade et al. 2004), in which the outstanding con-tributions of Fritz Feigl, Heinrich Rheinboldt, Heinrich Hauptman,Paschoal Senise, Antonio Celso Spinola Costa, Priest Leopoldo Hainber-ger, Henrique Bergamin-Filho, and Otto Alcides Ohlweiler, who pub-lished the first analytical chemistry textbook in Portuguese, werehighlighted. In 1935, a chemistry b. sc. course was initiated in the just-started University of Sao Paulo (USP). In this course, following Germa-nic standards by Prof. Rheinboldt and his then-assistant Hauptman,Senise studied and graduated in the first group, in 1937. After he com-pleted his Ph.D. in 1942, under the supervision of Prof. Rheinboldt,


Senise became the pioneer in analytical chemistry at the USP. Afterspending more than two years (1950–1952) in post-doctoral work withthe Professors P.W. West and Paul Delahay at the University of Louisi-ana in Baton Rouge, Prof. Senise started research on microchemicalanalysis and electroanalytical at the University of Sao Paulo. Of the 10Ph.D. students supervised by him, Oswaldo E.S. Godinho, Jaim Lichtig,and especially Eduardo Neves have built distinguished careers, gradu-ating approximately 60 M.Sc. and Ph.D. students, amplified to over fourhundred in the second to fourth generations, spreading throughout thecountry, and forming new research groups (Gutz 2006), many of themin electroanalytical chemistry.

The exponential growth recorded in analytical chemistry and also inelectroanalytical in Brazil in the last decades (Galembeck 1999; Senise1993; Fatibello-Filho et al. 2002; Zagatto and S�aa 2003; Andrade et al.2004) was also driven by at least two major mobilizing factors: (a) thefoundation of research agencies such as CNPq, the Conselho Nacionalde Desenvolvimento Cientıfico e Tecnol�oogico (The National Councilfor Scientific and Technological Development) (1951), CAPES, the Coor-denacao de Aperfeicoamento de Pessoal de Nıvel Superior (Coordinationfor the Improvement of Higher Education Personnel) (1951), FAPs (e.g.,FAPESP, the Fundacao de Amparo a Pesquisa do Estado de Sao Paulo(The State of Sao Paulo Research Foundation) (1962), FINEP, theFinanciadora de Estudos e Projetos (Research and Projects Funding)(1967) and PADCT, the Plano de Apoio de Desenvolvimento Cientıficoe Tecnol�oogico (Support Plan for Scientific and Technological Develop-ment) (1987) and (b) the SBQ, the Sociedade Brasileira de Quımica (Bra-zilian Chemical Society). The development of the Brazilian chemistrysector during the last 30 years is nowadays being attributed to PADCT.A history of this agency and the strategies, planning, and implementationof the second phase of this program was well discussed by Paniago(Paniago 2007). The impact of the NAS=CNPq (National Academy ofSciences, USA=CNPq) cooperative program on the development ofchemistry in Brazil was recently revised by several authors in a specialissue of Quımica Nova (New Chemistry) (Campbell 2007; Brocksom2007; Senise 2007; Mano 2007; Espinola 2007). Looking back over theselast 30 years, we realize that the foundation of the SBQ in 1977 has madea remarkable contribution toward the development and consolidation ofchemistry and analytical chemistry in Brazil, due to the Annual Meeting,the two journals Quımica Nova (New Chemistry) and JBCS (Journal ofthe Brazilian Chemical Society), and support to each one of the SBQ’sDivisions and their Scientific Meetings.

But going back to 1978, Prof. Eduardo Neves and Prof. TiborRab�ooczkay created the Brazilian Symposium of Electrochemistry and


Electroanalysis (SIBEE), one of the main forums to evaluate the state ofthe art in these areas in Brazil. The first event took place in October ofthis same year and was followed biannually. The history, evolution,and growth of electrochemistry=electroanalytical in Brazil in the periodbetween 1977 and 2002 were presented by Avaca and Tokoro (Avacaand Tokoro 2002). The activities of the electrochemistry and electroana-lytical division of SBQ from 1993 to 2002 are also briefly discussed, aswell as some considerations made on the present and future of thesefields. According to these authors, the support of the SBQ’s Divisionof Electrochemistry and Electroanalytical Chemistry through biannualmeetings and the aforementioned SIBEE have provided a vertiginousgrowth in these areas, both in magnitude as well as diversification. Thisevolution was well-evidenced by the great volume of studies published inseveral scientific journals, the formation and consolidation of pro-fessional scientific societies and their various subdivisions, a series of con-gresses that regularly bring together Brazilian as well as internationalscientists, and especially by the noteworthy quality of the professionalsturned out in this area (Zanoni 2003).

Concerning analytical chemistry, the National Meeting on AnalyticalChemistry (ENQA), which was held for the first time in Rio de Janeiro(RJ), in November 1982 and the last time (XIV ENQA) in Joao Pessoa(PB) in 2007, the support of the SBQ’s Division of Analytical Chemistryhas contributed toward promoting significantly, the developments of thisarea, as pointed out by Andrade et al. (Andrade et al. 2004).

Electroanalytical is one of the areas that is very well-established inSao Paulo State (i.e., Sao Paulo Capital, Campinas, Sao Carlos,Araraquara, and Ribeirao Preto), which is where Brazilian groups havereached a large size associated with high quality. The production ofBrazilian researchers in electroanalytical (including amperometry, chron-oamperometry, chronocoulometry, conductometry, polarography,potentiometry, voltammetry, and related techniques) in the period fromJanuary 1, 1990, to October 31, 2007, was about 890 scientific papers,which represent 9% of the total articles published by Brazilian analyticalchemists in this period. Of those articles published in electroanalytical,650 articles (72.7%) were published by researchers of the Sao Paulo State.An exponential growth was observed from 1994 to date. The reasons forthis achievement are the strong influence of Prof. Eduardo A. Neves,recognized as the Father of Electroanalysis in Brazil (Institute ofChemistry of University of Sao Paulo (1959–1989) and Department ofChemistry of the Federal University of Sao Carlos (1991–2006)), and alsoTibor Rab�ooczkay (IQ=USP), Oswaldo E.S. Godinho (IQ=UNICAMP),Graciliano de Oliveira-Neto (IQ=USP and IQ=UNICAMP), andyoung independent researchers (Galembeck 1999; Stradiotto et al.


2003; Andrade et al. 2004; Gutz 2006; Fatibello-Filho 2007). Beside thisinfluence—the financial support of the Brazilian agencies and the SBQ’ssupport—the well-established graduate programs in analytical chemistryspread through Sao Paulo State have also exerted a strong contributionto the evolution of electroanalytical chemistry. Apart from the Sao PauloState, there is a strong dissemination of electroanalytical widespreadthroughout the country and other states such as Rio de Janeiro (6.0%),Paran�aa (3.6%), Rio Grande do Sul (3.2%), Maranhao (2.6%), Paraıba(2.5%), Pernambuco (2.4%), Minas Gerais (2.1%), Santa Catarina(1.0%), and Sergipe (1.0%) have also contributed in the last decades.Each one of the states of Mato Grosso, Bahia, Mato Grosso do Sul,Goi�aas, Cear�aa, Alagoas, Rio Grande do Norte, Piauı, and Amazonas havecontributed with a percentage smaller than 1% (Fatibello-Filho 2007).The number of articles in chemistry (all areas) published in Quımica Novain the period of 2000–2006 by the researchers of Sao Paulo State was 549,which corresponds to 43.6% of the total articles published by Brazilianauthors (Torresi et al. 2007). Data from specialized literature show asignificant contribution from Brazilian electroanalytical chemists inhigh-impact periodicals, and there is a very good adherence among workscarried out in Brazil and abroad, according to a comparison of workspresented in the 14th Brazilian Meeting on Analytical Chemistry (JoaoPessoa=PB, October 2007) and the XIV European Conference on Ana-lytical Chemistry (Antwerp=Belgium, September 2007) (Fatibello-Filho2007). In a similar study published five years ago regarding adherence,the same conclusions were reached (Fatibello-Filho et al. 2002), whichwas reinforced by Zagatto and S�aa (Zagatto and S�aa 2003).

The interest toward electroanalytical techniques continues to grow inBrazil, as can be observed by analyzing the last five meetings in the area(ENQA and SIBEE) (Fatibello-Filho 2007), the number of articles pub-lished by Brazilian authors in several journals, and also the number ofresearchers working in this area, as can be observed in the Lattes Plat-form CNPq (www.cnpq.br). Electroanalytical techniques offer the possi-bility of determining the analyte concentration directly in the samplewithout any pretreatment or chemical separation, as well as analyzingcolored materials and samples with dispersed solid particles and offeringthe possibility of the simultaneous determination of several substances.

In the 2004–2007 period, many research activities of Brazilian groupsincluded most electroanalytical techniques, and important reviews werepublished, such as recent advances and new perspectives of ISE (Torreset al. 2006), applications of Moleculary Imprinted Polymers (MIP) inthe development of chemical sensors (Tarley et al. 2005), electrochemicalmodified electrodes based on metal-salen complexes (Fatibello-Filho et al.2007), electrochemical sensors in microenviroments (Lowinsohn and


Bertotti 2006), applications of nanoelectrodes in analytical chemistry(Pereira et al. 2006), biosensors as a tool for the antioxidant status evalu-ation (Mello and Kubota 2007), modern electrochemical methods formonitoring of chemical carcinogens (Barek et al. 2005), applications ofthe square wave voltammetry (Souza et al. 2004) and the history,production, and characterization of boron-doped diamond films (Barroset al. 2005).

Potentiometry involving ISE with poly(vinyl chloride) membranefor aluminium(III) (Piccin et al. 2004) and furosemide (Dias et al. 2004),electrode of a second kind, namely PtjHgjHg2(analyte)xjgraphite fordiclofenac (Santini et al. 2006), ibuprofenate (Santini et al. 2006), mefe-namic acid (Santini et al. 2007), and naproxen (Santini et al. 2006), anda flexible minisensor based on manganese dioxide-composite for hydro-gen peroxide (Fagury et al. 2005) have been developed.

Electrochemical and microgravimetric studies on palladium phthalo-cyanine films were also described in this period (Gaffo et al. 2005).

The importance of the Micro Total Analysis System (mTAS) in ana-lytical chemistry, the application of the microfluidic devices for chemicaland biochemical processing using optical or electrochemical detectionwas recently revised (Tomazelli Coltro et al. 2007). Contactless conduc-tivity detection has been applied with success in the monitoring of theelectroosmotic flow in capillary electrophoresis (Saito et al. 2007; Felixet al. 2006).

Mercury continues to be a very attractive electrode material becauseof its chemical and physical properties, as pointed out by Stradiotto et al.(2003). Several electroanalytical techniques in conjunction with DroppingMercury Electrode (DME) and=or Hanging Mercury Drop Electrode(HMDE) have been used to determine simultaneously cadmium, copper,lead, and zinc in amino acid parenteral nutrition solutions (Nascimentoet al. 2006), arsenic(III) (Carvalho et al. 2006) and cadmium, lead,copper, and thallium (Carvalho et al. 2007) in water and in highly salinesamples, sunscreen agents in cosmetic products (Silva et al. 2006),2-nitronaphthale in drinking and river water samples (Peckova et al.2005), dopamine in injectable formulations (Winter et al. 2007), andamfepramone in pharmaceutical formulations (Carvalho et al. 2007).The development of multiple square wave voltammetry and the possibi-lities of its use for electroanalytical determinations of organic and inor-ganic compounds with the improvement of the signal-to-noise ratiosand detection limits 2–3 orders of magnitude lower than those obtainedwith conventional square wave voltammetry were demonstrated bySouza et al. (2007).

Several metallic microelectrodes have been presented in this period.A copper microelectrode was used as liquid chromatographic detector


for the determination of herbicide glyphosate in tomato juice (Coutinhoet al. 2007). A gold microelectrode and square wave voltammetry at highfrequencies was proposed to determine the herbicide paraquat in naturalwater and fruit juice samples (Souza and Machado 2005). A coppermicroelectrode was used to measured ethanol content in gasohol samples(Paixao et al. 2007). An electrochemically etched platinum microelectrodewas developed to determine ascorbic acid in fruits and vegetables (Paixaoet al. 2006). A bismuth-film microelectrode was designed for analysis oftrace heavy metals (Legeai et al. 2005), and a metallic (Ni=Cr) microelec-trode arrays for iodide quantification in small sample volumes(Lowinsohn et al. 2006). A rapid and easy way to produce microelectrodeensembles (Richter et al. 2007), and a gold nanoelectrode for iodide iniodized table salt and ophthalmic drugs (Pereira et al. 2006) wereproposed in this period also. The fabrication, electrochemical characteriza-tion, and the application of interdigitated array of gold electrodes as detectorfor flow injection analysis was described by Daniel and Gutz (2005).

Conventional sized metallic electrodes of gold for mercury quantifi-cation in natural water by stripping chronopotentiometry at constantcurrent (Augelli et al. 2005), gold electrodes obtained from recordableCDs for cysteine (Lowinsohn et al. 2006), copper for herbicide glyphosatein natural waters (Garcia and Rollemberg 2007), copper solid amalgamfor atrazine in natural water samples (Souza et al. 2005) and tungstenoxide films for iodate in table salt samples (Rocha et al. 2006) have alsobeen developed.

Boron-Doped Diamond (BDD) electrodes, which have receivedmuch attention in recent years, are very attractive for many potentialapplications, due to their outstanding properties, which are significantlydifferent from those of other conventional electrodes, e.g., the glassy car-bon or platinum electrode. In addition, BDD is corrosion stable in veryaggressive media, has very low and stable background current, extremeelectrochemical stability in both alkaline and acidic media, high responsesensitivity, and a very wide working potential window, which can belarger than 3.5 V. On the other hand, Suffredini et al. (2004) called theattention to the effect of electrochemical surface pretreatments on theresponse of BDD electrodes, specifically showing that cathodic polariza-tions dramatically increased the electroanalytical detection limits ofchlorophenols. The BDD electrodes, in conjunction with many electroa-nalytical techniques to determine aspartame in dietary products(Medeiros et al. 2007), carbaryl in natural waters (Codognoto et al.2006), 4-nitrophenol in pure and natural water samples (Pedrosa et al.2004), nitrite ions in aqueous solutions (Oliveira et al. 2007), andlidocaine in pharmaceutical preparations (Oliveira et al. 2007) haverecently appeared in the literature.


Brazilian groups have also contributed in the preparation, character-ization, and application of a plethora of electrodes based on carbon pastemodified with 2-aminothiazole organofunctionalized silica to determinecopper (Takeuchi et al. 2007) and nickel in ethanol fuel (Takeuchi et al.2007), with SBA-15 nanostructured silica organofunctionalized with 2-benzothiazolethiol to determine cadmium(II) in natural water samples(Cesarino et al. 2007), with copper(II) hexacyanoferrate(III) to determineN-acetylcysteine in pharmaceutical formulations (Suarez et al. 2006),with mer-[RuCl3(dppd)(4-pic)] complex to determine dopamine andascorbic acid in synthetic and pharmaceutical samples (Santos et al.2007), with lead dioxide immobilized in a polyester resin to determineL-dopa and carbidopa in pharmaceuticals (Melo et al. 2007), with chito-san to determine mercury(II) in water (Marcolino-Junior et al. 2007) andwith polyaniline to determine imazaquin in synthetic samples (Consolinet al. 2006). Graphite-polyurethane composite electrodes have beendeveloped by Cervini’s group to determine atenolol (Cervini et al.2007) and imipramine (Toledo et al. 2006) in pharmaceutical productsand also hidroquinone in photographic developers (Mendes et al. 2006).

Glassy Carbon Electrodes (GCE) have been used with success in thedetermination of copper and lead (Cardoso et al. 2007) and quinoline andpyridine in gasoline (Okumura and Stardiotto 2007). A very good alter-native to carbon solid electrode was demonstrated by Felix et al. (2007).In this work, a carbon film resistor electrode was successfully applied foramperometric determination of acetaminophen in pharmaceutical formu-lations. Glassy carbon electrodes modified with films of polyglutamicacid were used to determine rutin in pharmaceuticals, with poly-L-lysineto determine cysteine in food supplement samples (Luz et al. 2006) andwith a tetraruthenated porphyrin to determine sodium metabisulfite ininjection formulations (Quintino et al. 2006). Alternative routes toprepare silver hexacyanoferrate(II)=polyanyline composite thin filmdeposited in platinum electrode (Azevedo et al. 2006), platinum nanopar-ticles incorporated into a polyaniline film to determine ethanol in sulfuricacid solutions (Fungaro et al. 2007), and the immobilization of hexacya-noferrate on a gold self-assembled monolayer and its application as asensor for ascorbic acid were recently published.

Amperometric methods associated with flow injection analysis havealso received attention in Brazil. Several flow cell configurations and work-ing electrodes were proposed for the determination flavonoids in tea sam-ples (Pedrosa et al. 2006), phosphite in fertilizers (Franzini et al. 2007),procaine in pharmaceutical formulation (Bergamini et al. 2007), L-lactatein blood samples (Lowinsohn and Bertotti 2007), paracetamol in pharma-ceuticals (Pedrosa et al. 2006), and L-dopa in pharmaceuticals (Teixeiraet al. 2007). A sequential injection system for determining methyl


parathion in water samples and a potentiometric flow injection system todetermine inositol phosphates and phosphate in seeds and grains, animalnursing feed, soybean meal, and corn (Perra et al. 2005) were also proposed.

There are at least seven Brazilian groups developing new biosensors,immunosensors, and=or genosensors for determination of severalanalytes. Most of those developments were based on immobilization ofenzymes such as uricase in layer-by-layer (LBL) films (Moraes et al.2007), glucose oxidase in LBL films (Ferreira et al. 2004; Crespilho etal. 2006), glucose oxidase in a polypyrrole matrix (Alves et al. 2006), alde-hyde dehydrogenase in a poly(vinyl alcohol) matrix (Lima et al. 2007),laccase entrapped in a carbon paste (Santhiago et al. 2007) and tyroni-nase in polycarbonate support (Albuquerque and Ferreira 2007).Recently in Brazil, there has been an increased preference for using veg-etable or plant crude extracts (homogenates) and plant tissues instead ofpurified enzymes for preparation of electrochemical biosensors(Fatibello-Filho and Vieira 2002). Vegetable or plant tissues may be useddirectly with minimal preparation. This class of biocatalytic materialsmaintains the enzyme of interest in its natural environment, often result-ing in better stability, lower cost, and higher enzyme activity, comparedwith those biosensors using the corresponding purified enzyme. Otheradvantages comprise simplicity of biosensor construction, and the requiredcofactors may already be present in the vegetable cell and may not need tobe separately immobilized. Green beans (Phaseolus vulgaris) crude extract(Fernandes et al. 2007), gilo (Solanum gilo) crude extract (Oliveira et al.2006) and coconut (Cocus nucifera L.) tissue fibers (Kosan et al. 2007) wererecently employed as a source of peroxidase in the preparation of biosensors.In another work, palm tree fruits (Livistona chinensis) were employed as asource of polyphenol oxidase in the construction of a biosensor, to determineepinephrine in pharmaceuticals. An immunosensor for the diagnosis ofChagas’ disease (Ferreira et al. 2005) and a genosensor for the diagnosis ofHepatitis C virus (Riccardi et al. 2006) were recently developed. Finally, bio-mimetic sensors for hydroquinone in cosmetics (Oliveira et al. 2007a;Oliveira et al. 2007b) and phenolic compounds in water samples (Franciscoet al. 2007) have also been developed and are very good alternatives to sub-stitute the respectively enzymes.

All these developments demonstrate the strength of electroanalyticalchemistry in Brazil, and we foresee strong and continuous growth in this area.

ENVIRONMENTAL ANALYTICAL CHEMISTRY

Throughout the last four years, environmental analytical chemistry inBrazil was responsible for almost 50 original articles, published in about


20 of the most accessed international periodicals devoted to the field ofanalytical chemistry.

The number of publications was almost equal in 2004 and 2005(�20% of the whole for both years), but it duplicated in 2006, and dur-ing the year of 2007 was about the same as the total published in the firsttwo years. Although researchers and=or research groups could be ident-ified in three out of the five geographical regions of Brazil, they are stillconcentrated in the southeastern region, especially in the Sao Paulo State,which alone contributes almost 60% of the total published research in thescope of this data collection (Almeida et al. 2006; Brondi and Lancas2004; Brondi et al. 2005; Buchmann et al. 2006; Codognoto et al. 2004;Franca et al. 2007; De Souza 2005; De Souza 2007; Favaro et al. 2006;Felix et al. 2006; Figueiredo et al. 2006; Flues et al. 2006; Kfouri et al.2005; Pereira et al. 2004; Rizzutto et al. 2006; Rodriguez et al. 2006;Salvador et al. 2004; Saueia et al. 2005; Silva et al. 2005; Silva 2006;Simoes et al. 2006; Titato and Lancas 2005; Titato and Lancas2006; Menegario et al. 2007; Vives et al. 2006; Barbosa et al. 2007; Meloet al. 2004; Moreira et al. 2006; Tarley 2004; Tarley 2005). The othergroups which could be identified were localized at Rio de Janeiro (10%of contribution) (Araujo et al. 2007; Barreto et al. 2007; Justo et al.2006; Sella et al. 2004; Oliveira et al. 2005); Bahia and Rio Grande doSul (6% of contribution each one) (Duarte et al. 2007; Amorim 2007;Bezerra 2006; Campos et al. 2006; Lima et al. 2004; Brasil et al. 2005);Minas Gerais and Paran�aa (4% of contribution each one) (Menezes etal. 2004; Barbosa et al. 2007; Falate et al. 2005; Sodre et al. 2005) andalso at Maranhao (Badea et al. 2006), Pernambuco (Junior et al. 2006),Santa Catarina (dos Santos 2007), and Sergipe (Dorea et al. 2007), eachone contributing with about 2% of the total publications considered,respectively.

In the Sao Paulo State, the research groups are spread across thecities where the main universities and research institutions are also loca-lized. Thus, cities such as Sao Paulo, Sao Carlos, Campinas, Araraquara,Piracicaba, and Ribeirao Preto are, each one, centers for environmentalanalytical chemistry development, together with their researchinstitutions.

The research in Rio de Janeiro was localized mainly in Niter�ooi, at theFederal University (UFF). However, it was done also at the MilitaryInstitute of Engineering (IME), the State University (UERJ), and atthe North State University (UENF). Although no articles could be loca-lized as published in the journals and the time span considered in thiswork, the Pontifical Catholic University (PUC-RJ) must be pointed outas a center of traditional and strong research groups in Brazilian environ-mental analytical chemistry. In Bahia, the published works found were


from researchers of the Federal University (UFBA) and the SouthwestState University (UESB). Rio Grande do Sul also contributed with pub-lications coming from researchers of Porto Alegre (Federal University ofRio Grande do Sul) and Santa Maria (Federal University of SantaMaria), while in Minas Gerais, works are being done in Belo Horizonte,at UFMG and CNEN-CDTN, and Alfenas, at the local federal univer-sity (UNIFAL). Although several of the research and publications arethe result of cooperation among two or more research institutions, inthese cases, however, we opt to follow the first addressed institution,which would be the top institution according to the Web of Sciencedatabase.

The distribution of publications according to the type of studiedmatrix is shown in Fig 1. As can be seen, papers focused on water samplesanalysis represent more than 50% of the total, followed by those focusedin air and soil samples, both with the same level of contribution. The con-tribution must be also be highlighted, of what we choose to refer to hereas ‘‘other,’’ meaning papers which had the terms ‘‘environment’’ or‘‘environmental’’ as keywords despite their primary application not beingin environmental matrices, although they had the full conditions for this.

Regarding the analyte, five articles were found with ‘‘metals’’ andnine with ‘‘elements’’ mentioned either in their title or in their keywords.However, if the search was extended to the abstracts, these numbers roseto seven and fifteen, respectively. Also, there were cases for which refer-ence was made to specific elements (e.g., lead, cadmium, or antimony).For organic species, the terms mentioned either in the title or in theabstract were ‘‘pesticides’’ (six articles), ‘‘PAHS’’ (three articles), and‘‘herbicides’’ ‘‘BTEX’’ and ‘‘aldehydes’’ (one article, each one). Probablythis number would have increased, as for the inorganic species, if we hadmade searches for specific compounds. The results are summarized inFig. 2.

Looking to the techniques more significantly employed, radioanaly-tical techniques were the most frequent, with neutron activation analysisresponsible alone for about 35% of the total (Almeida et al. 2006;Buchmann et al. 2006; Franca et al. 2007; Favaro et al. 2006; Figueiredo

Figure 1. Relative contribution, according to the matrix studied.


et al. 2006; Flues et al. 2006; Junior et al. 2006; Justo et al. 2006; Kfouriet al. 2005; Menezes et al. 2004; Moreira et al. 2006; Rizzutto et al. 2006;Saueia et al. 2005; Silva 2005; Silva 2006; Vives et al. 2006). They werefollowed by the atomic (absorption or emission) spectrometries (Amorim2007; Barbosa et al. 2007; Bezerra 2006; Brasil et al. 2005; Dorea et al.2007; dos Santos 2007; Lima et al. 2004; Menegario et al. 2007; Oliveiraet al. 2005; Tarley 2004; Tarley 2005; Sella et al. 2004). Mass spec-trometry, coupled to gas chromatography (GC-MS), or liquid chromato-graphy (LC-MS) either by ICP or APCI ionization sources, was thehyphenated technique employed in about 14% of the research paperscomputed (Barreto et al. 2007; Dorea et al. 2007; Duarte et al. 2007;Rodriguez et al. 2006; Titato and Lancas 2006; Buchmann et al. 2006),followed by the electro analysis (Codognoto et al. 2004; De Souza2007; Simoes et al. 2006; De Souza 2005) and liquid chromatography(Brondi and Lancas 2004; Brondi et al. 2005; Melo et al. 2004; Titatoand Lancas 2005), which were, each one, the applied techniques in 8%of the works done. Sensors and biosensors were cited in the time spanconsidered, in 6% of the total production (Badea et al. 2006; Falateet al. 2005; Felix et al. 2006). Although this still represents a less signifi-cant contribution, it is expected for this field to experience a significantgrowth in the near future. The results are summarized in Fig. 3.

Research works based on radioanalysis were, as expected, more fre-quently produced by groups at institutions where this kind of technique isthe common analysis tool, such as IPEN and CNEN in Sao Paulo, whichwere responsible alone for about 65% of all the papers. Nevertheless,other groups and institutions, such as UFPE (Pernambuco), CDTNand UFMG (Minas Gerais), and IME (Rio de Janeiro), for example,are also working with the radioanalytical techniques.

On the other hand, the other commonly employed techniques werespread throughout several institutions localized in the south (SC andRS), southeast (RJ, SP, and MG) and northeast (BA, SE) of Brazil—possibly because, despite the Brazilian region or state, equipment

Figure 2. Relative contribution, according to the analytes determined.


required in this case is, in general, more accessible to researchers at theuniversities and research centers.

Regarding the periodicals in which articles were published, the resultsare summarized in Fig. 4. It is interesting to observe that all researchbased on the radioanalytical techniques was published in a uniqueperiodical, namely the Journal of Radioanalytical and Nuclear Chemistry.Following this journal, but with a minor participation, are featured jour-nals devoted to the general field of analytical techniques, such as, forexample, the Microchemical Journal, Microchimica Acta, and the Inter-national Journal of Environmental Analytical Chemistry. Almost allpapers were published in journals from outside Brazil, with the onlytwo exceptions being one article in the JBCS and another in QuimicaNova. The first one, published in 2006, was about cooperation amongresearchers from Brazil, in Maranhao, and Romania, and France, for

Figure 4. Number of published papers by periodical.

Figure 3. Relative contribution, according to the employed technique.


development of biosensors for organophosporous pesticides detection inaqueous media. The second one, also from 2006, was about the develop-ment, construction, and application of passive air samplers, and suchactivities used as in laboratory classrooms for undergraduate students.

In conclusion, this datacollecting work identified a very productivecommunity of environmental analytical chemists in Brazil, who havebeen publishing a significant number of original research articles forthe last four years, with focus in a wide variety of techniques, matrices,and analytes. However, it is clear that a challenge remains, and this isto support and to strengthen groups outside the southeastern region,especially from the northern and western states of Brazil, giving themconditions to enhance their contributions to the field.

PRECONCENTRATION AND SEPARATION PROCEDURES

Several Brazilian research groups have performed preconcentration pro-cedures for determination of inorganic and organic species in a plethoraof sample types. These procedures have been established using separationtechniques such as Solid Phase Extraction (SPE), liquid-liquid extraction,cloud point extraction, and co-precipitation, including knotted reactorsystems, employing mainly spectroanalytical techniques such as FlameAtomic Absorption Spectrometry (FAAS), Graphite Furnace AtomicAbsorption Spectrometry (GF AAS), Cold Vapor Atomic AbsorptionSpectrometry (CV AAS), Inductively Coupled Plasma-Optical EmissionSpectrometry (ICP-OES), Inductively Coupled Plasma Mass Spec-trometry (ICP-MS), and also Molecular Absorption Spectrophotometry(MAS) (Korn et al.2006; Lemos et al. 2007).

The most used separation technique was SPE, and many proceduresby batch and on-line systems have been published. Some researchers haveused common sorbents such as cellulose paper (Teixeira et al. 2007), acti-vated carbon (Quinaia et al. 2006), naphthalene (Anjos et al. 2007), silicamodified with zirconium oxide (Macarovscha et al. 2007), silica gel che-mically modified with niobium(V) oxide (Dutra et al. 2006), polyurethanefoam (Tarley et al. 2005; Santos et al. 2004; Santos et al. 2006), silica gelloaded with 1,3-diaminepropane-3-propyl (de Moraes et al. 2005) andAmberlite resins (Silva et al. 2005; Amorim and Bezerra 2007). Otherspublished papers have proposed new solid phase as: multiwall carbonnanotubes (Barbosa et al. 2007), sugar cane bagasse (Borges et al.2006), grape bagasse (Matos and Arruda 2006), and rice husks (Tarleyet al. 2004). Other researchers have worked with functionalization ofresins, and excellent results were obtained (Cassela et al. 2005; Silvaet al. 2004; Lemos et al. 2005). Among other works found was a


procedure for chromium speciation and pre-concentration using zirco-nium(IV) and zirconium(VI) phosphate chemically immobilized onto asilica gel surface, employing a flow system and FAAS (Maltez andCarasek 2005). A field sampling system for determination of cadmiumand nickel in fresh water by FAAS was proposed, using a minicolumnof Amberlite XAD-2 loaded with TAM reagent (dos Santos et al.2005). A system using activated alumina was proposed for determinationand speciation of arsenic, employing hydride-generation atomic absorp-tion spectrometry (Bortoleto and Cadore2005). In analytical proceduresfor determination of organic species, SPE has been also intensely used.Bortoluzzi et al. used SPE in the preconcentration step for determinationof pesticide residues in rural wells and surface waters, employing GasChromatography with Electron Capture Detection (GC-ECD) or High-Performance Liquid Chromatography with Diode Array Detection(HPLC-DAD) (Bortoluzzi et al. 2005). Molecularly imprinted polymershave been also proposed for selective extraction of organic species(Figueiredo et al. 2005; Tarley et al. 2006). Montmorillonite was testedas an adsorbent for extraction and quantification of several herbicides(Zarpon et al. 2006). Poly(methyloctylsiloxane) immobilized on silicahas been investigated as sorbent in pre-concentration procedure forquantification of pesticides (Queiroz et al. 2006). A method for determi-nation of chloramphenicol (CAP) antibiotic in milk, powder milk, andhoney was established using SPE for pre-concentration and quantifi-cation by mass spectrometry (Martins et al. 2006).

Cloud Point Extraction (CPE) is another separation technique fre-quently employed by Brazilian researchers. A recently published book(Bezerra and Ferreira 2006) and a review paper (Bezerra et al. 2005) showadvantages and applications of this technique. Silva and co-workers haveused CPE for separation, pre-concentration, and determination of metalions employing ICP-MS (Silva et al. 2001), GFAAS (Maranhao et al.2007) and CV AAS (Dittert et al. 2007). Other groups have also usedCPE for determination of metal ions using FAAS (Lemos et al. 2007;Bezerra et al.2007; Coelho and Arruda 2005), ICP-OES (Bezerra et al.2007), thermospray FAAS (Donati et al. 2006), and MAS (Ferreiraet al. 2006). Lopes et al. used CPE for determination of casein proteinsof cow milk, employing mass spectrometry (Lopes et al. 2007). CloudPE was also used for preconcentration and determination of disulfotonin surface waters using gas chromatography (Faria et al. 2007).

Pre-concentration procedures based on co-precipitation techniquehave rarely been used by Brazilian researchers. A procedure involvingsolid sampling analysis by FAAS was proposed for lead determinationin seawater samples after co-precipitation using naphthalene and alizarinred (Korn et al. 2005). On-line preconcentration systems involving


knotted reactors have been proposed for determination of metal ionsemploying ICP-MS (Silva et al. 2004) and FAAS (Cerutti et al. 2004;Souza et al. 2005).

Analytical procedures using liquid-liquid extraction have beenavoided, due to the need of organic solvents. However, some strategieshave been proposed for decreasing the solvent volume needed. An auto-mated system for liquid-liquid extraction, based on a new micro-batchextraction chamber was proposed for determination of copper (Dinizet al. 2004). An interesting method was recently proposed for determi-nation of lead by electrothermal atomic absorption spectrometry. It dealswith a single drop micro-extraction where lead was extracted as theO,O-diethyldithiophosphate (DDTP) complex from aqueous solutioninto a drop of chloroform immersed in the solution (Maltez et al. 2008).

A critical analysis of the published papers about pre-concentration=separation in the period from 2004 to 2007 shows thatSPE is the most used technique by Brazilian researchers. Several papershave been published about preparation of new solid phases, including func-tionalized resins and molecularly imprinted polymers. On the other hand,liquid-liquid extraction has been substituted by CPE with great efficiency.

SPECTROCHEMICAL ANALYSIS

The period was marked by intense activity in the spectrochemical area,and the most remarkable Brazilian contributions are occurring in atomicspectrometry techniques with different atomizers and instrumentalarrangements. One of the highlights of the period was the strongBrazilian contribution in the Young Analytical Scientists Issue publishedby the Journal of Analytical Atomic Spectrometry in November 2006. Thisissue had a total of 29 papers, and 6 of them were published by Braziliangroups from different regions of the country. Two of these papers dealtwith tube atomizers in FAAS (Petrucelli et al. 2006; Tarley et al. 2006),High-Resolution Continuum Source AAS (HR-CS-AAS) (Silva et al.2006), mercury determination in petroleum products by ETAAS (Santoset al. 2006), and the use of ICP-MS and ICP-OES for direct analysis offuel ethanol and determination of trace elements in crude oil, respectively(Saint Pierre et al. 2006a; Souza et al. 2006). We can foresee a continuousdevelopment of these areas.

Strong research activities are concentrated in the development ofapplications using HR-CS-AAS. Based on the new instrument capabili-ties, particularly those related to background correction, new chemicalknowledge is amassing, such as the vanadium species in petroleum andderivatives (Damin et al. 2005; Amorim et al. 2007) and also about the


use of internal standards in AAS measurements (Oliveira et al. 2004; Cor-reia and Oliveira 2005). The same technique was successfully applied fordirect solid analysis of many analytes in coal samples, such as recentlydemonstrated for lead (Borges et al. 2006). An interesting strategy alsobased in direct solid sampling using conventional flame AAS was pro-posed by Flores et al. (2004) for manganese determination in coal sam-ples. The main aspect of this work was the use of a simple andeffective lab-made device for solid analysis. This device was previouslyused by this same group for determination of cadmium and copper inbiological samples. The use of a continuum source was also associatedwith a tungsten coil atomizer (N�oobrega et al. 2005). The performanceof this atomizer for emission measurements was recently demonstrated(Rust et al. 2006). Brazilian groups are also contributing to the develop-ment of analytical applications with thermospray flame furnace AAS,and some of these works are investigating the coupling of preconcentra-tion columns and TS-FF-AAS (Pereira et al. 2004) and cloud pointextraction for cobalt in biological materials (Donati et al. 2006). A veryinteresting and sound study about the thermospray formation at low flowrate was presented by Brancalion et al. (2007). The Leidenfrost effectplays an important role in the process, with the aid of a high-speed cam-era. On the other hand, other alternatives for improving FAAS sensitivitywere demonstrated for determination of cadmium and lead in foods,using beam injection flame furnace AAS (Aleixo et al. 2004). Finally,the lifetime of graphite tubes as electrothermal atomizers was improved,using permanent chemical modifiers, such as iridium plus rhodium (Gia-comelli et al. 2004) and tungsten plus rhodium (Nomura et al. 2004).

All these strategies expand the capabilities of the AAS techniquesand increase their capacity to cope with modern multielement techniquesbased on inductively coupled plasmas (ICP). Some research groups arealso developing procedures using ICP coupled to optical emission spec-trometry or mass spectrometry, but the use of this latter technique isbelow the necessity. Taking into account the leadership of Brazil in theproduction of biofuels, there are applications of ICP-MS with ultrasonicnebulizer (Saint Pierre et al. 2006a) and coupled to electrothermal vapor-ization (Saint Pierre et al. 2006b) for fuel ethanol analysis. Effluents of apetroleum refinery were also analyzed by ion chromatography coupled toICP-MS for speciation of selenium (Miekeley et al. 2005). Additionally,the use of isotopic dilution ICP-MS was applied for determination ofmolybdenum in plants (Bellato et al. 2005). On the other hand, the useof ICP-OES is mainly related to applications employing axial view, aswas recently reviewed (Trevizan and N�oobrega 2007).

Investigations with laser ionization breakdown spectroscopy are stillincipient; however, an excellent review published by Pasquini et al. (2007)


indicates a trend to evolution in this area, and there are at least two Bra-zilian groups investigating the instrumentation and applications of LIBSfor routine analysis.

Other important reviews were published about the application ofmultivariate techniques in optimization of spectroanalytical methods(Ferreira et al. 2007), direct solid analysis by ETAAS (Vale et al.2006), and slurry analysis of inorganic samples by inductively coupledplasmas (Santos and N�oobrega 2006).

Finally, there is a remarkable development of useful procedures fordeterminations of manganese and zinc in powdered chocolate slurries(Silva et al. 2006), metals in sweeteners (Sousa et al. 2006), aluminumin soft drinks (Amorim et al. 2006), and so on. Last, but not least, thereare two recent papers investigating the use of scanner image analysis forquantification of mercury spot tests (Paciornik et al. 2006) and titrations(Gaiao et al. 2006).

Sample Preparation

There are well-established and consolidated groups developing new tech-niques and procedures for sample preparation. Most developments arebased on microwave-assisted procedures and deal with sample digestionfor inorganic analysis. However, procedures using ultrasound are alsobeing investigated, and there are important contributions in both areas.

One of the main developments was the proposal of microwaveinduced combustion by Flores’s group (2004) and its application for bio-logical materials (Mesko et al. 2006). Another important contribution inthe area was a book edited by Arruda (2007) emphasizing recent achieve-ments in sample preparation strategies.

In addition to the proposals using cavity-microwave oven and closed-vessels, focused-microwave radiation was employed for gradual sampleaddition to preheated acids (Santos et al. 2005) and to the preparationof industrial effluent analysis for free and total cyanide determinations(Quaresma et al. 2007). Focused-microwave was also employed foracid-vapor extraction of cobalt and iron in biological samples (Araujoet al. 2004) and medicinal plants decomposition in mini-vials forcadmium determination (Brancallion and Arruda 2005).

The optimization of digestion parameters in microwave ovens wascarried out, using factorial design for samples of beans and lubricatingoil (Costa et al. 2006; Costa et al. 2005).

The use of ultrasound for sample preparation was reviewed bySantos, Jr., et al. (2006). The most usual application of ultrasoundis in extraction procedures, as for example cadmium and lead in foods


(Aleixo et al. 2004). Ultrasound can also be employed for generation ofreagents as demonstrated for chloride and hypochlorite (Korn et al.2005) and can also influence chemical processes, such as the reductionof nitrate to nitrite (Silva et al. 2007).

Despite sound application of microwave radiation and ultrasound, itis necessary to investigate less drastic procedures for sample preparationbecause of needs imposed by speciation analysis. This could be performedby using sample solubilization in alkaline medium as applied for solubi-lization of fish muscle tissue (Melo et al. 2005) and recently reviewed byN�oobrega et al. (2006). In this sense, metalloprotein analysis is being inves-tigated for horse chestnuts (Magalhaes and Arruda 2007) and soybeanseeds (Sussulini et al. 2007).

These works are representative of evolution trends in the samplepreparation area, and it may be supposed that future developments willfocus on soft chemical procedures suitable for speciation analysis.

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A Glimpse of Recent Developments in Brazilian Analytical Chemistry

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