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Consideration in potential titration paths to assay osmium compounds: toward the establishment of the mono-elemental standard solution

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Abstract

Demands for certified reference materials of osmium mono-element standard solutions are increasing to obtain reliable results in chemical instrument analyses. The International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH) issues the Guideline for Elemental Impurities (Q3D) and lists osmium as an elemental impurity to be measured. There are few reports on osmium standards although osmium is widely used as a catalyst and needed to measure. In the present paper, potential titration paths were explored to determine the mass fraction of osmium traceable to the International System of Units. Three stoichiometric reactions were examined to assay osmium compounds, and the availability was discussed. The presented discussions will contribute to establish first osmium mono-element standard solutions characterized by a metrologically valid procedure.

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Notes

  1. All osmium and ruthenium compounds are highly harmful to humans although several chemical forms of these compounds are commercially available. These materials should be handled with extreme caution.

References

  1. Tang B, Zhang H, Wang Y (2005) Flow injection kinetic spectrofluorimetric determination of trace amounts of osmium. Spectrochim Acta A 61:2239–2244

    Google Scholar 

  2. Khomutova EG, Ostanina OI (2011) A catalytic method for the determination of trace osmium in continuous flow and flow injection systems. J Anal Chem 66:522–527

    CAS  Google Scholar 

  3. Bazan JM (1987) Enhancement of osmium detection in inductively coupled plasma atomic emission spectrometry. Anal Chem 59:1066–1069

    CAS  Google Scholar 

  4. Hirata T, Akagi T, Shimizu H, Masuda A (1989) Determination of osmium and osmium isotope ratios by microelectrothermal vaporization inductively coupled plasma mass spectrometry. Anal Chem 61:2263–2266

    CAS  Google Scholar 

  5. Reddi GS, Rao CRM (1999) Analytical techniques for the determination of precious metals in geological and related materials. Analyst 124:1531–1540

    CAS  Google Scholar 

  6. Kolthoff IM, Parry EP (1953) Determination of osmium. Anal Chem 25:188–189

    CAS  Google Scholar 

  7. Locatelli C (2012) Simultaneous determination of osmium, ruthenium, copper and lead by electrocatalytic voltammetry—application to superficial waters. Microchem J 102:54–60

    CAS  Google Scholar 

  8. Ayres GH, Wells WN (1950) Spectrophotometric determination of osmium with thiourea. Anal Chem 22:317–320

    CAS  Google Scholar 

  9. Majumdar AK, Gupta JGS (1959) Spectrophotometric determination of osmium I. anthranilic acid as a reagent. Anal Chim Acta 20:532–539

    CAS  Google Scholar 

  10. Bera BC, Chakrabartty MM (1966) Spectrophotometric determination of osmium with 2-mercaptobenzothiazole. Microchem J 11:420–429

    CAS  Google Scholar 

  11. Jaya S, Ramakrishna TV (1982) Spectrophotometric determination of osmium with 1,5-diphenylcarbazide. Talanta 29:619–622

    CAS  Google Scholar 

  12. Gowda AT, Gowda HS (1984) Rapid spectrophotometric determination of osmium with perphenazine dihydrochloride. Analyst 109:651–653

    CAS  Google Scholar 

  13. National Institute of Standards and Technology (NIST) (2019) Standard reference materials (SRMs). NIST, MD. https://www.nist.gov/srm/. Accessed 11 Dec 2019

  14. European commission directorate general joint research centre (JRC), Geel (2018) Certified reference materials 2018. JRC, Geel

    Google Scholar 

  15. Bureau International des Poids et Mesures (BIPM) (2019) Calibration and measurement capabilities (CMCs). BIPM, Sèvres. https://kcdb.bipm.org/appendixC/. Accessed 11 Dec 2019

  16. Akiyama R, Kobayashi S (2009) “Microencapsulated” and related catalysts for organic chemistry and organic synthesis. Chem Rev 109:594–642

    CAS  PubMed  Google Scholar 

  17. Akiyama R, Matsuki N, Nomura H, Yoshida H, Yoshida T, Kobayashi S (2012) Nontoxic, nonvolatile, and highly efficient osmium catalysts for asymmetric dihydroxylation of alkenes and application to one mol-scale synthesis of an anticancer drug, camptothecin intermediate. RSC Adv 2:7456–7461

    CAS  Google Scholar 

  18. The International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH) (2014) ICH harmonised guideline, Guideline for elemental impurities, Q3D, Current Step 4 ver. ICH, Geneva

    Google Scholar 

  19. American Chemical Society (2000) ACS—specifications reagent chemicals, 9th edn. Oxford University Press, New York

    Google Scholar 

  20. Saxena OC (1967) New titrimetric microdetermination of osmium. Microchem J 12:609–611

    CAS  Google Scholar 

  21. Crowell WR, Kirschman HD (1929) The potentiometric determination of bromine, octavalent and quadrivalent osmium in hydrobromic acid solutions. J Am Chem Soc 51:1695–1702

    CAS  Google Scholar 

  22. Crowell WR, Baumbach HL (1935) The potentiometric determination of quadrivalent osmium with chromous sulfate. J Am Chem Soc 53:2607–2609

    Google Scholar 

  23. Meites L, Cover RE (1968) Standardization of osmium(VIII) solutions by potentiometric titration with chromium(II) sulfate. Anal Chem 40:209–210

    CAS  Google Scholar 

  24. Kaji S, Sawai O, Nunoura T (2015) 26th Japan society of material cycles and waste management meeting. Kyushu University, Fukuoka

    Google Scholar 

  25. Zaky M, Killa HM, Issa YM (1991) Some observations on the application of arsenite reduction to the potentiometric determination of osmium(VIII) and to the analysis of mixtures. Microchem J 44:54–58

    CAS  Google Scholar 

  26. Crowell WR, Kirschman HD (1929) The potentiometric determination of octavalent osmium. J Am Chem Soc 51:175–179

    CAS  Google Scholar 

  27. Zaky M, Issa YM (1984) Potentiometric determination of osmium(VIII) using hydrazine sulphate: analysis of binary and ternary mixtures. Analyst 109:1107–1108

    CAS  Google Scholar 

  28. Gilchrist R (1931) A method for the separation and gravimetric determination of osmium. J Res Bur Stand 6:421–448

    CAS  Google Scholar 

  29. Gilchrist R (1932) A new determination of the atomic weight of osmium. J Res Bur Stand 9:279–290

    CAS  Google Scholar 

  30. Hoffman I, Schweitzer JE, Ryan DE, Beamish FE (1953) Quantitative organic precipitants for osmium. Anal Chem 25:1091–1094

    CAS  Google Scholar 

  31. Meija J, Coplen TB, Berglund M, Brand WA, De Bièvre P, Gröning M, Holden N, Irrgeher J, Loss RD, Walczyk T, Prohaska T (2016) Atomic weights of the elements 2013 (IUPAC Technical Report). Pure Appl Chem 88:265–291

    CAS  Google Scholar 

  32. Murmann RK, Barnes CL (2002) Redetermination of the crystal structure of potassium trans-(dioxo)-tetra(hydroxo)osmate(VI), K2[Os(OH)4(O)2]. Z Kristallogr NCS 217:303–304

    CAS  Google Scholar 

  33. Bureau International des Poids et Mesures (BIPM) (2019) SI brochure: the international system of units (SI), 9th edn. BIPM, Sèvres

    Google Scholar 

  34. Asakai T, Hioki A (2012) Evaluation of the stability of iron(II) solutions by precise coulometric titration with electrogenerated cerium(IV). Anal Sci 28:601–605

    CAS  PubMed  Google Scholar 

  35. Asakai T, Hioki A (2013) Assay of high-purity sodium oxalate traceable to the international system of units by coulometric titration and gravimetric titration. Microchem J 108:24–31

    CAS  Google Scholar 

  36. Asakai T (2018) Chlorate ion standard solution established by multipath titration techniques. Microchem J 142:9–16

    CAS  Google Scholar 

  37. Asakai T, Kakihara Y, Kozuka Y, Hossaka S, Murayama M, Tanaka T (2006) Evaluation of certified reference materials for oxidation-reduction titration by precise coulometric titration and volumetric analysis. Anal Chim Acta 567:269–276

    CAS  Google Scholar 

  38. Asakai T, Hioki A (2012) Comparison of three electrochemical end-point detection methods to assay potassium dichromate by coulometric titration. Accred Qual Assur 17:45–52

    CAS  Google Scholar 

  39. Asakai T, Murayama M, Tanaka T (2007) Precise coulometric titration of sodium thiosulfate and development of potassium iodate as a redox standard. Talanta 73:346–351

    CAS  PubMed  Google Scholar 

  40. Asakai T, Hioki A (2011) Investigation of iodine liberation process in redox titration of potassium iodate with sodium thiosulfate. Anal Chim Acta 689:34–38

    CAS  PubMed  Google Scholar 

  41. Asakai T, Hioki A (2012) Precise coulometric titration of cerium(IV) as an oxidising agent with electrogenerated iron(II) and reliability in cerium(IV) standardisation with sodium thiosulfate. Anal Methods 4:3478–3483

    CAS  Google Scholar 

  42. Asakai T, Hioki A (2013) Potassium bromate assay by primary methods through iodine liberation reaction. Anal Methods 5:6240–6245

    CAS  Google Scholar 

  43. Asakai T, Hioki A (2014) SI traceable assay of periodate compounds. Accred Qual Assur 19:105–109

    CAS  Google Scholar 

  44. Asakai T, Hioki A (2015) Reliability in standardization of sodium thiosulfate with potassium dichromate. Microchem J 123:9–14

    CAS  Google Scholar 

  45. Lide DR (2005) CRC handbook of chemistry and physics, 2005–2006, 86th edn. CRC Press, Boca Raton

    Google Scholar 

  46. Asakai T, Hioki A (2010) Investigation on drying conditions and assays of amidosulfuric acid and sodium carbonate by acidimetric coulometric titration and gravimetric titration. Accred Qual Assur 15:391–399

    CAS  Google Scholar 

  47. Asakai T, Suzuki T, Miura T, Hioki A (2014) Certified reference material for ammonium ions in high-purity ammonium chloride: influence of pH on coulometric titration of ammonium ions with electrogenerated hypobromite. Microchem J 114:203–209

    CAS  Google Scholar 

  48. Asakai T (2020) Perchlorate ion standard solution: multipath titrimetric approach using three different stoichiometric reactions—towards the establishment of SI traceable chemical standards. Metrologia 57:035005

  49. Suzuki T, Miura T, Yamauchi Y, Cheong C, Asakai T, Ohata M (2020) Stability of standard solutions for metal and non-metal ion. Bunseki Kagaku, Tsukuba (submitted)

    Google Scholar 

  50. Vogl J, Kipphardt H, Richter S, Bremser W, Torres MRA, Manzano JVL, Buzoianu M, Hill S, Petrov P, Goenaga-Infante H, Sargent M, Fisicaro P, Labarraque G, Zhou T, Turk GC, Winchester M, Miura T, Methven B, Sturgeon R, Jährling R, Rienitz O, Mariassy M, Hankova Z, Sobina E, Krylov AI, Kustikov YA, Smirnov VV (2018) Establishing comparability and compatibility in the purity assessment of high purity zinc as demonstrated by the CCQM-P149 intercomparison. Metrologia 55:211–221

    CAS  Google Scholar 

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  1. National Metrology Institute of Japan, National Institute of Advanced Industrial Science and Technology, 1-1-1 Umezono, Tsukuba, Ibaraki, 305-8563, Japan

    Toshiaki Asakai

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Asakai, T. Consideration in potential titration paths to assay osmium compounds: toward the establishment of the mono-elemental standard solution. Accred Qual Assur 25, 293–302 (2020). https://doi.org/10.1007/s00769-020-01437-5

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