Abstract
Coulometric titrations with three electrochemical end-point detection methods were performed to assay potassium dichromate as a standard for oxidation–reduction titration. The assay as an oxidizing agent was carried out with ferrous ions produced by electrolytically reducing ferric ions. Three end-point detection methods were employed and compared with each other: constant potential amperometry, potentiometry, and constant voltage biamperometry (a dead-stop method). The last one was found to provide high accuracy in the coulometric titration of potassium dichromate. Solution form samples were also measured to confirm the possible existence of chromium(III) in potassium dichromate by both coulometric titration and ion-exchange chromatography with inductively coupled plasma time-of-flight mass spectrometry.
References
Kolthoff IM, Belcher R (1957) Volumetric analysis, volume III titration methods: oxidation-reduction reactions. Interscience publications, Inc., New York
American Chemical Society (2000) ACS—specifications reagent chemicals, 9th edn. Oxford University Press, New York
P. R. China Standard, GB 10731 (1989) Primary chemical—potassium dichromate (in Chinese), quality supervision and inspection and quarantine, Beijing
JIS K 8001 (2009) General rule for test methods of reagents (in Japanese). Japanese Industrial Standards Committee, Tokyo
JIS K 8005 (2006) Reference materials for volumetric analysis (in Japanese). Japanese Industrial Standards Committee, Tokyo
Asakai T, Murayama M (2008) Accred Qual Assur 13:351–360
Marinenko G, Taylor JK (1963) J Res Natl Bur Stand A67:453–459
Yoshimori T, Hino Y, Takeuchi T (1966) Jpn Anal (in Japanese) 15:1234–1238
Knoeck J, Diehl H (1969) Talanta 16:181–193
Yoshimori T, Matsubara I, Hirosawa K, Tanaka T (1970) Jpn Anal (in Japanese) 19:681–687
Champion CE, Marinenko G, Taylor JK, Schmidt WE (1970) Anal Chem 42:1210–1213
Sappenfield SA, Marinenko G, Hague JL (1972) NBS Special Publication 260-24
Yoshimori T, Tanaka T, Ogawa M, Horikoshi T (1973) Anal Chim Acta 63:351–357
Li Z, Shen Y (1978) Acta Metrol Sinica (in Chinese) 6:347–351
Yoshimori T, Kamijoh K (1982) Talanta 29:343–344
Pratt KW (1994) Anal Chim Acta 289:125–134
Asakai T, Kakihara Y, Kozuka Y, Hossaka S, Murayama M, Tanaka T (2006) Anal Chim Acta 567:269–276
Máriássy M, Pratt KW, Spitzer P (2009) Metrologia 46:199–213
Suzuki T, Ohata M, Hioki A, to be published elsewhere
IUPAC (2006) Pure Appl Chem 78:2051–2066
Lide DR (2005) CRC handbook of chemistry and physics, 86th edn, 2005–2006. CRC Press, Boca Raton
Mohr PJ, Taylor BN, Newell DB (2008) Rev Mod Phys 80:633–730
Asakai T, Hioki A (2010) Accred Qual Assur 15:391–399
Asakai T, Hioki A (2011) Anal Chim Acta 689:34–38
Yoshimori T, Tanaka T (1973) Jpn Anal (in Japanese) 22:1251–1260
Bard AJ, Faulkner LR (2001) Electrochemical methods—fundamentals and applications, 2nd edn. Wiley, New Jersey
Narukawa T, Riley KW, French DH, Chiba K (2007) Talanta 73:178–184
Acknowledgments
The authors thank Dr. M. Ohata (National Metrology Institute of Japan) for his support to obtain some of ICP-TOFMS spectra.
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Asakai, T., Hioki, A. Comparison of three electrochemical end-point detection methods to assay potassium dichromate by coulometric titration. Accred Qual Assur 17, 45–52 (2012). https://doi.org/10.1007/s00769-011-0834-6
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s00769-011-0834-6