Brazilian Journal of Analytical Chemistry - BRJAC - Brazilian Journal ...

More documents

Recommendations

Info

a m u l t iC o m m u t a t e d flow system f o r peraCetiC a C i d determination The sample consumption was 600 times lower for the flow system than for the reference method. The sampling throughput was 80 injections per hour, for the proposed system, which indicates that laboratory productivity would be enhanced by 3.6 or 18 times, compared to the Vacu-vials ® Kit and to the reference method, respectively. The performance of the multicommuted flow injection analysis process (MCFIA) in real sample analysis was evaluated using three disinfectant samples that were assayed using both the proposed procedure and the reference permanganate titration [12] method. The results are presented in Table III. taBlE iii. PEraCEtiC aCid C o n C E n t ra t i o n s (g l -1 ) in s a m P l E d i s i n fE C t a n t s o B t a i nE d By thE P ro P o s E d ProCEdurE (mCfia) a n d thE rEfErEnCE m E t h o d [12]. sa m P l E s Pro P o s E d m E t h o d (g l -1 ) rEfErEnCE m E t h o d (g l -1 ) rE l a t i v E Er r o r (%) 1 166.9 ± 16.4 163.4 ± 13.2 - 2.14 2 169.8 ± 18.2 162.1 ± 4.8 - 4.75 3 77.4 ± 6.4 101.3 ± 21.9 23.6 The data reported indicate the presence of peracetic acid concentrations between 77 and 170 g L -1 with a RSD between 6.4 and 18.2 % using the method under study, compared with 4.8 to 21.9% for the reference method. The values of relative errors were both positive and negative, indicating that both procedures provide comparable results without systematic errors. In the reference method, the hydrogen peroxide present is first titrated under cold conditions with a standard solution of potassium permanganate. This titration eliminates the peroxide. Potassium iodide is then rapidly added and the iodine liberated by the peracid is titrated with standard thiosulphate solution [12]. In the proposed method there is no step to eliminate peroxide. As mentioned, the proposed method is based on the reaction of PAA with I - solution. The concentration of I - in the sample solution should be high enough to dissolve the I 2 resulting from the reaction of PAA (and H 2 O 2 ) with I - (reference 3). Probably, in sample 3, there was a high concentration H 2 O 2 and this reacted with I - generating a larger amount of I 2 . Thus, the excess of I - was not enough to solubilize I 2 , so that the analytical signal was smaller, resulting in a lower PAA concentration. The standard addition method was also used to test the accuracy of the assessment samples, yielding the results showed in Table IV. As seen, the recoveries obtained are within the range of 95 to 106 %, which is considered acceptable for this type of sample. sa m P l E s taBlE iv. rECovEriEs o f PEraCEtiC aCid in w a t E r samPlEs. rEsults ExPrEssEd in m g l -1 Co n C E n t r a t i o n 162 Br J Anal Chem A n = 3 a d d E d st a n d a rd a d d i t i o n mE t h o d a rECovEry (%) 1 1.00 1.01 ± 0.04 101 ± 4 2 1.69 1.79 ± 0.16 106 ± 9 3 1.35 1.32 ± 0.05 97 ± 3 4 1.22 1.17 ± 0.09 95 ± 7 5 2.00 1.94 ± 0.12 97 ± 5 4. co n c l u s Io n s The proposed methodology (MCFIA) with spectrophotometric detection showed robustness and versatility and offers several advantages over the reference method for routine analyses of peracetic acid samples (permanganate titration) [12] and the Vacu-vials ® kit, such as higher analytical frequency and lower cost. The reaction and detection are integrated in the same manifold and all operations can be controlled from the computer, providing simplicity and reliability when compared to permanganate titration. Considering the advantages presented, it is feasible to employ this procedure for the analysis of peracetic acid in any water treatment laboratory. ac K n o w l e d g e m e n t s The authors thank the CNPq (Proc. 472358/2006-5) and CNPq/FACEPE/PRONEX (Proc. 0333-3.07/06) for financial support and Microbiana Descontaminações Ltda (São Paulo, SP – Brazil) for samples of peracetic acid. references 1. Alvaro, J.E.; Moreno, S.; Dianez, F.; Santos, M.; Carrasco, G.; Urrestarazu, M. Effects of peracetic acid disinfectant on the postharvest of some fresh vegetables. J. Food Eng. 2009, 95, 11-15. 2. Harms, D.; Karst, U. Rapid and selective determination of peroxyacetic acid in disinfectants using flow injection analysis. Anal.Chim. Acta 1999, 389, 233-238. 3. Awad, M.I.; Oritani, T.; Ohsaka, T. Simultaneous potentiometric determination of peracetic acid and hydrogen peroxide. Anal. Chem. 2003, 75, 2688-2693. 4. Pettas, I.A.; Karayannis, M.I. Simultaneous spectra-kinetic determination of peracetic acid and hydrogen peroxide in a brewery cleaning-in-place disinfection process. Anal. Chim. Acta 2004, 522, 275-280. 5. Baldry, M.G.C. The bactericidal, fungicidal and sporicidal properties of hydrogen peroxide and peracetic acid. J. Appl. Bacteriol. 1983, 54, 417-423. 6. Pinkernell, U.; Luke, H.J.; Karst, U. Selective photometric determination of peroxycarboxylic acids in the presence of
hydrogen peroxide. Analyst 1997, 122, 567-571. 7. Baldry, M.G.C.; Cavadore, A.; French, M.S.; Massa, G.; Rodrigues, L.M.; Schirch, P.F.T.; Threadgold, T.L. Effluent disinfection in warm climates with peracetic acid. Water Sci. Technol. 1995, 31, 161-164. 8. Rajala-Mustonen, R.L.; Toivola, P.S.; Heinonen-Tanski, H. Effects of peracetic acid and UV irradiation on the inactivation of coliphages in wastewater. Water Sci. Technol. 1997, 35, 237-241. 9. Kitis, M. Disinfection of wastewater with peracetic acid: a review. Environ. Int. 2004, 30, 47-55. 10. Souza, J.B.; Daniel, L.A. Comparação entre hipoclorito de sódio e ácido peracético na inativação de E. Coli, colifagos e C. perfringens em água com elevada concentração de matéria orgânica. Eng. Sanit. Ambient. 2005, 10, 111- 117. 11. Pinkernell, U.; Effkemann, S.; Nitzsche, F.; Karst, U. Rapid high-performance liquid chromatographic method for the determination of peroxyacetic acid. J. Chromatogr. A 1996, 730, 203-208. 12. Greenspan, F.P.; MacKellar, D.G. Analysis of aliphatic per acids. Anal. Chem. 1948, 20, 1061-1063. 13. Pinkernell, U.; Effkemann, S.; Karst, U. Simultaneous HPLC determination of peroxyacetic acid and hydrogen peroxide. Anal. Chem. 1997, 69, 3623-3627. 14. Sanz, V.; Marcos, S.; Galbán, J. Hydrogen peroxide and peracetic acid determination in waste water using a reversible reagentless biosensor. Anal. Chim. Acta 2007, 583, 332-339. 15. Higashi, N; Yokota, H.; Hiraki, S.; Ozak, Y. Direct determination of peracetic acid, hydrogen peroxide and acetic acid in disinfectant solutions by Far-Ultraviolet Absorption Spectroscopy, Anal. Chem. 2005, 77, 2272- 2277. 16. Galbán, J.; Sanz, V.; Marcos, S. Selective peracetic acid determination in the presence of hydrogen peroxide using a label free enzymatic method based on catalase. Anal. Bioanal. Chem. 2010, 398, 2117-2124. 17. Di Furia, F.; Prato, M.; Quintly, U.; Salvagno, S.; Scorrano, G. Gas-liquid-chromatographic method for the determination of peracids in the presence of a large excess of hydrogenperoxide. Analyst 1984, 109, 985-987. 18. Ruzicka, J.; Marshall, G. D. Sequential injection - a new concept for chemical sensors, process analysis and laboratory assays. Anal. Chim. Acta 1990, 237, 329-343. 19. Reis, B.F.; Giné, M.F.; Zagatto, E.A.G.; Lima, J.L.F.C.; Lapa, R. Multicommutation in flow analysis. Part 1. Binary sampling: concepts, instrumentation and www.brjac.com.br Silva et al. spectrophotometric determination of iron in plant digests. Anal. Chim Acta 1994, 293, 129-138. 20. Lavorante, A.F.; Feres, M.A.; Reis, B.F. Multi-commutation in flow analysis: a versatile tool for the development of the automatic analytical procedure focused on the reduction of reagent consumption. Spectrosc. Lett. 2006, 39, 631- 650. 21. Feres, M.A.; Zagatto, E.A.G.; Santos, J.L.M.; Lima, J.L.F.C. The concept of multi-commutation in Flow Analysis, in: M. Trojanowicz (Ed.), Advances in Flow Analyisis, Wiley- VCH Verlag GmbH & Co. Weinheim, 2008, pp. 167-192. 22. Lapa, R.A.S.; Lima, J.L.F.C.; Reis, B.F.; Santos, J.L.M.; Zagatto, E.A.G. Multi-pumping in flow analysis: concepts, instrumentation, potentialities. Anal. Chim. Acta 2002, 466, 125-132. 23. Lavorante, A.F.; Morales-Rubio, A.; De la Guardia, M.; Reis, B.F. A multicommuted stop-flow system employing LEDs-based photometer for the sequential determination of anionic and cationic surfactants in water. Anal. Chim. Acta 2007, 600, 58-65. 24. Lima, J.L.F.C.; Sá, S.M.O.; Santos, J.L.M.; Zagatto, E.A.G. Multi-pumping flow system for the spectrophotometric determination of dipyrone in pharmaceutical preparations. J. Pharm. Biomed. Anal. 2003, 32, 1011-1017. 25. Dias, A.C.B.; Santos, J.L.M.; Lima, J.L.F.C.; Zagatto, E.A.G. Multi-pumping flow system for spectrophotometric determination of bromhexine. Anal. Chim. Acta 2003, 499, 107-113. 26. Lima, J.L.F.C.; Santos, J.L.M.; Dias, A.C.B.; Ribeiro, M.F.T.; Zagatto, E.A.G. Multi-pumping flow systems: an automation tool. Talanta 2004, 64, 1091-1098. 27. Pons, C.; Tóth I.V.; Rangel, A.O.S.S.; Forteza, R.; Cerdà, V. Multi-pumping flow system for the determination of dissolved orthophosphate and dissolved organic phosphorus in wastewater samples. Anal. Chim. Acta 2006, 572, 148-154. 28. Ródenas–Torralba, E.; Morales-Rubio, A.; Lavorante, A.F.; Reis, B.F.; De la Guardia, M. Micropumping multicommutation turbidimetric analysis of waters. Talanta 2007, 73, 742-747. 29. Ródenas–Torralba, E.; Rocha, F.R.P.; Reis, B.F.; Morales- Rubio, A.; De la Guardia, M. Evaluation of a multicommuted flow system for photometric environmental measurements. J. Autom. Methods Manage. Chem. 2006, 2006, 1-9. 30. Davies, D.M.; Deary, M.E. Determination of peracids in the presence of a large excess of hydrogen peroxide using a rapid and convenient spectrophotometric method. Analyst 1988, 113, 1477-1479 163
Page 1:
Brazilian Journal of Analytical Che
Page 4 and 5:
ERRATUM DA SILVA, W.T.L.; THOBIE-GA
Page 7 and 8:
Editorial Bo a rd Ed i t o r-in-Chi
Page 9 and 10: ExPEdiEnt www.brjac.com.br BrJAC is
Page 11 and 12: intErviEw www.brjac.com.br Br a z i
Page 13 and 14: has developed before the hardware,
Page 15 and 16: in yo u r o P i n i o n, w h a t is
Page 17 and 18: Ch l o r i n E d E t E r m i n a t
Page 19 and 20: www.brjac.com.br Ch l o r i n e det
Page 21 and 22: 4. Co n C l u s i o n s The propose
Page 23 and 24: The purpose of the present work is
Page 25 and 26: 3.2. Maximization of room-temperatu
Page 27 and 28: the standard deviation from 16 blan
Page 29 and 30: Br J Anal Chem 2011, 03, 131-135 Cl
Page 31 and 32: Closed-vessel m iC ro w a v e-assis
Page 33 and 34: Closed-vessel m iC ro w a v e-assis
Page 35 and 36: With the purpose of minimizing the
Page 37 and 38: taken to the laboratory and stored
Page 39 and 40: In the study of accuracy, recovery
Page 41 and 42: Br J Anal Chem 2011, 03, 143-147 dE
Page 43 and 44: ma samples in three cycles was stud
Page 45 and 46: spiking it with the analyte at the
Page 47 and 48: esearch, tourism and other human ac
Page 49 and 50: minimize detector saturation by Fe
Page 51 and 52: High Cu content in King George Isla
Page 53 and 54: Pl a C E / ma t r i x rEfErEnCE Pb.
Page 55 and 56: 30. Gáspár, A.; Berndt, H.; Spect
Page 57 and 58: An early approach to PAA determinat
Page 59: fi g u rE 2. EffECt o f rE a g E n
Page 63 and 64: analytes from environmental samples
Page 65 and 66: RT (min) 13.29 14.04 14.28 15.92 16
Page 67 and 68: Br J Anal Chem 2011, 03, 169-174 dE
Page 69 and 70: cm) pieces, mixed with dry ice to a
Page 71 and 72: An analytical curve was obtained in
Page 73 and 74: Po i n t o f viEw www.brjac.com.br
Page 75 and 76: Po i n t o f viEw go o d fast ChEaP
Page 77 and 78: PuBliCation rulEs BrJAC, the Brazil
Page 80: 24 Br J Anal Chem
show all

Brazilian Journal of Analytical Chemistry - BRJAC - Brazilian Journal ...

Create successful ePaper yourself

Delete template?

Save as template?