Simultaneous SIA analysis of pH and total acidity measurements in milk

  • Ibrahim Isildak
  • Alime Gul Gones
Original Paper


The development of a sequential injection analysis method for automatic determination of pH and total acidity in milk is proposed. For this purpose, firstly, three micro-sized composite pH electrodes were prepared and tested. A microliter dead volume flow-cell was designed for composite pH and reference electrodes. Potentiometric performance characteristics of the pH electrodes were examined by a computer-controlled potentiometric system in both stagnant and flowing environments. Three different micro-columns with the best working pH electrode were applied on the flowing stream line in the sequential injection analysis system to fulfill the titration efficiency for total acidity. The sequential injection analysis system was optimized for two parameters (pH and total acidity) by testing all the variables. Mobile phase concentration, volume and flow-rate together with sample concentration, volume and sample flow-rate were fixed for the best stable values by arranging the experimental programming steps. Total acidity of ten different milk samples was analyzed using the sequential injection analysis system developed. The same samples were also titrated in the classical way using phenolphthalein indicator for the comparison. The results of both methods analyzed statistically by SPSS software were found to be compatible with each other. pH analysis of ten different milk samples carried out by using the sequential injection analysis system were also measured with a glass electrode. The results obtained by both methods analyzed by SPSS were also found to be compatible with each other.


Sequential injection analysis Measurement of pH Measurements of total acidity Composite pH electrode Trimethylhydroquinone Potentiometric titration 



The authors would like to acknowledge the financial support of TUBITAK 2211- PhD Scholarship Program (Application Number: 1649B031306054).


  1. 1.
    D.Y. Güdemez, A research on light (diet) milk and dairy products, MSc Thesis, Graduate School of Natural and Applied Sciences Namık Kemal University (2007)Google Scholar
  2. 2.
    S. Dhakal, K. Chao, J. Qin, M. Kim, D. Chan, Raman spectral ımaging for quantitative contaminant evaluation in skim milk powder. Food Measure. 10, 374–386 (2016)CrossRefGoogle Scholar
  3. 3.
    K. Maijala, Cow milk and human development and well-being. Livest. Prod. Sci. 65, pp. 1–18 (2000)CrossRefGoogle Scholar
  4. 4.
    A.M.S. Meshref, W.A. Moselhy, Heavy metals and trace elements levels in milk and milk products. Food Measure. 8, 381–388 (2014)CrossRefGoogle Scholar
  5. 5.
    P.F. Fox, P.L.H. McWeeney, Advanced Dairy Chemistry, 3rd edn. (Springer Verlag, New York, 2003), pp. 1–40Google Scholar
  6. 6.
    Y.S. Gülbaş, UHT the effect of aseptic homogenization and storage temperature on gelation problem at different pressures in milk production and its investigation with artificial neural networks”, PhD. Thesis, Graduate School of Natural and Applied Sciences, Hacettepe University, 2007Google Scholar
  7. 7.
    M. Beykaya, Determination of physical, chemical and microbiological characteristics of milks from some dairy administrations in sivas province, Msc Thesis, Graduate School of Natural and Applied Sciences, Gaziosmanpaşa University, 2010Google Scholar
  8. 8.
    M. Metin, Milk Technology, Composition and Processing, 6th edn. (Ege Universty, İzmir, 2005), pp. 1–50Google Scholar
  9. 9.
    M. Üçüncü, A to Z Cheese Technology, 1st edn. (Meta, İzmir, 2008), pp. 45–67Google Scholar
  10. 10.
    V Bulletin, milk conservation techniques (Jelsoft Enterprises publishing web site, 2000),ünde-kalite-kontrolu-630.html, Accessed 3 Mar 2016
  11. 11.
    T.C. Official Newspaper, Turkish food codex raw milk and heat treated drinking milk communique, (23964), pp. 1–13 (2000)Google Scholar
  12. 12.
    P. Benjakul, C. Chuenarrom, Association of dental enamel loss with the ph and titratable acidity of beverages. J. Dent. Sci. 6, 129–133 (2011)CrossRefGoogle Scholar
  13. 13.
    A.M. Cairns, M. Watson, S.L. Creanor,, The pH and titratable acidity of a range of diluting drinks and their potential effect on dental. J. Dens. 30, 313–317 (2002)CrossRefGoogle Scholar
  14. 14.
    W.E. Morf, The Principles of Ion-Selective Electrodes and of Membrane Transport, 1nd edn. (Elsevier Scientific, Budapest,1981), pp. 165–425Google Scholar
  15. 15.
    R. Kellner, J.M. Mermet, M. Otto,, Analytical Chemistry, 2nd edn. (Wiley, Weinheim, 2004), pp. 201–225Google Scholar
  16. 16.
    H.,F. Ayyıldız, Development of oil analysis methods by automated flow ınjection systems, PhD Thesis, Graduate School of Natural and Applied Sciences, Selçuk University, 2010Google Scholar
  17. 17.
    S.D. Kolev, I.D. Mckelvie, Comprehensive Analytical Chemistry-Advances in Flow Injection Analysis and Related Techniques”, 1st edn. (Elsevier, Budapest, 2008), pp. 3–18Google Scholar
  18. 18.
    M. Kuşçu, Removal and pretreatment of lead from water samples by flow-ınjection analysis, PhD Thesis, Graduate School of Natural and Applied Sciences, Trakya University, 2008Google Scholar
  19. 19.
    J.F. Staden, R.I. Stefan, Chemical speciation by sequential injection analysis: an overview. Sci. Direct 64, 1109–1113 (2004)Google Scholar
  20. 20.
    F. Çoldur, “Design and Applications of Potentiometric Multiple Microscope System”, PhD Thesis, Graduate School of Natural and Applied Sciences, Ondokuz Mayıs University, 2010Google Scholar
  21. 21.
    R. Pe´rez-Olmos, J.C. Soto, N. Za´rate, Application of Sequential Injection Analysis (SIA) To Food Analysis. Food. Chem. 90, 471–490 (2005)CrossRefGoogle Scholar
  22. 22.
    A. Economou, Sequential-injection analysis (SIA): a useful tool for on-line sample-handling and pre-treatment”. Trends Anal. Chem. 24, 416–425 (2005)CrossRefGoogle Scholar
  23. 23.
    P.H. Gonc., A.D. Diniz, L.F. Almeida,, Flow-batch analysis. Trends Anal. Chem. 35, 39–49 (2012)CrossRefGoogle Scholar
  24. 24.
    J. Wang, H.E. Hansen, Sequential ınjection lab-on-valve: the third generation of flow ınjection analysis. Trends Anal. Chem. 22, 225–231 (2003)CrossRefGoogle Scholar
  25. 25.
    I. Isildak, C. Yigit, H. Bati, Construction and response characteristics of a sulfite/hydrogensulfite-selective all-solid-state contact electrode based on the 4-methylpiperidinedithiocarbamate complex of mercury(II). Analyst 121(12), 1873–1876 (1996)CrossRefGoogle Scholar
  26. 26.
    I. Isildak, All solid-state contact lead(II) ion-selective PVC membrane electrode using dimethylene bis(4-methylpiperidinedithiocarbamate) neutral ionophore. Turk. J. Chem. 24(4), 389–394 (2000)Google Scholar
  27. 27.
    M.F.S Teixeira, L.A. Ramos, E.A. Neves,, A solid Fe2O3 based carbon-epoxy electrode for potentiometric measurements of pH”. Portugaliae Electrochim. Acta 20, 139–149 (2002)CrossRefGoogle Scholar
  28. 28.
    G. Gostkiewicz, M. Sophocleous., J.K. Atkinsona. et al., Performance of miniaturised thick-film solid state pH sensors. Sens. Actuators 202, 2–7 (2013)CrossRefGoogle Scholar
  29. 29.
    M. Hosseini., R.B. Heydari, M. Alimoradi, A novel pH optical sensor using methyl orange based on triacetylcellulose membranes as support. Spectrochim. Acta 128, 864–867 (2014)CrossRefGoogle Scholar
  30. 30.
    H. Kahlert, R. Pçrksen, I. Isildak et al., Application of a new ph-sensitive electrode as a detector in flow injection potentiometry. Electroanalysis 17, 1085–1090 (2005)CrossRefGoogle Scholar
  31. 31.
    P.J. Fletcher, J.F. Staden, Determination of carbonate and hydrogencarbonate by titration using sequential injection analysis. Anal. Chim. Acta 485, 187–194 (2003)CrossRefGoogle Scholar
  32. 32.
    J.A. Vieiraa., I.M. Raimundo, B.F. Reisc et al., Monosegemented flow potentiometric titration for the determination of chloride in milk and wine. J. Braz. Chem. Soc. 14(2), 259–264 (2003)CrossRefGoogle Scholar
  33. 33.
    A.R. Berkem, Electrochemistry, 1st edn. (İstanbul University, İstanbul,1993), pp. 373–421Google Scholar
  34. 34.
    E. Eymen, SPSS 15.0 Data Analysis Methods, 1st edn. (İstatistik Merkezi, Ankara, (2009), pp. 50–83Google Scholar
  35. 35.
    N. Lenghor, J. Jakmunee, M. Vilen, etal., Sequential ınjection redox or acid-base titration for determination of ascorbic acid or acetic acid. Talanta 58, 1139–1144 (2002)CrossRefGoogle Scholar
  36. 36.
    J.E. Silva, M.F. Pimentel, V.L. Silva et al., Simultaneous determination of pH, chloride and nickel in electroplating baths using sequential injection analysis. Anal. Chim. Acta 506, 197–202 (2004)CrossRefGoogle Scholar
  37. 37.
    G. Theodoridis, C.K. Zacharis, P.D. Tzanavaras,, Automated sample preparation based on the sequential injection principle solid-phase extraction on a molecularly imprinted polymer coupled on-line to high-performance liquid chromatography. J. Chromatogr. 1030, 69–76 (2004)CrossRefGoogle Scholar
  38. 38.
    A.N. Anthemidis, G.A. Zachariadis, J.A. Stratis, Determination of arsenic(ııı) and total ınorganic arsenic in water samples using an on-line sequential ınsertion system and hydride generation atomic absorption spectrometry. Anal. Chim. Acta 547, 237–242 (2005)CrossRefGoogle Scholar

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© Springer Science+Business Media, LLC 2017

Authors and Affiliations

  1. 1.Department of Bioengineering, Faculty of Chemistry-MetallurgyYildiz Tecnical UniverstyIstanbulTurkey

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