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Talanta Determination of chloride in admixtures and aggregates for ...

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368 J. Junsomboon, J. Jakmunee / <strong>Talanta</strong> 76 (2008) 365–368or Y = 96.5X − 16.1 (r 2 = 0.989), respectively, were obta<strong>in</strong>ed. However,these ions are usually present <strong>in</strong> the sample at relativelylow concentrations compared to Cl − <strong>and</strong> do not significantly<strong>in</strong>terfere.3.3. Application to real samplesThe system was applied to cement aggregate <strong>and</strong> <strong>admixtures</strong>amples. The samples were prepared as described <strong>in</strong> Section 2.4.The contents <strong>of</strong> Cl − <strong>in</strong> the samples were calculated us<strong>in</strong>g a calibrationgraph (Y =57.6X − 23.3, r 2 = 0.9994) <strong>and</strong> were found <strong>in</strong> range<strong>of</strong> 8–113 mg L −1 , which were converted to % (w/w) <strong>of</strong> Cl − <strong>in</strong> samplesas summarized <strong>in</strong> Table 2. The analysis <strong>of</strong> aggregate samples bytitrimetric st<strong>and</strong>ard method [2] <strong>and</strong> admixture samples by potentiometrictitration st<strong>and</strong>ard method [3] was also carried out <strong>for</strong>comparison. The st<strong>and</strong>ard methods are applied <strong>for</strong> determ<strong>in</strong>ation<strong>of</strong> total halides, except F − , reported as Cl − content. The Cl − contentsobta<strong>in</strong>ed from the proposed method were <strong>in</strong> good agreementwith those from the st<strong>and</strong>ard methods, evaluat<strong>in</strong>g by t-test at 95%confidence level [20]. It should be noted that the proposed methodhas lower detection limit (0.0002%, w/w), so it can determ<strong>in</strong>e lowerlevel<strong>of</strong>Cl − <strong>in</strong> samples with good precision. It is also faster <strong>and</strong> consumedsmaller amounts <strong>of</strong> reagents. The permission level <strong>of</strong> Cl − <strong>in</strong>concrete <strong>admixtures</strong> by Thai Industrial St<strong>and</strong>ard (TIS 733–2530) is0.20 ± 0.01%, while British St<strong>and</strong>ard is 0.10%. The application <strong>of</strong> themethod could be extended to analysis <strong>of</strong> water used <strong>in</strong> prepar<strong>in</strong>g<strong>of</strong> cement.4. ConclusionA simple Cl − ISE <strong>and</strong> FI potentiometric method have beendeveloped <strong>for</strong> the determ<strong>in</strong>ation <strong>of</strong> water soluble Cl − content <strong>in</strong><strong>aggregates</strong> <strong>and</strong> <strong>admixtures</strong> <strong>for</strong> concrete. In comparison to the st<strong>and</strong>ardmethods, the developed method provided agreeable results,moreover it is lower cost, lower reagent consumption, faster<strong>and</strong> has lower detection limit. The system gave l<strong>in</strong>ear range <strong>of</strong>10–100 mg L −1 Cl − , detection limit <strong>of</strong> 2 mg L −1 Cl − , relative st<strong>and</strong>arddeviation <strong>of</strong> 0.6–1.2% <strong>and</strong> sample throughput <strong>of</strong> 60 h −1 ,whicharecomparable to the previous flow based systems, but with simpler<strong>in</strong> <strong>in</strong>strumentation <strong>and</strong> no use <strong>of</strong> toxic or expensive chemicals.AcknowledgementsWe thank the Center <strong>for</strong> Innovation <strong>in</strong> Chemistry: PostgraduateEducation <strong>and</strong> Research Program <strong>in</strong> Chemistry (PERCH-CIC), theCommission on Higher Education (CHE) <strong>and</strong> the Thail<strong>and</strong> ResearchFund (TRF) <strong>for</strong> f<strong>in</strong>ancial support.References[1] http://en.wikipedia.org/wiki/Re<strong>in</strong><strong>for</strong>ced concrete (access on 26/1/2008).[2] British St<strong>and</strong>ard: test<strong>in</strong>g <strong>aggregates</strong>, Part 117: method <strong>for</strong> determ<strong>in</strong>ation <strong>of</strong>water soluble <strong>chloride</strong> salts (BS 812: Part 117: 1988, Method A), British St<strong>and</strong>ardInstitution, 1988.[3] British St<strong>and</strong>ard: <strong>admixtures</strong> <strong>for</strong> concrete, mortar <strong>and</strong> grout – Test Methods– Part 10: determ<strong>in</strong>ation <strong>of</strong> water soluble <strong>chloride</strong> content (BS EN 480 – 10:1997), British St<strong>and</strong>ard Institution, 1997.[4] J.F. Liu, Y.D. Feng, G.B. Jiang, J. AOAC Int. 84 (2001) 1179.[5] J.F. Liu, G.B. Jiang, <strong>Talanta</strong> 54 (2001) 329.[6] J.F. van Staden, S.I. Tlowana, Fresenius J. Anal. Chem. 371 (2001) 396.[7] C.R. Silva, H.J. Vieira, L.S. Canaes, J.A. Nobrega, O. Fatibello-Filho, <strong>Talanta</strong> 65(2005) 965.[8] F. Maya, J.M. Estela, V. Cerda, <strong>Talanta</strong> 74 (2008) 1534.[9] R.B.R. Mesquita, S.M.V. Fern<strong>and</strong>es, A. Rangel, J. Environ. Monitor. 4 (2002) 458.[10] M. Zenki, Y. Iwadou, <strong>Talanta</strong> 58 (2002) 1055.[11] V.G. Bonifacio, L.C. Figueiredo-Filho, L.H. Marcol<strong>in</strong>o, O. Fatibello-Filho, <strong>Talanta</strong>72 (2007) 663.[12] A. Andrade-Eiroa, J.A. Erustes, R. Forteza, V. Cerda, J. Lima, Anal. Chim. Acta 467(2002) 25.[13] A.M. Pimenta, A.N. Araujo, M. Conceição, B.S.M. Montenegro, C. Pasqu<strong>in</strong>i,J.J.R. Rohwedder, I.M. Raimundo-Júnior, J. Pharm. Biomed. Anal. 36 (2004)49.[14] J.E. da Silva, M.F. Pimentel, V.L. da Silva, M.D. Montenegro, A.N. Araujo, Anal.Chim. Acta 506 (2004) 197.[15] A.N. Araujo, M. Montenegro, L. Kousalova, H. Sklenarova, P. Solich, R.P. Olmos,Anal. Chim. Acta 505 (2004) 161.[16] I.S. da Silva, E.M. Richter, C.L. do Lago, I.G.R. Gutz, A.A. Tanaka, L. Angnes, <strong>Talanta</strong>67 (2005) 651.[17] J. Jakmunee, L. Patimapornlert, S. Suteerapataranon, N. Lenghor, K. Grudpan,<strong>Talanta</strong> 65 (2005) 789.[18] W. Frenzel, Fresenius J. Anal. Chem. 335 (1989) 931.[19] T. Altunbulduk, H. Meier zu Koecker, W. Frenzel, Fresenius J. Anal. Chem. 351(1995) 593.[20] G.D. Christian, Analytical Chemistry, 6th ed., Wiley, New York, USA, 2004.

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